#=========================================================================== _publ_requested_journal Crystal Growth & Design _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_phone +86-431-5098620 _publ_contact_author_fax +86-431-5098620 #=========================================================================== data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18.50 H14 N2 O5.50 Zn' _chemical_formula_sum 'C18.50 H14 N2 O5.50 Zn' _chemical_formula_weight 417.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-C2yc' 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 33.0540(12) _cell_length_b 5.845(3) _cell_length_c 20.702(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.116(3) _cell_angle_gamma 90.00 _cell_volume 3424(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9300 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 28.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9479 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.47 _reflns_number_total 3995 _reflns_number_gt 2967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3995 _refine_ls_number_parameters 251 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.747261(12) -0.21524(7) 0.58218(2) 0.02149(14) Uani 1 1 d . . . C1 C 1.0000 -0.9419(9) 0.7500 0.0325(12) Uani 1 2 d S . . C2 C 0.95406(11) -0.8152(6) 0.7081(2) 0.0254(7) Uani 1 1 d . . . C3 C 0.94957(11) -0.6103(6) 0.6712(2) 0.0285(8) Uani 1 1 d . . . H3 H 0.9761 -0.5412 0.6751 0.034 Uiso 1 1 calc R . . C4 C 0.90534(11) -0.5081(6) 0.6282(2) 0.0272(7) Uani 1 1 d . . . H4 H 0.9023 -0.3732 0.6023 0.033 Uiso 1 1 calc R . . C5 C 0.86575(10) -0.6058(6) 0.62383(17) 0.0205(6) Uani 1 1 d . . . C6 C 0.87007(10) -0.8105(6) 0.66177(18) 0.0213(7) Uani 1 1 d . . . C7 C 0.91396(11) -0.9144(6) 0.7027(2) 0.0253(7) Uani 1 1 d . . . H7 H 0.9168 -1.0524 0.7271 0.030 Uiso 1 1 calc R . . C8 C 0.82820(11) -0.9298(6) 0.65816(19) 0.0237(7) Uani 1 1 d . . . C9 C 0.81984(11) -0.4760(6) 0.58381(19) 0.0233(7) Uani 1 1 d . . . C10 C 0.72800(13) 0.0467(7) 0.6898(2) 0.0371(9) Uani 1 1 d . . . H10 H 0.7547 0.1386 0.7085 0.045 Uiso 1 1 calc R . . C11 C 0.69329(14) 0.0739(8) 0.7049(2) 0.0435(10) Uani 1 1 d . . . H11 H 0.6914 0.1857 0.7352 0.052 Uiso 1 1 calc R . . C12 C 0.67701(13) -0.2186(7) 0.6297(2) 0.0311(8) Uani 1 1 d . . . H12 H 0.6614 -0.3439 0.5991 0.037 Uiso 1 1 calc R . . C13 C 0.61567(15) -0.1219(10) 0.6609(3) 0.0553(13) Uani 1 1 d . . . H13A H 0.6202 -0.1146 0.7110 0.066 Uiso 1 1 calc R . . H13B H 0.6025 -0.2706 0.6397 0.066 Uiso 1 1 calc R . . C14 C 0.58142(13) 0.0622(8) 0.6122(2) 0.0438(11) Uani 1 1 d . . . C15 C 0.5810(2) 0.1553(14) 0.5511(4) 0.104(3) Uani 1 1 d . . . H15 H 0.6027 0.1031 0.5387 0.125 Uiso 1 1 calc R . . C16 C 0.5493(2) 0.3247(14) 0.5074(3) 0.101(3) Uani 1 1 d . . . H16 H 0.5501 0.3833 0.4663 0.121 Uiso 1 1 calc R . . C17 C 0.51695(14) 0.4071(9) 0.5236(2) 0.0464(11) Uani 1 1 d . . . C18 C 0.51844(19) 0.3201(11) 0.5858(4) 0.0744(19) Uani 1 1 d . . . H18 H 0.4977 0.3776 0.5996 0.089 Uiso 1 1 calc R . . C19 C 0.54971(18) 0.1491(11) 0.6293(3) 0.0697(17) Uani 1 1 d . . . H19 H 0.5491 0.0926 0.6708 0.084 Uiso 1 1 calc R . . N1 N 0.71805(9) -0.1369(5) 0.64252(16) 0.0276(6) Uani 1 1 d . . . N2 N 0.66123(10) -0.0969(6) 0.66643(18) 0.0355(8) Uani 1 1 d . . . O1 O 0.80601(8) -0.4077(5) 0.51821(14) 0.0371(6) Uani 1 1 d . . . O2 O 0.80025(9) -0.4392(4) 0.62071(15) 0.0356(6) Uani 1 1 d . . . O3 O 0.79070(7) -0.9483(4) 0.59195(13) 0.0265(5) Uani 1 1 d . . . O4 O 0.83245(9) -1.0074(5) 0.71664(15) 0.0398(7) Uani 1 1 d . . . O5 O 1.0000 -1.1498(7) 0.7500 0.0671(16) Uani 1 2 d S . . O1W O 0.70418(12) -0.5418(5) 0.53750(17) 0.0480(8) Uani 1 1 d D . . H1A H 0.7128(18) -0.677(4) 0.560(2) 0.072 Uiso 1 1 d D . . H1B H 0.6987(17) -0.570(8) 0.4916(11) 0.072 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0210(2) 0.0248(2) 0.0210(2) 0.00054(15) 0.01250(16) 0.00239(15) C1 0.021(2) 0.024(3) 0.046(3) 0.000 0.013(2) 0.000 C2 0.0175(14) 0.0238(18) 0.0294(18) -0.0038(14) 0.0083(14) 0.0003(13) C3 0.0201(15) 0.0301(19) 0.035(2) -0.0010(16) 0.0142(15) -0.0035(14) C4 0.0266(16) 0.0254(18) 0.0310(18) 0.0054(15) 0.0158(15) -0.0006(14) C5 0.0199(14) 0.0232(17) 0.0187(15) -0.0035(13) 0.0103(12) -0.0007(12) C6 0.0213(15) 0.0216(17) 0.0212(16) -0.0028(13) 0.0110(13) -0.0028(12) C7 0.0248(15) 0.0184(17) 0.0308(18) 0.0016(14) 0.0131(14) -0.0011(13) C8 0.0214(15) 0.0251(17) 0.0238(17) -0.0011(14) 0.0112(13) -0.0041(13) C9 0.0235(15) 0.0181(16) 0.0263(17) -0.0007(13) 0.0114(14) -0.0020(13) C10 0.0373(19) 0.045(2) 0.030(2) -0.0119(18) 0.0184(17) -0.0009(17) C11 0.043(2) 0.058(3) 0.033(2) -0.008(2) 0.0223(18) 0.008(2) C12 0.0321(18) 0.036(2) 0.033(2) 0.0010(16) 0.0216(16) 0.0012(15) C13 0.043(2) 0.076(3) 0.066(3) 0.028(3) 0.042(2) 0.023(2) C14 0.0326(19) 0.065(3) 0.039(2) 0.011(2) 0.0217(18) 0.0140(19) C15 0.113(5) 0.161(7) 0.070(4) 0.058(4) 0.070(4) 0.099(5) C16 0.124(5) 0.152(7) 0.058(4) 0.056(4) 0.070(4) 0.095(5) C17 0.034(2) 0.065(3) 0.034(2) 0.002(2) 0.0139(18) 0.014(2) C18 0.068(3) 0.092(5) 0.093(5) 0.040(4) 0.063(4) 0.043(3) C19 0.071(3) 0.088(4) 0.082(4) 0.040(3) 0.062(3) 0.034(3) N1 0.0268(14) 0.0341(16) 0.0273(15) -0.0023(13) 0.0180(12) -0.0006(13) N2 0.0317(15) 0.051(2) 0.0327(17) 0.0112(16) 0.0227(14) 0.0123(15) O1 0.0293(12) 0.0468(17) 0.0238(13) 0.0075(12) 0.0056(11) 0.0078(12) O2 0.0381(14) 0.0317(15) 0.0455(16) 0.0071(12) 0.0277(13) 0.0137(11) O3 0.0204(11) 0.0300(14) 0.0247(12) 0.0007(10) 0.0084(10) -0.0034(9) O4 0.0350(13) 0.0551(18) 0.0299(14) 0.0055(13) 0.0172(12) -0.0139(13) O5 0.0251(19) 0.025(2) 0.122(5) 0.000 0.018(2) 0.000 O1W 0.070(2) 0.0357(17) 0.0371(16) -0.0057(13) 0.0263(16) -0.0031(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.987(3) . ? Zn1 O2 1.993(2) . ? Zn1 O1 2.038(2) 7_646 ? Zn1 O3 2.058(2) 1_565 ? Zn1 O1W 2.273(3) . ? C1 O5 1.215(7) . ? C1 C2 1.499(4) 2_756 ? C1 C2 1.499(4) . ? C2 C3 1.387(5) . ? C2 C7 1.398(4) . ? C3 C4 1.394(5) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.398(5) . ? C5 C9 1.505(4) . ? C6 C7 1.386(4) . ? C6 C8 1.517(4) . ? C7 H7 0.9300 . ? C8 O4 1.231(4) . ? C8 O3 1.293(4) . ? C9 O2 1.249(4) . ? C9 O1 1.253(4) . ? C10 C11 1.345(5) . ? C10 N1 1.373(5) . ? C10 H10 0.9300 . ? C11 N2 1.372(6) . ? C11 H11 0.9300 . ? C12 N2 1.329(5) . ? C12 N1 1.329(4) . ? C12 H12 0.9300 . ? C13 N2 1.458(5) . ? C13 C14 1.509(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.366(6) . ? C14 C15 1.371(7) . ? C15 C16 1.386(8) . ? C15 H15 0.9300 . ? C16 C17 1.364(6) . ? C16 H16 0.9300 . ? C17 C18 1.362(7) . ? C17 C17 1.503(9) 5_666 ? C18 C19 1.384(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? O1 Zn1 2.038(2) 7_646 ? O3 Zn1 2.058(2) 1_545 ? O1W H1A 0.89(3) . ? O1W H1B 0.89(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 O2 120.77(12) . . ? N1 Zn1 O1 96.62(11) . 7_646 ? O2 Zn1 O1 139.21(11) . 7_646 ? N1 Zn1 O3 107.72(11) . 1_565 ? O2 Zn1 O3 91.97(11) . 1_565 ? O1 Zn1 O3 91.38(10) 7_646 1_565 ? N1 Zn1 O1W 92.50(12) . . ? O2 Zn1 O1W 81.23(12) . . ? O1 Zn1 O1W 81.47(12) 7_646 . ? O3 Zn1 O1W 159.26(11) 1_565 . ? O5 C1 C2 119.6(2) . 2_756 ? O5 C1 C2 119.6(2) . . ? C2 C1 C2 120.7(4) 2_756 . ? C3 C2 C7 119.2(3) . . ? C3 C2 C1 122.2(3) . . ? C7 C2 C1 118.5(3) . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C9 118.5(3) . . ? C6 C5 C9 121.5(3) . . ? C7 C6 C5 119.3(3) . . ? C7 C6 C8 117.9(3) . . ? C5 C6 C8 122.7(3) . . ? C6 C7 C2 121.1(3) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? O4 C8 O3 124.9(3) . . ? O4 C8 C6 118.9(3) . . ? O3 C8 C6 116.2(3) . . ? O2 C9 O1 126.4(3) . . ? O2 C9 C5 116.4(3) . . ? O1 C9 C5 117.1(3) . . ? C11 C10 N1 109.8(4) . . ? C11 C10 H10 125.1 . . ? N1 C10 H10 125.1 . . ? C10 C11 N2 105.9(4) . . ? C10 C11 H11 127.0 . . ? N2 C11 H11 127.0 . . ? N2 C12 N1 110.8(3) . . ? N2 C12 H12 124.6 . . ? N1 C12 H12 124.6 . . ? N2 C13 C14 111.7(4) . . ? N2 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N2 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C19 C14 C15 116.7(4) . . ? C19 C14 C13 120.2(4) . . ? C15 C14 C13 123.0(4) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 121.1(5) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 116.8(4) . . ? C18 C17 C17 122.4(5) . 5_666 ? C16 C17 C17 120.7(5) . 5_666 ? C17 C18 C19 122.3(4) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C14 C19 C18 121.0(5) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C12 N1 C10 105.5(3) . . ? C12 N1 Zn1 124.7(3) . . ? C10 N1 Zn1 127.8(2) . . ? C12 N2 C11 107.9(3) . . ? C12 N2 C13 126.6(4) . . ? C11 N2 C13 125.1(4) . . ? C9 O1 Zn1 148.9(2) . 7_646 ? C9 O2 Zn1 119.6(2) . . ? C8 O3 Zn1 113.9(2) . 1_545 ? Zn1 O1W H1A 125(3) . . ? Zn1 O1W H1B 109(3) . . ? H1A O1W H1B 103(4) . . ? 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 O5 C1 C2 C3 -144.7(3) . . . . ? C2 C1 C2 C3 35.3(3) 2_756 . . . ? O5 C1 C2 C7 31.6(4) . . . . ? C2 C1 C2 C7 -148.4(4) 2_756 . . . ? C7 C2 C3 C4 -1.2(5) . . . . ? C1 C2 C3 C4 175.1(3) . . . . ? C2 C3 C4 C5 2.0(5) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? C3 C4 C5 C9 173.4(3) . . . . ? C4 C5 C6 C7 -0.6(5) . . . . ? C9 C5 C6 C7 -174.9(3) . . . . ? C4 C5 C6 C8 -178.6(3) . . . . ? C9 C5 C6 C8 7.0(5) . . . . ? C5 C6 C7 C2 1.5(5) . . . . ? C8 C6 C7 C2 179.6(3) . . . . ? C3 C2 C7 C6 -0.5(5) . . . . ? C1 C2 C7 C6 -177.0(3) . . . . ? C7 C6 C8 O4 45.6(5) . . . . ? C5 C6 C8 O4 -136.4(4) . . . . ? C7 C6 C8 O3 -132.2(3) . . . . ? C5 C6 C8 O3 45.8(5) . . . . ? C4 C5 C9 O2 -124.6(3) . . . . ? C6 C5 C9 O2 49.8(4) . . . . ? C4 C5 C9 O1 52.6(4) . . . . ? C6 C5 C9 O1 -133.0(3) . . . . ? N1 C10 C11 N2 0.2(5) . . . . ? N2 C13 C14 C19 -144.9(5) . . . . ? N2 C13 C14 C15 33.2(8) . . . . ? C19 C14 C15 C16 -1.7(12) . . . . ? C13 C14 C15 C16 -179.8(7) . . . . ? C14 C15 C16 C17 0.2(14) . . . . ? C15 C16 C17 C18 2.0(12) . . . . ? C15 C16 C17 C17 179.3(7) . . . 5_666 ? C16 C17 C18 C19 -2.7(10) . . . . ? C17 C17 C18 C19 -179.9(6) 5_666 . . . ? C15 C14 C19 C18 1.0(10) . . . . ? C13 C14 C19 C18 179.2(6) . . . . ? C17 C18 C19 C14 1.2(11) . . . . ? N2 C12 N1 C10 -0.3(4) . . . . ? N2 C12 N1 Zn1 -165.1(2) . . . . ? C11 C10 N1 C12 0.0(5) . . . . ? C11 C10 N1 Zn1 164.2(3) . . . . ? O2 Zn1 N1 C12 -102.1(3) . . . . ? O1 Zn1 N1 C12 60.9(3) 7_646 . . . ? O3 Zn1 N1 C12 154.5(3) 1_565 . . . ? O1W Zn1 N1 C12 -20.8(3) . . . . ? O2 Zn1 N1 C10 96.5(3) . . . . ? O1 Zn1 N1 C10 -100.5(3) 7_646 . . . ? O3 Zn1 N1 C10 -6.9(3) 1_565 . . . ? O1W Zn1 N1 C10 177.8(3) . . . . ? N1 C12 N2 C11 0.4(4) . . . . ? N1 C12 N2 C13 174.1(4) . . . . ? C10 C11 N2 C12 -0.4(5) . . . . ? C10 C11 N2 C13 -174.2(4) . . . . ? C14 C13 N2 C12 -102.4(5) . . . . ? C14 C13 N2 C11 70.3(6) . . . . ? O2 C9 O1 Zn1 -18.9(8) . . . 7_646 ? C5 C9 O1 Zn1 164.2(4) . . . 7_646 ? O1 C9 O2 Zn1 -9.8(5) . . . . ? C5 C9 O2 Zn1 167.1(2) . . . . ? N1 Zn1 O2 C9 -175.9(2) . . . . ? O1 Zn1 O2 C9 30.5(3) 7_646 . . . ? O3 Zn1 O2 C9 -63.9(3) 1_565 . . . ? O1W Zn1 O2 C9 96.4(3) . . . . ? O4 C8 O3 Zn1 -22.1(4) . . . 1_545 ? C6 C8 O3 Zn1 155.6(2) . . . 1_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1B O3 0.89(3) 1.94(2) 2.772(4) 156(5) 7_636 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.647 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.131 #===end data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C31 H20 N4 O9 Zn2, 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 Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7710(3) _cell_length_b 4.7890(7) _cell_length_c 26.3290(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.8220(10) _cell_angle_gamma 90.00 _cell_volume 1473.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 28.36 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9155 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6009 _reflns_number_gt 5091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(13) _refine_ls_number_reflns 6009 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.90459(5) 1.70447(15) 0.449362(16) 0.05252(17) Uani 1 1 d . . . Zn2 Zn 1.17585(3) 1.72262(8) 0.029483(13) 0.02162(9) Uani 1 1 d . . . C1 C 1.1163(5) 1.0550(11) 0.45674(17) 0.0540(14) Uani 1 1 d . . . C2 C 1.1311(4) 0.9941(9) 0.40192(14) 0.0407(11) Uani 1 1 d . . . C3 C 1.2135(4) 0.7968(10) 0.39305(15) 0.0494(13) Uani 1 1 d . . . H3 H 1.2567 0.7102 0.4205 0.059 Uiso 1 1 calc R . . C4 C 1.2311(3) 0.7292(13) 0.34332(12) 0.0390(9) Uani 1 1 d . . . H4 H 1.2871 0.5998 0.3375 0.047 Uiso 1 1 calc R . . C5 C 1.1653(3) 0.8546(9) 0.30199(13) 0.0300(8) Uani 1 1 d . . . C6 C 1.0850(3) 1.0523(9) 0.31101(14) 0.0328(9) Uani 1 1 d . . . H6 H 1.0423 1.1389 0.2834 0.039 Uiso 1 1 calc R . . C7 C 1.0663(4) 1.1256(9) 0.36086(14) 0.0356(10) Uani 1 1 d . . . C8 C 0.9790(4) 1.3427(10) 0.36766(16) 0.0452(11) Uani 1 1 d . . . C9 C 1.1884(3) 0.7855(8) 0.24894(13) 0.0293(9) Uani 1 1 d . . . C10 C 1.1020(3) 0.8702(8) 0.20527(13) 0.0250(8) Uani 1 1 d . . . C11 C 0.9854(3) 0.8191(9) 0.20476(13) 0.0317(9) Uani 1 1 d . . . H11 H 0.9581 0.7288 0.2321 0.038 Uiso 1 1 calc R . . C12 C 0.9116(3) 0.9032(9) 0.16358(14) 0.0317(9) Uani 1 1 d . . . H12 H 0.8338 0.8696 0.1637 0.038 Uiso 1 1 calc R . . C13 C 0.9480(3) 1.0360(8) 0.12182(13) 0.0244(8) Uani 1 1 d . . . C14 C 1.0657(3) 1.0899(7) 0.12245(12) 0.0213(7) Uani 1 1 d . . . C15 C 1.1402(3) 1.0032(8) 0.16372(13) 0.0239(8) Uani 1 1 d . . . H15 H 1.2182 1.0346 0.1637 0.029 Uiso 1 1 calc R . . C16 C 1.1139(3) 1.2453(9) 0.08033(12) 0.0215(7) Uani 1 1 d . . . C17 C 0.8636(3) 1.1131(9) 0.07667(14) 0.0308(9) Uani 1 1 d . . . C18 C 0.7277(4) 1.8017(10) 0.36262(16) 0.0488(13) Uani 1 1 d . . . H18 H 0.7605 1.6681 0.3433 0.059 Uiso 1 1 calc R . . C19 C 0.7002(6) 2.0835(12) 0.4228(2) 0.0708(18) Uani 1 1 d . . . H19 H 0.7098 2.1814 0.4535 0.085 Uiso 1 1 calc R . . C20 C 0.6115(5) 2.1135(12) 0.3858(2) 0.0698(18) Uani 1 1 d . . . H20 H 0.5503 2.2358 0.3862 0.084 Uiso 1 1 calc R . . C21 C 0.5559(4) 1.8809(12) 0.29941(19) 0.0565(13) Uani 1 1 d . . . H21A H 0.4766 1.8796 0.3060 0.068 Uiso 1 1 calc R . . H21B H 0.5732 1.6981 0.2864 0.068 Uiso 1 1 calc R . . C22 C 0.5703(4) 2.0960(9) 0.25899(16) 0.0390(10) Uani 1 1 d . . . C23 C 0.6761(4) 2.1790(12) 0.24663(16) 0.0465(12) Uani 1 1 d . . . H23 H 0.7420 2.1118 0.2657 0.056 Uiso 1 1 calc R . . C24 C 0.6857(4) 2.3590(10) 0.20667(16) 0.0406(10) Uani 1 1 d . . . H24 H 0.7579 2.4093 0.1988 0.049 Uiso 1 1 calc R . . C25 C 0.5894(3) 2.4663(9) 0.17805(15) 0.0314(9) Uani 1 1 d . . . C26 C 0.4837(4) 2.3902(11) 0.19081(17) 0.0432(11) Uani 1 1 d . . . H26 H 0.4179 2.4617 0.1723 0.052 Uiso 1 1 calc R . . C27 C 0.4743(3) 2.2073(14) 0.23115(15) 0.0452(10) Uani 1 1 d . . . H27 H 0.4022 2.1594 0.2395 0.054 Uiso 1 1 calc R . . C28 C 0.6014(3) 2.6652(9) 0.13418(14) 0.0362(10) Uani 1 1 d . . . H28A H 0.5984 2.8559 0.1463 0.043 Uiso 1 1 calc R . . H28B H 0.6753 2.6371 0.1221 0.043 Uiso 1 1 calc R . . C29 C 0.4102(3) 2.7600(8) 0.08411(13) 0.0272(8) Uani 1 1 d . . . H29 H 0.3905 2.9127 0.1030 0.033 Uiso 1 1 calc R . . C30 C 0.4053(3) 2.4282(9) 0.02852(15) 0.0300(8) Uani 1 1 d . . . H30 H 0.3797 2.3098 0.0016 0.036 Uiso 1 1 calc R . . C31 C 0.5088(3) 2.4141(8) 0.05664(15) 0.0303(9) Uani 1 1 d . . . H31 H 0.5668 2.2867 0.0528 0.036 Uiso 1 1 calc R . . N1 N 0.7739(4) 1.8870(9) 0.40812(13) 0.0523(11) Uani 1 1 d . . . N2 N 0.6287(4) 1.9292(9) 0.34759(14) 0.0500(11) Uani 1 1 d . . . N3 N 0.5114(2) 2.6233(6) 0.09186(11) 0.0280(7) Uani 1 1 d . . . N4 N 0.3436(2) 2.6458(6) 0.04593(11) 0.0260(7) Uani 1 1 d . . . O1 O 1.1869(3) 1.1951(12) 0.48452(12) 0.0768(11) Uani 1 1 d . . . O2 O 1.0354(4) 0.9433(8) 0.47638(11) 0.0629(10) Uani 1 1 d . . . O3 O 0.9748(3) 1.4154(8) 0.41411(11) 0.0584(10) Uani 1 1 d . . . O4 O 0.9175(3) 1.4360(9) 0.33056(12) 0.0701(12) Uani 1 1 d . . . O5 O 1.2767(3) 0.6700(10) 0.24151(10) 0.0596(11) Uani 1 1 d . . . O6 O 1.1040(2) 1.5081(5) 0.08094(10) 0.0259(6) Uani 1 1 d . . . O7 O 1.1700(2) 1.1193(5) 0.04997(9) 0.0263(6) Uani 1 1 d . . . O8 O 0.7614(2) 1.1184(9) 0.08066(11) 0.0628(12) Uani 1 1 d . . . O9 O 0.9084(2) 1.1612(6) 0.03598(9) 0.0331(7) Uani 1 1 d . . . O1W O 1.4350(6) 1.212(2) 0.4803(3) 0.198(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0885(4) 0.0479(3) 0.0234(2) 0.0050(3) 0.0162(2) 0.0224(4) Zn2 0.02222(18) 0.02239(18) 0.02020(18) -0.0002(2) 0.00229(13) -0.0001(2) C1 0.086(4) 0.055(3) 0.022(2) 0.005(2) 0.011(3) 0.018(3) C2 0.065(3) 0.039(2) 0.0181(19) -0.0017(18) 0.006(2) 0.002(2) C3 0.076(3) 0.050(3) 0.0197(19) 0.0095(19) -0.002(2) 0.015(2) C4 0.049(2) 0.045(2) 0.0216(17) -0.003(3) -0.0007(15) 0.014(3) C5 0.036(2) 0.036(2) 0.0186(17) 0.0013(16) 0.0047(16) 0.0007(17) C6 0.041(2) 0.038(2) 0.0194(18) -0.0015(17) 0.0062(17) 0.0024(18) C7 0.050(3) 0.035(2) 0.0228(18) -0.0015(16) 0.0087(18) 0.0015(18) C8 0.064(3) 0.044(3) 0.030(2) -0.003(2) 0.014(2) 0.007(2) C9 0.032(2) 0.035(3) 0.0220(17) 0.0017(15) 0.0047(15) 0.0032(15) C10 0.0285(19) 0.0290(19) 0.0175(17) -0.0005(15) 0.0027(14) 0.0026(15) C11 0.036(2) 0.041(2) 0.0180(17) 0.0063(16) 0.0020(16) -0.0069(16) C12 0.0203(19) 0.046(2) 0.029(2) 0.0058(18) 0.0049(16) -0.0060(17) C13 0.0231(18) 0.0293(19) 0.0203(17) -0.0027(15) 0.0007(14) -0.0012(14) C14 0.0247(18) 0.0226(17) 0.0168(16) -0.0026(14) 0.0036(14) -0.0022(14) C15 0.0196(18) 0.031(2) 0.0215(18) -0.0017(16) 0.0049(14) 0.0002(14) C16 0.0204(15) 0.0232(19) 0.0207(15) 0.0004(17) 0.0011(12) -0.0043(17) C17 0.029(2) 0.037(2) 0.0264(19) 0.0058(16) 0.0035(16) 0.0005(16) C18 0.074(3) 0.041(3) 0.035(2) 0.0080(19) 0.020(2) 0.019(2) C19 0.117(5) 0.060(3) 0.038(3) -0.003(3) 0.024(3) 0.033(3) C20 0.095(4) 0.068(4) 0.051(3) 0.007(3) 0.029(3) 0.044(3) C21 0.058(3) 0.054(3) 0.058(3) 0.021(3) 0.009(3) 0.001(3) C22 0.045(3) 0.037(2) 0.035(2) 0.002(2) 0.007(2) 0.008(2) C23 0.040(2) 0.054(3) 0.043(2) 0.012(3) -0.0033(18) 0.014(2) C24 0.030(2) 0.048(3) 0.043(2) 0.008(2) 0.0035(19) -0.0005(19) C25 0.024(2) 0.034(2) 0.035(2) 0.0002(17) 0.0002(17) -0.0002(16) C26 0.031(2) 0.054(3) 0.044(3) 0.010(2) 0.0015(19) 0.008(2) C27 0.038(2) 0.052(2) 0.047(2) 0.009(3) 0.0137(17) 0.001(3) C28 0.0284(19) 0.040(3) 0.037(2) 0.0069(19) -0.0084(16) -0.0066(17) C29 0.0302(18) 0.019(2) 0.0318(18) -0.0037(16) 0.0022(15) -0.0022(15) C30 0.029(2) 0.031(2) 0.030(2) -0.0032(17) 0.0013(16) 0.0035(16) C31 0.0238(19) 0.030(2) 0.038(2) 0.0010(17) 0.0089(17) 0.0061(16) N1 0.084(3) 0.048(2) 0.028(2) 0.0090(18) 0.017(2) 0.018(2) N2 0.072(3) 0.045(2) 0.036(2) 0.0129(18) 0.018(2) 0.021(2) N3 0.0201(15) 0.0313(18) 0.0308(16) 0.0033(13) -0.0047(12) 0.0000(12) N4 0.0237(15) 0.0290(19) 0.0243(14) 0.0011(13) -0.0011(12) 0.0005(11) O1 0.094(3) 0.100(3) 0.0343(16) -0.030(3) -0.0016(17) -0.006(3) O2 0.112(3) 0.052(2) 0.0289(17) 0.0011(16) 0.0259(19) 0.003(2) O3 0.098(3) 0.052(2) 0.0278(16) -0.0045(15) 0.0190(17) 0.024(2) O4 0.091(3) 0.089(3) 0.0300(17) -0.0052(19) 0.0040(18) 0.049(2) O5 0.0469(18) 0.100(3) 0.0330(14) 0.009(2) 0.0082(13) 0.038(2) O6 0.0347(15) 0.0166(12) 0.0284(13) -0.0006(11) 0.0119(11) -0.0030(10) O7 0.0303(14) 0.0232(12) 0.0276(13) -0.0009(10) 0.0121(11) -0.0002(10) O8 0.0236(15) 0.121(4) 0.0433(17) 0.026(2) 0.0040(13) 0.0094(17) O9 0.0290(13) 0.048(2) 0.0216(12) 0.0057(13) 0.0002(10) -0.0017(12) O1W 0.180(6) 0.143(6) 0.290(9) -0.023(9) 0.108(6) 0.038(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.909(3) . ? Zn1 N1 1.978(4) . ? Zn1 O2 1.981(4) 1_565 ? Zn1 O1 2.153(3) 2_756 ? Zn1 O2 2.358(3) 2_756 ? Zn2 O9 1.906(2) 2_755 ? Zn2 O6 1.969(2) . ? Zn2 O7 1.978(2) 1_565 ? Zn2 N4 2.005(3) 1_645 ? C1 O1 1.238(7) . ? C1 O2 1.256(6) . ? C1 C2 1.503(6) . ? C2 C3 1.393(6) . ? C2 C7 1.397(6) . ? C3 C4 1.388(5) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 H4 0.9300 . ? C5 C6 1.378(5) . ? C5 C9 1.491(5) . ? C6 C7 1.401(5) . ? C6 H6 0.9300 . ? C7 C8 1.488(6) . ? C8 O4 1.229(5) . ? C8 O3 1.278(5) . ? C9 O5 1.214(4) . ? C9 C10 1.498(5) . ? C10 C15 1.386(5) . ? C10 C11 1.392(5) . ? C11 C12 1.367(5) . ? C11 H11 0.9300 . ? C12 C13 1.382(5) . ? C12 H12 0.9300 . ? C13 C14 1.406(5) . ? C13 C17 1.502(5) . ? C14 C15 1.377(5) . ? C14 C16 1.502(4) . ? C15 H15 0.9300 . ? C16 O7 1.251(4) . ? C16 O6 1.265(5) . ? C17 O8 1.220(5) . ? C17 O9 1.270(4) . ? C18 N1 1.320(6) . ? C18 N2 1.334(6) . ? C18 H18 0.9300 . ? C19 C20 1.348(8) . ? C19 N1 1.366(6) . ? C19 H19 0.9300 . ? C20 N2 1.372(6) . ? C20 H20 0.9300 . ? C21 N2 1.462(6) . ? C21 C22 1.505(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.380(6) . ? C22 C23 1.382(6) . ? C23 C24 1.375(6) . ? C23 H23 0.9300 . ? C24 C25 1.383(5) . ? C24 H24 0.9300 . ? C25 C26 1.377(6) . ? C25 C28 1.517(5) . ? C26 C27 1.391(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 N3 1.457(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.318(4) . ? C29 N3 1.353(4) . ? C29 H29 0.9300 . ? C30 C31 1.349(5) . ? C30 N4 1.380(5) . ? C30 H30 0.9300 . ? C31 N3 1.363(5) . ? C31 H31 0.9300 . ? N4 Zn2 2.005(3) 1_465 ? O1 Zn1 2.153(3) 2_746 ? O2 Zn1 1.981(4) 1_545 ? O2 Zn1 2.358(3) 2_746 ? O7 Zn2 1.978(2) 1_545 ? O9 Zn2 1.906(2) 2_745 ? 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 N1 114.02(15) . . ? O3 Zn1 O2 103.31(16) . 1_565 ? N1 Zn1 O2 117.56(18) . 1_565 ? O3 Zn1 O1 131.7(2) . 2_756 ? N1 Zn1 O1 91.26(15) . 2_756 ? O2 Zn1 O1 99.42(16) 1_565 2_756 ? O3 Zn1 O2 85.07(13) . 2_756 ? N1 Zn1 O2 145.75(15) . 2_756 ? O2 Zn1 O2 82.24(7) 1_565 2_756 ? O1 Zn1 O2 56.49(15) 2_756 2_756 ? O9 Zn2 O6 108.76(11) 2_755 . ? O9 Zn2 O7 111.33(12) 2_755 1_565 ? O6 Zn2 O7 106.36(10) . 1_565 ? O9 Zn2 N4 124.06(11) 2_755 1_645 ? O6 Zn2 N4 104.38(11) . 1_645 ? O7 Zn2 N4 100.50(11) 1_565 1_645 ? O1 C1 O2 118.4(4) . . ? O1 C1 C2 121.8(5) . . ? O2 C1 C2 119.5(5) . . ? C3 C2 C7 120.2(4) . . ? C3 C2 C1 117.1(4) . . ? C7 C2 C1 122.8(4) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 C9 121.2(3) . . ? C4 C5 C9 119.3(4) . . ? C5 C6 C7 121.4(4) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C2 C7 C6 118.7(4) . . ? C2 C7 C8 122.9(4) . . ? C6 C7 C8 118.4(4) . . ? O4 C8 O3 125.2(5) . . ? O4 C8 C7 120.6(4) . . ? O3 C8 C7 114.3(4) . . ? O5 C9 C5 120.4(3) . . ? O5 C9 C10 121.1(3) . . ? C5 C9 C10 118.5(3) . . ? C15 C10 C11 119.0(3) . . ? C15 C10 C9 118.4(3) . . ? C11 C10 C9 122.6(3) . . ? C12 C11 C10 119.3(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 122.6(3) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 118.2(3) . . ? C12 C13 C17 120.3(3) . . ? C14 C13 C17 121.5(3) . . ? C15 C14 C13 119.2(3) . . ? C15 C14 C16 118.1(3) . . ? C13 C14 C16 122.7(3) . . ? C14 C15 C10 121.7(3) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? O7 C16 O6 123.0(3) . . ? O7 C16 C14 120.5(3) . . ? O6 C16 C14 116.1(3) . . ? O8 C17 O9 125.5(4) . . ? O8 C17 C13 120.2(3) . . ? O9 C17 C13 114.2(3) . . ? N1 C18 N2 112.3(4) . . ? N1 C18 H18 123.9 . . ? N2 C18 H18 123.9 . . ? C20 C19 N1 109.4(5) . . ? C20 C19 H19 125.3 . . ? N1 C19 H19 125.3 . . ? C19 C20 N2 107.0(5) . . ? C19 C20 H20 126.5 . . ? N2 C20 H20 126.5 . . ? N2 C21 C22 113.7(4) . . ? N2 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N2 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C27 C22 C23 117.9(4) . . ? C27 C22 C21 119.1(4) . . ? C23 C22 C21 122.9(4) . . ? C24 C23 C22 121.2(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.9(4) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 118.4(4) . . ? C26 C25 C28 121.4(4) . . ? C24 C25 C28 120.3(3) . . ? C25 C26 C27 120.6(4) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 120.9(4) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? N3 C28 C25 111.8(3) . . ? N3 C28 H28A 109.3 . . ? C25 C28 H28A 109.3 . . ? N3 C28 H28B 109.3 . . ? C25 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? N4 C29 N3 110.4(3) . . ? N4 C29 H29 124.8 . . ? N3 C29 H29 124.8 . . ? C31 C30 N4 109.4(3) . . ? C31 C30 H30 125.3 . . ? N4 C30 H30 125.3 . . ? C30 C31 N3 106.4(3) . . ? C30 C31 H31 126.8 . . ? N3 C31 H31 126.8 . . ? C18 N1 C19 105.3(4) . . ? C18 N1 Zn1 124.8(3) . . ? C19 N1 Zn1 128.9(4) . . ? C18 N2 C20 106.0(4) . . ? C18 N2 C21 125.9(4) . . ? C20 N2 C21 128.0(5) . . ? C29 N3 C31 107.7(3) . . ? C29 N3 C28 126.6(3) . . ? C31 N3 C28 125.3(3) . . ? C29 N4 C30 106.1(3) . . ? C29 N4 Zn2 124.8(2) . 1_465 ? C30 N4 Zn2 127.7(2) . 1_465 ? C1 O1 Zn1 97.1(3) . 2_746 ? C1 O2 Zn1 133.9(3) . 1_545 ? C1 O2 Zn1 87.0(3) . 2_746 ? Zn1 O2 Zn1 138.39(17) 1_545 2_746 ? C8 O3 Zn1 137.0(3) . . ? C16 O6 Zn2 117.6(2) . . ? C16 O7 Zn2 132.5(2) . 1_545 ? C17 O9 Zn2 124.6(2) . 2_745 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 74.3(7) . . . . ? O2 C1 C2 C3 -99.9(6) . . . . ? O1 C1 C2 C7 -105.8(6) . . . . ? O2 C1 C2 C7 80.0(6) . . . . ? C7 C2 C3 C4 -0.3(7) . . . . ? C1 C2 C3 C4 179.6(5) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? C3 C4 C5 C6 1.9(7) . . . . ? C3 C4 C5 C9 178.1(4) . . . . ? C4 C5 C6 C7 -1.4(6) . . . . ? C9 C5 C6 C7 -177.5(4) . . . . ? C3 C2 C7 C6 0.8(7) . . . . ? C1 C2 C7 C6 -179.1(4) . . . . ? C3 C2 C7 C8 -178.5(4) . . . . ? C1 C2 C7 C8 1.6(7) . . . . ? C5 C6 C7 C2 0.0(6) . . . . ? C5 C6 C7 C8 179.4(4) . . . . ? C2 C7 C8 O4 -173.9(5) . . . . ? C6 C7 C8 O4 6.7(7) . . . . ? C2 C7 C8 O3 5.5(7) . . . . ? C6 C7 C8 O3 -173.9(4) . . . . ? C6 C5 C9 O5 160.8(4) . . . . ? C4 C5 C9 O5 -15.3(6) . . . . ? C6 C5 C9 C10 -17.2(6) . . . . ? C4 C5 C9 C10 166.7(4) . . . . ? O5 C9 C10 C15 -45.5(6) . . . . ? C5 C9 C10 C15 132.5(4) . . . . ? O5 C9 C10 C11 134.1(5) . . . . ? C5 C9 C10 C11 -47.9(5) . . . . ? C15 C10 C11 C12 -0.5(6) . . . . ? C9 C10 C11 C12 179.8(4) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? C11 C12 C13 C17 177.5(4) . . . . ? C12 C13 C14 C15 1.5(5) . . . . ? C17 C13 C14 C15 -176.9(3) . . . . ? C12 C13 C14 C16 -176.9(3) . . . . ? C17 C13 C14 C16 4.6(6) . . . . ? C13 C14 C15 C10 -1.6(5) . . . . ? C16 C14 C15 C10 176.9(3) . . . . ? C11 C10 C15 C14 1.1(5) . . . . ? C9 C10 C15 C14 -179.3(3) . . . . ? C15 C14 C16 O7 73.5(4) . . . . ? C13 C14 C16 O7 -108.0(4) . . . . ? C15 C14 C16 O6 -99.7(4) . . . . ? C13 C14 C16 O6 78.8(4) . . . . ? C12 C13 C17 O8 16.6(6) . . . . ? C14 C13 C17 O8 -164.9(4) . . . . ? C12 C13 C17 O9 -161.5(4) . . . . ? C14 C13 C17 O9 16.9(5) . . . . ? N1 C19 C20 N2 1.0(7) . . . . ? N2 C21 C22 C27 -134.7(5) . . . . ? N2 C21 C22 C23 48.4(6) . . . . ? C27 C22 C23 C24 -2.3(7) . . . . ? C21 C22 C23 C24 174.6(5) . . . . ? C22 C23 C24 C25 1.0(8) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C23 C24 C25 C28 179.8(4) . . . . ? C24 C25 C26 C27 -0.7(7) . . . . ? C28 C25 C26 C27 180.0(4) . . . . ? C23 C22 C27 C26 2.1(8) . . . . ? C21 C22 C27 C26 -175.0(5) . . . . ? C25 C26 C27 C22 -0.6(8) . . . . ? C26 C25 C28 N3 -36.2(5) . . . . ? C24 C25 C28 N3 144.5(4) . . . . ? N4 C30 C31 N3 0.2(4) . . . . ? N2 C18 N1 C19 -0.7(6) . . . . ? N2 C18 N1 Zn1 168.4(3) . . . . ? C20 C19 N1 C18 -0.2(6) . . . . ? C20 C19 N1 Zn1 -168.7(4) . . . . ? O3 Zn1 N1 C18 8.0(5) . . . . ? O2 Zn1 N1 C18 129.1(4) 1_565 . . . ? O1 Zn1 N1 C18 -129.6(4) 2_756 . . . ? O2 Zn1 N1 C18 -111.2(4) 2_756 . . . ? O3 Zn1 N1 C19 174.4(5) . . . . ? O2 Zn1 N1 C19 -64.5(5) 1_565 . . . ? O1 Zn1 N1 C19 36.8(5) 2_756 . . . ? O2 Zn1 N1 C19 55.2(6) 2_756 . . . ? N1 C18 N2 C20 1.3(6) . . . . ? N1 C18 N2 C21 -179.6(4) . . . . ? C19 C20 N2 C18 -1.4(6) . . . . ? C19 C20 N2 C21 179.6(5) . . . . ? C22 C21 N2 C18 -99.3(6) . . . . ? C22 C21 N2 C20 79.6(6) . . . . ? N4 C29 N3 C31 0.4(4) . . . . ? N4 C29 N3 C28 -172.0(3) . . . . ? C30 C31 N3 C29 -0.4(4) . . . . ? C30 C31 N3 C28 172.2(3) . . . . ? C25 C28 N3 C29 92.9(4) . . . . ? C25 C28 N3 C31 -78.2(4) . . . . ? N3 C29 N4 C30 -0.3(4) . . . . ? N3 C29 N4 Zn2 166.8(2) . . . 1_465 ? C31 C30 N4 C29 0.1(4) . . . . ? C31 C30 N4 Zn2 -166.5(3) . . . 1_465 ? O2 C1 O1 Zn1 -9.9(6) . . . 2_746 ? C2 C1 O1 Zn1 175.8(4) . . . 2_746 ? O1 C1 O2 Zn1 -179.6(4) . . . 1_545 ? C2 C1 O2 Zn1 -5.2(8) . . . 1_545 ? O1 C1 O2 Zn1 9.0(5) . . . 2_746 ? C2 C1 O2 Zn1 -176.6(4) . . . 2_746 ? O4 C8 O3 Zn1 -11.8(9) . . . . ? C7 C8 O3 Zn1 168.7(3) . . . . ? N1 Zn1 O3 C8 19.8(6) . . . . ? O2 Zn1 O3 C8 -109.0(5) 1_565 . . . ? O1 Zn1 O3 C8 135.2(5) 2_756 . . . ? O2 Zn1 O3 C8 170.2(5) 2_756 . . . ? O7 C16 O6 Zn2 2.5(5) . . . . ? C14 C16 O6 Zn2 175.6(2) . . . . ? O9 Zn2 O6 C16 70.9(3) 2_755 . . . ? O7 Zn2 O6 C16 -169.1(2) 1_565 . . . ? N4 Zn2 O6 C16 -63.4(3) 1_645 . . . ? O6 C16 O7 Zn2 -165.1(2) . . . 1_545 ? C14 C16 O7 Zn2 22.1(5) . . . 1_545 ? O8 C17 O9 Zn2 -5.4(6) . . . 2_745 ? C13 C17 O9 Zn2 172.6(2) . . . 2_745 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.757 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.068 #===end data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H34 N8 O9 Zn2, 3(H2 O)' _chemical_formula_sum 'C37 H40 N8 O12 Zn2' _chemical_formula_weight 919.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9080(5) _cell_length_b 24.5190(7) _cell_length_c 14.7000(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.9690(10) _cell_angle_gamma 90.00 _cell_volume 3910.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22563 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.686 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23854 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9071 _reflns_number_gt 6239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0470P)^2^+0.1138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9071 _refine_ls_number_parameters 550 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 0.49623(3) 0.195953(12) 0.45328(2) 0.03273(10) Uani 1 1 d . . . Zn2 Zn 0.74945(3) 0.085302(13) 0.131515(19) 0.03467(10) Uani 1 1 d . . . C1 C 0.7926(3) 0.09621(11) 0.31523(17) 0.0338(6) Uani 1 1 d . . . C2 C 0.8708(2) 0.09460(10) 0.40619(16) 0.0286(6) Uani 1 1 d . . . C3 C 0.9942(3) 0.07909(11) 0.40768(17) 0.0359(6) Uani 1 1 d . . . H3 H 1.0275 0.0738 0.3526 0.043 Uiso 1 1 calc R . . C4 C 1.0671(3) 0.07157(11) 0.48778(17) 0.0349(6) Uani 1 1 d . . . H4 H 1.1486 0.0606 0.4871 0.042 Uiso 1 1 calc R . . C5 C 1.0185(2) 0.08038(10) 0.57107(15) 0.0265(5) Uani 1 1 d . . . C6 C 0.8967(2) 0.09767(10) 0.57051(16) 0.0278(6) Uani 1 1 d . . . H6 H 0.8647 0.1042 0.6257 0.033 Uiso 1 1 calc R . . C7 C 0.8220(2) 0.10529(9) 0.48869(16) 0.0263(5) Uani 1 1 d . . . C8 C 0.6913(2) 0.12452(10) 0.49385(16) 0.0291(6) Uani 1 1 d . . . C9 C 1.0954(2) 0.06643(10) 0.65673(16) 0.0287(6) Uani 1 1 d . . . C10 C 0.9848(2) 0.14240(10) 0.85914(15) 0.0257(5) Uani 1 1 d . . . C11 C 1.0206(2) 0.13223(10) 0.77294(15) 0.0270(5) Uani 1 1 d . . . H11 H 1.0224 0.1607 0.7314 0.032 Uiso 1 1 calc R . . C12 C 1.0537(2) 0.08025(10) 0.74776(15) 0.0256(5) Uani 1 1 d . . . C13 C 1.0514(3) 0.03765(10) 0.80994(16) 0.0339(6) Uani 1 1 d . . . H13 H 1.0773 0.0030 0.7949 0.041 Uiso 1 1 calc R . . C14 C 1.0108(3) 0.04719(11) 0.89366(17) 0.0366(6) Uani 1 1 d . . . H14 H 1.0057 0.0182 0.9339 0.044 Uiso 1 1 calc R . . C15 C 0.9772(2) 0.09868(10) 0.91966(16) 0.0285(6) Uani 1 1 d . . . C16 C 0.9288(3) 0.10719(11) 1.01089(17) 0.0336(6) Uani 1 1 d . . . C17 C 0.9470(3) 0.19914(10) 0.88387(16) 0.0312(6) Uani 1 1 d . . . C18 C 0.5355(3) 0.16521(16) 0.1313(2) 0.0671(10) Uani 1 1 d . . . H18 H 0.5016 0.1481 0.1793 0.081 Uiso 1 1 calc R . . C19 C 0.4925(4) 0.21101(17) 0.0884(3) 0.0724(11) Uani 1 1 d . . . H19 H 0.4239 0.2310 0.1015 0.087 Uiso 1 1 calc R . . C20 C 0.6532(3) 0.18367(11) 0.02778(19) 0.0406(7) Uani 1 1 d . . . H20 H 0.7164 0.1819 -0.0100 0.049 Uiso 1 1 calc R . . C21 C 0.5627(4) 0.27090(13) -0.0385(2) 0.0613(9) Uani 1 1 d . . . H21A H 0.6463 0.2834 -0.0428 0.074 Uiso 1 1 calc R . . H21B H 0.5190 0.3000 -0.0109 0.074 Uiso 1 1 calc R . . C22 C 0.5013(3) 0.26099(14) -0.1343(2) 0.0564(9) Uani 1 1 d . . . H22A H 0.5084 0.2937 -0.1703 0.068 Uiso 1 1 calc R . . H22B H 0.5449 0.2320 -0.1622 0.068 Uiso 1 1 calc R . . C23 C 0.3689(3) 0.24588(14) -0.1373(2) 0.0550(9) Uani 1 1 d . . . H23A H 0.3318 0.2669 -0.0914 0.066 Uiso 1 1 calc R . . H23B H 0.3631 0.2077 -0.1212 0.066 Uiso 1 1 calc R . . C24 C 0.2937(3) 0.25527(13) -0.23117(19) 0.0478(8) Uani 1 1 d . . . H24A H 0.2075 0.2476 -0.2257 0.057 Uiso 1 1 calc R . . H24B H 0.3001 0.2933 -0.2480 0.057 Uiso 1 1 calc R . . C25 C 0.3213(3) 0.16582(12) -0.31373(19) 0.0424(7) Uani 1 1 d . . . H25 H 0.2846 0.1426 -0.2745 0.051 Uiso 1 1 calc R . . C26 C 0.3924(3) 0.23808(11) -0.37495(19) 0.0390(7) Uani 1 1 d . . . H26 H 0.4128 0.2743 -0.3849 0.047 Uiso 1 1 calc R . . C27 C 0.3705(3) 0.15145(11) -0.39004(19) 0.0418(7) Uani 1 1 d . . . H27 H 0.3732 0.1162 -0.4130 0.050 Uiso 1 1 calc R . . C28 C 0.3863(3) 0.09533(11) 0.3703(2) 0.0431(7) Uani 1 1 d . . . H28 H 0.4408 0.0745 0.4088 0.052 Uiso 1 1 calc R . . C29 C 0.2950(3) 0.16303(13) 0.3016(2) 0.0478(8) Uani 1 1 d . . . H29 H 0.2739 0.1985 0.2840 0.057 Uiso 1 1 calc R . . C30 C 0.2395(3) 0.11768(13) 0.2655(2) 0.0513(8) Uani 1 1 d . . . H30 H 0.1745 0.1160 0.2193 0.062 Uiso 1 1 calc R . . C31 C 0.2764(3) 0.01639(12) 0.2949(2) 0.0510(8) Uani 1 1 d . . . H31A H 0.1944 0.0073 0.3100 0.061 Uiso 1 1 calc R . . H31B H 0.3352 -0.0044 0.3352 0.061 Uiso 1 1 calc R . . C32 C 0.2882(3) 0.00023(12) 0.19661(19) 0.0448(7) Uani 1 1 d . . . H32A H 0.3549 0.0208 0.1743 0.054 Uiso 1 1 calc R . . H32B H 0.2126 0.0097 0.1592 0.054 Uiso 1 1 calc R . . C33 C 0.3132(3) -0.06074(12) 0.1865(2) 0.0490(8) Uani 1 1 d . . . H33A H 0.2550 -0.0810 0.2189 0.059 Uiso 1 1 calc R . . H33B H 0.2986 -0.0704 0.1223 0.059 Uiso 1 1 calc R . . C34 C 0.4426(3) -0.07801(12) 0.2222(2) 0.0509(8) Uani 1 1 d . . . H34A H 0.4574 -0.0692 0.2867 0.061 Uiso 1 1 calc R . . H34B H 0.4504 -0.1172 0.2157 0.061 Uiso 1 1 calc R . . C35 C 0.5698(3) -0.06482(14) 0.0889(2) 0.0579(9) Uani 1 1 d . . . H35 H 0.5463 -0.0959 0.0553 0.069 Uiso 1 1 calc R . . C36 C 0.6451(3) -0.02464(14) 0.0645(2) 0.0547(9) Uani 1 1 d . . . H36 H 0.6828 -0.0236 0.0107 0.066 Uiso 1 1 calc R . . C37 C 0.5905(3) -0.00344(11) 0.19521(19) 0.0401(7) Uani 1 1 d . . . H37 H 0.5828 0.0149 0.2497 0.048 Uiso 1 1 calc R . . N1 N 0.6571(2) 0.01442(10) 0.13189(15) 0.0398(6) Uani 1 1 d . . . N2 N 0.5351(2) -0.05076(9) 0.17259(16) 0.0425(6) Uani 1 1 d . . . N3 N 0.2984(2) 0.07447(9) 0.31064(16) 0.0410(6) Uani 1 1 d . . . N4 N 0.3868(2) 0.14915(9) 0.36807(15) 0.0379(5) Uani 1 1 d . . . N5 N 0.6378(2) 0.14794(10) 0.09235(15) 0.0414(6) Uani 1 1 d . . . N6 N 0.5673(2) 0.22284(10) 0.02268(16) 0.0477(6) Uani 1 1 d . . . N7 N 0.3353(2) 0.22103(9) -0.30451(14) 0.0371(5) Uani 1 1 d . . . N8 N 0.4165(2) 0.19726(9) -0.42918(15) 0.0358(5) Uani 1 1 d . . . O2 O 0.8365(2) 0.21002(8) 0.88349(15) 0.0490(5) Uani 1 1 d . . . O3 O 0.9635(2) 0.14565(8) 1.05976(13) 0.0582(6) Uani 1 1 d . . . O4 O 0.84997(19) 0.07146(8) 1.03037(12) 0.0437(5) Uani 1 1 d . . . O5 O 0.66984(17) 0.17370(7) 0.46798(12) 0.0386(4) Uani 1 1 d . . . O6 O 0.61614(19) 0.09379(8) 0.52350(14) 0.0445(5) Uani 1 1 d . . . O7 O 1.19113(18) 0.04058(8) 0.65541(12) 0.0456(5) Uani 1 1 d . . . O8 O 0.67984(19) 0.09539(9) 0.31173(12) 0.0466(5) Uani 1 1 d . . . O9 O 0.85329(18) 0.09635(8) 0.24511(11) 0.0418(5) Uani 1 1 d . . . O1 O 1.03414(19) 0.23272(7) 0.90169(13) 0.0447(5) Uani 1 1 d . . . O1W O 0.6111(3) 0.98752(9) 0.4484(2) 0.0761(8) Uani 1 1 d D . . O2W O 0.6833(4) 0.28426(16) 0.5831(3) 0.1218(12) Uani 1 1 d D . . O3W O 0.2240(7) 0.31297(18) 0.1995(4) 0.189(2) Uani 1 1 d D . . H1A H 0.673(5) 0.990(3) 0.417(5) 0.284 Uiso 1 1 d D . . H1B H 0.611(7) 1.0180(16) 0.476(5) 0.284 Uiso 1 1 d D . . H2A H 0.615(4) 0.303(3) 0.576(6) 0.284 Uiso 1 1 d D . . H2B H 0.732(6) 0.306(3) 0.556(6) 0.284 Uiso 1 1 d D . . H3A H 0.243(10) 0.284(2) 0.172(5) 0.284 Uiso 1 1 d D . . H3B H 0.236(9) 0.304(3) 0.2564(14) 0.284 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03482(19) 0.03162(17) 0.03250(17) 0.00243(12) 0.00710(13) 0.00378(14) Zn2 0.03488(19) 0.0464(2) 0.02301(15) 0.00013(13) 0.00439(13) -0.00027(15) C1 0.0397(18) 0.0375(15) 0.0242(13) -0.0025(11) 0.0025(12) -0.0005(13) C2 0.0326(15) 0.0335(14) 0.0197(12) -0.0008(10) 0.0035(10) 0.0019(11) C3 0.0360(16) 0.0513(17) 0.0215(12) -0.0044(12) 0.0085(11) 0.0054(13) C4 0.0284(15) 0.0498(17) 0.0274(13) -0.0029(12) 0.0079(11) 0.0081(12) C5 0.0279(14) 0.0317(14) 0.0202(11) -0.0010(10) 0.0041(10) 0.0016(11) C6 0.0354(15) 0.0299(13) 0.0197(12) -0.0005(10) 0.0101(10) -0.0001(11) C7 0.0316(15) 0.0226(12) 0.0253(12) -0.0008(10) 0.0063(10) 0.0014(10) C8 0.0282(15) 0.0340(15) 0.0250(12) -0.0046(11) 0.0020(11) 0.0036(12) C9 0.0310(15) 0.0298(13) 0.0262(13) -0.0028(10) 0.0066(11) 0.0014(11) C10 0.0246(13) 0.0282(13) 0.0242(12) -0.0043(10) 0.0023(10) -0.0008(10) C11 0.0300(14) 0.0288(13) 0.0224(12) 0.0031(10) 0.0042(10) 0.0000(11) C12 0.0241(13) 0.0334(14) 0.0193(11) -0.0012(10) 0.0029(10) 0.0019(11) C13 0.0433(17) 0.0311(14) 0.0279(13) 0.0003(11) 0.0067(12) 0.0140(12) C14 0.0496(18) 0.0333(15) 0.0277(13) 0.0092(11) 0.0088(12) 0.0104(13) C15 0.0316(15) 0.0320(14) 0.0226(12) -0.0005(10) 0.0059(10) 0.0031(11) C16 0.0408(17) 0.0350(15) 0.0260(13) 0.0057(11) 0.0075(12) 0.0086(13) C17 0.0392(17) 0.0320(14) 0.0234(13) 0.0015(10) 0.0079(11) 0.0002(13) C18 0.047(2) 0.101(3) 0.057(2) 0.016(2) 0.0228(17) 0.019(2) C19 0.052(2) 0.101(3) 0.066(2) 0.004(2) 0.0153(19) 0.034(2) C20 0.0345(17) 0.0500(18) 0.0374(16) -0.0013(13) 0.0042(12) 0.0065(14) C21 0.067(3) 0.052(2) 0.062(2) 0.0012(16) -0.0096(18) 0.0100(18) C22 0.058(2) 0.058(2) 0.054(2) 0.0065(16) 0.0061(16) 0.0122(17) C23 0.057(2) 0.067(2) 0.0442(18) -0.0157(15) 0.0188(15) -0.0007(17) C24 0.051(2) 0.0519(19) 0.0431(17) -0.0035(14) 0.0149(15) 0.0162(15) C25 0.0472(19) 0.0412(17) 0.0409(16) 0.0041(13) 0.0141(14) -0.0076(14) C26 0.0405(17) 0.0343(15) 0.0430(16) 0.0042(12) 0.0082(13) 0.0033(13) C27 0.0503(19) 0.0354(16) 0.0414(16) 0.0006(12) 0.0129(14) -0.0034(14) C28 0.0455(19) 0.0394(17) 0.0434(17) 0.0025(13) -0.0001(14) 0.0026(14) C29 0.052(2) 0.0438(18) 0.0462(17) 0.0048(14) -0.0037(15) 0.0077(15) C30 0.049(2) 0.053(2) 0.0492(18) -0.0024(15) -0.0076(15) 0.0016(16) C31 0.060(2) 0.0436(18) 0.0513(19) -0.0043(14) 0.0159(16) -0.0089(16) C32 0.0424(19) 0.0468(18) 0.0441(17) -0.0006(13) -0.0012(14) -0.0025(14) C33 0.047(2) 0.0493(19) 0.0502(18) -0.0060(14) 0.0023(15) -0.0135(15) C34 0.052(2) 0.0413(18) 0.060(2) 0.0075(14) 0.0077(16) -0.0052(15) C35 0.062(2) 0.053(2) 0.058(2) -0.0177(16) 0.0019(18) -0.0060(17) C36 0.059(2) 0.065(2) 0.0430(18) -0.0129(16) 0.0165(16) -0.0050(18) C37 0.0383(17) 0.0452(17) 0.0363(15) -0.0046(13) 0.0013(13) -0.0033(14) N1 0.0379(14) 0.0499(15) 0.0314(12) -0.0009(11) 0.0022(10) -0.0043(11) N2 0.0430(15) 0.0390(14) 0.0454(14) -0.0001(11) 0.0042(12) -0.0026(11) N3 0.0452(15) 0.0362(13) 0.0417(13) -0.0015(10) 0.0053(11) -0.0043(11) N4 0.0404(15) 0.0360(13) 0.0371(13) 0.0005(10) 0.0036(11) 0.0023(11) N5 0.0345(14) 0.0540(15) 0.0361(13) 0.0023(11) 0.0050(10) 0.0058(11) N6 0.0452(16) 0.0557(16) 0.0417(14) -0.0016(12) 0.0022(12) 0.0124(13) N7 0.0380(14) 0.0396(14) 0.0350(13) 0.0017(10) 0.0100(10) 0.0077(11) N8 0.0408(14) 0.0336(12) 0.0342(12) 0.0041(10) 0.0090(10) 0.0027(11) O2 0.0428(13) 0.0408(12) 0.0655(14) -0.0069(10) 0.0152(11) 0.0077(10) O3 0.0917(19) 0.0479(13) 0.0390(12) -0.0165(10) 0.0254(11) -0.0195(12) O4 0.0542(14) 0.0522(12) 0.0273(10) -0.0012(8) 0.0176(9) -0.0059(10) O5 0.0349(11) 0.0364(11) 0.0451(11) 0.0049(8) 0.0071(9) 0.0068(9) O6 0.0370(12) 0.0435(12) 0.0559(13) 0.0045(9) 0.0183(10) 0.0000(10) O7 0.0426(13) 0.0644(14) 0.0308(10) 0.0002(9) 0.0087(9) 0.0229(11) O8 0.0373(13) 0.0706(15) 0.0311(10) -0.0087(9) -0.0004(9) 0.0014(11) O9 0.0420(12) 0.0641(13) 0.0196(9) -0.0015(8) 0.0044(8) 0.0001(10) O1 0.0481(13) 0.0329(11) 0.0549(13) -0.0105(9) 0.0130(10) -0.0083(9) O1W 0.085(2) 0.0453(14) 0.108(2) -0.0048(13) 0.0542(16) -0.0030(13) O2W 0.082(2) 0.163(3) 0.117(3) -0.028(2) -0.008(2) -0.011(2) O3W 0.247(6) 0.156(4) 0.144(4) 0.045(3) -0.083(4) -0.043(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.9610(19) . ? Zn1 O1 1.9671(18) 4_565 ? Zn1 N4 2.000(2) . ? Zn1 N8 2.014(2) 1_556 ? Zn2 O9 1.9368(17) . ? Zn2 O4 1.9665(18) 1_554 ? Zn2 N5 2.007(2) . ? Zn2 N1 2.009(2) . ? C1 O8 1.226(3) . ? C1 O9 1.281(3) . ? C1 C2 1.510(3) . ? C2 C3 1.396(4) . ? C2 C7 1.399(3) . ? C3 C4 1.363(4) . ? C3 H3 0.9300 . ? C4 C5 1.400(3) . ? C4 H4 0.9300 . ? C5 C6 1.394(3) . ? C5 C9 1.478(3) . ? C6 C7 1.393(3) . ? C6 H6 0.9300 . ? C7 C8 1.511(3) . ? C8 O6 1.226(3) . ? C8 O5 1.279(3) . ? C9 O7 1.224(3) . ? C9 C12 1.496(3) . ? C10 C11 1.386(3) . ? C10 C15 1.401(3) . ? C10 C17 1.507(3) . ? C11 C12 1.386(3) . ? C11 H11 0.9300 . ? C12 C13 1.390(3) . ? C13 C14 1.371(3) . ? C13 H13 0.9300 . ? C14 C15 1.380(3) . ? C14 H14 0.9300 . ? C15 C16 1.506(3) . ? C16 O3 1.221(3) . ? C16 O4 1.281(3) . ? C17 O2 1.234(3) . ? C17 O1 1.264(3) . ? C18 C19 1.348(5) . ? C18 N5 1.373(4) . ? C18 H18 0.9300 . ? C19 N6 1.360(4) . ? C19 H19 0.9300 . ? C20 N5 1.315(3) . ? C20 N6 1.338(3) . ? C20 H20 0.9300 . ? C21 N6 1.480(4) . ? C21 C22 1.514(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.487(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.547(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N7 1.475(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C27 1.340(4) . ? C25 N7 1.367(3) . ? C25 H25 0.9300 . ? C26 N8 1.323(3) . ? C26 N7 1.330(3) . ? C26 H26 0.9300 . ? C27 N8 1.380(3) . ? C27 H27 0.9300 . ? C28 N4 1.320(3) . ? C28 N3 1.332(4) . ? C28 H28 0.9300 . ? C29 C30 1.348(4) . ? C29 N4 1.367(3) . ? C29 H29 0.9300 . ? C30 N3 1.374(4) . ? C30 H30 0.9300 . ? C31 N3 1.459(4) . ? C31 C32 1.517(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.530(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.514(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N2 1.466(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.354(5) . ? C35 N2 1.369(4) . ? C35 H35 0.9300 . ? C36 N1 1.374(4) . ? C36 H36 0.9300 . ? C37 N1 1.314(3) . ? C37 N2 1.334(3) . ? C37 H37 0.9300 . ? N8 Zn1 2.014(2) 1_554 ? O4 Zn2 1.9665(18) 1_556 ? O1 Zn1 1.9671(18) 4_666 ? O1W H1A 0.86(6) . ? O1W H1B 0.85(5) . ? O2W H2A 0.87(6) . ? O2W H2B 0.88(7) . ? O3W H3A 0.85(6) . ? O3W H3B 0.86(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O1 92.90(8) . 4_565 ? O5 Zn1 N4 114.59(9) . . ? O1 Zn1 N4 113.85(9) 4_565 . ? O5 Zn1 N8 114.09(8) . 1_556 ? O1 Zn1 N8 116.33(8) 4_565 1_556 ? N4 Zn1 N8 105.28(9) . 1_556 ? O9 Zn2 O4 110.72(8) . 1_554 ? O9 Zn2 N5 115.04(9) . . ? O4 Zn2 N5 106.53(9) 1_554 . ? O9 Zn2 N1 111.54(8) . . ? O4 Zn2 N1 99.90(9) 1_554 . ? N5 Zn2 N1 111.92(10) . . ? O8 C1 O9 124.5(2) . . ? O8 C1 C2 120.6(2) . . ? O9 C1 C2 114.9(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 118.4(2) . . ? C7 C2 C1 122.1(2) . . ? C4 C3 C2 121.7(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.2(2) . . ? C6 C5 C9 122.1(2) . . ? C4 C5 C9 118.5(2) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C2 118.8(2) . . ? C6 C7 C8 117.9(2) . . ? C2 C7 C8 123.3(2) . . ? O6 C8 O5 125.2(2) . . ? O6 C8 C7 119.7(2) . . ? O5 C8 C7 115.1(2) . . ? O7 C9 C5 121.0(2) . . ? O7 C9 C12 118.1(2) . . ? C5 C9 C12 120.8(2) . . ? C11 C10 C15 118.9(2) . . ? C11 C10 C17 119.8(2) . . ? C15 C10 C17 121.2(2) . . ? C12 C11 C10 121.0(2) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 119.5(2) . . ? C11 C12 C9 124.0(2) . . ? C13 C12 C9 116.5(2) . . ? C14 C13 C12 119.4(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.6(2) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 119.3(2) . . ? C14 C15 C16 120.1(2) . . ? C10 C15 C16 120.6(2) . . ? O3 C16 O4 124.8(3) . . ? O3 C16 C15 121.0(3) . . ? O4 C16 C15 114.2(2) . . ? O2 C17 O1 125.0(2) . . ? O2 C17 C10 119.4(2) . . ? O1 C17 C10 115.6(2) . . ? C19 C18 N5 108.7(3) . . ? C19 C18 H18 125.7 . . ? N5 C18 H18 125.7 . . ? C18 C19 N6 107.7(3) . . ? C18 C19 H19 126.1 . . ? N6 C19 H19 126.1 . . ? N5 C20 N6 112.2(3) . . ? N5 C20 H20 123.9 . . ? N6 C20 H20 123.9 . . ? N6 C21 C22 114.9(3) . . ? N6 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N6 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C21 113.7(3) . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 C24 114.4(3) . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N7 C24 C23 113.1(2) . . ? N7 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? N7 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C27 C25 N7 107.0(2) . . ? C27 C25 H25 126.5 . . ? N7 C25 H25 126.5 . . ? N8 C26 N7 111.7(2) . . ? N8 C26 H26 124.2 . . ? N7 C26 H26 124.2 . . ? C25 C27 N8 109.2(2) . . ? C25 C27 H27 125.4 . . ? N8 C27 H27 125.4 . . ? N4 C28 N3 111.8(3) . . ? N4 C28 H28 124.1 . . ? N3 C28 H28 124.1 . . ? C30 C29 N4 110.0(3) . . ? C30 C29 H29 125.0 . . ? N4 C29 H29 125.0 . . ? C29 C30 N3 106.1(3) . . ? C29 C30 H30 126.9 . . ? N3 C30 H30 126.9 . . ? N3 C31 C32 112.1(2) . . ? N3 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? N3 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 112.4(2) . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 114.1(2) . . ? C34 C33 H33A 108.7 . . ? C32 C33 H33A 108.7 . . ? C34 C33 H33B 108.7 . . ? C32 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N2 C34 C33 111.4(2) . . ? N2 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? N2 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 N2 106.6(3) . . ? C36 C35 H35 126.7 . . ? N2 C35 H35 126.7 . . ? C35 C36 N1 109.4(3) . . ? C35 C36 H36 125.3 . . ? N1 C36 H36 125.3 . . ? N1 C37 N2 112.5(2) . . ? N1 C37 H37 123.8 . . ? N2 C37 H37 123.8 . . ? C37 N1 C36 105.1(3) . . ? C37 N1 Zn2 127.20(19) . . ? C36 N1 Zn2 127.7(2) . . ? C37 N2 C35 106.4(3) . . ? C37 N2 C34 126.1(3) . . ? C35 N2 C34 127.0(3) . . ? C28 N3 C30 106.9(2) . . ? C28 N3 C31 125.0(3) . . ? C30 N3 C31 128.0(3) . . ? C28 N4 C29 105.2(2) . . ? C28 N4 Zn1 124.2(2) . . ? C29 N4 Zn1 130.53(19) . . ? C20 N5 C18 105.4(3) . . ? C20 N5 Zn2 126.7(2) . . ? C18 N5 Zn2 127.7(2) . . ? C20 N6 C19 106.0(3) . . ? C20 N6 C21 125.8(3) . . ? C19 N6 C21 128.1(3) . . ? C26 N7 C25 106.9(2) . . ? C26 N7 C24 126.5(3) . . ? C25 N7 C24 126.6(2) . . ? C26 N8 C27 105.1(2) . . ? C26 N8 Zn1 131.27(19) . 1_554 ? C27 N8 Zn1 123.57(18) . 1_554 ? C16 O4 Zn2 119.42(17) . 1_556 ? C8 O5 Zn1 116.11(17) . . ? C1 O9 Zn2 112.87(18) . . ? C17 O1 Zn1 118.37(18) . 4_666 ? H1A O1W H1B 104(7) . . ? H2A O2W H2B 100(6) . . ? H3A O3W H3B 103(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 O8 C1 C2 C3 160.8(3) . . . . ? O9 C1 C2 C3 -16.7(3) . . . . ? O8 C1 C2 C7 -15.7(4) . . . . ? O9 C1 C2 C7 166.8(2) . . . . ? C7 C2 C3 C4 3.1(4) . . . . ? C1 C2 C3 C4 -173.5(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C3 C4 C5 C9 173.7(2) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? C9 C5 C6 C7 -173.4(2) . . . . ? C5 C6 C7 C2 0.8(4) . . . . ? C5 C6 C7 C8 -179.5(2) . . . . ? C3 C2 C7 C6 -2.9(4) . . . . ? C1 C2 C7 C6 173.6(2) . . . . ? C3 C2 C7 C8 177.4(2) . . . . ? C1 C2 C7 C8 -6.1(4) . . . . ? C6 C7 C8 O6 -69.5(3) . . . . ? C2 C7 C8 O6 110.2(3) . . . . ? C6 C7 C8 O5 108.8(3) . . . . ? C2 C7 C8 O5 -71.6(3) . . . . ? C6 C5 C9 O7 164.1(3) . . . . ? C4 C5 C9 O7 -10.5(4) . . . . ? C6 C5 C9 C12 -11.7(4) . . . . ? C4 C5 C9 C12 173.7(2) . . . . ? C15 C10 C11 C12 -2.8(4) . . . . ? C17 C10 C11 C12 -178.8(2) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C10 C11 C12 C9 -178.8(2) . . . . ? O7 C9 C12 C11 129.4(3) . . . . ? C5 C9 C12 C11 -54.7(3) . . . . ? O7 C9 C12 C13 -49.3(3) . . . . ? C5 C9 C12 C13 126.6(3) . . . . ? C11 C12 C13 C14 3.1(4) . . . . ? C9 C12 C13 C14 -178.1(2) . . . . ? C12 C13 C14 C15 -3.0(4) . . . . ? C13 C14 C15 C10 0.0(4) . . . . ? C13 C14 C15 C16 177.9(3) . . . . ? C11 C10 C15 C14 3.0(4) . . . . ? C17 C10 C15 C14 178.9(2) . . . . ? C11 C10 C15 C16 -174.9(2) . . . . ? C17 C10 C15 C16 1.0(4) . . . . ? C14 C15 C16 O3 136.3(3) . . . . ? C10 C15 C16 O3 -45.8(4) . . . . ? C14 C15 C16 O4 -44.2(4) . . . . ? C10 C15 C16 O4 133.7(3) . . . . ? C11 C10 C17 O2 102.1(3) . . . . ? C15 C10 C17 O2 -73.8(3) . . . . ? C11 C10 C17 O1 -76.3(3) . . . . ? C15 C10 C17 O1 107.8(3) . . . . ? N5 C18 C19 N6 -0.1(4) . . . . ? N6 C21 C22 C23 63.0(4) . . . . ? C21 C22 C23 C24 159.5(3) . . . . ? C22 C23 C24 N7 63.8(4) . . . . ? N7 C25 C27 N8 0.4(3) . . . . ? N4 C29 C30 N3 0.0(4) . . . . ? N3 C31 C32 C33 158.7(3) . . . . ? C31 C32 C33 C34 -73.1(4) . . . . ? C32 C33 C34 N2 -61.3(4) . . . . ? N2 C35 C36 N1 -0.3(4) . . . . ? N2 C37 N1 C36 -1.0(3) . . . . ? N2 C37 N1 Zn2 176.38(18) . . . . ? C35 C36 N1 C37 0.8(4) . . . . ? C35 C36 N1 Zn2 -176.5(2) . . . . ? O9 Zn2 N1 C37 50.7(3) . . . . ? O4 Zn2 N1 C37 167.8(2) 1_554 . . . ? N5 Zn2 N1 C37 -79.8(2) . . . . ? O9 Zn2 N1 C36 -132.5(2) . . . . ? O4 Zn2 N1 C36 -15.5(3) 1_554 . . . ? N5 Zn2 N1 C36 97.0(3) . . . . ? N1 C37 N2 C35 0.8(3) . . . . ? N1 C37 N2 C34 -171.7(3) . . . . ? C36 C35 N2 C37 -0.2(4) . . . . ? C36 C35 N2 C34 172.1(3) . . . . ? C33 C34 N2 C37 90.7(3) . . . . ? C33 C34 N2 C35 -80.3(4) . . . . ? N4 C28 N3 C30 1.3(4) . . . . ? N4 C28 N3 C31 178.2(3) . . . . ? C29 C30 N3 C28 -0.7(3) . . . . ? C29 C30 N3 C31 -177.6(3) . . . . ? C32 C31 N3 C28 -120.4(3) . . . . ? C32 C31 N3 C30 55.9(4) . . . . ? N3 C28 N4 C29 -1.3(3) . . . . ? N3 C28 N4 Zn1 175.32(19) . . . . ? C30 C29 N4 C28 0.8(4) . . . . ? C30 C29 N4 Zn1 -175.5(2) . . . . ? O5 Zn1 N4 C28 47.5(3) . . . . ? O1 Zn1 N4 C28 152.7(2) 4_565 . . . ? N8 Zn1 N4 C28 -78.7(2) 1_556 . . . ? O5 Zn1 N4 C29 -136.9(3) . . . . ? O1 Zn1 N4 C29 -31.7(3) 4_565 . . . ? N8 Zn1 N4 C29 96.9(3) 1_556 . . . ? N6 C20 N5 C18 0.0(3) . . . . ? N6 C20 N5 Zn2 -175.42(18) . . . . ? C19 C18 N5 C20 0.1(4) . . . . ? C19 C18 N5 Zn2 175.4(2) . . . . ? O9 Zn2 N5 C20 103.5(2) . . . . ? O4 Zn2 N5 C20 -19.6(3) 1_554 . . . ? N1 Zn2 N5 C20 -127.9(2) . . . . ? O9 Zn2 N5 C18 -71.0(3) . . . . ? O4 Zn2 N5 C18 165.9(3) 1_554 . . . ? N1 Zn2 N5 C18 57.7(3) . . . . ? N5 C20 N6 C19 -0.1(4) . . . . ? N5 C20 N6 C21 176.0(3) . . . . ? C18 C19 N6 C20 0.1(4) . . . . ? C18 C19 N6 C21 -175.8(3) . . . . ? C22 C21 N6 C20 84.5(4) . . . . ? C22 C21 N6 C19 -100.2(4) . . . . ? N8 C26 N7 C25 -0.1(3) . . . . ? N8 C26 N7 C24 -179.4(2) . . . . ? C27 C25 N7 C26 -0.1(3) . . . . ? C27 C25 N7 C24 179.1(3) . . . . ? C23 C24 N7 C26 -110.6(3) . . . . ? C23 C24 N7 C25 70.3(4) . . . . ? N7 C26 N8 C27 0.4(3) . . . . ? N7 C26 N8 Zn1 178.44(18) . . . 1_554 ? C25 C27 N8 C26 -0.5(3) . . . . ? C25 C27 N8 Zn1 -178.72(19) . . . 1_554 ? O3 C16 O4 Zn2 13.6(4) . . . 1_556 ? C15 C16 O4 Zn2 -165.87(16) . . . 1_556 ? O6 C8 O5 Zn1 -12.2(3) . . . . ? C7 C8 O5 Zn1 169.68(15) . . . . ? O1 Zn1 O5 C8 -173.74(17) 4_565 . . . ? N4 Zn1 O5 C8 -55.80(19) . . . . ? N8 Zn1 O5 C8 65.66(18) 1_556 . . . ? O8 C1 O9 Zn2 -7.8(3) . . . . ? C2 C1 O9 Zn2 169.62(17) . . . . ? O4 Zn2 O9 C1 -168.78(17) 1_554 . . . ? N5 Zn2 O9 C1 70.4(2) . . . . ? N1 Zn2 O9 C1 -58.5(2) . . . . ? O2 C17 O1 Zn1 11.2(3) . . . 4_666 ? C10 C17 O1 Zn1 -170.48(15) . . . 4_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 O1W H1A O7 0.86(6) 2.06(3) 2.853(3) 155(6) 3_766 O1W H1B O6 0.85(5) 1.98(4) 2.828(3) 171(7) 1_565 O3W H3A O2W 0.85(6) 2.17(6) 2.941(7) 148(10) 4_565 O3W H3B O2 0.86(3) 2.09(4) 2.907(5) 157(10) 4_565 O2W H2A O3 0.87(6) 2.07(6) 2.941(4) 174(8) 4_565 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.538 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.072 #===end data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H31 N4 O11 Zn2.50' _chemical_formula_weight 799.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6480(8) _cell_length_b 11.7180(9) _cell_length_c 13.6380(10) _cell_angle_alpha 74.2110(10) _cell_angle_beta 72.8770(10) _cell_angle_gamma 80.5940(10) _cell_volume 1558.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 28.37 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.631 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9756 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.37 _reflns_number_total 7174 _reflns_number_gt 6162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0476P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7174 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.5000 0.0000 1.0000 0.01806(9) Uani 1 2 d S . . Zn2 Zn 0.34607(2) 0.16379(2) 0.78823(2) 0.01939(8) Uani 1 1 d . . . Zn3 Zn 0.38926(3) -0.14979(2) 0.87517(2) 0.01930(8) Uani 1 1 d . . . C1 C 0.3865(3) 0.1358(3) 0.5702(2) 0.0373(6) Uani 1 1 d . . . H1 H 0.4775 0.1310 0.5591 0.045 Uiso 1 1 calc R . . C2 C 0.3242(3) 0.1314(3) 0.4989(2) 0.0473(8) Uani 1 1 d . . . H2 H 0.3634 0.1236 0.4302 0.057 Uiso 1 1 calc R . . C3 C 0.1760(3) 0.1511(2) 0.6466(2) 0.0293(5) Uani 1 1 d . . . C4 C 0.0468(3) 0.1651(3) 0.7242(2) 0.0413(7) Uani 1 1 d . . . H4A H -0.0043 0.2341 0.6926 0.050 Uiso 1 1 calc R . . H4B H 0.0628 0.1820 0.7851 0.050 Uiso 1 1 calc R . . C5 C -0.0372(3) 0.0594(4) 0.7633(3) 0.0572(9) Uani 1 1 d . . . H5A H -0.1179 0.0782 0.8129 0.086 Uiso 1 1 calc R . . H5B H 0.0106 -0.0093 0.7970 0.086 Uiso 1 1 calc R . . H5C H -0.0569 0.0431 0.7044 0.086 Uiso 1 1 calc R . . C6 C 0.0846(4) 0.1325(3) 0.5019(3) 0.0539(9) Uani 1 1 d . . . H6A H 0.1057 0.1742 0.4279 0.065 Uiso 1 1 calc R . . H6B H 0.0033 0.1714 0.5378 0.065 Uiso 1 1 calc R . . C7 C 0.0644(3) 0.0044(3) 0.5116(3) 0.0539(9) Uani 1 1 d . . . H7A H 0.0636 -0.0417 0.5826 0.065 Uiso 1 1 calc R . . H7B H 0.1374 -0.0291 0.4627 0.065 Uiso 1 1 calc R . . C8 C 0.3056(3) -0.1689(2) 0.68771(19) 0.0261(5) Uani 1 1 d . . . H8 H 0.2664 -0.0911 0.6784 0.031 Uiso 1 1 calc R . . C9 C 0.3076(3) -0.2452(2) 0.6284(2) 0.0298(6) Uani 1 1 d . . . H9 H 0.2716 -0.2297 0.5712 0.036 Uiso 1 1 calc R . . C10 C 0.4108(2) -0.3347(2) 0.75092(17) 0.0186(4) Uani 1 1 d . . . C11 C 0.4817(2) -0.4293(2) 0.8182(2) 0.0271(5) Uani 1 1 d . . . H11A H 0.5291 -0.3917 0.8500 0.033 Uiso 1 1 calc R . . H11B H 0.5462 -0.4751 0.7737 0.033 Uiso 1 1 calc R . . C12 C 0.3917(3) -0.5137(3) 0.9054(2) 0.0409(7) Uani 1 1 d . . . H12A H 0.4435 -0.5722 0.9454 0.061 Uiso 1 1 calc R . . H12B H 0.3457 -0.5527 0.8748 0.061 Uiso 1 1 calc R . . H12C H 0.3290 -0.4695 0.9512 0.061 Uiso 1 1 calc R . . C13 C 0.3962(3) -0.4586(2) 0.6295(2) 0.0276(5) Uani 1 1 d . . . H13A H 0.3132 -0.4773 0.6244 0.033 Uiso 1 1 calc R . . H13B H 0.4278 -0.5245 0.6797 0.033 Uiso 1 1 calc R . . C14 C 0.4955(2) -0.4459(2) 0.52225(19) 0.0266(5) Uani 1 1 d . . . H14A H 0.5815 -0.4373 0.5288 0.032 Uiso 1 1 calc R . . H14B H 0.4695 -0.3747 0.4738 0.032 Uiso 1 1 calc R . . C15 C 0.7260(2) 0.3114(2) 0.80296(17) 0.0183(4) Uani 1 1 d . . . C16 C 0.7074(2) 0.3035(2) 0.70756(18) 0.0190(4) Uani 1 1 d . . . C17 C 0.7719(2) 0.3756(2) 0.61376(18) 0.0242(5) Uani 1 1 d . . . H17 H 0.7585 0.3709 0.5507 0.029 Uiso 1 1 calc R . . C18 C 0.8562(2) 0.4547(2) 0.61197(18) 0.0249(5) Uani 1 1 d . . . H18 H 0.8994 0.5023 0.5481 0.030 Uiso 1 1 calc R . . C19 C 0.8759(2) 0.4626(2) 0.70605(18) 0.0200(4) Uani 1 1 d . . . C20 C 0.8094(2) 0.3925(2) 0.80082(18) 0.0198(4) Uani 1 1 d . . . H20 H 0.8206 0.3997 0.8639 0.024 Uiso 1 1 calc R . . C21 C 0.6638(2) 0.2313(2) 0.90718(18) 0.0203(4) Uani 1 1 d . . . C22 C 0.6090(2) 0.2257(2) 0.70462(18) 0.0233(5) Uani 1 1 d . . . C23 C 0.9786(2) 0.5369(2) 0.70408(19) 0.0237(5) Uani 1 1 d . . . C24 C 0.9504(2) 0.6001(2) 0.79039(18) 0.0212(5) Uani 1 1 d . . . C25 C 1.0444(2) 0.6003(2) 0.8425(2) 0.0271(5) Uani 1 1 d . . . H25 H 1.1270 0.5591 0.8249 0.032 Uiso 1 1 calc R . . C26 C 1.0141(2) 0.6624(2) 0.9209(2) 0.0283(5) Uani 1 1 d . . . H26 H 1.0761 0.6608 0.9572 0.034 Uiso 1 1 calc R . . C29 C 0.8293(2) 0.6646(2) 0.81506(19) 0.0220(5) Uani 1 1 d . . . H29 H 0.7663 0.6632 0.7806 0.026 Uiso 1 1 calc R . . N1 N 0.37065(19) -0.22448(17) 0.76390(15) 0.0204(4) Uani 1 1 d . . . N2 N 0.3731(2) -0.34956(17) 0.66912(15) 0.0218(4) Uani 1 1 d . . . N3 N 0.2941(2) 0.14849(18) 0.66256(16) 0.0253(4) Uani 1 1 d . . . N4 N 0.1915(2) 0.1405(2) 0.54744(19) 0.0379(6) Uani 1 1 d . . . O1 O 0.64719(19) 0.13608(19) 0.66989(18) 0.0418(5) Uani 1 1 d . . . O2 O 0.49043(16) 0.26681(15) 0.73600(14) 0.0279(4) Uani 1 1 d . . . O3 O 0.61922(18) 0.13999(15) 0.90654(13) 0.0294(4) Uani 1 1 d . . . O9 O 1.08034(19) 0.5449(2) 0.63449(16) 0.0450(6) Uani 1 1 d . . . O10 O 0.43707(16) 0.01376(14) 0.85443(13) 0.0190(3) Uani 1 1 d . . . H10 H 0.505(3) 0.019(3) 0.817(2) 0.029 Uiso 1 1 d . . . C27 C 0.7997(2) 0.7317(2) 0.89018(18) 0.0205(4) Uani 1 1 d . . . C28 C 0.8924(2) 0.7270(2) 0.94598(18) 0.0208(5) Uani 1 1 d . . . C30 C 0.8631(2) 0.7900(2) 1.03435(19) 0.0239(5) Uani 1 1 d . . . C31 C 0.6717(2) 0.8091(2) 0.90398(19) 0.0219(5) Uani 1 1 d . . . O5 O 0.65644(17) 0.88515(16) 0.95649(15) 0.0288(4) Uani 1 1 d . . . O7 O 0.77813(17) 0.74769(16) 1.11780(14) 0.0286(4) Uani 1 1 d . . . O6 O 0.59137(18) 0.79311(17) 0.85845(17) 0.0370(5) Uani 1 1 d . . . O8 O 0.9274(2) 0.87373(19) 1.02129(17) 0.0448(5) Uani 1 1 d . . . O4 O 0.6652(2) 0.26292(16) 0.98796(13) 0.0336(4) Uani 1 1 d . . . O1W O 0.18600(19) -0.06741(19) 0.90043(18) 0.0367(5) Uani 1 1 d . . . H1B H 0.158(4) -0.006(3) 0.919(3) 0.055 Uiso 1 1 d . . . H1A H 0.125(4) -0.106(3) 0.923(3) 0.055 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02006(18) 0.01739(18) 0.02287(19) -0.01047(14) -0.00991(14) -0.00117(14) Zn2 0.01875(14) 0.02202(14) 0.02336(14) -0.00915(10) -0.01041(10) -0.00300(10) Zn3 0.02675(15) 0.01929(14) 0.01900(14) -0.00923(10) -0.01070(10) -0.00531(10) C1 0.0344(15) 0.0511(17) 0.0337(15) -0.0182(13) -0.0071(12) -0.0134(13) C2 0.0537(19) 0.068(2) 0.0292(15) -0.0219(15) -0.0095(13) -0.0164(17) C3 0.0347(14) 0.0310(13) 0.0335(14) -0.0154(11) -0.0211(11) 0.0010(11) C4 0.0294(14) 0.0584(19) 0.0482(17) -0.0279(15) -0.0209(13) 0.0085(13) C5 0.0368(18) 0.077(3) 0.061(2) -0.0207(19) -0.0165(16) -0.0016(17) C6 0.062(2) 0.065(2) 0.057(2) -0.0243(18) -0.0410(18) -0.0019(18) C7 0.054(2) 0.064(2) 0.070(2) -0.0361(19) -0.0424(18) 0.0048(17) C8 0.0356(14) 0.0225(12) 0.0282(13) -0.0115(10) -0.0192(11) 0.0042(10) C9 0.0446(15) 0.0289(13) 0.0263(13) -0.0138(10) -0.0232(11) 0.0056(11) C10 0.0203(11) 0.0212(11) 0.0201(11) -0.0112(8) -0.0089(9) -0.0007(9) C11 0.0308(13) 0.0247(12) 0.0346(14) -0.0128(10) -0.0199(11) 0.0038(10) C12 0.0539(18) 0.0325(15) 0.0396(16) -0.0032(12) -0.0225(14) -0.0030(13) C13 0.0361(14) 0.0251(12) 0.0297(13) -0.0170(10) -0.0116(11) -0.0019(10) C14 0.0312(13) 0.0293(12) 0.0284(13) -0.0179(10) -0.0122(10) -0.0009(10) C15 0.0178(10) 0.0204(10) 0.0196(11) -0.0089(8) -0.0061(8) -0.0010(8) C16 0.0173(10) 0.0226(11) 0.0231(11) -0.0116(9) -0.0091(8) -0.0006(9) C17 0.0233(12) 0.0365(13) 0.0196(11) -0.0117(10) -0.0078(9) -0.0086(10) C18 0.0245(12) 0.0335(13) 0.0192(11) -0.0089(10) -0.0032(9) -0.0098(10) C19 0.0179(11) 0.0241(11) 0.0232(11) -0.0133(9) -0.0053(9) -0.0039(9) C20 0.0206(11) 0.0246(11) 0.0194(11) -0.0114(9) -0.0067(8) -0.0037(9) C21 0.0195(11) 0.0217(11) 0.0220(11) -0.0069(9) -0.0079(9) -0.0009(9) C22 0.0257(12) 0.0282(12) 0.0216(11) -0.0070(9) -0.0105(9) -0.0088(10) C23 0.0210(11) 0.0298(12) 0.0253(12) -0.0135(10) -0.0050(9) -0.0067(9) C24 0.0204(11) 0.0241(11) 0.0243(11) -0.0126(9) -0.0046(9) -0.0071(9) C25 0.0171(11) 0.0380(14) 0.0335(13) -0.0215(11) -0.0083(10) 0.0021(10) C26 0.0223(12) 0.0412(15) 0.0320(13) -0.0199(11) -0.0138(10) -0.0009(10) C29 0.0201(11) 0.0265(12) 0.0269(12) -0.0130(9) -0.0096(9) -0.0051(9) N1 0.0248(10) 0.0204(9) 0.0228(10) -0.0112(8) -0.0120(8) -0.0005(8) N2 0.0284(10) 0.0237(10) 0.0214(10) -0.0148(8) -0.0123(8) 0.0021(8) N3 0.0263(10) 0.0292(11) 0.0293(11) -0.0133(9) -0.0147(8) -0.0029(8) N4 0.0425(14) 0.0497(15) 0.0352(13) -0.0183(11) -0.0238(11) -0.0033(11) O1 0.0360(11) 0.0461(12) 0.0561(13) -0.0356(10) -0.0057(9) -0.0110(9) O2 0.0212(8) 0.0241(9) 0.0400(10) -0.0037(7) -0.0120(7) -0.0054(7) O3 0.0387(10) 0.0284(9) 0.0258(9) -0.0049(7) -0.0099(8) -0.0162(8) O9 0.0283(10) 0.0797(16) 0.0366(11) -0.0356(11) 0.0081(8) -0.0258(10) O10 0.0203(8) 0.0192(8) 0.0227(8) -0.0086(6) -0.0091(6) -0.0035(6) C27 0.0174(11) 0.0217(11) 0.0271(12) -0.0119(9) -0.0062(9) -0.0037(9) C28 0.0193(11) 0.0243(11) 0.0245(11) -0.0131(9) -0.0058(9) -0.0050(9) C30 0.0197(11) 0.0298(12) 0.0307(13) -0.0185(10) -0.0102(9) -0.0001(9) C31 0.0196(11) 0.0228(11) 0.0289(12) -0.0120(9) -0.0084(9) -0.0036(9) O5 0.0264(9) 0.0316(9) 0.0402(10) -0.0245(8) -0.0172(8) 0.0073(7) O7 0.0287(9) 0.0327(9) 0.0277(9) -0.0151(7) -0.0056(7) -0.0016(7) O6 0.0255(9) 0.0401(11) 0.0650(14) -0.0352(10) -0.0260(9) 0.0076(8) O8 0.0412(11) 0.0516(13) 0.0532(13) -0.0368(11) 0.0025(10) -0.0224(10) O4 0.0556(12) 0.0321(10) 0.0181(8) -0.0065(7) -0.0100(8) -0.0164(9) O1W 0.0238(10) 0.0337(11) 0.0599(14) -0.0251(10) -0.0090(9) -0.0030(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.0145(16) 2_667 ? Zn1 O5 2.0145(16) 1_545 ? Zn1 O3 2.1254(17) 2_657 ? Zn1 O3 2.1254(17) . ? Zn1 O10 2.2339(15) . ? Zn1 O10 2.2339(15) 2_657 ? Zn2 O7 1.9351(17) 2_667 ? Zn2 O2 1.9549(17) . ? Zn2 O10 1.9848(16) . ? Zn2 N3 2.0087(19) . ? Zn3 O4 1.9608(18) 2_657 ? Zn3 O10 1.9877(16) . ? Zn3 N1 2.0160(18) . ? Zn3 O6 2.1105(17) 1_545 ? Zn3 O1W 2.190(2) . ? C1 C2 1.344(4) . ? C1 N3 1.379(3) . ? C1 H1 0.9300 . ? C2 N4 1.373(4) . ? C2 H2 0.9300 . ? C3 N3 1.331(3) . ? C3 N4 1.351(3) . ? C3 C4 1.485(4) . ? C4 C5 1.529(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N4 1.474(3) . ? C6 C7 1.516(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C7 1.521(6) 2_556 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.354(3) . ? C8 N1 1.376(3) . ? C8 H8 0.9300 . ? C9 N2 1.367(3) . ? C9 H9 0.9300 . ? C10 N1 1.334(3) . ? C10 N2 1.352(3) . ? C10 C11 1.491(3) . ? C11 C12 1.520(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N2 1.477(3) . ? C13 C14 1.517(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C14 1.526(4) 2_646 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.392(3) . ? C15 C16 1.401(3) . ? C15 C21 1.504(3) . ? C16 C17 1.381(3) . ? C16 C22 1.512(3) . ? C17 C18 1.382(3) . ? C17 H17 0.9300 . ? C18 C19 1.389(3) . ? C18 H18 0.9300 . ? C19 C20 1.386(3) . ? C19 C23 1.495(3) . ? C20 H20 0.9300 . ? C21 O3 1.243(3) . ? C21 O4 1.259(3) . ? C22 O1 1.229(3) . ? C22 O2 1.266(3) . ? C23 O9 1.209(3) . ? C23 C24 1.489(3) . ? C24 C29 1.382(3) . ? C24 C25 1.388(3) . ? C25 C26 1.385(3) . ? C25 H25 0.9300 . ? C26 C28 1.389(3) . ? C26 H26 0.9300 . ? C29 C27 1.390(3) . ? C29 H29 0.9300 . ? O10 H10 0.75(3) . ? C27 C28 1.399(3) . ? C27 C31 1.501(3) . ? C28 C30 1.510(3) . ? C30 O8 1.231(3) . ? C30 O7 1.262(3) . ? C31 O5 1.251(3) . ? C31 O6 1.257(3) . ? O5 Zn1 2.0145(16) 1_565 ? O7 Zn2 1.9351(17) 2_667 ? O6 Zn3 2.1105(17) 1_565 ? O4 Zn3 1.9608(18) 2_657 ? O1W H1B 0.81(4) . ? O1W H1A 0.79(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O5 180.00(11) 2_667 1_545 ? O5 Zn1 O3 87.51(8) 2_667 2_657 ? O5 Zn1 O3 92.49(8) 1_545 2_657 ? O5 Zn1 O3 92.49(8) 2_667 . ? O5 Zn1 O3 87.51(8) 1_545 . ? O3 Zn1 O3 180.00(7) 2_657 . ? O5 Zn1 O10 88.48(6) 2_667 . ? O5 Zn1 O10 91.52(6) 1_545 . ? O3 Zn1 O10 94.42(6) 2_657 . ? O3 Zn1 O10 85.58(6) . . ? O5 Zn1 O10 91.52(6) 2_667 2_657 ? O5 Zn1 O10 88.48(6) 1_545 2_657 ? O3 Zn1 O10 85.58(6) 2_657 2_657 ? O3 Zn1 O10 94.42(6) . 2_657 ? O10 Zn1 O10 180.000(1) . 2_657 ? O7 Zn2 O2 99.38(8) 2_667 . ? O7 Zn2 O10 117.07(7) 2_667 . ? O2 Zn2 O10 100.15(7) . . ? O7 Zn2 N3 117.47(8) 2_667 . ? O2 Zn2 N3 107.63(8) . . ? O10 Zn2 N3 112.08(8) . . ? O4 Zn3 O10 125.30(7) 2_657 . ? O4 Zn3 N1 107.35(8) 2_657 . ? O10 Zn3 N1 127.12(7) . . ? O4 Zn3 O6 93.12(9) 2_657 1_545 ? O10 Zn3 O6 87.06(7) . 1_545 ? N1 Zn3 O6 95.38(7) . 1_545 ? O4 Zn3 O1W 88.49(9) 2_657 . ? O10 Zn3 O1W 84.85(7) . . ? N1 Zn3 O1W 92.52(8) . . ? O6 Zn3 O1W 171.07(7) 1_545 . ? C2 C1 N3 109.2(3) . . ? C2 C1 H1 125.4 . . ? N3 C1 H1 125.4 . . ? C1 C2 N4 106.6(3) . . ? C1 C2 H2 126.7 . . ? N4 C2 H2 126.7 . . ? N3 C3 N4 109.4(2) . . ? N3 C3 C4 125.9(2) . . ? N4 C3 C4 124.8(2) . . ? C3 C4 C5 116.6(3) . . ? C3 C4 H4A 108.1 . . ? C5 C4 H4A 108.1 . . ? C3 C4 H4B 108.1 . . ? C5 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 111.8(3) . . ? N4 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N4 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C7 111.4(4) . 2_556 ? C6 C7 H7A 109.4 . . ? C7 C7 H7A 109.4 2_556 . ? C6 C7 H7B 109.4 . . ? C7 C7 H7B 109.4 2_556 . ? H7A C7 H7B 108.0 . . ? C9 C8 N1 109.2(2) . . ? C9 C8 H8 125.4 . . ? N1 C8 H8 125.4 . . ? C8 C9 N2 106.5(2) . . ? C8 C9 H9 126.7 . . ? N2 C9 H9 126.7 . . ? N1 C10 N2 109.58(19) . . ? N1 C10 C11 125.74(19) . . ? N2 C10 C11 124.64(19) . . ? C10 C11 C12 113.9(2) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 112.5(2) . . ? N2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C14 111.1(3) . 2_646 ? C13 C14 H14A 109.4 . . ? C14 C14 H14A 109.4 2_646 . ? C13 C14 H14B 109.4 . . ? C14 C14 H14B 109.4 2_646 . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 118.9(2) . . ? C20 C15 C21 118.77(19) . . ? C16 C15 C21 122.2(2) . . ? C17 C16 C15 119.6(2) . . ? C17 C16 C22 118.35(19) . . ? C15 C16 C22 121.8(2) . . ? C16 C17 C18 121.2(2) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C19 119.6(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.6(2) . . ? C20 C19 C23 120.1(2) . . ? C18 C19 C23 120.0(2) . . ? C19 C20 C15 121.0(2) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? O3 C21 O4 126.0(2) . . ? O3 C21 C15 118.3(2) . . ? O4 C21 C15 115.7(2) . . ? O1 C22 O2 126.7(2) . . ? O1 C22 C16 120.4(2) . . ? O2 C22 C16 112.9(2) . . ? O9 C23 C24 121.7(2) . . ? O9 C23 C19 120.7(2) . . ? C24 C23 C19 117.52(19) . . ? C29 C24 C25 119.7(2) . . ? C29 C24 C23 118.5(2) . . ? C25 C24 C23 121.7(2) . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C28 120.9(2) . . ? C25 C26 H26 119.5 . . ? C28 C26 H26 119.5 . . ? C24 C29 C27 121.5(2) . . ? C24 C29 H29 119.3 . . ? C27 C29 H29 119.3 . . ? C10 N1 C8 106.55(18) . . ? C10 N1 Zn3 128.90(15) . . ? C8 N1 Zn3 124.49(15) . . ? C10 N2 C9 108.12(18) . . ? C10 N2 C13 127.0(2) . . ? C9 N2 C13 124.90(19) . . ? C3 N3 C1 106.8(2) . . ? C3 N3 Zn2 131.28(18) . . ? C1 N3 Zn2 121.90(17) . . ? C3 N4 C2 108.1(2) . . ? C3 N4 C6 125.7(3) . . ? C2 N4 C6 126.1(3) . . ? C22 O2 Zn2 121.31(15) . . ? C21 O3 Zn1 144.65(16) . . ? Zn2 O10 Zn3 125.90(8) . . ? Zn2 O10 Zn1 120.68(7) . . ? Zn3 O10 Zn1 102.44(7) . . ? Zn2 O10 H10 99(2) . . ? Zn3 O10 H10 108(2) . . ? Zn1 O10 H10 96(2) . . ? C29 C27 C28 118.5(2) . . ? C29 C27 C31 117.9(2) . . ? C28 C27 C31 123.5(2) . . ? C26 C28 C27 119.8(2) . . ? C26 C28 C30 118.7(2) . . ? C27 C28 C30 121.6(2) . . ? O8 C30 O7 125.6(2) . . ? O8 C30 C28 118.0(2) . . ? O7 C30 C28 116.3(2) . . ? O5 C31 O6 126.3(2) . . ? O5 C31 C27 117.50(19) . . ? O6 C31 C27 116.2(2) . . ? C31 O5 Zn1 130.67(15) . 1_565 ? C30 O7 Zn2 126.68(16) . 2_667 ? C31 O6 Zn3 131.48(16) . 1_565 ? C21 O4 Zn3 117.24(16) . 2_657 ? Zn3 O1W H1B 127(3) . . ? Zn3 O1W H1A 121(3) . . ? H1B O1W H1A 104(4) . . ? 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 C1 C2 N4 -0.5(4) . . . . ? N3 C3 C4 C5 -115.0(3) . . . . ? N4 C3 C4 C5 65.9(4) . . . . ? N4 C6 C7 C7 166.8(4) . . . 2_556 ? N1 C8 C9 N2 0.8(3) . . . . ? N1 C10 C11 C12 95.4(3) . . . . ? N2 C10 C11 C12 -82.1(3) . . . . ? N2 C13 C14 C14 -173.1(2) . . . 2_646 ? C20 C15 C16 C17 0.2(3) . . . . ? C21 C15 C16 C17 -177.0(2) . . . . ? C20 C15 C16 C22 -174.3(2) . . . . ? C21 C15 C16 C22 8.5(3) . . . . ? C15 C16 C17 C18 0.8(4) . . . . ? C22 C16 C17 C18 175.5(2) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C20 -1.0(4) . . . . ? C17 C18 C19 C23 172.7(2) . . . . ? C18 C19 C20 C15 2.0(3) . . . . ? C23 C19 C20 C15 -171.7(2) . . . . ? C16 C15 C20 C19 -1.6(3) . . . . ? C21 C15 C20 C19 175.7(2) . . . . ? C20 C15 C21 O3 -161.3(2) . . . . ? C16 C15 C21 O3 15.9(3) . . . . ? C20 C15 C21 O4 17.0(3) . . . . ? C16 C15 C21 O4 -165.8(2) . . . . ? C17 C16 C22 O1 74.2(3) . . . . ? C15 C16 C22 O1 -111.2(3) . . . . ? C17 C16 C22 O2 -102.8(3) . . . . ? C15 C16 C22 O2 71.8(3) . . . . ? C20 C19 C23 O9 139.2(3) . . . . ? C18 C19 C23 O9 -34.5(4) . . . . ? C20 C19 C23 C24 -41.0(3) . . . . ? C18 C19 C23 C24 145.3(2) . . . . ? O9 C23 C24 C29 131.6(3) . . . . ? C19 C23 C24 C29 -48.2(3) . . . . ? O9 C23 C24 C25 -45.2(4) . . . . ? C19 C23 C24 C25 134.9(3) . . . . ? C29 C24 C25 C26 1.9(4) . . . . ? C23 C24 C25 C26 178.8(2) . . . . ? C24 C25 C26 C28 -1.8(4) . . . . ? C25 C24 C29 C27 0.9(4) . . . . ? C23 C24 C29 C27 -176.0(2) . . . . ? N2 C10 N1 C8 0.1(3) . . . . ? C11 C10 N1 C8 -177.7(2) . . . . ? N2 C10 N1 Zn3 177.23(15) . . . . ? C11 C10 N1 Zn3 -0.5(3) . . . . ? C9 C8 N1 C10 -0.5(3) . . . . ? C9 C8 N1 Zn3 -177.84(18) . . . . ? O4 Zn3 N1 C10 -47.0(2) 2_657 . . . ? O10 Zn3 N1 C10 138.37(19) . . . . ? O6 Zn3 N1 C10 48.0(2) 1_545 . . . ? O1W Zn3 N1 C10 -136.2(2) . . . . ? O4 Zn3 N1 C8 129.7(2) 2_657 . . . ? O10 Zn3 N1 C8 -44.9(2) . . . . ? O6 Zn3 N1 C8 -135.3(2) 1_545 . . . ? O1W Zn3 N1 C8 40.5(2) . . . . ? N1 C10 N2 C9 0.4(3) . . . . ? C11 C10 N2 C9 178.2(2) . . . . ? N1 C10 N2 C13 -179.1(2) . . . . ? C11 C10 N2 C13 -1.3(4) . . . . ? C8 C9 N2 C10 -0.7(3) . . . . ? C8 C9 N2 C13 178.8(2) . . . . ? C14 C13 N2 C10 -110.0(3) . . . . ? C14 C13 N2 C9 70.6(3) . . . . ? N4 C3 N3 C1 0.0(3) . . . . ? C4 C3 N3 C1 -179.2(3) . . . . ? N4 C3 N3 Zn2 178.16(18) . . . . ? C4 C3 N3 Zn2 -1.0(4) . . . . ? C2 C1 N3 C3 0.3(3) . . . . ? C2 C1 N3 Zn2 -178.1(2) . . . . ? O7 Zn2 N3 C3 -26.4(3) 2_667 . . . ? O2 Zn2 N3 C3 -137.4(2) . . . . ? O10 Zn2 N3 C3 113.4(2) . . . . ? O7 Zn2 N3 C1 151.5(2) 2_667 . . . ? O2 Zn2 N3 C1 40.5(2) . . . . ? O10 Zn2 N3 C1 -68.6(2) . . . . ? N3 C3 N4 C2 -0.3(3) . . . . ? C4 C3 N4 C2 178.9(3) . . . . ? N3 C3 N4 C6 176.3(3) . . . . ? C4 C3 N4 C6 -4.5(5) . . . . ? C1 C2 N4 C3 0.5(4) . . . . ? C1 C2 N4 C6 -176.1(3) . . . . ? C7 C6 N4 C3 -94.9(4) . . . . ? C7 C6 N4 C2 81.0(4) . . . . ? O1 C22 O2 Zn2 25.4(3) . . . . ? C16 C22 O2 Zn2 -157.89(15) . . . . ? O7 Zn2 O2 C22 152.81(18) 2_667 . . . ? O10 Zn2 O2 C22 32.93(19) . . . . ? N3 Zn2 O2 C22 -84.30(19) . . . . ? O4 C21 O3 Zn1 14.7(4) . . . . ? C15 C21 O3 Zn1 -167.22(19) . . . . ? O5 Zn1 O3 C21 55.9(3) 2_667 . . . ? O5 Zn1 O3 C21 -124.1(3) 1_545 . . . ? O7 Zn2 O10 Zn3 100.14(11) 2_667 . . . ? O2 Zn2 O10 Zn3 -153.75(10) . . . . ? N3 Zn2 O10 Zn3 -39.89(13) . . . . ? O7 Zn2 O10 Zn1 -37.48(12) 2_667 . . . ? O2 Zn2 O10 Zn1 68.63(10) . . . . ? N3 Zn2 O10 Zn1 -177.50(9) . . . . ? O4 Zn3 O10 Zn2 -119.11(11) 2_657 . . . ? N1 Zn3 O10 Zn2 54.63(14) . . . . ? O6 Zn3 O10 Zn2 149.15(11) 1_545 . . . ? O1W Zn3 O10 Zn2 -34.63(11) . . . . ? O4 Zn3 O10 Zn1 24.47(12) 2_657 . . . ? N1 Zn3 O10 Zn1 -161.79(7) . . . . ? O6 Zn3 O10 Zn1 -67.27(8) 1_545 . . . ? O1W Zn3 O10 Zn1 108.94(8) . . . . ? O5 Zn1 O10 Zn2 31.68(10) 2_667 . . . ? O5 Zn1 O10 Zn2 -148.32(10) 1_545 . . . ? O3 Zn1 O10 Zn2 119.07(10) 2_657 . . . ? O3 Zn1 O10 Zn2 -60.93(10) . . . . ? O5 Zn1 O10 Zn3 -114.32(8) 2_667 . . . ? O5 Zn1 O10 Zn3 65.68(8) 1_545 . . . ? O3 Zn1 O10 Zn3 -26.93(8) 2_657 . . . ? O3 Zn1 O10 Zn3 153.07(8) . . . . ? C24 C29 C27 C28 -3.9(3) . . . . ? C24 C29 C27 C31 173.7(2) . . . . ? C25 C26 C28 C27 -1.3(4) . . . . ? C25 C26 C28 C30 178.2(2) . . . . ? C29 C27 C28 C26 4.1(3) . . . . ? C31 C27 C28 C26 -173.4(2) . . . . ? C29 C27 C28 C30 -175.4(2) . . . . ? C31 C27 C28 C30 7.1(4) . . . . ? C26 C28 C30 O8 66.8(3) . . . . ? C27 C28 C30 O8 -113.8(3) . . . . ? C26 C28 C30 O7 -109.9(3) . . . . ? C27 C28 C30 O7 69.5(3) . . . . ? C29 C27 C31 O5 -167.0(2) . . . . ? C28 C27 C31 O5 10.6(3) . . . . ? C29 C27 C31 O6 11.0(3) . . . . ? C28 C27 C31 O6 -171.5(2) . . . . ? O6 C31 O5 Zn1 5.7(4) . . . 1_565 ? C27 C31 O5 Zn1 -176.62(16) . . . 1_565 ? O8 C30 O7 Zn2 37.3(4) . . . 2_667 ? C28 C30 O7 Zn2 -146.23(17) . . . 2_667 ? O5 C31 O6 Zn3 -16.1(4) . . . 1_565 ? C27 C31 O6 Zn3 166.20(17) . . . 1_565 ? O3 C21 O4 Zn3 7.4(3) . . . 2_657 ? C15 C21 O4 Zn3 -170.73(15) . . . 2_657 ? 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 H1A O8 0.79(4) 2.15(4) 2.847(3) 148(4) 1_445 O1W H1B O8 0.81(4) 1.92(4) 2.722(3) 172(4) 2_667 O10 H10 O1 0.75(3) 2.37(3) 3.027(3) 147(3) . _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.601 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.084 #===end data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H36 N6 O14 Zn2' _chemical_formula_weight 967.50 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_H-M P-1 _symmetry_space_group_name_Hall '-P1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2800(13) _cell_length_b 13.6270(18) _cell_length_c 14.6140(19) _cell_angle_alpha 93.972(2) _cell_angle_beta 100.465(2) _cell_angle_gamma 95.312(2) _cell_volume 1996.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10236 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.631 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11884 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 28.43 _reflns_number_total 8729 _reflns_number_gt 4767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0934P)^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 8729 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _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 0.30781(5) 0.19328(3) 0.00090(3) 0.04298(16) Uani 1 1 d . . . Zn2 Zn 0.55972(6) 0.55494(3) 0.22969(4) 0.05339(18) Uani 1 1 d . . . C1 C 0.7686(5) 0.5549(3) 0.4183(4) 0.0646(14) Uani 1 1 d . . . H1 H 0.8161 0.6050 0.3942 0.078 Uiso 1 1 calc R . . C2 C 0.8202(5) 0.5285(4) 0.5047(4) 0.0680(14) Uani 1 1 d . . . H2 H 0.9019 0.5582 0.5377 0.082 Uiso 1 1 calc R . . C3 C 0.7482(5) 0.4572(4) 0.5412(4) 0.0647(13) Uani 1 1 d . . . H3 H 0.7794 0.4389 0.6006 0.078 Uiso 1 1 calc R . . C4 C 0.6304(5) 0.4129(3) 0.4905(3) 0.0532(11) Uani 1 1 d . . . H4 H 0.5813 0.3638 0.5149 0.064 Uiso 1 1 calc R . . C5 C 0.5843(4) 0.4415(3) 0.4024(3) 0.0426(10) Uani 1 1 d . . . C6 C 0.4599(4) 0.4059(3) 0.3392(3) 0.0415(9) Uani 1 1 d . . . C7 C 0.2994(5) 0.4045(3) 0.2200(3) 0.0612(13) Uani 1 1 d . . . H7 H 0.2485 0.4215 0.1652 0.073 Uiso 1 1 calc R . . C8 C 0.2648(5) 0.3303(3) 0.2704(3) 0.0566(12) Uani 1 1 d . . . H8 H 0.1870 0.2871 0.2565 0.068 Uiso 1 1 calc R . . C9 C 0.3752(5) 0.2590(3) 0.4170(3) 0.0506(11) Uani 1 1 d . . . H9A H 0.3735 0.2934 0.4771 0.061 Uiso 1 1 calc R . . H9B H 0.4596 0.2316 0.4215 0.061 Uiso 1 1 calc R . . C10 C 0.0267(5) 0.2386(4) 0.0206(3) 0.0607(13) Uani 1 1 d . . . H10 H 0.0461 0.2937 -0.0107 0.073 Uiso 1 1 calc R . . C11 C -0.0985(5) 0.2224(4) 0.0423(4) 0.0672(14) Uani 1 1 d . . . H11 H -0.1620 0.2658 0.0267 0.081 Uiso 1 1 calc R . . C12 C -0.1265(5) 0.1397(4) 0.0881(3) 0.0602(12) Uani 1 1 d . . . H12 H -0.2100 0.1266 0.1033 0.072 Uiso 1 1 calc R . . C13 C -0.0315(4) 0.0775(3) 0.1109(3) 0.0496(11) Uani 1 1 d . . . H13 H -0.0496 0.0216 0.1414 0.059 Uiso 1 1 calc R . . C14 C 0.0938(4) 0.0989(3) 0.0878(3) 0.0388(9) Uani 1 1 d . . . C15 C 0.2019(4) 0.0382(3) 0.1036(3) 0.0425(9) Uani 1 1 d . . . C16 C 0.3871(5) -0.0162(4) 0.0872(4) 0.0599(12) Uani 1 1 d . . . H16 H 0.4662 -0.0239 0.0666 0.072 Uiso 1 1 calc R . . C17 C 0.3414(5) -0.0686(4) 0.1510(4) 0.0601(12) Uani 1 1 d . . . H17 H 0.3820 -0.1183 0.1821 0.072 Uiso 1 1 calc R . . C18 C 0.1552(5) -0.0620(3) 0.2369(3) 0.0526(11) Uani 1 1 d . . . H18A H 0.1948 -0.1169 0.2658 0.063 Uiso 1 1 calc R . . H18B H 0.0627 -0.0841 0.2108 0.063 Uiso 1 1 calc R . . C19 C 0.1618(4) 0.0214(3) 0.3102(3) 0.0452(10) Uani 1 1 d . . . C20 C 0.0640(4) 0.0212(4) 0.3676(3) 0.0542(12) Uani 1 1 d . . . H20 H -0.0037 -0.0307 0.3584 0.065 Uiso 1 1 calc R . . C21 C 0.0670(5) 0.0937(4) 0.4345(3) 0.0580(12) Uani 1 1 d . . . H21 H 0.0025 0.0911 0.4717 0.070 Uiso 1 1 calc R . . C22 C 0.1651(5) 0.1726(3) 0.4490(3) 0.0538(11) Uani 1 1 d . . . H22 H 0.1650 0.2238 0.4945 0.065 Uiso 1 1 calc R . . C23 C 0.2635(4) 0.1753(3) 0.3957(3) 0.0444(10) Uani 1 1 d . . . C24 C 0.2605(4) 0.0998(3) 0.3269(3) 0.0462(10) Uani 1 1 d . . . H24 H 0.3266 0.1018 0.2910 0.055 Uiso 1 1 calc R . . C25 C 0.7137(5) 0.8628(3) 0.1805(3) 0.0414(9) Uani 1 1 d . . . C26 C 0.5610(5) 0.7444(3) 0.3035(3) 0.0470(10) Uani 1 1 d . . . C27 C 0.6797(4) 0.9063(3) 0.2697(2) 0.0325(8) Uani 1 1 d . . . C28 C 0.6051(4) 0.8539(3) 0.3244(3) 0.0362(9) Uani 1 1 d . . . C29 C 0.5757(5) 0.9024(3) 0.4037(3) 0.0468(10) Uani 1 1 d . . . H29 H 0.5251 0.8675 0.4398 0.056 Uiso 1 1 calc R . . C30 C 0.6185(5) 0.9994(3) 0.4301(3) 0.0489(11) Uani 1 1 d . . . H30 H 0.5990 1.0298 0.4842 0.059 Uiso 1 1 calc R . . C31 C 0.6929(4) 1.0535(3) 0.3747(3) 0.0388(9) Uani 1 1 d . . . C32 C 0.7207(4) 1.0055(3) 0.2950(3) 0.0372(9) Uani 1 1 d . . . H32 H 0.7683 1.0409 0.2575 0.045 Uiso 1 1 calc R . . C33 C 0.7421(4) 1.1580(3) 0.4071(3) 0.0443(10) Uani 1 1 d . . . C34 C 0.7560(4) 1.2299(3) 0.3355(3) 0.0402(9) Uani 1 1 d . . . C35 C 0.8606(5) 1.3040(3) 0.3519(3) 0.0554(11) Uani 1 1 d . . . H35 H 0.9260 1.3060 0.4052 0.066 Uiso 1 1 calc R . . C36 C 0.8689(5) 1.3743(3) 0.2905(3) 0.0534(11) Uani 1 1 d . . . H36 H 0.9425 1.4216 0.3006 0.064 Uiso 1 1 calc R . . C37 C 0.7687(4) 1.3760(3) 0.2133(3) 0.0426(10) Uani 1 1 d . . . C38 C 0.6636(4) 1.3015(3) 0.1952(3) 0.0396(9) Uani 1 1 d . . . C39 C 0.6595(4) 1.2278(3) 0.2562(3) 0.0398(9) Uani 1 1 d . . . H39 H 0.5908 1.1764 0.2433 0.048 Uiso 1 1 calc R . . C40 C 0.5545(5) 1.2967(3) 0.1102(3) 0.0500(11) Uani 1 1 d . . . C41 C 0.7799(5) 1.4627(3) 0.1544(3) 0.0541(12) Uani 1 1 d . . . N1 N 0.3018(3) 0.0496(3) 0.0571(2) 0.0466(8) Uani 1 1 d . . . N2 N 0.1204(4) 0.1788(3) 0.0425(2) 0.0449(8) Uani 1 1 d . . . N3 N 0.2233(4) -0.0349(2) 0.1616(2) 0.0457(8) Uani 1 1 d . . . N4 N 0.6549(4) 0.5134(2) 0.3665(3) 0.0510(9) Uani 1 1 d . . . N5 N 0.4214(4) 0.4508(2) 0.2624(2) 0.0503(9) Uani 1 1 d . . . N6 N 0.3659(3) 0.3305(2) 0.3458(2) 0.0419(8) Uani 1 1 d . . . O1 O 0.7687(4) 1.1854(2) 0.4890(2) 0.0729(10) Uani 1 1 d . . . O2 O 0.8305(4) 0.8551(3) 0.1763(3) 0.0849(13) Uani 1 1 d . . . O1W O 0.2888(4) 0.3453(2) -0.0214(2) 0.0640(9) Uani 1 1 d . . . O3 O 0.6201(4) 0.8433(2) 0.1124(2) 0.0605(8) Uani 1 1 d . . . O2W O 0.4151(5) 0.5783(4) 0.1113(3) 0.1044(15) Uani 1 1 d . . . O4 O 0.4566(3) 1.2351(3) 0.1071(2) 0.0653(9) Uani 1 1 d . . . O3W O 0.1198(9) 0.5522(7) 0.0804(6) 0.206(4) Uani 1 1 d . . . O5 O 0.5662(6) 1.3526(4) 0.0516(3) 0.144(3) Uani 1 1 d . . . O4W O 0.0308(9) 0.2661(7) 0.6392(8) 0.241(5) Uani 1 1 d . . . O6 O 0.6270(4) 0.6961(2) 0.2573(2) 0.0656(9) Uani 1 1 d . . . O5W O 0.1985(10) 0.6895(10) 0.2528(13) 0.335(8) Uani 1 1 d . . . O7 O 0.4684(4) 0.7070(2) 0.3378(3) 0.0794(11) Uani 1 1 d . . . O8 O 0.7078(4) 1.5293(2) 0.1618(2) 0.0675(10) Uani 1 1 d . . . O9 O 0.8683(5) 1.4659(3) 0.1084(3) 0.0971(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0498(3) 0.0450(3) 0.0377(3) 0.0074(2) 0.0158(2) 0.0066(2) Zn2 0.0828(4) 0.0291(3) 0.0546(3) 0.0135(2) 0.0285(3) 0.0010(2) C1 0.072(4) 0.044(3) 0.075(4) -0.003(2) 0.021(3) -0.018(2) C2 0.064(3) 0.058(3) 0.074(4) -0.008(3) 0.006(3) -0.016(3) C3 0.070(3) 0.055(3) 0.060(3) -0.002(2) 0.001(3) -0.010(2) C4 0.068(3) 0.041(2) 0.051(3) 0.005(2) 0.017(2) -0.005(2) C5 0.060(3) 0.0240(18) 0.046(2) 0.0036(16) 0.020(2) -0.0047(17) C6 0.059(3) 0.0291(19) 0.039(2) 0.0090(16) 0.0147(19) 0.0010(18) C7 0.083(4) 0.054(3) 0.043(2) 0.014(2) 0.004(2) -0.006(3) C8 0.062(3) 0.050(3) 0.052(3) 0.014(2) -0.001(2) -0.005(2) C9 0.059(3) 0.044(2) 0.048(2) 0.0171(19) 0.008(2) -0.007(2) C10 0.067(3) 0.055(3) 0.071(3) 0.019(2) 0.027(3) 0.023(2) C11 0.062(3) 0.066(3) 0.082(4) 0.012(3) 0.026(3) 0.027(3) C12 0.053(3) 0.072(3) 0.060(3) 0.001(2) 0.020(2) 0.012(2) C13 0.052(3) 0.054(3) 0.047(2) 0.005(2) 0.021(2) 0.004(2) C14 0.045(2) 0.038(2) 0.0328(19) 0.0013(16) 0.0075(17) 0.0014(17) C15 0.046(2) 0.038(2) 0.043(2) 0.0053(17) 0.0092(19) -0.0024(18) C16 0.051(3) 0.061(3) 0.077(3) 0.015(3) 0.026(3) 0.019(2) C17 0.052(3) 0.055(3) 0.077(3) 0.023(2) 0.011(3) 0.018(2) C18 0.059(3) 0.043(2) 0.055(3) 0.014(2) 0.011(2) -0.005(2) C19 0.046(2) 0.040(2) 0.050(2) 0.0169(19) 0.0095(19) -0.0040(18) C20 0.046(3) 0.054(3) 0.063(3) 0.017(2) 0.013(2) -0.009(2) C21 0.054(3) 0.062(3) 0.064(3) 0.017(3) 0.025(2) -0.001(2) C22 0.060(3) 0.049(3) 0.053(3) 0.013(2) 0.013(2) 0.000(2) C23 0.050(3) 0.040(2) 0.044(2) 0.0162(19) 0.0122(19) -0.0067(18) C24 0.047(2) 0.046(2) 0.047(2) 0.0153(19) 0.0132(19) -0.0067(19) C25 0.053(3) 0.0264(19) 0.049(3) 0.0044(17) 0.023(2) -0.0001(17) C26 0.061(3) 0.033(2) 0.051(2) 0.0124(18) 0.021(2) 0.0010(19) C27 0.040(2) 0.0272(18) 0.0340(19) 0.0065(15) 0.0126(16) 0.0064(15) C28 0.047(2) 0.0268(18) 0.038(2) 0.0098(15) 0.0137(18) 0.0057(16) C29 0.065(3) 0.037(2) 0.048(2) 0.0167(18) 0.030(2) 0.0078(19) C30 0.070(3) 0.043(2) 0.043(2) 0.0091(18) 0.030(2) 0.010(2) C31 0.052(2) 0.0282(19) 0.040(2) 0.0081(16) 0.0135(18) 0.0075(17) C32 0.045(2) 0.032(2) 0.038(2) 0.0079(16) 0.0165(17) -0.0029(16) C33 0.051(3) 0.034(2) 0.048(2) 0.0041(18) 0.008(2) 0.0048(18) C34 0.049(2) 0.029(2) 0.042(2) -0.0004(16) 0.0103(19) 0.0023(17) C35 0.062(3) 0.037(2) 0.059(3) 0.003(2) -0.007(2) 0.000(2) C36 0.054(3) 0.034(2) 0.070(3) 0.009(2) 0.011(2) -0.0054(19) C37 0.056(3) 0.0253(19) 0.049(2) 0.0012(17) 0.020(2) 0.0006(17) C38 0.052(2) 0.0300(19) 0.038(2) 0.0008(16) 0.0126(18) 0.0024(17) C39 0.050(2) 0.0241(18) 0.046(2) 0.0026(16) 0.013(2) -0.0020(16) C40 0.071(3) 0.036(2) 0.041(2) 0.0040(18) 0.012(2) -0.004(2) C41 0.074(3) 0.038(2) 0.053(3) 0.006(2) 0.023(2) -0.004(2) N1 0.046(2) 0.048(2) 0.049(2) 0.0088(16) 0.0139(17) 0.0077(16) N2 0.053(2) 0.044(2) 0.0412(18) 0.0062(15) 0.0165(16) 0.0078(16) N3 0.052(2) 0.0383(19) 0.047(2) 0.0092(15) 0.0107(17) 0.0002(16) N4 0.064(2) 0.0311(18) 0.061(2) 0.0041(16) 0.024(2) -0.0052(17) N5 0.074(3) 0.0344(18) 0.044(2) 0.0096(15) 0.0157(19) -0.0010(17) N6 0.054(2) 0.0339(17) 0.0377(18) 0.0089(14) 0.0096(16) -0.0043(15) O1 0.126(3) 0.0468(19) 0.0395(18) -0.0050(15) 0.0079(19) 0.0001(19) O2 0.059(2) 0.091(3) 0.104(3) -0.039(2) 0.045(2) -0.0179(19) O1W 0.088(2) 0.0500(18) 0.064(2) 0.0191(15) 0.0310(18) 0.0117(17) O3 0.079(2) 0.065(2) 0.0414(17) -0.0002(15) 0.0136(17) 0.0226(17) O2W 0.108(3) 0.135(4) 0.085(3) 0.074(3) 0.029(2) 0.018(3) O4 0.065(2) 0.069(2) 0.0543(19) 0.0201(16) -0.0040(16) -0.0157(17) O3W 0.191(7) 0.273(10) 0.179(7) 0.104(7) 0.056(6) 0.057(7) O5 0.146(4) 0.170(5) 0.083(3) 0.087(3) -0.041(3) -0.088(4) O4W 0.194(8) 0.221(8) 0.309(11) -0.072(8) 0.148(8) -0.099(7) O6 0.092(3) 0.0301(15) 0.088(2) 0.0095(15) 0.050(2) 0.0074(16) O5W 0.151(8) 0.256(12) 0.57(2) 0.112(14) -0.041(11) 0.034(8) O7 0.098(3) 0.0483(19) 0.100(3) 0.0026(19) 0.057(2) -0.0189(19) O8 0.109(3) 0.0451(18) 0.065(2) 0.0257(15) 0.042(2) 0.0295(19) O9 0.109(3) 0.086(3) 0.123(3) 0.043(3) 0.073(3) 0.018(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 O4 1.981(3) 1_545 ? Zn1 O3 1.985(3) 2_665 ? Zn1 N2 2.119(3) . ? Zn1 O1W 2.141(3) . ? Zn1 N1 2.175(3) . ? Zn2 O6 1.971(3) . ? Zn2 O8 2.005(3) 1_545 ? Zn2 N5 2.057(3) . ? Zn2 O2W 2.129(4) . ? Zn2 N4 2.197(4) . ? C1 N4 1.325(6) . ? C1 C2 1.364(7) . ? C1 H1 0.9300 . ? C2 C3 1.363(6) . ? C2 H2 0.9300 . ? C3 C4 1.362(7) . ? C3 H3 0.9300 . ? C4 C5 1.383(6) . ? C4 H4 0.9300 . ? C5 N4 1.356(5) . ? C5 C6 1.455(6) . ? C6 N5 1.330(5) . ? C6 N6 1.365(5) . ? C7 C8 1.351(6) . ? C7 N5 1.368(6) . ? C7 H7 0.9300 . ? C8 N6 1.370(6) . ? C8 H8 0.9300 . ? C9 N6 1.471(5) . ? C9 C23 1.515(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.328(6) . ? C10 C11 1.382(7) . ? C10 H10 0.9300 . ? C11 C12 1.383(7) . ? C11 H11 0.9300 . ? C12 C13 1.363(7) . ? C12 H12 0.9300 . ? C13 C14 1.400(6) . ? C13 H13 0.9300 . ? C14 N2 1.346(5) . ? C14 C15 1.440(6) . ? C15 N1 1.334(5) . ? C15 N3 1.360(5) . ? C16 C17 1.337(6) . ? C16 N1 1.351(6) . ? C16 H16 0.9300 . ? C17 N3 1.368(6) . ? C17 H17 0.9300 . ? C18 N3 1.458(5) . ? C18 C19 1.494(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.379(5) . ? C19 C20 1.422(6) . ? C20 C21 1.336(6) . ? C20 H20 0.9300 . ? C21 C22 1.381(6) . ? C21 H21 0.9300 . ? C22 C23 1.384(6) . ? C22 H22 0.9300 . ? C23 C24 1.383(6) . ? C24 H24 0.9300 . ? C25 O2 1.227(5) . ? C25 O3 1.247(5) . ? C25 C27 1.506(5) . ? C26 O6 1.239(5) . ? C26 O7 1.240(5) . ? C26 C28 1.512(5) . ? C27 C32 1.382(5) . ? C27 C28 1.392(5) . ? C28 C29 1.389(5) . ? C29 C30 1.360(6) . ? C29 H29 0.9300 . ? C30 C31 1.409(5) . ? C30 H30 0.9300 . ? C31 C32 1.384(5) . ? C31 C33 1.480(5) . ? C32 H32 0.9300 . ? C33 O1 1.204(5) . ? C33 C34 1.498(5) . ? C34 C39 1.379(6) . ? C34 C35 1.380(6) . ? C35 C36 1.365(6) . ? C35 H35 0.9300 . ? C36 C37 1.386(6) . ? C36 H36 0.9300 . ? C37 C38 1.387(5) . ? C37 C41 1.517(6) . ? C38 C39 1.392(5) . ? C38 C40 1.508(6) . ? C39 H39 0.9300 . ? C40 O5 1.199(5) . ? C40 O4 1.242(5) . ? C41 O9 1.224(6) . ? C41 O8 1.235(6) . ? O3 Zn1 1.985(3) 2_665 ? O4 Zn1 1.981(3) 1_565 ? O8 Zn2 2.005(3) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O3 109.59(15) 1_545 2_665 ? O4 Zn1 N2 112.61(14) 1_545 . ? O3 Zn1 N2 136.96(14) 2_665 . ? O4 Zn1 O1W 89.62(14) 1_545 . ? O3 Zn1 O1W 97.81(12) 2_665 . ? N2 Zn1 O1W 90.62(13) . . ? O4 Zn1 N1 85.85(14) 1_545 . ? O3 Zn1 N1 98.30(13) 2_665 . ? N2 Zn1 N1 76.93(13) . . ? O1W Zn1 N1 163.87(12) . . ? O6 Zn2 O8 91.66(14) . 1_545 ? O6 Zn2 N5 141.08(14) . . ? O8 Zn2 N5 126.66(14) 1_545 . ? O6 Zn2 O2W 94.39(18) . . ? O8 Zn2 O2W 97.55(16) 1_545 . ? N5 Zn2 O2W 87.61(15) . . ? O6 Zn2 N4 94.20(14) . . ? O8 Zn2 N4 97.19(14) 1_545 . ? N5 Zn2 N4 76.31(14) . . ? O2W Zn2 N4 162.69(14) . . ? N4 C1 C2 124.1(4) . . ? N4 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 117.9(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N4 C5 C4 120.6(4) . . ? N4 C5 C6 111.5(3) . . ? C4 C5 C6 127.8(3) . . ? N5 C6 N6 109.6(4) . . ? N5 C6 C5 120.3(3) . . ? N6 C6 C5 130.1(3) . . ? C8 C7 N5 109.1(4) . . ? C8 C7 H7 125.4 . . ? N5 C7 H7 125.4 . . ? C7 C8 N6 107.1(4) . . ? C7 C8 H8 126.4 . . ? N6 C8 H8 126.4 . . ? N6 C9 C23 112.9(4) . . ? N6 C9 H9A 109.0 . . ? C23 C9 H9A 109.0 . . ? N6 C9 H9B 109.0 . . ? C23 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C11 122.7(4) . . ? N2 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 118.1(5) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? N2 C14 C13 120.8(4) . . ? N2 C14 C15 113.5(3) . . ? C13 C14 C15 125.5(4) . . ? N1 C15 N3 109.3(4) . . ? N1 C15 C14 120.3(3) . . ? N3 C15 C14 130.3(4) . . ? C17 C16 N1 110.3(4) . . ? C17 C16 H16 124.8 . . ? N1 C16 H16 124.8 . . ? C16 C17 N3 106.6(4) . . ? C16 C17 H17 126.7 . . ? N3 C17 H17 126.7 . . ? N3 C18 C19 113.0(3) . . ? N3 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N3 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C24 C19 C20 117.0(4) . . ? C24 C19 C18 123.3(4) . . ? C20 C19 C18 119.7(4) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 120.6(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 119.9(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.3(4) . . ? C24 C23 C9 121.6(4) . . ? C22 C23 C9 119.0(4) . . ? C19 C24 C23 121.6(4) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? O2 C25 O3 123.7(4) . . ? O2 C25 C27 119.4(4) . . ? O3 C25 C27 116.7(4) . . ? O6 C26 O7 123.7(4) . . ? O6 C26 C28 116.8(4) . . ? O7 C26 C28 119.3(4) . . ? C32 C27 C28 119.1(3) . . ? C32 C27 C25 116.9(3) . . ? C28 C27 C25 123.9(3) . . ? C29 C28 C27 119.0(3) . . ? C29 C28 C26 118.6(3) . . ? C27 C28 C26 122.3(3) . . ? C30 C29 C28 122.1(3) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 119.4(4) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 118.5(3) . . ? C32 C31 C33 123.4(3) . . ? C30 C31 C33 118.1(3) . . ? C27 C32 C31 121.9(3) . . ? C27 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? O1 C33 C31 121.1(4) . . ? O1 C33 C34 120.3(4) . . ? C31 C33 C34 118.6(3) . . ? C39 C34 C35 119.1(4) . . ? C39 C34 C33 120.6(3) . . ? C35 C34 C33 120.1(4) . . ? C36 C35 C34 120.7(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.4(4) . . ? C36 C37 C41 116.8(4) . . ? C38 C37 C41 123.8(4) . . ? C37 C38 C39 119.3(4) . . ? C37 C38 C40 122.0(3) . . ? C39 C38 C40 118.7(3) . . ? C34 C39 C38 120.8(4) . . ? C34 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? O5 C40 O4 124.6(5) . . ? O5 C40 C38 118.9(4) . . ? O4 C40 C38 116.6(4) . . ? O9 C41 O8 124.2(4) . . ? O9 C41 C37 117.2(4) . . ? O8 C41 C37 118.4(4) . . ? C15 N1 C16 106.5(3) . . ? C15 N1 Zn1 110.2(3) . . ? C16 N1 Zn1 138.5(3) . . ? C10 N2 C14 119.3(4) . . ? C10 N2 Zn1 124.2(3) . . ? C14 N2 Zn1 116.3(3) . . ? C15 N3 C17 107.2(3) . . ? C15 N3 C18 129.1(4) . . ? C17 N3 C18 122.5(4) . . ? C1 N4 C5 117.9(4) . . ? C1 N4 Zn2 126.7(3) . . ? C5 N4 Zn2 115.3(3) . . ? C6 N5 C7 107.0(3) . . ? C6 N5 Zn2 116.0(3) . . ? C7 N5 Zn2 136.5(3) . . ? C6 N6 C8 107.1(3) . . ? C6 N6 C9 126.4(4) . . ? C8 N6 C9 126.4(3) . . ? C25 O3 Zn1 109.4(3) . 2_665 ? C40 O4 Zn1 128.4(3) . 1_565 ? C26 O6 Zn2 114.3(3) . . ? C41 O8 Zn2 136.8(3) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 C1 C2 C3 -2.1(8) . . . . ? C1 C2 C3 C4 1.7(8) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 N4 -0.3(7) . . . . ? C3 C4 C5 C6 -177.7(4) . . . . ? N4 C5 C6 N5 -7.2(5) . . . . ? C4 C5 C6 N5 170.4(4) . . . . ? N4 C5 C6 N6 175.0(4) . . . . ? C4 C5 C6 N6 -7.4(7) . . . . ? N5 C7 C8 N6 0.5(6) . . . . ? N2 C10 C11 C12 -0.6(8) . . . . ? C10 C11 C12 C13 0.4(7) . . . . ? C11 C12 C13 C14 0.3(7) . . . . ? C12 C13 C14 N2 -0.9(6) . . . . ? C12 C13 C14 C15 -177.1(4) . . . . ? N2 C14 C15 N1 -15.2(5) . . . . ? C13 C14 C15 N1 161.3(4) . . . . ? N2 C14 C15 N3 165.0(4) . . . . ? C13 C14 C15 N3 -18.5(7) . . . . ? N1 C16 C17 N3 0.0(6) . . . . ? N3 C18 C19 C24 -24.4(6) . . . . ? N3 C18 C19 C20 156.7(4) . . . . ? C24 C19 C20 C21 0.3(7) . . . . ? C18 C19 C20 C21 179.3(4) . . . . ? C19 C20 C21 C22 1.0(7) . . . . ? C20 C21 C22 C23 -1.9(7) . . . . ? C21 C22 C23 C24 1.5(7) . . . . ? C21 C22 C23 C9 -176.0(4) . . . . ? N6 C9 C23 C24 74.5(5) . . . . ? N6 C9 C23 C22 -108.1(5) . . . . ? C20 C19 C24 C23 -0.7(6) . . . . ? C18 C19 C24 C23 -179.7(4) . . . . ? C22 C23 C24 C19 -0.2(6) . . . . ? C9 C23 C24 C19 177.3(4) . . . . ? O2 C25 C27 C32 67.4(5) . . . . ? O3 C25 C27 C32 -107.3(4) . . . . ? O2 C25 C27 C28 -115.7(5) . . . . ? O3 C25 C27 C28 69.5(5) . . . . ? C32 C27 C28 C29 -1.0(6) . . . . ? C25 C27 C28 C29 -177.7(4) . . . . ? C32 C27 C28 C26 -177.7(4) . . . . ? C25 C27 C28 C26 5.6(6) . . . . ? O6 C26 C28 C29 -153.4(4) . . . . ? O7 C26 C28 C29 21.8(6) . . . . ? O6 C26 C28 C27 23.3(6) . . . . ? O7 C26 C28 C27 -161.5(4) . . . . ? C27 C28 C29 C30 -0.6(6) . . . . ? C26 C28 C29 C30 176.2(4) . . . . ? C28 C29 C30 C31 1.3(7) . . . . ? C29 C30 C31 C32 -0.5(6) . . . . ? C29 C30 C31 C33 -177.8(4) . . . . ? C28 C27 C32 C31 1.9(6) . . . . ? C25 C27 C32 C31 178.8(4) . . . . ? C30 C31 C32 C27 -1.1(6) . . . . ? C33 C31 C32 C27 176.1(4) . . . . ? C32 C31 C33 O1 -147.2(5) . . . . ? C30 C31 C33 O1 30.1(6) . . . . ? C32 C31 C33 C34 34.1(6) . . . . ? C30 C31 C33 C34 -148.7(4) . . . . ? O1 C33 C34 C39 -137.1(5) . . . . ? C31 C33 C34 C39 41.7(5) . . . . ? O1 C33 C34 C35 37.9(6) . . . . ? C31 C33 C34 C35 -143.3(4) . . . . ? C39 C34 C35 C36 0.0(7) . . . . ? C33 C34 C35 C36 -175.1(4) . . . . ? C34 C35 C36 C37 3.6(7) . . . . ? C35 C36 C37 C38 -4.3(6) . . . . ? C35 C36 C37 C41 174.1(4) . . . . ? C36 C37 C38 C39 1.5(6) . . . . ? C41 C37 C38 C39 -176.9(4) . . . . ? C36 C37 C38 C40 -177.4(4) . . . . ? C41 C37 C38 C40 4.3(6) . . . . ? C35 C34 C39 C38 -2.8(6) . . . . ? C33 C34 C39 C38 172.2(4) . . . . ? C37 C38 C39 C34 2.1(6) . . . . ? C40 C38 C39 C34 -179.0(4) . . . . ? C37 C38 C40 O5 8.1(7) . . . . ? C39 C38 C40 O5 -170.8(5) . . . . ? C37 C38 C40 O4 -170.7(4) . . . . ? C39 C38 C40 O4 10.5(6) . . . . ? C36 C37 C41 O9 70.1(6) . . . . ? C38 C37 C41 O9 -111.5(5) . . . . ? C36 C37 C41 O8 -103.9(5) . . . . ? C38 C37 C41 O8 74.5(6) . . . . ? N3 C15 N1 C16 -0.8(5) . . . . ? C14 C15 N1 C16 179.4(4) . . . . ? N3 C15 N1 Zn1 -161.0(3) . . . . ? C14 C15 N1 Zn1 19.1(5) . . . . ? C17 C16 N1 C15 0.5(5) . . . . ? C17 C16 N1 Zn1 152.0(4) . . . . ? O4 Zn1 N1 C15 101.7(3) 1_545 . . . ? O3 Zn1 N1 C15 -149.0(3) 2_665 . . . ? N2 Zn1 N1 C15 -12.6(3) . . . . ? O1W Zn1 N1 C15 27.7(6) . . . . ? O4 Zn1 N1 C16 -49.1(5) 1_545 . . . ? O3 Zn1 N1 C16 60.2(5) 2_665 . . . ? N2 Zn1 N1 C16 -163.4(5) . . . . ? O1W Zn1 N1 C16 -123.1(6) . . . . ? C11 C10 N2 C14 0.0(7) . . . . ? C11 C10 N2 Zn1 174.5(4) . . . . ? C13 C14 N2 C10 0.8(6) . . . . ? C15 C14 N2 C10 177.4(4) . . . . ? C13 C14 N2 Zn1 -174.2(3) . . . . ? C15 C14 N2 Zn1 2.4(4) . . . . ? O4 Zn1 N2 C10 110.9(4) 1_545 . . . ? O3 Zn1 N2 C10 -81.1(4) 2_665 . . . ? O1W Zn1 N2 C10 21.1(4) . . . . ? N1 Zn1 N2 C10 -169.3(4) . . . . ? O4 Zn1 N2 C14 -74.4(3) 1_545 . . . ? O3 Zn1 N2 C14 93.6(3) 2_665 . . . ? O1W Zn1 N2 C14 -164.2(3) . . . . ? N1 Zn1 N2 C14 5.4(3) . . . . ? N1 C15 N3 C17 0.7(5) . . . . ? C14 C15 N3 C17 -179.5(4) . . . . ? N1 C15 N3 C18 168.2(4) . . . . ? C14 C15 N3 C18 -12.0(7) . . . . ? C16 C17 N3 C15 -0.4(5) . . . . ? C16 C17 N3 C18 -168.9(4) . . . . ? C19 C18 N3 C15 -57.8(6) . . . . ? C19 C18 N3 C17 108.0(5) . . . . ? C2 C1 N4 C5 1.3(7) . . . . ? C2 C1 N4 Zn2 177.1(4) . . . . ? C4 C5 N4 C1 0.0(6) . . . . ? C6 C5 N4 C1 177.8(4) . . . . ? C4 C5 N4 Zn2 -176.3(3) . . . . ? C6 C5 N4 Zn2 1.5(4) . . . . ? O6 Zn2 N4 C1 -31.9(4) . . . . ? O8 Zn2 N4 C1 60.3(4) 1_545 . . . ? N5 Zn2 N4 C1 -173.6(4) . . . . ? O2W Zn2 N4 C1 -151.4(6) . . . . ? O6 Zn2 N4 C5 144.1(3) . . . . ? O8 Zn2 N4 C5 -123.7(3) 1_545 . . . ? N5 Zn2 N4 C5 2.4(3) . . . . ? O2W Zn2 N4 C5 24.5(7) . . . . ? N6 C6 N5 C7 1.1(5) . . . . ? C5 C6 N5 C7 -177.1(4) . . . . ? N6 C6 N5 Zn2 -172.2(3) . . . . ? C5 C6 N5 Zn2 9.6(5) . . . . ? C8 C7 N5 C6 -1.0(5) . . . . ? C8 C7 N5 Zn2 170.3(3) . . . . ? O6 Zn2 N5 C6 -85.7(4) . . . . ? O8 Zn2 N5 C6 82.6(3) 1_545 . . . ? O2W Zn2 N5 C6 -179.7(3) . . . . ? N4 Zn2 N5 C6 -6.2(3) . . . . ? O6 Zn2 N5 C7 103.6(5) . . . . ? O8 Zn2 N5 C7 -88.1(5) 1_545 . . . ? O2W Zn2 N5 C7 9.6(5) . . . . ? N4 Zn2 N5 C7 -176.9(5) . . . . ? N5 C6 N6 C8 -0.8(5) . . . . ? C5 C6 N6 C8 177.2(4) . . . . ? N5 C6 N6 C9 175.6(4) . . . . ? C5 C6 N6 C9 -6.4(7) . . . . ? C7 C8 N6 C6 0.2(5) . . . . ? C7 C8 N6 C9 -176.3(4) . . . . ? C23 C9 N6 C6 -171.0(4) . . . . ? C23 C9 N6 C8 4.8(6) . . . . ? O2 C25 O3 Zn1 -3.1(5) . . . 2_665 ? C27 C25 O3 Zn1 171.4(2) . . . 2_665 ? O5 C40 O4 Zn1 11.0(8) . . . 1_565 ? C38 C40 O4 Zn1 -170.3(3) . . . 1_565 ? O7 C26 O6 Zn2 6.9(6) . . . . ? C28 C26 O6 Zn2 -178.2(3) . . . . ? O8 Zn2 O6 C26 -179.0(3) 1_545 . . . ? N5 Zn2 O6 C26 -8.3(5) . . . . ? O2W Zn2 O6 C26 83.3(4) . . . . ? N4 Zn2 O6 C26 -81.6(3) . . . . ? O9 C41 O8 Zn2 -178.3(4) . . . 1_565 ? C37 C41 O8 Zn2 -4.7(8) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.297 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.099 #===end data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C41 H28 Cd2 N6 O10, H2 O' _chemical_formula_sum 'C41 H30 Cd2 N6 O11' _chemical_formula_weight 1007.51 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_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6390(4) _cell_length_b 11.3020(5) _cell_length_c 16.0970(6) _cell_angle_alpha 95.6190(10) _cell_angle_beta 101.7810(10) _cell_angle_gamma 100.5100(10) _cell_volume 1844.52(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10336 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 28.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.692 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11368 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.60 _reflns_number_total 8250 _reflns_number_gt 7433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^+0.8699P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8250 _refine_ls_number_parameters 553 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 -0.177191(15) -0.752543(14) 0.485981(10) 0.02545(5) Uani 1 1 d . . . Cd2 Cd 0.036800(17) 0.422460(15) 0.289109(11) 0.03185(6) Uani 1 1 d . . . C1 C 0.4694(3) 0.7228(3) 0.46790(18) 0.0439(6) Uani 1 1 d . . . H1 H 0.4534 0.6524 0.4930 0.053 Uiso 1 1 calc R . . C2 C 0.5888(3) 0.7547(3) 0.44500(18) 0.0468(7) Uani 1 1 d . . . H2 H 0.6514 0.7069 0.4544 0.056 Uiso 1 1 calc R . . C3 C 0.6119(3) 0.8586(3) 0.40823(17) 0.0455(7) Uani 1 1 d . . . H3 H 0.6919 0.8835 0.3937 0.055 Uiso 1 1 calc R . . C4 C 0.5155(3) 0.9266(3) 0.39279(16) 0.0389(6) Uani 1 1 d . . . H4 H 0.5292 0.9963 0.3668 0.047 Uiso 1 1 calc R . . C5 C 0.3975(2) 0.8885(2) 0.41701(14) 0.0290(5) Uani 1 1 d . . . C6 C 0.2872(2) 0.9519(2) 0.40666(14) 0.0274(4) Uani 1 1 d . . . C7 C 0.0955(3) 0.9849(2) 0.41487(16) 0.0354(5) Uani 1 1 d . . . H7 H 0.0126 0.9761 0.4268 0.042 Uiso 1 1 calc R . . C8 C 0.1498(3) 1.0736(2) 0.37432(16) 0.0366(5) Uani 1 1 d . . . H8 H 0.1120 1.1361 0.3538 0.044 Uiso 1 1 calc R . . C9 C 0.3545(3) 1.1279(2) 0.32289(16) 0.0366(5) Uani 1 1 d . . . H9A H 0.4435 1.1509 0.3574 0.044 Uiso 1 1 calc R . . H9B H 0.3222 1.2018 0.3144 0.044 Uiso 1 1 calc R . . C10 C 0.3557(3) 1.0623(2) 0.23741(15) 0.0331(5) Uani 1 1 d . . . C11 C 0.4593(3) 1.0978(3) 0.19886(19) 0.0475(7) Uani 1 1 d . . . H11 H 0.5277 1.1623 0.2259 0.057 Uiso 1 1 calc R . . C12 C 0.4610(4) 1.0370(3) 0.1196(2) 0.0589(8) Uani 1 1 d . . . H12 H 0.5291 1.0623 0.0931 0.071 Uiso 1 1 calc R . . C13 C 0.3608(4) 0.9384(3) 0.0802(2) 0.0527(8) Uani 1 1 d . . . H13 H 0.3626 0.8974 0.0276 0.063 Uiso 1 1 calc R . . C14 C 0.2586(3) 0.9013(2) 0.11879(16) 0.0381(6) Uani 1 1 d . . . C15 C 0.2550(3) 0.9654(2) 0.19605(15) 0.0346(5) Uani 1 1 d . . . H15 H 0.1839 0.9430 0.2206 0.041 Uiso 1 1 calc R . . C16 C 0.1585(3) 0.7848(2) 0.08526(17) 0.0407(6) Uani 1 1 d . . . H16A H 0.0708 0.7991 0.0829 0.049 Uiso 1 1 calc R . . H16B H 0.1640 0.7547 0.0278 0.049 Uiso 1 1 calc R . . C17 C 0.3074(3) 0.6992(3) 0.19676(18) 0.0410(6) Uani 1 1 d . . . H17 H 0.3850 0.7535 0.1979 0.049 Uiso 1 1 calc R . . C18 C 0.2917(3) 0.6104(3) 0.24634(17) 0.0397(6) Uani 1 1 d . . . H18 H 0.3576 0.5941 0.2886 0.048 Uiso 1 1 calc R . . C19 C 0.1018(2) 0.5999(2) 0.16292(14) 0.0298(5) Uani 1 1 d . . . C20 C -0.0366(2) 0.5497(2) 0.12129(15) 0.0306(5) Uani 1 1 d . . . C21 C -0.1021(3) 0.5761(2) 0.04319(16) 0.0391(6) Uani 1 1 d . . . H21 H -0.0603 0.6331 0.0145 0.047 Uiso 1 1 calc R . . C22 C -0.2306(3) 0.5159(3) 0.00940(18) 0.0499(7) Uani 1 1 d . . . H22 H -0.2762 0.5326 -0.0424 0.060 Uiso 1 1 calc R . . C23 C -0.2906(3) 0.4317(3) 0.05218(19) 0.0500(7) Uani 1 1 d . . . H23 H -0.3769 0.3906 0.0301 0.060 Uiso 1 1 calc R . . C24 C -0.2195(3) 0.4091(2) 0.12920(18) 0.0410(6) Uani 1 1 d . . . H0 H -0.2595 0.3510 0.1580 0.049 Uiso 1 1 calc R . . C25 C 0.0239(3) 0.2045(2) 0.16545(16) 0.0365(5) Uani 1 1 d . . . C26 C -0.1486(2) 0.1629(2) 0.30195(15) 0.0305(5) Uani 1 1 d . . . C27 C -0.1510(2) 0.0692(2) 0.22623(14) 0.0271(4) Uani 1 1 d . . . C28 C -0.0821(3) 0.0927(2) 0.16196(15) 0.0319(5) Uani 1 1 d . . . C29 C -0.1047(3) 0.0044(2) 0.09075(16) 0.0414(6) Uani 1 1 d . . . H29 H -0.0616 0.0207 0.0471 0.050 Uiso 1 1 calc R . . C30 C -0.1888(3) -0.1062(2) 0.08309(16) 0.0417(6) Uani 1 1 d . . . H30 H -0.2026 -0.1631 0.0346 0.050 Uiso 1 1 calc R . . C31 C -0.2523(2) -0.1322(2) 0.14761(15) 0.0314(5) Uani 1 1 d . . . C32 C -0.2330(2) -0.0441(2) 0.21895(14) 0.0302(5) Uani 1 1 d . . . H32 H -0.2759 -0.0617 0.2625 0.036 Uiso 1 1 calc R . . C33 C -0.3437(3) -0.2525(2) 0.13828(16) 0.0362(5) Uani 1 1 d . . . C34 C -0.2133(2) -0.3107(2) 0.27177(14) 0.0277(4) Uani 1 1 d . . . H34 H -0.1483 -0.2418 0.2755 0.033 Uiso 1 1 calc R . . C35 C -0.3272(2) -0.3311(2) 0.20702(15) 0.0297(5) Uani 1 1 d . . . C36 C -0.4249(2) -0.4338(2) 0.20304(16) 0.0337(5) Uani 1 1 d . . . H36 H -0.5014 -0.4488 0.1601 0.040 Uiso 1 1 calc R . . C37 C -0.4088(2) -0.5129(2) 0.26207(16) 0.0329(5) Uani 1 1 d . . . H37 H -0.4756 -0.5799 0.2593 0.040 Uiso 1 1 calc R . . C38 C -0.2940(2) -0.49469(19) 0.32606(14) 0.0267(4) Uani 1 1 d . . . C39 C -0.1953(2) -0.39193(19) 0.33114(14) 0.0251(4) Uani 1 1 d . . . C40 C -0.2796(2) -0.5904(2) 0.38444(15) 0.0296(5) Uani 1 1 d . . . C41 C -0.0644(2) -0.36139(19) 0.39538(14) 0.0252(4) Uani 1 1 d . . . N1 N -0.0965(2) 0.46712(19) 0.16359(13) 0.0333(4) Uani 1 1 d . . . N2 N 0.1649(2) 0.54865(19) 0.22510(13) 0.0333(4) Uani 1 1 d . . . N3 N 0.1862(2) 0.69378(19) 0.14403(13) 0.0333(4) Uani 1 1 d . . . N4 N 0.1812(2) 0.91024(18) 0.43542(13) 0.0312(4) Uani 1 1 d . . . N5 N 0.2716(2) 1.05322(17) 0.36946(12) 0.0302(4) Uani 1 1 d . . . N6 N 0.3760(2) 0.78882(18) 0.45546(13) 0.0325(4) Uani 1 1 d . . . O1 O 0.09603(18) 0.25097(15) 0.23800(11) 0.0366(4) Uani 1 1 d . . . O2 O 0.0368(3) 0.2398(2) 0.09673(13) 0.0649(7) Uani 1 1 d . . . O3 O -0.1362(2) 0.27199(16) 0.29191(14) 0.0481(5) Uani 1 1 d . . . O4 O -0.1672(2) 0.12120(17) 0.36920(11) 0.0399(4) Uani 1 1 d . . . O5 O 0.02975(16) -0.40177(16) 0.37665(11) 0.0339(4) Uani 1 1 d . . . O6 O -0.05257(16) -0.28637(15) 0.46077(10) 0.0322(4) Uani 1 1 d . . . O7 O -0.18020(19) -0.56753(15) 0.44685(11) 0.0385(4) Uani 1 1 d . . . O8 O -0.36213(19) -0.68646(17) 0.36914(13) 0.0448(5) Uani 1 1 d . . . O9 O -0.4280(2) -0.2875(2) 0.07304(14) 0.0657(7) Uani 1 1 d . . . O1W O 0.1658(2) 0.39876(18) 0.41673(12) 0.0437(4) Uani 1 1 d D . . H1A H 0.137(4) 0.3383(18) 0.4443(18) 0.066 Uiso 1 1 d D . . H1B H 0.173(4) 0.4628(16) 0.4550(16) 0.066 Uiso 1 1 d D . . O2W O 0.3230(4) 0.3264(4) 0.1412(4) 0.1281(15) Uani 1 1 d D . . H2A H 0.238(2) 0.299(6) 0.143(5) 0.192 Uiso 1 1 d D . . H2B H 0.351(6) 0.256(3) 0.139(5) 0.192 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02756(9) 0.02352(9) 0.02508(9) 0.00550(6) 0.00622(6) 0.00345(6) Cd2 0.03790(11) 0.02728(9) 0.02941(10) 0.00617(7) 0.00738(7) 0.00347(7) C1 0.0494(16) 0.0458(15) 0.0436(15) 0.0111(12) 0.0144(12) 0.0213(13) C2 0.0419(15) 0.0668(19) 0.0380(14) 0.0047(13) 0.0105(12) 0.0270(14) C3 0.0315(13) 0.072(2) 0.0349(14) 0.0048(13) 0.0122(11) 0.0124(13) C4 0.0344(13) 0.0512(15) 0.0314(12) 0.0089(11) 0.0101(10) 0.0050(11) C5 0.0297(11) 0.0329(12) 0.0227(10) 0.0024(9) 0.0050(8) 0.0039(9) C6 0.0317(12) 0.0276(11) 0.0221(10) 0.0043(8) 0.0068(8) 0.0026(9) C7 0.0349(13) 0.0413(13) 0.0358(13) 0.0117(10) 0.0131(10) 0.0137(11) C8 0.0419(14) 0.0352(13) 0.0360(13) 0.0087(10) 0.0101(11) 0.0128(11) C9 0.0447(14) 0.0268(11) 0.0355(13) 0.0087(10) 0.0106(11) -0.0033(10) C10 0.0399(13) 0.0301(12) 0.0301(12) 0.0117(9) 0.0097(10) 0.0035(10) C11 0.0484(17) 0.0441(15) 0.0469(16) 0.0100(12) 0.0165(13) -0.0066(12) C12 0.060(2) 0.065(2) 0.0535(18) 0.0123(15) 0.0314(16) -0.0054(16) C13 0.072(2) 0.0503(17) 0.0382(15) 0.0061(13) 0.0272(14) 0.0034(15) C14 0.0499(15) 0.0340(13) 0.0299(12) 0.0111(10) 0.0088(11) 0.0047(11) C15 0.0399(13) 0.0337(12) 0.0312(12) 0.0106(10) 0.0117(10) 0.0028(10) C16 0.0545(17) 0.0338(13) 0.0303(12) 0.0081(10) 0.0053(11) 0.0031(11) C17 0.0303(13) 0.0432(14) 0.0468(15) 0.0099(12) 0.0050(11) 0.0026(11) C18 0.0312(13) 0.0468(15) 0.0406(14) 0.0105(11) 0.0047(10) 0.0083(11) C19 0.0338(12) 0.0294(11) 0.0259(11) 0.0026(9) 0.0077(9) 0.0050(9) C20 0.0349(12) 0.0279(11) 0.0281(11) 0.0011(9) 0.0065(9) 0.0067(9) C21 0.0451(15) 0.0377(13) 0.0303(12) 0.0028(10) 0.0008(10) 0.0074(11) C22 0.0518(17) 0.0530(17) 0.0356(14) -0.0007(12) -0.0093(12) 0.0123(14) C23 0.0370(15) 0.0518(17) 0.0487(17) -0.0075(13) -0.0044(12) 0.0010(12) C24 0.0360(14) 0.0387(14) 0.0435(15) 0.0000(11) 0.0081(11) -0.0004(11) C25 0.0458(15) 0.0341(13) 0.0333(13) 0.0077(10) 0.0146(11) 0.0102(11) C26 0.0298(12) 0.0286(11) 0.0334(12) 0.0005(9) 0.0110(9) 0.0042(9) C27 0.0330(12) 0.0261(11) 0.0228(10) 0.0042(8) 0.0058(8) 0.0081(9) C28 0.0418(13) 0.0308(12) 0.0259(11) 0.0074(9) 0.0104(10) 0.0095(10) C29 0.0597(18) 0.0386(14) 0.0286(12) 0.0023(10) 0.0196(12) 0.0075(12) C30 0.0607(18) 0.0348(13) 0.0277(12) -0.0029(10) 0.0098(11) 0.0089(12) C31 0.0388(13) 0.0258(11) 0.0263(11) 0.0053(9) -0.0011(9) 0.0072(9) C32 0.0367(12) 0.0302(11) 0.0242(11) 0.0061(9) 0.0068(9) 0.0072(9) C33 0.0393(14) 0.0290(12) 0.0339(13) 0.0039(10) -0.0043(10) 0.0056(10) C34 0.0277(11) 0.0229(10) 0.0288(11) 0.0030(8) 0.0018(9) 0.0016(8) C35 0.0294(11) 0.0265(11) 0.0300(11) 0.0028(9) -0.0001(9) 0.0060(9) C36 0.0263(11) 0.0306(12) 0.0381(13) 0.0043(10) -0.0045(9) 0.0038(9) C37 0.0255(11) 0.0282(11) 0.0412(13) 0.0051(10) 0.0033(10) 0.0002(9) C38 0.0269(11) 0.0240(10) 0.0290(11) 0.0034(8) 0.0070(9) 0.0046(8) C39 0.0238(10) 0.0267(10) 0.0242(10) 0.0019(8) 0.0037(8) 0.0068(8) C40 0.0371(13) 0.0272(11) 0.0280(11) 0.0058(9) 0.0127(9) 0.0087(9) C41 0.0261(11) 0.0236(10) 0.0239(10) 0.0061(8) 0.0017(8) 0.0029(8) N1 0.0332(11) 0.0328(10) 0.0316(10) 0.0013(8) 0.0056(8) 0.0042(8) N2 0.0322(11) 0.0374(11) 0.0308(10) 0.0092(8) 0.0067(8) 0.0069(9) N3 0.0360(11) 0.0325(10) 0.0299(10) 0.0057(8) 0.0058(8) 0.0042(8) N4 0.0313(10) 0.0357(11) 0.0303(10) 0.0109(8) 0.0116(8) 0.0082(8) N5 0.0367(11) 0.0274(9) 0.0258(9) 0.0068(7) 0.0083(8) 0.0018(8) N6 0.0330(11) 0.0344(10) 0.0325(10) 0.0071(8) 0.0094(8) 0.0097(8) O1 0.0412(10) 0.0317(9) 0.0364(9) 0.0056(7) 0.0083(8) 0.0067(7) O2 0.0904(18) 0.0606(14) 0.0354(11) 0.0170(10) 0.0173(11) -0.0144(12) O3 0.0595(13) 0.0271(9) 0.0651(13) 0.0036(8) 0.0379(11) 0.0029(8) O4 0.0587(12) 0.0377(10) 0.0250(8) 0.0029(7) 0.0128(8) 0.0117(8) O5 0.0272(8) 0.0394(9) 0.0332(9) 0.0022(7) 0.0017(7) 0.0092(7) O6 0.0326(9) 0.0302(8) 0.0292(8) -0.0010(7) 0.0021(7) 0.0030(7) O7 0.0519(11) 0.0271(8) 0.0305(9) 0.0045(7) -0.0026(8) 0.0058(8) O8 0.0408(11) 0.0365(10) 0.0552(12) 0.0172(9) 0.0117(9) -0.0031(8) O9 0.0745(16) 0.0495(12) 0.0457(12) 0.0148(10) -0.0298(11) -0.0124(11) O1W 0.0618(13) 0.0385(10) 0.0308(9) 0.0042(8) 0.0075(9) 0.0140(9) O2W 0.080(2) 0.100(3) 0.190(4) 0.046(3) 0.001(3) 0.001(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 Cd1 O7 2.2459(17) . ? Cd1 O4 2.2788(17) 1_545 ? Cd1 N4 2.284(2) 2_556 ? Cd1 O6 2.3626(16) 2_546 ? Cd1 N6 2.471(2) 2_556 ? Cd2 N2 2.260(2) . ? Cd2 O1 2.2750(17) . ? Cd2 O3 2.2778(19) . ? Cd2 O1W 2.2948(19) . ? Cd2 O5 2.3425(17) 1_565 ? Cd2 N1 2.375(2) . ? C1 N6 1.343(3) . ? C1 C2 1.389(4) . ? C1 H1 0.9300 . ? C2 C3 1.371(4) . ? C2 H2 0.9300 . ? C3 C4 1.387(4) . ? C3 H3 0.9300 . ? C4 C5 1.396(3) . ? C4 H4 0.9300 . ? C5 N6 1.343(3) . ? C5 C6 1.473(3) . ? C6 N4 1.331(3) . ? C6 N5 1.364(3) . ? C7 C8 1.355(4) . ? C7 N4 1.365(3) . ? C7 H7 0.9300 . ? C8 N5 1.373(3) . ? C8 H8 0.9300 . ? C9 N5 1.474(3) . ? C9 C10 1.501(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.389(4) . ? C10 C15 1.389(3) . ? C11 C12 1.393(4) . ? C11 H11 0.9300 . ? C12 C13 1.390(5) . ? C12 H12 0.9300 . ? C13 C14 1.380(4) . ? C13 H13 0.9300 . ? C14 C15 1.388(4) . ? C14 C16 1.508(4) . ? C15 H15 0.9300 . ? C16 N3 1.492(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.349(4) . ? C17 N3 1.379(3) . ? C17 H17 0.9300 . ? C18 N2 1.359(3) . ? C18 H18 0.9300 . ? C19 N2 1.330(3) . ? C19 N3 1.360(3) . ? C19 C20 1.469(3) . ? C20 N1 1.351(3) . ? C20 C21 1.396(3) . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C23 1.369(5) . ? C22 H22 0.9300 . ? C23 C24 1.387(4) . ? C23 H23 0.9300 . ? C24 N1 1.330(3) . ? C24 H0 0.9300 . ? C25 O2 1.237(3) . ? C25 O1 1.263(3) . ? C25 C28 1.521(4) . ? C26 O3 1.246(3) . ? C26 O4 1.259(3) . ? C26 C27 1.527(3) . ? C27 C32 1.392(3) . ? C27 C28 1.404(3) . ? C28 C29 1.394(3) . ? C29 C30 1.377(4) . ? C29 H29 0.9300 . ? C30 C31 1.377(4) . ? C30 H30 0.9300 . ? C31 C32 1.399(3) . ? C31 C33 1.495(3) . ? C32 H32 0.9300 . ? C33 O9 1.212(3) . ? C33 C35 1.488(3) . ? C34 C35 1.394(3) . ? C34 C39 1.398(3) . ? C34 H34 0.9300 . ? C35 C36 1.397(3) . ? C36 C37 1.374(3) . ? C36 H36 0.9300 . ? C37 C38 1.396(3) . ? C37 H37 0.9300 . ? C38 C39 1.400(3) . ? C38 C40 1.509(3) . ? C39 C41 1.515(3) . ? C40 O8 1.234(3) . ? C40 O7 1.269(3) . ? C41 O5 1.252(3) . ? C41 O6 1.255(3) . ? N4 Cd1 2.284(2) 2_556 ? N6 Cd1 2.471(2) 2_556 ? O4 Cd1 2.2787(17) 1_565 ? O5 Cd2 2.3425(17) 1_545 ? O6 Cd1 2.3626(16) 2_546 ? O1W H1A 0.891(10) . ? O1W H1B 0.885(10) . ? O2W H2A 0.91(4) . ? O2W H2B 0.90(5) . ? 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 Cd1 O4 107.67(6) . 1_545 ? O7 Cd1 N4 162.18(7) . 2_556 ? O4 Cd1 N4 90.12(7) 1_545 2_556 ? O7 Cd1 O6 94.94(6) . 2_546 ? O4 Cd1 O6 92.47(6) 1_545 2_546 ? N4 Cd1 O6 85.04(7) 2_556 2_546 ? O7 Cd1 N6 101.05(7) . 2_556 ? O4 Cd1 N6 119.00(7) 1_545 2_556 ? N4 Cd1 N6 68.24(7) 2_556 2_556 ? O6 Cd1 N6 137.40(6) 2_546 2_556 ? N2 Cd2 O1 95.12(7) . . ? N2 Cd2 O3 154.78(8) . . ? O1 Cd2 O3 76.60(7) . . ? N2 Cd2 O1W 106.99(8) . . ? O1 Cd2 O1W 84.02(6) . . ? O3 Cd2 O1W 95.92(8) . . ? N2 Cd2 O5 85.66(7) . 1_565 ? O1 Cd2 O5 162.35(6) . 1_565 ? O3 Cd2 O5 109.45(6) . 1_565 ? O1W Cd2 O5 78.92(6) . 1_565 ? N2 Cd2 N1 71.43(7) . . ? O1 Cd2 N1 101.64(7) . . ? O3 Cd2 N1 86.76(8) . . ? O1W Cd2 N1 174.19(7) . . ? O5 Cd2 N1 95.33(6) 1_565 . ? N6 C1 C2 122.9(3) . . ? N6 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N6 C5 C4 121.7(2) . . ? N6 C5 C6 113.0(2) . . ? C4 C5 C6 125.3(2) . . ? N4 C6 N5 109.6(2) . . ? N4 C6 C5 120.3(2) . . ? N5 C6 C5 130.1(2) . . ? C8 C7 N4 109.4(2) . . ? C8 C7 H7 125.3 . . ? N4 C7 H7 125.3 . . ? C7 C8 N5 106.6(2) . . ? C7 C8 H8 126.7 . . ? N5 C8 H8 126.7 . . ? N5 C9 C10 112.38(19) . . ? N5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C15 119.0(2) . . ? C11 C10 C9 119.9(2) . . ? C15 C10 C9 121.1(2) . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.4(3) . . ? C13 C14 C16 122.1(3) . . ? C15 C14 C16 118.2(2) . . ? C14 C15 C10 121.2(2) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? N3 C16 C14 108.3(2) . . ? N3 C16 H16A 110.0 . . ? C14 C16 H16A 110.0 . . ? N3 C16 H16B 110.0 . . ? C14 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C18 C17 N3 106.8(2) . . ? C18 C17 H17 126.6 . . ? N3 C17 H17 126.6 . . ? C17 C18 N2 109.5(2) . . ? C17 C18 H18 125.2 . . ? N2 C18 H18 125.2 . . ? N2 C19 N3 109.9(2) . . ? N2 C19 C20 121.0(2) . . ? N3 C19 C20 129.0(2) . . ? N1 C20 C21 121.2(2) . . ? N1 C20 C19 113.5(2) . . ? C21 C20 C19 125.3(2) . . ? C22 C21 C20 118.7(3) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 118.4(3) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? N1 C24 C23 122.7(3) . . ? N1 C24 H0 118.7 . . ? C23 C24 H0 118.7 . . ? O2 C25 O1 124.9(3) . . ? O2 C25 C28 117.6(2) . . ? O1 C25 C28 117.4(2) . . ? O3 C26 O4 125.0(2) . . ? O3 C26 C27 118.8(2) . . ? O4 C26 C27 116.0(2) . . ? C32 C27 C28 118.7(2) . . ? C32 C27 C26 117.0(2) . . ? C28 C27 C26 124.2(2) . . ? C29 C28 C27 118.7(2) . . ? C29 C28 C25 115.8(2) . . ? C27 C28 C25 125.4(2) . . ? C30 C29 C28 122.0(2) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C31 C30 C29 119.6(2) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 119.3(2) . . ? C30 C31 C33 119.0(2) . . ? C32 C31 C33 121.6(2) . . ? C27 C32 C31 121.5(2) . . ? C27 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? O9 C33 C35 120.3(2) . . ? O9 C33 C31 119.5(2) . . ? C35 C33 C31 120.1(2) . . ? C35 C34 C39 121.1(2) . . ? C35 C34 H34 119.5 . . ? C39 C34 H34 119.5 . . ? C34 C35 C36 118.8(2) . . ? C34 C35 C33 122.2(2) . . ? C36 C35 C33 118.9(2) . . ? C37 C36 C35 120.4(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 121.3(2) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C39 119.0(2) . . ? C37 C38 C40 118.1(2) . . ? C39 C38 C40 122.9(2) . . ? C34 C39 C38 119.4(2) . . ? C34 C39 C41 115.39(19) . . ? C38 C39 C41 125.15(19) . . ? O8 C40 O7 123.3(2) . . ? O8 C40 C38 119.5(2) . . ? O7 C40 C38 117.2(2) . . ? O5 C41 O6 123.1(2) . . ? O5 C41 C39 118.66(19) . . ? O6 C41 C39 117.80(19) . . ? C24 N1 C20 119.1(2) . . ? C24 N1 Cd2 124.55(18) . . ? C20 N1 Cd2 116.06(16) . . ? C19 N2 C18 107.0(2) . . ? C19 N2 Cd2 115.82(16) . . ? C18 N2 Cd2 134.96(17) . . ? C19 N3 C17 106.8(2) . . ? C19 N3 C16 129.4(2) . . ? C17 N3 C16 123.6(2) . . ? C6 N4 C7 107.0(2) . . ? C6 N4 Cd1 120.37(15) . 2_556 ? C7 N4 Cd1 132.40(16) . 2_556 ? C6 N5 C8 107.3(2) . . ? C6 N5 C9 131.3(2) . . ? C8 N5 C9 121.1(2) . . ? C1 N6 C5 118.5(2) . . ? C1 N6 Cd1 123.85(18) . 2_556 ? C5 N6 Cd1 117.24(15) . 2_556 ? C25 O1 Cd2 111.25(16) . . ? C26 O3 Cd2 134.44(18) . . ? C26 O4 Cd1 120.60(16) . 1_565 ? C41 O5 Cd2 131.62(15) . 1_545 ? C41 O6 Cd1 100.34(14) . 2_546 ? C40 O7 Cd1 101.65(14) . . ? Cd2 O1W H1A 119(2) . . ? Cd2 O1W H1B 109(2) . . ? H1A O1W H1B 101.2(14) . . ? H2A O2W H2B 100(6) . . ? 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 N6 C1 C2 C3 0.1(4) . . . . ? C1 C2 C3 C4 -1.8(4) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C3 C4 C5 N6 0.7(4) . . . . ? C3 C4 C5 C6 178.7(2) . . . . ? N6 C5 C6 N4 1.0(3) . . . . ? C4 C5 C6 N4 -177.1(2) . . . . ? N6 C5 C6 N5 -178.4(2) . . . . ? C4 C5 C6 N5 3.5(4) . . . . ? N4 C7 C8 N5 0.2(3) . . . . ? N5 C9 C10 C11 -157.3(2) . . . . ? N5 C9 C10 C15 22.2(3) . . . . ? C15 C10 C11 C12 0.4(4) . . . . ? C9 C10 C11 C12 179.8(3) . . . . ? C10 C11 C12 C13 -1.8(5) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 1.8(5) . . . . ? C12 C13 C14 C16 -171.0(3) . . . . ? C13 C14 C15 C10 -3.3(4) . . . . ? C16 C14 C15 C10 169.8(2) . . . . ? C11 C10 C15 C14 2.2(4) . . . . ? C9 C10 C15 C14 -177.2(2) . . . . ? C13 C14 C16 N3 105.7(3) . . . . ? C15 C14 C16 N3 -67.2(3) . . . . ? N3 C17 C18 N2 1.0(3) . . . . ? N2 C19 C20 N1 13.1(3) . . . . ? N3 C19 C20 N1 -171.4(2) . . . . ? N2 C19 C20 C21 -163.2(2) . . . . ? N3 C19 C20 C21 12.3(4) . . . . ? N1 C20 C21 C22 0.0(4) . . . . ? C19 C20 C21 C22 176.0(2) . . . . ? C20 C21 C22 C23 -0.4(4) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C22 C23 C24 N1 1.0(4) . . . . ? O3 C26 C27 C32 -144.5(2) . . . . ? O4 C26 C27 C32 31.6(3) . . . . ? O3 C26 C27 C28 31.8(4) . . . . ? O4 C26 C27 C28 -152.1(2) . . . . ? C32 C27 C28 C29 3.9(3) . . . . ? C26 C27 C28 C29 -172.3(2) . . . . ? C32 C27 C28 C25 -171.7(2) . . . . ? C26 C27 C28 C25 12.1(4) . . . . ? O2 C25 C28 C29 34.0(4) . . . . ? O1 C25 C28 C29 -142.8(2) . . . . ? O2 C25 C28 C27 -150.2(3) . . . . ? O1 C25 C28 C27 32.9(4) . . . . ? C27 C28 C29 C30 -2.2(4) . . . . ? C25 C28 C29 C30 173.8(3) . . . . ? C28 C29 C30 C31 -0.6(4) . . . . ? C29 C30 C31 C32 1.7(4) . . . . ? C29 C30 C31 C33 179.8(2) . . . . ? C28 C27 C32 C31 -2.9(3) . . . . ? C26 C27 C32 C31 173.6(2) . . . . ? C30 C31 C32 C27 0.1(4) . . . . ? C33 C31 C32 C27 -178.0(2) . . . . ? C30 C31 C33 O9 -50.4(4) . . . . ? C32 C31 C33 O9 127.7(3) . . . . ? C30 C31 C33 C35 126.9(3) . . . . ? C32 C31 C33 C35 -55.1(3) . . . . ? C39 C34 C35 C36 1.0(3) . . . . ? C39 C34 C35 C33 -174.2(2) . . . . ? O9 C33 C35 C34 162.7(3) . . . . ? C31 C33 C35 C34 -14.5(4) . . . . ? O9 C33 C35 C36 -12.4(4) . . . . ? C31 C33 C35 C36 170.3(2) . . . . ? C34 C35 C36 C37 0.1(4) . . . . ? C33 C35 C36 C37 175.5(2) . . . . ? C35 C36 C37 C38 -1.5(4) . . . . ? C36 C37 C38 C39 1.7(4) . . . . ? C36 C37 C38 C40 -175.6(2) . . . . ? C35 C34 C39 C38 -0.8(3) . . . . ? C35 C34 C39 C41 177.3(2) . . . . ? C37 C38 C39 C34 -0.6(3) . . . . ? C40 C38 C39 C34 176.6(2) . . . . ? C37 C38 C39 C41 -178.4(2) . . . . ? C40 C38 C39 C41 -1.3(3) . . . . ? C37 C38 C40 O8 7.1(3) . . . . ? C39 C38 C40 O8 -170.1(2) . . . . ? C37 C38 C40 O7 -174.0(2) . . . . ? C39 C38 C40 O7 8.8(3) . . . . ? C34 C39 C41 O5 -89.1(3) . . . . ? C38 C39 C41 O5 88.8(3) . . . . ? C34 C39 C41 O6 83.5(3) . . . . ? C38 C39 C41 O6 -98.5(3) . . . . ? C23 C24 N1 C20 -1.5(4) . . . . ? C23 C24 N1 Cd2 -174.9(2) . . . . ? C21 C20 N1 C24 1.0(4) . . . . ? C19 C20 N1 C24 -175.5(2) . . . . ? C21 C20 N1 Cd2 174.92(18) . . . . ? C19 C20 N1 Cd2 -1.6(2) . . . . ? N2 Cd2 N1 C24 168.4(2) . . . . ? O1 Cd2 N1 C24 76.9(2) . . . . ? O3 Cd2 N1 C24 1.3(2) . . . . ? O5 Cd2 N1 C24 -108.0(2) 1_565 . . . ? N2 Cd2 N1 C20 -5.17(16) . . . . ? O1 Cd2 N1 C20 -96.71(17) . . . . ? O3 Cd2 N1 C20 -172.32(17) . . . . ? O5 Cd2 N1 C20 78.43(17) 1_565 . . . ? N3 C19 N2 C18 -0.1(3) . . . . ? C20 C19 N2 C18 176.2(2) . . . . ? N3 C19 N2 Cd2 165.57(15) . . . . ? C20 C19 N2 Cd2 -18.2(3) . . . . ? C17 C18 N2 C19 -0.6(3) . . . . ? C17 C18 N2 Cd2 -162.2(2) . . . . ? O1 Cd2 N2 C19 112.45(17) . . . . ? O3 Cd2 N2 C19 43.3(3) . . . . ? O1W Cd2 N2 C19 -162.25(16) . . . . ? O5 Cd2 N2 C19 -85.23(17) 1_565 . . . ? N1 Cd2 N2 C19 11.88(16) . . . . ? O1 Cd2 N2 C18 -87.1(2) . . . . ? O3 Cd2 N2 C18 -156.2(2) . . . . ? O1W Cd2 N2 C18 -1.8(3) . . . . ? O5 Cd2 N2 C18 75.2(2) 1_565 . . . ? N1 Cd2 N2 C18 172.3(3) . . . . ? N2 C19 N3 C17 0.7(3) . . . . ? C20 C19 N3 C17 -175.2(2) . . . . ? N2 C19 N3 C16 -173.6(2) . . . . ? C20 C19 N3 C16 10.5(4) . . . . ? C18 C17 N3 C19 -1.0(3) . . . . ? C18 C17 N3 C16 173.7(2) . . . . ? C14 C16 N3 C19 150.3(2) . . . . ? C14 C16 N3 C17 -23.2(3) . . . . ? N5 C6 N4 C7 1.1(3) . . . . ? C5 C6 N4 C7 -178.4(2) . . . . ? N5 C6 N4 Cd1 -173.80(14) . . . 2_556 ? C5 C6 N4 Cd1 6.7(3) . . . 2_556 ? C8 C7 N4 C6 -0.8(3) . . . . ? C8 C7 N4 Cd1 173.25(17) . . . 2_556 ? N4 C6 N5 C8 -1.0(3) . . . . ? C5 C6 N5 C8 178.5(2) . . . . ? N4 C6 N5 C9 -175.0(2) . . . . ? C5 C6 N5 C9 4.5(4) . . . . ? C7 C8 N5 C6 0.5(3) . . . . ? C7 C8 N5 C9 175.2(2) . . . . ? C10 C9 N5 C6 69.4(3) . . . . ? C10 C9 N5 C8 -103.9(3) . . . . ? C2 C1 N6 C5 1.9(4) . . . . ? C2 C1 N6 Cd1 -170.6(2) . . . 2_556 ? C4 C5 N6 C1 -2.3(4) . . . . ? C6 C5 N6 C1 179.5(2) . . . . ? C4 C5 N6 Cd1 170.73(18) . . . 2_556 ? C6 C5 N6 Cd1 -7.5(2) . . . 2_556 ? O2 C25 O1 Cd2 80.1(3) . . . . ? C28 C25 O1 Cd2 -103.3(2) . . . . ? N2 Cd2 O1 C25 -87.73(17) . . . . ? O3 Cd2 O1 C25 68.11(17) . . . . ? O1W Cd2 O1 C25 165.68(18) . . . . ? O5 Cd2 O1 C25 -179.5(2) 1_565 . . . ? N1 Cd2 O1 C25 -15.67(18) . . . . ? O4 C26 O3 Cd2 105.0(3) . . . . ? C27 C26 O3 Cd2 -79.3(3) . . . . ? N2 Cd2 O3 C26 103.6(3) . . . . ? O1 Cd2 O3 C26 30.5(2) . . . . ? O1W Cd2 O3 C26 -51.9(2) . . . . ? O5 Cd2 O3 C26 -132.2(2) 1_565 . . . ? N1 Cd2 O3 C26 133.2(2) . . . . ? O3 C26 O4 Cd1 -1.1(4) . . . 1_565 ? C27 C26 O4 Cd1 -176.87(15) . . . 1_565 ? O6 C41 O5 Cd2 158.77(16) . . . 1_545 ? C39 C41 O5 Cd2 -29.0(3) . . . 1_545 ? O5 C41 O6 Cd1 4.5(2) . . . 2_546 ? C39 C41 O6 Cd1 -167.78(16) . . . 2_546 ? O8 C40 O7 Cd1 14.4(3) . . . . ? C38 C40 O7 Cd1 -164.45(16) . . . . ? O4 Cd1 O7 C40 56.74(16) 1_545 . . . ? N4 Cd1 O7 C40 -119.9(2) 2_556 . . . ? O6 Cd1 O7 C40 150.92(15) 2_546 . . . ? N6 Cd1 O7 C40 -68.76(16) 2_556 . . . ? 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 H1A O6 0.891(10) 2.009(19) 2.803(3) 148(3) 2_556 O1W H1B O7 0.885(10) 1.86(3) 2.724(3) 165(3) 2_556 O2W H2A O2 0.91(4) 2.08(3) 2.937(5) 158(7) . _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.487 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.086 #===end data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H46 Cd2 N12 O9, 2(H2 O)' _chemical_formula_sum 'C32.50 H25 Cd N6 O5.50' _chemical_formula_weight 699.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.0950(14) _cell_length_b 10.8960(6) _cell_length_c 23.9680(13) _cell_angle_alpha 90.00 _cell_angle_beta 119.2840(10) _cell_angle_gamma 90.00 _cell_volume 5943.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16532 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18139 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7032 _reflns_number_gt 3857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7032 _refine_ls_number_parameters 413 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.184529(12) 0.22511(2) 0.639857(13) 0.03478(10) Uani 1 1 d . . . C1 C 0.1651(2) 0.0153(4) 0.5267(2) 0.0636(14) Uani 1 1 d . . . H1 H 0.1623 -0.0380 0.5554 0.076 Uiso 1 1 calc R . . C2 C 0.1688(3) -0.0333(4) 0.4756(2) 0.0766(16) Uani 1 1 d . . . H2 H 0.1671 -0.1177 0.4692 0.092 Uiso 1 1 calc R . . C3 C 0.1751(2) 0.0446(4) 0.4344(2) 0.0622(13) Uani 1 1 d . . . H3 H 0.1785 0.0136 0.4002 0.075 Uiso 1 1 calc R . . C4 C 0.17627(18) 0.1687(4) 0.44428(18) 0.0457(11) Uani 1 1 d . . . H4 H 0.1809 0.2230 0.4171 0.055 Uiso 1 1 calc R . . C5 C 0.17042(16) 0.2123(3) 0.49510(17) 0.0349(9) Uani 1 1 d . . . C6 C 0.17250(17) 0.3415(4) 0.51293(17) 0.0362(9) Uani 1 1 d . . . C7 C 0.18700(19) 0.4993(4) 0.5732(2) 0.0506(11) Uani 1 1 d . . . H7 H 0.1957 0.5471 0.6089 0.061 Uiso 1 1 calc R . . C8 C 0.17418(19) 0.5425(4) 0.5150(2) 0.0504(12) Uani 1 1 d . . . H8 H 0.1721 0.6246 0.5034 0.061 Uiso 1 1 calc R . . C9 C 0.14479(17) 0.4465(3) 0.40721(17) 0.0424(10) Uani 1 1 d . . . H9A H 0.1152 0.3836 0.3859 0.051 Uiso 1 1 calc R . . H9B H 0.1776 0.4282 0.4003 0.051 Uiso 1 1 calc R . . C10 C 0.11934(18) 0.5698(3) 0.37787(17) 0.0381(10) Uani 1 1 d . . . C11 C 0.15305(19) 0.6462(4) 0.36260(19) 0.0506(11) Uani 1 1 d . . . H11 H 0.1903 0.6209 0.3714 0.061 Uiso 1 1 calc R . . C12 C 0.1322(2) 0.7597(4) 0.3344(2) 0.0555(12) Uani 1 1 d . . . H12 H 0.1549 0.8108 0.3242 0.067 Uiso 1 1 calc R . . C13 C 0.0774(2) 0.7945(4) 0.3221(2) 0.0618(13) Uani 1 1 d . . . H13 H 0.0627 0.8702 0.3031 0.074 Uiso 1 1 calc R . . C14 C 0.04348(19) 0.7197(4) 0.33719(19) 0.0517(11) Uani 1 1 d . . . H14 H 0.0063 0.7459 0.3282 0.062 Uiso 1 1 calc R . . C15 C 0.06356(17) 0.6062(3) 0.36557(18) 0.0377(9) Uani 1 1 d . . . C16 C 0.02709(17) 0.5234(4) 0.3823(2) 0.0453(10) Uani 1 1 d . . . H16A H 0.0244 0.4436 0.3630 0.054 Uiso 1 1 calc R . . H16B H 0.0471 0.5122 0.4283 0.054 Uiso 1 1 calc R . . C17 C -0.0792(2) 0.5409(4) 0.3030(2) 0.0584(13) Uani 1 1 d . . . H17 H -0.0788 0.4904 0.2719 0.070 Uiso 1 1 calc R . . C18 C -0.12578(19) 0.6009(4) 0.2990(2) 0.0543(12) Uani 1 1 d . . . H18 H -0.1636 0.5972 0.2642 0.065 Uiso 1 1 calc R . . C19 C -0.05258(17) 0.6465(4) 0.39082(18) 0.0395(10) Uani 1 1 d . . . C20 C -0.01703(19) 0.6994(4) 0.4544(2) 0.0504(12) Uani 1 1 d . . . N6 N 0.0320(2) 0.6495(7) 0.4923(3) 0.174(3) Uani 1 1 d . . . C22 C 0.0652(3) 0.6993(9) 0.5504(4) 0.217(6) Uani 1 1 d . . . H22 H 0.1024 0.6660 0.5755 0.260 Uiso 1 1 calc R . . C23 C 0.0509(3) 0.7861(7) 0.5739(3) 0.142(3) Uani 1 1 d . . . H23 H 0.0743 0.8105 0.6162 0.170 Uiso 1 1 calc R . . C24 C 0.0007(4) 0.8414(9) 0.5355(4) 0.224(6) Uani 1 1 d . . . H24 H -0.0112 0.9096 0.5495 0.269 Uiso 1 1 calc R . . C25 C 0.16637(17) 0.0440(3) 0.7129(2) 0.0393(10) Uani 1 1 d . . . C26 C 0.20386(16) -0.2006(3) 0.79024(18) 0.0350(9) Uani 1 1 d . . . C27 C 0.12584(16) -0.0412(3) 0.72384(17) 0.0297(8) Uani 1 1 d . . . C28 C 0.14186(15) -0.1504(3) 0.75845(16) 0.0272(8) Uani 1 1 d . . . C29 C 0.10008(15) -0.2161(3) 0.76424(16) 0.0308(8) Uani 1 1 d . . . H29 H 0.1107 -0.2904 0.7861 0.037 Uiso 1 1 calc R . . C30 C 0.04268(15) -0.1766(3) 0.73897(17) 0.0315(9) Uani 1 1 d . . . C31 C 0.02698(17) -0.0680(3) 0.70404(18) 0.0393(10) Uani 1 1 d . . . H31 H -0.0114 -0.0392 0.6862 0.047 Uiso 1 1 calc R . . C32 C 0.06765(16) -0.0035(3) 0.69576(18) 0.0372(9) Uani 1 1 d . . . H32 H 0.0561 0.0672 0.6708 0.045 Uiso 1 1 calc R . . C33 C 0.0000 -0.2486(5) 0.7500 0.0397(14) Uani 1 2 d S . . N1 N 0.18507(14) 0.3746(3) 0.57114(14) 0.0417(8) Uani 1 1 d . . . N2 N 0.16486(13) 0.4430(3) 0.47603(14) 0.0364(8) Uani 1 1 d . . . N3 N 0.16543(14) 0.1358(3) 0.53631(15) 0.0436(9) Uani 1 1 d . . . N4 N -0.03237(14) 0.5684(3) 0.36157(15) 0.0440(9) Uani 1 1 d . . . N5 N -0.10989(14) 0.6683(3) 0.35328(15) 0.0433(8) Uani 1 1 d . . . C21 C -0.0344(3) 0.7958(7) 0.4731(3) 0.160(4) Uani 1 1 d . . . H21 H -0.0697 0.8340 0.4454 0.193 Uiso 1 1 calc R . . O1 O 0.19576(13) 0.1189(2) 0.75428(15) 0.0603(9) Uani 1 1 d . . . O2 O 0.16087(12) 0.0373(2) 0.65780(13) 0.0515(8) Uani 1 1 d . . . O3 O 0.24089(11) -0.1509(2) 0.77893(11) 0.0400(6) Uani 1 1 d . . . O4 O 0.21499(11) -0.2896(2) 0.82792(13) 0.0458(7) Uani 1 1 d . . . O5 O 0.0000 -0.3607(3) 0.7500 0.0534(12) Uani 1 2 d S . . O1W O 0.28003(19) 0.2875(4) 0.85334(15) 0.0822(11) Uani 1 1 d D . . H1A H 0.256(2) 0.240(4) 0.8240(17) 0.123 Uiso 1 1 d D . . H1B H 0.292(2) 0.342(4) 0.837(2) 0.123 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03282(15) 0.04043(17) 0.03468(15) -0.00075(15) 0.01929(12) -0.00504(15) C1 0.097(4) 0.043(3) 0.059(3) 0.007(2) 0.044(3) -0.006(3) C2 0.128(5) 0.038(3) 0.074(4) -0.011(3) 0.058(4) -0.004(3) C3 0.093(4) 0.051(3) 0.053(3) 0.001(2) 0.044(3) 0.012(3) C4 0.060(3) 0.040(2) 0.042(2) 0.004(2) 0.030(2) 0.012(2) C5 0.035(2) 0.037(2) 0.034(2) 0.0003(19) 0.0182(18) 0.0017(19) C6 0.042(2) 0.038(2) 0.034(2) 0.0047(19) 0.022(2) 0.0051(19) C7 0.064(3) 0.042(3) 0.042(3) -0.003(2) 0.023(2) 0.008(2) C8 0.065(3) 0.036(2) 0.050(3) -0.001(2) 0.028(3) 0.007(2) C9 0.047(3) 0.052(3) 0.036(2) 0.0074(19) 0.027(2) 0.014(2) C10 0.047(2) 0.040(2) 0.028(2) 0.0064(17) 0.018(2) 0.006(2) C11 0.051(3) 0.061(3) 0.049(3) 0.009(2) 0.031(2) 0.011(2) C12 0.078(3) 0.048(3) 0.057(3) 0.006(2) 0.046(3) -0.003(3) C13 0.092(4) 0.043(3) 0.062(3) 0.016(2) 0.046(3) 0.021(3) C14 0.052(3) 0.052(3) 0.054(3) 0.011(2) 0.028(2) 0.017(2) C15 0.040(2) 0.037(2) 0.040(2) 0.0047(19) 0.022(2) 0.008(2) C16 0.042(2) 0.046(3) 0.053(3) 0.003(2) 0.028(2) 0.011(2) C17 0.056(3) 0.071(3) 0.044(3) -0.019(2) 0.021(3) 0.011(3) C18 0.039(3) 0.075(3) 0.040(3) -0.013(2) 0.012(2) 0.006(2) C19 0.037(2) 0.046(3) 0.041(2) -0.0006(19) 0.023(2) 0.005(2) C20 0.035(2) 0.071(3) 0.043(2) -0.013(2) 0.017(2) 0.004(2) N6 0.097(4) 0.262(8) 0.082(4) -0.092(5) -0.019(3) 0.085(5) C22 0.101(6) 0.365(13) 0.104(6) -0.122(8) -0.013(5) 0.109(8) C23 0.082(5) 0.206(8) 0.084(5) -0.083(5) -0.001(4) 0.034(5) C24 0.124(7) 0.313(12) 0.144(8) -0.159(8) -0.006(6) 0.082(8) C25 0.041(2) 0.031(2) 0.056(3) 0.002(2) 0.032(2) 0.0059(19) C26 0.030(2) 0.040(3) 0.034(2) -0.0089(18) 0.0149(18) -0.0040(18) C27 0.034(2) 0.029(2) 0.035(2) -0.0030(16) 0.0233(19) -0.0026(17) C28 0.027(2) 0.030(2) 0.0278(19) -0.0023(16) 0.0165(17) -0.0010(17) C29 0.033(2) 0.0285(19) 0.0349(19) 0.0032(17) 0.0196(17) 0.0066(18) C30 0.031(2) 0.031(2) 0.039(2) -0.0008(17) 0.0224(19) 0.0024(17) C31 0.032(2) 0.041(2) 0.047(2) 0.008(2) 0.022(2) 0.0090(19) C32 0.041(2) 0.032(2) 0.044(2) 0.0114(18) 0.025(2) 0.0092(19) C33 0.030(3) 0.050(4) 0.039(3) 0.000 0.017(3) 0.000 N1 0.053(2) 0.039(2) 0.0332(18) -0.0021(15) 0.0209(17) 0.0039(17) N2 0.044(2) 0.0322(18) 0.0332(18) 0.0051(15) 0.0192(17) 0.0069(15) N3 0.058(2) 0.037(2) 0.040(2) 0.0037(16) 0.0271(19) -0.0031(17) N4 0.037(2) 0.053(2) 0.044(2) -0.0016(17) 0.0211(18) 0.0103(17) N5 0.039(2) 0.051(2) 0.044(2) -0.0029(17) 0.0237(18) 0.0078(17) C21 0.077(5) 0.233(9) 0.114(6) -0.104(6) 0.002(4) 0.049(5) O1 0.065(2) 0.0473(18) 0.082(2) -0.0285(17) 0.0471(19) -0.0277(17) O2 0.0587(19) 0.0565(19) 0.0521(19) 0.0056(15) 0.0370(16) -0.0080(15) O3 0.0303(15) 0.0540(17) 0.0406(15) 0.0029(13) 0.0213(13) 0.0011(13) O4 0.0339(15) 0.0483(18) 0.0563(18) 0.0140(15) 0.0229(14) 0.0062(14) O5 0.059(3) 0.030(2) 0.097(3) 0.000 0.058(3) 0.000 O1W 0.093(3) 0.093(3) 0.058(2) -0.002(2) 0.035(2) -0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.239(3) . ? Cd1 N1 2.322(3) . ? Cd1 N5 2.342(3) 5_566 ? Cd1 O4 2.349(2) 4_556 ? Cd1 O3 2.386(2) 4_556 ? Cd1 N3 2.479(3) . ? Cd1 C26 2.678(4) 4_556 ? C1 N3 1.333(5) . ? C1 C2 1.381(6) . ? C1 H1 0.9300 . ? C2 C3 1.370(6) . ? C2 H2 0.9300 . ? C3 C4 1.371(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 N3 1.347(4) . ? C5 C6 1.465(5) . ? C6 N1 1.318(4) . ? C6 N2 1.368(4) . ? C7 C8 1.351(5) . ? C7 N1 1.359(5) . ? C7 H7 0.9300 . ? C8 N2 1.373(5) . ? C8 H8 0.9300 . ? C9 N2 1.467(4) . ? C9 C10 1.511(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.384(5) . ? C10 C15 1.394(5) . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 C13 1.363(6) . ? C12 H12 0.9300 . ? C13 C14 1.376(6) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 H14 0.9300 . ? C15 C16 1.501(5) . ? C16 N4 1.463(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.341(5) . ? C17 N4 1.370(5) . ? C17 H17 0.9300 . ? C18 N5 1.370(5) . ? C18 H18 0.9300 . ? C19 N5 1.337(4) . ? C19 N4 1.362(5) . ? C19 C20 1.460(5) . ? C20 N6 1.273(6) . ? C20 C21 1.307(7) . ? N6 C22 1.343(7) . ? C22 C23 1.247(8) . ? C22 H22 0.9300 . ? C23 C24 1.321(9) . ? C23 H23 0.9300 . ? C24 C21 1.408(8) . ? C24 H24 0.9300 . ? C25 O1 1.222(4) . ? C25 O2 1.260(5) . ? C25 C27 1.522(5) . ? C26 O3 1.248(4) . ? C26 O4 1.258(4) . ? C26 C28 1.514(5) . ? C26 Cd1 2.678(4) 4_546 ? C27 C32 1.389(5) . ? C27 C28 1.393(5) . ? C28 C29 1.367(5) . ? C29 C30 1.381(5) . ? C29 H29 0.9300 . ? C30 C31 1.391(5) . ? C30 C33 1.488(4) . ? C31 C32 1.366(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O5 1.222(6) . ? C33 C30 1.488(4) 2_556 ? N5 Cd1 2.342(3) 5_566 ? C21 H21 0.9300 . ? O3 Cd1 2.386(2) 4_546 ? O4 Cd1 2.349(2) 4_546 ? O1W H1A 0.85(4) . ? O1W H1B 0.85(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 N1 151.11(11) . . ? O2 Cd1 N5 97.05(11) . 5_566 ? N1 Cd1 N5 89.76(11) . 5_566 ? O2 Cd1 O4 104.07(10) . 4_556 ? N1 Cd1 O4 83.56(10) . 4_556 ? N5 Cd1 O4 147.55(10) 5_566 4_556 ? O2 Cd1 O3 123.51(9) . 4_556 ? N1 Cd1 O3 84.03(10) . 4_556 ? N5 Cd1 O3 92.09(10) 5_566 4_556 ? O4 Cd1 O3 55.70(9) 4_556 4_556 ? O2 Cd1 N3 83.93(10) . . ? N1 Cd1 N3 68.48(11) . . ? N5 Cd1 N3 119.88(11) 5_566 . ? O4 Cd1 N3 87.01(10) 4_556 . ? O3 Cd1 N3 136.32(10) 4_556 . ? O2 Cd1 C26 118.29(10) . 4_556 ? N1 Cd1 C26 81.34(11) . 4_556 ? N5 Cd1 C26 119.58(12) 5_566 4_556 ? O4 Cd1 C26 28.02(10) 4_556 4_556 ? O3 Cd1 C26 27.76(9) 4_556 4_556 ? N3 Cd1 C26 111.69(11) . 4_556 ? N3 C1 C2 122.2(4) . . ? N3 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N3 C5 C4 121.7(4) . . ? N3 C5 C6 112.6(3) . . ? C4 C5 C6 125.6(4) . . ? N1 C6 N2 110.2(3) . . ? N1 C6 C5 121.8(3) . . ? N2 C6 C5 128.0(3) . . ? C8 C7 N1 108.9(4) . . ? C8 C7 H7 125.5 . . ? N1 C7 H7 125.5 . . ? C7 C8 N2 107.4(4) . . ? C7 C8 H8 126.3 . . ? N2 C8 H8 126.3 . . ? N2 C9 C10 112.4(3) . . ? N2 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N2 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C15 120.4(4) . . ? C11 C10 C9 117.8(4) . . ? C15 C10 C9 121.8(4) . . ? C10 C11 C12 121.0(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 118.3(4) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C10 117.6(4) . . ? C14 C15 C16 122.1(4) . . ? C10 C15 C16 120.4(3) . . ? N4 C16 C15 114.4(3) . . ? N4 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? N4 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 N4 106.8(4) . . ? C18 C17 H17 126.6 . . ? N4 C17 H17 126.6 . . ? C17 C18 N5 110.5(4) . . ? C17 C18 H18 124.7 . . ? N5 C18 H18 124.7 . . ? N5 C19 N4 110.6(3) . . ? N5 C19 C20 124.3(4) . . ? N4 C19 C20 125.1(4) . . ? N6 C20 C21 119.6(5) . . ? N6 C20 C19 118.7(4) . . ? C21 C20 C19 121.7(5) . . ? C20 N6 C22 118.8(6) . . ? C23 C22 N6 126.1(7) . . ? C23 C22 H22 116.9 . . ? N6 C22 H22 116.9 . . ? C22 C23 C24 116.5(7) . . ? C22 C23 H23 121.8 . . ? C24 C23 H23 121.8 . . ? C23 C24 C21 119.2(7) . . ? C23 C24 H24 120.4 . . ? C21 C24 H24 120.4 . . ? O1 C25 O2 126.4(4) . . ? O1 C25 C27 118.8(4) . . ? O2 C25 C27 114.4(4) . . ? O3 C26 O4 124.0(3) . . ? O3 C26 C28 119.0(3) . . ? O4 C26 C28 117.0(3) . . ? O3 C26 Cd1 63.00(19) . 4_546 ? O4 C26 Cd1 61.28(18) . 4_546 ? C28 C26 Cd1 172.6(3) . 4_546 ? C32 C27 C28 118.7(3) . . ? C32 C27 C25 115.0(3) . . ? C28 C27 C25 126.3(3) . . ? C29 C28 C27 119.1(3) . . ? C29 C28 C26 118.0(3) . . ? C27 C28 C26 122.9(3) . . ? C28 C29 C30 122.7(3) . . ? C28 C29 H29 118.6 . . ? C30 C29 H29 118.6 . . ? C29 C30 C31 117.8(3) . . ? C29 C30 C33 120.2(3) . . ? C31 C30 C33 122.0(3) . . ? C32 C31 C30 120.3(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C27 121.4(3) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? O5 C33 C30 121.8(2) . . ? O5 C33 C30 121.8(2) . 2_556 ? C30 C33 C30 116.4(5) . 2_556 ? C6 N1 C7 107.3(3) . . ? C6 N1 Cd1 118.3(3) . . ? C7 N1 Cd1 133.5(3) . . ? C6 N2 C8 106.1(3) . . ? C6 N2 C9 127.4(3) . . ? C8 N2 C9 126.2(3) . . ? C1 N3 C5 118.6(4) . . ? C1 N3 Cd1 122.7(3) . . ? C5 N3 Cd1 116.6(2) . . ? C19 N4 C17 106.8(3) . . ? C19 N4 C16 130.4(3) . . ? C17 N4 C16 122.8(3) . . ? C19 N5 C18 105.3(3) . . ? C19 N5 Cd1 137.4(3) . 5_566 ? C18 N5 Cd1 117.2(3) . 5_566 ? C20 C21 C24 119.5(6) . . ? C20 C21 H21 120.2 . . ? C24 C21 H21 120.2 . . ? C25 O2 Cd1 104.4(2) . . ? C26 O3 Cd1 89.2(2) . 4_546 ? C26 O4 Cd1 90.7(2) . 4_546 ? H1A O1W H1B 109(4) . . ? 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 C1 C2 C3 2.3(8) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C3 C4 C5 N3 2.1(6) . . . . ? C3 C4 C5 C6 178.1(4) . . . . ? N3 C5 C6 N1 18.1(5) . . . . ? C4 C5 C6 N1 -158.2(4) . . . . ? N3 C5 C6 N2 -164.8(4) . . . . ? C4 C5 C6 N2 18.9(6) . . . . ? N1 C7 C8 N2 -0.8(5) . . . . ? N2 C9 C10 C11 105.1(4) . . . . ? N2 C9 C10 C15 -75.7(5) . . . . ? C15 C10 C11 C12 -0.5(6) . . . . ? C9 C10 C11 C12 178.8(4) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C14 0.2(7) . . . . ? C12 C13 C14 C15 0.0(7) . . . . ? C13 C14 C15 C10 -0.5(6) . . . . ? C13 C14 C15 C16 -179.9(4) . . . . ? C11 C10 C15 C14 0.7(6) . . . . ? C9 C10 C15 C14 -178.5(3) . . . . ? C11 C10 C15 C16 -179.9(4) . . . . ? C9 C10 C15 C16 0.9(6) . . . . ? C14 C15 C16 N4 4.6(6) . . . . ? C10 C15 C16 N4 -174.8(3) . . . . ? N4 C17 C18 N5 1.1(5) . . . . ? N5 C19 C20 N6 161.9(6) . . . . ? N4 C19 C20 N6 -18.0(8) . . . . ? N5 C19 C20 C21 -17.9(8) . . . . ? N4 C19 C20 C21 162.2(6) . . . . ? C21 C20 N6 C22 -1.3(13) . . . . ? C19 C20 N6 C22 178.9(8) . . . . ? C20 N6 C22 C23 6.1(19) . . . . ? N6 C22 C23 C24 -7(2) . . . . ? C22 C23 C24 C21 3.6(18) . . . . ? O1 C25 C27 C32 96.9(4) . . . . ? O2 C25 C27 C32 -75.8(4) . . . . ? O1 C25 C27 C28 -83.3(5) . . . . ? O2 C25 C27 C28 104.1(4) . . . . ? C32 C27 C28 C29 -0.7(5) . . . . ? C25 C27 C28 C29 179.4(3) . . . . ? C32 C27 C28 C26 179.2(3) . . . . ? C25 C27 C28 C26 -0.6(6) . . . . ? O3 C26 C28 C29 171.0(3) . . . . ? O4 C26 C28 C29 -10.4(5) . . . . ? O3 C26 C28 C27 -9.0(5) . . . . ? O4 C26 C28 C27 169.6(3) . . . . ? C27 C28 C29 C30 -2.3(5) . . . . ? C26 C28 C29 C30 177.8(3) . . . . ? C28 C29 C30 C31 2.8(5) . . . . ? C28 C29 C30 C33 -176.5(3) . . . . ? C29 C30 C31 C32 -0.3(6) . . . . ? C33 C30 C31 C32 179.0(3) . . . . ? C30 C31 C32 C27 -2.7(6) . . . . ? C28 C27 C32 C31 3.2(6) . . . . ? C25 C27 C32 C31 -177.0(4) . . . . ? C29 C30 C33 O5 -38.2(4) . . . . ? C31 C30 C33 O5 142.5(3) . . . . ? C29 C30 C33 C30 141.8(4) . . . 2_556 ? C31 C30 C33 C30 -37.5(3) . . . 2_556 ? N2 C6 N1 C7 -1.3(5) . . . . ? C5 C6 N1 C7 176.3(4) . . . . ? N2 C6 N1 Cd1 169.5(2) . . . . ? C5 C6 N1 Cd1 -12.9(5) . . . . ? C8 C7 N1 C6 1.3(5) . . . . ? C8 C7 N1 Cd1 -167.5(3) . . . . ? O2 Cd1 N1 C6 -14.8(4) . . . . ? N5 Cd1 N1 C6 -119.0(3) 5_566 . . . ? O4 Cd1 N1 C6 92.8(3) 4_556 . . . ? O3 Cd1 N1 C6 148.8(3) 4_556 . . . ? N3 Cd1 N1 C6 3.5(3) . . . . ? C26 Cd1 N1 C6 121.0(3) 4_556 . . . ? O2 Cd1 N1 C7 153.0(3) . . . . ? N5 Cd1 N1 C7 48.8(4) 5_566 . . . ? O4 Cd1 N1 C7 -99.4(4) 4_556 . . . ? O3 Cd1 N1 C7 -43.4(4) 4_556 . . . ? N3 Cd1 N1 C7 171.3(4) . . . . ? C26 Cd1 N1 C7 -71.2(4) 4_556 . . . ? N1 C6 N2 C8 0.8(4) . . . . ? C5 C6 N2 C8 -176.6(4) . . . . ? N1 C6 N2 C9 -173.4(3) . . . . ? C5 C6 N2 C9 9.2(6) . . . . ? C7 C8 N2 C6 0.1(5) . . . . ? C7 C8 N2 C9 174.3(4) . . . . ? C10 C9 N2 C6 157.8(4) . . . . ? C10 C9 N2 C8 -15.3(6) . . . . ? C2 C1 N3 C5 -1.0(7) . . . . ? C2 C1 N3 Cd1 -163.8(4) . . . . ? C4 C5 N3 C1 -1.2(6) . . . . ? C6 C5 N3 C1 -177.7(4) . . . . ? C4 C5 N3 Cd1 162.7(3) . . . . ? C6 C5 N3 Cd1 -13.8(4) . . . . ? O2 Cd1 N3 C1 -19.3(3) . . . . ? N1 Cd1 N3 C1 169.4(4) . . . . ? N5 Cd1 N3 C1 -114.0(3) 5_566 . . . ? O4 Cd1 N3 C1 85.2(3) 4_556 . . . ? O3 Cd1 N3 C1 114.5(3) 4_556 . . . ? C26 Cd1 N3 C1 98.8(3) 4_556 . . . ? O2 Cd1 N3 C5 177.5(3) . . . . ? N1 Cd1 N3 C5 6.3(3) . . . . ? N5 Cd1 N3 C5 82.9(3) 5_566 . . . ? O4 Cd1 N3 C5 -78.0(3) 4_556 . . . ? O3 Cd1 N3 C5 -48.6(3) 4_556 . . . ? C26 Cd1 N3 C5 -64.4(3) 4_556 . . . ? N5 C19 N4 C17 0.4(5) . . . . ? C20 C19 N4 C17 -179.7(4) . . . . ? N5 C19 N4 C16 176.6(4) . . . . ? C20 C19 N4 C16 -3.5(7) . . . . ? C18 C17 N4 C19 -0.9(5) . . . . ? C18 C17 N4 C16 -177.4(4) . . . . ? C15 C16 N4 C19 -85.8(5) . . . . ? C15 C16 N4 C17 89.8(5) . . . . ? N4 C19 N5 C18 0.3(5) . . . . ? C20 C19 N5 C18 -179.6(4) . . . . ? N4 C19 N5 Cd1 175.6(3) . . . 5_566 ? C20 C19 N5 Cd1 -4.3(7) . . . 5_566 ? C17 C18 N5 C19 -0.9(5) . . . . ? C17 C18 N5 Cd1 -177.3(3) . . . 5_566 ? N6 C20 C21 C24 -1.5(13) . . . . ? C19 C20 C21 C24 178.3(8) . . . . ? C23 C24 C21 C20 0.4(17) . . . . ? O1 C25 O2 Cd1 -21.6(5) . . . . ? C27 C25 O2 Cd1 150.4(2) . . . . ? N1 Cd1 O2 C25 -163.8(2) . . . . ? N5 Cd1 O2 C25 -61.4(3) 5_566 . . . ? O4 Cd1 O2 C25 93.8(3) 4_556 . . . ? O3 Cd1 O2 C25 35.9(3) 4_556 . . . ? N3 Cd1 O2 C25 179.2(3) . . . . ? C26 Cd1 O2 C25 67.8(3) 4_556 . . . ? O4 C26 O3 Cd1 -6.5(4) . . . 4_546 ? C28 C26 O3 Cd1 172.0(3) . . . 4_546 ? O3 C26 O4 Cd1 6.6(4) . . . 4_546 ? C28 C26 O4 Cd1 -171.9(3) . . . 4_546 ? 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 H1A O1 0.85(4) 2.11(4) 2.957(4) 177(5) . O1W H1B O3 0.85(5) 2.47(4) 3.017(4) 123(4) 4_556 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.744 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.093