# Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Huai-Ming Hu' _publ_contact_author_email CHEMHU1@NWU.EDU.CN _publ_section_title ; Four novel Zn(II)/Cd(II) metal-organic frameworks constructed from 4'-(4-pyridyl)-4,2':6',4''-terpyridine: hydrothermal synthesis, crystal structures, and luminescent properties ; loop_ _publ_author_name 'Huai-Ming Hu' 'Xiao-Li Chen' 'Yi-Qing Shangguan' 'Bao-Cheng Wang' ; Qing-Ran Wu ; 'Ganglin Xue' 'Meng-Lin Yang' 'Zhen-Hua Yang' # Attachment 'complex1.cif' data_nw0282 _database_code_depnum_ccdc_archive 'CCDC 722288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 Cl2 N4 Zn' _chemical_formula_weight 446.62 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4268(13) _cell_length_b 20.661(3) _cell_length_c 11.3627(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.242(2) _cell_angle_gamma 90.00 _cell_volume 1946.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2647 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 23.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7881 _exptl_absorpt_correction_T_max 0.8606 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9519 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3431 _reflns_number_gt 2580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.8022P] 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 3431 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.71637(5) 0.78676(2) 0.41830(4) 0.06297(17) Uani 1 1 d . . . Cl1 Cl 0.91489(13) 0.74598(5) 0.33366(9) 0.0750(3) Uani 1 1 d . . . Cl2 Cl 0.76811(16) 0.84692(5) 0.58131(9) 0.0896(4) Uani 1 1 d . . . N1 N 0.5760(3) 0.71200(13) 0.4612(2) 0.0536(7) Uani 1 1 d . . . N2 N 0.2508(3) 0.50709(13) 0.4757(2) 0.0472(6) Uani 1 1 d . . . N3 N -0.0826(4) 0.33927(14) 0.2186(2) 0.0560(7) Uani 1 1 d . . . N4 N 0.3232(4) 0.41724(19) 1.0842(3) 0.0732(9) Uani 1 1 d . . . C1 C 0.5883(5) 0.69463(17) 0.5758(3) 0.0580(9) Uani 1 1 d . . . H1 H 0.6507 0.7201 0.6339 0.070 Uiso 1 1 calc R . . C2 C 0.5132(4) 0.64088(16) 0.6119(3) 0.0545(9) Uani 1 1 d . . . H2 H 0.5266 0.6306 0.6928 0.065 Uiso 1 1 calc R . . C3 C 0.4178(4) 0.60198(15) 0.5288(3) 0.0432(7) Uani 1 1 d . . . C4 C 0.4043(5) 0.62033(18) 0.4101(3) 0.0620(10) Uani 1 1 d . . . H4 H 0.3417 0.5960 0.3503 0.074 Uiso 1 1 calc R . . C5 C 0.4834(5) 0.6744(2) 0.3808(3) 0.0696(11) Uani 1 1 d . . . H5 H 0.4721 0.6855 0.3004 0.084 Uiso 1 1 calc R . . C6 C 0.3363(4) 0.54332(15) 0.5639(3) 0.0420(7) Uani 1 1 d . . . C7 C 0.3464(4) 0.52636(15) 0.6828(3) 0.0434(7) Uani 1 1 d . . . H7 H 0.4064 0.5518 0.7422 0.052 Uiso 1 1 calc R . . C8 C 0.2680(4) 0.47204(15) 0.7140(3) 0.0452(8) Uani 1 1 d . . . C9 C 0.1801(4) 0.43549(15) 0.6231(3) 0.0437(7) Uani 1 1 d . . . H9 H 0.1256 0.3987 0.6413 0.052 Uiso 1 1 calc R . . C10 C 0.1734(4) 0.45356(14) 0.5054(3) 0.0410(7) Uani 1 1 d . . . C11 C -0.0890(5) 0.32598(17) 0.3326(3) 0.0598(10) Uani 1 1 d . . . H11 H -0.1504 0.2908 0.3490 0.072 Uiso 1 1 calc R . . C12 C -0.0099(4) 0.36144(16) 0.4266(3) 0.0534(9) Uani 1 1 d . . . H12 H -0.0177 0.3501 0.5046 0.064 Uiso 1 1 calc R . . C13 C 0.0818(4) 0.41438(15) 0.4054(3) 0.0423(7) Uani 1 1 d . . . C14 C 0.0872(4) 0.42917(19) 0.2876(3) 0.0606(10) Uani 1 1 d . . . H14 H 0.1459 0.4647 0.2689 0.073 Uiso 1 1 calc R . . C15 C 0.0043(5) 0.3906(2) 0.1979(3) 0.0664(11) Uani 1 1 d . . . H15 H 0.0094 0.4009 0.1190 0.080 Uiso 1 1 calc R . . C16 C 0.3139(5) 0.4784(2) 1.0493(3) 0.0677(11) Uani 1 1 d . . . H16 H 0.3209 0.5100 1.1082 0.081 Uiso 1 1 calc R . . C17 C 0.2944(4) 0.49873(18) 0.9320(3) 0.0572(9) Uani 1 1 d . . . H17 H 0.2913 0.5426 0.9136 0.069 Uiso 1 1 calc R . . C18 C 0.2796(4) 0.45275(16) 0.8420(3) 0.0473(8) Uani 1 1 d . . . C19 C 0.2827(5) 0.38834(18) 0.8764(3) 0.0644(10) Uani 1 1 d . . . H19 H 0.2693 0.3554 0.8196 0.077 Uiso 1 1 calc R . . C20 C 0.3065(5) 0.3742(2) 0.9978(4) 0.0749(12) Uani 1 1 d . . . H20 H 0.3108 0.3307 1.0197 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0737(3) 0.0609(3) 0.0487(3) 0.0192(2) -0.0045(2) -0.0123(2) Cl1 0.0797(7) 0.0676(6) 0.0760(7) 0.0245(5) 0.0092(5) -0.0001(5) Cl2 0.1308(10) 0.0736(7) 0.0536(6) 0.0095(5) -0.0130(6) -0.0247(7) N1 0.0631(18) 0.0550(17) 0.0397(15) 0.0096(13) 0.0010(13) -0.0069(14) N2 0.0492(16) 0.0504(16) 0.0408(15) -0.0004(12) 0.0046(12) 0.0031(13) N3 0.0599(19) 0.0606(19) 0.0446(17) -0.0139(14) 0.0013(14) 0.0036(15) N4 0.085(2) 0.088(3) 0.0492(19) 0.0058(19) 0.0174(17) 0.003(2) C1 0.078(3) 0.056(2) 0.0373(18) 0.0008(16) 0.0018(17) -0.0154(19) C2 0.078(2) 0.055(2) 0.0292(17) 0.0024(15) 0.0051(16) -0.0106(18) C3 0.0488(19) 0.0483(19) 0.0316(16) 0.0003(14) 0.0052(14) 0.0006(15) C4 0.077(3) 0.070(2) 0.0355(18) -0.0001(17) 0.0004(17) -0.022(2) C5 0.086(3) 0.083(3) 0.0351(19) 0.0126(19) -0.0029(19) -0.021(2) C6 0.0434(18) 0.0433(18) 0.0375(17) -0.0032(14) 0.0026(14) 0.0012(14) C7 0.0493(19) 0.0429(18) 0.0365(17) -0.0033(14) 0.0036(14) -0.0066(14) C8 0.0465(19) 0.0452(19) 0.0426(18) -0.0009(14) 0.0041(15) 0.0042(15) C9 0.0499(19) 0.0389(17) 0.0410(18) 0.0001(14) 0.0046(15) -0.0047(14) C10 0.0403(17) 0.0404(17) 0.0410(18) 0.0002(14) 0.0043(14) 0.0015(14) C11 0.081(3) 0.046(2) 0.047(2) -0.0004(16) -0.0054(18) -0.0038(18) C12 0.073(2) 0.046(2) 0.0366(18) 0.0018(15) -0.0018(16) -0.0022(17) C13 0.0446(18) 0.0445(18) 0.0364(17) -0.0016(14) 0.0029(14) 0.0055(14) C14 0.060(2) 0.080(3) 0.042(2) -0.0015(18) 0.0098(17) -0.0182(19) C15 0.064(2) 0.098(3) 0.038(2) -0.0068(19) 0.0104(18) -0.007(2) C16 0.077(3) 0.082(3) 0.044(2) -0.006(2) 0.0110(19) -0.004(2) C17 0.068(2) 0.055(2) 0.047(2) -0.0014(17) 0.0056(17) -0.0046(18) C18 0.049(2) 0.048(2) 0.0431(18) 0.0025(15) 0.0043(15) -0.0018(15) C19 0.085(3) 0.056(2) 0.052(2) 0.0015(18) 0.013(2) -0.003(2) C20 0.099(3) 0.067(3) 0.061(3) 0.021(2) 0.020(2) 0.006(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 N1 2.056(3) . ? Zn1 N3 2.060(3) 2 ? Zn1 Cl2 2.2088(12) . ? Zn1 Cl1 2.2373(12) . ? N1 C1 1.336(4) . ? N1 C5 1.340(4) . ? N2 C6 1.352(4) . ? N2 C10 1.357(4) . ? N3 C15 1.332(5) . ? N3 C11 1.335(4) . ? N3 Zn1 2.060(3) 2_545 ? N4 C20 1.314(5) . ? N4 C16 1.323(5) . ? C1 C2 1.376(4) . ? C1 H1 0.9300 . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.386(4) . ? C3 C6 1.482(4) . ? C4 C5 1.371(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.383(4) . ? C7 C8 1.380(4) . ? C7 H7 0.9300 . ? C8 C9 1.384(4) . ? C8 C18 1.494(4) . ? C9 C10 1.380(4) . ? C9 H9 0.9300 . ? C10 C13 1.493(4) . ? C11 C12 1.367(4) . ? C11 H11 0.9300 . ? C12 C13 1.385(4) . ? C12 H12 0.9300 . ? C13 C14 1.381(4) . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.379(5) . ? C16 H16 0.9300 . ? C17 C18 1.385(4) . ? C17 H17 0.9300 . ? C18 C19 1.386(5) . ? C19 C20 1.390(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N3 108.31(11) . 2 ? N1 Zn1 Cl2 105.07(8) . . ? N3 Zn1 Cl2 109.67(9) 2 . ? N1 Zn1 Cl1 108.96(9) . . ? N3 Zn1 Cl1 102.96(9) 2 . ? Cl2 Zn1 Cl1 121.41(5) . . ? C1 N1 C5 116.4(3) . . ? C1 N1 Zn1 119.0(2) . . ? C5 N1 Zn1 124.3(2) . . ? C6 N2 C10 119.0(3) . . ? C15 N3 C11 116.9(3) . . ? C15 N3 Zn1 122.0(2) . 2_545 ? C11 N3 Zn1 120.9(3) . 2_545 ? C20 N4 C16 115.5(3) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.5(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 116.3(3) . . ? C2 C3 C6 122.1(3) . . ? C4 C3 C6 121.6(3) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 123.8(3) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N2 C6 C7 121.0(3) . . ? N2 C6 C3 117.7(3) . . ? C7 C6 C3 121.3(3) . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 118.0(3) . . ? C7 C8 C18 121.0(3) . . ? C9 C8 C18 121.0(3) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 121.5(3) . . ? N2 C10 C13 117.4(3) . . ? C9 C10 C13 121.1(3) . . ? N3 C11 C12 123.4(3) . . ? N3 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 119.8(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 117.3(3) . . ? C14 C13 C10 121.0(3) . . ? C12 C13 C10 121.7(3) . . ? C13 C14 C15 119.2(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 123.4(3) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N4 C16 C17 124.9(4) . . ? N4 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C16 C17 C18 119.0(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 117.1(3) . . ? C17 C18 C8 121.2(3) . . ? C19 C18 C8 121.7(3) . . ? C18 C19 C20 118.3(4) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 125.2(4) . . ? N4 C20 H20 117.4 . . ? C19 C20 H20 117.4 . . ? 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 Zn1 N1 C1 -142.9(3) 2 . . . ? Cl2 Zn1 N1 C1 -25.7(3) . . . . ? Cl1 Zn1 N1 C1 105.8(3) . . . . ? N3 Zn1 N1 C5 44.4(3) 2 . . . ? Cl2 Zn1 N1 C5 161.5(3) . . . . ? Cl1 Zn1 N1 C5 -66.9(3) . . . . ? C5 N1 C1 C2 0.8(6) . . . . ? Zn1 N1 C1 C2 -172.6(3) . . . . ? N1 C1 C2 C3 -0.7(6) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C1 C2 C3 C6 179.3(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C6 C3 C4 C5 -179.0(3) . . . . ? C1 N1 C5 C4 -0.4(6) . . . . ? Zn1 N1 C5 C4 172.5(3) . . . . ? C3 C4 C5 N1 0.0(6) . . . . ? C10 N2 C6 C7 0.3(4) . . . . ? C10 N2 C6 C3 -179.2(3) . . . . ? C2 C3 C6 N2 -177.5(3) . . . . ? C4 C3 C6 N2 1.5(5) . . . . ? C2 C3 C6 C7 2.9(5) . . . . ? C4 C3 C6 C7 -178.0(3) . . . . ? N2 C6 C7 C8 -0.4(5) . . . . ? C3 C6 C7 C8 179.1(3) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C6 C7 C8 C18 179.2(3) . . . . ? C7 C8 C9 C10 0.3(5) . . . . ? C18 C8 C9 C10 -178.8(3) . . . . ? C6 N2 C10 C9 0.1(4) . . . . ? C6 N2 C10 C13 -179.3(3) . . . . ? C8 C9 C10 N2 -0.4(5) . . . . ? C8 C9 C10 C13 178.9(3) . . . . ? C15 N3 C11 C12 -1.0(5) . . . . ? Zn1 N3 C11 C12 -176.3(3) 2_545 . . . ? N3 C11 C12 C13 0.4(6) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C11 C12 C13 C10 -178.5(3) . . . . ? N2 C10 C13 C14 5.3(4) . . . . ? C9 C10 C13 C14 -174.0(3) . . . . ? N2 C10 C13 C12 -175.6(3) . . . . ? C9 C10 C13 C12 5.1(5) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? C10 C13 C14 C15 178.2(3) . . . . ? C11 N3 C15 C14 0.6(6) . . . . ? Zn1 N3 C15 C14 175.9(3) 2_545 . . . ? C13 C14 C15 N3 0.3(6) . . . . ? C20 N4 C16 C17 -2.5(6) . . . . ? N4 C16 C17 C18 1.5(6) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C16 C17 C18 C8 -176.4(3) . . . . ? C7 C8 C18 C17 32.4(5) . . . . ? C9 C8 C18 C17 -148.5(3) . . . . ? C7 C8 C18 C19 -144.9(3) . . . . ? C9 C8 C18 C19 34.2(5) . . . . ? C17 C18 C19 C20 -2.4(5) . . . . ? C8 C18 C19 C20 175.0(3) . . . . ? C16 N4 C20 C19 1.0(6) . . . . ? C18 C19 C20 N4 1.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.377 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.049 # Attachment 'complex2.cif' data_nw0237 _database_code_depnum_ccdc_archive 'CCDC 722289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H30 N8 O9 Zn2' _chemical_formula_weight 945.50 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.694(7) _cell_length_b 9.283(3) _cell_length_c 17.354(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.759(4) _cell_angle_gamma 90.00 _cell_volume 4194(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3403 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7280 _exptl_absorpt_correction_T_max 0.8299 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10026 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3687 _reflns_number_gt 2831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+2.9105P] 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 3687 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.046435(12) 0.24713(3) 0.06042(2) 0.04029(16) Uani 1 1 d . . . N1 N 0.12184(10) 0.3137(3) 0.04794(15) 0.0473(6) Uani 1 1 d . . . N2 N 0.29583(9) 0.5312(3) 0.08534(15) 0.0452(6) Uani 1 1 d . . . N3 N 0.42635(9) 0.6911(3) 0.31782(15) 0.0435(6) Uani 1 1 d . . . N4 N 0.32395(19) 0.8748(4) -0.2669(2) 0.0903(12) Uani 1 1 d . . . O1 O 0.02414(9) 0.4457(2) 0.09759(12) 0.0535(6) Uani 1 1 d . . . O2 O -0.01440(9) 0.6495(2) 0.05138(12) 0.0525(6) Uani 1 1 d . . . O3 O -0.02455(7) 0.1428(2) 0.04582(13) 0.0479(5) Uani 1 1 d . . . O4 O -0.06381(7) -0.0540(2) -0.01035(13) 0.0467(5) Uani 1 1 d . . . C1 C 0.13213(13) 0.3261(5) -0.0237(2) 0.0654(11) Uani 1 1 d . . . H1 H 0.1077 0.2936 -0.0670 0.078 Uiso 1 1 calc R . . C2 C 0.17661(13) 0.3839(5) -0.0371(2) 0.0659(11) Uani 1 1 d . . . H2 H 0.1817 0.3905 -0.0883 0.079 Uiso 1 1 calc R . . C3 C 0.21410(11) 0.4327(3) 0.02630(17) 0.0425(7) Uani 1 1 d . . . C4 C 0.20456(12) 0.4127(4) 0.10038(18) 0.0507(8) Uani 1 1 d . . . H4 H 0.2294 0.4375 0.1450 0.061 Uiso 1 1 calc R . . C5 C 0.15832(12) 0.3559(4) 0.10866(19) 0.0499(8) Uani 1 1 d . . . H5 H 0.1524 0.3467 0.1593 0.060 Uiso 1 1 calc R . . C6 C 0.26111(11) 0.5109(4) 0.01758(17) 0.0423(7) Uani 1 1 d . . . C7 C 0.26720(11) 0.5680(3) -0.05328(17) 0.0430(7) Uani 1 1 d . . . H7 H 0.2427 0.5503 -0.0994 0.052 Uiso 1 1 calc R . . C8 C 0.30997(12) 0.6519(3) -0.05556(18) 0.0437(7) Uani 1 1 d . . . C9 C 0.34600(11) 0.6718(3) 0.01526(17) 0.0438(7) Uani 1 1 d . . . H9 H 0.3754 0.7261 0.0163 0.053 Uiso 1 1 calc R . . C10 C 0.33760(11) 0.6102(3) 0.08392(17) 0.0425(7) Uani 1 1 d . . . C11 C 0.39467(14) 0.5791(4) 0.3007(2) 0.0580(9) Uani 1 1 d . . . H11 H 0.3910 0.5183 0.3417 0.070 Uiso 1 1 calc R . . C12 C 0.36711(14) 0.5482(4) 0.2260(2) 0.0598(9) Uani 1 1 d . . . H12 H 0.3453 0.4689 0.2177 0.072 Uiso 1 1 calc R . . C13 C 0.37171(11) 0.6342(3) 0.16362(17) 0.0422(7) Uani 1 1 d . . . C14 C 0.40624(13) 0.7478(4) 0.1804(2) 0.0521(9) Uani 1 1 d . . . H14 H 0.4120 0.8070 0.1400 0.063 Uiso 1 1 calc R . . C15 C 0.43165(13) 0.7720(4) 0.2568(2) 0.0514(9) Uani 1 1 d . . . H15 H 0.4541 0.8499 0.2668 0.062 Uiso 1 1 calc R . . C16 C 0.2796(2) 0.8255(5) -0.2558(2) 0.0845(14) Uani 1 1 d . . . H16 H 0.2505 0.8427 -0.2953 0.101 Uiso 1 1 calc R . . C17 C 0.27323(18) 0.7511(4) -0.1903(2) 0.0623(10) Uani 1 1 d . . . H17 H 0.2408 0.7193 -0.1866 0.075 Uiso 1 1 calc R . . C18 C 0.31538(14) 0.7238(4) -0.13008(19) 0.0483(8) Uani 1 1 d . . . C19 C 0.36259(15) 0.7697(4) -0.1416(2) 0.0577(9) Uani 1 1 d . . . H19 H 0.3924 0.7505 -0.1039 0.069 Uiso 1 1 calc R . . C20 C 0.3649(2) 0.8441(5) -0.2094(3) 0.0789(13) Uani 1 1 d . . . H20 H 0.3969 0.8748 -0.2156 0.095 Uiso 1 1 calc R . . C21 C 0.00268(11) 0.5281(3) 0.04271(17) 0.0426(7) Uani 1 1 d . . . C22 C -0.02547(10) 0.0258(3) 0.01032(17) 0.0379(7) Uani 1 1 d . . . O5 O 1.0117(10) 0.835(2) 0.1892(11) 0.212(13) Uani 0.25 1 d P . . O6 O 0.9642(7) 0.590(2) 0.2058(8) 0.142(7) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0367(2) 0.0359(2) 0.0428(2) -0.00032(14) -0.00287(17) -0.00205(14) N1 0.0456(15) 0.0498(16) 0.0428(15) -0.0040(12) 0.0018(12) -0.0140(13) N2 0.0390(14) 0.0538(16) 0.0401(14) -0.0039(12) 0.0026(11) -0.0081(12) N3 0.0372(13) 0.0451(15) 0.0440(15) -0.0059(12) -0.0001(11) 0.0002(12) N4 0.139(4) 0.089(3) 0.046(2) -0.0053(18) 0.026(2) -0.038(3) O1 0.0707(15) 0.0420(13) 0.0398(12) 0.0006(10) -0.0051(10) 0.0095(11) O2 0.0661(14) 0.0404(13) 0.0442(12) -0.0031(10) -0.0021(10) 0.0087(11) O3 0.0364(11) 0.0430(13) 0.0636(14) -0.0137(11) 0.0094(10) -0.0012(9) O4 0.0320(11) 0.0442(13) 0.0624(14) -0.0096(10) 0.0071(9) -0.0042(9) C1 0.051(2) 0.096(3) 0.0442(19) -0.014(2) 0.0003(16) -0.029(2) C2 0.056(2) 0.104(3) 0.0374(17) -0.0133(19) 0.0090(15) -0.030(2) C3 0.0387(16) 0.0485(19) 0.0374(16) -0.0048(13) 0.0019(12) -0.0072(13) C4 0.0515(19) 0.058(2) 0.0366(17) -0.0008(14) -0.0037(14) -0.0194(16) C5 0.0546(19) 0.053(2) 0.0384(17) 0.0020(14) 0.0036(14) -0.0182(16) C6 0.0385(16) 0.0473(19) 0.0393(16) -0.0061(14) 0.0047(12) -0.0037(14) C7 0.0406(16) 0.0519(19) 0.0344(15) -0.0049(13) 0.0036(13) -0.0049(14) C8 0.0469(17) 0.0449(19) 0.0409(16) -0.0073(13) 0.0132(14) -0.0007(14) C9 0.0373(16) 0.050(2) 0.0444(17) -0.0037(14) 0.0104(13) -0.0062(14) C10 0.0352(16) 0.0479(18) 0.0427(17) -0.0064(14) 0.0048(13) -0.0027(13) C11 0.068(2) 0.044(2) 0.051(2) 0.0049(15) -0.0102(16) -0.0105(17) C12 0.065(2) 0.052(2) 0.051(2) 0.0026(16) -0.0110(16) -0.0198(17) C13 0.0346(15) 0.0471(18) 0.0425(17) -0.0048(14) 0.0033(13) -0.0028(13) C14 0.0472(19) 0.069(3) 0.0419(18) -0.0021(15) 0.0131(15) -0.0172(16) C15 0.0454(18) 0.065(2) 0.0447(19) -0.0107(16) 0.0118(15) -0.0198(15) C16 0.116(4) 0.085(3) 0.044(2) 0.004(2) -0.002(2) -0.027(3) C17 0.071(3) 0.074(3) 0.0396(19) -0.0017(16) 0.0055(18) -0.0137(19) C18 0.060(2) 0.049(2) 0.0379(17) -0.0092(14) 0.0148(16) -0.0070(15) C19 0.062(2) 0.058(2) 0.059(2) -0.0059(17) 0.0260(19) -0.0063(17) C20 0.104(3) 0.079(3) 0.066(3) -0.012(2) 0.044(3) -0.029(3) C21 0.0431(16) 0.0389(18) 0.0398(16) -0.0006(13) -0.0038(13) -0.0046(14) C22 0.0318(15) 0.0389(17) 0.0392(15) 0.0005(13) -0.0005(12) 0.0001(12) O5 0.29(2) 0.127(15) 0.143(14) 0.068(12) -0.127(16) -0.150(17) O6 0.173(14) 0.203(19) 0.084(9) 0.008(10) 0.102(9) -0.008(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.083(2) . ? Zn1 O4 2.088(2) 5 ? Zn1 O3 2.093(2) . ? Zn1 N3 2.141(3) 4_545 ? Zn1 N1 2.162(3) . ? Zn1 O2 2.164(2) 5_565 ? N1 C5 1.326(4) . ? N1 C1 1.337(4) . ? N2 C10 1.340(4) . ? N2 C6 1.340(4) . ? N3 C11 1.332(4) . ? N3 C15 1.330(4) . ? N3 Zn1 2.141(3) 4 ? N4 C16 1.322(6) . ? N4 C20 1.337(6) . ? O1 C21 1.256(4) . ? O2 C21 1.238(4) . ? O2 Zn1 2.164(2) 5_565 ? O3 C22 1.247(3) . ? O4 C22 1.250(3) . ? O4 Zn1 2.088(2) 5 ? C1 C2 1.368(5) . ? C1 H1 0.9300 . ? C2 C3 1.389(4) . ? C2 H2 0.9300 . ? C3 C4 1.377(4) . ? C3 C6 1.486(4) . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.381(4) . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 C9 1.396(4) . ? C8 C18 1.490(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9300 . ? C10 C13 1.495(4) . ? C11 C12 1.372(4) . ? C11 H11 0.9300 . ? C12 C13 1.373(4) . ? C12 H12 0.9300 . ? C13 C14 1.388(4) . ? C14 C15 1.368(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.371(5) . ? C16 H16 0.9300 . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 C19 1.386(5) . ? C19 C20 1.377(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C21 1.548(6) 5_565 ? C22 C22 1.556(6) 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 O1 Zn1 O4 173.44(8) . 5 ? O1 Zn1 O3 97.70(9) . . ? O4 Zn1 O3 80.27(8) 5 . ? O1 Zn1 N3 88.11(9) . 4_545 ? O4 Zn1 N3 98.29(10) 5 4_545 ? O3 Zn1 N3 96.20(9) . 4_545 ? O1 Zn1 N1 96.55(10) . . ? O4 Zn1 N1 84.63(9) 5 . ? O3 Zn1 N1 163.40(9) . . ? N3 Zn1 N1 92.73(10) 4_545 . ? O1 Zn1 O2 78.57(8) . 5_565 ? O4 Zn1 O2 95.03(9) 5 5_565 ? O3 Zn1 O2 85.90(9) . 5_565 ? N3 Zn1 O2 166.68(9) 4_545 5_565 ? N1 Zn1 O2 88.61(10) . 5_565 ? C5 N1 C1 116.6(3) . . ? C5 N1 Zn1 122.8(2) . . ? C1 N1 Zn1 120.3(2) . . ? C10 N2 C6 118.5(3) . . ? C11 N3 C15 115.9(3) . . ? C11 N3 Zn1 118.0(2) . 4 ? C15 N3 Zn1 125.2(2) . 4 ? C16 N4 C20 115.3(4) . . ? C21 O1 Zn1 114.7(2) . . ? C21 O2 Zn1 112.22(19) . 5_565 ? C22 O3 Zn1 112.43(18) . . ? C22 O4 Zn1 112.65(18) . 5 ? N1 C1 C2 123.7(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 119.6(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 116.5(3) . . ? C4 C3 C6 119.7(3) . . ? C2 C3 C6 123.7(3) . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C7 122.2(3) . . ? N2 C6 C3 114.5(3) . . ? C7 C6 C3 123.1(3) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 117.4(3) . . ? C7 C8 C18 120.9(3) . . ? C9 C8 C18 121.7(3) . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N2 C10 C9 122.4(3) . . ? N2 C10 C13 113.8(3) . . ? C9 C10 C13 123.6(3) . . ? N3 C11 C12 123.7(3) . . ? N3 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 116.5(3) . . ? C12 C13 C10 120.1(3) . . ? C14 C13 C10 123.2(3) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? N3 C15 C14 124.2(3) . . ? N3 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? N4 C16 C17 125.0(4) . . ? N4 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? C16 C17 C18 119.4(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C19 116.7(3) . . ? C17 C18 C8 121.4(3) . . ? C19 C18 C8 121.9(3) . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N4 C20 C19 124.1(4) . . ? N4 C20 H20 118.0 . . ? C19 C20 H20 118.0 . . ? O2 C21 O1 125.5(3) . . ? O2 C21 C21 117.7(3) . 5_565 ? O1 C21 C21 116.8(3) . 5_565 ? O3 C22 O4 125.7(3) . . ? O3 C22 C22 117.3(3) . 5 ? O4 C22 C22 117.0(3) . 5 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.616 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.068 # Attachment 'complex3.cif' data_nw0256 _database_code_depnum_ccdc_archive 'CCDC 722290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H19 Cd N4 O6' _chemical_formula_weight 571.83 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 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 27.178(12) _cell_length_b 11.287(5) _cell_length_c 14.980(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.480(5) _cell_angle_gamma 90.00 _cell_volume 4383(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2078 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8338 _exptl_absorpt_correction_T_max 0.9024 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10435 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3875 _reflns_number_gt 2527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+29.5725P] 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 3875 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.236751(18) 1.25504(4) 1.11896(3) 0.04457(19) Uani 1 1 d . . . N1 N 0.1639(2) 1.1387(5) 1.0600(4) 0.0455(13) Uani 1 1 d . . . N2 N -0.0106(2) 0.9894(5) 0.8641(3) 0.0450(13) Uani 1 1 d . . . N3 N -0.1873(2) 1.1312(5) 0.6752(4) 0.0462(13) Uani 1 1 d . . . N4 N -0.0110(3) 0.3619(6) 0.8693(5) 0.078(2) Uani 1 1 d . . . O1 O 0.28034(17) 1.1492(4) 1.0244(3) 0.0503(12) Uani 1 1 d . . . O2 O 0.3416(2) 1.0275(5) 1.0110(4) 0.0740(16) Uani 1 1 d . . . O3 O 0.28451(19) 1.0783(4) 1.1908(3) 0.0609(13) Uani 1 1 d . . . O4 O 0.2578(2) 0.7460(5) 1.2106(4) 0.0787(16) Uani 1 1 d . . . O5 O 0.3093(2) 0.8716(5) 1.2999(4) 0.0817(18) Uani 1 1 d . . . O6 O 0.3349(3) 0.1655(8) 0.4005(7) 0.166(4) Uani 1 1 d . . . C1 C 0.1649(3) 1.0200(6) 1.0635(5) 0.0571(19) Uani 1 1 d . . . H1 H 0.1952 0.9829 1.0981 0.069 Uiso 1 1 calc R . . C2 C 0.1234(2) 0.9507(6) 1.0187(5) 0.0527(18) Uani 1 1 d . . . H2 H 0.1264 0.8687 1.0227 0.063 Uiso 1 1 calc R . . C3 C 0.0773(2) 1.0013(5) 0.9675(4) 0.0368(14) Uani 1 1 d . . . C4 C 0.0754(3) 1.1239(6) 0.9674(5) 0.0514(18) Uani 1 1 d . . . H4 H 0.0450 1.1633 0.9363 0.062 Uiso 1 1 calc R . . C5 C 0.1196(3) 1.1880(6) 1.0145(5) 0.0515(18) Uani 1 1 d . . . H5 H 0.1175 1.2702 1.0136 0.062 Uiso 1 1 calc R . . C6 C 0.0313(2) 0.9299(6) 0.9160(4) 0.0423(15) Uani 1 1 d . . . C7 C 0.0318(2) 0.8078(5) 0.9196(4) 0.0425(16) Uani 1 1 d . . . H7 H 0.0609 0.7681 0.9560 0.051 Uiso 1 1 calc R . . C8 C -0.0109(2) 0.7449(6) 0.8695(4) 0.0457(15) Uani 1 1 d . . . C9 C -0.0535(2) 0.8049(5) 0.8163(4) 0.0397(15) Uani 1 1 d . . . H9 H -0.0826 0.7634 0.7817 0.048 Uiso 1 1 calc R . . C10 C -0.0531(2) 0.9270(5) 0.8146(4) 0.0399(15) Uani 1 1 d . . . C11 C -0.1879(3) 1.0140(6) 0.6742(5) 0.062(2) Uani 1 1 d . . . H11 H -0.2186 0.9760 0.6427 0.075 Uiso 1 1 calc R . . C12 C -0.1458(3) 0.9455(6) 0.7168(5) 0.059(2) Uani 1 1 d . . . H12 H -0.1488 0.8634 0.7147 0.071 Uiso 1 1 calc R . . C13 C -0.0991(2) 0.9969(5) 0.7625(4) 0.0390(15) Uani 1 1 d . . . C14 C -0.0976(3) 1.1198(6) 0.7617(6) 0.065(2) Uani 1 1 d . . . H14 H -0.0672 1.1603 0.7904 0.078 Uiso 1 1 calc R . . C15 C -0.1424(3) 1.1807(6) 0.7171(6) 0.066(2) Uani 1 1 d . . . H15 H -0.1406 1.2630 0.7167 0.079 Uiso 1 1 calc R . . C16 C 0.0311(3) 0.4243(7) 0.8734(6) 0.075(2) Uani 1 1 d . . . H16 H 0.0611 0.3829 0.8759 0.090 Uiso 1 1 calc R . . C17 C 0.0332(3) 0.5472(7) 0.8742(5) 0.062(2) Uani 1 1 d . . . H17 H 0.0638 0.5859 0.8770 0.074 Uiso 1 1 calc R . . C18 C -0.0111(2) 0.6122(6) 0.8707(4) 0.0486(17) Uani 1 1 d . . . C19 C -0.0548(3) 0.5474(7) 0.8674(5) 0.061(2) Uani 1 1 d . . . H19 H -0.0855 0.5860 0.8642 0.073 Uiso 1 1 calc R . . C20 C -0.0527(4) 0.4245(7) 0.8688(6) 0.071(2) Uani 1 1 d . . . H20 H -0.0822 0.3832 0.8695 0.086 Uiso 1 1 calc R . . C21 C 0.3121(3) 1.0660(6) 1.0524(5) 0.0473(17) Uani 1 1 d . . . C22 C 0.3145(3) 1.0103(6) 1.1465(5) 0.0498(17) Uani 1 1 d . . . H22 H 0.3505 1.0138 1.1861 0.060 Uiso 1 1 calc R . . C23 C 0.2989(3) 0.8824(6) 1.1356(5) 0.059(2) Uani 1 1 d . . . H23A H 0.3261 0.8370 1.1219 0.071 Uiso 1 1 calc R . . H23B H 0.2681 0.8745 1.0825 0.071 Uiso 1 1 calc R . . C24 C 0.2883(3) 0.8299(6) 1.2220(6) 0.0557(19) 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 Cd1 0.0450(3) 0.0425(3) 0.0462(3) -0.0062(2) 0.0137(2) -0.0096(2) N1 0.038(3) 0.046(3) 0.052(3) 0.000(3) 0.013(3) -0.005(2) N2 0.040(3) 0.048(3) 0.044(3) 0.004(3) 0.007(2) 0.003(3) N3 0.043(3) 0.040(3) 0.053(3) 0.003(3) 0.010(3) 0.006(3) N4 0.077(5) 0.058(4) 0.089(5) 0.000(4) 0.009(4) -0.001(4) O1 0.050(3) 0.046(3) 0.054(3) 0.012(2) 0.015(2) 0.006(2) O2 0.086(4) 0.068(3) 0.082(4) 0.008(3) 0.046(3) 0.013(3) O3 0.063(3) 0.050(3) 0.070(3) 0.002(3) 0.022(3) 0.008(2) O4 0.087(4) 0.073(4) 0.085(4) 0.007(3) 0.039(3) -0.017(3) O5 0.099(5) 0.081(4) 0.064(4) 0.014(3) 0.022(3) -0.025(3) O6 0.098(6) 0.150(7) 0.260(11) 0.121(8) 0.068(7) 0.021(5) C1 0.040(4) 0.047(4) 0.074(5) 0.004(4) 0.001(4) 0.000(3) C2 0.035(4) 0.041(4) 0.076(5) -0.001(3) 0.007(4) 0.003(3) C3 0.033(3) 0.040(3) 0.036(3) -0.001(3) 0.010(3) -0.004(3) C4 0.035(4) 0.051(4) 0.067(5) 0.008(4) 0.012(3) 0.002(3) C5 0.048(4) 0.040(4) 0.067(5) -0.001(3) 0.017(4) -0.004(3) C6 0.032(3) 0.051(4) 0.043(4) 0.001(3) 0.011(3) 0.005(3) C7 0.030(3) 0.045(4) 0.047(4) 0.004(3) 0.004(3) 0.005(3) C8 0.041(3) 0.048(4) 0.045(3) -0.006(3) 0.008(3) 0.002(3) C9 0.032(3) 0.039(3) 0.042(4) -0.007(3) 0.003(3) -0.003(3) C10 0.037(4) 0.045(4) 0.035(3) -0.004(3) 0.006(3) -0.002(3) C11 0.044(4) 0.052(4) 0.076(5) -0.001(4) -0.006(4) 0.003(3) C12 0.041(4) 0.036(4) 0.084(5) -0.001(4) -0.007(4) 0.002(3) C13 0.037(4) 0.040(3) 0.037(3) -0.001(3) 0.006(3) -0.001(3) C14 0.055(5) 0.037(4) 0.090(6) -0.005(4) 0.002(4) -0.003(3) C15 0.055(5) 0.034(4) 0.097(6) 0.006(4) 0.004(4) 0.003(3) C16 0.062(6) 0.067(5) 0.081(6) 0.003(5) -0.003(5) 0.013(4) C17 0.045(4) 0.059(5) 0.074(6) -0.001(4) 0.006(4) 0.004(4) C18 0.039(4) 0.056(4) 0.043(4) -0.001(3) 0.001(3) 0.001(3) C19 0.049(5) 0.058(5) 0.065(5) -0.004(4) 0.001(4) 0.002(4) C20 0.077(6) 0.067(5) 0.068(5) -0.006(4) 0.019(5) -0.014(5) C21 0.050(4) 0.036(4) 0.057(4) -0.002(3) 0.017(4) -0.009(3) C22 0.051(4) 0.043(4) 0.053(4) 0.001(3) 0.011(3) 0.006(3) C23 0.064(5) 0.044(4) 0.070(5) 0.008(4) 0.022(4) 0.002(4) C24 0.052(5) 0.043(4) 0.073(6) 0.010(4) 0.021(4) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.318(5) . ? Cd1 O1 2.323(4) 7_577 ? Cd1 N3 2.360(5) 8_576 ? Cd1 O5 2.384(5) 4_557 ? Cd1 O1 2.418(5) . ? Cd1 O3 2.446(5) . ? Cd1 O4 2.515(6) 4_557 ? N1 C5 1.317(8) . ? N1 C1 1.341(8) . ? N2 C6 1.348(8) . ? N2 C10 1.366(8) . ? N3 C15 1.320(8) . ? N3 C11 1.323(8) . ? N3 Cd1 2.360(5) 8_475 ? N4 C16 1.328(10) . ? N4 C20 1.333(10) . ? O1 C21 1.259(8) . ? O1 Cd1 2.323(4) 7_577 ? O2 C21 1.231(8) . ? O3 C22 1.422(8) . ? O4 C24 1.237(9) . ? O4 Cd1 2.515(6) 4_547 ? O5 C24 1.227(9) . ? O5 Cd1 2.384(5) 4_547 ? C1 C2 1.370(9) . ? C1 H1 0.9300 . ? C2 C3 1.382(8) . ? C2 H2 0.9300 . ? C3 C4 1.385(9) . ? C3 C6 1.493(8) . ? C4 C5 1.396(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.380(9) . ? C7 C8 1.374(8) . ? C7 H7 0.9300 . ? C8 C9 1.371(8) . ? C8 C18 1.498(9) . ? C9 C10 1.378(8) . ? C9 H9 0.9300 . ? C10 C13 1.486(8) . ? C11 C12 1.369(9) . ? C11 H11 0.9300 . ? C12 C13 1.376(8) . ? C12 H12 0.9300 . ? C13 C14 1.388(9) . ? C14 C15 1.382(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.388(10) . ? C16 H16 0.9300 . ? C17 C18 1.396(9) . ? C17 H17 0.9300 . ? C18 C19 1.383(10) . ? C19 C20 1.388(10) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.526(9) . ? C22 C23 1.500(9) . ? C22 H22 0.9800 . ? C23 C24 1.528(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O1 90.02(17) . 7_577 ? N1 Cd1 N3 177.58(19) . 8_576 ? O1 Cd1 N3 89.28(17) 7_577 8_576 ? N1 Cd1 O5 89.3(2) . 4_557 ? O1 Cd1 O5 102.99(19) 7_577 4_557 ? N3 Cd1 O5 93.1(2) 8_576 4_557 ? N1 Cd1 O1 90.55(17) . . ? O1 Cd1 O1 71.65(17) 7_577 . ? N3 Cd1 O1 87.03(17) 8_576 . ? O5 Cd1 O1 174.64(17) 4_557 . ? N1 Cd1 O3 89.16(18) . . ? O1 Cd1 O3 135.94(17) 7_577 . ? N3 Cd1 O3 89.72(18) 8_576 . ? O5 Cd1 O3 121.05(19) 4_557 . ? O1 Cd1 O3 64.31(16) . . ? N1 Cd1 O4 98.45(19) . 4_557 ? O1 Cd1 O4 153.11(17) 7_577 4_557 ? N3 Cd1 O4 83.18(19) 8_576 4_557 ? O5 Cd1 O4 52.02(18) 4_557 4_557 ? O1 Cd1 O4 133.25(16) . 4_557 ? O3 Cd1 O4 70.03(17) . 4_557 ? C5 N1 C1 116.5(6) . . ? C5 N1 Cd1 120.2(4) . . ? C1 N1 Cd1 123.1(4) . . ? C6 N2 C10 119.1(5) . . ? C15 N3 C11 115.8(6) . . ? C15 N3 Cd1 121.7(4) . 8_475 ? C11 N3 Cd1 122.3(5) . 8_475 ? C16 N4 C20 116.0(7) . . ? C21 O1 Cd1 125.5(5) . 7_577 ? C21 O1 Cd1 125.5(4) . . ? Cd1 O1 Cd1 108.35(17) 7_577 . ? C22 O3 Cd1 122.5(4) . . ? C24 O4 Cd1 89.7(5) . 4_547 ? C24 O5 Cd1 96.3(5) . 4_547 ? N1 C1 C2 123.2(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.8(6) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C2 C3 C4 116.1(6) . . ? C2 C3 C6 122.9(6) . . ? C4 C3 C6 120.9(6) . . ? C3 C4 C5 119.4(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 123.9(6) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N2 C6 C7 121.1(6) . . ? N2 C6 C3 117.4(5) . . ? C7 C6 C3 121.5(6) . . ? C8 C7 C6 119.8(6) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 119.3(6) . . ? C9 C8 C18 119.7(6) . . ? C7 C8 C18 121.0(6) . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 121.1(6) . . ? N2 C10 C13 116.9(5) . . ? C9 C10 C13 122.0(5) . . ? N3 C11 C12 123.7(7) . . ? N3 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 120.7(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 116.2(6) . . ? C12 C13 C10 122.9(6) . . ? C14 C13 C10 120.9(6) . . ? C15 C14 C13 118.6(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? N3 C15 C14 125.0(6) . . ? N3 C15 H15 117.5 . . ? C14 C15 H15 117.5 . . ? N4 C16 C17 124.2(8) . . ? N4 C16 H16 117.9 . . ? C17 C16 H16 117.9 . . ? C16 C17 C18 119.5(7) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 116.4(7) . . ? C19 C18 C8 122.3(6) . . ? C17 C18 C8 121.3(6) . . ? C18 C19 C20 119.8(8) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N4 C20 C19 124.1(8) . . ? N4 C20 H20 118.0 . . ? C19 C20 H20 118.0 . . ? O2 C21 O1 125.5(7) . . ? O2 C21 C22 117.7(6) . . ? O1 C21 C22 116.7(6) . . ? O3 C22 C23 112.8(6) . . ? O3 C22 C21 109.8(5) . . ? C23 C22 C21 111.3(6) . . ? O3 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C21 C22 H22 107.6 . . ? C22 C23 C24 113.6(6) . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O5 C24 O4 121.7(8) . . ? O5 C24 C23 120.4(7) . . ? O4 C24 C23 117.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 N1 C5 -48.5(5) 7_577 . . . ? N3 Cd1 N1 C5 -122(4) 8_576 . . . ? O5 Cd1 N1 C5 54.5(5) 4_557 . . . ? O1 Cd1 N1 C5 -120.1(5) . . . . ? O3 Cd1 N1 C5 175.6(5) . . . . ? O4 Cd1 N1 C5 105.9(5) 4_557 . . . ? O1 Cd1 N1 C1 126.4(6) 7_577 . . . ? N3 Cd1 N1 C1 53(5) 8_576 . . . ? O5 Cd1 N1 C1 -130.6(6) 4_557 . . . ? O1 Cd1 N1 C1 54.8(6) . . . . ? O3 Cd1 N1 C1 -9.5(6) . . . . ? O4 Cd1 N1 C1 -79.2(6) 4_557 . . . ? N1 Cd1 O1 C21 -98.5(5) . . . . ? O1 Cd1 O1 C21 171.6(6) 7_577 . . . ? N3 Cd1 O1 C21 81.4(5) 8_576 . . . ? O5 Cd1 O1 C21 172.9(18) 4_557 . . . ? O3 Cd1 O1 C21 -9.7(5) . . . . ? O4 Cd1 O1 C21 3.7(6) 4_557 . . . ? N1 Cd1 O1 Cd1 89.8(2) . . . 7_577 ? O1 Cd1 O1 Cd1 0.0 7_577 . . 7_577 ? N3 Cd1 O1 Cd1 -90.2(2) 8_576 . . 7_577 ? O5 Cd1 O1 Cd1 1(2) 4_557 . . 7_577 ? O3 Cd1 O1 Cd1 178.6(2) . . . 7_577 ? O4 Cd1 O1 Cd1 -167.99(19) 4_557 . . 7_577 ? N1 Cd1 O3 C22 94.7(5) . . . . ? O1 Cd1 O3 C22 5.5(6) 7_577 . . . ? N3 Cd1 O3 C22 -83.2(5) 8_576 . . . ? O5 Cd1 O3 C22 -176.7(5) 4_557 . . . ? O1 Cd1 O3 C22 3.6(4) . . . . ? O4 Cd1 O3 C22 -166.0(5) 4_557 . . . ? C5 N1 C1 C2 3.5(11) . . . . ? Cd1 N1 C1 C2 -171.6(6) . . . . ? N1 C1 C2 C3 -1.0(12) . . . . ? C1 C2 C3 C4 -2.0(10) . . . . ? C1 C2 C3 C6 178.9(7) . . . . ? C2 C3 C4 C5 2.4(10) . . . . ? C6 C3 C4 C5 -178.5(6) . . . . ? C1 N1 C5 C4 -3.0(11) . . . . ? Cd1 N1 C5 C4 172.2(5) . . . . ? C3 C4 C5 N1 0.1(11) . . . . ? C10 N2 C6 C7 0.1(9) . . . . ? C10 N2 C6 C3 178.9(5) . . . . ? C2 C3 C6 N2 -176.2(6) . . . . ? C4 C3 C6 N2 4.8(9) . . . . ? C2 C3 C6 C7 2.5(10) . . . . ? C4 C3 C6 C7 -176.5(7) . . . . ? N2 C6 C7 C8 0.2(10) . . . . ? C3 C6 C7 C8 -178.4(6) . . . . ? C6 C7 C8 C9 0.0(10) . . . . ? C6 C7 C8 C18 178.8(6) . . . . ? C7 C8 C9 C10 -0.5(10) . . . . ? C18 C8 C9 C10 -179.4(6) . . . . ? C6 N2 C10 C9 -0.7(9) . . . . ? C6 N2 C10 C13 176.9(6) . . . . ? C8 C9 C10 N2 0.9(10) . . . . ? C8 C9 C10 C13 -176.6(6) . . . . ? C15 N3 C11 C12 2.9(12) . . . . ? Cd1 N3 C11 C12 -171.4(6) 8_475 . . . ? N3 C11 C12 C13 -1.4(13) . . . . ? C11 C12 C13 C14 -0.6(11) . . . . ? C11 C12 C13 C10 176.3(7) . . . . ? N2 C10 C13 C12 -174.1(7) . . . . ? C9 C10 C13 C12 3.4(10) . . . . ? N2 C10 C13 C14 2.7(9) . . . . ? C9 C10 C13 C14 -179.8(7) . . . . ? C12 C13 C14 C15 1.0(12) . . . . ? C10 C13 C14 C15 -176.0(7) . . . . ? C11 N3 C15 C14 -2.4(13) . . . . ? Cd1 N3 C15 C14 171.8(7) 8_475 . . . ? C13 C14 C15 N3 0.6(14) . . . . ? C20 N4 C16 C17 -2.1(13) . . . . ? N4 C16 C17 C18 0.2(14) . . . . ? C16 C17 C18 C19 0.5(11) . . . . ? C16 C17 C18 C8 -178.8(7) . . . . ? C9 C8 C18 C19 -36.4(10) . . . . ? C7 C8 C18 C19 144.8(7) . . . . ? C9 C8 C18 C17 142.9(7) . . . . ? C7 C8 C18 C17 -36.0(10) . . . . ? C17 C18 C19 C20 0.8(11) . . . . ? C8 C18 C19 C20 -179.9(7) . . . . ? C16 N4 C20 C19 3.5(13) . . . . ? C18 C19 C20 N4 -3.0(13) . . . . ? Cd1 O1 C21 O2 5.2(10) 7_577 . . . ? Cd1 O1 C21 O2 -165.1(5) . . . . ? Cd1 O1 C21 C22 -176.0(4) 7_577 . . . ? Cd1 O1 C21 C22 13.8(8) . . . . ? Cd1 O3 C22 C23 -123.9(5) . . . . ? Cd1 O3 C22 C21 0.8(7) . . . . ? O2 C21 C22 O3 170.2(6) . . . . ? O1 C21 C22 O3 -8.8(8) . . . . ? O2 C21 C22 C23 -64.2(8) . . . . ? O1 C21 C22 C23 116.8(7) . . . . ? O3 C22 C23 C24 -42.5(8) . . . . ? C21 C22 C23 C24 -166.4(6) . . . . ? Cd1 O5 C24 O4 -5.6(8) 4_547 . . . ? Cd1 O5 C24 C23 173.4(6) 4_547 . . . ? Cd1 O4 C24 O5 5.3(8) 4_547 . . . ? Cd1 O4 C24 C23 -173.8(6) 4_547 . . . ? C22 C23 C24 O5 -26.2(10) . . . . ? C22 C23 C24 O4 152.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.812 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.095 # Attachment 'complex4.cif' data_nw0293 _database_code_depnum_ccdc_archive 'CCDC 722291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H18 N4 O7 Zn2' _chemical_formula_weight 665.21 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 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 35.332(10) _cell_length_b 10.979(3) _cell_length_c 16.158(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.232(4) _cell_angle_gamma 90.00 _cell_volume 5622(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2455 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 21.04 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 1.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13558 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4948 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^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 4948 _refine_ls_number_parameters 406 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24073(2) 0.82674(6) 0.34114(5) 0.0559(3) Uani 1 1 d . . . Zn2 Zn 0.16337(2) 0.62765(7) 0.26185(5) 0.0691(3) Uani 1 1 d . . . N1 N 0.30012(13) 0.7564(4) 0.3974(3) 0.0540(11) Uani 1 1 d . . . N2 N 0.49483(17) 0.4507(6) 0.6202(5) 0.094(2) Uani 1 1 d . . . N3 N 0.60859(15) 0.7708(5) 0.7227(4) 0.0785(16) Uani 1 1 d . . . O1 O 0.25127(14) 0.9454(4) 0.4778(3) 0.0741(12) Uani 1 1 d . . . O2 O 0.21885(15) 0.9960(4) 0.3319(3) 0.0732(12) Uani 1 1 d . . . O3 O 0.16633(18) 1.4411(4) 0.2696(4) 0.0970(17) Uani 1 1 d . . . O4 O 0.13768(16) 1.5075(4) 0.3529(4) 0.0964(16) Uani 1 1 d . . . O5 O 0.17351(15) 1.3334(5) 0.6537(3) 0.0918(16) Uani 1 1 d . . . O6 O 0.22296(15) 1.1895(4) 0.7059(3) 0.0772(13) Uani 1 1 d . . . O7 O 0.20753(12) 0.7060(4) 0.3650(3) 0.0740(12) Uani 1 1 d . . . C1 C 0.22804(18) 1.0156(5) 0.4157(5) 0.0592(15) Uani 1 1 d . . . C2 C 0.1572(2) 1.4285(6) 0.3347(5) 0.0715(18) Uani 1 1 d . . . C3 C 0.19775(19) 1.2540(5) 0.6447(5) 0.0620(15) Uani 1 1 d . . . C4 C 0.20996(16) 1.1269(4) 0.4406(4) 0.0518(14) Uani 1 1 d . . . C5 C 0.19021(17) 1.2188(5) 0.3741(4) 0.0569(14) Uani 1 1 d . . . H5 H 0.1886 1.2114 0.3153 0.068 Uiso 1 1 calc R . . C6 C 0.17335(18) 1.3196(4) 0.3966(4) 0.0560(15) Uani 1 1 d . . . C7 C 0.17480(17) 1.3277(5) 0.4825(4) 0.0555(15) Uani 1 1 d . . . H7 H 0.1621 1.3937 0.4966 0.067 Uiso 1 1 calc R . . C8 C 0.19475(16) 1.2397(5) 0.5488(4) 0.0525(14) Uani 1 1 d . . . C9 C 0.21281(16) 1.1403(5) 0.5273(4) 0.0498(13) Uani 1 1 d . . . H9 H 0.2270 1.0821 0.5722 0.060 Uiso 1 1 calc R . . C10 C 0.30703(19) 0.6498(5) 0.3663(5) 0.0635(16) Uani 1 1 d . . . H10 H 0.2854 0.6164 0.3138 0.076 Uiso 1 1 calc R . . C11 C 0.34416(17) 0.5875(5) 0.4077(4) 0.0639(17) Uani 1 1 d . . . H11 H 0.3477 0.5149 0.3822 0.077 Uiso 1 1 calc R . . C12 C 0.37665(18) 0.6328(5) 0.4878(4) 0.0594(15) Uani 1 1 d . . . C13 C 0.36964(18) 0.7425(5) 0.5197(4) 0.0677(17) Uani 1 1 d . . . H13 H 0.3909 0.7766 0.5725 0.081 Uiso 1 1 calc R . . C14 C 0.3317(2) 0.8032(5) 0.4748(5) 0.0681(17) Uani 1 1 d . . . H14 H 0.3277 0.8772 0.4979 0.082 Uiso 1 1 calc R . . C15 C 0.4578(2) 0.3865(7) 0.5813(6) 0.092(2) Uani 1 1 d . . . C16 C 0.41975(19) 0.4419(5) 0.5396(5) 0.077(2) Uani 1 1 d . . . H16 H 0.3952 0.3957 0.5138 0.093 Uiso 1 1 calc R . . C17 C 0.41758(18) 0.5689(6) 0.5355(5) 0.0700(17) Uani 1 1 d . . . C18 C 0.45489(17) 0.6316(6) 0.5764(5) 0.0698(18) Uani 1 1 d . . . H18 H 0.4547 0.7163 0.5761 0.084 Uiso 1 1 calc R . . C19 C 0.49272(18) 0.5703(6) 0.6179(5) 0.0739(19) Uani 1 1 d . . . C20 C 0.5727(2) 0.8277(7) 0.7002(7) 0.115(3) Uani 1 1 d . . . H20 H 0.5725 0.9120 0.7060 0.138 Uiso 1 1 calc R . . C21 C 0.5346(2) 0.7629(6) 0.6676(7) 0.109(3) Uani 1 1 d . . . H21 H 0.5097 0.8056 0.6521 0.131 Uiso 1 1 calc R A . C22 C 0.53292(19) 0.6385(6) 0.6578(5) 0.075(2) Uani 1 1 d . . . C23 C 0.5721(2) 0.5825(7) 0.6856(6) 0.101(3) Uani 1 1 d . . . H23 H 0.5738 0.4981 0.6829 0.121 Uiso 1 1 calc R A . C24 C 0.6082(2) 0.6520(6) 0.7169(6) 0.096(3) Uani 1 1 d . . . H24 H 0.6338 0.6120 0.7352 0.115 Uiso 1 1 calc R . . N4 N 0.4686(10) -0.006(2) 0.5539(15) 0.191(13) Uani 0.50 1 d PD A 1 C25 C 0.4594(3) 0.2496(8) 0.5837(7) 0.132(4) Uani 0.50 1 d PD A 1 C26 C 0.5028(6) 0.2020(19) 0.5910(13) 0.132(8) Uani 0.50 1 d PD A 1 C27 C 0.5017(8) 0.073(2) 0.5757(16) 0.160(10) Uani 0.50 1 d PD A 1 C28 C 0.4316(4) 0.0466(9) 0.5496(10) 0.167(5) Uani 0.50 1 d PD A 1 C29 C 0.4297(3) 0.1731(7) 0.5465(9) 0.148(5) Uani 0.50 1 d PD A 1 N4' N 0.4596(9) -0.015(2) 0.6170(19) 0.145(9) Uani 0.50 1 d PD A 2 C25' C 0.4594(3) 0.2496(8) 0.5837(7) 0.132(4) Uani 0.50 1 d PD A 2 C26' C 0.4927(7) 0.186(2) 0.6674(14) 0.156(10) Uani 0.50 1 d PD A 2 C27' C 0.4890(9) 0.053(2) 0.6779(19) 0.164(11) Uani 0.50 1 d PD A 2 C28' C 0.4316(4) 0.0466(9) 0.5496(10) 0.167(5) Uani 0.50 1 d PD A 2 C29' C 0.4297(3) 0.1731(7) 0.5465(9) 0.148(5) Uani 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0514(4) 0.0478(4) 0.0619(5) 0.0032(3) 0.0191(3) 0.0053(3) Zn2 0.0532(4) 0.0641(5) 0.0767(6) 0.0238(4) 0.0167(4) -0.0009(3) N1 0.048(3) 0.045(3) 0.065(3) -0.008(2) 0.021(2) -0.002(2) N2 0.054(3) 0.077(4) 0.117(5) -0.008(4) 0.007(3) 0.009(3) N3 0.046(3) 0.073(4) 0.096(4) -0.033(3) 0.013(3) 0.003(3) O1 0.075(3) 0.060(3) 0.076(3) 0.009(2) 0.024(2) 0.022(2) O2 0.103(3) 0.055(3) 0.063(3) 0.005(2) 0.038(3) 0.022(2) O3 0.141(5) 0.065(3) 0.089(4) 0.021(3) 0.055(4) 0.020(3) O4 0.103(4) 0.058(3) 0.105(4) 0.011(3) 0.025(3) 0.026(3) O5 0.080(3) 0.107(4) 0.076(3) -0.013(3) 0.024(3) 0.034(3) O6 0.096(3) 0.071(3) 0.065(3) 0.009(2) 0.035(3) 0.019(3) O7 0.055(2) 0.078(3) 0.076(3) 0.017(2) 0.018(2) -0.004(2) C1 0.060(4) 0.040(3) 0.078(5) 0.007(3) 0.031(3) 0.007(3) C2 0.071(4) 0.056(4) 0.075(5) 0.008(4) 0.021(4) 0.009(3) C3 0.058(4) 0.052(4) 0.072(4) -0.003(3) 0.024(3) -0.005(3) C4 0.047(3) 0.035(3) 0.069(4) 0.005(3) 0.022(3) 0.001(2) C5 0.054(3) 0.051(3) 0.061(4) 0.008(3) 0.022(3) 0.004(3) C6 0.056(3) 0.031(3) 0.075(4) 0.005(3) 0.024(3) 0.007(2) C7 0.049(3) 0.038(3) 0.073(4) -0.006(3) 0.021(3) -0.002(2) C8 0.044(3) 0.046(3) 0.063(4) 0.002(3) 0.020(3) -0.002(2) C9 0.049(3) 0.039(3) 0.057(4) 0.005(3) 0.019(3) -0.001(2) C10 0.049(3) 0.061(4) 0.075(4) -0.014(3) 0.022(3) -0.006(3) C11 0.044(3) 0.050(3) 0.082(4) -0.015(3) 0.014(3) 0.001(3) C12 0.047(3) 0.048(3) 0.075(4) -0.007(3) 0.020(3) 0.000(3) C13 0.051(4) 0.055(4) 0.079(4) -0.016(3) 0.013(3) -0.007(3) C14 0.063(4) 0.051(3) 0.081(5) -0.008(3) 0.022(4) 0.002(3) C15 0.051(4) 0.072(5) 0.116(6) -0.009(4) 0.004(4) 0.000(3) C16 0.047(3) 0.053(4) 0.110(6) -0.005(4) 0.015(4) 0.002(3) C17 0.046(3) 0.063(4) 0.088(5) -0.002(4) 0.017(3) 0.000(3) C18 0.041(3) 0.054(3) 0.097(5) -0.008(3) 0.015(3) -0.006(3) C19 0.044(3) 0.068(4) 0.089(5) -0.011(4) 0.010(3) 0.001(3) C20 0.045(4) 0.073(5) 0.181(9) -0.040(5) 0.009(5) 0.006(4) C21 0.047(4) 0.061(4) 0.181(9) -0.029(5) 0.015(5) 0.002(3) C22 0.047(3) 0.066(4) 0.090(5) -0.019(4) 0.010(3) 0.009(3) C23 0.048(4) 0.067(4) 0.157(8) -0.031(5) 0.017(4) 0.006(3) C24 0.052(4) 0.074(5) 0.137(7) -0.037(5) 0.021(4) 0.006(3) N4 0.132(19) 0.090(14) 0.28(4) 0.05(2) 0.03(2) 0.056(14) C25 0.078(6) 0.085(6) 0.163(9) -0.006(6) -0.011(6) 0.035(5) C26 0.117(15) 0.110(15) 0.18(2) 0.053(15) 0.078(16) 0.047(12) C27 0.126(19) 0.109(18) 0.21(3) 0.014(18) 0.045(18) 0.056(16) C28 0.121(9) 0.080(7) 0.288(17) 0.027(9) 0.080(10) 0.015(6) C29 0.066(5) 0.066(5) 0.281(15) 0.028(7) 0.050(7) -0.003(4) N4' 0.130(18) 0.101(14) 0.17(2) 0.057(16) 0.037(15) 0.033(13) C25' 0.078(6) 0.085(6) 0.163(9) -0.006(6) -0.011(6) 0.035(5) C26' 0.18(2) 0.16(2) 0.100(16) 0.020(15) 0.030(16) 0.053(18) C27' 0.14(2) 0.092(16) 0.21(3) 0.052(17) 0.04(2) 0.070(15) C28' 0.121(9) 0.080(7) 0.288(17) 0.027(9) 0.080(10) 0.015(6) C29' 0.066(5) 0.066(5) 0.281(15) 0.028(7) 0.050(7) -0.003(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 O7 1.919(4) . ? Zn1 O2 1.993(4) . ? Zn1 O6 1.997(5) 6_575 ? Zn1 N1 2.035(4) . ? Zn1 O1 2.447(4) . ? Zn2 O7 1.911(4) . ? Zn2 O5 1.980(5) 6_575 ? Zn2 O3 2.051(5) 1_545 ? Zn2 N3 2.075(5) 8_465 ? Zn2 O4 2.431(6) 1_545 ? Zn2 C2 2.538(7) 1_545 ? N1 C10 1.338(7) . ? N1 C14 1.355(7) . ? N2 C19 1.315(9) . ? N2 C15 1.369(9) . ? N3 C24 1.308(8) . ? N3 C20 1.314(8) . ? N3 Zn2 2.075(5) 8_566 ? O1 C1 1.243(7) . ? O2 C1 1.264(7) . ? O3 C2 1.236(8) . ? O3 Zn2 2.051(5) 1_565 ? O4 C2 1.223(8) . ? O4 Zn2 2.431(5) 1_565 ? O5 C3 1.275(7) . ? O5 Zn2 1.980(5) 6_576 ? O6 C3 1.222(7) . ? O6 Zn1 1.997(5) 6_576 ? C1 C4 1.513(8) . ? C2 C6 1.500(8) . ? C2 Zn2 2.538(7) 1_565 ? C3 C8 1.514(8) . ? C4 C9 1.366(8) . ? C4 C5 1.414(7) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 C7 1.370(8) . ? C7 C8 1.382(7) . ? C7 H7 0.9300 . ? C8 C9 1.384(7) . ? C9 H9 0.9300 . ? C10 C11 1.363(8) . ? C10 H10 0.9300 . ? C11 C12 1.388(8) . ? C11 H11 0.9300 . ? C12 C13 1.375(8) . ? C12 C17 1.481(8) . ? C13 C14 1.382(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.355(9) . ? C15 C25 1.503(12) . ? C16 C17 1.396(9) . ? C16 H16 0.9300 . ? C17 C18 1.370(8) . ? C18 C19 1.377(8) . ? C18 H18 0.9300 . ? C19 C22 1.478(8) . ? C20 C21 1.402(9) . ? C20 H20 0.9300 . ? C21 C22 1.372(9) . ? C21 H21 0.9300 . ? C22 C23 1.395(8) . ? C23 C24 1.375(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? N4 C27 1.37(3) . ? N4 C28 1.40(3) . ? C25 C29 1.269(11) . ? C25 C26 1.575(19) . ? C26 C27 1.44(3) . ? C28 C29 1.390(12) . ? N4' C27' 1.30(4) . ? C26' C27' 1.48(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 O7 Zn1 O2 114.09(19) . . ? O7 Zn1 O6 103.51(18) . 6_575 ? O2 Zn1 O6 94.42(18) . 6_575 ? O7 Zn1 N1 104.42(18) . . ? O2 Zn1 N1 132.60(19) . . ? O6 Zn1 N1 102.63(19) 6_575 . ? O7 Zn1 O1 92.84(17) . . ? O2 Zn1 O1 58.02(15) . . ? O6 Zn1 O1 152.12(16) 6_575 . ? N1 Zn1 O1 94.78(16) . . ? O7 Zn2 O5 106.02(19) . 6_575 ? O7 Zn2 O3 113.3(2) . 1_545 ? O5 Zn2 O3 104.2(2) 6_575 1_545 ? O7 Zn2 N3 108.5(2) . 8_465 ? O5 Zn2 N3 97.1(2) 6_575 8_465 ? O3 Zn2 N3 124.8(2) 1_545 8_465 ? O7 Zn2 O4 95.49(18) . 1_545 ? O5 Zn2 O4 155.96(19) 6_575 1_545 ? O3 Zn2 O4 56.22(18) 1_545 1_545 ? N3 Zn2 O4 85.91(18) 8_465 1_545 ? O7 Zn2 C2 100.8(2) . 1_545 ? O5 Zn2 C2 133.0(2) 6_575 1_545 ? O3 Zn2 C2 28.84(19) 1_545 1_545 ? N3 Zn2 C2 110.2(2) 8_465 1_545 ? O4 Zn2 C2 28.40(18) 1_545 1_545 ? C10 N1 C14 117.8(5) . . ? C10 N1 Zn1 119.2(4) . . ? C14 N1 Zn1 122.2(4) . . ? C19 N2 C15 118.1(6) . . ? C24 N3 C20 118.4(6) . . ? C24 N3 Zn2 122.5(4) . 8_566 ? C20 N3 Zn2 119.1(5) . 8_566 ? C1 O1 Zn1 79.6(4) . . ? C1 O2 Zn1 99.8(3) . . ? C2 O3 Zn2 98.0(4) . 1_565 ? C2 O4 Zn2 80.6(4) . 1_565 ? C3 O5 Zn2 129.9(5) . 6_576 ? C3 O6 Zn1 134.5(4) . 6_576 ? Zn2 O7 Zn1 118.2(2) . . ? O1 C1 O2 121.7(5) . . ? O1 C1 C4 119.4(6) . . ? O2 C1 C4 118.9(5) . . ? O4 C2 O3 120.8(6) . . ? O4 C2 C6 119.6(7) . . ? O3 C2 C6 119.4(6) . . ? O4 C2 Zn2 71.0(4) . 1_565 ? O3 C2 Zn2 53.2(3) . 1_565 ? C6 C2 Zn2 155.6(5) . 1_565 ? O6 C3 O5 126.2(6) . . ? O6 C3 C8 117.7(5) . . ? O5 C3 C8 116.2(6) . . ? C9 C4 C5 119.4(5) . . ? C9 C4 C1 120.7(5) . . ? C5 C4 C1 119.9(6) . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 119.5(5) . . ? C7 C6 C2 117.2(5) . . ? C5 C6 C2 123.0(6) . . ? C6 C7 C8 121.2(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 119.4(5) . . ? C7 C8 C3 120.1(5) . . ? C9 C8 C3 120.5(5) . . ? C4 C9 C8 120.6(5) . . ? C4 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N1 C10 C11 123.4(6) . . ? N1 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 116.8(5) . . ? C13 C12 C17 121.0(5) . . ? C11 C12 C17 122.1(5) . . ? C12 C13 C14 121.3(6) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? N1 C14 C13 120.8(6) . . ? N1 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 N2 122.3(7) . . ? C16 C15 C25 118.6(6) . . ? N2 C15 C25 119.1(6) . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 117.2(6) . . ? C18 C17 C12 121.6(6) . . ? C16 C17 C12 121.2(5) . . ? C17 C18 C19 120.6(6) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? N2 C19 C18 122.2(6) . . ? N2 C19 C22 117.5(6) . . ? C18 C19 C22 120.2(6) . . ? N3 C20 C21 120.8(6) . . ? N3 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 122.3(6) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 114.5(6) . . ? C21 C22 C19 122.6(6) . . ? C23 C22 C19 122.8(6) . . ? C24 C23 C22 120.0(6) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N3 C24 C23 124.0(6) . . ? N3 C24 H24 118.0 . . ? C23 C24 H24 118.0 . . ? C27 N4 C28 115(2) . . ? C29 C25 C15 129.6(7) . . ? C29 C25 C26 112.9(11) . . ? C15 C25 C26 110.9(10) . . ? C27 C26 C25 111.3(18) . . ? N4 C27 C26 128(2) . . ? C29 C28 N4 116.1(15) . . ? C25 C29 C28 128.9(9) . . ? N4' C27' C26' 124(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Zn1 N1 C10 60.1(5) . . . . ? O2 Zn1 N1 C10 -155.9(4) . . . . ? O6 Zn1 N1 C10 -47.6(5) 6_575 . . . ? O1 Zn1 N1 C10 154.3(4) . . . . ? O7 Zn1 N1 C14 -109.3(5) . . . . ? O2 Zn1 N1 C14 34.7(6) . . . . ? O6 Zn1 N1 C14 142.9(5) 6_575 . . . ? O1 Zn1 N1 C14 -15.1(5) . . . . ? O7 Zn1 O1 C1 -111.2(4) . . . . ? O2 Zn1 O1 C1 5.6(4) . . . . ? O6 Zn1 O1 C1 15.2(6) 6_575 . . . ? N1 Zn1 O1 C1 144.1(4) . . . . ? O7 Zn1 O2 C1 72.0(4) . . . . ? O6 Zn1 O2 C1 179.0(4) 6_575 . . . ? N1 Zn1 O2 C1 -69.4(5) . . . . ? O1 Zn1 O2 C1 -5.5(3) . . . . ? O5 Zn2 O7 Zn1 14.1(3) 6_575 . . . ? O3 Zn2 O7 Zn1 127.8(3) 1_545 . . . ? N3 Zn2 O7 Zn1 -89.2(3) 8_465 . . . ? O4 Zn2 O7 Zn1 -176.7(2) 1_545 . . . ? C2 Zn2 O7 Zn1 155.1(3) 1_545 . . . ? O2 Zn1 O7 Zn2 91.5(3) . . . . ? O6 Zn1 O7 Zn2 -9.7(3) 6_575 . . . ? N1 Zn1 O7 Zn2 -116.8(2) . . . . ? O1 Zn1 O7 Zn2 147.5(2) . . . . ? Zn1 O1 C1 O2 -8.9(6) . . . . ? Zn1 O1 C1 C4 170.7(5) . . . . ? Zn1 O2 C1 O1 10.9(7) . . . . ? Zn1 O2 C1 C4 -168.7(4) . . . . ? Zn2 O4 C2 O3 -19.3(7) 1_565 . . . ? Zn2 O4 C2 C6 155.8(6) 1_565 . . . ? Zn2 O3 C2 O4 23.0(8) 1_565 . . . ? Zn2 O3 C2 C6 -152.2(5) 1_565 . . . ? Zn1 O6 C3 O5 -1.7(10) 6_576 . . . ? Zn1 O6 C3 C8 178.0(4) 6_576 . . . ? Zn2 O5 C3 O6 -6.1(10) 6_576 . . . ? Zn2 O5 C3 C8 174.1(4) 6_576 . . . ? O1 C1 C4 C9 -11.2(8) . . . . ? O2 C1 C4 C9 168.4(5) . . . . ? O1 C1 C4 C5 168.2(5) . . . . ? O2 C1 C4 C5 -12.2(8) . . . . ? C9 C4 C5 C6 -1.3(8) . . . . ? C1 C4 C5 C6 179.3(5) . . . . ? C4 C5 C6 C7 -2.0(8) . . . . ? C4 C5 C6 C2 171.4(5) . . . . ? O4 C2 C6 C7 -16.1(9) . . . . ? O3 C2 C6 C7 159.1(6) . . . . ? Zn2 C2 C6 C7 94.1(13) 1_565 . . . ? O4 C2 C6 C5 170.4(6) . . . . ? O3 C2 C6 C5 -14.4(10) . . . . ? Zn2 C2 C6 C5 -79.5(14) 1_565 . . . ? C5 C6 C7 C8 3.3(8) . . . . ? C2 C6 C7 C8 -170.5(5) . . . . ? C6 C7 C8 C9 -1.3(8) . . . . ? C6 C7 C8 C3 177.0(5) . . . . ? O6 C3 C8 C7 -164.6(5) . . . . ? O5 C3 C8 C7 15.2(8) . . . . ? O6 C3 C8 C9 13.7(8) . . . . ? O5 C3 C8 C9 -166.5(5) . . . . ? C5 C4 C9 C8 3.3(8) . . . . ? C1 C4 C9 C8 -177.3(5) . . . . ? C7 C8 C9 C4 -2.0(8) . . . . ? C3 C8 C9 C4 179.7(5) . . . . ? C14 N1 C10 C11 -0.9(9) . . . . ? Zn1 N1 C10 C11 -170.8(5) . . . . ? N1 C10 C11 C12 2.0(10) . . . . ? C10 C11 C12 C13 -2.0(10) . . . . ? C10 C11 C12 C17 179.9(6) . . . . ? C11 C12 C13 C14 1.2(10) . . . . ? C17 C12 C13 C14 179.3(6) . . . . ? C10 N1 C14 C13 0.0(9) . . . . ? Zn1 N1 C14 C13 169.6(5) . . . . ? C12 C13 C14 N1 -0.2(10) . . . . ? C19 N2 C15 C16 1.1(13) . . . . ? C19 N2 C15 C25 -179.5(8) . . . . ? N2 C15 C16 C17 0.1(13) . . . . ? C25 C15 C16 C17 -179.3(8) . . . . ? C15 C16 C17 C18 -1.2(12) . . . . ? C15 C16 C17 C12 177.9(7) . . . . ? C13 C12 C17 C18 -35.3(11) . . . . ? C11 C12 C17 C18 142.7(7) . . . . ? C13 C12 C17 C16 145.7(7) . . . . ? C11 C12 C17 C16 -36.4(11) . . . . ? C16 C17 C18 C19 1.2(11) . . . . ? C12 C17 C18 C19 -177.9(7) . . . . ? C15 N2 C19 C18 -1.2(12) . . . . ? C15 N2 C19 C22 -178.2(7) . . . . ? C17 C18 C19 N2 0.0(12) . . . . ? C17 C18 C19 C22 177.0(7) . . . . ? C24 N3 C20 C21 -2.4(15) . . . . ? Zn2 N3 C20 C21 175.8(8) 8_566 . . . ? N3 C20 C21 C22 0.2(16) . . . . ? C20 C21 C22 C23 1.9(14) . . . . ? C20 C21 C22 C19 -176.0(9) . . . . ? N2 C19 C22 C21 -173.3(8) . . . . ? C18 C19 C22 C21 9.6(12) . . . . ? N2 C19 C22 C23 9.0(12) . . . . ? C18 C19 C22 C23 -168.2(8) . . . . ? C21 C22 C23 C24 -1.9(13) . . . . ? C19 C22 C23 C24 176.0(8) . . . . ? C20 N3 C24 C23 2.4(14) . . . . ? Zn2 N3 C24 C23 -175.7(7) 8_566 . . . ? C22 C23 C24 N3 -0.2(15) . . . . ? C16 C15 C25 C29 5.1(17) . . . . ? N2 C15 C25 C29 -174.2(11) . . . . ? C16 C15 C25 C26 153.9(10) . . . . ? N2 C15 C25 C26 -25.4(13) . . . . ? C29 C25 C26 C27 -14.6(13) . . . . ? C15 C25 C26 C27 -168.9(12) . . . . ? C28 N4 C27 C26 -3(3) . . . . ? C25 C26 C27 N4 2(2) . . . . ? C27 N4 C28 C29 14(2) . . . . ? C15 C25 C29 C28 -179.7(12) . . . . ? C26 C25 C29 C28 32.0(17) . . . . ? N4 C28 C29 C25 -33(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.611 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.084