# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publication_text _journal_name_full 'Dalton Trans.' #TrackingRef '- ZZU1-Ms.cif' _journal_coden_Cambridge 0222 _ccdc_journal_manuscript_code ? _publ_contact_author_name 'Shuang-Quan Zang' _publ_contact_author_address ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China ; _publ_contact_author_email zangsqzg@zzu.edu.cn _publ_contact_author_phone +86-0371-67780136 _publ_contact_author_fax +86-0371-67780136 loop_ _publ_author_name _publ_author_address 'Shuang-Quan Zang' ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China ; 'Ya-Juan Fan' ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China ; 'Ran Liang' ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China ; 'Hong-Wei Hou' ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China ; 'Thomas C. W. Mak' ;Department of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, People's Republic of China Department of Chemistry, The Chinese University of Hong Kong, Shatin, New Territories, Shatin, New territories, Hong Kong SAR, P. R. China ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 774752' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H20 N2 O9 Zn2), 2(H2 O), 2(H0.50 O0.25), 2(H0.50 O0.25), 2(H0.50 O0.25)' _chemical_formula_sum 'C60 H47 N4 O21.50 Zn4' _chemical_formula_weight 1429.50 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_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4663(14) _cell_length_b 11.4985(14) _cell_length_c 12.4691(15) _cell_angle_alpha 93.944(2) _cell_angle_beta 108.388(2) _cell_angle_gamma 94.247(2) _cell_volume 1548.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 2.1505 _cell_measurement_theta_max 25.650 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 727 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_T_max 0.7183 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7905 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_sigmaI/netI 0.1518 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5402 _reflns_number_gt 2955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5402 _refine_ls_number_parameters 424 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1838 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.071 _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 0.22593(8) 1.05177(8) 0.55674(8) 0.0357(3) Uani 1 1 d . . . Zn2 Zn -0.03320(8) 0.33114(8) 0.43557(8) 0.0343(3) Uani 1 1 d . . . N1 N 0.9302(6) 1.2529(6) 1.2765(5) 0.0399(17) Uani 1 1 d . . . N2 N 0.3826(6) 0.9860(6) 0.6425(5) 0.0389(17) Uani 1 1 d . . . O1 O 0.1031(4) 0.8213(4) 0.5132(4) 0.0371(13) Uani 1 1 d . . . O2 O 0.1477(5) 0.9560(4) 0.4100(4) 0.0371(13) Uani 1 1 d . . . O3 O -0.1194(4) 0.9111(5) 0.3552(4) 0.0379(13) Uani 1 1 d . . . O4 O -0.2712(5) 0.7856(6) 0.2376(6) 0.0652(19) Uani 1 1 d . . . O5 O 0.3348(5) 0.7790(5) 0.4148(6) 0.0539(17) Uani 1 1 d . . . O6 O 0.0357(5) 0.4953(5) 0.3942(5) 0.0466(15) Uani 1 1 d . . . O7 O 0.1774(5) 0.5932(5) 0.5442(5) 0.0507(16) Uani 1 1 d . . . O8 O 0.1437(4) 0.3070(5) 0.5142(4) 0.0376(13) Uani 1 1 d . . . O9 O 0.2870(5) 0.1908(4) 0.4977(5) 0.0461(15) Uani 1 1 d . . . C1 C 0.1368(7) 0.6995(7) 0.2835(7) 0.0332(19) Uani 1 1 d . . . C2 C 0.0564(7) 0.7724(6) 0.3120(6) 0.0294(18) Uani 1 1 d . . . C3 C -0.0635(7) 0.7628(7) 0.2439(7) 0.039(2) Uani 1 1 d . . . C4 C -0.1046(7) 0.6892(7) 0.1406(7) 0.049(2) Uani 1 1 d . . . H4 H -0.1862 0.6853 0.0937 0.059 Uiso 1 1 calc R . . C5 C -0.0238(8) 0.6246(8) 0.1107(8) 0.056(3) Uani 1 1 d . . . H5 H -0.0488 0.5795 0.0410 0.067 Uiso 1 1 calc R . . C6 C 0.0945(8) 0.6251(7) 0.1824(7) 0.050(2) Uani 1 1 d . . . H6 H 0.1473 0.5756 0.1638 0.061 Uiso 1 1 calc R . . C7 C 0.2671(8) 0.6938(7) 0.3604(7) 0.040(2) Uani 1 1 d . . . C8 C 0.3119(7) 0.5722(7) 0.3719(6) 0.0334(19) Uani 1 1 d . . . C9 C 0.2500(7) 0.4876(6) 0.4150(6) 0.0316(18) Uani 1 1 d . . . C10 C 0.2955(7) 0.3792(6) 0.4318(6) 0.0344(19) Uani 1 1 d . . . C11 C 0.4002(7) 0.3549(7) 0.4017(7) 0.042(2) Uani 1 1 d . . . H11 H 0.4313 0.2827 0.4133 0.050 Uiso 1 1 calc R . . C12 C 0.4566(7) 0.4381(8) 0.3553(7) 0.048(2) Uani 1 1 d . . . H12 H 0.5236 0.4201 0.3327 0.057 Uiso 1 1 calc R . . C13 C 0.4156(7) 0.5479(7) 0.3414(7) 0.041(2) Uani 1 1 d . . . H13 H 0.4562 0.6045 0.3124 0.050 Uiso 1 1 calc R . . C14 C 0.1028(7) 0.8547(7) 0.4182(7) 0.0342(19) Uani 1 1 d . . . C15 C -0.1613(7) 0.8244(7) 0.2794(7) 0.039(2) Uani 1 1 d . . . C16 C 0.1438(8) 0.5251(7) 0.4526(8) 0.038(2) Uani 1 1 d . . . C17 C 0.2359(7) 0.2849(7) 0.4838(6) 0.0347(19) Uani 1 1 d . . . C18 C 0.8717(8) 1.3021(8) 1.1844(8) 0.055(3) Uani 1 1 d . . . H18 H 0.8549 1.3795 1.1921 0.066 Uiso 1 1 calc R . . C19 C 0.8340(9) 1.2419(8) 1.0757(7) 0.059(3) Uani 1 1 d . . . H19 H 0.7922 1.2796 1.0134 0.071 Uiso 1 1 calc R . . C20 C 0.8578(7) 1.1280(7) 1.0601(7) 0.042(2) Uani 1 1 d . . . C21 C 0.9210(7) 1.0792(7) 1.1564(7) 0.045(2) Uani 1 1 d . . . H21 H 0.9413 1.0027 1.1507 0.054 Uiso 1 1 calc R . . C22 C 0.9546(7) 1.1423(7) 1.2611(7) 0.042(2) Uani 1 1 d . . . H22 H 0.9964 1.1060 1.3246 0.050 Uiso 1 1 calc R . . C23 C 0.8159(8) 1.0616(8) 0.9441(7) 0.058(3) Uani 1 1 d . . . H23A H 0.8796 1.0755 0.9092 0.070 Uiso 1 1 calc R . . H23B H 0.7423 1.0929 0.8978 0.070 Uiso 1 1 calc R . . C24 C 0.7877(8) 0.9302(7) 0.9427(7) 0.057(3) Uani 1 1 d . . . H24A H 0.7308 0.9161 0.9849 0.068 Uiso 1 1 calc R . . H24B H 0.8635 0.8973 0.9814 0.068 Uiso 1 1 calc R . . C25 C 0.7320(7) 0.8665(8) 0.8240(8) 0.057(3) Uani 1 1 d . . . H25A H 0.7222 0.7829 0.8300 0.068 Uiso 1 1 calc R . . H25B H 0.7887 0.8802 0.7815 0.068 Uiso 1 1 calc R . . C26 C 0.6065(7) 0.9058(7) 0.7585(7) 0.044(2) Uani 1 1 d . . . C27 C 0.5989(7) 0.9915(8) 0.6861(7) 0.045(2) Uani 1 1 d . . . H27 H 0.6704 1.0229 0.6743 0.054 Uiso 1 1 calc R . . C28 C 0.4892(7) 1.0319(7) 0.6312(7) 0.039(2) Uani 1 1 d . . . H28 H 0.4878 1.0922 0.5850 0.047 Uiso 1 1 calc R . . C30 C 0.3884(8) 0.9006(8) 0.7104(8) 0.057(3) Uani 1 1 d . . . H30 H 0.3154 0.8670 0.7178 0.069 Uiso 1 1 calc R . . C31 C 0.4980(8) 0.8602(8) 0.7702(8) 0.060(3) Uani 1 1 d . . . H31 H 0.4983 0.8019 0.8184 0.072 Uiso 1 1 calc R . . O1W O 0.6886(7) 0.5285(7) 0.2453(6) 0.100(3) Uani 1 1 d . . . H1WA H 0.6833 0.6008 0.2365 0.120 Uiso 1 1 d R . . H1WB H 0.7430 0.5278 0.3099 0.120 Uiso 1 1 d R . . O2W O 0.4869(18) 0.7887(19) 0.0923(18) 0.050(6) Uani 0.25 1 d PU . . H2WA H 0.4627 0.7389 0.1300 0.059 Uiso 0.25 1 d PR . . H2WB H 0.5179 0.7487 0.0502 0.059 Uiso 0.25 1 d PR . . O3W O 0.476(2) 0.6154(17) 0.9295(17) 0.052(6) Uani 0.25 1 d PU . . H3WA H 0.5174 0.5710 0.9015 0.062 Uiso 0.25 1 d PR . . H3WB H 0.4189 0.6328 0.8723 0.062 Uiso 0.25 1 d PR . . O4W O 0.658(2) 0.463(2) 0.996(2) 0.066(7) Uani 0.25 1 d PU . . H4WA H 0.5867 0.4449 1.0001 0.079 Uiso 0.25 1 d PR . . H4WB H 0.6458 0.4760 0.9273 0.079 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0321(5) 0.0290(6) 0.0469(6) 0.0041(4) 0.0120(5) 0.0111(4) Zn2 0.0319(5) 0.0332(6) 0.0403(6) 0.0038(4) 0.0139(4) 0.0081(4) N1 0.047(4) 0.040(4) 0.040(4) 0.018(3) 0.019(4) 0.016(3) N2 0.035(4) 0.039(4) 0.042(4) 0.004(3) 0.009(3) 0.011(3) O1 0.038(3) 0.036(3) 0.039(3) 0.005(3) 0.014(3) 0.006(3) O2 0.046(3) 0.022(3) 0.048(4) 0.003(3) 0.021(3) 0.008(3) O3 0.038(3) 0.034(3) 0.044(4) 0.004(3) 0.015(3) 0.011(3) O4 0.039(4) 0.072(5) 0.077(5) -0.016(4) 0.011(4) 0.012(3) O5 0.046(4) 0.028(3) 0.089(5) 0.006(3) 0.024(4) 0.005(3) O6 0.031(3) 0.051(4) 0.063(4) 0.025(3) 0.017(3) 0.012(3) O7 0.049(4) 0.034(4) 0.082(5) 0.002(3) 0.041(4) 0.003(3) O8 0.029(3) 0.040(3) 0.047(4) 0.011(3) 0.013(3) 0.013(3) O9 0.043(3) 0.023(3) 0.080(5) 0.013(3) 0.027(3) 0.015(3) C1 0.036(4) 0.029(5) 0.039(5) 0.008(4) 0.015(4) 0.009(4) C2 0.037(4) 0.023(4) 0.032(5) 0.007(3) 0.015(4) 0.005(3) C3 0.048(5) 0.031(5) 0.045(5) -0.003(4) 0.022(4) 0.014(4) C4 0.041(5) 0.049(6) 0.053(6) -0.001(5) 0.007(5) 0.016(4) C5 0.060(6) 0.064(7) 0.037(6) -0.005(5) 0.003(5) 0.027(5) C6 0.064(6) 0.042(6) 0.054(6) 0.004(5) 0.027(5) 0.024(5) C7 0.050(5) 0.032(5) 0.051(6) 0.010(4) 0.034(5) 0.011(4) C8 0.038(4) 0.025(4) 0.040(5) 0.002(4) 0.017(4) 0.009(4) C9 0.034(4) 0.026(4) 0.039(5) 0.001(4) 0.016(4) 0.009(4) C10 0.045(5) 0.023(4) 0.036(5) 0.001(4) 0.014(4) 0.005(4) C11 0.036(5) 0.038(5) 0.053(6) 0.003(4) 0.014(4) 0.019(4) C12 0.041(5) 0.047(6) 0.068(6) 0.009(5) 0.031(5) 0.015(4) C13 0.035(5) 0.043(5) 0.053(6) 0.011(4) 0.023(4) 0.011(4) C14 0.029(4) 0.040(5) 0.038(5) 0.010(4) 0.012(4) 0.014(4) C15 0.035(5) 0.041(5) 0.041(5) 0.004(4) 0.008(4) 0.016(4) C16 0.052(6) 0.018(4) 0.050(6) 0.007(4) 0.025(5) 0.009(4) C17 0.043(5) 0.022(4) 0.035(5) -0.001(4) 0.006(4) 0.004(4) C18 0.084(7) 0.033(5) 0.052(6) 0.007(5) 0.023(6) 0.017(5) C19 0.091(7) 0.045(6) 0.031(5) 0.011(4) 0.002(5) 0.019(5) C20 0.046(5) 0.040(5) 0.042(5) 0.004(4) 0.016(4) 0.007(4) C21 0.059(6) 0.040(5) 0.038(5) 0.002(4) 0.015(5) 0.026(4) C22 0.042(5) 0.045(6) 0.037(5) 0.009(4) 0.008(4) 0.017(4) C23 0.065(6) 0.054(7) 0.050(6) 0.002(5) 0.010(5) 0.014(5) C24 0.060(6) 0.046(6) 0.051(6) 0.002(5) -0.004(5) 0.024(5) C25 0.052(5) 0.041(6) 0.064(7) 0.003(5) -0.005(5) 0.029(5) C26 0.039(5) 0.037(5) 0.048(6) -0.003(4) 0.002(4) 0.013(4) C27 0.035(5) 0.049(6) 0.048(6) 0.000(5) 0.008(4) 0.008(4) C28 0.040(5) 0.031(5) 0.042(5) 0.004(4) 0.008(4) 0.003(4) C30 0.042(5) 0.055(6) 0.081(7) 0.034(6) 0.022(5) 0.001(5) C31 0.046(6) 0.059(7) 0.076(7) 0.037(6) 0.011(5) 0.016(5) O1W 0.107(6) 0.080(6) 0.099(6) -0.002(5) 0.020(5) -0.005(5) O2W 0.039(7) 0.050(7) 0.051(7) -0.006(5) 0.003(5) 0.011(5) O3W 0.079(13) 0.022(11) 0.030(11) -0.004(9) -0.017(10) 0.021(10) O4W 0.063(8) 0.058(8) 0.070(8) -0.003(5) 0.011(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.933(5) 2_576 ? Zn1 O2 1.976(5) . ? Zn1 O9 1.978(5) 1_565 ? Zn1 N2 2.011(6) . ? Zn2 O7 2.000(5) 2_566 ? Zn2 O8 2.005(5) . ? Zn2 N1 2.023(7) 1_444 ? Zn2 O1 2.096(5) 2_566 ? Zn2 O6 2.150(5) . ? N1 C18 1.322(10) . ? N1 C22 1.336(10) . ? N1 Zn2 2.023(7) 1_666 ? N2 C30 1.332(10) . ? N2 C28 1.347(9) . ? O1 C14 1.269(9) . ? O1 Zn2 2.096(5) 2_566 ? O2 C14 1.262(9) . ? O3 C15 1.278(9) . ? O3 Zn1 1.933(5) 2_576 ? O4 C15 1.237(9) . ? O5 C7 1.219(9) . ? O6 C16 1.232(9) . ? O7 C16 1.273(9) . ? O7 Zn2 2.000(5) 2_566 ? O8 C17 1.267(8) . ? O9 C17 1.264(9) . ? O9 Zn1 1.978(5) 1_545 ? C1 C2 1.400(10) . ? C1 C6 1.400(10) . ? C1 C7 1.508(11) . ? C2 C3 1.361(10) . ? C2 C14 1.498(10) . ? C3 C4 1.416(10) . ? C3 C15 1.531(10) . ? C4 C5 1.353(11) . ? C4 H4 0.9300 . ? C5 C6 1.368(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.526(10) . ? C8 C9 1.395(10) . ? C8 C13 1.400(10) . ? C9 C10 1.390(10) . ? C9 C16 1.516(10) . ? C10 C11 1.407(10) . ? C10 C17 1.526(10) . ? C11 C12 1.374(11) . ? C11 H11 0.9300 . ? C12 C13 1.383(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 C19 1.399(11) . ? C18 H18 0.9300 . ? C19 C20 1.371(11) . ? C19 H19 0.9300 . ? C20 C21 1.373(11) . ? C20 C23 1.504(11) . ? C21 C22 1.375(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.520(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.523(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.533(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C31 1.369(11) . ? C26 C27 1.370(11) . ? C27 C28 1.361(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C30 C31 1.376(11) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? 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 O2 116.6(2) 2_576 . ? O3 Zn1 O9 112.8(2) 2_576 1_565 ? O2 Zn1 O9 97.9(2) . 1_565 ? O3 Zn1 N2 115.2(2) 2_576 . ? O2 Zn1 N2 109.3(2) . . ? O9 Zn1 N2 102.9(2) 1_565 . ? O7 Zn2 O8 143.3(2) 2_566 . ? O7 Zn2 N1 112.4(3) 2_566 1_444 ? O8 Zn2 N1 104.3(2) . 1_444 ? O7 Zn2 O1 87.4(2) 2_566 2_566 ? O8 Zn2 O1 94.0(2) . 2_566 ? N1 Zn2 O1 91.0(2) 1_444 2_566 ? O7 Zn2 O6 89.3(2) 2_566 . ? O8 Zn2 O6 86.6(2) . . ? N1 Zn2 O6 93.2(2) 1_444 . ? O1 Zn2 O6 175.4(2) 2_566 . ? C18 N1 C22 116.7(7) . . ? C18 N1 Zn2 123.0(6) . 1_666 ? C22 N1 Zn2 120.0(6) . 1_666 ? C30 N2 C28 117.7(7) . . ? C30 N2 Zn1 124.5(6) . . ? C28 N2 Zn1 117.9(6) . . ? C14 O1 Zn2 134.4(5) . 2_566 ? C14 O2 Zn1 114.4(5) . . ? C15 O3 Zn1 115.1(5) . 2_576 ? C16 O6 Zn2 112.0(5) . . ? C16 O7 Zn2 110.4(5) . 2_566 ? C17 O8 Zn2 136.0(5) . . ? C17 O9 Zn1 125.0(5) . 1_545 ? C2 C1 C6 119.5(7) . . ? C2 C1 C7 122.4(7) . . ? C6 C1 C7 118.1(7) . . ? C3 C2 C1 118.6(7) . . ? C3 C2 C14 121.9(7) . . ? C1 C2 C14 119.5(7) . . ? C2 C3 C4 121.3(7) . . ? C2 C3 C15 121.5(7) . . ? C4 C3 C15 117.1(7) . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.4(8) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.6(8) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O5 C7 C1 123.9(7) . . ? O5 C7 C8 119.7(8) . . ? C1 C7 C8 116.4(7) . . ? C9 C8 C13 121.0(7) . . ? C9 C8 C7 119.4(6) . . ? C13 C8 C7 119.6(7) . . ? C10 C9 C8 119.2(6) . . ? C10 C9 C16 123.5(7) . . ? C8 C9 C16 116.9(7) . . ? C9 C10 C11 119.7(7) . . ? C9 C10 C17 121.9(7) . . ? C11 C10 C17 118.4(7) . . ? C12 C11 C10 119.9(8) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.3(7) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 118.7(8) . . ? C12 C13 H13 120.7 . . ? C8 C13 H13 120.7 . . ? O2 C14 O1 121.7(7) . . ? O2 C14 C2 117.1(7) . . ? O1 C14 C2 121.1(7) . . ? O4 C15 O3 125.4(7) . . ? O4 C15 C3 119.3(7) . . ? O3 C15 C3 115.3(7) . . ? O6 C16 O7 124.8(7) . . ? O6 C16 C9 121.1(7) . . ? O7 C16 C9 114.0(7) . . ? O9 C17 O8 124.7(8) . . ? O9 C17 C10 116.3(7) . . ? O8 C17 C10 118.9(7) . . ? N1 C18 C19 122.5(8) . . ? N1 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 120.8(9) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 115.9(8) . . ? C19 C20 C23 121.4(8) . . ? C21 C20 C23 122.7(8) . . ? C20 C21 C22 120.7(8) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? N1 C22 C21 123.4(8) . . ? N1 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C20 C23 C24 114.9(8) . . ? C20 C23 H23A 108.6 . . ? C24 C23 H23A 108.6 . . ? C20 C23 H23B 108.6 . . ? C24 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? C23 C24 C25 114.0(8) . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C24 C25 C26 112.9(7) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C31 C26 C27 116.8(8) . . ? C31 C26 C25 122.6(8) . . ? C27 C26 C25 120.6(8) . . ? C28 C27 C26 121.6(8) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? N2 C28 C27 121.2(8) . . ? N2 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? N2 C30 C31 122.7(8) . . ? N2 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C26 C31 C30 119.9(8) . . ? C26 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? H1WA O1W H1WB 104.5 . . ? H2WA O2W H2WB 104.5 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N2 C30 47.0(8) 2_576 . . . ? O2 Zn1 N2 C30 -86.6(7) . . . . ? O9 Zn1 N2 C30 170.2(7) 1_565 . . . ? O3 Zn1 N2 C28 -132.5(5) 2_576 . . . ? O2 Zn1 N2 C28 93.9(6) . . . . ? O9 Zn1 N2 C28 -9.3(6) 1_565 . . . ? O3 Zn1 O2 C14 -62.8(5) 2_576 . . . ? O9 Zn1 O2 C14 176.7(5) 1_565 . . . ? N2 Zn1 O2 C14 70.0(5) . . . . ? O7 Zn2 O6 C16 127.3(5) 2_566 . . . ? O8 Zn2 O6 C16 -16.2(6) . . . . ? N1 Zn2 O6 C16 -120.3(6) 1_444 . . . ? O7 Zn2 O8 C17 -155.5(7) 2_566 . . . ? N1 Zn2 O8 C17 21.2(8) 1_444 . . . ? O1 Zn2 O8 C17 113.3(7) 2_566 . . . ? O6 Zn2 O8 C17 -71.2(7) . . . . ? C6 C1 C2 C3 4.4(11) . . . . ? C7 C1 C2 C3 -172.9(7) . . . . ? C6 C1 C2 C14 -178.0(7) . . . . ? C7 C1 C2 C14 4.6(11) . . . . ? C1 C2 C3 C4 -6.0(12) . . . . ? C14 C2 C3 C4 176.6(8) . . . . ? C1 C2 C3 C15 169.8(7) . . . . ? C14 C2 C3 C15 -7.6(12) . . . . ? C2 C3 C4 C5 2.0(13) . . . . ? C15 C3 C4 C5 -174.0(8) . . . . ? C3 C4 C5 C6 3.7(14) . . . . ? C4 C5 C6 C1 -5.2(14) . . . . ? C2 C1 C6 C5 1.1(12) . . . . ? C7 C1 C6 C5 178.5(8) . . . . ? C2 C1 C7 O5 -39.5(12) . . . . ? C6 C1 C7 O5 143.1(8) . . . . ? C2 C1 C7 C8 138.2(7) . . . . ? C6 C1 C7 C8 -39.2(10) . . . . ? O5 C7 C8 C9 117.2(8) . . . . ? C1 C7 C8 C9 -60.6(10) . . . . ? O5 C7 C8 C13 -61.5(11) . . . . ? C1 C7 C8 C13 120.7(8) . . . . ? C13 C8 C9 C10 2.6(11) . . . . ? C7 C8 C9 C10 -176.1(7) . . . . ? C13 C8 C9 C16 176.2(8) . . . . ? C7 C8 C9 C16 -2.5(11) . . . . ? C8 C9 C10 C11 -2.2(11) . . . . ? C16 C9 C10 C11 -175.3(8) . . . . ? C8 C9 C10 C17 177.1(6) . . . . ? C16 C9 C10 C17 3.9(12) . . . . ? C9 C10 C11 C12 -0.4(12) . . . . ? C17 C10 C11 C12 -179.7(7) . . . . ? C10 C11 C12 C13 2.7(13) . . . . ? C11 C12 C13 C8 -2.3(13) . . . . ? C9 C8 C13 C12 -0.4(12) . . . . ? C7 C8 C13 C12 178.3(8) . . . . ? Zn1 O2 C14 O1 3.6(9) . . . . ? Zn1 O2 C14 C2 -172.5(5) . . . . ? Zn2 O1 C14 O2 176.5(5) 2_566 . . . ? Zn2 O1 C14 C2 -7.6(11) 2_566 . . . ? C3 C2 C14 O2 -92.3(9) . . . . ? C1 C2 C14 O2 90.3(9) . . . . ? C3 C2 C14 O1 91.6(10) . . . . ? C1 C2 C14 O1 -85.8(9) . . . . ? Zn1 O3 C15 O4 21.0(11) 2_576 . . . ? Zn1 O3 C15 C3 -156.0(5) 2_576 . . . ? C2 C3 C15 O4 -156.2(8) . . . . ? C4 C3 C15 O4 19.8(12) . . . . ? C2 C3 C15 O3 21.1(12) . . . . ? C4 C3 C15 O3 -163.0(7) . . . . ? Zn2 O6 C16 O7 -94.6(8) . . . . ? Zn2 O6 C16 C9 89.5(8) . . . . ? Zn2 O7 C16 O6 -10.7(10) 2_566 . . . ? Zn2 O7 C16 C9 165.5(5) 2_566 . . . ? C10 C9 C16 O6 -82.5(11) . . . . ? C8 C9 C16 O6 104.2(9) . . . . ? C10 C9 C16 O7 101.1(9) . . . . ? C8 C9 C16 O7 -72.2(9) . . . . ? Zn1 O9 C17 O8 6.0(11) 1_545 . . . ? Zn1 O9 C17 C10 -177.2(4) 1_545 . . . ? Zn2 O8 C17 O9 -113.6(9) . . . . ? Zn2 O8 C17 C10 69.7(9) . . . . ? C9 C10 C17 O9 -178.3(7) . . . . ? C11 C10 C17 O9 1.0(11) . . . . ? C9 C10 C17 O8 -1.3(11) . . . . ? C11 C10 C17 O8 177.9(7) . . . . ? C22 N1 C18 C19 1.4(13) . . . . ? Zn2 N1 C18 C19 -172.3(7) 1_666 . . . ? N1 C18 C19 C20 -0.7(15) . . . . ? C18 C19 C20 C21 -0.7(13) . . . . ? C18 C19 C20 C23 178.9(8) . . . . ? C19 C20 C21 C22 1.4(13) . . . . ? C23 C20 C21 C22 -178.2(8) . . . . ? C18 N1 C22 C21 -0.7(12) . . . . ? Zn2 N1 C22 C21 173.2(6) 1_666 . . . ? C20 C21 C22 N1 -0.7(13) . . . . ? C19 C20 C23 C24 -150.0(9) . . . . ? C21 C20 C23 C24 29.6(12) . . . . ? C20 C23 C24 C25 173.6(7) . . . . ? C23 C24 C25 C26 -62.7(10) . . . . ? C24 C25 C26 C31 -84.2(10) . . . . ? C24 C25 C26 C27 94.5(10) . . . . ? C31 C26 C27 C28 1.9(13) . . . . ? C25 C26 C27 C28 -176.8(7) . . . . ? C30 N2 C28 C27 0.8(12) . . . . ? Zn1 N2 C28 C27 -179.7(6) . . . . ? C26 C27 C28 N2 -2.5(12) . . . . ? C28 N2 C30 C31 1.4(14) . . . . ? Zn1 N2 C30 C31 -178.1(7) . . . . ? C27 C26 C31 C30 0.2(14) . . . . ? C25 C26 C31 C30 178.9(8) . . . . ? N2 C30 C31 C26 -1.8(15) . . . . ? 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 H1WA O4 0.85 2.15 2.970(10) 162.8 1_655 O1W H1WB O7 0.85 2.36 3.081(10) 142.9 2_666 O2W H2WB O3W 0.85 1.99 2.71(3) 142.2 1_554 O3W H3WA O4W 0.85 2.20 2.79(3) 126.2 . O3W H3WB O1W 0.85 2.29 2.74(2) 112.9 2_666 O4W H4WA O3W 0.85 1.48 2.20(3) 141.4 2_667 O4W H4WA O3W 0.85 2.48 2.79(3) 102.6 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.097 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.145 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 774753' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H20 N4 O9 Zn2, H2 O' _chemical_formula_sum 'C31 H22 N4 O10 Zn2' _chemical_formula_weight 741.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9889(7) _cell_length_b 11.4124(7) _cell_length_c 12.3293(8) _cell_angle_alpha 80.8810(10) _cell_angle_beta 84.8950(10) _cell_angle_gamma 68.2990(10) _cell_volume 1417.69(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 2.1505 _cell_measurement_theta_max 25.650 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7421 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7247 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4929 _reflns_number_gt 3317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4929 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 0.96858(5) 0.35492(4) 0.43154(4) 0.02797(15) Uani 1 1 d . . . Zn2 Zn 1.17476(5) -0.07042(4) 0.35713(4) 0.03102(15) Uani 1 1 d . . . N1 N 0.2350(4) 0.0262(3) 0.2269(3) 0.0350(10) Uani 1 1 d . . . N2 N 0.2868(4) 0.1708(3) 0.1136(3) 0.0373(10) Uani 1 1 d . . . N3 N 0.8938(4) 0.2819(3) 0.1302(3) 0.0358(9) Uani 1 1 d . . . N4 N 0.9161(3) 0.3535(3) 0.2800(3) 0.0307(9) Uani 1 1 d . . . O1 O 1.1351(3) 0.3894(2) 0.3967(2) 0.0323(7) Uani 1 1 d . . . O2 O 1.1380(3) 0.4529(2) 0.5585(2) 0.0324(7) Uani 1 1 d . . . O3 O 1.1438(3) 0.6794(2) 0.4391(2) 0.0421(9) Uani 1 1 d . . . O4 O 1.2948(3) 0.7501(2) 0.3576(2) 0.0371(8) Uani 1 1 d . . . O5 O 1.4151(3) 0.0992(2) 0.4014(2) 0.0373(8) Uani 1 1 d . . . O6 O 1.0831(3) 0.1627(2) 0.4418(2) 0.0284(7) Uani 1 1 d . . . O7 O 1.2222(3) -0.0308(2) 0.4927(2) 0.0320(7) Uani 1 1 d . . . O8 O 1.0070(3) 0.0471(2) 0.6591(2) 0.0325(7) Uani 1 1 d . . . O9 O 0.9557(3) 0.1586(3) 0.8005(3) 0.0505(9) Uani 1 1 d . . . O1W O 0.8667(4) 0.4257(3) 0.8171(3) 0.0689(11) Uani 1 1 d . . . H1WA H 0.9032 0.3514 0.7974 0.083 Uiso 1 1 d R . . H1WB H 0.8582 0.4791 0.7586 0.083 Uiso 1 1 d R . . C1 C 1.4214(4) 0.2985(4) 0.4265(3) 0.0248(10) Uani 1 1 d . . . C2 C 1.3253(4) 0.4193(4) 0.4321(3) 0.0236(10) Uani 1 1 d . . . C3 C 1.3561(4) 0.5281(4) 0.3959(3) 0.0274(10) Uani 1 1 d . . . C4 C 1.4820(4) 0.5124(4) 0.3548(4) 0.0368(12) Uani 1 1 d . . . H4 H 1.5030 0.5839 0.3289 0.044 Uiso 1 1 calc R . . C5 C 1.5760(4) 0.3942(4) 0.3516(4) 0.0444(13) Uani 1 1 d . . . H5 H 1.6603 0.3862 0.3254 0.053 Uiso 1 1 calc R . . C6 C 1.5466(4) 0.2871(4) 0.3869(3) 0.0329(11) Uani 1 1 d . . . H6 H 1.6108 0.2069 0.3842 0.040 Uiso 1 1 calc R . . C7 C 1.3904(4) 0.1779(4) 0.4619(3) 0.0281(10) Uani 1 1 d . . . C8 C 1.3279(4) 0.1676(3) 0.5735(3) 0.0256(10) Uani 1 1 d . . . C9 C 1.2191(4) 0.1297(3) 0.5951(3) 0.0231(10) Uani 1 1 d . . . C10 C 1.1545(4) 0.1416(3) 0.6982(3) 0.0277(10) Uani 1 1 d . . . C11 C 1.2043(5) 0.1798(4) 0.7797(4) 0.0399(12) Uani 1 1 d . . . H11 H 1.1608 0.1882 0.8479 0.048 Uiso 1 1 calc R . . C12 C 1.3175(5) 0.2056(4) 0.7608(4) 0.0398(12) Uani 1 1 d . . . H12 H 1.3539 0.2250 0.8177 0.048 Uiso 1 1 calc R . . C13 C 1.3770(4) 0.2027(4) 0.6580(4) 0.0338(11) Uani 1 1 d . . . H13 H 1.4511 0.2245 0.6448 0.041 Uiso 1 1 calc R . . C14 C 1.1876(4) 0.4242(3) 0.4664(4) 0.0263(10) Uani 1 1 d . . . C15 C 1.2564(4) 0.6618(4) 0.3986(3) 0.0290(10) Uani 1 1 d . . . C16 C 1.1686(4) 0.0854(4) 0.5049(3) 0.0262(10) Uani 1 1 d . . . C17 C 1.0294(4) 0.1151(4) 0.7221(4) 0.0330(11) Uani 1 1 d . . . C18 C 0.2369(4) 0.1426(4) 0.2135(4) 0.0339(11) Uani 1 1 d . . . H18 H 0.2076 0.1978 0.2662 0.041 Uiso 1 1 calc R . . C19 C 0.3210(5) 0.0653(4) 0.0617(4) 0.0497(14) Uani 1 1 d . . . H19 H 0.3597 0.0556 -0.0082 0.060 Uiso 1 1 calc R . . C20 C 0.2875(5) -0.0218(4) 0.1317(4) 0.0506(15) Uani 1 1 d . . . H20 H 0.2986 -0.1027 0.1173 0.061 Uiso 1 1 calc R . . C21 C 0.3126(5) 0.2872(4) 0.0733(4) 0.0448(13) Uani 1 1 d . . . H21A H 0.2682 0.3504 0.1218 0.054 Uiso 1 1 calc R . . H21B H 0.2771 0.3207 0.0008 0.054 Uiso 1 1 calc R . . C22 C 0.4573(5) 0.2647(4) 0.0672(4) 0.0362(12) Uani 1 1 d . . . C23 C 0.5399(5) 0.1766(4) 0.1443(4) 0.0477(14) Uani 1 1 d . . . H23 H 0.5067 0.1299 0.1994 0.057 Uiso 1 1 calc R . . C24 C 0.6708(5) 0.1582(4) 0.1394(4) 0.0484(14) Uani 1 1 d . . . H24 H 0.7248 0.0984 0.1918 0.058 Uiso 1 1 calc R . . C25 C 0.7248(5) 0.2246(4) 0.0603(4) 0.0369(12) Uani 1 1 d . . . C26 C 0.6417(5) 0.3141(4) -0.0163(4) 0.0424(13) Uani 1 1 d . . . H26 H 0.6751 0.3616 -0.0705 0.051 Uiso 1 1 calc R . . C27 C 0.5095(5) 0.3333(4) -0.0129(4) 0.0447(13) Uani 1 1 d . . . H27 H 0.4552 0.3932 -0.0651 0.054 Uiso 1 1 calc R . . C28 C 0.8695(5) 0.2011(4) 0.0596(4) 0.0438(13) Uani 1 1 d . . . H28A H 0.9175 0.1123 0.0857 0.053 Uiso 1 1 calc R . . H28B H 0.9005 0.2197 -0.0150 0.053 Uiso 1 1 calc R . . C29 C 0.8868(5) 0.4053(4) 0.0996(4) 0.0573(16) Uani 1 1 d . . . H29 H 0.8745 0.4502 0.0291 0.069 Uiso 1 1 calc R . . C30 C 0.9011(5) 0.4486(4) 0.1912(4) 0.0514(14) Uani 1 1 d . . . H30 H 0.9010 0.5295 0.1945 0.062 Uiso 1 1 calc R . . C31 C 0.9107(4) 0.2564(4) 0.2381(4) 0.0316(11) Uani 1 1 d . . . H31 H 0.9178 0.1787 0.2794 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0276(3) 0.0256(3) 0.0294(3) -0.0065(2) 0.0012(2) -0.0075(2) Zn2 0.0381(3) 0.0238(3) 0.0332(3) -0.0053(2) 0.0023(3) -0.0138(2) N1 0.047(3) 0.029(2) 0.032(2) -0.0095(17) 0.008(2) -0.0179(19) N2 0.047(3) 0.035(2) 0.029(2) 0.0010(18) 0.005(2) -0.017(2) N3 0.043(2) 0.036(2) 0.029(2) -0.0056(18) -0.0040(19) -0.0143(19) N4 0.033(2) 0.024(2) 0.033(2) -0.0043(17) -0.0025(18) -0.0069(17) O1 0.0256(17) 0.0290(17) 0.043(2) -0.0113(14) -0.0007(15) -0.0088(14) O2 0.0386(19) 0.0234(16) 0.0295(18) -0.0037(13) 0.0075(15) -0.0067(14) O3 0.0308(19) 0.0267(18) 0.052(2) 0.0044(15) 0.0203(17) 0.0009(15) O4 0.044(2) 0.0206(17) 0.049(2) -0.0066(14) 0.0036(17) -0.0150(15) O5 0.049(2) 0.0266(17) 0.0376(19) -0.0149(14) 0.0081(16) -0.0127(15) O6 0.0345(18) 0.0197(16) 0.0288(17) -0.0012(13) -0.0083(15) -0.0067(14) O7 0.0406(19) 0.0142(15) 0.0403(19) -0.0069(13) -0.0095(15) -0.0058(14) O8 0.043(2) 0.0244(17) 0.0334(18) -0.0052(13) -0.0019(15) -0.0157(15) O9 0.060(2) 0.066(2) 0.036(2) -0.0196(17) 0.0121(19) -0.034(2) O1W 0.102(3) 0.061(2) 0.048(2) -0.0072(18) 0.001(2) -0.035(2) C1 0.025(2) 0.023(2) 0.025(2) -0.0038(18) 0.002(2) -0.008(2) C2 0.023(2) 0.023(2) 0.023(2) -0.0064(18) 0.001(2) -0.0057(19) C3 0.027(3) 0.025(2) 0.028(3) -0.0046(19) 0.004(2) -0.008(2) C4 0.033(3) 0.032(3) 0.046(3) -0.008(2) 0.005(2) -0.014(2) C5 0.026(3) 0.044(3) 0.063(4) -0.012(3) 0.016(3) -0.015(2) C6 0.026(3) 0.023(2) 0.044(3) -0.007(2) 0.001(2) -0.001(2) C7 0.025(3) 0.023(2) 0.033(3) -0.003(2) -0.007(2) -0.004(2) C8 0.028(3) 0.016(2) 0.029(3) -0.0014(18) -0.008(2) -0.0019(19) C9 0.027(2) 0.013(2) 0.026(2) -0.0015(17) -0.006(2) -0.0042(18) C10 0.037(3) 0.020(2) 0.028(3) 0.0005(19) -0.007(2) -0.013(2) C11 0.057(3) 0.041(3) 0.023(3) -0.002(2) -0.001(2) -0.021(3) C12 0.054(3) 0.045(3) 0.030(3) -0.004(2) -0.013(3) -0.027(3) C13 0.036(3) 0.029(3) 0.040(3) -0.004(2) -0.003(2) -0.015(2) C14 0.031(3) 0.011(2) 0.033(3) 0.0023(19) -0.004(2) -0.0051(19) C15 0.035(3) 0.023(2) 0.027(3) -0.0044(19) 0.001(2) -0.008(2) C16 0.033(3) 0.022(2) 0.027(3) -0.007(2) 0.010(2) -0.016(2) C17 0.042(3) 0.028(3) 0.027(3) 0.008(2) -0.006(2) -0.013(2) C18 0.039(3) 0.034(3) 0.032(3) -0.009(2) 0.005(2) -0.017(2) C19 0.077(4) 0.048(3) 0.031(3) -0.017(2) 0.013(3) -0.028(3) C20 0.080(4) 0.040(3) 0.042(3) -0.015(2) 0.011(3) -0.032(3) C21 0.054(3) 0.031(3) 0.047(3) 0.003(2) 0.007(3) -0.018(3) C22 0.044(3) 0.029(3) 0.036(3) -0.004(2) -0.001(2) -0.014(2) C23 0.055(4) 0.048(3) 0.047(3) 0.002(3) 0.000(3) -0.030(3) C24 0.068(4) 0.042(3) 0.036(3) 0.004(2) -0.012(3) -0.022(3) C25 0.050(3) 0.031(3) 0.036(3) -0.015(2) -0.002(3) -0.017(2) C26 0.056(4) 0.039(3) 0.036(3) 0.000(2) 0.002(3) -0.024(3) C27 0.050(3) 0.041(3) 0.045(3) 0.007(2) -0.007(3) -0.023(3) C28 0.055(4) 0.045(3) 0.036(3) -0.017(2) -0.003(3) -0.018(3) C29 0.088(5) 0.047(3) 0.044(3) 0.016(3) -0.022(3) -0.037(3) C30 0.077(4) 0.032(3) 0.049(3) 0.007(2) -0.025(3) -0.024(3) C31 0.033(3) 0.027(3) 0.034(3) -0.002(2) -0.006(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.006(3) . ? Zn1 O3 2.008(3) 2_766 ? Zn1 N4 2.008(4) . ? Zn1 O6 2.076(3) . ? Zn1 O2 2.087(3) 2_766 ? Zn2 O8 1.939(3) 2_756 ? Zn2 O7 1.959(3) . ? Zn2 O4 1.984(3) 1_545 ? Zn2 N1 2.006(3) 1_655 ? N1 C18 1.321(4) . ? N1 C20 1.363(5) . ? N1 Zn2 2.006(3) 1_455 ? N2 C18 1.344(5) . ? N2 C19 1.367(5) . ? N2 C21 1.461(4) . ? N3 C31 1.330(5) . ? N3 C29 1.374(5) . ? N3 C28 1.469(5) . ? N4 C31 1.317(5) . ? N4 C30 1.388(5) . ? O1 C14 1.263(5) . ? O2 C14 1.253(4) . ? O2 Zn1 2.087(3) 2_766 ? O3 C15 1.249(5) . ? O3 Zn1 2.008(3) 2_766 ? O4 C15 1.250(4) . ? O4 Zn2 1.984(3) 1_565 ? O5 C7 1.196(4) . ? O6 C16 1.251(5) . ? O7 C16 1.264(4) . ? O8 C17 1.277(5) . ? O8 Zn2 1.939(3) 2_756 ? O9 C17 1.245(5) . ? O1W H1WA 0.8584 . ? O1W H1WB 0.8543 . ? C1 C6 1.385(5) . ? C1 C2 1.400(5) . ? C1 C7 1.527(5) . ? C2 C3 1.401(5) . ? C2 C14 1.517(5) . ? C3 C4 1.388(5) . ? C3 C15 1.518(5) . ? C4 C5 1.366(5) . ? C4 H4 0.9300 . ? C5 C6 1.373(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.490(5) . ? C8 C13 1.390(5) . ? C8 C9 1.406(5) . ? C9 C10 1.400(5) . ? C9 C16 1.516(5) . ? C10 C11 1.384(5) . ? C10 C17 1.508(6) . ? C11 C12 1.373(6) . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.345(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.511(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.379(5) . ? C22 C23 1.383(6) . ? C23 C24 1.371(6) . ? C23 H23 0.9300 . ? C24 C25 1.369(6) . ? C24 H24 0.9300 . ? C25 C26 1.388(6) . ? C25 C28 1.511(6) . ? C26 C27 1.384(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.346(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 140.55(13) . 2_766 ? O1 Zn1 N4 100.72(13) . . ? O3 Zn1 N4 118.70(14) 2_766 . ? O1 Zn1 O6 87.05(10) . . ? O3 Zn1 O6 90.98(10) 2_766 . ? N4 Zn1 O6 90.46(12) . . ? O1 Zn1 O2 91.33(10) . 2_766 ? O3 Zn1 O2 85.64(10) 2_766 2_766 ? N4 Zn1 O2 97.00(12) . 2_766 ? O6 Zn1 O2 172.53(11) . 2_766 ? O8 Zn2 O7 118.07(12) 2_756 . ? O8 Zn2 O4 112.89(11) 2_756 1_545 ? O7 Zn2 O4 101.12(12) . 1_545 ? O8 Zn2 N1 109.31(14) 2_756 1_655 ? O7 Zn2 N1 109.59(13) . 1_655 ? O4 Zn2 N1 104.89(13) 1_545 1_655 ? C18 N1 C20 105.7(4) . . ? C18 N1 Zn2 129.9(3) . 1_455 ? C20 N1 Zn2 124.5(3) . 1_455 ? C18 N2 C19 107.0(3) . . ? C18 N2 C21 126.1(4) . . ? C19 N2 C21 126.6(4) . . ? C31 N3 C29 106.6(4) . . ? C31 N3 C28 127.0(4) . . ? C29 N3 C28 126.0(4) . . ? C31 N4 C30 104.8(4) . . ? C31 N4 Zn1 127.8(3) . . ? C30 N4 Zn1 126.5(3) . . ? C14 O1 Zn1 121.9(3) . . ? C14 O2 Zn1 117.0(2) . 2_766 ? C15 O3 Zn1 147.9(3) . 2_766 ? C15 O4 Zn2 119.8(3) . 1_565 ? C16 O6 Zn1 135.6(3) . . ? C16 O7 Zn2 113.3(3) . . ? C17 O8 Zn2 117.0(3) . 2_756 ? H1WA O1W H1WB 106.6 . . ? C6 C1 C2 120.0(3) . . ? C6 C1 C7 118.8(4) . . ? C2 C1 C7 121.2(4) . . ? C1 C2 C3 119.7(4) . . ? C1 C2 C14 116.7(3) . . ? C3 C2 C14 123.3(3) . . ? C4 C3 C2 118.5(4) . . ? C4 C3 C15 119.0(4) . . ? C2 C3 C15 122.5(4) . . ? C5 C4 C3 121.5(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.0(4) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O5 C7 C8 123.9(4) . . ? O5 C7 C1 120.5(4) . . ? C8 C7 C1 115.6(3) . . ? C13 C8 C9 119.3(4) . . ? C13 C8 C7 117.7(4) . . ? C9 C8 C7 123.0(4) . . ? C10 C9 C8 118.9(4) . . ? C10 C9 C16 121.3(4) . . ? C8 C9 C16 119.7(4) . . ? C11 C10 C9 120.0(4) . . ? C11 C10 C17 118.9(4) . . ? C9 C10 C17 121.1(4) . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 120.8(4) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O2 C14 O1 125.3(4) . . ? O2 C14 C2 121.3(4) . . ? O1 C14 C2 113.3(4) . . ? O3 C15 O4 123.6(4) . . ? O3 C15 C3 120.7(4) . . ? O4 C15 C3 115.7(4) . . ? O6 C16 O7 122.1(4) . . ? O6 C16 C9 120.8(3) . . ? O7 C16 C9 116.9(4) . . ? O9 C17 O8 124.2(4) . . ? O9 C17 C10 119.4(4) . . ? O8 C17 C10 116.4(4) . . ? N1 C18 N2 111.0(4) . . ? N1 C18 H18 124.5 . . ? N2 C18 H18 124.5 . . ? C20 C19 N2 106.3(4) . . ? C20 C19 H19 126.8 . . ? N2 C19 H19 126.8 . . ? C19 C20 N1 110.0(4) . . ? C19 C20 H20 125.0 . . ? N1 C20 H20 125.0 . . ? N2 C21 C22 112.2(4) . . ? N2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C27 C22 C23 118.5(5) . . ? C27 C22 C21 121.2(4) . . ? C23 C22 C21 120.2(4) . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 122.4(5) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 117.5(5) . . ? C24 C25 C28 120.1(5) . . ? C26 C25 C28 122.3(4) . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C22 C27 C26 120.7(5) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N3 C28 C25 110.3(4) . . ? N3 C28 H28A 109.6 . . ? C25 C28 H28A 109.6 . . ? N3 C28 H28B 109.6 . . ? C25 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 N3 106.8(4) . . ? C30 C29 H29 126.6 . . ? N3 C29 H29 126.6 . . ? C29 C30 N4 109.3(4) . . ? C29 C30 H30 125.4 . . ? N4 C30 H30 125.4 . . ? N4 C31 N3 112.5(4) . . ? N4 C31 H31 123.7 . . ? N3 C31 H31 123.7 . . ? 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 Zn1 N4 C31 113.6(4) . . . . ? O3 Zn1 N4 C31 -64.9(4) 2_766 . . . ? O6 Zn1 N4 C31 26.5(4) . . . . ? O2 Zn1 N4 C31 -153.8(4) 2_766 . . . ? O1 Zn1 N4 C30 -53.8(4) . . . . ? O3 Zn1 N4 C30 127.8(4) 2_766 . . . ? O6 Zn1 N4 C30 -140.9(4) . . . . ? O2 Zn1 N4 C30 38.9(4) 2_766 . . . ? O3 Zn1 O1 C14 -17.1(4) 2_766 . . . ? N4 Zn1 O1 C14 165.0(3) . . . . ? O6 Zn1 O1 C14 -105.1(3) . . . . ? O2 Zn1 O1 C14 67.6(3) 2_766 . . . ? O1 Zn1 O6 C16 67.1(4) . . . . ? O3 Zn1 O6 C16 -73.5(4) 2_766 . . . ? N4 Zn1 O6 C16 167.8(4) . . . . ? O8 Zn2 O7 C16 -64.1(3) 2_756 . . . ? O4 Zn2 O7 C16 172.2(2) 1_545 . . . ? N1 Zn2 O7 C16 61.9(3) 1_655 . . . ? C6 C1 C2 C3 0.9(6) . . . . ? C7 C1 C2 C3 -178.1(4) . . . . ? C6 C1 C2 C14 174.5(4) . . . . ? C7 C1 C2 C14 -4.5(6) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C14 C2 C3 C4 -172.9(4) . . . . ? C1 C2 C3 C15 179.4(4) . . . . ? C14 C2 C3 C15 6.2(6) . . . . ? C2 C3 C4 C5 -1.6(7) . . . . ? C15 C3 C4 C5 179.3(4) . . . . ? C3 C4 C5 C6 1.6(7) . . . . ? C4 C5 C6 C1 -0.3(7) . . . . ? C2 C1 C6 C5 -0.9(6) . . . . ? C7 C1 C6 C5 178.1(4) . . . . ? C6 C1 C7 O5 -51.8(6) . . . . ? C2 C1 C7 O5 127.2(5) . . . . ? C6 C1 C7 C8 128.8(4) . . . . ? C2 C1 C7 C8 -52.2(5) . . . . ? O5 C7 C8 C13 137.8(4) . . . . ? C1 C7 C8 C13 -42.8(5) . . . . ? O5 C7 C8 C9 -45.1(6) . . . . ? C1 C7 C8 C9 134.3(4) . . . . ? C13 C8 C9 C10 6.8(5) . . . . ? C7 C8 C9 C10 -170.2(4) . . . . ? C13 C8 C9 C16 -177.2(4) . . . . ? C7 C8 C9 C16 5.8(5) . . . . ? C8 C9 C10 C11 -5.4(6) . . . . ? C16 C9 C10 C11 178.7(4) . . . . ? C8 C9 C10 C17 173.8(3) . . . . ? C16 C9 C10 C17 -2.2(6) . . . . ? C9 C10 C11 C12 -0.5(6) . . . . ? C17 C10 C11 C12 -179.6(4) . . . . ? C10 C11 C12 C13 4.9(6) . . . . ? C11 C12 C13 C8 -3.3(6) . . . . ? C9 C8 C13 C12 -2.6(6) . . . . ? C7 C8 C13 C12 174.7(4) . . . . ? Zn1 O2 C14 O1 -93.8(4) 2_766 . . . ? Zn1 O2 C14 C2 90.9(4) 2_766 . . . ? Zn1 O1 C14 O2 -7.3(5) . . . . ? Zn1 O1 C14 C2 168.3(2) . . . . ? C1 C2 C14 O2 108.7(4) . . . . ? C3 C2 C14 O2 -77.8(5) . . . . ? C1 C2 C14 O1 -67.1(5) . . . . ? C3 C2 C14 O1 106.3(4) . . . . ? Zn1 O3 C15 O4 -126.7(5) 2_766 . . . ? Zn1 O3 C15 C3 53.7(7) 2_766 . . . ? Zn2 O4 C15 O3 1.1(6) 1_565 . . . ? Zn2 O4 C15 C3 -179.4(3) 1_565 . . . ? C4 C3 C15 O3 -177.1(4) . . . . ? C2 C3 C15 O3 3.9(6) . . . . ? C4 C3 C15 O4 3.3(6) . . . . ? C2 C3 C15 O4 -175.7(4) . . . . ? Zn1 O6 C16 O7 178.4(2) . . . . ? Zn1 O6 C16 C9 -5.8(6) . . . . ? Zn2 O7 C16 O6 7.4(5) . . . . ? Zn2 O7 C16 C9 -168.6(3) . . . . ? C10 C9 C16 O6 86.0(5) . . . . ? C8 C9 C16 O6 -89.9(5) . . . . ? C10 C9 C16 O7 -98.0(4) . . . . ? C8 C9 C16 O7 86.1(4) . . . . ? Zn2 O8 C17 O9 26.5(5) 2_756 . . . ? Zn2 O8 C17 C10 -154.0(3) 2_756 . . . ? C11 C10 C17 O9 18.8(6) . . . . ? C9 C10 C17 O9 -160.3(4) . . . . ? C11 C10 C17 O8 -160.7(4) . . . . ? C9 C10 C17 O8 20.2(5) . . . . ? C20 N1 C18 N2 0.8(5) . . . . ? Zn2 N1 C18 N2 179.2(3) 1_455 . . . ? C19 N2 C18 N1 -1.3(5) . . . . ? C21 N2 C18 N1 -175.2(4) . . . . ? C18 N2 C19 C20 1.4(6) . . . . ? C21 N2 C19 C20 175.2(4) . . . . ? N2 C19 C20 N1 -0.9(6) . . . . ? C18 N1 C20 C19 0.1(6) . . . . ? Zn2 N1 C20 C19 -178.4(3) 1_455 . . . ? C18 N2 C21 C22 106.7(5) . . . . ? C19 N2 C21 C22 -66.0(6) . . . . ? N2 C21 C22 C27 147.2(4) . . . . ? N2 C21 C22 C23 -34.6(6) . . . . ? C27 C22 C23 C24 -0.6(7) . . . . ? C21 C22 C23 C24 -178.8(4) . . . . ? C22 C23 C24 C25 0.2(7) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C23 C24 C25 C28 179.5(4) . . . . ? C24 C25 C26 C27 -0.8(7) . . . . ? C28 C25 C26 C27 -179.8(4) . . . . ? C23 C22 C27 C26 0.3(7) . . . . ? C21 C22 C27 C26 178.5(4) . . . . ? C25 C26 C27 C22 0.4(7) . . . . ? C31 N3 C28 C25 85.6(6) . . . . ? C29 N3 C28 C25 -85.5(5) . . . . ? C24 C25 C28 N3 -87.2(5) . . . . ? C26 C25 C28 N3 91.7(5) . . . . ? C31 N3 C29 C30 0.6(6) . . . . ? C28 N3 C29 C30 173.1(4) . . . . ? N3 C29 C30 N4 -0.5(6) . . . . ? C31 N4 C30 C29 0.2(6) . . . . ? Zn1 N4 C30 C29 169.9(3) . . . . ? C30 N4 C31 N3 0.2(5) . . . . ? Zn1 N4 C31 N3 -169.3(3) . . . . ? C29 N3 C31 N4 -0.5(5) . . . . ? C28 N3 C31 N4 -172.9(4) . . . . ? 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 H1WA O9 0.86 2.05 2.873(4) 159.5 . O1W H1WB O1 0.85 2.25 3.101(4) 172.5 2_766 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.444 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.096 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 774754' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H27 N3 O12 Zn2, H2 O' _chemical_formula_sum 'C35 H29 N3 O13 Zn2' _chemical_formula_weight 830.35 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_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.966(2) _cell_length_b 10.974(2) _cell_length_c 14.562(3) _cell_angle_alpha 84.32(3) _cell_angle_beta 87.14(3) _cell_angle_gamma 71.83(3) _cell_volume 1656.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2145 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.18 _exptl_crystal_description rectangle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7503 _exptl_absorpt_correction_T_max 0.7503 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16776 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5831 _reflns_number_gt 5412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.3540P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5831 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.85803(3) 0.35937(3) 0.111100(19) 0.02528(9) Uani 1 1 d . . . Zn2 Zn 0.93879(3) -0.09701(3) 0.179132(19) 0.02556(9) Uani 1 1 d . . . N1 N 0.8180(2) -0.0101(2) 0.28100(15) 0.0293(5) Uani 1 1 d . . . N2 N 0.3811(2) 0.2714(2) 0.83058(16) 0.0403(6) Uani 1 1 d . . . N3 N 0.7237(2) 0.3745(2) 0.22511(14) 0.0282(5) Uani 1 1 d . . . O1 O 1.1250(2) 0.7636(2) 0.32664(18) 0.0607(7) Uani 1 1 d . . . O2 O 0.98855(18) 0.72294(17) 0.23557(13) 0.0355(4) Uani 1 1 d . . . O3 O 1.12282(18) 0.49482(18) 0.13755(12) 0.0328(4) Uani 1 1 d . . . O4 O 0.96124(18) 0.42639(19) 0.19742(12) 0.0347(4) Uani 1 1 d . . . O5 O 1.0997(2) 0.12734(18) 0.33967(13) 0.0379(5) Uani 1 1 d . . . O6 O 0.95467(16) 0.16284(16) 0.15655(12) 0.0296(4) Uani 1 1 d . . . O7 O 1.08755(17) -0.03570(16) 0.15366(13) 0.0313(4) Uani 1 1 d . . . O8 O 1.11987(17) 0.11663(18) -0.05717(12) 0.0341(4) Uani 1 1 d . . . O9 O 1.29999(18) -0.04774(19) -0.04901(14) 0.0400(5) Uani 1 1 d . . . O1W O 0.76039(18) 0.54690(18) 0.04936(13) 0.0373(5) Uani 1 1 d . . . H1WA H 0.7229 0.6093 0.0813 0.045 Uiso 1 1 d R . . H1WB H 0.7975 0.5797 0.0055 0.045 Uiso 1 1 d R . . O2W O 0.99213(18) 0.34979(17) 0.00459(12) 0.0338(4) Uani 1 1 d . . . H2WA H 0.9634 0.4000 -0.0431 0.041 Uiso 1 1 d R . . H2WB H 1.0260 0.2765 -0.0157 0.041 Uiso 1 1 d R . . O3W O 0.7336(2) 0.29112(19) 0.04078(14) 0.0435(5) Uani 1 1 d . . . H3WA H 0.7409 0.2113 0.0477 0.052 Uiso 1 1 d R . . H3WB H 0.7304 0.3098 -0.0173 0.052 Uiso 1 1 d R . . O4W O 0.2853(3) 0.6357(3) 0.14155(17) 0.0770(9) Uani 1 1 d . . . H4WA H 0.2176 0.6236 0.1661 0.092 Uiso 1 1 d R . . H4WB H 0.2922 0.7002 0.1662 0.092 Uiso 1 1 d R . . C1 C 1.0710(3) 0.6913(3) 0.2991(2) 0.0342(6) Uani 1 1 d . . . C2 C 1.1037(2) 0.5558(2) 0.34543(18) 0.0287(6) Uani 1 1 d . . . C3 C 1.1333(3) 0.5392(3) 0.4382(2) 0.0387(7) Uani 1 1 d . . . H3 H 1.1319 0.6104 0.4684 0.046 Uiso 1 1 calc R . . C4 C 1.1647(3) 0.4202(3) 0.4866(2) 0.0436(7) Uani 1 1 d . . . H4 H 1.1835 0.4113 0.5489 0.052 Uiso 1 1 calc R . . C5 C 1.1682(3) 0.3130(3) 0.44210(18) 0.0367(7) Uani 1 1 d . . . H5 H 1.1906 0.2319 0.4743 0.044 Uiso 1 1 calc R . . C6 C 1.1382(2) 0.3271(2) 0.34923(17) 0.0267(5) Uani 1 1 d . . . C7 C 1.1035(2) 0.4491(2) 0.30054(16) 0.0242(5) Uani 1 1 d . . . C8 C 1.0591(2) 0.4593(2) 0.20281(17) 0.0239(5) Uani 1 1 d . . . C9 C 1.1448(2) 0.2085(2) 0.30264(17) 0.0258(5) Uani 1 1 d . . . C10 C 1.2176(2) 0.1897(2) 0.21208(17) 0.0240(5) Uani 1 1 d . . . C11 C 1.3286(2) 0.2265(3) 0.20152(19) 0.0303(6) Uani 1 1 d . . . H11A H 1.3496 0.2703 0.2468 0.036 Uiso 1 1 calc R . . C12 C 1.4077(3) 0.1985(3) 0.12458(19) 0.0341(6) Uani 1 1 d . . . H12A H 1.4827 0.2214 0.1187 0.041 Uiso 1 1 calc R . . C13 C 1.3746(2) 0.1361(2) 0.05642(18) 0.0296(6) Uani 1 1 d . . . H13 H 1.4291 0.1149 0.0055 0.036 Uiso 1 1 calc R . . C14 C 1.2607(2) 0.1047(2) 0.06307(17) 0.0245(5) Uani 1 1 d . . . C15 C 1.1823(2) 0.1288(2) 0.14191(16) 0.0223(5) Uani 1 1 d . . . C16 C 1.0641(2) 0.0855(2) 0.15134(16) 0.0230(5) Uani 1 1 d . . . C17 C 1.2258(2) 0.0497(2) -0.01948(17) 0.0265(5) Uani 1 1 d . . . C18 C 0.6911(3) 0.0357(3) 0.27566(19) 0.0377(7) Uani 1 1 d . . . H18 H 0.6533 0.0381 0.2194 0.045 Uiso 1 1 calc R . . C19 C 0.6131(3) 0.0798(3) 0.3503(2) 0.0414(7) Uani 1 1 d . . . H19 H 0.5246 0.1111 0.3435 0.050 Uiso 1 1 calc R . . C20 C 0.6654(3) 0.0781(3) 0.43532(19) 0.0332(6) Uani 1 1 d . . . C21 C 0.7983(3) 0.0322(3) 0.43962(19) 0.0368(6) Uani 1 1 d . . . H21 H 0.8386 0.0302 0.4947 0.044 Uiso 1 1 calc R . . C22 C 0.8702(3) -0.0103(3) 0.3625(2) 0.0366(6) Uani 1 1 d . . . H22 H 0.9591 -0.0406 0.3669 0.044 Uiso 1 1 calc R . . C23 C 0.5809(3) 0.1251(3) 0.5142(2) 0.0394(7) Uani 1 1 d . . . H23 H 0.4932 0.1553 0.5038 0.047 Uiso 1 1 calc R . . C24 C 0.6178(3) 0.1286(3) 0.5984(2) 0.0390(7) Uani 1 1 d . . . H24 H 0.7055 0.0973 0.6091 0.047 Uiso 1 1 calc R . . C25 C 0.5333(3) 0.1772(3) 0.67712(18) 0.0322(6) Uani 1 1 d . . . C26 C 0.5864(3) 0.1695(3) 0.76253(19) 0.0367(6) Uani 1 1 d . . . H26 H 0.6743 0.1326 0.7703 0.044 Uiso 1 1 calc R . . C27 C 0.5076(3) 0.2170(3) 0.8361(2) 0.0404(7) Uani 1 1 d . . . H27 H 0.5451 0.2105 0.8930 0.048 Uiso 1 1 calc R . . C28 C 0.3297(3) 0.2781(3) 0.7482(2) 0.0421(7) Uani 1 1 d . . . H28 H 0.2414 0.3152 0.7427 0.051 Uiso 1 1 calc R . . C29 C 0.4008(3) 0.2327(3) 0.6712(2) 0.0418(7) Uani 1 1 d . . . H29 H 0.3606 0.2391 0.6154 0.050 Uiso 1 1 calc R . . C30 C 0.5990(3) 0.4378(3) 0.21605(19) 0.0339(6) Uani 1 1 d . . . H30 H 0.5657 0.4571 0.1570 0.041 Uiso 1 1 calc R . . C31 C 0.5168(3) 0.4761(3) 0.29007(19) 0.0359(6) Uani 1 1 d . . . H31 H 0.4303 0.5196 0.2804 0.043 Uiso 1 1 calc R . . C32 C 0.5636(3) 0.4494(3) 0.37867(18) 0.0317(6) Uani 1 1 d . . . C33 C 0.6915(3) 0.3745(3) 0.38835(18) 0.0319(6) Uani 1 1 d . . . H33 H 0.7256 0.3473 0.4468 0.038 Uiso 1 1 calc R . . C34 C 0.7667(3) 0.3412(3) 0.31120(18) 0.0314(6) Uani 1 1 d . . . H34 H 0.8524 0.2929 0.3191 0.038 Uiso 1 1 calc R . . C35 C 0.4812(3) 0.5018(3) 0.45738(19) 0.0386(7) Uani 1 1 d . . . H35 H 0.3944 0.5413 0.4460 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02595(17) 0.02757(17) 0.02172(16) -0.00308(12) 0.00216(11) -0.00752(13) Zn2 0.02645(17) 0.02423(16) 0.02635(16) -0.00522(12) 0.00305(12) -0.00796(13) N1 0.0336(12) 0.0254(11) 0.0278(11) -0.0037(9) 0.0052(9) -0.0080(10) N2 0.0432(15) 0.0425(14) 0.0355(14) -0.0107(11) 0.0118(11) -0.0134(12) N3 0.0268(11) 0.0322(12) 0.0257(11) -0.0050(9) 0.0051(9) -0.0092(10) O1 0.0704(16) 0.0410(13) 0.0815(18) 0.0000(12) -0.0244(14) -0.0312(12) O2 0.0390(11) 0.0257(10) 0.0412(11) 0.0006(8) -0.0052(9) -0.0096(8) O3 0.0366(10) 0.0367(10) 0.0254(9) 0.0025(8) 0.0011(8) -0.0138(9) O4 0.0344(11) 0.0466(12) 0.0287(10) -0.0047(8) -0.0023(8) -0.0201(9) O5 0.0527(12) 0.0323(11) 0.0313(10) 0.0018(8) 0.0021(9) -0.0187(10) O6 0.0213(9) 0.0281(10) 0.0366(10) 0.0012(8) 0.0025(7) -0.0054(8) O7 0.0279(10) 0.0246(10) 0.0426(11) -0.0054(8) 0.0051(8) -0.0098(8) O8 0.0319(10) 0.0360(11) 0.0309(10) -0.0099(8) -0.0044(8) -0.0026(8) O9 0.0349(11) 0.0355(11) 0.0462(12) -0.0174(9) 0.0039(9) -0.0028(9) O1W 0.0440(12) 0.0294(10) 0.0304(10) -0.0019(8) 0.0102(8) -0.0016(9) O2W 0.0408(11) 0.0291(10) 0.0241(9) -0.0014(8) 0.0047(8) -0.0011(8) O3W 0.0603(14) 0.0387(11) 0.0361(11) -0.0025(9) -0.0105(10) -0.0207(10) O4W 0.0769(19) 0.130(3) 0.0512(15) 0.0027(16) -0.0075(13) -0.0734(19) C1 0.0342(15) 0.0273(14) 0.0420(16) -0.0067(12) 0.0016(12) -0.0101(12) C2 0.0252(13) 0.0291(14) 0.0324(14) -0.0043(11) -0.0014(11) -0.0088(11) C3 0.0430(17) 0.0387(16) 0.0365(16) -0.0118(13) -0.0067(13) -0.0121(14) C4 0.058(2) 0.0458(18) 0.0244(14) -0.0048(13) -0.0105(13) -0.0110(15) C5 0.0472(17) 0.0355(15) 0.0265(14) 0.0016(12) -0.0078(12) -0.0116(13) C6 0.0282(13) 0.0272(13) 0.0238(13) -0.0009(10) -0.0008(10) -0.0075(11) C7 0.0226(12) 0.0284(13) 0.0222(12) -0.0016(10) -0.0005(10) -0.0090(11) C8 0.0268(13) 0.0180(12) 0.0247(13) -0.0020(10) -0.0007(10) -0.0036(10) C9 0.0258(13) 0.0244(13) 0.0246(13) 0.0021(10) -0.0075(10) -0.0043(11) C10 0.0248(13) 0.0188(12) 0.0260(13) 0.0000(10) -0.0019(10) -0.0037(10) C11 0.0259(14) 0.0298(14) 0.0357(15) -0.0071(11) -0.0045(11) -0.0074(11) C12 0.0225(13) 0.0369(15) 0.0447(16) -0.0048(13) 0.0002(12) -0.0119(12) C13 0.0216(13) 0.0312(14) 0.0347(14) -0.0031(11) 0.0061(11) -0.0073(11) C14 0.0229(12) 0.0212(12) 0.0262(13) -0.0003(10) -0.0006(10) -0.0026(10) C15 0.0222(12) 0.0165(11) 0.0257(13) 0.0002(9) 0.0000(10) -0.0030(10) C16 0.0269(13) 0.0256(13) 0.0175(11) -0.0014(10) 0.0003(9) -0.0099(11) C17 0.0262(13) 0.0272(14) 0.0266(13) -0.0031(11) 0.0061(10) -0.0100(11) C18 0.0350(16) 0.0448(17) 0.0306(15) -0.0041(13) -0.0006(12) -0.0084(13) C19 0.0302(15) 0.0523(19) 0.0362(16) -0.0084(14) 0.0026(12) -0.0041(14) C20 0.0374(15) 0.0283(14) 0.0317(14) -0.0034(11) 0.0078(12) -0.0079(12) C21 0.0379(16) 0.0430(17) 0.0282(14) -0.0083(12) -0.0001(12) -0.0094(13) C22 0.0305(15) 0.0385(16) 0.0387(16) -0.0080(13) 0.0025(12) -0.0069(12) C23 0.0347(16) 0.0457(17) 0.0350(16) -0.0068(13) 0.0068(12) -0.0087(13) C24 0.0349(16) 0.0412(17) 0.0351(16) -0.0069(13) 0.0050(12) -0.0032(13) C25 0.0355(15) 0.0294(14) 0.0288(14) -0.0035(11) 0.0058(11) -0.0064(12) C26 0.0346(15) 0.0391(16) 0.0341(15) -0.0044(12) 0.0011(12) -0.0083(13) C27 0.0433(17) 0.0478(18) 0.0311(15) -0.0055(13) 0.0031(13) -0.0157(15) C28 0.0326(15) 0.0437(17) 0.0472(18) -0.0119(14) 0.0081(13) -0.0067(13) C29 0.0403(17) 0.0469(18) 0.0321(15) -0.0088(13) -0.0010(13) -0.0030(14) C30 0.0297(14) 0.0430(16) 0.0297(14) -0.0057(12) 0.0017(11) -0.0116(13) C31 0.0262(14) 0.0417(16) 0.0385(16) -0.0069(13) 0.0036(12) -0.0080(12) C32 0.0326(15) 0.0356(15) 0.0315(14) -0.0089(12) 0.0094(11) -0.0169(12) C33 0.0335(15) 0.0389(15) 0.0254(13) -0.0049(11) 0.0031(11) -0.0139(12) C34 0.0266(13) 0.0353(15) 0.0296(14) -0.0016(11) 0.0032(11) -0.0066(12) C35 0.0316(15) 0.0483(18) 0.0377(15) -0.0129(14) 0.0146(12) -0.0143(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 2.0606(19) . ? Zn1 O2W 2.0705(19) . ? Zn1 O3W 2.098(2) . ? Zn1 O1W 2.132(2) . ? Zn1 O6 2.1388(19) . ? Zn1 N3 2.147(2) . ? Zn2 O7 1.9560(18) . ? Zn2 O8 1.9723(18) 2_755 ? Zn2 O2 1.9819(19) 1_545 ? Zn2 N1 2.040(2) . ? N1 C18 1.328(4) . ? N1 C22 1.342(4) . ? N2 C27 1.331(4) . ? N2 C28 1.336(4) . ? N3 C30 1.334(3) . ? N3 C34 1.337(3) . ? O1 C1 1.232(3) . ? O2 C1 1.272(3) . ? O2 Zn2 1.9819(19) 1_565 ? O3 C8 1.254(3) . ? O4 C8 1.243(3) . ? O5 C9 1.218(3) . ? O6 C16 1.239(3) . ? O7 C16 1.271(3) . ? O8 C17 1.282(3) . ? O8 Zn2 1.9723(18) 2_755 ? O9 C17 1.226(3) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? C1 C2 1.514(4) . ? C2 C3 1.387(4) . ? C2 C7 1.397(4) . ? C3 C4 1.372(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 C7 1.400(3) . ? C6 C9 1.506(4) . ? C7 C8 1.509(3) . ? C9 C10 1.505(3) . ? C10 C11 1.394(4) . ? C10 C15 1.406(3) . ? C11 C12 1.381(4) . ? C11 H11A 0.9300 . ? C12 C13 1.382(4) . ? C12 H12A 0.9300 . ? C13 C14 1.392(4) . ? C13 H13 0.9300 . ? C14 C15 1.396(3) . ? C14 C17 1.513(4) . ? C15 C16 1.509(3) . ? C18 C19 1.378(4) . ? C18 H18 0.9300 . ? C19 C20 1.387(4) . ? C19 H19 0.9300 . ? C20 C21 1.388(4) . ? C20 C23 1.468(4) . ? C21 C22 1.374(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.318(4) . ? C23 H23 0.9300 . ? C24 C25 1.471(4) . ? C24 H24 0.9300 . ? C25 C26 1.383(4) . ? C25 C29 1.392(4) . ? C26 C27 1.380(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.377(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.381(4) . ? C30 H30 0.9300 . ? C31 C32 1.383(4) . ? C31 H31 0.9300 . ? C32 C33 1.393(4) . ? C32 C35 1.471(4) . ? C33 C34 1.370(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C35 1.320(6) 2_666 ? C35 H35 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O2W 92.47(8) . . ? O4 Zn1 O3W 171.14(8) . . ? O2W Zn1 O3W 96.37(8) . . ? O4 Zn1 O1W 93.59(8) . . ? O2W Zn1 O1W 86.20(8) . . ? O3W Zn1 O1W 87.58(8) . . ? O4 Zn1 O6 92.46(8) . . ? O2W Zn1 O6 89.67(8) . . ? O3W Zn1 O6 87.03(8) . . ? O1W Zn1 O6 172.81(7) . . ? O4 Zn1 N3 84.74(8) . . ? O2W Zn1 N3 177.16(8) . . ? O3W Zn1 N3 86.43(8) . . ? O1W Zn1 N3 93.43(8) . . ? O6 Zn1 N3 90.98(8) . . ? O7 Zn2 O8 105.37(8) . 2_755 ? O7 Zn2 O2 111.97(8) . 1_545 ? O8 Zn2 O2 101.37(8) 2_755 1_545 ? O7 Zn2 N1 114.48(8) . . ? O8 Zn2 N1 123.48(9) 2_755 . ? O2 Zn2 N1 99.06(9) 1_545 . ? C18 N1 C22 117.6(2) . . ? C18 N1 Zn2 125.03(19) . . ? C22 N1 Zn2 117.09(18) . . ? C27 N2 C28 116.7(2) . . ? C30 N3 C34 116.8(2) . . ? C30 N3 Zn1 122.29(18) . . ? C34 N3 Zn1 119.79(17) . . ? C1 O2 Zn2 117.79(17) . 1_565 ? C8 O4 Zn1 144.12(17) . . ? C16 O6 Zn1 137.72(16) . . ? C16 O7 Zn2 115.29(16) . . ? C17 O8 Zn2 126.35(16) . 2_755 ? Zn1 O1W H1WA 122.2 . . ? Zn1 O1W H1WB 118.8 . . ? H1WA O1W H1WB 104.5 . . ? Zn1 O2W H2WA 114.0 . . ? Zn1 O2W H2WB 116.5 . . ? H2WA O2W H2WB 104.5 . . ? Zn1 O3W H3WA 119.1 . . ? Zn1 O3W H3WB 116.0 . . ? H3WA O3W H3WB 104.5 . . ? H4WA O4W H4WB 104.5 . . ? O1 C1 O2 124.8(3) . . ? O1 C1 C2 117.5(3) . . ? O2 C1 C2 117.6(2) . . ? C3 C2 C7 119.2(2) . . ? C3 C2 C1 117.0(2) . . ? C7 C2 C1 123.8(2) . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.3(2) . . ? C5 C6 C9 118.5(2) . . ? C7 C6 C9 121.2(2) . . ? C2 C7 C6 119.3(2) . . ? C2 C7 C8 123.1(2) . . ? C6 C7 C8 117.5(2) . . ? O4 C8 O3 127.4(2) . . ? O4 C8 C7 113.2(2) . . ? O3 C8 C7 119.4(2) . . ? O5 C9 C10 121.3(2) . . ? O5 C9 C6 121.1(2) . . ? C10 C9 C6 117.4(2) . . ? C11 C10 C15 119.9(2) . . ? C11 C10 C9 117.8(2) . . ? C15 C10 C9 122.2(2) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 119.5(2) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 120.0(2) . . ? C13 C14 C17 116.9(2) . . ? C15 C14 C17 123.0(2) . . ? C14 C15 C10 119.0(2) . . ? C14 C15 C16 119.5(2) . . ? C10 C15 C16 121.5(2) . . ? O6 C16 O7 123.8(2) . . ? O6 C16 C15 122.1(2) . . ? O7 C16 C15 114.1(2) . . ? O9 C17 O8 124.5(2) . . ? O9 C17 C14 120.4(2) . . ? O8 C17 C14 114.9(2) . . ? N1 C18 C19 122.5(3) . . ? N1 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 116.3(3) . . ? C19 C20 C23 120.0(3) . . ? C21 C20 C23 123.7(3) . . ? C22 C21 C20 119.9(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N1 C22 C21 123.0(3) . . ? N1 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C20 126.1(3) . . ? C24 C23 H23 116.9 . . ? C20 C23 H23 116.9 . . ? C23 C24 C25 126.1(3) . . ? C23 C24 H24 117.0 . . ? C25 C24 H24 117.0 . . ? C26 C25 C29 116.9(3) . . ? C26 C25 C24 119.2(3) . . ? C29 C25 C24 123.8(3) . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? N2 C27 C26 123.9(3) . . ? N2 C27 H27 118.0 . . ? C26 C27 H27 118.0 . . ? N2 C28 C29 123.3(3) . . ? N2 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C25 119.8(3) . . ? C28 C29 H29 120.1 . . ? C25 C29 H29 120.1 . . ? N3 C30 C31 123.2(3) . . ? N3 C30 H30 118.4 . . ? C31 C30 H30 118.4 . . ? C30 C31 C32 119.7(3) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 116.8(2) . . ? C31 C32 C35 120.5(3) . . ? C33 C32 C35 122.7(3) . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? N3 C34 C33 123.6(3) . . ? N3 C34 H34 118.2 . . ? C33 C34 H34 118.2 . . ? C35 C35 C32 126.2(4) 2_666 . ? C35 C35 H35 116.9 2_666 . ? C32 C35 H35 116.9 . . ? 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 Zn2 N1 C18 133.3(2) . . . . ? O8 Zn2 N1 C18 2.7(3) 2_755 . . . ? O2 Zn2 N1 C18 -107.5(2) 1_545 . . . ? O7 Zn2 N1 C22 -53.3(2) . . . . ? O8 Zn2 N1 C22 176.12(18) 2_755 . . . ? O2 Zn2 N1 C22 66.0(2) 1_545 . . . ? O4 Zn1 N3 C30 128.0(2) . . . . ? O3W Zn1 N3 C30 -52.7(2) . . . . ? O1W Zn1 N3 C30 34.7(2) . . . . ? O6 Zn1 N3 C30 -139.7(2) . . . . ? O4 Zn1 N3 C34 -39.4(2) . . . . ? O3W Zn1 N3 C34 140.0(2) . . . . ? O1W Zn1 N3 C34 -132.7(2) . . . . ? O6 Zn1 N3 C34 53.0(2) . . . . ? O2W Zn1 O4 C8 2.2(3) . . . . ? O1W Zn1 O4 C8 -84.2(3) . . . . ? O6 Zn1 O4 C8 91.9(3) . . . . ? N3 Zn1 O4 C8 -177.3(3) . . . . ? O4 Zn1 O6 C16 -67.5(2) . . . . ? O2W Zn1 O6 C16 24.9(2) . . . . ? O3W Zn1 O6 C16 121.3(3) . . . . ? N3 Zn1 O6 C16 -152.3(2) . . . . ? O8 Zn2 O7 C16 96.20(18) 2_755 . . . ? O2 Zn2 O7 C16 -154.45(17) 1_545 . . . ? N1 Zn2 O7 C16 -42.7(2) . . . . ? Zn2 O2 C1 O1 -2.0(4) 1_565 . . . ? Zn2 O2 C1 C2 176.89(17) 1_565 . . . ? O1 C1 C2 C3 32.4(4) . . . . ? O2 C1 C2 C3 -146.6(3) . . . . ? O1 C1 C2 C7 -148.6(3) . . . . ? O2 C1 C2 C7 32.5(4) . . . . ? C7 C2 C3 C4 1.1(4) . . . . ? C1 C2 C3 C4 -179.8(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C4 C5 C6 C9 179.1(3) . . . . ? C3 C2 C7 C6 -2.5(4) . . . . ? C1 C2 C7 C6 178.5(2) . . . . ? C3 C2 C7 C8 173.3(2) . . . . ? C1 C2 C7 C8 -5.7(4) . . . . ? C5 C6 C7 C2 2.2(4) . . . . ? C9 C6 C7 C2 -177.4(2) . . . . ? C5 C6 C7 C8 -173.9(2) . . . . ? C9 C6 C7 C8 6.5(3) . . . . ? Zn1 O4 C8 O3 21.4(5) . . . . ? Zn1 O4 C8 C7 -156.6(2) . . . . ? C2 C7 C8 O4 -114.9(3) . . . . ? C6 C7 C8 O4 61.1(3) . . . . ? C2 C7 C8 O3 67.0(3) . . . . ? C6 C7 C8 O3 -117.1(3) . . . . ? C5 C6 C9 O5 45.0(4) . . . . ? C7 C6 C9 O5 -135.4(3) . . . . ? C5 C6 C9 C10 -130.7(3) . . . . ? C7 C6 C9 C10 48.9(3) . . . . ? O5 C9 C10 C11 -138.6(3) . . . . ? C6 C9 C10 C11 37.0(3) . . . . ? O5 C9 C10 C15 36.8(4) . . . . ? C6 C9 C10 C15 -147.6(2) . . . . ? C15 C10 C11 C12 -3.0(4) . . . . ? C9 C10 C11 C12 172.6(2) . . . . ? C10 C11 C12 C13 1.6(4) . . . . ? C11 C12 C13 C14 1.9(4) . . . . ? C12 C13 C14 C15 -4.0(4) . . . . ? C12 C13 C14 C17 173.6(2) . . . . ? C13 C14 C15 C10 2.6(3) . . . . ? C17 C14 C15 C10 -174.9(2) . . . . ? C13 C14 C15 C16 -175.5(2) . . . . ? C17 C14 C15 C16 7.0(3) . . . . ? C11 C10 C15 C14 0.9(3) . . . . ? C9 C10 C15 C14 -174.5(2) . . . . ? C11 C10 C15 C16 179.0(2) . . . . ? C9 C10 C15 C16 3.6(3) . . . . ? Zn1 O6 C16 O7 -152.47(19) . . . . ? Zn1 O6 C16 C15 27.7(4) . . . . ? Zn2 O7 C16 O6 -6.1(3) . . . . ? Zn2 O7 C16 C15 173.69(15) . . . . ? C14 C15 C16 O6 -117.6(3) . . . . ? C10 C15 C16 O6 64.3(3) . . . . ? C14 C15 C16 O7 62.6(3) . . . . ? C10 C15 C16 O7 -115.5(3) . . . . ? Zn2 O8 C17 O9 -9.6(4) 2_755 . . . ? Zn2 O8 C17 C14 166.12(16) 2_755 . . . ? C13 C14 C17 O9 57.0(3) . . . . ? C15 C14 C17 O9 -125.5(3) . . . . ? C13 C14 C17 O8 -118.9(3) . . . . ? C15 C14 C17 O8 58.6(3) . . . . ? C22 N1 C18 C19 -1.2(4) . . . . ? Zn2 N1 C18 C19 172.2(2) . . . . ? N1 C18 C19 C20 0.1(5) . . . . ? C18 C19 C20 C21 1.1(4) . . . . ? C18 C19 C20 C23 -179.8(3) . . . . ? C19 C20 C21 C22 -1.0(4) . . . . ? C23 C20 C21 C22 179.8(3) . . . . ? C18 N1 C22 C21 1.2(4) . . . . ? Zn2 N1 C22 C21 -172.7(2) . . . . ? C20 C21 C22 N1 -0.1(5) . . . . ? C19 C20 C23 C24 179.8(3) . . . . ? C21 C20 C23 C24 -1.1(5) . . . . ? C20 C23 C24 C25 179.1(3) . . . . ? C23 C24 C25 C26 177.4(3) . . . . ? C23 C24 C25 C29 -3.2(5) . . . . ? C29 C25 C26 C27 -0.5(4) . . . . ? C24 C25 C26 C27 179.0(3) . . . . ? C28 N2 C27 C26 0.7(4) . . . . ? C25 C26 C27 N2 -0.2(5) . . . . ? C27 N2 C28 C29 -0.4(5) . . . . ? N2 C28 C29 C25 -0.4(5) . . . . ? C26 C25 C29 C28 0.8(4) . . . . ? C24 C25 C29 C28 -178.7(3) . . . . ? C34 N3 C30 C31 4.1(4) . . . . ? Zn1 N3 C30 C31 -163.6(2) . . . . ? N3 C30 C31 C32 0.4(4) . . . . ? C30 C31 C32 C33 -5.3(4) . . . . ? C30 C31 C32 C35 173.1(3) . . . . ? C31 C32 C33 C34 5.8(4) . . . . ? C35 C32 C33 C34 -172.5(3) . . . . ? C30 N3 C34 C33 -3.5(4) . . . . ? Zn1 N3 C34 C33 164.5(2) . . . . ? C32 C33 C34 N3 -1.5(4) . . . . ? C31 C32 C35 C35 -170.2(4) . . . 2_666 ? C33 C32 C35 C35 8.1(6) . . . 2_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4W H4WA O2 0.85 2.60 3.355(3) 148.0 1_455 O4W H4WA O3 0.85 2.08 2.705(3) 129.9 1_455 O3W H3WB O4W 0.85 1.85 2.696(3) 175.1 2_665 O3W H3WA O9 0.85 1.98 2.798(3) 161.3 2_755 O2W H2WB O8 0.85 1.88 2.723(3) 173.1 . O2W H2WA O3 0.85 1.80 2.646(3) 170.6 2_765 O1W H1WB O2W 0.85 2.65 3.286(3) 133.1 2_765 O1W H1WB O3 0.85 2.34 2.965(3) 130.5 2_765 O1W H1WA N2 0.85 1.98 2.816(3) 167.9 2_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.962 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.059 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 774755' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 N2 O10 Zn2' _chemical_formula_sum 'C27 H16 N2 O10 Zn2' _chemical_formula_weight 659.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0753(7) _cell_length_b 8.7427(6) _cell_length_c 24.9801(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.0080(10) _cell_angle_gamma 90.00 _cell_volume 2400.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 2.1505 _cell_measurement_theta_max 25.650 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7073 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11731 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4225 _reflns_number_gt 2678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4225 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 0.37547(5) 0.95394(6) 0.47317(2) 0.02289(17) Uani 1 1 d . . . Zn2 Zn 0.59289(5) 0.77089(7) 0.41483(2) 0.02958(19) Uani 1 1 d . . . N1 N 0.2025(3) 1.0630(4) 0.46575(16) 0.0258(10) Uani 1 1 d . . . N2 N -0.2909(3) 1.5860(5) 0.42755(17) 0.0290(11) Uani 1 1 d . . . O1 O 0.2952(3) 0.7801(4) 0.42089(12) 0.0246(8) Uani 1 1 d . . . O2 O 0.4439(3) 0.7055(4) 0.37187(13) 0.0297(9) Uani 1 1 d . . . O3 O 0.1274(3) 0.8959(4) 0.31494(15) 0.0418(10) Uani 1 1 d . . . O4 O -0.0155(3) 0.7773(4) 0.35599(17) 0.0498(11) Uani 1 1 d . . . H4 H -0.0610 0.8469 0.3443 0.075 Uiso 1 1 calc R . . O5 O 0.4353(3) 0.3963(4) 0.42264(14) 0.0331(9) Uani 1 1 d . . . O6 O 0.4496(3) 0.0609(4) 0.41012(12) 0.0255(8) Uani 1 1 d . . . O7 O 0.6369(3) 0.1261(4) 0.45023(12) 0.0247(8) Uani 1 1 d . . . O8 O 0.6882(3) -0.1094(4) 0.36817(13) 0.0345(9) Uani 1 1 d . . . O9 O 0.8491(3) 0.0065(4) 0.34295(16) 0.0495(11) Uani 1 1 d . . . O10 O 0.5495(3) 0.8420(4) 0.48242(12) 0.0257(8) Uani 1 1 d . . . H10A H 0.5467 0.7687 0.5027 0.031 Uiso 1 1 d R . . C1 C 0.3025(4) 0.4446(5) 0.34322(18) 0.0241(12) Uani 1 1 d . . . C2 C 0.2557(4) 0.5894(5) 0.35248(18) 0.0207(11) Uani 1 1 d . . . C3 C 0.1383(4) 0.6266(6) 0.32825(19) 0.0258(12) Uani 1 1 d . . . C4 C 0.0724(4) 0.5196(6) 0.2956(2) 0.0349(14) Uani 1 1 d . . . H4A H -0.0062 0.5431 0.2803 0.042 Uiso 1 1 calc R . . C5 C 0.1206(5) 0.3813(7) 0.2856(2) 0.0400(15) Uani 1 1 d . . . H5 H 0.0757 0.3119 0.2631 0.048 Uiso 1 1 calc R . . C6 C 0.2360(5) 0.3435(6) 0.3089(2) 0.0344(14) Uani 1 1 d . . . H6 H 0.2692 0.2494 0.3014 0.041 Uiso 1 1 calc R . . C7 C 0.4198(4) 0.3928(5) 0.3731(2) 0.0240(12) Uani 1 1 d . . . C8 C 0.5110(4) 0.3276(6) 0.34113(19) 0.0245(12) Uani 1 1 d . . . C9 C 0.5786(4) 0.1993(5) 0.36013(18) 0.0214(11) Uani 1 1 d . . . C10 C 0.6677(4) 0.1439(5) 0.33084(19) 0.0233(12) Uani 1 1 d . . . C11 C 0.6910(5) 0.2167(6) 0.2837(2) 0.0354(14) Uani 1 1 d . . . H11 H 0.7526 0.1808 0.2648 0.042 Uiso 1 1 calc R . . C12 C 0.6223(5) 0.3430(7) 0.2646(2) 0.0439(16) Uani 1 1 d . . . H12 H 0.6371 0.3908 0.2327 0.053 Uiso 1 1 calc R . . C13 C 0.5323(5) 0.3964(6) 0.2932(2) 0.0337(14) Uani 1 1 d . . . H13 H 0.4854 0.4797 0.2802 0.040 Uiso 1 1 calc R . . C14 C 0.3369(4) 0.7033(5) 0.38532(19) 0.0231(12) Uani 1 1 d . . . C15 C 0.0858(4) 0.7838(7) 0.3333(2) 0.0298(13) Uani 1 1 d . . . C16 C 0.5523(5) 0.1229(5) 0.4112(2) 0.0226(12) Uani 1 1 d . . . C17 C 0.7403(5) 0.0024(6) 0.34888(19) 0.0268(12) Uani 1 1 d . . . C18 C 0.1555(5) 1.1108(6) 0.4169(2) 0.0370(14) Uani 1 1 d . . . H18 H 0.1918 1.0792 0.3871 0.044 Uiso 1 1 calc R . . C19 C 0.0551(5) 1.2053(6) 0.4088(2) 0.0378(15) Uani 1 1 d . . . H19 H 0.0250 1.2348 0.3739 0.045 Uiso 1 1 calc R . . C20 C -0.0010(4) 1.2561(5) 0.4515(2) 0.0251(12) Uani 1 1 d . . . C21 C 0.0454(4) 1.2021(6) 0.5023(2) 0.0309(13) Uani 1 1 d . . . H21 H 0.0092 1.2297 0.5325 0.037 Uiso 1 1 calc R . . C22 C 0.1455(4) 1.1072(6) 0.5071(2) 0.0285(13) Uani 1 1 d . . . H22 H 0.1751 1.0718 0.5413 0.034 Uiso 1 1 calc R . . C23 C -0.1050(4) 1.3674(5) 0.4435(2) 0.0239(12) Uani 1 1 d . . . C24 C -0.1300(5) 1.4445(6) 0.3954(2) 0.0387(14) Uani 1 1 d . . . H24 H -0.0848 1.4241 0.3672 0.046 Uiso 1 1 calc R . . C25 C -0.2225(4) 1.5526(6) 0.3887(2) 0.0368(14) Uani 1 1 d . . . H25 H -0.2374 1.6036 0.3559 0.044 Uiso 1 1 calc R . . C27 C -0.2695(5) 1.5079(6) 0.4738(2) 0.0358(14) Uani 1 1 d . . . H27 H -0.3179 1.5274 0.5009 0.043 Uiso 1 1 calc R . . C28 C -0.1791(4) 1.4000(6) 0.4829(2) 0.0312(13) Uani 1 1 d . . . H28 H -0.1677 1.3486 0.5157 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0196(3) 0.0200(3) 0.0290(3) -0.0011(3) 0.0026(2) 0.0038(3) Zn2 0.0236(3) 0.0266(4) 0.0390(4) -0.0036(3) 0.0055(3) 0.0044(3) N1 0.022(2) 0.022(2) 0.033(2) -0.004(2) -0.001(2) 0.0003(19) N2 0.023(2) 0.022(2) 0.042(3) -0.002(2) 0.003(2) 0.0090(19) O1 0.0236(19) 0.0214(19) 0.0297(19) -0.0076(17) 0.0070(15) 0.0032(16) O2 0.020(2) 0.032(2) 0.038(2) -0.0070(18) 0.0070(16) 0.0006(16) O3 0.037(2) 0.028(2) 0.062(3) 0.008(2) 0.010(2) 0.0056(19) O4 0.033(2) 0.035(2) 0.085(3) 0.017(2) 0.025(2) 0.0203(19) O5 0.035(2) 0.030(2) 0.034(2) 0.0019(18) 0.0049(18) 0.0138(17) O6 0.0230(19) 0.0208(19) 0.0326(19) -0.0008(17) 0.0025(16) 0.0038(16) O7 0.0200(19) 0.022(2) 0.0313(19) -0.0006(17) 0.0012(16) 0.0054(16) O8 0.041(2) 0.020(2) 0.046(2) 0.0009(19) 0.0183(19) 0.0085(18) O9 0.026(2) 0.033(2) 0.093(3) 0.010(2) 0.023(2) 0.0137(18) O10 0.0278(19) 0.0201(19) 0.0301(19) 0.0010(16) 0.0071(16) 0.0036(15) C1 0.023(3) 0.022(3) 0.027(3) -0.001(3) 0.002(2) 0.005(2) C2 0.019(3) 0.024(3) 0.020(3) -0.003(2) 0.003(2) 0.000(2) C3 0.022(3) 0.023(3) 0.034(3) 0.000(3) 0.008(2) 0.003(2) C4 0.021(3) 0.041(4) 0.042(3) 0.000(3) -0.004(3) 0.003(3) C5 0.038(4) 0.043(4) 0.036(3) -0.010(3) -0.007(3) -0.007(3) C6 0.039(3) 0.024(3) 0.041(3) -0.011(3) 0.005(3) 0.005(3) C7 0.025(3) 0.014(3) 0.032(3) 0.002(2) 0.000(2) 0.000(2) C8 0.025(3) 0.024(3) 0.026(3) 0.005(2) 0.006(2) 0.004(2) C9 0.021(3) 0.017(3) 0.026(3) -0.002(2) 0.001(2) -0.001(2) C10 0.021(3) 0.022(3) 0.027(3) 0.001(2) 0.002(2) 0.003(2) C11 0.039(3) 0.031(3) 0.038(3) -0.002(3) 0.013(3) 0.011(3) C12 0.058(4) 0.043(4) 0.033(3) 0.014(3) 0.016(3) 0.011(3) C13 0.036(3) 0.032(3) 0.035(3) 0.010(3) 0.008(3) 0.015(3) C14 0.021(3) 0.016(3) 0.031(3) 0.007(2) -0.004(2) 0.002(2) C15 0.019(3) 0.037(4) 0.032(3) 0.000(3) -0.001(2) 0.014(3) C16 0.026(3) 0.010(3) 0.032(3) -0.001(2) 0.005(3) 0.012(2) C17 0.025(3) 0.027(3) 0.029(3) -0.002(3) 0.004(2) 0.009(2) C18 0.039(3) 0.046(4) 0.025(3) -0.009(3) 0.002(3) 0.015(3) C19 0.039(3) 0.047(4) 0.027(3) 0.005(3) 0.005(3) 0.021(3) C20 0.022(3) 0.019(3) 0.035(3) 0.002(3) 0.004(2) 0.001(2) C21 0.028(3) 0.030(3) 0.036(3) -0.001(3) 0.011(3) 0.004(3) C22 0.021(3) 0.033(3) 0.032(3) 0.002(3) 0.004(2) 0.008(2) C23 0.019(3) 0.020(3) 0.034(3) 0.000(3) 0.008(2) 0.003(2) C24 0.038(3) 0.041(4) 0.041(3) 0.008(3) 0.020(3) 0.019(3) C25 0.035(3) 0.039(4) 0.037(3) 0.010(3) 0.008(3) 0.017(3) C27 0.038(3) 0.036(3) 0.038(3) 0.004(3) 0.022(3) 0.012(3) C28 0.036(3) 0.026(3) 0.033(3) 0.010(3) 0.007(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 2.058(3) 3_666 ? Zn1 O6 2.084(3) 1_565 ? Zn1 O1 2.127(3) . ? Zn1 N1 2.128(4) . ? Zn1 O10 2.149(3) . ? Zn1 O10 2.209(3) 3_676 ? Zn1 Zn1 3.0253(11) 3_676 ? Zn2 O10 1.915(3) . ? Zn2 O2 1.941(3) . ? Zn2 O8 1.967(4) 1_565 ? Zn2 N2 2.067(4) 1_645 ? N1 C22 1.332(6) . ? N1 C18 1.333(6) . ? N2 C25 1.333(6) . ? N2 C27 1.337(6) . ? N2 Zn2 2.067(4) 1_465 ? O1 C14 1.246(5) . ? O2 C14 1.271(5) . ? O3 C15 1.199(6) . ? O4 C15 1.318(6) . ? O4 H4 0.8200 . ? O5 C7 1.229(5) . ? O6 C16 1.257(5) . ? O6 Zn1 2.084(3) 1_545 ? O7 C16 1.268(5) . ? O7 Zn1 2.058(3) 3_666 ? O8 C17 1.260(6) . ? O8 Zn2 1.967(4) 1_545 ? O9 C17 1.232(5) . ? O10 Zn1 2.209(3) 3_676 ? O10 H10A 0.8201 . ? C1 C6 1.380(6) . ? C1 C2 1.398(6) . ? C1 C7 1.488(6) . ? C2 C3 1.404(6) . ? C2 C14 1.514(6) . ? C3 C4 1.389(6) . ? C3 C15 1.503(7) . ? C4 C5 1.357(7) . ? C4 H4A 0.9300 . ? C5 C6 1.377(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.476(6) . ? C8 C13 1.386(6) . ? C8 C9 1.399(6) . ? C9 C10 1.385(6) . ? C9 C16 1.499(6) . ? C10 C11 1.390(6) . ? C10 C17 1.514(6) . ? C11 C12 1.392(7) . ? C11 H11 0.9300 . ? C12 C13 1.378(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 C19 1.380(6) . ? C18 H18 0.9300 . ? C19 C20 1.373(6) . ? C19 H19 0.9300 . ? C20 C21 1.391(6) . ? C20 C23 1.502(6) . ? C21 C22 1.379(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.376(6) . ? C23 C28 1.386(6) . ? C24 C25 1.389(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C27 C28 1.374(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O6 158.80(12) 3_666 1_565 ? O7 Zn1 O1 104.93(12) 3_666 . ? O6 Zn1 O1 91.73(12) 1_565 . ? O7 Zn1 N1 94.12(14) 3_666 . ? O6 Zn1 N1 99.60(14) 1_565 . ? O1 Zn1 N1 87.86(13) . . ? O7 Zn1 O10 84.60(12) 3_666 . ? O6 Zn1 O10 81.64(12) 1_565 . ? O1 Zn1 O10 92.44(12) . . ? N1 Zn1 O10 178.72(14) . . ? O7 Zn1 O10 82.60(12) 3_666 3_676 ? O6 Zn1 O10 81.87(12) 1_565 3_676 ? O1 Zn1 O10 171.54(12) . 3_676 ? N1 Zn1 O10 87.77(13) . 3_676 ? O10 Zn1 O10 92.09(11) . 3_676 ? O7 Zn1 Zn1 80.74(9) 3_666 3_676 ? O6 Zn1 Zn1 78.08(9) 1_565 3_676 ? O1 Zn1 Zn1 138.80(9) . 3_676 ? N1 Zn1 Zn1 132.99(11) . 3_676 ? O10 Zn1 Zn1 46.86(8) . 3_676 ? O10 Zn1 Zn1 45.23(8) 3_676 3_676 ? O10 Zn2 O2 107.18(13) . . ? O10 Zn2 O8 124.09(14) . 1_565 ? O2 Zn2 O8 108.09(14) . 1_565 ? O10 Zn2 N2 109.69(15) . 1_645 ? O2 Zn2 N2 109.03(15) . 1_645 ? O8 Zn2 N2 97.92(16) 1_565 1_645 ? C22 N1 C18 116.8(4) . . ? C22 N1 Zn1 124.7(3) . . ? C18 N1 Zn1 117.8(3) . . ? C25 N2 C27 117.3(4) . . ? C25 N2 Zn2 117.2(3) . 1_465 ? C27 N2 Zn2 125.0(3) . 1_465 ? C14 O1 Zn1 131.3(3) . . ? C14 O2 Zn2 128.0(3) . . ? C15 O4 H4 109.5 . . ? C16 O6 Zn1 128.1(3) . 1_545 ? C16 O7 Zn1 125.5(3) . 3_666 ? C17 O8 Zn2 160.5(3) . 1_545 ? Zn2 O10 Zn1 111.79(14) . . ? Zn2 O10 Zn1 125.85(16) . 3_676 ? Zn1 O10 Zn1 87.92(11) . 3_676 ? Zn2 O10 H10A 108.9 . . ? Zn1 O10 H10A 108.7 . . ? Zn1 O10 H10A 111.1 3_676 . ? C6 C1 C2 120.2(4) . . ? C6 C1 C7 119.0(4) . . ? C2 C1 C7 120.7(4) . . ? C1 C2 C3 118.7(4) . . ? C1 C2 C14 118.5(4) . . ? C3 C2 C14 122.6(4) . . ? C4 C3 C2 119.3(5) . . ? C4 C3 C15 119.0(4) . . ? C2 C3 C15 121.5(4) . . ? C5 C4 C3 121.2(5) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 120.2(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O5 C7 C8 122.2(4) . . ? O5 C7 C1 120.3(4) . . ? C8 C7 C1 117.3(4) . . ? C13 C8 C9 120.0(5) . . ? C13 C8 C7 120.0(4) . . ? C9 C8 C7 119.9(4) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 C16 121.2(4) . . ? C8 C9 C16 119.6(4) . . ? C9 C10 C11 120.4(4) . . ? C9 C10 C17 121.0(4) . . ? C11 C10 C17 118.6(4) . . ? C10 C11 C12 120.2(5) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.3(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C8 120.8(5) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O1 C14 O2 128.2(4) . . ? O1 C14 C2 119.6(4) . . ? O2 C14 C2 112.2(4) . . ? O3 C15 O4 126.0(5) . . ? O3 C15 C3 122.9(5) . . ? O4 C15 C3 110.8(5) . . ? O6 C16 O7 127.4(5) . . ? O6 C16 C9 116.3(4) . . ? O7 C16 C9 116.2(4) . . ? O9 C17 O8 124.6(5) . . ? O9 C17 C10 115.6(5) . . ? O8 C17 C10 119.8(4) . . ? N1 C18 C19 122.7(5) . . ? N1 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C20 C19 C18 120.8(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 116.6(4) . . ? C19 C20 C23 121.2(4) . . ? C21 C20 C23 122.2(5) . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N1 C22 C21 123.9(5) . . ? N1 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? C24 C23 C28 116.4(4) . . ? C24 C23 C20 120.2(4) . . ? C28 C23 C20 123.4(5) . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? N2 C25 C24 122.5(5) . . ? N2 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N2 C27 C28 122.8(5) . . ? N2 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C23 120.4(5) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? 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 N1 C22 22.9(4) 3_666 . . . ? O6 Zn1 N1 C22 -140.9(4) 1_565 . . . ? O1 Zn1 N1 C22 127.7(4) . . . . ? O10 Zn1 N1 C22 -59.5(4) 3_676 . . . ? Zn1 Zn1 N1 C22 -58.3(4) 3_676 . . . ? O7 Zn1 N1 C18 -167.4(4) 3_666 . . . ? O6 Zn1 N1 C18 28.9(4) 1_565 . . . ? O1 Zn1 N1 C18 -62.5(4) . . . . ? O10 Zn1 N1 C18 110.2(4) 3_676 . . . ? Zn1 Zn1 N1 C18 111.5(4) 3_676 . . . ? O7 Zn1 O1 C14 -121.8(4) 3_666 . . . ? O6 Zn1 O1 C14 45.0(4) 1_565 . . . ? N1 Zn1 O1 C14 144.5(4) . . . . ? O10 Zn1 O1 C14 -36.7(4) . . . . ? Zn1 Zn1 O1 C14 -28.8(4) 3_676 . . . ? O10 Zn2 O2 C14 -2.4(4) . . . . ? O8 Zn2 O2 C14 -138.3(4) 1_565 . . . ? N2 Zn2 O2 C14 116.3(4) 1_645 . . . ? O2 Zn2 O10 Zn1 -35.11(19) . . . . ? O8 Zn2 O10 Zn1 91.89(18) 1_565 . . . ? N2 Zn2 O10 Zn1 -153.35(15) 1_645 . . . ? O2 Zn2 O10 Zn1 -139.03(17) . . . 3_676 ? O8 Zn2 O10 Zn1 -12.0(2) 1_565 . . 3_676 ? N2 Zn2 O10 Zn1 102.7(2) 1_645 . . 3_676 ? O7 Zn1 O10 Zn2 149.56(17) 3_666 . . . ? O6 Zn1 O10 Zn2 -46.61(15) 1_565 . . . ? O1 Zn1 O10 Zn2 44.78(16) . . . . ? O10 Zn1 O10 Zn2 -128.1(2) 3_676 . . . ? Zn1 Zn1 O10 Zn2 -128.1(2) 3_676 . . . ? O7 Zn1 O10 Zn1 -82.37(12) 3_666 . . 3_676 ? O6 Zn1 O10 Zn1 81.47(12) 1_565 . . 3_676 ? O1 Zn1 O10 Zn1 172.86(11) . . . 3_676 ? O10 Zn1 O10 Zn1 0.0 3_676 . . 3_676 ? C6 C1 C2 C3 2.9(7) . . . . ? C7 C1 C2 C3 -172.5(4) . . . . ? C6 C1 C2 C14 -173.2(4) . . . . ? C7 C1 C2 C14 11.3(7) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? C14 C2 C3 C4 175.5(5) . . . . ? C1 C2 C3 C15 -175.7(5) . . . . ? C14 C2 C3 C15 0.3(7) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? C15 C3 C4 C5 173.7(5) . . . . ? C3 C4 C5 C6 1.3(9) . . . . ? C4 C5 C6 C1 1.3(8) . . . . ? C2 C1 C6 C5 -3.4(8) . . . . ? C7 C1 C6 C5 172.2(5) . . . . ? C6 C1 C7 O5 -121.7(5) . . . . ? C2 C1 C7 O5 53.9(7) . . . . ? C6 C1 C7 C8 53.9(6) . . . . ? C2 C1 C7 C8 -130.5(5) . . . . ? O5 C7 C8 C13 -141.7(5) . . . . ? C1 C7 C8 C13 42.8(7) . . . . ? O5 C7 C8 C9 36.2(7) . . . . ? C1 C7 C8 C9 -139.3(5) . . . . ? C13 C8 C9 C10 0.9(7) . . . . ? C7 C8 C9 C10 -177.0(4) . . . . ? C13 C8 C9 C16 -178.2(4) . . . . ? C7 C8 C9 C16 3.9(7) . . . . ? C8 C9 C10 C11 1.1(7) . . . . ? C16 C9 C10 C11 -179.8(4) . . . . ? C8 C9 C10 C17 -178.0(4) . . . . ? C16 C9 C10 C17 1.1(7) . . . . ? C9 C10 C11 C12 -2.0(8) . . . . ? C17 C10 C11 C12 177.1(5) . . . . ? C10 C11 C12 C13 0.9(8) . . . . ? C11 C12 C13 C8 1.1(8) . . . . ? C9 C8 C13 C12 -2.0(8) . . . . ? C7 C8 C13 C12 175.9(5) . . . . ? Zn1 O1 C14 O2 2.8(7) . . . . ? Zn1 O1 C14 C2 -177.7(3) . . . . ? Zn2 O2 C14 O1 23.0(7) . . . . ? Zn2 O2 C14 C2 -156.5(3) . . . . ? C1 C2 C14 O1 -135.7(5) . . . . ? C3 C2 C14 O1 48.3(6) . . . . ? C1 C2 C14 O2 43.8(6) . . . . ? C3 C2 C14 O2 -132.1(5) . . . . ? C4 C3 C15 O3 -110.9(6) . . . . ? C2 C3 C15 O3 64.4(7) . . . . ? C4 C3 C15 O4 63.7(6) . . . . ? C2 C3 C15 O4 -121.1(5) . . . . ? Zn1 O6 C16 O7 4.6(7) 1_545 . . . ? Zn1 O6 C16 C9 -176.5(3) 1_545 . . . ? Zn1 O7 C16 O6 -6.0(7) 3_666 . . . ? Zn1 O7 C16 C9 175.2(3) 3_666 . . . ? C10 C9 C16 O6 -113.8(5) . . . . ? C8 C9 C16 O6 65.3(6) . . . . ? C10 C9 C16 O7 65.2(6) . . . . ? C8 C9 C16 O7 -115.8(5) . . . . ? Zn2 O8 C17 O9 124.3(9) 1_545 . . . ? Zn2 O8 C17 C10 -56.1(12) 1_545 . . . ? C9 C10 C17 O9 -141.0(5) . . . . ? C11 C10 C17 O9 39.9(7) . . . . ? C9 C10 C17 O8 39.4(7) . . . . ? C11 C10 C17 O8 -139.8(5) . . . . ? C22 N1 C18 C19 2.0(8) . . . . ? Zn1 N1 C18 C19 -168.6(4) . . . . ? N1 C18 C19 C20 0.7(9) . . . . ? C18 C19 C20 C21 -2.8(8) . . . . ? C18 C19 C20 C23 175.8(5) . . . . ? C19 C20 C21 C22 2.3(7) . . . . ? C23 C20 C21 C22 -176.2(4) . . . . ? C18 N1 C22 C21 -2.4(7) . . . . ? Zn1 N1 C22 C21 167.4(4) . . . . ? C20 C21 C22 N1 0.2(8) . . . . ? C19 C20 C23 C24 -13.4(7) . . . . ? C21 C20 C23 C24 165.1(5) . . . . ? C19 C20 C23 C28 167.3(5) . . . . ? C21 C20 C23 C28 -14.2(7) . . . . ? C28 C23 C24 C25 2.3(8) . . . . ? C20 C23 C24 C25 -177.1(5) . . . . ? C27 N2 C25 C24 -1.7(8) . . . . ? Zn2 N2 C25 C24 171.3(4) 1_465 . . . ? C23 C24 C25 N2 -0.4(9) . . . . ? C25 N2 C27 C28 1.9(8) . . . . ? Zn2 N2 C27 C28 -170.5(4) 1_465 . . . ? N2 C27 C28 C23 0.0(8) . . . . ? C24 C23 C28 C27 -2.1(8) . . . . ? C20 C23 C28 C27 177.2(5) . . . . ? 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 O4 H4 O9 0.82 1.71 2.500(5) 160.4 1_465 O10 H10A O5 0.82 2.35 3.146(5) 165.0 3_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.825 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.106 data_compound5 _database_code_depnum_ccdc_archive 'CCDC 774756' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H34 Cd2 N4 O11' _chemical_formula_sum 'C41 H34 Cd2 N4 O11' _chemical_formula_weight 983.52 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' 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 21.3161(10) _cell_length_b 12.4028(10) _cell_length_c 18.6010(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.7400(10) _cell_angle_gamma 90.00 _cell_volume 4567.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 2.1505 _cell_measurement_theta_max 25.650 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7831 _exptl_absorpt_correction_T_max 0.8579 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11270 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4027 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+2.7812P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4027 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.731719(8) 0.821639(14) 0.362669(8) 0.03463(9) Uani 1 1 d . . . N1 N 0.75208(12) 0.79895(19) 0.25010(12) 0.0436(5) Uani 1 1 d . . . N2 N 0.66141(12) 0.9681(2) 0.31226(13) 0.0515(6) Uani 1 1 d . . . O1 O 0.66431(10) 0.58290(19) 0.58474(10) 0.0613(6) Uani 1 1 d . . . O2 O 0.72127(9) 0.57783(16) 0.50820(10) 0.0508(5) Uani 1 1 d . . . O3 O 0.64974(9) 0.76396(14) 0.41351(9) 0.0445(4) Uani 1 1 d . . . O4 O 0.65352(12) 0.66504(17) 0.31707(12) 0.0564(5) Uani 1 1 d . . . O5 O 0.5000 0.7406(2) 0.2500 0.0617(8) Uani 1 2 d S . . C1 C 0.58558(11) 0.60139(18) 0.38312(12) 0.0318(5) Uani 1 1 d . . . C2 C 0.60323(12) 0.54550(19) 0.45329(12) 0.0340(5) Uani 1 1 d . . . C3 C 0.55940(13) 0.4685(2) 0.46228(13) 0.0424(6) Uani 1 1 d . . . H3 H 0.5714 0.4305 0.5085 0.051 Uiso 1 1 calc R . . C4 C 0.49766(14) 0.4475(2) 0.40277(14) 0.0470(6) Uani 1 1 d . . . H4 H 0.4683 0.3965 0.4094 0.056 Uiso 1 1 calc R . . C5 C 0.48076(12) 0.5028(2) 0.33438(13) 0.0432(6) Uani 1 1 d . . . H5 H 0.4399 0.4883 0.2944 0.052 Uiso 1 1 calc R . . C6 C 0.52354(11) 0.57976(19) 0.32382(12) 0.0344(5) Uani 1 1 d . . . C7 C 0.5000 0.6437(3) 0.2500 0.0397(8) Uani 1 2 d S . . C8 C 0.66768(13) 0.5697(2) 0.51957(13) 0.0399(6) Uani 1 1 d . . . C9 C 0.63284(13) 0.68286(19) 0.37031(14) 0.0376(6) Uani 1 1 d . . . C10 C 0.72391(16) 0.7193(2) 0.20149(14) 0.0526(7) Uani 1 1 d . . . H10 H 0.6992 0.6675 0.2159 0.063 Uiso 1 1 calc R . . C11 C 0.72973(18) 0.7101(3) 0.13026(16) 0.0619(8) Uani 1 1 d . . . H11 H 0.7103 0.6518 0.0983 0.074 Uiso 1 1 calc R . . C12 C 0.76452(16) 0.7879(3) 0.10634(15) 0.0546(7) Uani 1 1 d . . . C13 C 0.79311(16) 0.8697(3) 0.15685(15) 0.0548(7) Uani 1 1 d . . . H13 H 0.8166 0.9240 0.1430 0.066 Uiso 1 1 calc R . . C14 C 0.78751(14) 0.8725(2) 0.22771(15) 0.0493(6) Uani 1 1 d . . . H14 H 0.8091 0.9275 0.2619 0.059 Uiso 1 1 calc R . . C15 C 0.7719(2) 0.7871(4) 0.02864(18) 0.0786(11) Uani 1 1 d . . . H15A H 0.7633 0.8594 0.0074 0.094 Uiso 1 1 calc R . . H15B H 0.8184 0.7695 0.0368 0.094 Uiso 1 1 calc R . . C16 C 0.63323(17) 1.0126(3) 0.35809(19) 0.0640(8) Uani 1 1 d . . . H16 H 0.6429 0.9835 0.4071 0.077 Uiso 1 1 calc R . . C17 C 0.59011(17) 1.1003(3) 0.3359(2) 0.0729(9) Uani 1 1 d . . . H17 H 0.5706 1.1277 0.3693 0.088 Uiso 1 1 calc R . . C18 C 0.57618(16) 1.1466(3) 0.2650(2) 0.0698(10) Uani 1 1 d . . . C24 C 0.60584(19) 1.1019(3) 0.2190(2) 0.0812(11) Uani 1 1 d . . . H19 H 0.5981 1.1315 0.1706 0.097 Uiso 1 1 calc R . . C20 C 0.64713(18) 1.0134(3) 0.24330(18) 0.0698(9) Uani 1 1 d . . . H20 H 0.6660 0.9839 0.2099 0.084 Uiso 1 1 calc R . . C21 C 0.53061(17) 1.2434(3) 0.2389(3) 0.1012(16) Uani 1 1 d . . . H21A H 0.5155 1.2484 0.1830 0.121 Uiso 1 1 calc R . . H21B H 0.5569 1.3076 0.2603 0.121 Uiso 1 1 calc R . . O1W O 0.79829(11) 0.67573(15) 0.43146(12) 0.0531(5) Uani 1 1 d . . . H1WA H 0.8371 0.6988 0.4599 0.064 Uiso 1 1 d R . . H1WB H 0.7794 0.6466 0.4596 0.064 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03345(13) 0.04366(14) 0.02447(11) 0.00196(6) 0.00800(8) -0.00268(6) N1 0.0471(13) 0.0533(12) 0.0336(10) -0.0025(10) 0.0188(9) -0.0048(11) N2 0.0474(14) 0.0529(14) 0.0503(13) 0.0138(11) 0.0136(10) 0.0062(11) O1 0.0539(12) 0.0928(16) 0.0297(9) -0.0091(10) 0.0067(8) -0.0141(11) O2 0.0329(9) 0.0682(12) 0.0444(10) 0.0126(9) 0.0064(7) -0.0046(9) O3 0.0452(10) 0.0426(10) 0.0380(9) 0.0029(8) 0.0063(7) -0.0118(8) O4 0.0615(14) 0.0713(14) 0.0443(11) -0.0016(9) 0.0287(10) -0.0157(10) O5 0.080(2) 0.0428(15) 0.0427(14) 0.000 -0.0002(13) 0.000 C1 0.0313(12) 0.0351(12) 0.0282(10) -0.0021(9) 0.0102(9) -0.0017(10) C2 0.0355(12) 0.0385(12) 0.0267(10) -0.0029(9) 0.0099(9) -0.0023(10) C3 0.0521(15) 0.0449(14) 0.0310(11) -0.0015(10) 0.0163(10) -0.0098(12) C4 0.0486(15) 0.0533(16) 0.0403(13) -0.0079(12) 0.0180(11) -0.0205(13) C5 0.0365(13) 0.0535(15) 0.0343(12) -0.0099(11) 0.0069(10) -0.0119(11) C6 0.0324(12) 0.0402(12) 0.0263(11) -0.0032(9) 0.0058(9) -0.0014(10) C7 0.0332(18) 0.044(2) 0.0346(17) 0.000 0.0044(14) 0.000 C8 0.0421(14) 0.0383(13) 0.0310(12) 0.0059(10) 0.0040(10) -0.0038(11) C9 0.0294(13) 0.0459(14) 0.0298(12) 0.0072(10) 0.0021(10) -0.0025(10) C10 0.0692(19) 0.0570(17) 0.0382(14) -0.0051(13) 0.0274(13) -0.0161(15) C11 0.081(2) 0.0716(19) 0.0396(15) -0.0153(14) 0.0295(15) -0.0238(18) C12 0.0608(19) 0.0744(19) 0.0343(13) -0.0026(14) 0.0243(12) -0.0134(16) C13 0.0598(18) 0.0665(19) 0.0444(14) 0.0008(14) 0.0268(13) -0.0142(16) C14 0.0539(16) 0.0558(16) 0.0406(14) -0.0056(12) 0.0203(12) -0.0108(14) C15 0.097(3) 0.105(3) 0.0450(17) -0.0129(18) 0.0396(18) -0.032(2) C16 0.066(2) 0.0614(19) 0.0686(19) 0.0211(16) 0.0294(16) 0.0163(16) C17 0.063(2) 0.061(2) 0.099(3) 0.0130(19) 0.0342(18) 0.0124(17) C18 0.0391(17) 0.0470(16) 0.104(3) 0.0279(19) 0.0036(17) -0.0050(14) C24 0.067(2) 0.088(3) 0.075(2) 0.042(2) 0.0095(18) 0.011(2) C20 0.064(2) 0.085(2) 0.0539(17) 0.0253(17) 0.0137(14) 0.0133(18) C21 0.0549(19) 0.0446(17) 0.170(4) 0.029(2) 0.002(2) -0.0027(15) O1W 0.0484(12) 0.0618(13) 0.0464(11) 0.0097(8) 0.0145(9) 0.0042(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 N1 2.308(2) . ? Cd1 N2 2.320(2) . ? Cd1 O1W 2.3624(18) . ? Cd1 O1 2.380(2) 7_666 ? Cd1 O3 2.3841(18) . ? Cd1 O4 2.495(2) . ? Cd1 O2 2.5583(18) 7_666 ? N1 C10 1.324(3) . ? N1 C14 1.345(4) . ? N2 C20 1.329(4) . ? N2 C16 1.331(4) . ? O1 C8 1.251(3) . ? O1 Cd1 2.380(2) 7_666 ? O2 C8 1.240(3) . ? O2 Cd1 2.5582(18) 7_666 ? O3 C9 1.254(3) . ? O4 C9 1.244(3) . ? O5 C7 1.202(5) . ? C1 C6 1.399(3) . ? C1 C2 1.401(3) . ? C1 C9 1.507(3) . ? C2 C3 1.388(3) . ? C2 C8 1.498(3) . ? C3 C4 1.395(4) . ? C3 H3 0.9300 . ? C4 C5 1.370(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(3) . ? C5 H5 0.9300 . ? C6 C7 1.502(3) . ? C7 C6 1.502(3) 2_655 ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 C13 1.363(4) . ? C12 C15 1.511(4) . ? C13 C14 1.367(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C15 1.455(7) 7_665 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.385(4) . ? C16 H16 0.9300 . ? C17 C18 1.366(5) . ? C17 H17 0.9300 . ? C18 C24 1.356(6) . ? C18 C21 1.507(5) . ? C24 C20 1.374(5) . ? C24 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C21 1.507(9) 2_655 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? 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 N1 Cd1 N2 92.25(8) . . ? N1 Cd1 O1W 96.94(8) . . ? N2 Cd1 O1W 170.78(8) . . ? N1 Cd1 O1 88.52(7) . 7_666 ? N2 Cd1 O1 98.07(8) . 7_666 ? O1W Cd1 O1 82.96(8) . 7_666 ? N1 Cd1 O3 137.32(7) . . ? N2 Cd1 O3 86.37(7) . . ? O1W Cd1 O3 86.37(7) . . ? O1 Cd1 O3 133.95(6) 7_666 . ? N1 Cd1 O4 85.59(7) . . ? N2 Cd1 O4 102.82(9) . . ? O1W Cd1 O4 77.26(8) . . ? O1 Cd1 O4 158.48(8) 7_666 . ? O3 Cd1 O4 53.53(6) . . ? N1 Cd1 O2 140.48(7) . 7_666 ? N2 Cd1 O2 88.14(7) . 7_666 ? O1W Cd1 O2 85.24(7) . 7_666 ? O1 Cd1 O2 52.44(6) 7_666 7_666 ? O3 Cd1 O2 82.16(6) . 7_666 ? O4 Cd1 O2 132.74(6) . 7_666 ? C10 N1 C14 117.3(2) . . ? C10 N1 Cd1 121.38(18) . . ? C14 N1 Cd1 120.94(18) . . ? C20 N2 C16 116.5(3) . . ? C20 N2 Cd1 127.2(2) . . ? C16 N2 Cd1 116.28(18) . . ? C8 O1 Cd1 94.84(16) . 7_666 ? C8 O2 Cd1 86.84(15) . 7_666 ? C9 O3 Cd1 93.74(15) . . ? C9 O4 Cd1 88.86(16) . . ? C6 C1 C2 119.3(2) . . ? C6 C1 C9 119.74(19) . . ? C2 C1 C9 120.97(19) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 C8 119.4(2) . . ? C1 C2 C8 121.1(2) . . ? C2 C3 C4 120.8(2) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 C7 118.65(19) . . ? C1 C6 C7 121.2(2) . . ? O5 C7 C6 121.86(15) . . ? O5 C7 C6 121.86(15) . 2_655 ? C6 C7 C6 116.3(3) . 2_655 ? O2 C8 O1 122.8(2) . . ? O2 C8 C2 119.9(2) . . ? O1 C8 C2 117.4(2) . . ? O4 C9 O3 123.4(2) . . ? O4 C9 C1 117.5(2) . . ? O3 C9 C1 119.1(2) . . ? N1 C10 C11 122.6(3) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 119.9(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 116.9(2) . . ? C13 C12 C15 119.1(3) . . ? C11 C12 C15 124.0(3) . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? N1 C14 C13 122.8(3) . . ? N1 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C15 C15 C12 116.1(4) 7_665 . ? C15 C15 H15A 108.3 7_665 . ? C12 C15 H15A 108.3 . . ? C15 C15 H15B 108.3 7_665 . ? C12 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? N2 C16 C17 122.8(3) . . ? N2 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C24 C18 C17 116.8(3) . . ? C24 C18 C21 121.2(4) . . ? C17 C18 C21 122.0(4) . . ? C18 C24 C20 120.7(3) . . ? C18 C24 H19 119.6 . . ? C20 C24 H19 119.6 . . ? N2 C20 C24 123.0(4) . . ? N2 C20 H20 118.5 . . ? C24 C20 H20 118.5 . . ? C18 C21 C21 115.6(3) . 2_655 ? C18 C21 H21A 108.4 . . ? C21 C21 H21A 108.4 2_655 . ? C18 C21 H21B 108.4 . . ? C21 C21 H21B 108.4 2_655 . ? H21A C21 H21B 107.4 . . ? Cd1 O1W H1WA 109.3 . . ? Cd1 O1W H1WB 109.4 . . ? H1WA O1W H1WB 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cd1 N1 C10 -105.4(2) . . . . ? O1W Cd1 N1 C10 73.9(2) . . . . ? O1 Cd1 N1 C10 156.6(2) 7_666 . . . ? O3 Cd1 N1 C10 -18.3(3) . . . . ? O4 Cd1 N1 C10 -2.7(2) . . . . ? O2 Cd1 N1 C10 164.8(2) 7_666 . . . ? N2 Cd1 N1 C14 67.8(2) . . . . ? O1W Cd1 N1 C14 -112.9(2) . . . . ? O1 Cd1 N1 C14 -30.2(2) 7_666 . . . ? O3 Cd1 N1 C14 154.90(19) . . . . ? O4 Cd1 N1 C14 170.5(2) . . . . ? O2 Cd1 N1 C14 -22.0(3) 7_666 . . . ? N1 Cd1 N2 C20 -2.7(3) . . . . ? O1 Cd1 N2 C20 86.1(3) 7_666 . . . ? O3 Cd1 N2 C20 -140.0(3) . . . . ? O4 Cd1 N2 C20 -88.7(3) . . . . ? O2 Cd1 N2 C20 137.8(3) 7_666 . . . ? N1 Cd1 N2 C16 178.5(2) . . . . ? O1 Cd1 N2 C16 -92.7(2) 7_666 . . . ? O3 Cd1 N2 C16 41.2(2) . . . . ? O4 Cd1 N2 C16 92.5(2) . . . . ? O2 Cd1 N2 C16 -41.0(2) 7_666 . . . ? N1 Cd1 O3 C9 23.30(18) . . . . ? N2 Cd1 O3 C9 112.67(14) . . . . ? O1W Cd1 O3 C9 -73.02(14) . . . . ? O1 Cd1 O3 C9 -149.62(14) 7_666 . . . ? O4 Cd1 O3 C9 3.80(14) . . . . ? O2 Cd1 O3 C9 -158.70(14) 7_666 . . . ? N1 Cd1 O4 C9 -170.71(17) . . . . ? N2 Cd1 O4 C9 -79.41(17) . . . . ? O1W Cd1 O4 C9 91.14(16) . . . . ? O1 Cd1 O4 C9 114.7(2) 7_666 . . . ? O3 Cd1 O4 C9 -3.83(14) . . . . ? O2 Cd1 O4 C9 20.1(2) 7_666 . . . ? C6 C1 C2 C3 1.0(3) . . . . ? C9 C1 C2 C3 -178.0(2) . . . . ? C6 C1 C2 C8 -177.2(2) . . . . ? C9 C1 C2 C8 3.8(3) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C8 C2 C3 C4 177.2(2) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C1 0.8(4) . . . . ? C4 C5 C6 C7 -175.3(2) . . . . ? C2 C1 C6 C5 -0.9(3) . . . . ? C9 C1 C6 C5 178.1(2) . . . . ? C2 C1 C6 C7 175.1(2) . . . . ? C9 C1 C6 C7 -5.9(3) . . . . ? C5 C6 C7 O5 125.90(19) . . . . ? C1 C6 C7 O5 -50.2(2) . . . . ? C5 C6 C7 C6 -54.10(19) . . . 2_655 ? C1 C6 C7 C6 129.8(2) . . . 2_655 ? Cd1 O2 C8 O1 -17.6(3) 7_666 . . . ? Cd1 O2 C8 C2 161.0(2) 7_666 . . . ? Cd1 O1 C8 O2 19.0(3) 7_666 . . . ? Cd1 O1 C8 C2 -159.67(19) 7_666 . . . ? C3 C2 C8 O2 135.1(3) . . . . ? C1 C2 C8 O2 -46.7(3) . . . . ? C3 C2 C8 O1 -46.2(4) . . . . ? C1 C2 C8 O1 132.0(3) . . . . ? Cd1 O4 C9 O3 7.0(3) . . . . ? Cd1 O4 C9 C1 -172.43(18) . . . . ? Cd1 O3 C9 O4 -7.4(3) . . . . ? Cd1 O3 C9 C1 172.08(18) . . . . ? C6 C1 C9 O4 -60.4(3) . . . . ? C2 C1 C9 O4 118.6(3) . . . . ? C6 C1 C9 O3 120.1(2) . . . . ? C2 C1 C9 O3 -60.8(3) . . . . ? C14 N1 C10 C11 -0.1(5) . . . . ? Cd1 N1 C10 C11 173.3(3) . . . . ? N1 C10 C11 C12 -1.9(6) . . . . ? C10 C11 C12 C13 1.6(5) . . . . ? C10 C11 C12 C15 -178.0(4) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C15 C12 C13 C14 -179.8(3) . . . . ? C10 N1 C14 C13 2.4(5) . . . . ? Cd1 N1 C14 C13 -171.1(2) . . . . ? C12 C13 C14 N1 -2.7(5) . . . . ? C13 C12 C15 C15 -166.6(5) . . . 7_665 ? C11 C12 C15 C15 13.1(8) . . . 7_665 ? C20 N2 C16 C17 1.2(5) . . . . ? Cd1 N2 C16 C17 -179.9(3) . . . . ? N2 C16 C17 C18 -1.6(5) . . . . ? C16 C17 C18 C24 0.6(5) . . . . ? C16 C17 C18 C21 -178.8(3) . . . . ? C17 C18 C24 C20 0.8(6) . . . . ? C21 C18 C24 C20 -179.8(3) . . . . ? C16 N2 C20 C24 0.3(5) . . . . ? Cd1 N2 C20 C24 -178.5(3) . . . . ? C18 C24 C20 N2 -1.2(6) . . . . ? C24 C18 C21 C21 141.3(5) . . . 2_655 ? C17 C18 C21 C21 -39.3(6) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.85 2.31 2.781(3) 115.1 7_666 O1W H1WB O2 0.85 1.98 2.818(3) 170.0 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.659 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.069 data_compound6 _database_code_depnum_ccdc_archive 'CCDC 774757' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H38 Cd2 N4 O11' _chemical_formula_sum 'C43 H38 Cd2 N4 O11' _chemical_formula_weight 1011.57 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 triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6833(13) _cell_length_b 12.4887(14) _cell_length_c 16.2276(18) _cell_angle_alpha 71.931(2) _cell_angle_beta 74.323(2) _cell_angle_gamma 69.001(2) _cell_volume 2067.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2250 _cell_measurement_theta_min 2.1505 _cell_measurement_theta_max 25.650 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8273 _exptl_absorpt_correction_T_max 0.8530 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10447 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7160 _reflns_number_gt 5196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7160 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 0.44482(3) 0.52174(3) 0.66291(2) 0.03696(13) Uani 1 1 d . . . Cd2 Cd 1.00804(3) 0.90650(3) 0.16659(2) 0.03868(13) Uani 1 1 d . . . N1 N 0.5301(4) 0.5314(4) 0.7739(3) 0.0407(10) Uani 1 1 d . . . N2 N 1.2569(4) 0.5384(4) 0.7634(3) 0.0461(11) Uani 1 1 d . . . N3 N 1.0075(4) 0.7275(4) 0.2639(3) 0.0434(11) Uani 1 1 d . . . N4 N 1.0121(4) -0.0237(4) 0.2841(3) 0.0420(11) Uani 1 1 d . . . O1 O 0.7805(3) 1.0010(4) 0.1885(3) 0.0588(11) Uani 1 1 d . . . O2 O 0.8659(3) 0.9062(3) 0.0828(2) 0.0528(10) Uani 1 1 d . . . O3 O 0.8356(3) 1.1506(4) -0.0343(3) 0.0580(11) Uani 1 1 d . . . O4 O 0.7685(4) 1.1241(4) -0.1371(3) 0.0682(12) Uani 1 1 d . . . O5 O 0.6403(4) 0.8136(3) 0.2168(3) 0.0669(13) Uani 1 1 d . . . O6 O 0.4428(4) 0.6959(3) 0.3084(3) 0.0530(10) Uani 1 1 d . . . O7 O 0.5881(3) 0.6217(3) 0.3896(2) 0.0461(9) Uani 1 1 d . . . O8 O 0.3584(4) 0.6628(3) 0.5299(2) 0.0536(10) Uani 1 1 d . . . O9 O 0.4261(4) 0.7299(4) 0.6109(3) 0.0655(12) Uani 1 1 d . . . O1W O 0.6344(3) 0.5045(3) 0.5583(2) 0.0501(10) Uani 1 1 d . . . H1WA H 0.6212 0.5501 0.5084 0.060 Uiso 1 1 d R . . H1WB H 0.6594 0.4339 0.5527 0.060 Uiso 1 1 d R . . O2W O 0.9969(4) 1.1020(3) 0.0823(2) 0.0537(10) Uani 1 1 d . . . H2WA H 1.0517 1.1083 0.0358 0.064 Uiso 1 1 d R . . H2WB H 0.9278 1.1174 0.0667 0.064 Uiso 1 1 d R . . C1 C 0.6528(4) 1.0302(4) 0.0882(3) 0.0336(11) Uani 1 1 d . . . C2 C 0.6431(4) 1.1045(4) 0.0047(3) 0.0342(11) Uani 1 1 d . . . C3 C 0.5285(4) 1.1521(4) -0.0224(3) 0.0364(11) Uani 1 1 d . . . H3 H 0.5231 1.1985 -0.0792 0.044 Uiso 1 1 calc R . . C4 C 0.4221(5) 1.1316(4) 0.0338(4) 0.0420(12) Uani 1 1 d . . . H4 H 0.3453 1.1667 0.0157 0.050 Uiso 1 1 calc R . . C5 C 0.4307(5) 1.0582(4) 0.1175(3) 0.0408(12) Uani 1 1 d . . . H5 H 0.3595 1.0445 0.1559 0.049 Uiso 1 1 calc R . . C6 C 0.5460(4) 1.0055(4) 0.1438(3) 0.0358(11) Uani 1 1 d . . . C7 C 0.5623(5) 0.9068(5) 0.2240(4) 0.0414(13) Uani 1 1 d . . . C8 C 0.4880(4) 0.9229(4) 0.3118(3) 0.0360(11) Uani 1 1 d . . . C9 C 0.4675(4) 0.8245(4) 0.3778(3) 0.0345(11) Uani 1 1 d . . . C10 C 0.4157(4) 0.8393(4) 0.4645(3) 0.0368(12) Uani 1 1 d . . . C11 C 0.3862(5) 0.9489(5) 0.4819(4) 0.0427(12) Uani 1 1 d . . . H11 H 0.3535 0.9579 0.5392 0.051 Uiso 1 1 calc R . . C12 C 0.4046(5) 1.0448(5) 0.4154(4) 0.0466(13) Uani 1 1 d . . . H12 H 0.3833 1.1181 0.4279 0.056 Uiso 1 1 calc R . . C13 C 0.4544(5) 1.0320(5) 0.3309(4) 0.0442(13) Uani 1 1 d . . . H13 H 0.4656 1.0971 0.2861 0.053 Uiso 1 1 calc R . . C14 C 0.7749(5) 0.9754(5) 0.1222(3) 0.0412(13) Uani 1 1 d . . . C15 C 0.7579(5) 1.1283(4) -0.0597(4) 0.0435(13) Uani 1 1 d . . . C16 C 0.5015(5) 0.7058(4) 0.3564(3) 0.0385(12) Uani 1 1 d . . . C17 C 0.3981(5) 0.7371(5) 0.5394(3) 0.0422(13) Uani 1 1 d . . . C18 C 0.9044(5) 0.6972(5) 0.3038(4) 0.0543(15) Uani 1 1 d . . . H18 H 0.8281 0.7514 0.2926 0.065 Uiso 1 1 calc R . . C19 C 0.9052(6) 0.5892(5) 0.3611(4) 0.0578(16) Uani 1 1 d . . . H19 H 0.8304 0.5725 0.3874 0.069 Uiso 1 1 calc R . . C20 C 1.0155(6) 0.5062(5) 0.3798(4) 0.0528(15) Uani 1 1 d . . . C21 C 1.1225(6) 0.5378(5) 0.3397(4) 0.0594(16) Uani 1 1 d . . . H21 H 1.1998 0.4847 0.3497 0.071 Uiso 1 1 calc R . . C22 C 1.1148(5) 0.6490(5) 0.2844(4) 0.0590(16) Uani 1 1 d . . . H22 H 1.1878 0.6700 0.2605 0.071 Uiso 1 1 calc R . . C23 C 1.0210(7) 0.3859(5) 0.4404(4) 0.0656(18) Uani 1 1 d . . . H23A H 1.0951 0.3560 0.4667 0.079 Uiso 1 1 calc R . . H23B H 0.9490 0.3926 0.4875 0.079 Uiso 1 1 calc R . . C24 C 1.0232(7) 0.3008(5) 0.3916(4) 0.0616(17) Uani 1 1 d . . . H24A H 1.0965 0.2931 0.3456 0.074 Uiso 1 1 calc R . . H24B H 0.9506 0.3328 0.3636 0.074 Uiso 1 1 calc R . . C25 C 1.0246(6) 0.1775(5) 0.4509(4) 0.0537(15) Uani 1 1 d . . . H25A H 1.0995 0.1424 0.4766 0.064 Uiso 1 1 calc R . . H25B H 0.9531 0.1842 0.4984 0.064 Uiso 1 1 calc R . . C26 C 1.0209(5) 0.1008(5) 0.3974(3) 0.0443(13) Uani 1 1 d . . . C27 C 0.9113(5) 0.1073(5) 0.3787(4) 0.0512(14) Uani 1 1 d . . . H27 H 0.8369 0.1544 0.4042 0.061 Uiso 1 1 calc R . . C28 C 0.9090(5) 0.0457(5) 0.3228(4) 0.0527(15) Uani 1 1 d . . . H28 H 0.8325 0.0526 0.3114 0.063 Uiso 1 1 calc R . . C29 C 1.1185(5) -0.0355(5) 0.3059(4) 0.0523(15) Uani 1 1 d . . . H29 H 1.1912 -0.0874 0.2830 0.063 Uiso 1 1 calc R . . C30 C 1.1263(5) 0.0250(6) 0.3604(4) 0.0550(15) Uani 1 1 d . . . H30 H 1.2034 0.0148 0.3725 0.066 Uiso 1 1 calc R . . C31 C 0.5188(5) 0.6332(5) 0.7915(4) 0.0549(16) Uani 1 1 d . . . H31 H 0.4786 0.7036 0.7557 0.066 Uiso 1 1 calc R . . C32 C 0.5636(5) 0.6387(5) 0.8596(4) 0.0514(14) Uani 1 1 d . . . H32 H 0.5517 0.7116 0.8697 0.062 Uiso 1 1 calc R . . C33 C 0.6260(4) 0.5368(5) 0.9129(3) 0.0372(12) Uani 1 1 d . . . C34 C 0.6341(5) 0.4325(5) 0.8966(3) 0.0449(13) Uani 1 1 d . . . H34 H 0.6737 0.3610 0.9316 0.054 Uiso 1 1 calc R . . C35 C 0.5842(5) 0.4331(5) 0.8288(3) 0.0424(12) Uani 1 1 d . . . H35 H 0.5885 0.3610 0.8209 0.051 Uiso 1 1 calc R . . C36 C 0.6864(4) 0.5369(5) 0.9839(4) 0.0493(14) Uani 1 1 d . . . H36A H 0.6676 0.4785 1.0367 0.059 Uiso 1 1 calc R . . H36B H 0.6522 0.6136 0.9978 0.059 Uiso 1 1 calc R . . C37 C 0.8290(6) 0.5089(8) 0.9548(4) 0.081(2) Uani 1 1 d . . . H37A H 0.8661 0.4925 1.0059 0.097 Uiso 1 1 calc R . . H37B H 0.8610 0.4383 0.9323 0.097 Uiso 1 1 calc R . . C38 C 0.8662(6) 0.6021(7) 0.8891(5) 0.083(2) Uani 1 1 d . . . H38A H 0.8393 0.6703 0.9140 0.100 Uiso 1 1 calc R . . H38B H 0.8217 0.6232 0.8410 0.100 Uiso 1 1 calc R . . C39 C 1.0112(6) 0.5770(6) 0.8490(4) 0.0639(18) Uani 1 1 d . . . C40 C 1.0639(6) 0.6617(6) 0.8244(4) 0.0676(18) Uani 1 1 d . . . H40 H 1.0199 0.7352 0.8365 0.081 Uiso 1 1 calc R . . C41 C 1.1838(5) 0.6400(6) 0.7809(4) 0.0598(16) Uani 1 1 d . . . H41 H 1.2174 0.7026 0.7618 0.072 Uiso 1 1 calc R . . C42 C 1.2091(6) 0.4491(6) 0.7938(5) 0.072(2) Uani 1 1 d . . . H42 H 1.2586 0.3744 0.7863 0.087 Uiso 1 1 calc R . . C43 C 1.0822(7) 0.4661(7) 0.8382(5) 0.079(2) Uani 1 1 d . . . H43 H 1.0487 0.4033 0.8593 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0414(2) 0.0402(2) 0.0278(2) -0.00517(16) -0.00327(15) -0.01527(18) Cd2 0.0429(2) 0.0409(2) 0.0294(2) -0.00304(17) -0.00387(16) -0.01568(18) N1 0.047(2) 0.044(3) 0.034(2) -0.007(2) -0.0101(19) -0.017(2) N2 0.043(2) 0.055(3) 0.039(3) -0.012(2) -0.004(2) -0.016(2) N3 0.051(3) 0.039(2) 0.035(3) -0.001(2) -0.007(2) -0.014(2) N4 0.041(2) 0.049(3) 0.033(2) -0.011(2) -0.0012(19) -0.013(2) O1 0.057(2) 0.078(3) 0.045(3) -0.012(2) -0.0161(19) -0.022(2) O2 0.039(2) 0.060(3) 0.041(2) 0.0006(19) -0.0006(17) -0.0097(19) O3 0.047(2) 0.072(3) 0.047(2) 0.010(2) -0.0088(18) -0.029(2) O4 0.074(3) 0.094(3) 0.031(2) -0.014(2) 0.0092(19) -0.034(3) O5 0.064(3) 0.042(2) 0.053(3) 0.007(2) 0.021(2) -0.005(2) O6 0.065(2) 0.046(2) 0.055(3) -0.010(2) -0.017(2) -0.022(2) O7 0.052(2) 0.036(2) 0.037(2) 0.0002(17) -0.0020(17) -0.0101(18) O8 0.067(2) 0.049(2) 0.037(2) -0.0054(18) 0.0048(18) -0.023(2) O9 0.089(3) 0.065(3) 0.038(2) 0.003(2) -0.022(2) -0.022(2) O1W 0.045(2) 0.056(2) 0.040(2) -0.0048(19) -0.0047(16) -0.0136(19) O2W 0.066(2) 0.054(2) 0.039(2) -0.0051(19) -0.0057(18) -0.022(2) C1 0.034(3) 0.034(3) 0.032(3) -0.005(2) -0.003(2) -0.014(2) C2 0.041(3) 0.030(3) 0.028(3) -0.007(2) -0.001(2) -0.011(2) C3 0.043(3) 0.032(3) 0.033(3) -0.007(2) -0.008(2) -0.008(2) C4 0.041(3) 0.037(3) 0.046(3) -0.009(3) -0.012(2) -0.006(2) C5 0.039(3) 0.040(3) 0.041(3) -0.013(3) 0.005(2) -0.015(2) C6 0.040(3) 0.032(3) 0.033(3) -0.005(2) -0.001(2) -0.014(2) C7 0.040(3) 0.035(3) 0.041(3) -0.004(2) 0.003(2) -0.014(3) C8 0.035(3) 0.036(3) 0.034(3) -0.002(2) -0.007(2) -0.013(2) C9 0.033(3) 0.036(3) 0.034(3) -0.006(2) -0.007(2) -0.012(2) C10 0.037(3) 0.043(3) 0.031(3) -0.004(2) -0.006(2) -0.017(2) C11 0.048(3) 0.042(3) 0.041(3) -0.012(3) -0.012(2) -0.013(3) C12 0.063(3) 0.037(3) 0.046(3) -0.007(3) -0.017(3) -0.019(3) C13 0.054(3) 0.040(3) 0.043(3) -0.003(3) -0.014(3) -0.021(3) C14 0.042(3) 0.046(3) 0.027(3) 0.010(2) -0.001(2) -0.024(3) C15 0.041(3) 0.033(3) 0.037(3) 0.005(2) -0.001(2) -0.004(2) C16 0.039(3) 0.037(3) 0.032(3) -0.001(2) 0.000(2) -0.014(2) C17 0.043(3) 0.037(3) 0.034(3) -0.008(2) 0.002(2) -0.005(3) C18 0.053(3) 0.054(4) 0.056(4) -0.002(3) -0.017(3) -0.020(3) C19 0.062(4) 0.064(4) 0.055(4) 0.002(3) -0.015(3) -0.039(3) C20 0.077(4) 0.047(3) 0.042(3) -0.006(3) -0.017(3) -0.027(3) C21 0.056(4) 0.045(3) 0.062(4) -0.006(3) -0.009(3) -0.005(3) C22 0.048(3) 0.060(4) 0.057(4) -0.011(3) 0.006(3) -0.017(3) C23 0.109(5) 0.056(4) 0.039(4) 0.002(3) -0.019(3) -0.041(4) C24 0.100(5) 0.048(4) 0.042(4) -0.003(3) -0.018(3) -0.032(4) C25 0.078(4) 0.047(3) 0.037(3) -0.007(3) -0.005(3) -0.026(3) C26 0.065(4) 0.035(3) 0.031(3) 0.003(2) -0.007(3) -0.023(3) C27 0.045(3) 0.053(4) 0.052(4) -0.021(3) -0.003(3) -0.007(3) C28 0.040(3) 0.069(4) 0.049(4) -0.015(3) -0.007(3) -0.018(3) C29 0.041(3) 0.071(4) 0.050(4) -0.026(3) -0.007(3) -0.013(3) C30 0.046(3) 0.070(4) 0.054(4) -0.020(3) -0.010(3) -0.018(3) C31 0.072(4) 0.035(3) 0.062(4) -0.001(3) -0.039(3) -0.010(3) C32 0.070(4) 0.040(3) 0.056(4) -0.013(3) -0.026(3) -0.018(3) C33 0.030(3) 0.044(3) 0.033(3) -0.009(2) -0.003(2) -0.008(2) C34 0.050(3) 0.036(3) 0.040(3) 0.001(2) -0.014(2) -0.006(3) C35 0.052(3) 0.037(3) 0.039(3) -0.008(2) -0.008(2) -0.016(3) C36 0.043(3) 0.071(4) 0.040(3) -0.017(3) -0.007(2) -0.021(3) C37 0.078(5) 0.138(7) 0.042(4) -0.010(4) -0.014(3) -0.058(5) C38 0.065(4) 0.089(6) 0.086(6) -0.019(5) 0.001(4) -0.023(4) C39 0.062(4) 0.075(5) 0.061(4) -0.034(4) -0.012(3) -0.012(4) C40 0.068(4) 0.072(5) 0.053(4) -0.011(4) -0.005(3) -0.018(4) C41 0.055(4) 0.063(4) 0.048(4) -0.010(3) -0.002(3) -0.009(3) C42 0.081(5) 0.074(5) 0.068(5) -0.034(4) 0.022(4) -0.041(4) C43 0.102(6) 0.085(5) 0.076(5) -0.024(4) 0.005(4) -0.068(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 Cd1 N1 2.333(4) . ? Cd1 N2 2.339(4) 1_455 ? Cd1 O1W 2.384(3) . ? Cd1 O7 2.388(4) 2_666 ? Cd1 O9 2.418(4) . ? Cd1 O6 2.513(4) 2_666 ? Cd1 O8 2.515(4) . ? Cd2 N3 2.304(4) . ? Cd2 N4 2.348(4) 1_565 ? Cd2 O2W 2.377(4) . ? Cd2 O2 2.416(4) . ? Cd2 O4 2.432(4) 2_775 ? Cd2 O1 2.467(4) . ? Cd2 O3 2.520(4) 2_775 ? N1 C35 1.331(6) . ? N1 C31 1.341(7) . ? N2 C41 1.317(7) . ? N2 C42 1.325(7) . ? N2 Cd1 2.339(4) 1_655 ? N3 C18 1.329(7) . ? N3 C22 1.336(7) . ? N4 C29 1.329(6) . ? N4 C28 1.333(6) . ? N4 Cd2 2.348(4) 1_545 ? O1 C14 1.237(6) . ? O2 C14 1.267(6) . ? O3 C15 1.235(6) . ? O3 Cd2 2.520(4) 2_775 ? O4 C15 1.245(7) . ? O4 Cd2 2.432(4) 2_775 ? O5 C7 1.211(6) . ? O6 C16 1.227(6) . ? O6 Cd1 2.513(4) 2_666 ? O7 C16 1.264(6) . ? O7 Cd1 2.388(4) 2_666 ? O8 C17 1.239(6) . ? O9 C17 1.257(7) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? C1 C2 1.391(6) . ? C1 C6 1.400(6) . ? C1 C14 1.517(7) . ? C2 C3 1.387(7) . ? C2 C15 1.521(7) . ? C3 C4 1.383(7) . ? C3 H3 0.9300 . ? C4 C5 1.389(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 H5 0.9300 . ? C6 C7 1.491(7) . ? C7 C8 1.486(7) . ? C8 C13 1.386(7) . ? C8 C9 1.403(7) . ? C9 C10 1.415(7) . ? C9 C16 1.516(7) . ? C10 C11 1.386(7) . ? C10 C17 1.495(7) . ? C11 C12 1.379(7) . ? C11 H11 0.9300 . ? C12 C13 1.372(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C18 C19 1.378(8) . ? C18 H18 0.9300 . ? C19 C20 1.373(8) . ? C19 H19 0.9300 . ? C20 C21 1.377(8) . ? C20 C23 1.509(8) . ? C21 C22 1.386(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.499(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.539(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.497(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.363(8) . ? C26 C30 1.375(8) . ? C27 C28 1.369(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.366(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.373(8) . ? C31 H31 0.9300 . ? C32 C33 1.376(7) . ? C32 H32 0.9300 . ? C33 C34 1.375(7) . ? C33 C36 1.504(7) . ? C34 C35 1.373(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.543(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.421(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.595(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.315(9) . ? C39 C43 1.373(9) . ? C40 C41 1.358(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.433(9) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N2 86.84(15) . 1_455 ? N1 Cd1 O1W 94.35(14) . . ? N2 Cd1 O1W 178.81(14) 1_455 . ? N1 Cd1 O7 139.56(14) . 2_666 ? N2 Cd1 O7 91.67(14) 1_455 2_666 ? O1W Cd1 O7 87.42(12) . 2_666 ? N1 Cd1 O9 84.11(15) . . ? N2 Cd1 O9 97.64(16) 1_455 . ? O1W Cd1 O9 82.52(14) . . ? O7 Cd1 O9 135.95(13) 2_666 . ? N1 Cd1 O6 88.33(14) . 2_666 ? N2 Cd1 O6 104.74(15) 1_455 2_666 ? O1W Cd1 O6 75.29(13) . 2_666 ? O7 Cd1 O6 53.06(12) 2_666 2_666 ? O9 Cd1 O6 155.92(14) . 2_666 ? N1 Cd1 O8 136.63(14) . . ? N2 Cd1 O8 97.89(14) 1_455 . ? O1W Cd1 O8 81.26(12) . . ? O7 Cd1 O8 83.62(13) 2_666 . ? O9 Cd1 O8 52.52(13) . . ? O6 Cd1 O8 130.77(13) 2_666 . ? N3 Cd2 N4 88.49(15) . 1_565 ? N3 Cd2 O2W 172.60(14) . . ? N4 Cd2 O2W 84.82(14) 1_565 . ? N3 Cd2 O2 95.79(14) . . ? N4 Cd2 O2 141.53(14) 1_565 . ? O2W Cd2 O2 87.53(13) . . ? N3 Cd2 O4 97.70(15) . 2_775 ? N4 Cd2 O4 83.22(14) 1_565 2_775 ? O2W Cd2 O4 84.67(14) . 2_775 ? O2 Cd2 O4 133.49(13) . 2_775 ? N3 Cd2 O1 97.44(15) . . ? N4 Cd2 O1 88.02(14) 1_565 . ? O2W Cd2 O1 79.21(14) . . ? O2 Cd2 O1 53.51(13) . . ? O4 Cd2 O1 162.28(15) 2_775 . ? N3 Cd2 O3 103.41(14) . 2_775 ? N4 Cd2 O3 134.66(14) 1_565 2_775 ? O2W Cd2 O3 83.60(13) . 2_775 ? O2 Cd2 O3 81.45(13) . 2_775 ? O4 Cd2 O3 52.14(13) 2_775 2_775 ? O1 Cd2 O3 131.98(13) . 2_775 ? C35 N1 C31 116.1(5) . . ? C35 N1 Cd1 120.4(3) . . ? C31 N1 Cd1 123.3(4) . . ? C41 N2 C42 116.2(5) . . ? C41 N2 Cd1 122.5(4) . 1_655 ? C42 N2 Cd1 120.3(4) . 1_655 ? C18 N3 C22 116.6(5) . . ? C18 N3 Cd2 123.6(4) . . ? C22 N3 Cd2 119.8(4) . . ? C29 N4 C28 116.5(5) . . ? C29 N4 Cd2 121.9(4) . 1_545 ? C28 N4 Cd2 120.8(4) . 1_545 ? C14 O1 Cd2 90.5(3) . . ? C14 O2 Cd2 92.2(3) . . ? C15 O3 Cd2 88.7(3) . 2_775 ? C15 O4 Cd2 92.5(3) . 2_775 ? C16 O6 Cd1 89.2(3) . 2_666 ? C16 O7 Cd1 94.1(3) . 2_666 ? C17 O8 Cd1 89.0(3) . . ? C17 O9 Cd1 93.0(4) . . ? Cd1 O1W H1WA 110.7 . . ? Cd1 O1W H1WB 105.8 . . ? H1WA O1W H1WB 107.7 . . ? Cd2 O2W H2WA 115.9 . . ? Cd2 O2W H2WB 96.8 . . ? H2WA O2W H2WB 107.7 . . ? C2 C1 C6 119.2(4) . . ? C2 C1 C14 122.5(4) . . ? C6 C1 C14 118.2(4) . . ? C3 C2 C1 119.7(4) . . ? C3 C2 C15 119.2(4) . . ? C1 C2 C15 121.0(4) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.5(5) . . ? C5 C6 C7 120.5(4) . . ? C1 C6 C7 118.2(4) . . ? O5 C7 C8 120.3(5) . . ? O5 C7 C6 118.5(5) . . ? C8 C7 C6 121.1(4) . . ? C13 C8 C9 120.6(5) . . ? C13 C8 C7 119.1(5) . . ? C9 C8 C7 119.7(5) . . ? C8 C9 C10 118.1(5) . . ? C8 C9 C16 120.7(4) . . ? C10 C9 C16 121.3(4) . . ? C11 C10 C9 119.8(5) . . ? C11 C10 C17 118.9(5) . . ? C9 C10 C17 121.2(5) . . ? C12 C11 C10 120.9(5) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 120.0(5) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.5(5) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? O1 C14 O2 122.8(5) . . ? O1 C14 C1 117.6(5) . . ? O2 C14 C1 119.7(5) . . ? O3 C15 O4 122.8(5) . . ? O3 C15 C2 120.1(5) . . ? O4 C15 C2 117.1(5) . . ? O6 C16 O7 123.3(5) . . ? O6 C16 C9 118.3(5) . . ? O7 C16 C9 118.4(5) . . ? O8 C17 O9 122.1(5) . . ? O8 C17 C10 120.5(5) . . ? O9 C17 C10 117.4(5) . . ? N3 C18 C19 123.1(5) . . ? N3 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 116.5(5) . . ? C19 C20 C23 122.4(5) . . ? C21 C20 C23 121.1(6) . . ? C20 C21 C22 119.9(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? N3 C22 C21 123.1(5) . . ? N3 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? C24 C23 C20 111.2(5) . . ? C24 C23 H23A 109.4 . . ? C20 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C20 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 113.5(5) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 109.6(5) . . ? C26 C25 H25A 109.8 . . ? C24 C25 H25A 109.8 . . ? C26 C25 H25B 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C30 116.0(5) . . ? C27 C26 C25 121.1(5) . . ? C30 C26 C25 122.9(5) . . ? C26 C27 C28 121.2(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? N4 C28 C27 122.5(5) . . ? N4 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? N4 C29 C30 123.2(5) . . ? N4 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C29 C30 C26 120.4(5) . . ? C29 C30 H30 119.8 . . ? C26 C30 H30 119.8 . . ? N1 C31 C32 123.2(5) . . ? N1 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C31 C32 C33 120.3(5) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C34 116.3(5) . . ? C32 C33 C36 123.0(5) . . ? C34 C33 C36 120.7(5) . . ? C35 C34 C33 120.4(5) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? N1 C35 C34 123.4(5) . . ? N1 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C33 C36 C37 111.5(4) . . ? C33 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C33 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 113.4(6) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 116.9(6) . . ? C37 C38 H38A 108.1 . . ? C39 C38 H38A 108.1 . . ? C37 C38 H38B 108.1 . . ? C39 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? C40 C39 C43 119.2(6) . . ? C40 C39 C38 121.0(6) . . ? C43 C39 C38 119.8(6) . . ? C39 C40 C41 118.9(7) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? N2 C41 C40 126.0(7) . . ? N2 C41 H41 117.0 . . ? C40 C41 H41 117.0 . . ? N2 C42 C43 120.9(6) . . ? N2 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C39 C43 C42 118.5(6) . . ? C39 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? 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 Cd1 N1 C35 91.7(4) 1_455 . . . ? O1W Cd1 N1 C35 -88.3(4) . . . . ? O7 Cd1 N1 C35 2.8(5) 2_666 . . . ? O9 Cd1 N1 C35 -170.3(4) . . . . ? O6 Cd1 N1 C35 -13.2(4) 2_666 . . . ? O8 Cd1 N1 C35 -170.1(3) . . . . ? N2 Cd1 N1 C31 -82.4(4) 1_455 . . . ? O1W Cd1 N1 C31 97.7(4) . . . . ? O7 Cd1 N1 C31 -171.2(4) 2_666 . . . ? O9 Cd1 N1 C31 15.7(4) . . . . ? O6 Cd1 N1 C31 172.8(4) 2_666 . . . ? O8 Cd1 N1 C31 15.8(5) . . . . ? N4 Cd2 N3 C18 95.3(4) 1_565 . . . ? O2 Cd2 N3 C18 -46.4(4) . . . . ? O4 Cd2 N3 C18 178.2(4) 2_775 . . . ? O1 Cd2 N3 C18 7.5(5) . . . . ? O3 Cd2 N3 C18 -129.0(4) 2_775 . . . ? N4 Cd2 N3 C22 -82.9(4) 1_565 . . . ? O2 Cd2 N3 C22 135.4(4) . . . . ? O4 Cd2 N3 C22 0.1(4) 2_775 . . . ? O1 Cd2 N3 C22 -170.7(4) . . . . ? O3 Cd2 N3 C22 52.9(4) 2_775 . . . ? N3 Cd2 O1 C14 -97.4(3) . . . . ? N4 Cd2 O1 C14 174.4(3) 1_565 . . . ? O2W Cd2 O1 C14 89.3(3) . . . . ? O2 Cd2 O1 C14 -5.7(3) . . . . ? O4 Cd2 O1 C14 114.2(5) 2_775 . . . ? O3 Cd2 O1 C14 18.2(4) 2_775 . . . ? N3 Cd2 O2 C14 100.5(3) . . . . ? N4 Cd2 O2 C14 5.6(4) 1_565 . . . ? O2W Cd2 O2 C14 -72.9(3) . . . . ? O4 Cd2 O2 C14 -153.1(3) 2_775 . . . ? O1 Cd2 O2 C14 5.5(3) . . . . ? O3 Cd2 O2 C14 -156.8(3) 2_775 . . . ? N1 Cd1 O8 C17 10.1(4) . . . . ? N2 Cd1 O8 C17 103.8(3) 1_455 . . . ? O1W Cd1 O8 C17 -77.0(3) . . . . ? O7 Cd1 O8 C17 -165.4(3) 2_666 . . . ? O9 Cd1 O8 C17 10.2(3) . . . . ? O6 Cd1 O8 C17 -138.9(3) 2_666 . . . ? N1 Cd1 O9 C17 169.8(3) . . . . ? N2 Cd1 O9 C17 -104.2(3) 1_455 . . . ? O1W Cd1 O9 C17 74.6(3) . . . . ? O7 Cd1 O9 C17 -3.8(4) 2_666 . . . ? O6 Cd1 O9 C17 97.4(4) 2_666 . . . ? O8 Cd1 O9 C17 -10.1(3) . . . . ? C6 C1 C2 C3 -0.6(7) . . . . ? C14 C1 C2 C3 -179.8(5) . . . . ? C6 C1 C2 C15 -176.6(5) . . . . ? C14 C1 C2 C15 4.2(7) . . . . ? C1 C2 C3 C4 3.2(7) . . . . ? C15 C2 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 -2.7(8) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C4 C5 C6 C1 3.1(8) . . . . ? C4 C5 C6 C7 -166.3(5) . . . . ? C2 C1 C6 C5 -2.6(7) . . . . ? C14 C1 C6 C5 176.6(5) . . . . ? C2 C1 C6 C7 167.1(5) . . . . ? C14 C1 C6 C7 -13.7(7) . . . . ? C5 C6 C7 O5 122.9(6) . . . . ? C1 C6 C7 O5 -46.7(7) . . . . ? C5 C6 C7 C8 -59.2(7) . . . . ? C1 C6 C7 C8 131.2(5) . . . . ? O5 C7 C8 C13 144.8(5) . . . . ? C6 C7 C8 C13 -33.1(7) . . . . ? O5 C7 C8 C9 -26.7(8) . . . . ? C6 C7 C8 C9 155.4(5) . . . . ? C13 C8 C9 C10 -2.2(7) . . . . ? C7 C8 C9 C10 169.1(4) . . . . ? C13 C8 C9 C16 178.5(5) . . . . ? C7 C8 C9 C16 -10.1(7) . . . . ? C8 C9 C10 C11 0.5(7) . . . . ? C16 C9 C10 C11 179.7(5) . . . . ? C8 C9 C10 C17 -176.3(4) . . . . ? C16 C9 C10 C17 3.0(7) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C17 C10 C11 C12 177.9(5) . . . . ? C10 C11 C12 C13 -0.9(8) . . . . ? C11 C12 C13 C8 -0.9(8) . . . . ? C9 C8 C13 C12 2.4(8) . . . . ? C7 C8 C13 C12 -168.9(5) . . . . ? Cd2 O1 C14 O2 10.3(5) . . . . ? Cd2 O1 C14 C1 -169.8(4) . . . . ? Cd2 O2 C14 O1 -10.6(5) . . . . ? Cd2 O2 C14 C1 169.5(4) . . . . ? C2 C1 C14 O1 118.4(5) . . . . ? C6 C1 C14 O1 -60.8(7) . . . . ? C2 C1 C14 O2 -61.7(7) . . . . ? C6 C1 C14 O2 119.1(5) . . . . ? Cd2 O3 C15 O4 -20.0(5) 2_775 . . . ? Cd2 O3 C15 C2 160.0(4) 2_775 . . . ? Cd2 O4 C15 O3 20.7(6) 2_775 . . . ? Cd2 O4 C15 C2 -159.3(4) 2_775 . . . ? C3 C2 C15 O3 138.6(5) . . . . ? C1 C2 C15 O3 -45.3(7) . . . . ? C3 C2 C15 O4 -41.4(7) . . . . ? C1 C2 C15 O4 134.7(5) . . . . ? Cd1 O6 C16 O7 5.7(5) 2_666 . . . ? Cd1 O6 C16 C9 -173.6(4) 2_666 . . . ? Cd1 O7 C16 O6 -6.0(5) 2_666 . . . ? Cd1 O7 C16 C9 173.3(4) 2_666 . . . ? C8 C9 C16 O6 -66.8(6) . . . . ? C10 C9 C16 O6 113.9(5) . . . . ? C8 C9 C16 O7 113.8(5) . . . . ? C10 C9 C16 O7 -65.5(6) . . . . ? Cd1 O8 C17 O9 -18.7(5) . . . . ? Cd1 O8 C17 C10 160.7(4) . . . . ? Cd1 O9 C17 O8 19.5(5) . . . . ? Cd1 O9 C17 C10 -159.9(4) . . . . ? C11 C10 C17 O8 141.4(5) . . . . ? C9 C10 C17 O8 -41.8(7) . . . . ? C11 C10 C17 O9 -39.2(7) . . . . ? C9 C10 C17 O9 137.6(5) . . . . ? C22 N3 C18 C19 -2.6(9) . . . . ? Cd2 N3 C18 C19 179.2(5) . . . . ? N3 C18 C19 C20 0.0(10) . . . . ? C18 C19 C20 C21 1.1(9) . . . . ? C18 C19 C20 C23 -178.6(6) . . . . ? C19 C20 C21 C22 0.5(9) . . . . ? C23 C20 C21 C22 -179.9(6) . . . . ? C18 N3 C22 C21 4.3(9) . . . . ? Cd2 N3 C22 C21 -177.4(5) . . . . ? C20 C21 C22 N3 -3.3(10) . . . . ? C19 C20 C23 C24 85.7(8) . . . . ? C21 C20 C23 C24 -93.9(7) . . . . ? C20 C23 C24 C25 -178.2(5) . . . . ? C23 C24 C25 C26 177.4(6) . . . . ? C24 C25 C26 C27 -81.2(7) . . . . ? C24 C25 C26 C30 95.2(7) . . . . ? C30 C26 C27 C28 -3.0(8) . . . . ? C25 C26 C27 C28 173.6(5) . . . . ? C29 N4 C28 C27 3.3(8) . . . . ? Cd2 N4 C28 C27 -166.5(4) 1_545 . . . ? C26 C27 C28 N4 0.2(9) . . . . ? C28 N4 C29 C30 -4.2(9) . . . . ? Cd2 N4 C29 C30 165.5(5) 1_545 . . . ? N4 C29 C30 C26 1.4(10) . . . . ? C27 C26 C30 C29 2.2(8) . . . . ? C25 C26 C30 C29 -174.3(5) . . . . ? C35 N1 C31 C32 2.3(9) . . . . ? Cd1 N1 C31 C32 176.7(4) . . . . ? N1 C31 C32 C33 1.4(10) . . . . ? C31 C32 C33 C34 -3.2(8) . . . . ? C31 C32 C33 C36 174.9(5) . . . . ? C32 C33 C34 C35 1.5(8) . . . . ? C36 C33 C34 C35 -176.7(5) . . . . ? C31 N1 C35 C34 -4.2(8) . . . . ? Cd1 N1 C35 C34 -178.7(4) . . . . ? C33 C34 C35 N1 2.4(8) . . . . ? C32 C33 C36 C37 -102.8(7) . . . . ? C34 C33 C36 C37 75.3(7) . . . . ? C33 C36 C37 C38 71.2(8) . . . . ? C36 C37 C38 C39 -174.9(6) . . . . ? C37 C38 C39 C40 -146.4(8) . . . . ? C37 C38 C39 C43 34.9(10) . . . . ? C43 C39 C40 C41 6.6(10) . . . . ? C38 C39 C40 C41 -172.1(6) . . . . ? C42 N2 C41 C40 -2.4(9) . . . . ? Cd1 N2 C41 C40 166.4(5) 1_655 . . . ? C39 C40 C41 N2 -3.0(10) . . . . ? C41 N2 C42 C43 3.9(10) . . . . ? Cd1 N2 C42 C43 -165.2(5) 1_655 . . . ? C40 C39 C43 C42 -5.0(11) . . . . ? C38 C39 C43 C42 173.7(7) . . . . ? N2 C42 C43 C39 -0.4(11) . . . . ? 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 H1WA O7 0.85 1.94 2.771(5) 166.6 . O1W H1WB O8 0.85 2.15 2.843(6) 138.3 2_666 O2W H2WA O2 0.85 1.94 2.736(5) 156.0 2_775 O2W H2WB O3 0.85 2.06 2.811(6) 147.3 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.154 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.109 data_compound7 _database_code_depnum_ccdc_archive 'CCDC 774758' #TrackingRef '- ZZU1-Ms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C31 H22 Cd2 N4 O10), H O0.50, 4(H2 O)' _chemical_formula_sum 'C62 H53 Cd4 N8 O24.50' _chemical_formula_weight 1751.72 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 triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.659(2) _cell_length_b 11.789(2) _cell_length_c 12.945(3) _cell_angle_alpha 70.39(3) _cell_angle_beta 67.92(3) _cell_angle_gamma 85.77(3) _cell_volume 1550.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2200 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.46 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 869 _exptl_absorpt_coefficient_mu 1.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7608 _exptl_absorpt_correction_T_max 0.7911 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15743 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5440 _reflns_number_gt 4763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2(Bruker, 2009)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT(Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2009)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^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 SHELXL _refine_ls_extinction_coef 0.0110(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5440 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 Cd1 Cd 0.46394(4) 0.31993(3) 0.02166(3) 0.03242(19) Uani 1 1 d . . . Cd2 Cd 0.34090(4) -0.01135(3) -0.11895(4) 0.03846(19) Uani 1 1 d . . . O1 O 0.4579(4) -0.0374(4) 0.2942(5) 0.0665(15) Uani 1 1 d . . . O2 O 0.4784(4) 0.1028(4) 0.1243(4) 0.0424(10) Uani 1 1 d . . . O3 O 0.2952(4) 0.2069(4) 0.0019(4) 0.0457(11) Uani 1 1 d . . . O4 O 0.2774(4) 0.0058(4) 0.0621(4) 0.0430(10) Uani 1 1 d . . . O5 O -0.1833(4) 0.1685(4) 0.0299(4) 0.0486(11) Uani 1 1 d . . . O6 O -0.2943(4) 0.1272(4) 0.2202(4) 0.0568(12) Uani 1 1 d . . . O7 O -0.3489(4) 0.3571(4) 0.0360(4) 0.0473(11) Uani 1 1 d . . . O8 O -0.3652(5) 0.5307(4) 0.0656(5) 0.0630(14) Uani 1 1 d . . . O9 O 0.0033(5) 0.1020(5) 0.1297(6) 0.0767(17) Uani 1 1 d . . . N1 N 0.3839(4) 0.3404(4) 0.2012(4) 0.0354(11) Uani 1 1 d . . . N2 N 0.3668(5) 0.3248(5) 0.3792(4) 0.0415(12) Uani 1 1 d . . . N3 N 0.5838(4) 0.2952(4) -0.1463(4) 0.0360(11) Uani 1 1 d . . . N4 N 0.7437(5) 0.2743(4) -0.2939(4) 0.0409(12) Uani 1 1 d . . . O1W O 0.2627(4) 0.1673(4) -0.1835(4) 0.0491(11) Uani 1 1 d . . . H1WA H 0.2641 0.2026 -0.1364 0.059 Uiso 1 1 d R . . H1WB H 0.2003 0.1937 -0.2013 0.059 Uiso 1 1 d R . . O2W O 1.0225(4) 0.1472(5) 0.8453(5) 0.0680(14) Uani 1 1 d . . . H2WA H 0.9448 0.1409 0.8843 0.082 Uiso 1 1 d R . . H2WB H 1.0302 0.1300 0.7844 0.082 Uiso 1 1 d R . . C1 C 0.4134(5) 0.0403(5) 0.2300(6) 0.0379(14) Uani 1 1 d . . . C2 C 0.2668(5) 0.1063(5) 0.0781(5) 0.0357(13) Uani 1 1 d . . . C3 C -0.2134(5) 0.1915(5) 0.1234(6) 0.0385(14) Uani 1 1 d . . . C4 C -0.3166(5) 0.4340(5) 0.0656(5) 0.0319(12) Uani 1 1 d . . . C5 C 0.0128(5) 0.1720(5) 0.1766(5) 0.0371(13) Uani 1 1 d . . . C6 C 0.2800(5) 0.0693(4) 0.2786(5) 0.0340(13) Uani 1 1 d . . . C7 C 0.2107(5) 0.1028(5) 0.2065(5) 0.0334(13) Uani 1 1 d . . . C8 C 0.0906(5) 0.1428(5) 0.2506(5) 0.0341(13) Uani 1 1 d . . . C9 C 0.0433(5) 0.1487(5) 0.3639(5) 0.0430(14) Uani 1 1 d . . . H9 H -0.0352 0.1767 0.3923 0.052 Uiso 1 1 calc R . . C10 C 0.1113(6) 0.1137(6) 0.4348(6) 0.0484(16) Uani 1 1 d . . . H10 H 0.0787 0.1175 0.5110 0.058 Uiso 1 1 calc R . . C11 C 0.2278(6) 0.0729(5) 0.3928(6) 0.0472(16) Uani 1 1 d . . . H11 H 0.2724 0.0472 0.4421 0.057 Uiso 1 1 calc R . . C12 C -0.0522(5) 0.2873(5) 0.1610(5) 0.0312(12) Uani 1 1 d . . . C13 C -0.1552(5) 0.2993(5) 0.1274(5) 0.0277(11) Uani 1 1 d . . . C14 C -0.2090(5) 0.4124(5) 0.1058(4) 0.0298(12) Uani 1 1 d . . . C15 C -0.1590(5) 0.5072(5) 0.1190(5) 0.0332(12) Uani 1 1 d . . . H15 H -0.1949 0.5812 0.1057 0.040 Uiso 1 1 calc R . . C16 C -0.0577(6) 0.4948(5) 0.1512(5) 0.0398(14) Uani 1 1 d . . . H16 H -0.0251 0.5602 0.1584 0.048 Uiso 1 1 calc R . . C17 C -0.0046(5) 0.3852(5) 0.1727(5) 0.0361(13) Uani 1 1 d . . . H17 H 0.0633 0.3766 0.1952 0.043 Uiso 1 1 calc R . . C18 C 0.2885(6) 0.4078(5) 0.2447(6) 0.0447(15) Uani 1 1 d . . . H18 H 0.2402 0.4534 0.2045 0.054 Uiso 1 1 calc R . . C19 C 0.2766(6) 0.3969(6) 0.3557(6) 0.0493(16) Uani 1 1 d . . . H19 H 0.2181 0.4318 0.4062 0.059 Uiso 1 1 calc R . . C20 C 0.4287(6) 0.2933(5) 0.2842(5) 0.0403(14) Uani 1 1 d . . . H20 H 0.4954 0.2440 0.2776 0.048 Uiso 1 1 calc R . . C21 C 0.3921(7) 0.2923(6) 0.4890(6) 0.0578(19) Uani 1 1 d . . . H21A H 0.4482 0.2273 0.4916 0.069 Uiso 1 1 calc R . . H21B H 0.3153 0.2642 0.5570 0.069 Uiso 1 1 calc R . . C22 C 0.4493(7) 0.4005(6) 0.4945(5) 0.0484(16) Uani 1 1 d . . . C23 C 0.3838(6) 0.4518(6) 0.5790(5) 0.0529(17) Uani 1 1 d . . . H23 H 0.3049 0.4198 0.6325 0.063 Uiso 1 1 calc R . . C24 C 0.4345(7) 0.5500(6) 0.5842(5) 0.0489(16) Uani 1 1 d . . . H24 H 0.3896 0.5838 0.6419 0.059 Uiso 1 1 calc R . . C25 C 0.5514(6) 0.3102(6) -0.2415(5) 0.0482(16) Uani 1 1 d . . . H25 H 0.4722 0.3258 -0.2422 0.058 Uiso 1 1 calc R . . C26 C 0.7014(5) 0.2747(5) -0.1821(5) 0.0364(13) Uani 1 1 d . . . H26 H 0.7496 0.2621 -0.1364 0.044 Uiso 1 1 calc R . . C27 C 0.6468(6) 0.2997(7) -0.3307(6) 0.0547(18) Uani 1 1 d . . . H27 H 0.6485 0.3079 -0.4053 0.066 Uiso 1 1 calc R . . C28 C 0.8736(6) 0.2641(6) -0.3652(6) 0.0516(17) Uani 1 1 d . . . H28A H 0.8761 0.2203 -0.4173 0.062 Uiso 1 1 calc R . . H28B H 0.9147 0.2177 -0.3130 0.062 Uiso 1 1 calc R . . C29 C 0.9384(6) 0.4492(6) -0.5474(5) 0.0500(16) Uani 1 1 d . . . H29 H 0.8968 0.4156 -0.5800 0.060 Uiso 1 1 calc R . . C30 C 0.9424(6) 0.3825(6) -0.4370(5) 0.0475(16) Uani 1 1 d . . . C31 C 1.0056(6) 0.4369(6) -0.3913(5) 0.0501(17) Uani 1 1 d . . . H31 H 1.0097 0.3950 -0.3179 0.060 Uiso 1 1 calc R . . O3W O 0.7060(9) 0.1842(7) 0.4335(7) 0.151(4) Uani 1 1 d . . . H3WB H 0.7422 0.2496 0.4225 0.181 Uiso 1 1 d R . . H3WA H 0.6663 0.1562 0.5078 0.181 Uiso 1 1 d R . . O4W O 0.5000 1.0000 0.5000 0.120(8) Uani 0.50 2 d SP . . H4WA H 0.5683 0.9666 0.4807 0.145 Uiso 0.25 1 d PR . . H4WB H 0.4971 1.0193 0.5585 0.145 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0289(3) 0.0345(3) 0.0403(3) -0.0178(2) -0.0165(2) 0.01023(18) Cd2 0.0265(3) 0.0326(3) 0.0688(4) -0.0255(2) -0.0251(2) 0.00882(18) O1 0.041(3) 0.044(3) 0.112(4) -0.007(3) -0.045(3) 0.013(2) O2 0.025(2) 0.047(2) 0.069(3) -0.030(2) -0.024(2) 0.0167(18) O3 0.051(3) 0.035(2) 0.049(2) -0.017(2) -0.014(2) -0.0016(19) O4 0.048(3) 0.037(2) 0.063(3) -0.030(2) -0.030(2) 0.0148(19) O5 0.043(3) 0.052(3) 0.081(3) -0.048(3) -0.036(2) 0.017(2) O6 0.054(3) 0.041(2) 0.083(3) -0.018(2) -0.034(3) -0.006(2) O7 0.037(2) 0.059(3) 0.073(3) -0.042(2) -0.036(2) 0.0207(19) O8 0.063(3) 0.040(3) 0.112(4) -0.028(3) -0.062(3) 0.023(2) O9 0.069(3) 0.073(3) 0.154(5) -0.083(4) -0.082(4) 0.048(3) N1 0.031(3) 0.036(3) 0.045(3) -0.019(2) -0.016(2) 0.004(2) N2 0.044(3) 0.045(3) 0.045(3) -0.022(2) -0.020(2) -0.004(2) N3 0.033(3) 0.040(3) 0.034(2) -0.012(2) -0.010(2) -0.003(2) N4 0.035(3) 0.048(3) 0.040(3) -0.022(2) -0.007(2) -0.002(2) O1W 0.055(3) 0.041(2) 0.060(3) -0.020(2) -0.031(2) 0.018(2) O2W 0.043(3) 0.078(4) 0.090(4) -0.039(3) -0.025(3) 0.012(3) C1 0.029(3) 0.025(3) 0.066(4) -0.016(3) -0.024(3) 0.001(2) C2 0.022(3) 0.039(3) 0.054(4) -0.021(3) -0.018(3) 0.003(2) C3 0.025(3) 0.033(3) 0.069(4) -0.018(3) -0.029(3) 0.010(2) C4 0.033(3) 0.031(3) 0.037(3) -0.013(2) -0.016(2) 0.004(2) C5 0.030(3) 0.035(3) 0.062(4) -0.025(3) -0.027(3) 0.006(2) C6 0.024(3) 0.022(3) 0.054(4) -0.008(2) -0.018(3) 0.004(2) C7 0.027(3) 0.024(3) 0.053(3) -0.013(3) -0.019(3) 0.003(2) C8 0.025(3) 0.029(3) 0.052(3) -0.014(3) -0.017(3) 0.005(2) C9 0.028(3) 0.049(4) 0.049(4) -0.017(3) -0.011(3) 0.005(3) C10 0.043(4) 0.056(4) 0.042(3) -0.012(3) -0.013(3) -0.002(3) C11 0.047(4) 0.045(4) 0.051(4) -0.006(3) -0.027(3) 0.000(3) C12 0.018(3) 0.038(3) 0.042(3) -0.019(3) -0.010(2) 0.003(2) C13 0.023(3) 0.031(3) 0.038(3) -0.020(2) -0.014(2) 0.004(2) C14 0.028(3) 0.033(3) 0.029(3) -0.013(2) -0.010(2) 0.002(2) C15 0.040(3) 0.028(3) 0.036(3) -0.014(2) -0.016(3) 0.004(2) C16 0.049(4) 0.030(3) 0.046(3) -0.017(3) -0.019(3) -0.004(3) C17 0.028(3) 0.046(3) 0.043(3) -0.020(3) -0.019(3) 0.002(2) C18 0.035(3) 0.047(4) 0.066(4) -0.032(3) -0.022(3) 0.007(3) C19 0.044(4) 0.058(4) 0.058(4) -0.037(3) -0.018(3) 0.008(3) C20 0.043(4) 0.038(3) 0.048(4) -0.021(3) -0.021(3) 0.005(3) C21 0.082(5) 0.052(4) 0.045(4) -0.015(3) -0.029(4) -0.007(4) C22 0.064(5) 0.054(4) 0.043(4) -0.024(3) -0.029(3) 0.003(3) C23 0.051(4) 0.070(5) 0.042(4) -0.022(3) -0.018(3) -0.001(3) C24 0.062(4) 0.056(4) 0.035(3) -0.025(3) -0.016(3) 0.006(3) C25 0.036(4) 0.073(5) 0.039(3) -0.017(3) -0.019(3) -0.007(3) C26 0.034(3) 0.043(3) 0.035(3) -0.018(3) -0.012(3) 0.006(3) C27 0.045(4) 0.079(5) 0.042(4) -0.023(4) -0.014(3) -0.007(4) C28 0.046(4) 0.060(4) 0.050(4) -0.031(3) -0.009(3) 0.011(3) C29 0.040(4) 0.066(4) 0.041(3) -0.025(3) -0.006(3) 0.003(3) C30 0.035(3) 0.058(4) 0.044(4) -0.025(3) -0.004(3) 0.014(3) C31 0.045(4) 0.071(5) 0.032(3) -0.020(3) -0.011(3) 0.012(3) O3W 0.170(9) 0.105(6) 0.122(6) 0.001(5) -0.031(6) 0.024(6) O4W 0.19(2) 0.078(13) 0.144(18) -0.040(13) -0.110(18) 0.003(14) _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 N3 2.202(5) . ? Cd1 O8 2.246(4) 2_565 ? Cd1 N1 2.246(5) . ? Cd1 O7 2.343(4) 1_655 ? Cd1 O2 2.484(4) . ? Cd1 O3 2.590(4) . ? Cd2 O4 2.252(4) . ? Cd2 O1W 2.253(4) . ? Cd2 O2 2.283(4) 2_655 ? Cd2 O5 2.369(5) 2 ? Cd2 O6 2.392(5) 2 ? Cd2 O1 2.510(5) 2_655 ? Cd2 C3 2.708(6) 2 ? Cd2 C1 2.735(6) 2_655 ? O1 C1 1.242(7) . ? O1 Cd2 2.510(5) 2_655 ? O2 C1 1.271(7) . ? O2 Cd2 2.283(4) 2_655 ? O3 C2 1.231(7) . ? O4 C2 1.259(7) . ? O5 C3 1.244(8) . ? O5 Cd2 2.369(5) 2 ? O6 C3 1.271(7) . ? O6 Cd2 2.392(5) 2 ? O7 C4 1.227(6) . ? O7 Cd1 2.343(4) 1_455 ? O8 C4 1.235(7) . ? O8 Cd1 2.246(4) 2_565 ? O9 C5 1.209(7) . ? N1 C20 1.310(7) . ? N1 C18 1.373(7) . ? N2 C20 1.331(8) . ? N2 C19 1.362(8) . ? N2 C21 1.479(8) . ? N3 C26 1.305(7) . ? N3 C25 1.374(7) . ? N4 C26 1.343(7) . ? N4 C27 1.361(8) . ? N4 C28 1.469(8) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? C1 C6 1.504(7) . ? C1 Cd2 2.735(6) 2_655 ? C2 C7 1.528(8) . ? C3 C13 1.509(7) . ? C3 Cd2 2.708(6) 2 ? C4 C14 1.504(7) . ? C5 C12 1.498(8) . ? C5 C8 1.497(8) . ? C6 C11 1.385(8) . ? C6 C7 1.398(8) . ? C7 C8 1.411(7) . ? C8 C9 1.385(8) . ? C9 C10 1.372(9) . ? C9 H9 0.9300 . ? C10 C11 1.378(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.393(7) . ? C12 C13 1.405(7) . ? C13 C14 1.417(7) . ? C14 C15 1.384(7) . ? C15 C16 1.377(8) . ? C15 H15 0.9300 . ? C16 C17 1.378(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.352(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.517(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C24 1.376(9) 2_666 ? C22 C23 1.376(9) . ? C23 C24 1.371(9) . ? C23 H23 0.9300 . ? C24 C22 1.376(9) 2_666 ? C24 H24 0.9300 . ? C25 C27 1.303(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C30 1.480(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C31 1.373(9) 2_764 ? C29 C30 1.398(9) . ? C29 H29 0.9300 . ? C30 C31 1.399(9) . ? C31 C29 1.373(9) 2_764 ? C31 H31 0.9300 . ? O3W H3WB 0.8500 . ? O3W H3WA 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? 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 N3 Cd1 O8 93.3(2) . 2_565 ? N3 Cd1 N1 166.30(17) . . ? O8 Cd1 N1 96.76(19) 2_565 . ? N3 Cd1 O7 84.52(16) . 1_655 ? O8 Cd1 O7 121.72(17) 2_565 1_655 ? N1 Cd1 O7 82.30(16) . 1_655 ? N3 Cd1 O2 88.71(16) . . ? O8 Cd1 O2 150.49(15) 2_565 . ? N1 Cd1 O2 87.08(16) . . ? O7 Cd1 O2 87.79(14) 1_655 . ? N3 Cd1 O3 84.24(15) . . ? O8 Cd1 O3 76.44(15) 2_565 . ? N1 Cd1 O3 107.12(15) . . ? O7 Cd1 O3 159.17(14) 1_655 . ? O2 Cd1 O3 74.49(13) . . ? O4 Cd2 O1W 89.52(15) . . ? O4 Cd2 O2 99.25(16) . 2_655 ? O1W Cd2 O2 143.23(15) . 2_655 ? O4 Cd2 O5 85.24(16) . 2 ? O1W Cd2 O5 110.11(16) . 2 ? O2 Cd2 O5 106.18(15) 2_655 2 ? O4 Cd2 O6 140.48(15) . 2 ? O1W Cd2 O6 102.88(16) . 2 ? O2 Cd2 O6 92.81(15) 2_655 2 ? O5 Cd2 O6 55.23(15) 2 2 ? O4 Cd2 O1 134.11(17) . 2_655 ? O1W Cd2 O1 94.37(15) . 2_655 ? O2 Cd2 O1 54.44(15) 2_655 2_655 ? O5 Cd2 O1 134.56(16) 2 2_655 ? O6 Cd2 O1 82.85(17) 2 2_655 ? O4 Cd2 C3 112.54(18) . 2 ? O1W Cd2 C3 110.30(16) . 2 ? O2 Cd2 C3 99.18(15) 2_655 2 ? O5 Cd2 C3 27.34(17) 2 2 ? O6 Cd2 C3 27.98(17) 2 2 ? O1 Cd2 C3 108.76(19) 2_655 2 ? O4 Cd2 C1 118.49(17) . 2_655 ? O1W Cd2 C1 119.04(17) . 2_655 ? O2 Cd2 C1 27.50(16) 2_655 2_655 ? O5 Cd2 C1 124.14(15) 2 2_655 ? O6 Cd2 C1 88.16(17) 2 2_655 ? O1 Cd2 C1 26.95(16) 2_655 2_655 ? C3 Cd2 C1 106.39(17) 2 2_655 ? C1 O1 Cd2 86.6(4) . 2_655 ? C1 O2 Cd2 96.5(3) . 2_655 ? C1 O2 Cd1 127.3(3) . . ? Cd2 O2 Cd1 124.83(18) 2_655 . ? C2 O3 Cd1 111.1(4) . . ? C2 O4 Cd2 122.6(4) . . ? C3 O5 Cd2 91.7(4) . 2 ? C3 O6 Cd2 90.0(4) . 2 ? C4 O7 Cd1 131.4(4) . 1_455 ? C4 O8 Cd1 146.0(4) . 2_565 ? C20 N1 C18 106.1(5) . . ? C20 N1 Cd1 124.3(4) . . ? C18 N1 Cd1 129.5(4) . . ? C20 N2 C19 107.2(5) . . ? C20 N2 C21 127.3(6) . . ? C19 N2 C21 125.5(6) . . ? C26 N3 C25 105.0(5) . . ? C26 N3 Cd1 128.7(4) . . ? C25 N3 Cd1 126.0(4) . . ? C26 N4 C27 106.7(5) . . ? C26 N4 C28 125.4(5) . . ? C27 N4 C28 127.5(5) . . ? Cd2 O1W H1WA 102.9 . . ? Cd2 O1W H1WB 138.5 . . ? H1WA O1W H1WB 104.5 . . ? H2WA O2W H2WB 104.5 . . ? O1 C1 O2 122.4(5) . . ? O1 C1 C6 120.2(6) . . ? O2 C1 C6 117.3(5) . . ? O1 C1 Cd2 66.4(3) . 2_655 ? O2 C1 Cd2 56.0(3) . 2_655 ? C6 C1 Cd2 173.2(4) . 2_655 ? O3 C2 O4 127.3(6) . . ? O3 C2 C7 116.5(5) . . ? O4 C2 C7 116.2(5) . . ? O5 C3 O6 122.7(5) . . ? O5 C3 C13 121.2(5) . . ? O6 C3 C13 116.1(6) . . ? O5 C3 Cd2 61.0(3) . 2 ? O6 C3 Cd2 62.1(3) . 2 ? C13 C3 Cd2 173.7(4) . 2 ? O7 C4 O8 125.4(5) . . ? O7 C4 C14 119.1(5) . . ? O8 C4 C14 115.4(5) . . ? O9 C5 C12 120.5(5) . . ? O9 C5 C8 119.5(5) . . ? C12 C5 C8 120.0(5) . . ? C11 C6 C7 119.2(5) . . ? C11 C6 C1 120.0(5) . . ? C7 C6 C1 120.6(5) . . ? C6 C7 C8 119.2(5) . . ? C6 C7 C2 120.9(5) . . ? C8 C7 C2 119.7(5) . . ? C9 C8 C7 119.8(5) . . ? C9 C8 C5 120.6(5) . . ? C7 C8 C5 119.5(5) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.9(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C6 121.3(6) . . ? C10 C11 H11 119.3 . . ? C6 C11 H11 119.3 . . ? C17 C12 C13 120.2(5) . . ? C17 C12 C5 119.1(5) . . ? C13 C12 C5 120.5(5) . . ? C12 C13 C14 118.8(5) . . ? C12 C13 C3 120.6(5) . . ? C14 C13 C3 120.4(5) . . ? C15 C14 C13 119.1(5) . . ? C15 C14 C4 118.8(5) . . ? C13 C14 C4 122.1(5) . . ? C16 C15 C14 121.7(5) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.8(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 120.4(5) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 N1 108.6(6) . . ? C19 C18 H18 125.7 . . ? N1 C18 H18 125.7 . . ? C18 C19 N2 106.7(6) . . ? C18 C19 H19 126.7 . . ? N2 C19 H19 126.7 . . ? N1 C20 N2 111.4(6) . . ? N1 C20 H20 124.3 . . ? N2 C20 H20 124.3 . . ? N2 C21 C22 110.4(5) . . ? N2 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N2 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C24 C22 C23 118.9(6) 2_666 . ? C24 C22 C21 121.5(6) 2_666 . ? C23 C22 C21 119.7(6) . . ? C24 C23 C22 120.1(6) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C22 121.1(6) . 2_666 ? C23 C24 H24 119.5 . . ? C22 C24 H24 119.5 2_666 . ? C27 C25 N3 110.6(6) . . ? C27 C25 H25 124.7 . . ? N3 C25 H25 124.7 . . ? N3 C26 N4 110.9(5) . . ? N3 C26 H26 124.6 . . ? N4 C26 H26 124.6 . . ? C25 C27 N4 106.9(6) . . ? C25 C27 H27 126.6 . . ? N4 C27 H27 126.6 . . ? N4 C28 C30 113.0(5) . . ? N4 C28 H28A 109.0 . . ? C30 C28 H28A 109.0 . . ? N4 C28 H28B 109.0 . . ? C30 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C31 C29 C30 121.5(6) 2_764 . ? C31 C29 H29 119.3 2_764 . ? C30 C29 H29 119.3 . . ? C31 C30 C29 117.2(6) . . ? C31 C30 C28 120.4(6) . . ? C29 C30 C28 122.2(6) . . ? C29 C31 C30 121.3(6) 2_764 . ? C29 C31 H31 119.4 2_764 . ? C30 C31 H31 119.4 . . ? H3WB O3W H3WA 104.5 . . ? H4WA O4W H4WB 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cd1 O2 C1 -167.9(4) . . . . ? O8 Cd1 O2 C1 -73.5(6) 2_565 . . . ? N1 Cd1 O2 C1 25.1(4) . . . . ? O7 Cd1 O2 C1 107.5(4) 1_655 . . . ? O3 Cd1 O2 C1 -83.6(4) . . . . ? N3 Cd1 O2 Cd2 57.4(2) . . . 2_655 ? O8 Cd1 O2 Cd2 151.8(3) 2_565 . . 2_655 ? N1 Cd1 O2 Cd2 -109.6(2) . . . 2_655 ? O7 Cd1 O2 Cd2 -27.2(2) 1_655 . . 2_655 ? O3 Cd1 O2 Cd2 141.8(2) . . . 2_655 ? N3 Cd1 O3 C2 111.3(4) . . . . ? O8 Cd1 O3 C2 -153.8(4) 2_565 . . . ? N1 Cd1 O3 C2 -60.8(4) . . . . ? O7 Cd1 O3 C2 53.7(6) 1_655 . . . ? O2 Cd1 O3 C2 21.1(4) . . . . ? O1W Cd2 O4 C2 -28.2(4) . . . . ? O2 Cd2 O4 C2 115.9(4) 2_655 . . . ? O5 Cd2 O4 C2 -138.4(4) 2 . . . ? O6 Cd2 O4 C2 -138.1(4) 2 . . . ? O1 Cd2 O4 C2 67.5(5) 2_655 . . . ? C3 Cd2 O4 C2 -140.0(4) 2 . . . ? C1 Cd2 O4 C2 95.0(4) 2_655 . . . ? N3 Cd1 N1 C20 -27.3(9) . . . . ? O8 Cd1 N1 C20 -164.3(4) 2_565 . . . ? O7 Cd1 N1 C20 -43.1(4) 1_655 . . . ? O2 Cd1 N1 C20 45.0(4) . . . . ? O3 Cd1 N1 C20 117.8(4) . . . . ? N3 Cd1 N1 C18 147.7(6) . . . . ? O8 Cd1 N1 C18 10.6(5) 2_565 . . . ? O7 Cd1 N1 C18 131.8(5) 1_655 . . . ? O2 Cd1 N1 C18 -140.0(5) . . . . ? O3 Cd1 N1 C18 -67.2(5) . . . . ? O8 Cd1 N3 C26 139.7(5) 2_565 . . . ? N1 Cd1 N3 C26 2.3(10) . . . . ? O7 Cd1 N3 C26 18.1(5) 1_655 . . . ? O2 Cd1 N3 C26 -69.8(5) . . . . ? O3 Cd1 N3 C26 -144.3(5) . . . . ? O8 Cd1 N3 C25 -33.4(5) 2_565 . . . ? N1 Cd1 N3 C25 -170.8(6) . . . . ? O7 Cd1 N3 C25 -155.0(5) 1_655 . . . ? O2 Cd1 N3 C25 117.1(5) . . . . ? O3 Cd1 N3 C25 42.6(5) . . . . ? Cd2 O1 C1 O2 -2.5(6) 2_655 . . . ? Cd2 O1 C1 C6 -178.5(5) 2_655 . . . ? Cd2 O2 C1 O1 2.8(6) 2_655 . . . ? Cd1 O2 C1 O1 -141.3(5) . . . . ? Cd2 O2 C1 C6 178.9(4) 2_655 . . . ? Cd1 O2 C1 C6 34.9(7) . . . . ? Cd1 O2 C1 Cd2 -144.0(4) . . . 2_655 ? Cd1 O3 C2 O4 -119.0(5) . . . . ? Cd1 O3 C2 C7 62.0(5) . . . . ? Cd2 O4 C2 O3 -4.9(8) . . . . ? Cd2 O4 C2 C7 174.2(3) . . . . ? Cd2 O5 C3 O6 6.5(6) 2 . . . ? Cd2 O5 C3 C13 -173.2(4) 2 . . . ? Cd2 O6 C3 O5 -6.4(6) 2 . . . ? Cd2 O6 C3 C13 173.3(4) 2 . . . ? Cd1 O7 C4 O8 -20.6(9) 1_455 . . . ? Cd1 O7 C4 C14 159.5(4) 1_455 . . . ? Cd1 O8 C4 O7 -32.1(12) 2_565 . . . ? Cd1 O8 C4 C14 147.8(6) 2_565 . . . ? O1 C1 C6 C11 38.7(8) . . . . ? O2 C1 C6 C11 -137.6(6) . . . . ? O1 C1 C6 C7 -146.8(6) . . . . ? O2 C1 C6 C7 37.0(7) . . . . ? C11 C6 C7 C8 1.8(8) . . . . ? C1 C6 C7 C8 -172.8(5) . . . . ? C11 C6 C7 C2 176.9(5) . . . . ? C1 C6 C7 C2 2.3(7) . . . . ? O3 C2 C7 C6 -105.3(6) . . . . ? O4 C2 C7 C6 75.6(6) . . . . ? O3 C2 C7 C8 69.8(7) . . . . ? O4 C2 C7 C8 -109.3(6) . . . . ? C6 C7 C8 C9 0.3(8) . . . . ? C2 C7 C8 C9 -174.9(5) . . . . ? C6 C7 C8 C5 -176.5(5) . . . . ? C2 C7 C8 C5 8.4(7) . . . . ? O9 C5 C8 C9 -129.1(7) . . . . ? C12 C5 C8 C9 51.0(8) . . . . ? O9 C5 C8 C7 47.6(8) . . . . ? C12 C5 C8 C7 -132.3(6) . . . . ? C7 C8 C9 C10 -1.4(9) . . . . ? C5 C8 C9 C10 175.3(6) . . . . ? C8 C9 C10 C11 0.4(9) . . . . ? C9 C10 C11 C6 1.8(10) . . . . ? C7 C6 C11 C10 -2.9(9) . . . . ? C1 C6 C11 C10 171.8(5) . . . . ? O9 C5 C12 C17 -154.5(6) . . . . ? C8 C5 C12 C17 25.4(8) . . . . ? O9 C5 C12 C13 21.4(9) . . . . ? C8 C5 C12 C13 -158.7(5) . . . . ? C17 C12 C13 C14 0.0(8) . . . . ? C5 C12 C13 C14 -175.8(5) . . . . ? C17 C12 C13 C3 -175.4(5) . . . . ? C5 C12 C13 C3 8.8(8) . . . . ? O5 C3 C13 C12 -94.6(7) . . . . ? O6 C3 C13 C12 85.7(7) . . . . ? O5 C3 C13 C14 90.0(7) . . . . ? O6 C3 C13 C14 -89.7(6) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C3 C13 C14 C15 175.1(5) . . . . ? C12 C13 C14 C4 177.9(5) . . . . ? C3 C13 C14 C4 -6.6(8) . . . . ? O7 C4 C14 C15 168.7(5) . . . . ? O8 C4 C14 C15 -11.2(8) . . . . ? O7 C4 C14 C13 -9.6(8) . . . . ? O8 C4 C14 C13 170.5(5) . . . . ? C13 C14 C15 C16 0.8(8) . . . . ? C4 C14 C15 C16 -177.6(5) . . . . ? C14 C15 C16 C17 -0.9(9) . . . . ? C15 C16 C17 C12 0.6(9) . . . . ? C13 C12 C17 C16 -0.2(8) . . . . ? C5 C12 C17 C16 175.7(5) . . . . ? C20 N1 C18 C19 -1.4(7) . . . . ? Cd1 N1 C18 C19 -177.1(4) . . . . ? N1 C18 C19 N2 1.4(7) . . . . ? C20 N2 C19 C18 -0.8(7) . . . . ? C21 N2 C19 C18 177.3(5) . . . . ? C18 N1 C20 N2 0.9(6) . . . . ? Cd1 N1 C20 N2 176.9(4) . . . . ? C19 N2 C20 N1 -0.1(7) . . . . ? C21 N2 C20 N1 -178.2(5) . . . . ? C20 N2 C21 C22 106.5(7) . . . . ? C19 N2 C21 C22 -71.3(8) . . . . ? N2 C21 C22 C24 -66.5(9) . . . 2_666 ? N2 C21 C22 C23 112.8(7) . . . . ? C24 C22 C23 C24 -0.4(11) 2_666 . . . ? C21 C22 C23 C24 -179.7(6) . . . . ? C22 C23 C24 C22 0.4(12) . . . 2_666 ? C26 N3 C25 C27 -0.4(8) . . . . ? Cd1 N3 C25 C27 174.1(5) . . . . ? C25 N3 C26 N4 -1.0(6) . . . . ? Cd1 N3 C26 N4 -175.2(4) . . . . ? C27 N4 C26 N3 1.9(7) . . . . ? C28 N4 C26 N3 174.6(5) . . . . ? N3 C25 C27 N4 1.5(8) . . . . ? C26 N4 C27 C25 -2.0(8) . . . . ? C28 N4 C27 C25 -174.6(6) . . . . ? C26 N4 C28 C30 -91.9(7) . . . . ? C27 N4 C28 C30 79.4(8) . . . . ? C31 C29 C30 C31 0.2(10) 2_764 . . . ? C31 C29 C30 C28 174.7(6) 2_764 . . . ? N4 C28 C30 C31 90.4(7) . . . . ? N4 C28 C30 C29 -83.9(7) . . . . ? C29 C30 C31 C29 -0.2(10) . . . 2_764 ? C28 C30 C31 C29 -174.8(6) . . . 2_764 ? 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 H1WA O3 0.85 1.97 2.754(6) 152.2 . O1W H1WB O2W 0.85 1.99 2.700(7) 140.1 1_454 O2W H2WA O5 0.85 2.03 2.745(7) 141.6 1_656 O3W H3WA O1 0.85 2.39 3.226(9) 166.1 2_656 O4W H4WB O1 0.85 2.24 3.056(6) 162.1 2_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.902 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.245