# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email lidongsheng1@126.com _publ_contact_author_name 'Dr Dong-Sheng Li' _publ_section_title ; Isomeric phenylenediacetates as modular tecton for a series of ZnII/CdII coordination polymers incorporating flexible bis (imidazole) co-ligands ; loop_ _publ_author_name 'Dong-Sheng Li' 'Yao-Yu Wang' # Attachment '- Complex 1-7.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 839122' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H20 N4 O4 Zn' _chemical_formula_weight 433.76 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0802(18) _cell_length_b 11.246(2) _cell_length_c 19.815(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.95(3) _cell_angle_gamma 90.00 _cell_volume 1902.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9389 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3356 _reflns_number_gt 2349 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.1' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. ; _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^)+(0.1157P)^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 3356 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.91992(6) 0.01307(5) 0.27853(3) 0.0378(2) Uani 1 1 d . . . C1 C 0.7316(5) -0.0774(4) 0.1454(2) 0.0335(11) Uani 1 1 d . . . C2 C 0.7174(5) -0.1360(4) 0.0743(3) 0.0371(11) Uani 1 1 d . . . H2A H 0.7327 -0.0750 0.0428 0.045 Uiso 1 1 calc R . . H2B H 0.8031 -0.1921 0.0832 0.045 Uiso 1 1 calc R . . C3 C 0.5672(5) -0.2010(4) 0.0341(3) 0.0371(11) Uani 1 1 d . . . C4 C 0.4688(6) -0.1525(4) -0.0296(3) 0.0416(12) Uani 1 1 d . . . H4 H 0.4961 -0.0809 -0.0457 0.050 Uiso 1 1 calc R . . C5 C 0.3308(6) -0.2082(5) -0.0700(3) 0.0482(14) Uani 1 1 d . . . H5 H 0.2648 -0.1736 -0.1121 0.058 Uiso 1 1 calc R . . C6 C 0.2929(6) -0.3149(5) -0.0471(3) 0.0540(15) Uani 1 1 d . . . H6 H 0.2014 -0.3537 -0.0741 0.065 Uiso 1 1 calc R . . C7 C 0.3886(6) -0.3647(5) 0.0153(3) 0.0461(13) Uani 1 1 d . . . H7 H 0.3618 -0.4377 0.0299 0.055 Uiso 1 1 calc R . . C8 C 0.5267(5) -0.3080(4) 0.0577(3) 0.0369(11) Uani 1 1 d . . . C9 C 0.6219(6) -0.3632(5) 0.1282(3) 0.0464(13) Uani 1 1 d . . . H9A H 0.5633 -0.4301 0.1369 0.056 Uiso 1 1 calc R . . H9B H 0.6317 -0.3054 0.1658 0.056 Uiso 1 1 calc R . . C10 C 0.7842(6) -0.4065(4) 0.1359(3) 0.0401(12) Uani 1 1 d . . . C11 C 0.6687(7) 0.2078(5) 0.2541(3) 0.0552(15) Uani 1 1 d . . . H11 H 0.6071 0.1829 0.2084 0.066 Uiso 1 1 calc R . . C12 C 0.6357(7) 0.3008(5) 0.2899(3) 0.0546(15) Uani 1 1 d . . . H12 H 0.5492 0.3509 0.2739 0.066 Uiso 1 1 calc R . . C13 C 0.8522(6) 0.2178(4) 0.3554(3) 0.0479(13) Uani 1 1 d . . . H13 H 0.9424 0.2013 0.3941 0.057 Uiso 1 1 calc R . . C14 C 0.7707(7) 0.3884(4) 0.4138(3) 0.0486(14) Uani 1 1 d . . . H14A H 0.8337 0.3506 0.4583 0.058 Uiso 1 1 calc R . . H14B H 0.6678 0.4035 0.4167 0.058 Uiso 1 1 calc R . . C15 C 0.8458(7) 0.5064(4) 0.4065(3) 0.0506(14) Uani 1 1 d . . . H15A H 0.8752 0.5484 0.4519 0.061 Uiso 1 1 calc R . . H15B H 0.9406 0.4911 0.3957 0.061 Uiso 1 1 calc R . . C16 C 0.7411(7) 0.5822(5) 0.3499(3) 0.0558(15) Uani 1 1 d . . . H16A H 0.6356 0.5771 0.3513 0.067 Uiso 1 1 calc R . . H16B H 0.7391 0.5538 0.3034 0.067 Uiso 1 1 calc R . . C17 C 0.8508(6) 0.7687(5) 0.3158(3) 0.0482(13) Uani 1 1 d . . . H17 H 0.8683 0.7365 0.2759 0.058 Uiso 1 1 calc R . . C18 C 0.8417(8) 0.8887(5) 0.3978(4) 0.0637(17) Uani 1 1 d . . . H18 H 0.8521 0.9568 0.4257 0.076 Uiso 1 1 calc R . . C19 C 0.7882(9) 0.7847(6) 0.4112(4) 0.0721(19) Uani 1 1 d . . . H19 H 0.7535 0.7676 0.4492 0.086 Uiso 1 1 calc R . . N1 N 0.8059(5) 0.1560(4) 0.2951(3) 0.0458(11) Uani 1 1 d . . . N2 N 0.7544(5) 0.3063(4) 0.3541(2) 0.0431(10) Uani 1 1 d . . . N3 N 0.7935(6) 0.7075(4) 0.3591(3) 0.0558(13) Uani 1 1 d . . . N4 N 0.8795(5) 0.8799(4) 0.3364(2) 0.0420(10) Uani 1 1 d . . . O1 O 0.6188(4) -0.0587(3) 0.16316(19) 0.0470(9) Uani 1 1 d . . . O2 O 0.8732(4) -0.0476(3) 0.18225(19) 0.0467(9) Uani 1 1 d . . . O3 O 0.8641(4) -0.4374(3) 0.20086(19) 0.0477(9) Uani 1 1 d . . . O4 O 0.8337(4) -0.4102(3) 0.0854(2) 0.0477(9) 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 0.0431(4) 0.0340(4) 0.0337(4) -0.0039(2) 0.0098(3) -0.0049(2) C1 0.037(3) 0.031(2) 0.025(3) 0.000(2) 0.001(2) -0.001(2) C2 0.038(3) 0.042(3) 0.030(3) -0.005(2) 0.009(2) -0.002(2) C3 0.036(2) 0.036(3) 0.036(3) -0.005(2) 0.009(2) 0.002(2) C4 0.055(3) 0.033(3) 0.030(3) -0.002(2) 0.007(2) 0.002(2) C5 0.054(3) 0.046(3) 0.031(3) -0.005(2) -0.003(2) 0.008(2) C6 0.046(3) 0.047(3) 0.053(4) -0.010(3) -0.004(3) -0.003(2) C7 0.043(3) 0.037(3) 0.051(4) -0.002(2) 0.007(3) -0.002(2) C8 0.036(2) 0.037(3) 0.034(3) 0.000(2) 0.008(2) 0.003(2) C9 0.042(3) 0.044(3) 0.048(4) 0.009(2) 0.008(2) 0.002(2) C10 0.038(3) 0.034(3) 0.043(3) 0.000(2) 0.006(2) 0.002(2) C11 0.055(3) 0.061(4) 0.044(4) -0.009(3) 0.009(3) 0.001(3) C12 0.052(3) 0.054(3) 0.054(4) 0.001(3) 0.012(3) 0.012(3) C13 0.053(3) 0.035(3) 0.051(4) -0.002(3) 0.011(3) 0.001(2) C14 0.069(4) 0.039(3) 0.043(3) -0.001(3) 0.025(3) 0.001(3) C15 0.058(3) 0.044(3) 0.049(4) -0.005(3) 0.017(3) -0.001(2) C16 0.066(4) 0.053(4) 0.044(4) 0.001(3) 0.013(3) -0.014(3) C17 0.062(3) 0.045(3) 0.038(3) 0.002(3) 0.018(3) -0.003(3) C18 0.096(5) 0.045(3) 0.058(4) -0.011(3) 0.036(4) -0.001(3) C19 0.119(6) 0.056(4) 0.061(5) 0.004(3) 0.057(4) -0.003(4) N1 0.049(3) 0.039(2) 0.047(3) -0.010(2) 0.012(2) -0.006(2) N2 0.044(2) 0.038(2) 0.045(3) -0.005(2) 0.013(2) -0.0020(19) N3 0.079(3) 0.038(3) 0.053(3) 0.001(2) 0.026(3) -0.010(2) N4 0.054(3) 0.038(2) 0.032(3) -0.0032(19) 0.012(2) -0.0054(19) O1 0.046(2) 0.060(2) 0.035(2) -0.0098(18) 0.0132(17) -0.0047(18) O2 0.0387(19) 0.058(2) 0.039(2) -0.0088(18) 0.0068(16) -0.0099(16) O3 0.0445(19) 0.054(2) 0.037(2) 0.0065(18) 0.0037(17) 0.0153(17) O4 0.050(2) 0.048(2) 0.045(2) 0.0001(17) 0.0157(18) 0.0030(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.932(4) . ? Zn1 O3 1.943(3) 2_755 ? Zn1 N4 1.994(4) 1_545 ? Zn1 N1 1.998(4) . ? C1 O1 1.209(6) . ? C1 O2 1.287(5) . ? C1 C2 1.521(7) . ? C2 C3 1.512(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.385(7) . ? C3 C4 1.386(7) . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.368(8) . ? C5 H5 0.9300 . ? C6 C7 1.365(8) . ? C6 H6 0.9300 . ? C7 C8 1.403(7) . ? C7 H7 0.9300 . ? C8 C9 1.503(7) . ? C9 C10 1.509(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O4 1.229(6) . ? C10 O3 1.291(6) . ? C11 C12 1.355(8) . ? C11 N1 1.364(7) . ? C11 H11 0.9300 . ? C12 N2 1.359(7) . ? C12 H12 0.9300 . ? C13 N1 1.321(7) . ? C13 N2 1.328(6) . ? C13 H13 0.9300 . ? C14 N2 1.468(7) . ? C14 C15 1.521(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.469(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N3 1.479(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N4 1.314(6) . ? C17 N3 1.337(7) . ? C17 H17 0.9300 . ? C18 C19 1.327(8) . ? C18 N4 1.377(7) . ? C18 H18 0.9300 . ? C19 N3 1.362(8) . ? C19 H19 0.9300 . ? N4 Zn1 1.994(4) 1_565 ? O3 Zn1 1.943(3) 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 O2 Zn1 O3 100.05(15) . 2_755 ? O2 Zn1 N4 106.32(16) . 1_545 ? O3 Zn1 N4 117.69(16) 2_755 1_545 ? O2 Zn1 N1 119.64(17) . . ? O3 Zn1 N1 106.10(16) 2_755 . ? N4 Zn1 N1 107.59(18) 1_545 . ? O1 C1 O2 124.8(5) . . ? O1 C1 C2 122.1(4) . . ? O2 C1 C2 113.0(4) . . ? C3 C2 C1 118.3(4) . . ? C3 C2 H2A 107.7 . . ? C1 C2 H2A 107.7 . . ? C3 C2 H2B 107.7 . . ? C1 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? C8 C3 C4 119.1(4) . . ? C8 C3 C2 122.5(4) . . ? C4 C3 C2 118.4(4) . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 119.0(5) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 121.3(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C3 C8 C7 118.6(5) . . ? C3 C8 C9 122.5(4) . . ? C7 C8 C9 118.8(5) . . ? C8 C9 C10 117.4(5) . . ? C8 C9 H9A 108.0 . . ? C10 C9 H9A 108.0 . . ? C8 C9 H9B 108.0 . . ? C10 C9 H9B 108.0 . . ? H9A C9 H9B 107.2 . . ? O4 C10 O3 124.4(5) . . ? O4 C10 C9 123.0(5) . . ? O3 C10 C9 112.6(5) . . ? C12 C11 N1 109.8(5) . . ? C12 C11 H11 125.1 . . ? N1 C11 H11 125.1 . . ? C11 C12 N2 106.2(5) . . ? C11 C12 H12 126.9 . . ? N2 C12 H12 126.9 . . ? N1 C13 N2 111.9(5) . . ? N1 C13 H13 124.1 . . ? N2 C13 H13 124.1 . . ? N2 C14 C15 113.4(5) . . ? N2 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? N2 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 112.6(5) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 N3 111.2(5) . . ? C15 C16 H16A 109.4 . . ? N3 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? N3 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 N3 111.7(5) . . ? N4 C17 H17 124.2 . . ? N3 C17 H17 124.2 . . ? C19 C18 N4 109.4(5) . . ? C19 C18 H18 125.3 . . ? N4 C18 H18 125.3 . . ? C18 C19 N3 107.5(5) . . ? C18 C19 H19 126.2 . . ? N3 C19 H19 126.2 . . ? C13 N1 C11 104.9(5) . . ? C13 N1 Zn1 123.3(4) . . ? C11 N1 Zn1 131.6(4) . . ? C13 N2 C12 107.2(5) . . ? C13 N2 C14 124.9(5) . . ? C12 N2 C14 127.7(5) . . ? C17 N3 C19 106.3(5) . . ? C17 N3 C16 126.2(5) . . ? C19 N3 C16 127.4(5) . . ? C17 N4 C18 105.1(5) . . ? C17 N4 Zn1 126.3(4) . 1_565 ? C18 N4 Zn1 127.2(4) . 1_565 ? C1 O2 Zn1 119.5(3) . . ? C10 O3 Zn1 118.0(3) . 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 -16.2(7) . . . . ? O2 C1 C2 C3 165.9(4) . . . . ? C1 C2 C3 C8 -71.0(6) . . . . ? C1 C2 C3 C4 110.7(6) . . . . ? C8 C3 C4 C5 0.3(8) . . . . ? C2 C3 C4 C5 178.7(5) . . . . ? C3 C4 C5 C6 -1.5(8) . . . . ? C4 C5 C6 C7 1.0(9) . . . . ? C5 C6 C7 C8 0.7(9) . . . . ? C4 C3 C8 C7 1.3(7) . . . . ? C2 C3 C8 C7 -177.0(5) . . . . ? C4 C3 C8 C9 -176.5(5) . . . . ? C2 C3 C8 C9 5.2(8) . . . . ? C6 C7 C8 C3 -1.8(8) . . . . ? C6 C7 C8 C9 176.1(5) . . . . ? C3 C8 C9 C10 -66.8(7) . . . . ? C7 C8 C9 C10 115.5(5) . . . . ? C8 C9 C10 O4 -8.2(8) . . . . ? C8 C9 C10 O3 171.2(4) . . . . ? N1 C11 C12 N2 -0.1(7) . . . . ? N2 C14 C15 C16 71.9(7) . . . . ? C14 C15 C16 N3 161.5(5) . . . . ? N4 C18 C19 N3 1.0(8) . . . . ? N2 C13 N1 C11 -1.3(6) . . . . ? N2 C13 N1 Zn1 -178.1(3) . . . . ? C12 C11 N1 C13 0.8(7) . . . . ? C12 C11 N1 Zn1 177.2(4) . . . . ? O2 Zn1 N1 C13 -165.2(4) . . . . ? O3 Zn1 N1 C13 -53.3(5) 2_755 . . . ? N4 Zn1 N1 C13 73.5(5) 1_545 . . . ? O2 Zn1 N1 C11 18.9(6) . . . . ? O3 Zn1 N1 C11 130.8(5) 2_755 . . . ? N4 Zn1 N1 C11 -102.4(5) 1_545 . . . ? N1 C13 N2 C12 1.3(7) . . . . ? N1 C13 N2 C14 177.9(5) . . . . ? C11 C12 N2 C13 -0.7(7) . . . . ? C11 C12 N2 C14 -177.2(5) . . . . ? C15 C14 N2 C13 98.4(6) . . . . ? C15 C14 N2 C12 -85.7(7) . . . . ? N4 C17 N3 C19 -1.1(7) . . . . ? N4 C17 N3 C16 176.8(5) . . . . ? C18 C19 N3 C17 0.0(8) . . . . ? C18 C19 N3 C16 -177.9(6) . . . . ? C15 C16 N3 C17 112.1(7) . . . . ? C15 C16 N3 C19 -70.4(8) . . . . ? N3 C17 N4 C18 1.7(7) . . . . ? N3 C17 N4 Zn1 -165.5(4) . . . 1_565 ? C19 C18 N4 C17 -1.6(7) . . . . ? C19 C18 N4 Zn1 165.4(5) . . . 1_565 ? O1 C1 O2 Zn1 8.6(7) . . . . ? C2 C1 O2 Zn1 -173.6(3) . . . . ? O3 Zn1 O2 C1 -172.0(3) 2_755 . . . ? N4 Zn1 O2 C1 65.0(4) 1_545 . . . ? N1 Zn1 O2 C1 -56.9(4) . . . . ? O4 C10 O3 Zn1 2.7(7) . . . 2_745 ? C9 C10 O3 Zn1 -176.6(3) . . . 2_745 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.364 _refine_diff_density_min -1.461 _refine_diff_density_rms 0.126 data_2 _database_code_depnum_ccdc_archive 'CCDC 839123' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 Cd N4 O5' _chemical_formula_weight 526.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 11.524(9) _cell_length_b 12.671(10) _cell_length_c 15.484(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.353(16) _cell_angle_gamma 90.00 _cell_volume 2224(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11000 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0966 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3934 _reflns_number_gt 2480 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.1' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. Although the hydrogen atoms of lattice water molecule O5 in complex 2 were located using the Difference Fourier method, meantime, the H5A and H5B atoms may have higher thermal parameters, so the hydrogen atoms of O5 atom should be omitted. ; _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^)+(0.0955P)^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 3934 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.08399(5) 0.81693(4) 0.01283(4) 0.0457(2) Uani 1 1 d . . . C1 C 0.1426(7) 0.8149(6) 0.1088(6) 0.0485(18) Uani 1 1 d U . . C2 C 0.2689(7) 0.8200(6) 0.1587(5) 0.054(2) Uani 1 1 d . . . H2A H 0.3028 0.8869 0.1457 0.065 Uiso 1 1 calc R . . H2B H 0.2671 0.8190 0.2211 0.065 Uiso 1 1 calc R . . C3 C 0.3485(6) 0.7334(6) 0.1392(5) 0.0445(18) Uani 1 1 d . . . C4 C 0.3526(6) 0.6358(6) 0.1809(5) 0.0462(19) Uani 1 1 d . . . C5 C 0.4319(8) 0.5595(7) 0.1614(6) 0.067(3) Uani 1 1 d . . . H5 H 0.4370 0.4947 0.1900 0.080 Uiso 1 1 calc R . . C6 C 0.5031(9) 0.5797(11) 0.0997(7) 0.083(3) Uani 1 1 d . . . H6 H 0.5543 0.5279 0.0865 0.100 Uiso 1 1 calc R . . C7 C 0.4980(9) 0.6735(11) 0.0592(7) 0.088(4) Uani 1 1 d . . . H7 H 0.5458 0.6866 0.0179 0.106 Uiso 1 1 calc R . . C8 C 0.4232(8) 0.7498(8) 0.0784(6) 0.065(2) Uani 1 1 d . . . H8 H 0.4217 0.8148 0.0503 0.078 Uiso 1 1 calc R . . C9 C 0.2728(8) 0.6109(7) 0.2451(5) 0.062(2) Uani 1 1 d . . . H9A H 0.2631 0.5349 0.2469 0.074 Uiso 1 1 calc R . . H9B H 0.1958 0.6411 0.2232 0.074 Uiso 1 1 calc R . . C10 C 0.3145(8) 0.6501(6) 0.3385(5) 0.051(2) Uani 1 1 d . . . C11 C -0.0667(7) 0.5890(6) 0.0962(6) 0.054(2) Uani 1 1 d . . . H11 H -0.0097 0.6140 0.1418 0.065 Uiso 1 1 calc R . . C12 C -0.2038(7) 0.5825(7) -0.0157(5) 0.055(2) Uani 1 1 d . . . H12 H -0.2605 0.6026 -0.0635 0.066 Uiso 1 1 calc R . . C13 C -0.1815(7) 0.4837(7) 0.0127(5) 0.054(2) Uani 1 1 d . . . H13 H -0.2196 0.4231 -0.0117 0.065 Uiso 1 1 calc R . . C14 C -0.0395(7) 0.3995(7) 0.1373(6) 0.059(2) Uani 1 1 d . . . H14A H 0.0447 0.4120 0.1533 0.071 Uiso 1 1 calc R . . H14B H -0.0507 0.3352 0.1028 0.071 Uiso 1 1 calc R . . C15 C -0.0898(8) 0.3842(7) 0.2196(5) 0.064(2) Uani 1 1 d . . . H15A H -0.0739 0.4470 0.2556 0.077 Uiso 1 1 calc R . . H15B H -0.0493 0.3257 0.2524 0.077 Uiso 1 1 calc R . . C16 C -0.2221(8) 0.3627(7) 0.2036(6) 0.062(2) Uani 1 1 d . . . H16A H -0.2470 0.3561 0.2600 0.074 Uiso 1 1 calc R . . H16B H -0.2627 0.4230 0.1737 0.074 Uiso 1 1 calc R . . C17 C -0.2599(7) 0.2650(7) 0.1504(5) 0.055(2) Uani 1 1 d . . . H17A H -0.2273 0.2671 0.0969 0.066 Uiso 1 1 calc R . . H17B H -0.3451 0.2645 0.1341 0.066 Uiso 1 1 calc R . . C18 C -0.2200(9) 0.1647(6) 0.2001(6) 0.064(2) Uani 1 1 d . . . H18A H -0.1371 0.1706 0.2260 0.077 Uiso 1 1 calc R . . H18B H -0.2641 0.1555 0.2473 0.077 Uiso 1 1 calc R . . C19 C -0.1527(7) 0.0117(6) 0.1211(5) 0.0475(19) Uani 1 1 d . . . H19 H -0.0730 0.0206 0.1440 0.057 Uiso 1 1 calc R . . C20 C -0.3143(7) -0.0479(7) 0.0480(6) 0.059(2) Uani 1 1 d . . . H20 H -0.3682 -0.0884 0.0100 0.071 Uiso 1 1 calc R . . C21 C -0.3407(8) 0.0330(7) 0.0953(5) 0.059(2) Uani 1 1 d . . . H21 H -0.4161 0.0587 0.0963 0.071 Uiso 1 1 calc R . . N1 N -0.1295(6) 0.6490(5) 0.0370(4) 0.0511(17) Uani 1 1 d . . . N2 N -0.0940(5) 0.4879(5) 0.0831(4) 0.0487(16) Uani 1 1 d . . . N3 N -0.2374(6) 0.0722(5) 0.1423(4) 0.0536(17) Uani 1 1 d . . . N4 N -0.1936(5) -0.0620(5) 0.0645(4) 0.0472(16) Uani 1 1 d . . . O1 O 0.0609(6) 0.8472(6) 0.1463(5) 0.098(3) Uani 1 1 d U . . O2 O 0.1208(5) 0.7821(5) 0.0344(4) 0.0696(17) Uani 1 1 d . . . O3 O 0.2420(6) 0.6854(6) 0.3810(4) 0.083(2) Uani 1 1 d . . . O4 O 0.4221(5) 0.6459(5) 0.3704(4) 0.0656(16) Uani 1 1 d . . . O5 O 0.4789(7) 0.2314(11) 0.1996(7) 0.161(4) 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 0.0404(4) 0.0502(4) 0.0445(4) -0.0027(3) 0.0018(2) 0.0016(3) C1 0.038(4) 0.049(5) 0.052(5) -0.003(4) -0.007(3) 0.001(3) C2 0.046(5) 0.064(6) 0.048(5) -0.009(4) -0.004(4) -0.001(4) C3 0.032(4) 0.058(5) 0.042(4) -0.006(4) 0.000(3) 0.001(4) C4 0.038(4) 0.054(5) 0.041(4) -0.010(4) -0.006(4) 0.004(4) C5 0.072(6) 0.057(6) 0.058(5) -0.009(4) -0.027(5) 0.013(5) C6 0.061(6) 0.115(10) 0.067(7) -0.038(7) -0.004(6) 0.036(6) C7 0.060(7) 0.152(12) 0.053(6) -0.029(7) 0.011(5) 0.009(7) C8 0.052(5) 0.086(7) 0.058(6) -0.003(5) 0.012(5) -0.002(5) C9 0.069(6) 0.060(6) 0.050(5) 0.001(4) -0.007(4) -0.021(4) C10 0.053(5) 0.053(5) 0.046(5) 0.004(4) 0.006(4) -0.010(4) C11 0.045(5) 0.048(5) 0.063(5) -0.007(4) -0.005(4) -0.002(4) C12 0.049(5) 0.060(6) 0.051(5) 0.001(4) -0.002(4) -0.008(4) C13 0.057(5) 0.051(5) 0.053(5) -0.008(4) 0.004(4) -0.011(4) C14 0.048(5) 0.056(5) 0.070(6) 0.002(4) -0.001(4) 0.007(4) C15 0.075(7) 0.063(6) 0.052(5) 0.002(4) 0.001(5) 0.007(5) C16 0.074(6) 0.049(5) 0.067(6) -0.001(4) 0.024(5) 0.009(5) C17 0.044(5) 0.067(6) 0.055(5) 0.002(4) 0.013(4) 0.006(4) C18 0.088(7) 0.054(6) 0.053(5) -0.002(4) 0.020(5) 0.014(5) C19 0.035(4) 0.054(5) 0.054(5) -0.002(4) 0.008(4) 0.007(4) C20 0.040(5) 0.067(6) 0.069(6) -0.002(5) 0.004(4) -0.002(4) C21 0.049(5) 0.070(6) 0.058(5) 0.013(5) 0.007(4) 0.013(4) N1 0.043(4) 0.051(4) 0.055(4) -0.005(3) -0.005(3) -0.006(3) N2 0.044(4) 0.045(4) 0.053(4) -0.003(3) -0.002(3) -0.001(3) N3 0.056(4) 0.053(4) 0.052(4) 0.008(3) 0.010(3) 0.010(3) N4 0.032(3) 0.055(4) 0.054(4) 0.001(3) 0.005(3) -0.003(3) O1 0.057(4) 0.135(6) 0.096(6) -0.049(5) -0.004(3) 0.033(4) O2 0.038(3) 0.115(5) 0.052(4) -0.012(3) -0.004(3) 0.001(3) O3 0.061(4) 0.133(7) 0.050(4) -0.002(4) -0.001(3) 0.012(4) O4 0.051(4) 0.093(5) 0.048(3) -0.018(3) -0.005(3) 0.001(3) O5 0.061(5) 0.287(13) 0.142(9) -0.008(9) 0.036(5) -0.023(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 Cd1 N4 2.225(6) 1_565 ? Cd1 N1 2.239(7) . ? Cd1 O4 2.269(6) 4_575 ? Cd1 O2 2.365(6) . ? Cd1 O1 2.442(7) . ? Cd1 O3 2.592(6) 4_575 ? C1 O2 1.208(9) . ? C1 O1 1.261(10) . ? C1 C2 1.521(11) . ? C2 C3 1.495(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.391(11) . ? C3 C8 1.401(11) . ? C4 C5 1.400(11) . ? C4 C9 1.504(11) . ? C5 C6 1.390(14) . ? C5 H5 0.9300 . ? C6 C7 1.341(14) . ? C6 H6 0.9300 . ? C7 C8 1.363(14) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.524(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O3 1.235(10) . ? C10 O4 1.251(10) . ? C11 N1 1.305(9) . ? C11 N2 1.326(9) . ? C11 H11 0.9300 . ? C12 C13 1.337(11) . ? C12 N1 1.363(9) . ? C12 H12 0.9300 . ? C13 N2 1.347(10) . ? C13 H13 0.9300 . ? C14 N2 1.470(9) . ? C14 C15 1.504(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.525(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.506(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.514(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N3 1.466(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N4 1.310(9) . ? C19 N3 1.328(9) . ? C19 H19 0.9300 . ? C20 C21 1.326(11) . ? C20 N4 1.379(9) . ? C20 H20 0.9300 . ? C21 N3 1.373(10) . ? C21 H21 0.9300 . ? N4 Cd1 2.225(6) 1_545 ? O3 Cd1 2.592(6) 4_676 ? O4 Cd1 2.269(6) 4_676 ? 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 N4 Cd1 N1 115.4(2) 1_565 . ? N4 Cd1 O4 109.0(2) 1_565 4_575 ? N1 Cd1 O4 114.2(2) . 4_575 ? N4 Cd1 O2 134.0(2) 1_565 . ? N1 Cd1 O2 93.3(2) . . ? O4 Cd1 O2 88.4(2) 4_575 . ? N4 Cd1 O1 86.2(2) 1_565 . ? N1 Cd1 O1 98.8(3) . . ? O4 Cd1 O1 130.9(3) 4_575 . ? O2 Cd1 O1 52.9(2) . . ? N4 Cd1 O3 83.2(2) 1_565 4_575 ? N1 Cd1 O3 87.1(2) . 4_575 ? O4 Cd1 O3 52.5(2) 4_575 4_575 ? O2 Cd1 O3 136.1(2) . 4_575 ? O1 Cd1 O3 169.3(2) . 4_575 ? O2 C1 O1 120.4(7) . . ? O2 C1 C2 121.0(8) . . ? O1 C1 C2 118.6(7) . . ? C3 C2 C1 115.6(6) . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C8 118.1(7) . . ? C4 C3 C2 121.9(7) . . ? C8 C3 C2 120.0(8) . . ? C3 C4 C5 118.8(8) . . ? C3 C4 C9 121.4(7) . . ? C5 C4 C9 119.8(8) . . ? C6 C5 C4 120.7(9) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 120.2(9) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.2(11) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 122.0(10) . . ? C7 C8 H8 119.0 . . ? C3 C8 H8 119.0 . . ? C4 C9 C10 115.7(7) . . ? C4 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? C4 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? O3 C10 O4 121.5(8) . . ? O3 C10 C9 119.7(8) . . ? O4 C10 C9 118.8(8) . . ? N1 C11 N2 111.7(7) . . ? N1 C11 H11 124.1 . . ? N2 C11 H11 124.1 . . ? C13 C12 N1 108.6(7) . . ? C13 C12 H12 125.7 . . ? N1 C12 H12 125.7 . . ? C12 C13 N2 107.6(7) . . ? C12 C13 H13 126.2 . . ? N2 C13 H13 126.2 . . ? N2 C14 C15 113.0(7) . . ? N2 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 114.3(7) . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 114.7(7) . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C18 112.4(7) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? N3 C18 C17 111.5(7) . . ? N3 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? N3 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? N4 C19 N3 112.6(7) . . ? N4 C19 H19 123.7 . . ? N3 C19 H19 123.7 . . ? C21 C20 N4 108.8(8) . . ? C21 C20 H20 125.6 . . ? N4 C20 H20 125.6 . . ? C20 C21 N3 108.0(8) . . ? C20 C21 H21 126.0 . . ? N3 C21 H21 126.0 . . ? C11 N1 C12 105.6(7) . . ? C11 N1 Cd1 123.7(5) . . ? C12 N1 Cd1 128.9(5) . . ? C11 N2 C13 106.5(7) . . ? C11 N2 C14 125.7(7) . . ? C13 N2 C14 127.8(7) . . ? C19 N3 C21 105.4(7) . . ? C19 N3 C18 125.9(8) . . ? C21 N3 C18 128.6(8) . . ? C19 N4 C20 105.1(6) . . ? C19 N4 Cd1 124.9(5) . 1_545 ? C20 N4 Cd1 129.9(5) . 1_545 ? C1 O1 Cd1 90.7(5) . . ? C1 O2 Cd1 95.9(5) . . ? C10 O3 Cd1 85.0(5) . 4_676 ? C10 O4 Cd1 99.9(5) . 4_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -34.5(12) . . . . ? O1 C1 C2 C3 146.6(8) . . . . ? C1 C2 C3 C4 -84.0(9) . . . . ? C1 C2 C3 C8 97.1(9) . . . . ? C8 C3 C4 C5 0.9(10) . . . . ? C2 C3 C4 C5 -178.0(7) . . . . ? C8 C3 C4 C9 -178.3(7) . . . . ? C2 C3 C4 C9 2.8(10) . . . . ? C3 C4 C5 C6 -1.7(11) . . . . ? C9 C4 C5 C6 177.5(8) . . . . ? C4 C5 C6 C7 1.2(14) . . . . ? C5 C6 C7 C8 0.1(16) . . . . ? C6 C7 C8 C3 -0.9(15) . . . . ? C4 C3 C8 C7 0.4(12) . . . . ? C2 C3 C8 C7 179.3(8) . . . . ? C3 C4 C9 C10 -82.9(9) . . . . ? C5 C4 C9 C10 98.0(9) . . . . ? C4 C9 C10 O3 141.5(8) . . . . ? C4 C9 C10 O4 -38.4(11) . . . . ? N1 C12 C13 N2 0.2(9) . . . . ? N2 C14 C15 C16 59.2(10) . . . . ? C14 C15 C16 C17 60.1(10) . . . . ? C15 C16 C17 C18 69.5(9) . . . . ? C16 C17 C18 N3 -169.2(7) . . . . ? N4 C20 C21 N3 0.3(10) . . . . ? N2 C11 N1 C12 1.7(10) . . . . ? N2 C11 N1 Cd1 -164.2(5) . . . . ? C13 C12 N1 C11 -1.1(9) . . . . ? C13 C12 N1 Cd1 163.7(6) . . . . ? N4 Cd1 N1 C11 -104.7(7) 1_565 . . . ? O4 Cd1 N1 C11 127.8(7) 4_575 . . . ? O2 Cd1 N1 C11 38.2(7) . . . . ? O1 Cd1 N1 C11 -14.8(7) . . . . ? O3 Cd1 N1 C11 174.2(7) 4_575 . . . ? N4 Cd1 N1 C12 92.9(7) 1_565 . . . ? O4 Cd1 N1 C12 -34.5(8) 4_575 . . . ? O2 Cd1 N1 C12 -124.2(7) . . . . ? O1 Cd1 N1 C12 -177.2(7) . . . . ? O3 Cd1 N1 C12 11.8(7) 4_575 . . . ? N1 C11 N2 C13 -1.6(10) . . . . ? N1 C11 N2 C14 179.6(7) . . . . ? C12 C13 N2 C11 0.8(9) . . . . ? C12 C13 N2 C14 179.5(7) . . . . ? C15 C14 N2 C11 81.1(10) . . . . ? C15 C14 N2 C13 -97.4(10) . . . . ? N4 C19 N3 C21 0.3(9) . . . . ? N4 C19 N3 C18 -176.5(7) . . . . ? C20 C21 N3 C19 -0.4(9) . . . . ? C20 C21 N3 C18 176.3(8) . . . . ? C17 C18 N3 C19 114.7(9) . . . . ? C17 C18 N3 C21 -61.3(11) . . . . ? N3 C19 N4 C20 -0.1(9) . . . . ? N3 C19 N4 Cd1 -178.7(5) . . . 1_545 ? C21 C20 N4 C19 -0.1(9) . . . . ? C21 C20 N4 Cd1 178.3(6) . . . 1_545 ? O2 C1 O1 Cd1 -2.9(9) . . . . ? C2 C1 O1 Cd1 176.0(6) . . . . ? N4 Cd1 O1 C1 -155.8(6) 1_565 . . . ? N1 Cd1 O1 C1 89.0(6) . . . . ? O4 Cd1 O1 C1 -43.9(7) 4_575 . . . ? O2 Cd1 O1 C1 1.6(5) . . . . ? O3 Cd1 O1 C1 -147.9(12) 4_575 . . . ? O1 C1 O2 Cd1 3.0(9) . . . . ? C2 C1 O2 Cd1 -175.9(6) . . . . ? N4 Cd1 O2 C1 30.6(7) 1_565 . . . ? N1 Cd1 O2 C1 -100.2(5) . . . . ? O4 Cd1 O2 C1 145.7(5) 4_575 . . . ? O1 Cd1 O2 C1 -1.7(5) . . . . ? O3 Cd1 O2 C1 170.5(5) 4_575 . . . ? O4 C10 O3 Cd1 -9.4(8) . . . 4_676 ? C9 C10 O3 Cd1 170.7(7) . . . 4_676 ? O3 C10 O4 Cd1 10.8(9) . . . 4_676 ? C9 C10 O4 Cd1 -169.3(6) . . . 4_676 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.567 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.127 data_3 _database_code_depnum_ccdc_archive 'CCDC 839124' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H28 N4 O7 Zn' _chemical_formula_weight 501.83 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3845(8) _cell_length_b 9.6801(11) _cell_length_c 16.410(2) _cell_angle_alpha 86.5730(10) _cell_angle_beta 84.2020(10) _cell_angle_gamma 83.4070(10) _cell_volume 1157.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7182 _exptl_absorpt_correction_T_max 0.8514 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11388 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4081 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.03' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. The water hydrogen atoms were located from difference maps and refined with isotropic thermal parameters 1.5 times those of their carrier atoms. The disordered C20 and C21 atoms have splited over two sites with occupancy of 0.50 and 0.50. ; _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^)+(0.0548P)^2^+0.9982P] 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 4081 _refine_ls_number_parameters 307 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.154 _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 0.32968(5) 0.71472(4) 0.30718(2) 0.03529(15) Uani 1 1 d . . . O1 O 0.1968(3) 0.8946(2) 0.27678(16) 0.0493(6) Uani 1 1 d . . . O1W O 0.6901(5) 0.9140(4) 0.0755(2) 0.0793(10) Uani 1 1 d D . . H1WB H 0.651(5) 0.927(7) 0.1228(16) 0.119 Uiso 1 1 d D . . O2 O 0.4697(4) 0.9347(3) 0.21890(18) 0.0602(7) Uani 1 1 d . . . O2W O 0.3584(6) 0.8255(4) 0.0122(2) 0.0851(10) Uani 1 1 d D . . H2WB H 0.345(8) 0.909(4) -0.011(4) 0.128 Uiso 1 1 d D . . H2WA H 0.455(6) 0.822(6) 0.037(4) 0.128 Uiso 1 1 d D . . O3 O 0.1776(3) 1.5932(3) 0.38024(15) 0.0485(6) Uani 1 1 d . . . O3W O 0.0346(5) 0.7900(4) 0.1160(2) 0.0770(9) Uani 1 1 d D . . H3WB H 0.056(7) 0.766(7) 0.1638(16) 0.116 Uiso 1 1 d D . . H3WA H 0.125(6) 0.811(7) 0.085(3) 0.116 Uiso 1 1 d D . . O4 O 0.0105(3) 1.6227(3) 0.27561(16) 0.0487(6) Uani 1 1 d . . . N1 N 0.4574(3) 0.5977(3) 0.21806(16) 0.0354(6) Uani 1 1 d . . . N2 N 0.6797(4) 0.4934(3) 0.13876(17) 0.0394(7) Uani 1 1 d . . . N3 N 0.5071(4) 0.7508(3) 0.38779(17) 0.0408(7) Uani 1 1 d . . . N4 N 0.7299(5) 0.8265(5) 0.4430(2) 0.0764(13) Uani 1 1 d . . . C1 C 0.3027(5) 0.9687(4) 0.2321(2) 0.0430(8) Uani 1 1 d . . . C2 C 0.2171(6) 1.1022(4) 0.1933(3) 0.0566(10) Uani 1 1 d . . . H2A H 0.3076 1.1681 0.1862 0.068 Uiso 1 1 calc R . . H2B H 0.1869 1.0833 0.1392 0.068 Uiso 1 1 calc R . . C3 C 0.0480(5) 1.1695(3) 0.2400(2) 0.0441(8) Uani 1 1 d . . . C4 C 0.0579(5) 1.2773(3) 0.2906(2) 0.0395(8) Uani 1 1 d . . . H4 H 0.1722 1.3045 0.2971 0.047 Uiso 1 1 calc R . . C5 C -0.0964(5) 1.3462(3) 0.3320(2) 0.0378(7) Uani 1 1 d . . . C6 C -0.2650(5) 1.3035(4) 0.3229(2) 0.0482(9) Uani 1 1 d . . . H6 H -0.3704 1.3484 0.3498 0.058 Uiso 1 1 calc R . . C7 C -0.2775(6) 1.1946(4) 0.2741(3) 0.0616(12) Uani 1 1 d . . . H7 H -0.3914 1.1655 0.2689 0.074 Uiso 1 1 calc R . . C8 C -0.1230(6) 1.1284(4) 0.2329(3) 0.0581(11) Uani 1 1 d . . . H8 H -0.1336 1.0553 0.2000 0.070 Uiso 1 1 calc R . . C9 C -0.0802(5) 1.4651(4) 0.3850(2) 0.0463(9) Uani 1 1 d . . . H9A H -0.0314 1.4283 0.4356 0.056 Uiso 1 1 calc R . . H9B H -0.2011 1.5129 0.3991 0.056 Uiso 1 1 calc R . . C10 C 0.0431(4) 1.5689(3) 0.3429(2) 0.0371(8) Uani 1 1 d . . . C11 C 0.6349(4) 0.5839(4) 0.1966(2) 0.0393(8) Uani 1 1 d . . . H11 H 0.7182 0.6319 0.2193 0.047 Uiso 1 1 calc R . . C12 C 0.5243(5) 0.4443(4) 0.1213(2) 0.0476(9) Uani 1 1 d . . . H12 H 0.5143 0.3792 0.0829 0.057 Uiso 1 1 calc R . . C13 C 0.3863(5) 0.5086(4) 0.1707(2) 0.0442(8) Uani 1 1 d . . . H13 H 0.2634 0.4948 0.1724 0.053 Uiso 1 1 calc R . . C14 C 0.8668(5) 0.4536(4) 0.1017(2) 0.0493(9) Uani 1 1 d . . . H14A H 0.8874 0.3531 0.0996 0.059 Uiso 1 1 calc R . . H14B H 0.9536 0.4825 0.1361 0.059 Uiso 1 1 calc R . . C15 C 0.9006(4) 0.5175(4) 0.0170(2) 0.0408(8) Uani 1 1 d . . . H15A H 0.8724 0.6178 0.0182 0.049 Uiso 1 1 calc R . . H15B H 0.8205 0.4833 -0.0187 0.049 Uiso 1 1 calc R . . C16 C 0.6467(5) 0.8246(4) 0.3756(2) 0.0523(10) Uani 1 1 d . . . H16 H 0.6824 0.8697 0.3259 0.063 Uiso 1 1 calc R . . C17 C 0.5023(5) 0.7032(5) 0.4679(2) 0.0558(10) Uani 1 1 d . . . H17 H 0.4200 0.6450 0.4938 0.067 Uiso 1 1 calc R . . C18 C 0.6324(5) 0.7526(4) 0.5023(2) 0.0864(18) Uani 1 1 d . . . H18 H 0.6544 0.7397 0.5572 0.104 Uiso 1 1 calc R . . C19 C 0.9006(5) 0.8881(4) 0.4499(2) 0.112(2) Uani 1 1 d RDU . . H19A H 0.9543 0.9168 0.3968 0.135 Uiso 1 1 d R . . H19B H 0.9866 0.8203 0.4746 0.135 Uiso 1 1 d R . . C20 C 0.8577(5) 1.0021(4) 0.4988(2) 0.062(2) Uani 0.50 1 d PRD . . H20A H 0.8275 0.9665 0.5538 0.074 Uiso 0.50 1 d PR . . H20B H 0.7481 1.0529 0.4811 0.074 Uiso 0.50 1 d PR . . C21 C 0.9900(14) 1.1017(12) 0.5025(7) 0.093(3) Uani 0.50 1 d PDU . . H21A H 0.9482 1.1772 0.5375 0.139 Uiso 0.50 1 d PR . . H21B H 1.0256 1.1382 0.4483 0.139 Uiso 0.50 1 d PR . . H1WA H 0.8250 0.8753 0.0840 0.139 Uiso 1 1 d RD . . 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 0.0365(2) 0.0335(2) 0.0367(2) -0.00385(15) -0.00468(16) -0.00557(15) O1 0.0463(14) 0.0341(13) 0.0646(17) 0.0077(12) 0.0026(12) -0.0036(11) O1W 0.068(2) 0.104(3) 0.062(2) -0.0016(19) -0.0025(16) 0.0002(19) O2 0.0528(17) 0.0665(18) 0.0611(18) 0.0035(14) -0.0012(14) -0.0138(14) O2W 0.096(3) 0.083(2) 0.081(3) -0.0049(19) -0.018(2) -0.020(2) O3 0.0440(14) 0.0573(16) 0.0483(15) 0.0010(12) -0.0095(12) -0.0196(12) O3W 0.078(2) 0.091(3) 0.064(2) 0.0020(19) -0.0162(17) -0.0120(19) O4 0.0493(15) 0.0483(15) 0.0513(16) 0.0075(12) -0.0101(12) -0.0181(12) N1 0.0311(14) 0.0386(15) 0.0374(15) -0.0054(12) -0.0029(11) -0.0058(11) N2 0.0296(14) 0.0519(17) 0.0355(15) -0.0003(13) -0.0005(11) -0.0027(12) N3 0.0386(16) 0.0465(17) 0.0396(16) -0.0044(13) -0.0065(12) -0.0108(13) N4 0.050(2) 0.141(4) 0.049(2) -0.011(2) -0.0092(17) -0.048(2) C1 0.056(2) 0.0349(18) 0.0403(19) -0.0084(15) -0.0038(17) -0.0109(16) C2 0.082(3) 0.0342(19) 0.051(2) 0.0007(17) 0.005(2) -0.0061(19) C3 0.061(2) 0.0277(17) 0.044(2) 0.0065(15) -0.0095(17) -0.0058(16) C4 0.0427(19) 0.0348(18) 0.0434(19) 0.0048(15) -0.0097(15) -0.0125(15) C5 0.0417(19) 0.0316(17) 0.0413(18) 0.0059(14) -0.0039(15) -0.0126(14) C6 0.042(2) 0.041(2) 0.062(2) 0.0069(17) -0.0066(17) -0.0129(16) C7 0.054(2) 0.052(2) 0.087(3) 0.006(2) -0.029(2) -0.025(2) C8 0.077(3) 0.038(2) 0.066(3) -0.0052(18) -0.024(2) -0.018(2) C9 0.051(2) 0.045(2) 0.044(2) -0.0065(16) 0.0071(16) -0.0179(17) C10 0.0352(18) 0.0326(17) 0.044(2) -0.0111(15) 0.0035(15) -0.0063(14) C11 0.0338(18) 0.048(2) 0.0375(18) -0.0029(15) -0.0047(14) -0.0109(15) C12 0.046(2) 0.055(2) 0.044(2) -0.0147(17) -0.0052(16) -0.0075(17) C13 0.0325(18) 0.057(2) 0.045(2) -0.0139(17) -0.0026(15) -0.0118(16) C14 0.0346(19) 0.066(2) 0.042(2) 0.0019(18) 0.0059(15) 0.0054(17) C15 0.0349(18) 0.051(2) 0.0354(18) -0.0030(15) -0.0008(14) -0.0014(15) C16 0.048(2) 0.069(3) 0.044(2) -0.0032(18) -0.0060(17) -0.0196(19) C17 0.045(2) 0.082(3) 0.044(2) 0.001(2) -0.0044(17) -0.022(2) C18 0.063(3) 0.166(6) 0.038(2) 0.004(3) -0.012(2) -0.045(3) C19 0.088(3) 0.169(5) 0.094(3) -0.009(3) -0.020(3) -0.061(3) C20 0.069(6) 0.043(4) 0.078(6) -0.004(4) 0.000(5) -0.034(4) C21 0.101(5) 0.094(5) 0.093(5) -0.014(4) -0.027(4) -0.034(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 O1 1.962(2) . ? Zn1 O3 1.986(2) 1_545 ? Zn1 N1 1.996(3) . ? Zn1 N3 2.025(3) . ? O1 C1 1.271(4) . ? O1W H1WB 0.81(2) . ? O1W H1WA 1.0436 . ? O2 C1 1.240(4) . ? O2W H2WB 0.87(2) . ? O2W H2WA 0.85(2) . ? O3 C10 1.269(4) . ? O3 Zn1 1.986(2) 1_565 ? O3W H3WB 0.83(2) . ? O3W H3WA 0.83(2) . ? O4 C10 1.226(4) . ? N1 C11 1.316(4) . ? N1 C13 1.375(4) . ? N2 C11 1.322(4) . ? N2 C12 1.355(5) . ? N2 C14 1.470(4) . ? N3 C16 1.313(5) . ? N3 C17 1.365(5) . ? N4 C16 1.320(5) . ? N4 C18 1.369(5) . ? N4 C19 1.472(4) . ? C1 C2 1.506(5) . ? C2 C3 1.500(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.384(6) . ? C3 C4 1.385(5) . ? C4 C5 1.389(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C5 C9 1.506(5) . ? C6 C7 1.379(6) . ? C6 H6 0.9300 . ? C7 C8 1.377(6) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.522(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 H11 0.9300 . ? C12 C13 1.353(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.497(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C15 1.524(6) 2_765 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16 0.9300 . ? C17 C18 1.311(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C21 1.194(10) 2_776 ? C19 C20 1.3915 . ? C19 H19A 0.9599 . ? C19 H19B 0.9601 . ? C20 C21 1.418(12) 2_776 ? C20 C21 1.457(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C21 C19 1.194(10) 2_776 ? C21 C20 1.418(12) 2_776 ? C21 C21 1.96(2) 2_776 ? C21 H21A 0.9599 . ? C21 H21B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 113.26(11) . 1_545 ? O1 Zn1 N1 118.59(11) . . ? O3 Zn1 N1 107.00(11) 1_545 . ? O1 Zn1 N3 107.35(12) . . ? O3 Zn1 N3 98.27(11) 1_545 . ? N1 Zn1 N3 110.49(11) . . ? C1 O1 Zn1 110.1(2) . . ? H1WB O1W H1WA 99.5 . . ? H2WB O2W H2WA 106(3) . . ? C10 O3 Zn1 108.4(2) . 1_565 ? H3WB O3W H3WA 115(4) . . ? C11 N1 C13 105.4(3) . . ? C11 N1 Zn1 125.5(2) . . ? C13 N1 Zn1 128.9(2) . . ? C11 N2 C12 107.8(3) . . ? C11 N2 C14 125.2(3) . . ? C12 N2 C14 127.0(3) . . ? C16 N3 C17 105.8(3) . . ? C16 N3 Zn1 128.3(3) . . ? C17 N3 Zn1 125.9(2) . . ? C16 N4 C18 106.2(3) . . ? C16 N4 C19 126.1(3) . . ? C18 N4 C19 127.6(4) . . ? O2 C1 O1 122.9(3) . . ? O2 C1 C2 119.9(3) . . ? O1 C1 C2 117.2(3) . . ? C3 C2 C1 115.6(3) . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C8 C3 C4 117.7(4) . . ? C8 C3 C2 121.5(4) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 122.4(3) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 118.3(3) . . ? C6 C5 C9 120.9(3) . . ? C4 C5 C9 120.8(3) . . ? C5 C6 C7 120.2(4) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 120.7(4) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? C5 C9 C10 112.4(3) . . ? C5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? O4 C10 O3 123.6(3) . . ? O4 C10 C9 119.6(3) . . ? O3 C10 C9 116.7(3) . . ? N1 C11 N2 111.5(3) . . ? N1 C11 H11 124.3 . . ? N2 C11 H11 124.3 . . ? C13 C12 N2 106.3(3) . . ? C13 C12 H12 126.8 . . ? N2 C12 H12 126.8 . . ? C12 C13 N1 108.9(3) . . ? C12 C13 H13 125.5 . . ? N1 C13 H13 125.5 . . ? N2 C14 C15 112.4(3) . . ? N2 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N2 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C15 110.9(4) . 2_765 ? C14 C15 H15A 109.5 . . ? C15 C15 H15A 109.5 2_765 . ? C14 C15 H15B 109.5 . . ? C15 C15 H15B 109.5 2_765 . ? H15A C15 H15B 108.1 . . ? N3 C16 N4 111.2(4) . . ? N3 C16 H16 124.4 . . ? N4 C16 H16 124.4 . . ? C18 C17 N3 109.0(3) . . ? C18 C17 H17 125.5 . . ? N3 C17 H17 125.5 . . ? C17 C18 N4 107.7(3) . . ? C17 C18 H18 126.2 . . ? N4 C18 H18 126.2 . . ? C21 C19 C20 66.0(6) 2_776 . ? C21 C19 N4 141.4(7) 2_776 . ? C20 C19 N4 107.7(2) . . ? C21 C19 H19A 107.0 2_776 . ? C20 C19 H19A 110.2 . . ? N4 C19 H19A 110.6 . . ? C21 C19 H19B 48.2 2_776 . ? C20 C19 H19B 110.2 . . ? N4 C19 H19B 109.6 . . ? H19A C19 H19B 108.5 . . ? C21 C20 C19 50.3(4) 2_776 . ? C21 C20 C21 86.1(7) 2_776 . ? C19 C20 C21 120.2(5) . . ? C21 C20 H20A 85.6 2_776 . ? C19 C20 H20A 107.2 . . ? C21 C20 H20A 107.5 . . ? C21 C20 H20B 157.3 2_776 . ? C19 C20 H20B 107.2 . . ? C21 C20 H20B 107.3 . . ? H20A C20 H20B 106.8 . . ? C19 C21 C20 63.7(5) 2_776 2_776 ? C19 C21 C20 131.8(10) 2_776 . ? C20 C21 C20 93.9(7) 2_776 . ? C19 C21 C21 100.1(9) 2_776 2_776 ? C20 C21 C21 47.8(5) 2_776 2_776 ? C20 C21 C21 46.1(4) . 2_776 ? C19 C21 H21A 69.9 2_776 . ? C20 C21 H21A 133.3 2_776 . ? C20 C21 H21A 114.3 . . ? C21 C21 H21A 143.3 2_776 . ? C19 C21 H21B 113.2 2_776 . ? C20 C21 H21B 93.1 2_776 . ? C20 C21 H21B 109.9 . . ? C21 C21 H21B 106.9 2_776 . ? H21A C21 H21B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C1 178.2(2) 1_545 . . . ? N1 Zn1 O1 C1 -55.2(3) . . . . ? N3 Zn1 O1 C1 70.8(3) . . . . ? O1 Zn1 N1 C11 102.9(3) . . . . ? O3 Zn1 N1 C11 -127.5(3) 1_545 . . . ? N3 Zn1 N1 C11 -21.6(3) . . . . ? O1 Zn1 N1 C13 -82.1(3) . . . . ? O3 Zn1 N1 C13 47.4(3) 1_545 . . . ? N3 Zn1 N1 C13 153.4(3) . . . . ? O1 Zn1 N3 C16 -63.5(3) . . . . ? O3 Zn1 N3 C16 178.9(3) 1_545 . . . ? N1 Zn1 N3 C16 67.2(4) . . . . ? O1 Zn1 N3 C17 115.4(3) . . . . ? O3 Zn1 N3 C17 -2.2(3) 1_545 . . . ? N1 Zn1 N3 C17 -113.9(3) . . . . ? Zn1 O1 C1 O2 -7.5(4) . . . . ? Zn1 O1 C1 C2 171.6(3) . . . . ? O2 C1 C2 C3 -151.8(4) . . . . ? O1 C1 C2 C3 29.1(5) . . . . ? C1 C2 C3 C8 -83.6(5) . . . . ? C1 C2 C3 C4 97.6(4) . . . . ? C8 C3 C4 C5 -1.6(5) . . . . ? C2 C3 C4 C5 177.2(3) . . . . ? C3 C4 C5 C6 1.0(5) . . . . ? C3 C4 C5 C9 -178.6(3) . . . . ? C4 C5 C6 C7 0.4(5) . . . . ? C9 C5 C6 C7 179.9(4) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? C6 C7 C8 C3 0.3(6) . . . . ? C4 C3 C8 C7 1.0(6) . . . . ? C2 C3 C8 C7 -177.8(4) . . . . ? C6 C5 C9 C10 -133.1(4) . . . . ? C4 C5 C9 C10 46.5(5) . . . . ? Zn1 O3 C10 O4 -5.2(4) 1_565 . . . ? Zn1 O3 C10 C9 173.9(2) 1_565 . . . ? C5 C9 C10 O4 55.3(5) . . . . ? C5 C9 C10 O3 -123.8(3) . . . . ? C13 N1 C11 N2 0.5(4) . . . . ? Zn1 N1 C11 N2 176.4(2) . . . . ? C12 N2 C11 N1 -0.3(4) . . . . ? C14 N2 C11 N1 -179.6(3) . . . . ? C11 N2 C12 C13 -0.1(4) . . . . ? C14 N2 C12 C13 179.2(3) . . . . ? N2 C12 C13 N1 0.4(4) . . . . ? C11 N1 C13 C12 -0.5(4) . . . . ? Zn1 N1 C13 C12 -176.3(2) . . . . ? C11 N2 C14 C15 -105.2(4) . . . . ? C12 N2 C14 C15 75.7(5) . . . . ? N2 C14 C15 C15 175.9(4) . . . 2_765 ? C17 N3 C16 N4 -0.1(5) . . . . ? Zn1 N3 C16 N4 179.0(3) . . . . ? C18 N4 C16 N3 -2.0(5) . . . . ? C19 N4 C16 N3 174.1(4) . . . . ? C16 N3 C17 C18 2.3(5) . . . . ? Zn1 N3 C17 C18 -176.9(3) . . . . ? N3 C17 C18 N4 -3.5(5) . . . . ? C16 N4 C18 C17 3.4(6) . . . . ? C19 N4 C18 C17 -172.7(4) . . . . ? C16 N4 C19 C21 -173.6(10) . . . 2_776 ? C18 N4 C19 C21 1.7(14) . . . 2_776 ? C16 N4 C19 C20 112.9(5) . . . . ? C18 N4 C19 C20 -71.8(6) . . . . ? N4 C19 C20 C21 139.1(7) . . . 2_776 ? C21 C19 C20 C21 54.2(11) 2_776 . . . ? N4 C19 C20 C21 -166.7(6) . . . . ? C21 C20 C21 C19 -57.7(10) 2_776 . . 2_776 ? C19 C20 C21 C19 -96.3(12) . . . 2_776 ? C21 C20 C21 C20 0.000(1) 2_776 . . 2_776 ? C19 C20 C21 C20 -38.7(8) . . . 2_776 ? C19 C20 C21 C21 -38.7(8) . . . 2_776 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.263 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.064 data_4 _database_code_depnum_ccdc_archive 'CCDC 839125' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Cd N2 O5' _chemical_formula_weight 431.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7106(9) _cell_length_b 10.4086(10) _cell_length_c 10.9644(11) _cell_angle_alpha 64.4050(10) _cell_angle_beta 69.9560(10) _cell_angle_gamma 77.723(2) _cell_volume 839.79(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.787 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4458 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2961 _reflns_number_gt 2777 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.1' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. The water hydrogen atoms were located from difference maps and refined with isotropic thermal parameters 1.5 times those of their carrier atoms. ; _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^)+(0.0194P)^2^+0.4810P] 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 2961 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.22908(2) 0.086448(18) 0.088483(18) 0.02741(7) Uani 1 1 d . . . C1 C 0.4972(3) -0.1445(3) 0.2009(2) 0.0262(5) Uani 1 1 d . . . C2 C 0.3827(3) -0.2430(3) 0.3335(2) 0.0306(5) Uani 1 1 d . . . H2A H 0.2703 -0.2147 0.3300 0.037 Uiso 1 1 calc R . . H2B H 0.4084 -0.3403 0.3390 0.037 Uiso 1 1 calc R . . C3 C 0.4012(3) -0.2356(3) 0.4630(2) 0.0287(5) Uani 1 1 d . . . C4 C 0.3178(3) -0.1272(3) 0.5076(2) 0.0288(5) Uani 1 1 d . . . H4 H 0.2438 -0.0630 0.4616 0.035 Uiso 1 1 calc R . . C5 C 0.3426(3) -0.1125(3) 0.6195(2) 0.0311(6) Uani 1 1 d . . . C6 C 0.4491(3) -0.2108(3) 0.6897(3) 0.0409(7) Uani 1 1 d . . . H6 H 0.4661 -0.2027 0.7652 0.049 Uiso 1 1 calc R . . C7 C 0.5305(4) -0.3210(3) 0.6487(3) 0.0459(7) Uani 1 1 d . . . H7 H 0.6005 -0.3876 0.6977 0.055 Uiso 1 1 calc R . . C8 C 0.5085(3) -0.3327(3) 0.5350(3) 0.0377(6) Uani 1 1 d . . . H8 H 0.5658 -0.4060 0.5065 0.045 Uiso 1 1 calc R . . C9 C 0.2540(3) 0.0102(3) 0.6618(3) 0.0377(6) Uani 1 1 d . . . H9A H 0.2504 0.0957 0.5779 0.045 Uiso 1 1 calc R . . H9B H 0.3135 0.0285 0.7123 0.045 Uiso 1 1 calc R . . C10 C 0.0808(3) -0.0234(3) 0.7548(3) 0.0315(6) Uani 1 1 d . . . C11 C 0.0652(3) 0.3509(3) 0.1766(3) 0.0404(7) Uani 1 1 d . . . H11 H -0.0227 0.2973 0.2404 0.049 Uiso 1 1 calc R . . C12 C 0.2165(4) 0.5284(3) 0.0498(3) 0.0536(8) Uani 1 1 d . . . H12 H 0.2554 0.6187 0.0085 0.064 Uiso 1 1 calc R . . C13 C 0.2947(4) 0.4125(3) 0.0253(3) 0.0489(8) Uani 1 1 d . . . H13 H 0.3981 0.4095 -0.0371 0.059 Uiso 1 1 calc R . . C14 C -0.0599(4) 0.5813(3) 0.2028(3) 0.0495(8) Uani 1 1 d . . . H14A H -0.1620 0.5352 0.2457 0.059 Uiso 1 1 calc R . . H14B H -0.0751 0.6706 0.1258 0.059 Uiso 1 1 calc R . . C15 C -0.0214(4) 0.6128(3) 0.3116(3) 0.0461(7) Uani 1 1 d . . . H15A H 0.0835 0.6542 0.2698 0.055 Uiso 1 1 calc R . . H15B H -0.1040 0.6832 0.3361 0.055 Uiso 1 1 calc R . . C16 C -0.0153(4) 0.4830(3) 0.4444(3) 0.0421(7) Uani 1 1 d . . . H16A H 0.0711 0.4144 0.4207 0.051 Uiso 1 1 calc R . . H16B H -0.1183 0.4388 0.4839 0.051 Uiso 1 1 calc R . . H5B H 0.198(4) -0.109(4) -0.009(4) 0.063 Uiso 1 1 d . . . N1 N 0.1997(3) 0.2997(2) 0.1056(2) 0.0364(5) Uani 1 1 d . . . N2 N 0.0699(3) 0.4890(2) 0.1461(2) 0.0369(5) Uani 1 1 d . . . O1 O 0.45765(19) -0.01120(16) 0.15921(16) 0.0265(4) Uani 1 1 d . . . O2 O 0.6266(2) -0.19957(19) 0.14209(18) 0.0381(4) Uani 1 1 d . . . O3 O 0.0566(2) -0.0934(2) 0.88595(18) 0.0377(4) Uani 1 1 d . . . O4 O -0.0331(2) 0.0147(2) 0.69941(19) 0.0444(5) Uani 1 1 d . . . O5 O 0.2642(2) -0.1142(2) 0.03250(19) 0.0350(4) Uani 1 1 d . . . H5A H 0.3492 -0.1106 -0.0312 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02325(10) 0.02890(11) 0.02819(11) -0.01291(8) -0.00428(7) 0.00051(7) C1 0.0271(13) 0.0335(14) 0.0213(12) -0.0119(11) -0.0084(10) -0.0042(10) C2 0.0348(14) 0.0262(13) 0.0291(13) -0.0112(11) -0.0038(11) -0.0072(11) C3 0.0258(13) 0.0305(13) 0.0228(12) -0.0076(10) 0.0008(10) -0.0075(10) C4 0.0244(12) 0.0313(13) 0.0262(13) -0.0097(11) -0.0026(10) -0.0046(10) C5 0.0228(12) 0.0398(14) 0.0267(13) -0.0154(11) 0.0058(10) -0.0109(11) C6 0.0379(15) 0.0573(18) 0.0275(14) -0.0157(13) -0.0070(12) -0.0092(14) C7 0.0444(17) 0.0476(17) 0.0370(16) -0.0076(14) -0.0182(13) 0.0051(14) C8 0.0375(15) 0.0320(14) 0.0359(15) -0.0116(12) -0.0052(12) 0.0004(12) C9 0.0314(14) 0.0460(16) 0.0377(15) -0.0241(13) 0.0039(12) -0.0129(12) C10 0.0300(14) 0.0351(14) 0.0348(15) -0.0236(12) -0.0012(11) -0.0047(11) C11 0.0416(16) 0.0392(16) 0.0409(16) -0.0215(13) -0.0033(13) -0.0050(13) C12 0.063(2) 0.0373(16) 0.0534(19) -0.0198(15) 0.0019(16) -0.0160(15) C13 0.0445(17) 0.0468(17) 0.0518(18) -0.0262(15) 0.0041(14) -0.0111(14) C14 0.0579(19) 0.0463(17) 0.0525(18) -0.0307(15) -0.0259(15) 0.0219(15) C15 0.060(2) 0.0365(16) 0.0430(17) -0.0220(13) -0.0110(14) 0.0019(14) C16 0.0456(16) 0.0404(16) 0.0402(16) -0.0201(13) -0.0038(13) -0.0077(13) N1 0.0381(13) 0.0337(12) 0.0382(13) -0.0186(10) -0.0056(10) -0.0029(10) N2 0.0448(14) 0.0336(12) 0.0376(13) -0.0203(10) -0.0151(11) 0.0063(10) O1 0.0250(8) 0.0242(9) 0.0292(9) -0.0097(7) -0.0081(7) -0.0008(7) O2 0.0381(11) 0.0331(10) 0.0292(10) -0.0118(8) 0.0001(8) 0.0080(8) O3 0.0290(10) 0.0538(12) 0.0309(10) -0.0177(9) -0.0039(8) -0.0097(8) O4 0.0326(10) 0.0611(13) 0.0346(11) -0.0154(10) -0.0072(9) -0.0050(9) O5 0.0321(10) 0.0428(11) 0.0334(10) -0.0191(9) -0.0058(8) -0.0062(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 Cd1 N1 2.261(2) . ? Cd1 O1 2.2617(16) . ? Cd1 O2 2.2884(17) 2_655 ? Cd1 O4 2.3147(18) 2_556 ? Cd1 O5 2.3531(18) . ? Cd1 O3 2.3961(17) 2_556 ? Cd1 C10 2.696(2) 2_556 ? C1 O2 1.250(3) . ? C1 O1 1.269(3) . ? C1 C2 1.521(3) . ? C2 C3 1.518(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.387(3) . ? C3 C8 1.391(4) . ? C4 C5 1.391(3) . ? C4 H4 0.9300 . ? C5 C6 1.380(4) . ? C5 C9 1.513(3) . ? C6 C7 1.379(4) . ? C6 H6 0.9300 . ? C7 C8 1.383(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.516(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O4 1.244(3) . ? C10 O3 1.263(3) . ? C10 Cd1 2.696(2) 2_556 ? C11 N1 1.315(3) . ? C11 N2 1.335(3) . ? C11 H11 0.9300 . ? C12 C13 1.340(4) . ? C12 N2 1.356(4) . ? C12 H12 0.9300 . ? C13 N1 1.364(4) . ? C13 H13 0.9300 . ? C14 N2 1.469(3) . ? C14 C15 1.517(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.507(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C16 1.522(5) 2_566 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? O2 Cd1 2.2884(17) 2_655 ? O3 Cd1 2.3961(17) 2_556 ? O4 Cd1 2.3147(18) 2_556 ? O5 H5B 0.82(3) . ? O5 H5A 0.8200 . ? 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 100.18(7) . . ? N1 Cd1 O2 86.45(7) . 2_655 ? O1 Cd1 O2 93.48(6) . 2_655 ? N1 Cd1 O4 94.17(8) . 2_556 ? O1 Cd1 O4 99.26(6) . 2_556 ? O2 Cd1 O4 166.92(7) 2_655 2_556 ? N1 Cd1 O5 170.94(7) . . ? O1 Cd1 O5 84.21(6) . . ? O2 Cd1 O5 85.37(6) 2_655 . ? O4 Cd1 O5 92.93(7) 2_556 . ? N1 Cd1 O3 92.52(7) . 2_556 ? O1 Cd1 O3 152.62(6) . 2_556 ? O2 Cd1 O3 111.56(6) 2_655 2_556 ? O4 Cd1 O3 55.36(6) 2_556 2_556 ? O5 Cd1 O3 86.88(6) . 2_556 ? N1 Cd1 C10 93.88(8) . 2_556 ? O1 Cd1 C10 126.05(7) . 2_556 ? O2 Cd1 C10 139.49(7) 2_655 2_556 ? O4 Cd1 C10 27.43(7) 2_556 2_556 ? O5 Cd1 C10 89.83(7) . 2_556 ? O3 Cd1 C10 27.94(7) 2_556 2_556 ? O2 C1 O1 124.0(2) . . ? O2 C1 C2 118.0(2) . . ? O1 C1 C2 118.0(2) . . ? C3 C2 C1 110.0(2) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C8 118.6(2) . . ? C4 C3 C2 120.6(2) . . ? C8 C3 C2 120.7(2) . . ? C3 C4 C5 121.4(2) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 118.8(2) . . ? C6 C5 C9 121.2(2) . . ? C4 C5 C9 119.9(2) . . ? C7 C6 C5 120.5(2) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 120.3(3) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C5 C9 C10 111.0(2) . . ? C5 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C5 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O4 C10 O3 121.7(2) . . ? O4 C10 C9 119.2(2) . . ? O3 C10 C9 119.1(2) . . ? O4 C10 Cd1 58.96(13) . 2_556 ? O3 C10 Cd1 62.70(13) . 2_556 ? C9 C10 Cd1 177.43(18) . 2_556 ? N1 C11 N2 112.0(3) . . ? N1 C11 H11 124.0 . . ? N2 C11 H11 124.0 . . ? C13 C12 N2 106.9(3) . . ? C13 C12 H12 126.5 . . ? N2 C12 H12 126.5 . . ? C12 C13 N1 109.8(3) . . ? C12 C13 H13 125.1 . . ? N1 C13 H13 125.1 . . ? N2 C14 C15 112.6(2) . . ? N2 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N2 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 113.7(2) . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 C16 113.2(3) . 2_566 ? C15 C16 H16A 108.9 . . ? C16 C16 H16A 108.9 2_566 . ? C15 C16 H16B 108.9 . . ? C16 C16 H16B 108.9 2_566 . ? H16A C16 H16B 107.7 . . ? C11 N1 C13 104.9(2) . . ? C11 N1 Cd1 124.70(19) . . ? C13 N1 Cd1 128.92(18) . . ? C11 N2 C12 106.4(2) . . ? C11 N2 C14 126.8(3) . . ? C12 N2 C14 126.7(3) . . ? C1 O1 Cd1 122.14(15) . . ? C1 O2 Cd1 122.71(15) . 2_655 ? C10 O3 Cd1 89.36(15) . 2_556 ? C10 O4 Cd1 93.61(15) . 2_556 ? Cd1 O5 H5B 111(2) . . ? Cd1 O5 H5A 109.5 . . ? H5B O5 H5A 98.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 102.3(2) . . . . ? O1 C1 C2 C3 -75.7(3) . . . . ? C1 C2 C3 C4 83.1(3) . . . . ? C1 C2 C3 C8 -93.5(3) . . . . ? C8 C3 C4 C5 1.5(4) . . . . ? C2 C3 C4 C5 -175.2(2) . . . . ? C3 C4 C5 C6 -1.9(4) . . . . ? C3 C4 C5 C9 177.8(2) . . . . ? C4 C5 C6 C7 0.5(4) . . . . ? C9 C5 C6 C7 -179.2(2) . . . . ? C5 C6 C7 C8 1.2(4) . . . . ? C6 C7 C8 C3 -1.5(4) . . . . ? C4 C3 C8 C7 0.2(4) . . . . ? C2 C3 C8 C7 176.9(2) . . . . ? C6 C5 C9 C10 -98.6(3) . . . . ? C4 C5 C9 C10 81.7(3) . . . . ? C5 C9 C10 O4 -92.8(3) . . . . ? C5 C9 C10 O3 84.9(3) . . . . ? C5 C9 C10 Cd1 -50(4) . . . 2_556 ? N2 C12 C13 N1 -0.3(4) . . . . ? N2 C14 C15 C16 -65.7(4) . . . . ? C14 C15 C16 C16 -177.2(3) . . . 2_566 ? N2 C11 N1 C13 -0.2(3) . . . . ? N2 C11 N1 Cd1 -167.35(17) . . . . ? C12 C13 N1 C11 0.3(4) . . . . ? C12 C13 N1 Cd1 166.7(2) . . . . ? O1 Cd1 N1 C11 -126.6(2) . . . . ? O2 Cd1 N1 C11 140.5(2) 2_655 . . . ? O4 Cd1 N1 C11 -26.4(2) 2_556 . . . ? O5 Cd1 N1 C11 115.0(4) . . . . ? O3 Cd1 N1 C11 29.0(2) 2_556 . . . ? C10 Cd1 N1 C11 1.1(2) 2_556 . . . ? O1 Cd1 N1 C13 69.4(3) . . . . ? O2 Cd1 N1 C13 -23.5(3) 2_655 . . . ? O4 Cd1 N1 C13 169.6(2) 2_556 . . . ? O5 Cd1 N1 C13 -49.0(6) . . . . ? O3 Cd1 N1 C13 -135.0(3) 2_556 . . . ? C10 Cd1 N1 C13 -162.9(3) 2_556 . . . ? N1 C11 N2 C12 0.0(3) . . . . ? N1 C11 N2 C14 178.4(2) . . . . ? C13 C12 N2 C11 0.2(4) . . . . ? C13 C12 N2 C14 -178.2(3) . . . . ? C15 C14 N2 C11 105.4(3) . . . . ? C15 C14 N2 C12 -76.5(4) . . . . ? O2 C1 O1 Cd1 118.6(2) . . . . ? C2 C1 O1 Cd1 -63.5(2) . . . . ? N1 Cd1 O1 C1 161.43(17) . . . . ? O2 Cd1 O1 C1 -111.56(17) 2_655 . . . ? O4 Cd1 O1 C1 65.45(18) 2_556 . . . ? O5 Cd1 O1 C1 -26.58(17) . . . . ? O3 Cd1 O1 C1 45.1(2) 2_556 . . . ? C10 Cd1 O1 C1 58.97(19) 2_556 . . . ? O1 C1 O2 Cd1 -22.2(3) . . . 2_655 ? C2 C1 O2 Cd1 159.89(16) . . . 2_655 ? O4 C10 O3 Cd1 -0.4(2) . . . 2_556 ? C9 C10 O3 Cd1 -177.9(2) . . . 2_556 ? O3 C10 O4 Cd1 0.4(3) . . . 2_556 ? C9 C10 O4 Cd1 177.95(19) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.321 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.060 data_5 _database_code_depnum_ccdc_archive 'CCDC 839126' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 Cd N4 O5' _chemical_formula_weight 498.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.413(9) _cell_length_b 17.212(13) _cell_length_c 11.724(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.240(7) _cell_angle_gamma 90.00 _cell_volume 2066(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12759 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3528 _reflns_number_gt 3196 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.03' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. The water hydrogen atoms were located from difference maps and refined with isotropic thermal parameters 1.5 times those of their carrier atoms. ; _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^)+(0.0448P)^2^+0.6869P] 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 SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3528 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _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 0.884027(16) 0.165871(11) 1.088313(16) 0.03406(10) Uani 1 1 d . . . C1 C 0.7360(2) 0.27633(16) 1.1371(3) 0.0421(6) Uani 1 1 d . . . C2 C 0.6350(3) 0.33155(16) 1.1453(3) 0.0516(8) Uani 1 1 d . . . H2A H 0.6574 0.3424 1.2337 0.062 Uiso 1 1 calc R . . H2B H 0.6349 0.3802 1.1037 0.062 Uiso 1 1 calc R . . C3 C 0.5004(2) 0.29483(15) 1.0817(3) 0.0402(6) Uani 1 1 d . . . C4 C 0.4578(3) 0.24325(16) 1.1479(3) 0.0436(6) Uani 1 1 d . . . H4 H 0.5122 0.2324 1.2328 0.052 Uiso 1 1 calc R . . C5 C 0.3357(3) 0.20794(15) 1.0893(3) 0.0410(6) Uani 1 1 d . . . H5 H 0.3098 0.1742 1.1357 0.049 Uiso 1 1 calc R . . C6 C 0.2522(2) 0.22231(15) 0.9626(2) 0.0380(6) Uani 1 1 d . . . C7 C 0.2935(3) 0.27404(17) 0.8965(3) 0.0471(7) Uani 1 1 d . . . H7 H 0.2387 0.2850 0.8118 0.056 Uiso 1 1 calc R . . C8 C 0.4156(3) 0.30963(17) 0.9552(3) 0.0470(7) Uani 1 1 d . . . H8 H 0.4407 0.3440 0.9089 0.056 Uiso 1 1 calc R . . C9 C 0.1224(3) 0.18071(19) 0.8972(3) 0.0472(7) Uani 1 1 d . . . H9A H 0.1385 0.1290 0.8744 0.057 Uiso 1 1 calc R . . H9B H 0.0695 0.2080 0.8187 0.057 Uiso 1 1 calc R . . C10 C 0.0426(3) 0.17270(15) 0.9724(3) 0.0380(6) Uani 1 1 d . . . C11 C 0.5822(2) 0.10944(16) 0.9425(2) 0.0396(6) Uani 1 1 d . . . H11 H 0.5548 0.1547 0.9669 0.048 Uiso 1 1 calc R . . C12 C 0.5778(3) -0.00260(16) 0.8544(3) 0.0479(7) Uani 1 1 d . . . H12 H 0.5490 -0.0483 0.8079 0.058 Uiso 1 1 calc R . . C13 C 0.7020(3) 0.02064(17) 0.9199(3) 0.0469(7) Uani 1 1 d . . . H13 H 0.7748 -0.0070 0.9268 0.056 Uiso 1 1 calc R . . C14 C 0.3579(2) 0.05619(17) 0.8088(2) 0.0422(6) Uani 1 1 d . . . H14A H 0.3287 0.0970 0.8472 0.051 Uiso 1 1 calc R . . H14B H 0.3246 0.0071 0.8231 0.051 Uiso 1 1 calc R . . C15 C 0.3041(2) 0.07075(16) 0.6670(2) 0.0400(6) Uani 1 1 d . . . H15A H 0.3279 0.1227 0.6527 0.048 Uiso 1 1 calc R . . H15B H 0.3424 0.0340 0.6305 0.048 Uiso 1 1 calc R . . C16 C 0.1568(2) 0.06245(17) 0.6020(2) 0.0423(6) Uani 1 1 d . . . H16A H 0.1322 0.0149 0.6301 0.051 Uiso 1 1 calc R . . H16B H 0.1177 0.1057 0.6258 0.051 Uiso 1 1 calc R . . C17 C 0.0298(2) 0.11409(14) 0.3813(2) 0.0352(6) Uani 1 1 d . . . H17 H -0.0014 0.1581 0.4048 0.042 Uiso 1 1 calc R . . C18 C 0.0685(3) 0.02662(16) 0.2699(3) 0.0450(7) Uani 1 1 d . . . H18 H 0.0682 -0.0003 0.2010 0.054 Uiso 1 1 calc R . . C19 C 0.1321(3) 0.00428(17) 0.3929(3) 0.0472(7) Uani 1 1 d . . . H19 H 0.1826 -0.0402 0.4241 0.057 Uiso 1 1 calc R . . H5A H 0.705(4) 0.357(2) 0.899(4) 0.071 Uiso 1 1 d . . . H5B H 0.712(4) 0.354(3) 0.812(4) 0.071 Uiso 1 1 d . . . N1 N 0.7054(2) 0.09166(13) 0.9755(2) 0.0407(5) Uani 1 1 d . . . N2 N 0.50137(19) 0.05406(12) 0.86927(19) 0.0372(5) Uani 1 1 d . . . N3 N 0.10713(19) 0.06077(12) 0.46294(19) 0.0359(5) Uani 1 1 d . . . N4 N 0.00370(18) 0.09598(12) 0.26272(18) 0.0374(5) Uani 1 1 d . . . O1 O 0.7647(3) 0.28280(14) 1.0473(3) 0.0765(7) Uani 1 1 d . . . O2 O 0.7821(3) 0.22331(15) 1.2153(2) 0.0742(7) Uani 1 1 d . . . O3 O 0.0415(2) 0.22700(11) 1.0440(2) 0.0498(5) Uani 1 1 d . . . O4 O -0.0220(2) 0.11235(14) 0.9589(2) 0.0692(7) Uani 1 1 d . . . O5 O 0.6882(3) 0.38349(15) 0.8441(3) 0.0752(8) 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 0.02659(13) 0.04407(15) 0.03165(14) 0.00253(7) 0.01300(9) -0.00045(7) C1 0.0329(13) 0.0479(16) 0.0450(15) -0.0073(12) 0.0167(12) -0.0044(12) C2 0.0466(17) 0.0484(17) 0.065(2) -0.0120(13) 0.0291(15) -0.0008(12) C3 0.0384(13) 0.0379(14) 0.0530(16) -0.0049(12) 0.0281(12) 0.0069(11) C4 0.0416(15) 0.0467(15) 0.0435(15) 0.0049(12) 0.0197(12) 0.0126(12) C5 0.0420(14) 0.0402(14) 0.0500(16) 0.0090(12) 0.0288(12) 0.0077(12) C6 0.0349(13) 0.0430(14) 0.0437(14) 0.0022(11) 0.0244(11) 0.0088(11) C7 0.0417(15) 0.0629(18) 0.0421(15) 0.0119(13) 0.0235(12) 0.0076(13) C8 0.0455(16) 0.0538(16) 0.0548(17) 0.0103(14) 0.0341(14) 0.0029(14) C9 0.0456(17) 0.0562(17) 0.0493(17) -0.0038(13) 0.0299(15) -0.0017(13) C10 0.0348(14) 0.0439(15) 0.0376(14) 0.0029(11) 0.0181(12) 0.0038(11) C11 0.0328(13) 0.0446(14) 0.0357(13) -0.0061(11) 0.0098(11) 0.0004(11) C12 0.0434(15) 0.0414(15) 0.0530(16) -0.0084(13) 0.0158(13) 0.0016(12) C13 0.0383(14) 0.0489(16) 0.0507(16) 0.0006(13) 0.0171(13) 0.0089(12) C14 0.0299(12) 0.0546(16) 0.0373(14) -0.0027(12) 0.0105(11) -0.0040(11) C15 0.0333(13) 0.0459(15) 0.0365(13) 0.0056(11) 0.0116(11) -0.0091(11) C16 0.0339(13) 0.0582(17) 0.0309(13) 0.0033(12) 0.0107(11) -0.0028(12) C17 0.0313(12) 0.0345(13) 0.0369(13) -0.0002(10) 0.0125(10) -0.0013(10) C18 0.0453(15) 0.0507(16) 0.0410(15) -0.0057(12) 0.0209(13) 0.0051(13) C19 0.0446(15) 0.0451(16) 0.0508(16) 0.0038(13) 0.0202(13) 0.0155(13) N1 0.0320(11) 0.0506(13) 0.0356(11) -0.0020(10) 0.0113(9) -0.0008(10) N2 0.0314(10) 0.0426(12) 0.0326(11) -0.0022(9) 0.0096(9) -0.0016(9) N3 0.0302(10) 0.0423(12) 0.0311(10) 0.0014(9) 0.0097(8) -0.0006(9) N4 0.0327(11) 0.0418(12) 0.0333(11) 0.0022(9) 0.0106(9) 0.0028(9) O1 0.0980(19) 0.0738(16) 0.0911(18) 0.0287(14) 0.0722(16) 0.0362(14) O2 0.0823(17) 0.0843(17) 0.0639(14) 0.0235(13) 0.0395(13) 0.0352(14) O3 0.0591(12) 0.0428(11) 0.0672(13) -0.0033(9) 0.0460(11) -0.0014(9) O4 0.0793(15) 0.0710(15) 0.0839(17) -0.0307(12) 0.0602(14) -0.0342(13) O5 0.099(2) 0.0495(15) 0.0696(18) -0.0015(12) 0.0300(16) 0.0046(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 Cd1 N4 2.242(2) 1_656 ? Cd1 N1 2.270(2) . ? Cd1 O3 2.331(2) 1_655 ? Cd1 O1 2.357(3) . ? Cd1 O4 2.396(2) 1_655 ? Cd1 O2 2.465(3) . ? Cd1 C10 2.703(3) 1_655 ? C1 O2 1.234(3) . ? C1 O1 1.238(4) . ? C1 C2 1.530(4) . ? C2 C3 1.517(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.389(4) . ? C3 C4 1.400(4) . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 C7 1.393(4) . ? C6 C9 1.514(4) . ? C7 C8 1.393(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.529(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O4 1.243(3) . ? C10 O3 1.260(3) . ? C10 Cd1 2.703(3) 1_455 ? C11 N1 1.319(3) . ? C11 N2 1.340(3) . ? C11 H11 0.9300 . ? C12 C13 1.341(4) . ? C12 N2 1.370(4) . ? C12 H12 0.9300 . ? C13 N1 1.378(4) . ? C13 H13 0.9300 . ? C14 N2 1.469(3) . ? C14 C15 1.517(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.514(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N3 1.470(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N4 1.324(3) . ? C17 N3 1.338(3) . ? C17 H17 0.9300 . ? C18 C19 1.352(4) . ? C18 N4 1.387(3) . ? C18 H18 0.9300 . ? C19 N3 1.381(4) . ? C19 H19 0.9300 . ? N4 Cd1 2.242(2) 1_454 ? O3 Cd1 2.331(2) 1_455 ? O4 Cd1 2.396(2) 1_455 ? O5 H5A 0.74(4) . ? O5 H5B 0.75(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 N4 Cd1 N1 104.92(9) 1_656 . ? N4 Cd1 O3 103.10(9) 1_656 1_655 ? N1 Cd1 O3 134.97(9) . 1_655 ? N4 Cd1 O1 135.10(9) 1_656 . ? N1 Cd1 O1 94.17(10) . . ? O3 Cd1 O1 90.10(9) 1_655 . ? N4 Cd1 O4 96.22(10) 1_656 1_655 ? N1 Cd1 O4 87.30(9) . 1_655 ? O3 Cd1 O4 55.06(8) 1_655 1_655 ? O1 Cd1 O4 125.38(9) . 1_655 ? N4 Cd1 O2 85.66(9) 1_656 . ? N1 Cd1 O2 92.03(10) . . ? O3 Cd1 O2 124.73(9) 1_655 . ? O1 Cd1 O2 52.89(8) . . ? O4 Cd1 O2 178.11(8) 1_655 . ? N4 Cd1 C10 102.04(9) 1_656 1_655 ? N1 Cd1 C10 111.10(10) . 1_655 ? O3 Cd1 C10 27.75(7) 1_655 1_655 ? O1 Cd1 C10 108.35(8) . 1_655 ? O4 Cd1 C10 27.36(8) 1_655 1_655 ? O2 Cd1 C10 152.31(9) . 1_655 ? O2 C1 O1 120.8(3) . . ? O2 C1 C2 119.8(3) . . ? O1 C1 C2 119.2(3) . . ? C3 C2 C1 109.7(2) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C8 C3 C4 117.3(3) . . ? C8 C3 C2 121.6(3) . . ? C4 C3 C2 121.0(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C6 C5 C4 121.0(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 117.9(2) . . ? C5 C6 C9 120.9(2) . . ? C7 C6 C9 121.1(2) . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C3 C8 C7 121.3(3) . . ? C3 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C6 C9 C10 116.7(2) . . ? C6 C9 H9A 108.1 . . ? C10 C9 H9A 108.1 . . ? C6 C9 H9B 108.1 . . ? C10 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? O4 C10 O3 121.7(3) . . ? O4 C10 C9 118.2(3) . . ? O3 C10 C9 120.1(2) . . ? O4 C10 Cd1 62.39(15) . 1_455 ? O3 C10 Cd1 59.44(14) . 1_455 ? C9 C10 Cd1 174.8(2) . 1_455 ? N1 C11 N2 111.4(2) . . ? N1 C11 H11 124.3 . . ? N2 C11 H11 124.3 . . ? C13 C12 N2 106.6(2) . . ? C13 C12 H12 126.7 . . ? N2 C12 H12 126.7 . . ? C12 C13 N1 109.7(2) . . ? C12 C13 H13 125.1 . . ? N1 C13 H13 125.1 . . ? N2 C14 C15 111.0(2) . . ? N2 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N2 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.0(2) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N3 C16 C15 111.0(2) . . ? N3 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? N3 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 N3 111.2(2) . . ? N4 C17 H17 124.4 . . ? N3 C17 H17 124.4 . . ? C19 C18 N4 109.3(2) . . ? C19 C18 H18 125.4 . . ? N4 C18 H18 125.4 . . ? C18 C19 N3 106.2(2) . . ? C18 C19 H19 126.9 . . ? N3 C19 H19 126.9 . . ? C11 N1 C13 105.3(2) . . ? C11 N1 Cd1 127.36(18) . . ? C13 N1 Cd1 127.25(18) . . ? C11 N2 C12 107.0(2) . . ? C11 N2 C14 126.6(2) . . ? C12 N2 C14 126.3(2) . . ? C17 N3 C19 107.6(2) . . ? C17 N3 C16 126.1(2) . . ? C19 N3 C16 126.4(2) . . ? C17 N4 C18 105.8(2) . . ? C17 N4 Cd1 126.52(17) . 1_454 ? C18 N4 Cd1 127.66(18) . 1_454 ? C1 O1 Cd1 95.49(18) . . ? C1 O2 Cd1 90.43(19) . . ? C10 O3 Cd1 92.82(17) . 1_455 ? C10 O4 Cd1 90.24(17) . 1_455 ? H5A O5 H5B 91(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 O2 C1 C2 C3 -82.6(4) . . . . ? O1 C1 C2 C3 93.2(3) . . . . ? C1 C2 C3 C8 -94.2(3) . . . . ? C1 C2 C3 C4 84.5(3) . . . . ? C8 C3 C4 C5 0.3(4) . . . . ? C2 C3 C4 C5 -178.4(2) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C4 C5 C6 C9 176.8(2) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C9 C6 C7 C8 -177.0(3) . . . . ? C4 C3 C8 C7 -0.5(4) . . . . ? C2 C3 C8 C7 178.2(3) . . . . ? C6 C7 C8 C3 0.0(4) . . . . ? C5 C6 C9 C10 42.9(4) . . . . ? C7 C6 C9 C10 -139.5(3) . . . . ? C6 C9 C10 O4 -144.4(3) . . . . ? C6 C9 C10 O3 36.9(4) . . . . ? C6 C9 C10 Cd1 120(2) . . . 1_455 ? N2 C12 C13 N1 -0.4(3) . . . . ? N2 C14 C15 C16 172.5(2) . . . . ? C14 C15 C16 N3 -168.5(2) . . . . ? N4 C18 C19 N3 -0.4(3) . . . . ? N2 C11 N1 C13 -0.1(3) . . . . ? N2 C11 N1 Cd1 176.04(17) . . . . ? C12 C13 N1 C11 0.4(3) . . . . ? C12 C13 N1 Cd1 -175.83(19) . . . . ? N4 Cd1 N1 C11 119.4(2) 1_656 . . . ? O3 Cd1 N1 C11 -113.9(2) 1_655 . . . ? O1 Cd1 N1 C11 -19.6(2) . . . . ? O4 Cd1 N1 C11 -144.9(2) 1_655 . . . ? O2 Cd1 N1 C11 33.3(2) . . . . ? C10 Cd1 N1 C11 -131.1(2) 1_655 . . . ? N4 Cd1 N1 C13 -65.3(2) 1_656 . . . ? O3 Cd1 N1 C13 61.4(3) 1_655 . . . ? O1 Cd1 N1 C13 155.8(2) . . . . ? O4 Cd1 N1 C13 30.5(2) 1_655 . . . ? O2 Cd1 N1 C13 -151.3(2) . . . . ? C10 Cd1 N1 C13 44.3(2) 1_655 . . . ? N1 C11 N2 C12 -0.1(3) . . . . ? N1 C11 N2 C14 -176.1(2) . . . . ? C13 C12 N2 C11 0.3(3) . . . . ? C13 C12 N2 C14 176.3(3) . . . . ? C15 C14 N2 C11 105.6(3) . . . . ? C15 C14 N2 C12 -69.6(3) . . . . ? N4 C17 N3 C19 -0.3(3) . . . . ? N4 C17 N3 C16 179.3(2) . . . . ? C18 C19 N3 C17 0.4(3) . . . . ? C18 C19 N3 C16 -179.2(2) . . . . ? C15 C16 N3 C17 -114.9(3) . . . . ? C15 C16 N3 C19 64.7(3) . . . . ? N3 C17 N4 C18 0.1(3) . . . . ? N3 C17 N4 Cd1 -178.21(15) . . . 1_454 ? C19 C18 N4 C17 0.2(3) . . . . ? C19 C18 N4 Cd1 178.47(19) . . . 1_454 ? O2 C1 O1 Cd1 6.3(3) . . . . ? C2 C1 O1 Cd1 -169.5(2) . . . . ? N4 Cd1 O1 C1 -30.1(2) 1_656 . . . ? N1 Cd1 O1 C1 86.0(2) . . . . ? O3 Cd1 O1 C1 -138.88(19) 1_655 . . . ? O4 Cd1 O1 C1 175.64(16) 1_655 . . . ? O2 Cd1 O1 C1 -3.40(17) . . . . ? C10 Cd1 O1 C1 -160.16(18) 1_655 . . . ? O1 C1 O2 Cd1 -6.0(3) . . . . ? C2 C1 O2 Cd1 169.7(2) . . . . ? N4 Cd1 O2 C1 164.89(19) 1_656 . . . ? N1 Cd1 O2 C1 -90.30(19) . . . . ? O3 Cd1 O2 C1 61.9(2) 1_655 . . . ? O1 Cd1 O2 C1 3.40(17) . . . . ? O4 Cd1 O2 C1 -21(3) 1_655 . . . ? C10 Cd1 O2 C1 57.1(3) 1_655 . . . ? O4 C10 O3 Cd1 -4.7(3) . . . 1_455 ? C9 C10 O3 Cd1 174.0(2) . . . 1_455 ? O3 C10 O4 Cd1 4.6(3) . . . 1_455 ? C9 C10 O4 Cd1 -174.1(2) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.429 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.059 data_6 _database_code_depnum_ccdc_archive 'CCDC 839127' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 N4 O4 Zn' _chemical_formula_weight 447.79 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 Cc 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' _cell_length_a 7.7981(6) _cell_length_b 16.0351(14) _cell_length_c 16.4278(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.2430(10) _cell_angle_gamma 90.00 _cell_volume 1999.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7032 _exptl_absorpt_correction_T_max 0.8531 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4703 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 24.15 _reflns_number_total 2210 _reflns_number_gt 1975 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.1' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. ; _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^)+(0.0667P)^2^+0.1960P] 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 0.00(3) _refine_ls_number_reflns 2210 _refine_ls_number_parameters 263 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _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 1.12709(7) 0.18669(4) 0.44747(6) 0.0453(2) Uani 1 1 d . . . O1 O 0.9840(6) 0.2843(4) 0.4090(5) 0.092(2) Uani 1 1 d . . . O2 O 0.7675(13) 0.2143(8) 0.3628(13) 0.309(12) Uani 1 1 d . . . O3 O -0.0285(8) 0.3676(4) 0.0523(4) 0.097(2) Uani 1 1 d . . . O4 O -0.2003(6) 0.2578(3) 0.0347(4) 0.0686(14) Uani 1 1 d . . . N1 N 1.0126(6) 0.0855(3) 0.4856(3) 0.0480(12) Uani 1 1 d . . . N2 N 0.8233(6) -0.0048(3) 0.5122(3) 0.0500(13) Uani 1 1 d . . . N3 N 0.3844(6) -0.0823(3) 0.7755(3) 0.0484(12) Uani 1 1 d . . . N4 N 0.2173(6) -0.1321(3) 0.8551(3) 0.0468(12) Uani 1 1 d . . . C1 C 0.8498(7) 0.0737(4) 0.4948(4) 0.0491(15) Uani 1 1 d . . . H1 H 0.7652 0.1155 0.4896 0.059 Uiso 1 1 calc R . . C2 C 1.0905(9) 0.0083(5) 0.4986(5) 0.0628(19) Uani 1 1 d . . . H2 H 1.2058 -0.0040 0.4961 0.075 Uiso 1 1 calc R . . C3 C 0.9761(10) -0.0456(5) 0.5153(5) 0.0657(19) Uani 1 1 d . . . H3 H 0.9967 -0.1019 0.5272 0.079 Uiso 1 1 calc R . . C4 C 0.6641(9) -0.0385(4) 0.5353(4) 0.0584(17) Uani 1 1 d . . . H4A H 0.6396 -0.0939 0.5118 0.070 Uiso 1 1 calc R . . H4B H 0.5638 -0.0032 0.5120 0.070 Uiso 1 1 calc R . . C5 C 0.6896(9) -0.0426(4) 0.6290(4) 0.0560(16) Uani 1 1 d . . . H5A H 0.7354 0.0104 0.6531 0.067 Uiso 1 1 calc R . . H5B H 0.7758 -0.0853 0.6510 0.067 Uiso 1 1 calc R . . C6 C 0.5193(9) -0.0618(5) 0.6546(5) 0.0626(18) Uani 1 1 d . . . H6A H 0.4315 -0.0205 0.6306 0.075 Uiso 1 1 calc R . . H6B H 0.4761 -0.1160 0.6326 0.075 Uiso 1 1 calc R . . C7 C 0.5444(8) -0.0621(5) 0.7475(4) 0.0639(18) Uani 1 1 d . . . H7A H 0.6350 -0.1024 0.7711 0.077 Uiso 1 1 calc R . . H7B H 0.5857 -0.0076 0.7689 0.077 Uiso 1 1 calc R . . C8 C 0.3774(8) -0.1310(4) 0.8403(4) 0.0496(15) Uani 1 1 d . . . H8 H 0.4729 -0.1606 0.8714 0.060 Uiso 1 1 calc R . . C9 C 0.1183(8) -0.0805(4) 0.7952(4) 0.0533(16) Uani 1 1 d . . . H9 H -0.0008 -0.0691 0.7895 0.064 Uiso 1 1 calc R . . C10 C 0.2177(8) -0.0495(4) 0.7469(4) 0.0545(16) Uani 1 1 d . . . H10 H 0.1821 -0.0128 0.7024 0.065 Uiso 1 1 calc R . . C11 C 0.8362(9) 0.2775(6) 0.3706(5) 0.070(2) Uani 1 1 d . . . C12 C 0.7440(9) 0.3533(5) 0.3265(6) 0.082(3) Uani 1 1 d . . . H12A H 0.8148 0.3758 0.2902 0.099 Uiso 1 1 calc R . . H12B H 0.7375 0.3954 0.3681 0.099 Uiso 1 1 calc R . . C13 C 0.5586(9) 0.3371(4) 0.2744(5) 0.0602(19) Uani 1 1 d . . . C14 C 0.5310(11) 0.3045(5) 0.1961(6) 0.076(2) Uani 1 1 d . . . H14 H 0.6253 0.2980 0.1708 0.091 Uiso 1 1 calc R . . C15 C 0.3583(12) 0.2804(5) 0.1524(5) 0.076(2) Uani 1 1 d . . . H15 H 0.3409 0.2575 0.0991 0.091 Uiso 1 1 calc R . . C16 C 0.2183(10) 0.2907(4) 0.1885(6) 0.063(2) Uani 1 1 d . . . C17 C 0.2500(9) 0.3253(5) 0.2642(6) 0.070(2) Uani 1 1 d . . . H17 H 0.1559 0.3338 0.2893 0.084 Uiso 1 1 calc R . . C18 C 0.4154(9) 0.3490(5) 0.3069(5) 0.070(2) Uani 1 1 d . . . H18 H 0.4297 0.3738 0.3592 0.084 Uiso 1 1 calc R . . C19 C 0.0411(11) 0.2565(6) 0.1496(7) 0.098(3) Uani 1 1 d . . . H19A H -0.0306 0.2597 0.1906 0.118 Uiso 1 1 calc R . . H19B H 0.0548 0.1979 0.1378 0.118 Uiso 1 1 calc R . . C20 C -0.0612(10) 0.2983(4) 0.0687(5) 0.0492(17) 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 0.0340(3) 0.0516(4) 0.0499(4) -0.0033(4) 0.0087(2) -0.0010(4) O1 0.047(3) 0.070(3) 0.142(6) 0.013(4) -0.015(3) 0.006(2) O2 0.105(7) 0.175(10) 0.53(3) 0.213(15) -0.160(11) -0.054(7) O3 0.081(4) 0.077(4) 0.109(5) 0.035(3) -0.026(3) -0.020(3) O4 0.049(3) 0.070(3) 0.073(3) 0.010(3) -0.015(2) -0.012(2) N1 0.041(3) 0.053(3) 0.051(3) 0.004(3) 0.013(2) 0.007(2) N2 0.055(3) 0.050(3) 0.048(3) -0.002(2) 0.019(3) -0.006(2) N3 0.048(3) 0.056(3) 0.045(3) -0.006(2) 0.017(2) -0.010(2) N4 0.044(3) 0.053(3) 0.045(3) -0.001(2) 0.014(2) 0.005(2) C1 0.039(3) 0.055(4) 0.056(4) 0.000(3) 0.014(3) -0.002(3) C2 0.055(4) 0.077(5) 0.063(5) 0.016(4) 0.028(4) 0.017(4) C3 0.076(5) 0.057(4) 0.074(5) 0.014(4) 0.039(4) 0.019(4) C4 0.064(4) 0.055(4) 0.062(4) -0.005(3) 0.026(3) -0.015(3) C5 0.060(4) 0.058(4) 0.052(4) 0.002(3) 0.018(3) -0.003(3) C6 0.063(4) 0.071(5) 0.059(4) 0.006(4) 0.024(3) -0.013(4) C7 0.055(4) 0.086(5) 0.056(4) 0.004(4) 0.022(3) -0.015(4) C8 0.046(3) 0.062(4) 0.043(4) 0.000(3) 0.013(3) 0.001(3) C9 0.044(3) 0.070(4) 0.045(4) 0.002(3) 0.008(3) 0.014(3) C10 0.062(4) 0.053(4) 0.048(4) 0.008(3) 0.012(3) 0.010(3) C11 0.044(4) 0.077(5) 0.080(5) 0.018(4) -0.006(4) -0.031(4) C12 0.047(4) 0.070(5) 0.114(7) 0.008(5) -0.014(4) -0.004(4) C13 0.045(4) 0.054(4) 0.073(5) 0.010(4) -0.003(4) 0.003(3) C14 0.065(5) 0.087(6) 0.078(6) 0.022(5) 0.020(4) 0.015(4) C15 0.105(7) 0.068(5) 0.045(4) 0.011(4) -0.004(4) 0.013(4) C16 0.053(4) 0.043(4) 0.081(6) 0.023(4) -0.010(4) -0.001(3) C17 0.045(4) 0.077(5) 0.088(7) 0.021(5) 0.013(4) 0.004(3) C18 0.059(4) 0.073(5) 0.068(5) -0.006(4) -0.006(4) 0.013(4) C19 0.078(5) 0.073(5) 0.113(8) 0.032(5) -0.041(5) -0.014(4) C20 0.050(4) 0.034(4) 0.052(4) -0.007(3) -0.012(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.941(5) . ? Zn1 O4 1.943(5) 4_655 ? Zn1 N4 2.012(5) 2_654 ? Zn1 N1 2.019(5) . ? O1 C11 1.186(8) . ? O2 C11 1.140(12) . ? O3 C20 1.185(9) . ? O4 C20 1.277(9) . ? O4 Zn1 1.943(5) 4_354 ? N1 C1 1.326(7) . ? N1 C2 1.375(8) . ? N2 C1 1.318(8) . ? N2 C3 1.350(8) . ? N2 C4 1.481(7) . ? N3 C8 1.332(8) . ? N3 C10 1.381(8) . ? N3 C7 1.461(8) . ? N4 C8 1.326(7) . ? N4 C9 1.379(8) . ? N4 Zn1 2.012(5) 2_455 ? C1 H1 0.9300 . ? C2 C3 1.315(10) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.508(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.514(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.494(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9300 . ? C9 C10 1.327(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.509(12) . ? C12 C13 1.524(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.359(12) . ? C13 C18 1.357(10) . ? C14 C15 1.427(12) . ? C14 H14 0.9300 . ? C15 C16 1.366(11) . ? C15 H15 0.9300 . ? C16 C17 1.333(12) . ? C16 C19 1.488(10) . ? C17 C18 1.373(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.539(11) . ? C19 H19A 0.9700 . ? C19 H19B 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 O1 Zn1 O4 96.9(3) . 4_655 ? O1 Zn1 N4 112.3(3) . 2_654 ? O4 Zn1 N4 116.9(2) 4_655 2_654 ? O1 Zn1 N1 119.1(2) . . ? O4 Zn1 N1 114.8(2) 4_655 . ? N4 Zn1 N1 98.0(2) 2_654 . ? C11 O1 Zn1 121.1(6) . . ? C20 O4 Zn1 117.7(5) . 4_354 ? C1 N1 C2 104.7(5) . . ? C1 N1 Zn1 130.7(4) . . ? C2 N1 Zn1 124.1(4) . . ? C1 N2 C3 106.9(5) . . ? C1 N2 C4 125.9(5) . . ? C3 N2 C4 126.7(6) . . ? C8 N3 C10 106.7(5) . . ? C8 N3 C7 125.2(5) . . ? C10 N3 C7 127.8(6) . . ? C8 N4 C9 105.0(5) . . ? C8 N4 Zn1 130.6(4) . 2_455 ? C9 N4 Zn1 124.3(4) . 2_455 ? N2 C1 N1 111.3(5) . . ? N2 C1 H1 124.4 . . ? N1 C1 H1 124.4 . . ? C3 C2 N1 109.1(6) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 108.0(6) . . ? C2 C3 H3 126.0 . . ? N2 C3 H3 126.0 . . ? N2 C4 C5 110.8(5) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 112.0(6) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 111.5(6) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C6 113.6(6) . . ? N3 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N3 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N4 C8 N3 111.5(5) . . ? N4 C8 H8 124.2 . . ? N3 C8 H8 124.2 . . ? C10 C9 N4 110.1(5) . . ? C10 C9 H9 124.9 . . ? N4 C9 H9 124.9 . . ? C9 C10 N3 106.7(6) . . ? C9 C10 H10 126.7 . . ? N3 C10 H10 126.7 . . ? O2 C11 O1 121.0(9) . . ? O2 C11 C12 120.1(7) . . ? O1 C11 C12 118.7(7) . . ? C11 C12 C13 114.8(6) . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? C11 C12 H12B 108.6 . . ? C13 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C18 117.4(7) . . ? C14 C13 C12 121.4(8) . . ? C18 C13 C12 121.0(7) . . ? C13 C14 C15 120.5(8) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.3(8) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 117.4(7) . . ? C17 C16 C19 120.6(9) . . ? C15 C16 C19 121.7(9) . . ? C16 C17 C18 122.9(8) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C13 C18 C17 121.5(8) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C16 C19 C20 117.2(7) . . ? C16 C19 H19A 108.0 . . ? C20 C19 H19A 108.0 . . ? C16 C19 H19B 108.0 . . ? C20 C19 H19B 108.0 . . ? H19A C19 H19B 107.2 . . ? O3 C20 O4 125.6(7) . . ? O3 C20 C19 120.6(7) . . ? O4 C20 C19 112.1(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 O4 Zn1 O1 C11 -159.7(8) 4_655 . . . ? N4 Zn1 O1 C11 77.5(8) 2_654 . . . ? N1 Zn1 O1 C11 -36.2(9) . . . . ? O1 Zn1 N1 C1 -4.9(7) . . . . ? O4 Zn1 N1 C1 109.3(6) 4_655 . . . ? N4 Zn1 N1 C1 -126.1(6) 2_654 . . . ? O1 Zn1 N1 C2 167.0(6) . . . . ? O4 Zn1 N1 C2 -78.9(6) 4_655 . . . ? N4 Zn1 N1 C2 45.8(6) 2_654 . . . ? C3 N2 C1 N1 0.7(7) . . . . ? C4 N2 C1 N1 173.0(6) . . . . ? C2 N1 C1 N2 -0.2(7) . . . . ? Zn1 N1 C1 N2 172.9(4) . . . . ? C1 N1 C2 C3 -0.5(8) . . . . ? Zn1 N1 C2 C3 -174.1(5) . . . . ? N1 C2 C3 N2 0.9(9) . . . . ? C1 N2 C3 C2 -1.0(8) . . . . ? C4 N2 C3 C2 -173.2(6) . . . . ? C1 N2 C4 C5 -94.8(8) . . . . ? C3 N2 C4 C5 76.0(8) . . . . ? N2 C4 C5 C6 169.7(6) . . . . ? C4 C5 C6 C7 -177.5(7) . . . . ? C8 N3 C7 C6 139.4(7) . . . . ? C10 N3 C7 C6 -47.7(10) . . . . ? C5 C6 C7 N3 -178.7(6) . . . . ? C9 N4 C8 N3 0.0(7) . . . . ? Zn1 N4 C8 N3 -175.5(4) 2_455 . . . ? C10 N3 C8 N4 0.3(7) . . . . ? C7 N3 C8 N4 174.5(6) . . . . ? C8 N4 C9 C10 -0.4(7) . . . . ? Zn1 N4 C9 C10 175.5(5) 2_455 . . . ? N4 C9 C10 N3 0.6(7) . . . . ? C8 N3 C10 C9 -0.6(7) . . . . ? C7 N3 C10 C9 -174.5(6) . . . . ? Zn1 O1 C11 O2 9(2) . . . . ? Zn1 O1 C11 C12 -166.9(7) . . . . ? O2 C11 C12 C13 0.8(19) . . . . ? O1 C11 C12 C13 176.3(9) . . . . ? C11 C12 C13 C14 -81.3(10) . . . . ? C11 C12 C13 C18 93.9(10) . . . . ? C18 C13 C14 C15 -3.1(11) . . . . ? C12 C13 C14 C15 172.3(7) . . . . ? C13 C14 C15 C16 0.8(12) . . . . ? C14 C15 C16 C17 1.3(11) . . . . ? C14 C15 C16 C19 -172.0(7) . . . . ? C15 C16 C17 C18 -1.2(11) . . . . ? C19 C16 C17 C18 172.2(7) . . . . ? C14 C13 C18 C17 3.2(12) . . . . ? C12 C13 C18 C17 -172.1(7) . . . . ? C16 C17 C18 C13 -1.1(12) . . . . ? C17 C16 C19 C20 116.4(9) . . . . ? C15 C16 C19 C20 -70.4(11) . . . . ? Zn1 O4 C20 O3 0.8(11) 4_354 . . . ? Zn1 O4 C20 C19 166.2(6) 4_354 . . . ? C16 C19 C20 O3 -22.3(14) . . . . ? C16 C19 C20 O4 171.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.15 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.452 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.056 data_7 _database_code_depnum_ccdc_archive 'CCDC 839128' #TrackingRef '- Complex 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Cd N4 O5' _chemical_formula_weight 540.88 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 20.5170(17) _cell_length_b 10.5876(9) _cell_length_c 21.9335(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.4190(10) _cell_angle_gamma 90.00 _cell_volume 4593.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8189 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16484 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4069 _reflns_number_gt 3303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, the command 'omit -3 50.1' was used to omit the weak reflections above 50 degree. The command 'isor' was also used to restrain the non-H atoms with NPD and ADP problems. The hydrogen atoms of organic ligands were placed in calculated positions and refined using a riding on attached atoms with isotropic thermal parameters 1.2 times those of their carrier atoms. Although the hydrogen atoms of lattice water molecule O1w and O2w in complex 7 were located using the Difference Fourier method, meantime, the hydrogen atoms may have higher thermal parameters, so the hydrogen atoms of O1w and O2w atoms should be omitted. ; _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^)+(0.0613P)^2^+9.8963P] 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 4069 _refine_ls_number_parameters 290 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.032 _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 0.162467(14) 0.71318(4) 0.440431(15) 0.06704(16) Uani 1 1 d . . . O1 O 0.07939(15) 0.8634(4) 0.39658(17) 0.0839(10) Uani 1 1 d . . . O2 O 0.04802(18) 0.6785(4) 0.35379(17) 0.0867(10) Uani 1 1 d . . . O3 O -0.23208(15) 1.1258(3) 0.50049(17) 0.0773(9) Uani 1 1 d . . . O4 O -0.29802(19) 0.9874(5) 0.4446(3) 0.136(2) Uani 1 1 d . . . N1 N 0.2112(2) 0.7469(7) 0.3609(2) 0.1083(19) Uani 1 1 d . . . N2 N 0.2854(3) 0.7551(8) 0.3058(2) 0.129(2) Uani 1 1 d . . . N3 N 0.52202(19) 0.8757(4) 0.05668(18) 0.0669(9) Uani 1 1 d . . . N4 N 0.60429(18) 0.8422(4) 0.01188(17) 0.0649(9) Uani 1 1 d . . . C1 C 0.0378(2) 0.7927(6) 0.3602(2) 0.0694(13) Uani 1 1 d . . . C2 C -0.0295(2) 0.8527(6) 0.3247(2) 0.0766(14) Uani 1 1 d . . . H2A H -0.0517 0.8000 0.2891 0.092 Uiso 1 1 calc R . . H2B H -0.0213 0.9348 0.3086 0.092 Uiso 1 1 calc R . . C3 C -0.07501(19) 0.8675(5) 0.3689(2) 0.0634(11) Uani 1 1 d . . . C4 C -0.0615(3) 0.9635(5) 0.4139(3) 0.0797(14) Uani 1 1 d . . . H4 H -0.0266 1.0199 0.4143 0.096 Uiso 1 1 calc R . . C5 C -0.0977(2) 0.9778(5) 0.4578(3) 0.0809(15) Uani 1 1 d . . . H5 H -0.0869 1.0418 0.4878 0.097 Uiso 1 1 calc R . . C6 C -0.1504(2) 0.8959(4) 0.4569(2) 0.0676(12) Uani 1 1 d . . . C7 C -0.1650(2) 0.8011(5) 0.4140(3) 0.0727(13) Uani 1 1 d . . . H7 H -0.2000 0.7453 0.4137 0.087 Uiso 1 1 calc R . . C8 C -0.1265(3) 0.7877(5) 0.3695(3) 0.0824(15) Uani 1 1 d . . . H8 H -0.1367 0.7226 0.3400 0.099 Uiso 1 1 calc R . . C9 C -0.1904(3) 0.9139(5) 0.5055(3) 0.0862(15) Uani 1 1 d . . . H9A H -0.2117 0.8350 0.5119 0.103 Uiso 1 1 calc R . . H9B H -0.1603 0.9396 0.5457 0.103 Uiso 1 1 calc R . . C10 C -0.2440(2) 1.0149(5) 0.4818(3) 0.0790(14) Uani 1 1 d . . . C11 C 0.2660(3) 0.6961(9) 0.3507(3) 0.123(3) Uani 1 1 d . . . H11 H 0.2883 0.6267 0.3727 0.148 Uiso 1 1 calc R . . C12 C 0.2440(4) 0.8553(10) 0.2860(3) 0.138(3) Uani 1 1 d . . . H12 H 0.2462 0.9157 0.2558 0.166 Uiso 1 1 calc R . . C13 C 0.1972(3) 0.8457(10) 0.3219(4) 0.132(3) Uani 1 1 d . . . H13 H 0.1612 0.9007 0.3189 0.158 Uiso 1 1 calc R . . C14 C 0.3471(3) 0.7279(11) 0.2849(3) 0.159(4) Uani 1 1 d D . . H14A H 0.3755 0.8026 0.2916 0.191 Uiso 1 1 calc R . . H14B H 0.3723 0.6609 0.3110 0.191 Uiso 1 1 calc R . . C15 C 0.3343(4) 0.6934(11) 0.2237(4) 0.156(4) Uani 1 1 d D . . H15A H 0.3037 0.7544 0.1980 0.188 Uiso 1 1 calc R . . H15B H 0.3116 0.6122 0.2182 0.188 Uiso 1 1 calc R . . C16 C 0.3984(3) 0.6836(9) 0.1994(3) 0.131(3) Uani 1 1 d D . . H16A H 0.4381 0.6967 0.2344 0.157 Uiso 1 1 calc R . . H16B H 0.4011 0.5994 0.1829 0.157 Uiso 1 1 calc R . . C17 C 0.3981(3) 0.7776(6) 0.1493(3) 0.0864(16) Uani 1 1 d D . . H17A H 0.3944 0.8613 0.1661 0.104 Uiso 1 1 calc R . . H17B H 0.3581 0.7638 0.1146 0.104 Uiso 1 1 calc R . . C18 C 0.4590(3) 0.7744(5) 0.1237(2) 0.0761(14) Uani 1 1 d D . . H18A H 0.4989 0.7911 0.1580 0.091 Uiso 1 1 calc R . . H18B H 0.4635 0.6901 0.1080 0.091 Uiso 1 1 calc R . . C19 C 0.4568(2) 0.8670(5) 0.0719(2) 0.0780(14) Uani 1 1 d D . . H19A H 0.4223 0.8415 0.0344 0.094 Uiso 1 1 calc R . . H19B H 0.4446 0.9495 0.0846 0.094 Uiso 1 1 calc R . . C20 C 0.5416(2) 0.8152(4) 0.0112(2) 0.0622(11) Uani 1 1 d . . . H20 H 0.5141 0.7603 -0.0176 0.075 Uiso 1 1 calc R . . C21 C 0.6251(3) 0.9256(6) 0.0605(3) 0.0944(18) Uani 1 1 d . . . H21 H 0.6679 0.9618 0.0727 0.113 Uiso 1 1 calc R . . C22 C 0.5762(3) 0.9481(5) 0.0879(3) 0.0970(18) Uani 1 1 d . . . H22 H 0.5781 1.0023 0.1217 0.116 Uiso 1 1 calc R . . O1W O 0.0005(3) 0.5273(5) 0.2496(3) 0.344(11) Uani 1 2 d SR . . O2W O 0.3611(3) 1.0431(5) 0.2412(3) 0.231(8) Uani 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03504(19) 0.1000(3) 0.0673(2) -0.02559(17) 0.01576(14) 0.00593(15) O1 0.0433(16) 0.128(3) 0.081(2) -0.017(2) 0.0182(15) 0.0038(19) O2 0.072(2) 0.112(3) 0.074(2) -0.011(2) 0.0150(17) 0.022(2) O3 0.0507(16) 0.076(2) 0.099(2) -0.0225(19) 0.0103(16) 0.0027(16) O4 0.057(2) 0.136(4) 0.199(5) -0.087(4) 0.005(3) 0.002(2) N1 0.055(3) 0.208(6) 0.065(3) -0.010(3) 0.022(2) 0.037(3) N2 0.065(3) 0.257(8) 0.069(3) -0.009(4) 0.026(3) 0.044(4) N3 0.063(2) 0.071(2) 0.069(2) 0.0069(19) 0.0229(18) 0.0017(19) N4 0.051(2) 0.078(2) 0.066(2) 0.012(2) 0.0169(17) -0.0051(18) C1 0.042(2) 0.117(4) 0.053(2) -0.004(3) 0.019(2) 0.012(3) C2 0.049(2) 0.123(4) 0.060(3) 0.007(3) 0.019(2) 0.019(3) C3 0.039(2) 0.082(3) 0.069(3) 0.016(2) 0.0151(19) 0.017(2) C4 0.069(3) 0.069(3) 0.115(4) -0.002(3) 0.050(3) 0.001(2) C5 0.067(3) 0.067(3) 0.120(4) -0.019(3) 0.044(3) -0.002(2) C6 0.045(2) 0.055(3) 0.106(4) 0.005(2) 0.025(2) 0.0069(19) C7 0.054(3) 0.073(3) 0.095(4) -0.005(3) 0.027(3) -0.002(2) C8 0.054(3) 0.098(4) 0.091(4) -0.018(3) 0.013(3) -0.003(3) C9 0.071(3) 0.087(4) 0.113(4) -0.004(3) 0.046(3) 0.009(3) C10 0.046(2) 0.085(4) 0.110(4) -0.031(3) 0.029(3) -0.001(2) C11 0.073(4) 0.232(9) 0.071(4) -0.006(4) 0.032(3) 0.046(5) C12 0.104(5) 0.230(10) 0.095(5) 0.023(6) 0.051(4) 0.039(6) C13 0.070(4) 0.227(9) 0.107(5) -0.001(6) 0.040(4) 0.047(5) C14 0.070(4) 0.334(13) 0.082(4) -0.026(6) 0.034(3) 0.051(6) C15 0.093(5) 0.287(12) 0.112(6) -0.030(6) 0.067(5) 0.002(6) C16 0.080(4) 0.241(9) 0.090(4) 0.033(5) 0.056(4) 0.030(5) C17 0.064(3) 0.110(4) 0.095(4) -0.007(3) 0.039(3) 0.011(3) C18 0.062(3) 0.100(4) 0.075(3) 0.010(3) 0.034(2) 0.021(3) C19 0.063(3) 0.091(4) 0.087(3) 0.009(3) 0.033(3) 0.014(3) C20 0.048(2) 0.072(3) 0.067(3) 0.004(2) 0.016(2) -0.004(2) C21 0.077(3) 0.129(5) 0.079(3) -0.006(3) 0.023(3) -0.045(3) C22 0.107(4) 0.102(4) 0.088(4) -0.015(3) 0.035(3) -0.037(4) O1W 0.66(3) 0.102(6) 0.136(8) 0.000 -0.126(12) 0.000 O2W 0.42(3) 0.145(11) 0.191(13) 0.028(10) 0.191(16) 0.052(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.258(5) . ? Cd1 N4 2.285(4) 8_466 ? Cd1 O1 2.343(4) . ? Cd1 O3 2.375(3) 5_576 ? Cd1 O3 2.400(3) 3_545 ? Cd1 O4 2.518(5) 3_545 ? Cd1 O2 2.624(4) . ? O1 C1 1.250(6) . ? O2 C1 1.241(6) . ? O3 C10 1.246(6) . ? O3 Cd1 2.375(3) 5_576 ? O3 Cd1 2.400(3) 3_455 ? O4 C10 1.224(6) . ? O4 Cd1 2.518(5) 3_455 ? N1 C11 1.317(7) . ? N1 C13 1.334(10) . ? N2 C12 1.357(10) . ? N2 C11 1.315(9) . ? N2 C14 1.485(7) . ? N3 C20 1.334(6) . ? N3 C22 1.374(6) . ? N3 C19 1.464(6) . ? N4 C20 1.314(5) . ? N4 C21 1.363(7) . ? N4 Cd1 2.285(4) 8_565 ? C1 C2 1.532(6) . ? C2 C3 1.521(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.355(7) . ? C3 C4 1.393(7) . ? C4 C5 1.372(7) . ? C4 H4 0.9300 . ? C5 C6 1.382(6) . ? C5 H5 0.9300 . ? C6 C7 1.354(7) . ? C6 C9 1.520(7) . ? C7 C8 1.417(8) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.524(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 H11 0.9300 . ? C12 C13 1.398(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.349(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.548(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.481(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.501(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.493(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20 0.9300 . ? C21 C22 1.320(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N4 171.91(18) . 8_466 ? N1 Cd1 O1 89.95(17) . . ? N4 Cd1 O1 90.01(13) 8_466 . ? N1 Cd1 O3 88.99(18) . 5_576 ? N4 Cd1 O3 99.10(13) 8_466 5_576 ? O1 Cd1 O3 90.17(12) . 5_576 ? N1 Cd1 O3 87.99(15) . 3_545 ? N4 Cd1 O3 94.80(13) 8_466 3_545 ? O1 Cd1 O3 159.84(12) . 3_545 ? O3 Cd1 O3 69.75(13) 5_576 3_545 ? N1 Cd1 O4 88.5(2) . 3_545 ? N4 Cd1 O4 87.34(16) 8_466 3_545 ? O1 Cd1 O4 148.36(13) . 3_545 ? O3 Cd1 O4 121.38(12) 5_576 3_545 ? O3 Cd1 O4 51.64(12) 3_545 3_545 ? N1 Cd1 O2 87.57(15) . . ? N4 Cd1 O2 86.03(12) 8_466 . ? O1 Cd1 O2 51.99(13) . . ? O3 Cd1 O2 141.98(12) 5_576 . ? O3 Cd1 O2 147.80(12) 3_545 . ? O4 Cd1 O2 96.36(13) 3_545 . ? C1 O1 Cd1 98.9(3) . . ? C1 O2 Cd1 85.8(3) . . ? C10 O3 Cd1 153.2(3) . 5_576 ? C10 O3 Cd1 96.5(3) . 3_455 ? Cd1 O3 Cd1 110.25(13) 5_576 3_455 ? C10 O4 Cd1 91.4(3) . 3_455 ? C11 N1 C13 105.1(6) . . ? C11 N1 Cd1 129.8(5) . . ? C13 N1 Cd1 123.7(4) . . ? C12 N2 C11 108.8(5) . . ? C12 N2 C14 124.4(7) . . ? C11 N2 C14 126.4(7) . . ? C20 N3 C22 106.0(4) . . ? C20 N3 C19 127.9(4) . . ? C22 N3 C19 126.1(4) . . ? C20 N4 C21 104.5(4) . . ? C20 N4 Cd1 128.7(3) . 8_565 ? C21 N4 Cd1 126.3(3) . 8_565 ? O2 C1 O1 123.3(4) . . ? O2 C1 C2 120.2(5) . . ? O1 C1 C2 116.5(5) . . ? C1 C2 C3 110.0(4) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C8 C3 C4 117.2(4) . . ? C8 C3 C2 123.7(5) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 122.3(5) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C6 119.2(5) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 120.1(5) . . ? C7 C6 C9 121.4(4) . . ? C5 C6 C9 118.5(5) . . ? C6 C7 C8 119.5(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C3 C8 C7 121.6(5) . . ? C3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C6 108.9(4) . . ? C10 C9 H9A 109.9 . . ? C6 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? C6 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O4 C10 O3 120.5(5) . . ? O4 C10 C9 120.3(5) . . ? O3 C10 C9 119.2(5) . . ? N1 C11 N2 112.1(7) . . ? N1 C11 H11 124.0 . . ? N2 C11 H11 124.0 . . ? N2 C12 C13 103.2(7) . . ? N2 C12 H12 128.4 . . ? C13 C12 H12 128.4 . . ? C12 C13 N1 110.8(7) . . ? C12 C13 H13 124.6 . . ? N1 C13 H13 124.6 . . ? C15 C14 N2 113.8(6) . . ? C15 C14 H14A 108.8 . . ? N2 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? N2 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 113.7(7) . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 112.0(6) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 115.0(5) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 114.3(4) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N3 C19 C18 111.8(4) . . ? N3 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? N3 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? N4 C20 N3 112.1(4) . . ? N4 C20 H20 124.0 . . ? N3 C20 H20 124.0 . . ? C22 C21 N4 110.8(5) . . ? C22 C21 H21 124.6 . . ? N4 C21 H21 124.6 . . ? C21 C22 N3 106.5(5) . . ? C21 C22 H22 126.7 . . ? N3 C22 H22 126.7 . . ? 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 N1 Cd1 O1 C1 88.2(3) . . . . ? N4 Cd1 O1 C1 -83.7(3) 8_466 . . . ? O3 Cd1 O1 C1 177.2(3) 5_576 . . . ? O3 Cd1 O1 C1 172.2(3) 3_545 . . . ? O4 Cd1 O1 C1 1.2(4) 3_545 . . . ? O2 Cd1 O1 C1 1.2(3) . . . . ? N1 Cd1 O2 C1 -93.1(3) . . . . ? N4 Cd1 O2 C1 91.9(3) 8_466 . . . ? O1 Cd1 O2 C1 -1.2(3) . . . . ? O3 Cd1 O2 C1 -7.8(4) 5_576 . . . ? O3 Cd1 O2 C1 -175.4(3) 3_545 . . . ? O4 Cd1 O2 C1 178.8(3) 3_545 . . . ? N4 Cd1 N1 C11 -91.6(12) 8_466 . . . ? O1 Cd1 N1 C11 178.7(7) . . . . ? O3 Cd1 N1 C11 88.6(7) 5_576 . . . ? O3 Cd1 N1 C11 18.8(7) 3_545 . . . ? O4 Cd1 N1 C11 -32.9(7) 3_545 . . . ? O2 Cd1 N1 C11 -129.3(7) . . . . ? N4 Cd1 N1 C13 104.3(14) 8_466 . . . ? O1 Cd1 N1 C13 14.6(6) . . . . ? O3 Cd1 N1 C13 -75.6(6) 5_576 . . . ? O3 Cd1 N1 C13 -145.3(6) 3_545 . . . ? O4 Cd1 N1 C13 163.0(6) 3_545 . . . ? O2 Cd1 N1 C13 66.6(6) . . . . ? Cd1 O2 C1 O1 2.2(5) . . . . ? Cd1 O2 C1 C2 -175.2(4) . . . . ? Cd1 O1 C1 O2 -2.4(5) . . . . ? Cd1 O1 C1 C2 175.0(3) . . . . ? O2 C1 C2 C3 100.7(5) . . . . ? O1 C1 C2 C3 -76.9(6) . . . . ? C1 C2 C3 C8 -100.8(6) . . . . ? C1 C2 C3 C4 75.4(6) . . . . ? C8 C3 C4 C5 0.5(8) . . . . ? C2 C3 C4 C5 -175.9(5) . . . . ? C3 C4 C5 C6 -1.2(8) . . . . ? C4 C5 C6 C7 1.4(8) . . . . ? C4 C5 C6 C9 -179.5(5) . . . . ? C5 C6 C7 C8 -0.9(8) . . . . ? C9 C6 C7 C8 -180.0(5) . . . . ? C4 C3 C8 C7 0.1(7) . . . . ? C2 C3 C8 C7 176.3(5) . . . . ? C6 C7 C8 C3 0.2(8) . . . . ? C7 C6 C9 C10 -97.7(6) . . . . ? C5 C6 C9 C10 83.2(6) . . . . ? Cd1 O4 C10 O3 0.6(6) 3_455 . . . ? Cd1 O4 C10 C9 -178.9(4) 3_455 . . . ? Cd1 O3 C10 O4 -178.4(5) 5_576 . . . ? Cd1 O3 C10 O4 -0.6(6) 3_455 . . . ? Cd1 O3 C10 C9 1.0(11) 5_576 . . . ? Cd1 O3 C10 C9 178.9(4) 3_455 . . . ? C6 C9 C10 O4 82.9(7) . . . . ? C6 C9 C10 O3 -96.6(6) . . . . ? C13 N1 C11 N2 -2.4(9) . . . . ? Cd1 N1 C11 N2 -168.7(5) . . . . ? C12 N2 C11 N1 3.0(10) . . . . ? C14 N2 C11 N1 176.1(7) . . . . ? C11 N2 C12 C13 -2.3(9) . . . . ? C14 N2 C12 C13 -175.5(7) . . . . ? N2 C12 C13 N1 0.9(10) . . . . ? C11 N1 C13 C12 0.8(10) . . . . ? Cd1 N1 C13 C12 168.3(5) . . . . ? C12 N2 C14 C15 -68.6(13) . . . . ? C11 N2 C14 C15 119.3(10) . . . . ? N2 C14 C15 C16 171.8(8) . . . . ? C14 C15 C16 C17 -115.7(10) . . . . ? C15 C16 C17 C18 179.6(6) . . . . ? C16 C17 C18 C19 178.2(6) . . . . ? C20 N3 C19 C18 95.7(6) . . . . ? C22 N3 C19 C18 -83.3(6) . . . . ? C17 C18 C19 N3 169.8(5) . . . . ? C21 N4 C20 N3 -0.5(5) . . . . ? Cd1 N4 C20 N3 -172.6(3) 8_565 . . . ? C22 N3 C20 N4 1.0(5) . . . . ? C19 N3 C20 N4 -178.2(4) . . . . ? C20 N4 C21 C22 -0.2(6) . . . . ? Cd1 N4 C21 C22 172.2(4) 8_565 . . . ? N4 C21 C22 N3 0.8(7) . . . . ? C20 N3 C22 C21 -1.1(6) . . . . ? C19 N3 C22 C21 178.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.661 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.063