# 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_name 'Gang Yuan' _publ_contact_author_email yuang568@nenu.edu.cn loop_ _publ_author_name 'Gang Yuan' 'Kui-Zhan Shao' 'Xin-Long Wang' 'Zhong-Min Su' ; Jian-Fang Ma ; data_1 _database_code_depnum_ccdc_archive 'CCDC 837789' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H18 Cd2 N8 O8' _chemical_formula_sum 'C30 H18 Cd2 N8 O8' _chemical_formula_weight 843.32 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 Orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 13.860(4) _cell_length_b 15.780(3) _cell_length_c 13.325(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2914.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17410 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6778 _reflns_number_gt 5081 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; H atom of carboxyl was located in difference Fourier maps. The restraint command 'dfix' was used to restrict the distance of H---O of carboxyl groups. 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_number_reflns 6778 _refine_ls_number_parameters 441 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.13148(2) 0.51035(2) 1.07080(4) 0.02745(8) Uani 1 1 d . . . Cd2 Cd 0.01745(2) 0.14488(2) 0.82763(4) 0.03487(10) Uani 1 1 d . . . C1 C -0.0086(4) 0.3722(4) 1.1587(6) 0.0330(16) Uani 1 1 d . . . C2 C 0.0247(3) 0.3387(3) 1.0600(5) 0.0279(12) Uani 1 1 d . . . C3 C 0.0080(4) 0.2620(4) 1.0130(5) 0.0272(14) Uani 1 1 d . . . C4 C -0.0578(4) 0.1922(4) 1.0385(5) 0.0376(15) Uani 1 1 d . . . C5 C 0.0996(3) 0.3378(3) 0.9183(4) 0.0269(13) Uani 1 1 d . . . C6 C 0.1490(3) 0.3710(3) 0.8281(5) 0.0258(10) Uani 1 1 d . . . C7 C 0.2070(4) 0.3202(3) 0.7680(4) 0.0370(14) Uani 1 1 d . . . H7 H 0.2138 0.2627 0.7813 0.044 Uiso 1 1 calc R . . C8 C 0.2541(4) 0.3574(3) 0.6881(4) 0.0377(14) Uani 1 1 d . . . H8 H 0.2931 0.3230 0.6484 0.045 Uiso 1 1 calc R . . C9 C 0.1887(4) 0.4858(3) 0.7196(4) 0.0297(12) Uani 1 1 d . . . H9 H 0.1806 0.5425 0.7026 0.036 Uiso 1 1 calc R . . C10 C 0.1383(3) 0.4548(3) 0.8019(4) 0.0269(12) Uani 1 1 d . . . H10 H 0.0979 0.4902 0.8387 0.032 Uiso 1 1 calc R . . C11 C 0.0201(5) 0.3606(4) 0.4890(5) 0.0328(15) Uani 1 1 d . . . C12 C -0.0140(3) 0.3228(3) 0.5840(4) 0.0270(12) Uani 1 1 d . . . C13 C 0.0085(4) 0.2475(4) 0.6321(5) 0.0278(14) Uani 1 1 d . . . C14 C 0.0835(4) 0.1828(4) 0.6089(5) 0.0378(15) Uani 1 1 d . . . C15 C -0.0906(3) 0.3186(3) 0.7236(4) 0.0265(12) Uani 1 1 d . . . C16 C -0.1455(3) 0.3501(3) 0.8112(4) 0.0263(12) Uani 1 1 d . . . C17 C -0.2130(4) 0.3015(3) 0.8628(4) 0.0429(16) Uani 1 1 d . . . H17 H -0.2242 0.2455 0.8446 0.051 Uiso 1 1 calc R . . C18 C -0.2633(4) 0.3376(3) 0.9415(5) 0.0431(16) Uani 1 1 d . . . H18 H -0.3092 0.3045 0.9740 0.052 Uiso 1 1 calc R . . C19 C -0.1291(3) 0.4317(3) 0.8479(4) 0.0296(13) Uani 1 1 d . . . H19 H -0.0815 0.4653 0.8191 0.036 Uiso 1 1 calc R . . C20 C -0.1831(4) 0.4625(3) 0.9263(4) 0.0317(13) Uani 1 1 d . . . H20 H -0.1724 0.5178 0.9475 0.038 Uiso 1 1 calc R . . C21 C -0.1327(6) 0.0052(6) 0.7437(7) 0.084(4) Uani 1 1 d . . . H21 H -0.1676 0.0524 0.7229 0.101 Uiso 1 1 calc R . . C22 C -0.1658(6) -0.0777(7) 0.7195(6) 0.085(3) Uani 1 1 d . . . H22 H -0.2224 -0.0852 0.6830 0.102 Uiso 1 1 calc R . . C23 C -0.1140(7) -0.1453(6) 0.7502(7) 0.099(3) Uani 1 1 d . . . H23 H -0.1345 -0.1999 0.7350 0.119 Uiso 1 1 calc R . . C24 C -0.0325(5) -0.1331(4) 0.8029(6) 0.076(3) Uani 1 1 d . . . H24 H 0.0040 -0.1795 0.8233 0.091 Uiso 1 1 calc R . . C25 C -0.0029(4) -0.0529(3) 0.8268(8) 0.0465(13) Uani 1 1 d . . . C26 C 0.0857(5) -0.0369(4) 0.8869(5) 0.0439(17) Uani 1 1 d . . . C27 C 0.1331(6) -0.1017(4) 0.9402(6) 0.071(2) Uani 1 1 d . . . H27 H 0.1081 -0.1564 0.9406 0.085 Uiso 1 1 calc R . . C28 C 0.2161(6) -0.0836(6) 0.9913(6) 0.079(3) Uani 1 1 d . . . H28 H 0.2481 -0.1262 1.0263 0.095 Uiso 1 1 calc R . . C29 C 0.2517(5) -0.0041(5) 0.9911(5) 0.070(2) Uani 1 1 d . . . H29 H 0.3095 0.0086 1.0233 0.083 Uiso 1 1 calc R . . C30 C 0.2004(4) 0.0571(4) 0.9421(5) 0.0511(17) Uani 1 1 d . . . H30 H 0.2223 0.1128 0.9455 0.061 Uiso 1 1 calc R . . N1 N 0.0819(3) 0.3870(3) 0.9988(3) 0.0275(10) Uani 1 1 d . . . N2 N 0.0581(3) 0.2607(3) 0.9242(3) 0.0282(10) Uani 1 1 d . . . N3 N 0.2476(3) 0.4394(3) 0.6638(3) 0.0302(10) Uani 1 1 d . . . N4 N -0.0773(3) 0.3682(2) 0.6426(3) 0.0267(10) Uani 1 1 d . . . N5 N -0.0426(3) 0.2448(3) 0.7204(3) 0.0283(10) Uani 1 1 d . . . N6 N -0.2505(3) 0.4164(3) 0.9738(3) 0.0315(11) Uani 1 1 d . . . N7 N -0.0525(3) 0.0151(3) 0.7957(3) 0.0430(13) Uani 1 1 d . . . N8 N 0.1199(3) 0.0410(3) 0.8892(4) 0.0376(13) Uani 1 1 d . . . O1 O 0.0223(3) 0.4427(3) 1.1849(3) 0.0375(10) Uani 1 1 d . . . O2 O -0.0691(3) 0.3287(3) 1.2084(3) 0.0451(11) Uani 1 1 d D . . O3 O -0.1065(3) 0.1974(3) 1.1200(3) 0.0492(12) Uani 1 1 d D . . O4 O -0.0672(3) 0.1316(2) 0.9796(3) 0.0512(11) Uani 1 1 d . . . O5 O -0.0140(3) 0.4283(3) 0.4598(3) 0.0391(11) Uani 1 1 d . . . O6 O 0.0848(3) 0.3201(3) 0.4380(3) 0.0501(12) Uani 1 1 d D . . O7 O 0.1292(3) 0.1902(3) 0.5275(3) 0.0549(14) Uani 1 1 d D . . O8 O 0.1008(3) 0.1290(3) 0.6744(3) 0.0464(11) Uani 1 1 d . . . H2 H -0.094(4) 0.263(2) 1.168(4) 0.07(2) Uiso 1 1 d D . . H6 H 0.103(4) 0.253(2) 0.481(5) 0.09(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02856(17) 0.02302(18) 0.03078(16) -0.0014(2) 0.0001(2) 0.00102(15) Cd2 0.0433(2) 0.02424(18) 0.0371(2) 0.0018(2) -0.0036(3) 0.00168(18) C1 0.023(3) 0.036(4) 0.040(4) 0.001(3) 0.002(3) 0.005(3) C2 0.022(2) 0.025(3) 0.037(3) 0.006(3) -0.001(3) 0.001(2) C3 0.025(3) 0.028(3) 0.029(4) 0.006(3) -0.001(2) -0.001(2) C4 0.037(3) 0.032(3) 0.044(4) 0.002(3) -0.001(3) -0.008(3) C5 0.023(3) 0.024(3) 0.033(3) 0.003(2) -0.006(2) -0.004(2) C6 0.021(2) 0.027(3) 0.030(3) -0.002(3) 0.003(3) -0.0054(18) C7 0.047(4) 0.019(3) 0.045(4) 0.007(3) 0.012(3) 0.006(2) C8 0.043(3) 0.028(3) 0.042(4) -0.003(3) 0.013(3) 0.007(3) C9 0.026(3) 0.030(3) 0.033(3) 0.004(3) 0.003(2) -0.001(2) C10 0.023(3) 0.025(3) 0.032(3) -0.005(2) -0.001(2) -0.002(2) C11 0.030(3) 0.036(4) 0.033(4) 0.002(3) 0.001(3) 0.001(3) C12 0.025(3) 0.029(3) 0.027(4) -0.004(3) 0.002(3) 0.004(2) C13 0.030(3) 0.025(3) 0.029(4) 0.000(3) -0.005(2) 0.010(2) C14 0.043(4) 0.033(3) 0.038(4) -0.004(3) 0.001(3) 0.007(3) C15 0.025(3) 0.029(3) 0.026(3) 0.004(2) -0.001(2) -0.006(2) C16 0.026(2) 0.027(3) 0.027(3) 0.006(2) -0.004(2) 0.006(2) C17 0.048(4) 0.025(3) 0.056(5) -0.002(3) 0.016(3) 0.000(3) C18 0.043(4) 0.031(3) 0.055(4) 0.012(3) 0.021(3) -0.001(3) C19 0.020(3) 0.035(3) 0.033(4) 0.004(2) 0.008(3) -0.002(2) C20 0.035(3) 0.025(3) 0.035(4) -0.002(3) -0.004(3) -0.003(2) C21 0.078(7) 0.124(10) 0.051(5) -0.009(6) -0.017(4) -0.043(6) C22 0.070(6) 0.140(10) 0.044(5) -0.016(6) -0.006(4) -0.050(6) C23 0.103(8) 0.106(8) 0.087(7) -0.037(6) 0.025(6) -0.071(6) C24 0.087(5) 0.048(4) 0.094(8) -0.026(4) 0.033(6) -0.037(4) C25 0.052(3) 0.038(3) 0.050(3) -0.013(4) 0.022(3) -0.013(3) C26 0.043(4) 0.030(4) 0.059(5) -0.001(3) 0.011(3) 0.004(3) C27 0.082(6) 0.030(4) 0.101(7) 0.022(4) 0.024(5) 0.019(4) C28 0.060(6) 0.091(7) 0.087(7) 0.031(5) 0.012(5) 0.039(5) C29 0.050(5) 0.102(7) 0.056(5) 0.013(5) -0.007(4) 0.028(5) C30 0.043(4) 0.061(5) 0.050(4) -0.002(3) -0.004(3) 0.000(3) N1 0.025(2) 0.027(2) 0.030(3) -0.002(2) 0.000(2) -0.0004(19) N2 0.029(3) 0.026(3) 0.030(3) -0.002(2) 0.000(2) -0.0045(19) N3 0.033(3) 0.027(3) 0.031(3) 0.000(2) 0.001(2) 0.003(2) N4 0.026(2) 0.024(2) 0.030(3) 0.003(2) 0.002(2) 0.0022(18) N5 0.027(2) 0.031(3) 0.026(3) -0.001(2) 0.002(2) 0.0037(19) N6 0.036(3) 0.025(3) 0.033(3) -0.004(2) 0.009(2) 0.004(2) N7 0.039(3) 0.052(3) 0.037(3) -0.009(2) 0.001(2) -0.016(2) N8 0.038(3) 0.034(3) 0.041(3) -0.001(3) 0.002(2) -0.005(2) O1 0.041(2) 0.036(2) 0.035(3) -0.0089(19) 0.010(2) -0.0092(19) O2 0.050(3) 0.042(3) 0.043(3) -0.007(2) 0.018(2) -0.010(2) O3 0.058(3) 0.045(3) 0.045(3) -0.007(2) 0.019(2) -0.020(2) O4 0.062(3) 0.035(3) 0.056(3) -0.010(2) 0.016(2) -0.025(2) O5 0.046(3) 0.030(2) 0.041(3) 0.007(2) 0.005(2) 0.0105(19) O6 0.063(3) 0.048(3) 0.039(3) 0.004(2) 0.020(2) 0.025(2) O7 0.069(3) 0.051(3) 0.045(3) 0.009(2) 0.019(2) 0.030(2) O8 0.052(3) 0.044(3) 0.044(3) 0.006(2) 0.005(2) 0.023(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.270(4) 2_565 ? Cd1 N1 2.277(4) . ? Cd1 N3 2.365(4) 3 ? Cd1 N6 2.384(4) 4_565 ? Cd1 O1 2.396(4) . ? Cd1 O5 2.404(4) 2_565 ? Cd2 N5 2.285(4) . ? Cd2 N2 2.306(4) . ? Cd2 N7 2.306(5) . ? Cd2 N8 2.318(5) . ? Cd2 O4 2.349(4) . ? Cd2 O8 2.360(4) . ? C1 O1 1.242(7) . ? C1 O2 1.270(7) . ? C1 C2 1.491(9) . ? C2 N1 1.369(6) . ? C2 C3 1.382(8) . ? C3 N2 1.372(7) . ? C3 C4 1.470(7) . ? C4 O4 1.245(6) . ? C4 O3 1.280(6) . ? C5 N1 1.346(7) . ? C5 N2 1.348(6) . ? C5 C6 1.479(7) . ? C6 C10 1.376(6) . ? C6 C7 1.389(7) . ? C7 C8 1.381(7) . ? C7 H7 0.9300 . ? C8 N3 1.338(6) . ? C8 H8 0.9300 . ? C9 N3 1.325(6) . ? C9 C10 1.390(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O5 1.231(7) . ? C11 O6 1.294(7) . ? C11 C12 1.477(8) . ? C12 N4 1.375(6) . ? C12 C13 1.386(8) . ? C13 N5 1.373(7) . ? C13 C14 1.489(7) . ? C14 O8 1.240(7) . ? C14 O7 1.261(6) . ? C15 N5 1.343(6) . ? C15 N4 1.345(6) . ? C15 C16 1.479(7) . ? C16 C17 1.391(6) . ? C16 C19 1.395(7) . ? C17 C18 1.382(7) . ? C17 H17 0.9300 . ? C18 N6 1.327(6) . ? C18 H18 0.9300 . ? C19 C20 1.374(7) . ? C19 H19 0.9300 . ? C20 N6 1.343(7) . ? C20 H20 0.9300 . ? C21 N7 1.318(8) . ? C21 C22 1.424(11) . ? C21 H21 0.9300 . ? C22 C23 1.349(11) . ? C22 H22 0.9300 . ? C23 C24 1.344(10) . ? C23 H23 0.9300 . ? C24 C25 1.369(7) . ? C24 H24 0.9300 . ? C25 N7 1.340(7) . ? C25 C26 1.487(10) . ? C26 N8 1.318(8) . ? C26 C27 1.408(9) . ? C27 C28 1.368(10) . ? C27 H27 0.9300 . ? C28 C29 1.348(9) . ? C28 H28 0.9300 . ? C29 C30 1.366(8) . ? C29 H29 0.9300 . ? C30 N8 1.344(7) . ? C30 H30 0.9300 . ? N3 Cd1 2.365(4) 3_554 ? N4 Cd1 2.270(4) 2_564 ? N6 Cd1 2.384(4) 4_465 ? O2 H2 1.222(15) . ? O3 H2 1.224(15) . ? O5 Cd1 2.404(4) 2_564 ? O6 H6 1.224(15) . ? O7 H6 1.229(15) . ? 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 143.10(13) 2_565 . ? N4 Cd1 N3 114.39(15) 2_565 3 ? N1 Cd1 N3 91.72(15) . 3 ? N4 Cd1 N6 92.66(15) 2_565 4_565 ? N1 Cd1 N6 113.16(16) . 4_565 ? N3 Cd1 N6 91.56(14) 3 4_565 ? N4 Cd1 O1 84.23(14) 2_565 . ? N1 Cd1 O1 72.30(15) . . ? N3 Cd1 O1 84.51(15) 3 . ? N6 Cd1 O1 173.44(14) 4_565 . ? N4 Cd1 O5 72.25(14) 2_565 2_565 ? N1 Cd1 O5 83.14(14) . 2_565 ? N3 Cd1 O5 173.15(15) 3 2_565 ? N6 Cd1 O5 86.35(15) 4_565 2_565 ? O1 Cd1 O5 98.15(11) . 2_565 ? N5 Cd2 N2 83.74(13) . . ? N5 Cd2 N7 110.14(16) . . ? N2 Cd2 N7 155.54(16) . . ? N5 Cd2 N8 158.75(16) . . ? N2 Cd2 N8 102.31(17) . . ? N7 Cd2 N8 72.25(19) . . ? N5 Cd2 O4 114.76(15) . . ? N2 Cd2 O4 73.24(14) . . ? N7 Cd2 O4 82.54(14) . . ? N8 Cd2 O4 86.45(16) . . ? N5 Cd2 O8 73.14(14) . . ? N2 Cd2 O8 116.58(15) . . ? N7 Cd2 O8 87.24(15) . . ? N8 Cd2 O8 86.07(16) . . ? O4 Cd2 O8 168.79(12) . . ? O1 C1 O2 124.4(7) . . ? O1 C1 C2 117.3(6) . . ? O2 C1 C2 118.2(6) . . ? N1 C2 C3 108.3(6) . . ? N1 C2 C1 120.5(5) . . ? C3 C2 C1 131.2(5) . . ? N2 C3 C2 108.6(5) . . ? N2 C3 C4 120.2(5) . . ? C2 C3 C4 130.9(6) . . ? O4 C4 O3 122.0(5) . . ? O4 C4 C3 119.6(6) . . ? O3 C4 C3 118.4(6) . . ? N1 C5 N2 113.3(5) . . ? N1 C5 C6 121.8(4) . . ? N2 C5 C6 124.4(5) . . ? C10 C6 C7 118.1(5) . . ? C10 C6 C5 119.8(5) . . ? C7 C6 C5 122.1(5) . . ? C8 C7 C6 118.3(5) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? N3 C8 C7 124.5(5) . . ? N3 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? N3 C9 C10 124.0(5) . . ? N3 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C6 C10 C9 118.9(5) . . ? C6 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? O5 C11 O6 121.9(6) . . ? O5 C11 C12 119.9(6) . . ? O6 C11 C12 118.2(5) . . ? N4 C12 C13 109.1(5) . . ? N4 C12 C11 118.8(5) . . ? C13 C12 C11 132.1(5) . . ? N5 C13 C12 107.9(5) . . ? N5 C13 C14 121.1(5) . . ? C12 C13 C14 130.4(6) . . ? O8 C14 O7 124.8(6) . . ? O8 C14 C13 117.2(6) . . ? O7 C14 C13 117.7(6) . . ? N5 C15 N4 114.2(5) . . ? N5 C15 C16 124.9(5) . . ? N4 C15 C16 120.6(5) . . ? C17 C16 C19 116.4(5) . . ? C17 C16 C15 123.4(5) . . ? C19 C16 C15 120.2(4) . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N6 C18 C17 124.4(5) . . ? N6 C18 H18 117.8 . . ? C17 C18 H18 117.8 . . ? C20 C19 C16 120.3(5) . . ? C20 C19 H19 119.9 . . ? C16 C19 H19 119.9 . . ? N6 C20 C19 123.1(5) . . ? N6 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? N7 C21 C22 120.0(9) . . ? N7 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.1(9) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 119.5(9) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.4(8) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? N7 C25 C24 121.0(7) . . ? N7 C25 C26 117.0(5) . . ? C24 C25 C26 122.0(7) . . ? N8 C26 C27 119.9(6) . . ? N8 C26 C25 117.9(6) . . ? C27 C26 C25 122.2(6) . . ? C28 C27 C26 119.5(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 120.1(7) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 118.0(7) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? N8 C30 C29 123.3(7) . . ? N8 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C5 N1 C2 105.0(4) . . ? C5 N1 Cd1 140.7(3) . . ? C2 N1 Cd1 113.5(4) . . ? C5 N2 C3 104.6(4) . . ? C5 N2 Cd2 142.0(4) . . ? C3 N2 Cd2 111.7(3) . . ? C9 N3 C8 116.1(5) . . ? C9 N3 Cd1 118.0(3) . 3_554 ? C8 N3 Cd1 122.5(4) . 3_554 ? C15 N4 C12 103.9(4) . . ? C15 N4 Cd1 141.6(3) . 2_564 ? C12 N4 Cd1 114.3(3) . 2_564 ? C15 N5 C13 104.8(4) . . ? C15 N5 Cd2 139.4(4) . . ? C13 N5 Cd2 111.7(3) . . ? C18 N6 C20 116.6(5) . . ? C18 N6 Cd1 122.5(4) . 4_465 ? C20 N6 Cd1 118.1(3) . 4_465 ? C21 N7 C25 120.0(7) . . ? C21 N7 Cd2 123.8(6) . . ? C25 N7 Cd2 116.0(4) . . ? C26 N8 C30 119.2(6) . . ? C26 N8 Cd2 115.5(4) . . ? C30 N8 Cd2 124.1(4) . . ? C1 O1 Cd1 116.0(4) . . ? C1 O2 H2 114(3) . . ? C4 O3 H2 115(3) . . ? C4 O4 Cd2 115.1(4) . . ? C11 O5 Cd1 114.5(4) . 2_564 ? C11 O6 H6 109(3) . . ? C14 O7 H6 111(3) . . ? C14 O8 Cd2 116.2(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 O1 C1 C2 N1 -4.2(8) . . . . ? O2 C1 C2 N1 173.2(5) . . . . ? O1 C1 C2 C3 176.0(6) . . . . ? O2 C1 C2 C3 -6.6(9) . . . . ? N1 C2 C3 N2 2.5(6) . . . . ? C1 C2 C3 N2 -177.7(5) . . . . ? N1 C2 C3 C4 -170.8(5) . . . . ? C1 C2 C3 C4 9.0(10) . . . . ? N2 C3 C4 O4 0.7(8) . . . . ? C2 C3 C4 O4 173.4(6) . . . . ? N2 C3 C4 O3 -177.0(5) . . . . ? C2 C3 C4 O3 -4.3(9) . . . . ? N1 C5 C6 C10 -30.8(7) . . . . ? N2 C5 C6 C10 140.9(5) . . . . ? N1 C5 C6 C7 149.1(5) . . . . ? N2 C5 C6 C7 -39.3(8) . . . . ? C10 C6 C7 C8 3.0(8) . . . . ? C5 C6 C7 C8 -176.9(5) . . . . ? C6 C7 C8 N3 -0.4(9) . . . . ? C7 C6 C10 C9 -2.7(7) . . . . ? C5 C6 C10 C9 177.1(4) . . . . ? N3 C9 C10 C6 -0.2(8) . . . . ? O5 C11 C12 N4 -5.8(9) . . . . ? O6 C11 C12 N4 175.2(5) . . . . ? O5 C11 C12 C13 177.3(6) . . . . ? O6 C11 C12 C13 -1.8(10) . . . . ? N4 C12 C13 N5 1.2(6) . . . . ? C11 C12 C13 N5 178.4(6) . . . . ? N4 C12 C13 C14 -169.6(5) . . . . ? C11 C12 C13 C14 7.6(10) . . . . ? N5 C13 C14 O8 -3.1(8) . . . . ? C12 C13 C14 O8 166.7(6) . . . . ? N5 C13 C14 O7 -178.4(5) . . . . ? C12 C13 C14 O7 -8.6(9) . . . . ? N5 C15 C16 C17 -49.6(7) . . . . ? N4 C15 C16 C17 137.4(5) . . . . ? N5 C15 C16 C19 128.7(5) . . . . ? N4 C15 C16 C19 -44.3(7) . . . . ? C19 C16 C17 C18 4.0(8) . . . . ? C15 C16 C17 C18 -177.6(5) . . . . ? C16 C17 C18 N6 -1.5(9) . . . . ? C17 C16 C19 C20 -4.5(7) . . . . ? C15 C16 C19 C20 177.0(5) . . . . ? C16 C19 C20 N6 2.5(8) . . . . ? N7 C21 C22 C23 -0.2(13) . . . . ? C21 C22 C23 C24 0.1(14) . . . . ? C22 C23 C24 C25 1.0(13) . . . . ? C23 C24 C25 N7 -2.2(12) . . . . ? C23 C24 C25 C26 178.7(8) . . . . ? N7 C25 C26 N8 -12.9(10) . . . . ? C24 C25 C26 N8 166.3(7) . . . . ? N7 C25 C26 C27 167.2(7) . . . . ? C24 C25 C26 C27 -13.6(11) . . . . ? N8 C26 C27 C28 -2.1(10) . . . . ? C25 C26 C27 C28 177.8(7) . . . . ? C26 C27 C28 C29 0.5(12) . . . . ? C27 C28 C29 C30 2.6(12) . . . . ? C28 C29 C30 N8 -4.3(11) . . . . ? N2 C5 N1 C2 -0.5(6) . . . . ? C6 C5 N1 C2 172.0(4) . . . . ? N2 C5 N1 Cd1 168.2(4) . . . . ? C6 C5 N1 Cd1 -19.3(8) . . . . ? C3 C2 N1 C5 -1.2(6) . . . . ? C1 C2 N1 C5 178.9(5) . . . . ? C3 C2 N1 Cd1 -173.5(3) . . . . ? C1 C2 N1 Cd1 6.7(6) . . . . ? N4 Cd1 N1 C5 134.0(5) 2_565 . . . ? N3 Cd1 N1 C5 -89.3(5) 3 . . . ? N6 Cd1 N1 C5 3.2(6) 4_565 . . . ? O1 Cd1 N1 C5 -172.9(6) . . . . ? O5 Cd1 N1 C5 86.2(5) 2_565 . . . ? N4 Cd1 N1 C2 -57.9(5) 2_565 . . . ? N3 Cd1 N1 C2 78.9(3) 3 . . . ? N6 Cd1 N1 C2 171.3(3) 4_565 . . . ? O1 Cd1 N1 C2 -4.8(3) . . . . ? O5 Cd1 N1 C2 -105.7(4) 2_565 . . . ? N1 C5 N2 C3 2.0(6) . . . . ? C6 C5 N2 C3 -170.3(5) . . . . ? N1 C5 N2 Cd2 164.4(4) . . . . ? C6 C5 N2 Cd2 -7.9(9) . . . . ? C2 C3 N2 C5 -2.7(6) . . . . ? C4 C3 N2 C5 171.5(5) . . . . ? C2 C3 N2 Cd2 -171.1(3) . . . . ? C4 C3 N2 Cd2 3.1(6) . . . . ? N5 Cd2 N2 C5 -47.0(6) . . . . ? N7 Cd2 N2 C5 -173.5(5) . . . . ? N8 Cd2 N2 C5 112.4(6) . . . . ? O4 Cd2 N2 C5 -165.2(6) . . . . ? O8 Cd2 N2 C5 20.6(6) . . . . ? N5 Cd2 N2 C3 114.7(3) . . . . ? N7 Cd2 N2 C3 -11.9(6) . . . . ? N8 Cd2 N2 C3 -86.0(4) . . . . ? O4 Cd2 N2 C3 -3.6(3) . . . . ? O8 Cd2 N2 C3 -177.7(3) . . . . ? C10 C9 N3 C8 2.7(7) . . . . ? C10 C9 N3 Cd1 -157.0(4) . . . 3_554 ? C7 C8 N3 C9 -2.5(8) . . . . ? C7 C8 N3 Cd1 156.3(5) . . . 3_554 ? N5 C15 N4 C12 -1.3(6) . . . . ? C16 C15 N4 C12 172.4(4) . . . . ? N5 C15 N4 Cd1 172.2(4) . . . 2_564 ? C16 C15 N4 Cd1 -14.1(8) . . . 2_564 ? C13 C12 N4 C15 0.0(6) . . . . ? C11 C12 N4 C15 -177.7(5) . . . . ? C13 C12 N4 Cd1 -175.6(3) . . . 2_564 ? C11 C12 N4 Cd1 6.8(6) . . . 2_564 ? N4 C15 N5 C13 2.0(6) . . . . ? C16 C15 N5 C13 -171.4(5) . . . . ? N4 C15 N5 Cd2 155.7(4) . . . . ? C16 C15 N5 Cd2 -17.6(8) . . . . ? C12 C13 N5 C15 -1.9(6) . . . . ? C14 C13 N5 C15 170.0(5) . . . . ? C12 C13 N5 Cd2 -163.8(3) . . . . ? C14 C13 N5 Cd2 8.0(6) . . . . ? N2 Cd2 N5 C15 -39.1(5) . . . . ? N7 Cd2 N5 C15 120.1(5) . . . . ? N8 Cd2 N5 C15 -147.2(5) . . . . ? O4 Cd2 N5 C15 29.2(5) . . . . ? O8 Cd2 N5 C15 -159.3(5) . . . . ? N2 Cd2 N5 C13 113.5(4) . . . . ? N7 Cd2 N5 C13 -87.3(4) . . . . ? N8 Cd2 N5 C13 5.4(7) . . . . ? O4 Cd2 N5 C13 -178.2(3) . . . . ? O8 Cd2 N5 C13 -6.7(3) . . . . ? C17 C18 N6 C20 -0.7(9) . . . . ? C17 C18 N6 Cd1 159.9(5) . . . 4_465 ? C19 C20 N6 C18 0.2(8) . . . . ? C19 C20 N6 Cd1 -161.3(4) . . . 4_465 ? C22 C21 N7 C25 -0.9(12) . . . . ? C22 C21 N7 Cd2 174.0(6) . . . . ? C24 C25 N7 C21 2.1(11) . . . . ? C26 C25 N7 C21 -178.7(7) . . . . ? C24 C25 N7 Cd2 -173.3(6) . . . . ? C26 C25 N7 Cd2 5.9(9) . . . . ? N5 Cd2 N7 C21 -17.2(6) . . . . ? N2 Cd2 N7 C21 104.5(6) . . . . ? N8 Cd2 N7 C21 -174.8(6) . . . . ? O4 Cd2 N7 C21 96.5(6) . . . . ? O8 Cd2 N7 C21 -88.1(6) . . . . ? N5 Cd2 N7 C25 157.9(5) . . . . ? N2 Cd2 N7 C25 -80.4(6) . . . . ? N8 Cd2 N7 C25 0.3(5) . . . . ? O4 Cd2 N7 C25 -88.4(5) . . . . ? O8 Cd2 N7 C25 87.0(5) . . . . ? C27 C26 N8 C30 0.5(9) . . . . ? C25 C26 N8 C30 -179.4(6) . . . . ? C27 C26 N8 Cd2 -167.2(5) . . . . ? C25 C26 N8 Cd2 12.8(7) . . . . ? C29 C30 N8 C26 2.7(10) . . . . ? C29 C30 N8 Cd2 169.4(5) . . . . ? N5 Cd2 N8 C26 -107.2(5) . . . . ? N2 Cd2 N8 C26 148.1(4) . . . . ? N7 Cd2 N8 C26 -7.2(4) . . . . ? O4 Cd2 N8 C26 76.1(4) . . . . ? O8 Cd2 N8 C26 -95.5(4) . . . . ? N5 Cd2 N8 C30 85.7(7) . . . . ? N2 Cd2 N8 C30 -19.0(5) . . . . ? N7 Cd2 N8 C30 -174.3(5) . . . . ? O4 Cd2 N8 C30 -91.0(5) . . . . ? O8 Cd2 N8 C30 97.4(5) . . . . ? O2 C1 O1 Cd1 -177.8(5) . . . . ? C2 C1 O1 Cd1 -0.6(7) . . . . ? N4 Cd1 O1 C1 154.1(4) 2_565 . . . ? N1 Cd1 O1 C1 3.0(4) . . . . ? N3 Cd1 O1 C1 -90.6(4) 3 . . . ? N6 Cd1 O1 C1 -144.0(12) 4_565 . . . ? O5 Cd1 O1 C1 83.0(4) 2_565 . . . ? O3 C4 O4 Cd2 173.5(4) . . . . ? C3 C4 O4 Cd2 -4.1(7) . . . . ? N5 Cd2 O4 C4 -70.5(4) . . . . ? N2 Cd2 O4 C4 4.2(4) . . . . ? N7 Cd2 O4 C4 -179.2(4) . . . . ? N8 Cd2 O4 C4 108.2(4) . . . . ? O8 Cd2 O4 C4 156.4(7) . . . . ? O6 C11 O5 Cd1 -179.4(5) . . . 2_564 ? C12 C11 O5 Cd1 1.6(7) . . . 2_564 ? O7 C14 O8 Cd2 171.3(5) . . . . ? C13 C14 O8 Cd2 -3.6(7) . . . . ? N5 Cd2 O8 C14 5.8(4) . . . . ? N2 Cd2 O8 C14 -68.0(5) . . . . ? N7 Cd2 O8 C14 117.8(4) . . . . ? N8 Cd2 O8 C14 -169.8(5) . . . . ? O4 Cd2 O8 C14 142.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.430 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.096 data_2 _database_code_depnum_ccdc_archive 'CCDC 837790' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H18 Cd3 N6 O20, 2(H2O0.50)' _chemical_formula_sum 'C30 H22 Cd3 N6 O21' _chemical_formula_weight 1139.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.652(2) _cell_length_b 9.105(6) _cell_length_c 12.290(5) _cell_angle_alpha 93.175(4) _cell_angle_beta 100.408(3) _cell_angle_gamma 113.747(8) _cell_volume 862.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.450 _exptl_absorpt_correction_T_max 0.565 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5288 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.26 _reflns_number_total 3839 _reflns_number_gt 3255 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. H atoms of two water molecules were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1A...H1B and H2A...H2B were restrained to 1.35+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.7954P] 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 3004 _refine_ls_number_parameters 293 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.998 _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 0.0000 0.0000 1.0000 0.02707(15) Uani 1 2 d S . . Cd2 Cd 0.51622(4) 0.45830(4) 0.66688(2) 0.02065(13) Uani 1 1 d . . . C1 C 0.4222(6) 0.5934(5) 0.8698(4) 0.0229(9) Uani 1 1 d . . . C2 C 0.3377(6) 0.4165(5) 0.8670(3) 0.0185(9) Uani 1 1 d . . . C3 C 0.2202(5) 0.3214(5) 0.9267(3) 0.0177(9) Uani 1 1 d . . . C4 C 0.1459(6) 0.3670(5) 1.0139(4) 0.0244(10) Uani 1 1 d . . . C5 C 0.2725(5) 0.1661(5) 0.8156(3) 0.0184(9) Uani 1 1 d . . . C6 C 0.2651(6) 0.0170(5) 0.7548(3) 0.0192(9) Uani 1 1 d . . . C7 C 0.3931(6) 0.0206(5) 0.7004(4) 0.0297(11) Uani 1 1 d . . . H7 H 0.4854 0.1183 0.6988 0.036 Uiso 1 1 calc R . . C8 C 0.3818(6) -0.1219(6) 0.6489(4) 0.0312(11) Uani 1 1 d . . . H8 H 0.4680 -0.1206 0.6128 0.037 Uiso 1 1 calc R . . C9 C 0.1214(7) -0.2685(6) 0.6988(4) 0.0314(11) Uani 1 1 d . . . H9 H 0.0285 -0.3672 0.6972 0.038 Uiso 1 1 calc R . . C10 C 0.1270(6) -0.1287(5) 0.7517(4) 0.0274(10) Uani 1 1 d . . . H10 H 0.0376 -0.1327 0.7853 0.033 Uiso 1 1 calc R . . C11 C 1.0839(5) 1.3334(5) 0.5877(3) 0.0198(9) Uani 1 1 d . . . C12 C 1.0435(5) 1.1609(5) 0.5415(3) 0.0174(8) Uani 1 1 d . . . C13 C 0.9015(5) 1.0347(5) 0.5646(3) 0.0186(9) Uani 1 1 d . . . H13 H 0.8352 1.0582 0.6086 0.022 Uiso 1 1 calc R . . C14 C 0.8568(5) 0.8746(5) 0.5235(3) 0.0176(9) Uani 1 1 d . . . C15 C 0.7018(6) 0.7417(5) 0.5538(3) 0.0214(9) Uani 1 1 d . . . N1 N 0.3692(5) 0.3163(4) 0.7966(3) 0.0199(8) Uani 1 1 d . . . N2 N 0.1800(5) 0.1632(4) 0.8931(3) 0.0206(8) Uani 1 1 d . . . N3 N 0.2490(5) -0.2627(4) 0.6497(3) 0.0281(9) Uani 1 1 d . . . O1 O 0.5240(4) 0.6494(4) 0.8068(3) 0.0278(7) Uani 1 1 d . . . O2 O 0.3887(5) 0.6828(4) 0.9365(3) 0.0337(8) Uani 1 1 d . . . O1W O 0.7274(4) 0.3660(4) 0.7278(3) 0.0331(8) Uani 1 1 d D . . O3 O 0.1918(4) 0.5189(4) 1.0453(3) 0.0305(8) Uani 1 1 d . . . O2W O 0.2322(6) 0.0321(5) 1.1433(4) 0.0561(12) Uani 1 1 d D . . O4 O 0.0433(5) 0.2606(4) 1.0565(3) 0.0335(8) Uani 1 1 d . . . O3W O 0.4435(14) 0.9821(13) 0.0284(9) 0.073(3) Uani 0.50 1 d PU . . O5 O 1.2332(4) 1.4424(3) 0.5882(3) 0.0242(7) Uani 1 1 d . . . O6 O 0.9707(5) 1.3604(4) 0.6201(4) 0.0462(10) Uani 1 1 d . . . O7 O 0.5531(4) 0.7042(4) 0.4950(3) 0.0278(7) Uani 1 1 d . . . O8 O 0.7323(4) 0.6830(4) 0.6400(3) 0.0328(8) Uani 1 1 d . . . H1A H 0.798(6) 0.358(8) 0.692(4) 0.06(2) Uiso 1 1 d D . . H1B H 0.782(6) 0.405(7) 0.794(2) 0.06(2) Uiso 1 1 d D . . H2A H 0.306(7) 0.129(3) 1.159(6) 0.08(3) Uiso 1 1 d D . . H2B H 0.285(8) -0.021(7) 1.123(8) 0.11(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0318(3) 0.0154(2) 0.0313(3) 0.00457(19) 0.0155(2) 0.0034(2) Cd2 0.0217(2) 0.01523(19) 0.02268(19) 0.00075(13) 0.01108(13) 0.00301(14) C1 0.027(2) 0.016(2) 0.023(2) 0.0010(18) 0.0052(18) 0.0067(19) C2 0.023(2) 0.014(2) 0.018(2) 0.0016(16) 0.0079(16) 0.0060(18) C3 0.023(2) 0.013(2) 0.018(2) 0.0022(16) 0.0086(17) 0.0066(17) C4 0.025(2) 0.019(2) 0.028(2) 0.0026(19) 0.0123(19) 0.006(2) C5 0.024(2) 0.012(2) 0.018(2) 0.0023(16) 0.0069(17) 0.0053(18) C6 0.026(2) 0.014(2) 0.019(2) 0.0022(16) 0.0055(17) 0.0102(18) C7 0.029(3) 0.014(2) 0.044(3) 0.000(2) 0.013(2) 0.006(2) C8 0.030(3) 0.026(3) 0.042(3) -0.002(2) 0.014(2) 0.015(2) C9 0.040(3) 0.013(2) 0.034(3) -0.0015(19) 0.009(2) 0.004(2) C10 0.033(3) 0.016(2) 0.031(2) 0.0019(19) 0.016(2) 0.005(2) C11 0.024(2) 0.014(2) 0.022(2) 0.0009(17) 0.0107(17) 0.0064(19) C12 0.017(2) 0.014(2) 0.018(2) -0.0002(16) 0.0053(16) 0.0035(17) C13 0.022(2) 0.014(2) 0.023(2) 0.0010(17) 0.0094(17) 0.0078(18) C14 0.020(2) 0.013(2) 0.018(2) 0.0029(16) 0.0066(16) 0.0050(17) C15 0.030(3) 0.010(2) 0.022(2) -0.0035(17) 0.0137(19) 0.0039(18) N1 0.023(2) 0.0142(18) 0.0228(18) 0.0006(14) 0.0088(15) 0.0076(16) N2 0.022(2) 0.0119(18) 0.0259(19) 0.0021(15) 0.0103(15) 0.0038(15) N3 0.036(2) 0.0175(19) 0.032(2) -0.0013(16) 0.0050(18) 0.0146(18) O1 0.0347(19) 0.0146(15) 0.0291(17) -0.0002(13) 0.0159(14) 0.0019(14) O2 0.051(2) 0.0131(16) 0.0402(19) 0.0017(14) 0.0275(17) 0.0102(15) O1W 0.0288(19) 0.037(2) 0.035(2) 0.0006(16) 0.0127(16) 0.0139(17) O3 0.044(2) 0.0163(16) 0.0344(18) -0.0010(14) 0.0213(15) 0.0114(15) O2W 0.046(3) 0.026(2) 0.073(3) 0.007(2) -0.010(2) 0.001(2) O4 0.046(2) 0.0184(16) 0.0394(19) 0.0051(14) 0.0311(17) 0.0071(15) O3W 0.082(5) 0.058(4) 0.081(5) 0.002(4) 0.019(4) 0.030(4) O5 0.0264(17) 0.0096(14) 0.0354(18) -0.0006(13) 0.0117(13) 0.0048(13) O6 0.036(2) 0.0196(18) 0.084(3) -0.0086(18) 0.037(2) 0.0038(16) O7 0.0188(17) 0.0244(17) 0.0363(18) -0.0082(14) 0.0106(14) 0.0049(14) O8 0.0318(19) 0.0224(17) 0.0342(19) 0.0067(15) 0.0130(15) -0.0013(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.294(3) 2_557 ? Cd1 O4 2.294(3) . ? Cd1 O2W 2.327(4) 2_557 ? Cd1 O2W 2.327(4) . ? Cd1 N2 2.335(4) . ? Cd1 N2 2.335(4) 2_557 ? Cd2 O8 2.238(3) . ? Cd2 O7 2.243(3) 2_666 ? Cd2 O1W 2.328(4) . ? Cd2 N1 2.339(4) . ? Cd2 O1 2.350(3) . ? Cd2 O5 2.408(3) 1_445 ? C1 O1 1.250(6) . ? C1 O2 1.274(6) . ? C1 C2 1.471(6) . ? C2 N1 1.361(5) . ? C2 C3 1.398(6) . ? C3 N2 1.358(5) . ? C3 C4 1.466(6) . ? C4 O4 1.238(5) . ? C4 O3 1.289(5) . ? C5 N2 1.344(5) . ? C5 N1 1.345(5) . ? C5 C6 1.486(6) . ? C6 C10 1.375(6) . ? C6 C7 1.383(6) . ? C7 C8 1.371(6) . ? C7 H7 0.9300 . ? C8 N3 1.335(6) . ? C8 H8 0.9300 . ? C9 N3 1.336(6) . ? C9 C10 1.376(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 O6 1.225(5) . ? C11 O5 1.272(5) . ? C11 C12 1.516(6) . ? C12 C13 1.391(6) . ? C12 C14 1.390(6) 2_776 ? C13 C14 1.387(6) . ? C13 H13 0.9300 . ? C14 C12 1.390(6) 2_776 ? C14 C15 1.525(6) . ? C15 O8 1.245(5) . ? C15 O7 1.256(5) . ? O1W H1A 0.839(19) . ? O1W H1B 0.84(2) . ? O2W H2A 0.84(2) . ? O2W H2B 0.85(2) . ? O3W O3W 1.25(2) 2_675 ? O5 Cd2 2.408(3) 1_665 ? O7 Cd2 2.243(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O4 180.000(1) 2_557 . ? O4 Cd1 O2W 89.02(15) 2_557 2_557 ? O4 Cd1 O2W 90.98(15) . 2_557 ? O4 Cd1 O2W 90.98(15) 2_557 . ? O4 Cd1 O2W 89.02(15) . . ? O2W Cd1 O2W 180.000(1) 2_557 . ? O4 Cd1 N2 106.19(12) 2_557 . ? O4 Cd1 N2 73.81(12) . . ? O2W Cd1 N2 87.07(15) 2_557 . ? O2W Cd1 N2 92.93(15) . . ? O4 Cd1 N2 73.81(12) 2_557 2_557 ? O4 Cd1 N2 106.19(12) . 2_557 ? O2W Cd1 N2 92.93(15) 2_557 2_557 ? O2W Cd1 N2 87.07(15) . 2_557 ? N2 Cd1 N2 180.000(1) . 2_557 ? O8 Cd2 O7 102.05(12) . 2_666 ? O8 Cd2 O1W 86.35(14) . . ? O7 Cd2 O1W 87.25(12) 2_666 . ? O8 Cd2 N1 146.18(12) . . ? O7 Cd2 N1 110.79(12) 2_666 . ? O1W Cd2 N1 87.34(13) . . ? O8 Cd2 O1 78.90(12) . . ? O7 Cd2 O1 162.65(12) 2_666 . ? O1W Cd2 O1 110.08(13) . . ? N1 Cd2 O1 72.22(12) . . ? O8 Cd2 O5 113.41(12) . 1_445 ? O7 Cd2 O5 78.98(11) 2_666 1_445 ? O1W Cd2 O5 157.77(12) . 1_445 ? N1 Cd2 O5 81.46(12) . 1_445 ? O1 Cd2 O5 84.74(11) . 1_445 ? O1 C1 O2 122.8(4) . . ? O1 C1 C2 118.7(4) . . ? O2 C1 C2 118.5(4) . . ? N1 C2 C3 108.4(4) . . ? N1 C2 C1 120.5(4) . . ? C3 C2 C1 131.1(4) . . ? N2 C3 C2 108.3(4) . . ? N2 C3 C4 120.8(4) . . ? C2 C3 C4 131.0(4) . . ? O4 C4 O3 121.6(4) . . ? O4 C4 C3 119.9(4) . . ? O3 C4 C3 118.5(4) . . ? N2 C5 N1 113.8(4) . . ? N2 C5 C6 123.1(4) . . ? N1 C5 C6 123.1(4) . . ? C10 C6 C7 118.9(4) . . ? C10 C6 C5 119.3(4) . . ? C7 C6 C5 121.8(4) . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N3 C8 C7 121.0(4) . . ? N3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? N3 C9 C10 120.1(4) . . ? N3 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C6 119.9(4) . . ? C9 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? O6 C11 O5 123.9(4) . . ? O6 C11 C12 118.5(4) . . ? O5 C11 C12 117.6(4) . . ? C13 C12 C14 119.2(4) . 2_776 ? C13 C12 C11 118.8(4) . . ? C14 C12 C11 122.0(4) 2_776 . ? C12 C13 C14 121.4(4) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C12 119.4(4) . 2_776 ? C13 C14 C15 118.7(4) . . ? C12 C14 C15 121.8(4) 2_776 . ? O8 C15 O7 124.4(4) . . ? O8 C15 C14 116.5(4) . . ? O7 C15 C14 119.0(4) . . ? C5 N1 C2 104.7(4) . . ? C5 N1 Cd2 142.7(3) . . ? C2 N1 Cd2 110.8(3) . . ? C5 N2 C3 104.9(3) . . ? C5 N2 Cd1 145.2(3) . . ? C3 N2 Cd1 109.6(3) . . ? C9 N3 C8 121.0(4) . . ? C1 O1 Cd2 115.2(3) . . ? Cd2 O1W H1A 126(4) . . ? Cd2 O1W H1B 113(4) . . ? H1A O1W H1B 108(3) . . ? Cd1 O2W H2A 112(5) . . ? Cd1 O2W H2B 110(6) . . ? H2A O2W H2B 106(3) . . ? C4 O4 Cd1 115.7(3) . . ? C11 O5 Cd2 130.2(3) . 1_665 ? C15 O7 Cd2 115.9(3) . 2_666 ? C15 O8 Cd2 116.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 -0.4(6) . . . . ? O2 C1 C2 N1 179.8(4) . . . . ? O1 C1 C2 C3 -180.0(4) . . . . ? O2 C1 C2 C3 0.2(7) . . . . ? N1 C2 C3 N2 0.1(5) . . . . ? C1 C2 C3 N2 179.7(4) . . . . ? N1 C2 C3 C4 178.7(4) . . . . ? C1 C2 C3 C4 -1.7(8) . . . . ? N2 C3 C4 O4 -1.1(7) . . . . ? C2 C3 C4 O4 -179.5(4) . . . . ? N2 C3 C4 O3 178.0(4) . . . . ? C2 C3 C4 O3 -0.4(7) . . . . ? N2 C5 C6 C10 19.0(6) . . . . ? N1 C5 C6 C10 -159.5(4) . . . . ? N2 C5 C6 C7 -161.3(4) . . . . ? N1 C5 C6 C7 20.2(7) . . . . ? C10 C6 C7 C8 -2.5(7) . . . . ? C5 C6 C7 C8 177.8(4) . . . . ? C6 C7 C8 N3 0.7(8) . . . . ? N3 C9 C10 C6 -0.6(7) . . . . ? C7 C6 C10 C9 2.5(7) . . . . ? C5 C6 C10 C9 -177.9(4) . . . . ? O6 C11 C12 C13 -17.2(6) . . . . ? O5 C11 C12 C13 164.2(4) . . . . ? O6 C11 C12 C14 162.4(4) . . . 2_776 ? O5 C11 C12 C14 -16.2(6) . . . 2_776 ? C14 C12 C13 C14 -0.5(7) 2_776 . . . ? C11 C12 C13 C14 179.2(4) . . . . ? C12 C13 C14 C12 0.5(7) . . . 2_776 ? C12 C13 C14 C15 178.8(4) . . . . ? C13 C14 C15 O8 -90.5(5) . . . . ? C12 C14 C15 O8 87.8(5) 2_776 . . . ? C13 C14 C15 O7 86.2(5) . . . . ? C12 C14 C15 O7 -95.5(5) 2_776 . . . ? N2 C5 N1 C2 0.4(5) . . . . ? C6 C5 N1 C2 179.0(4) . . . . ? N2 C5 N1 Cd2 -161.2(3) . . . . ? C6 C5 N1 Cd2 17.5(7) . . . . ? C3 C2 N1 C5 -0.3(5) . . . . ? C1 C2 N1 C5 -179.9(4) . . . . ? C3 C2 N1 Cd2 167.9(3) . . . . ? C1 C2 N1 Cd2 -11.8(5) . . . . ? O8 Cd2 N1 C5 -154.0(4) . . . . ? O7 Cd2 N1 C5 11.5(5) 2_666 . . . ? O1W Cd2 N1 C5 -74.5(5) . . . . ? O1 Cd2 N1 C5 173.4(5) . . . . ? O5 Cd2 N1 C5 86.2(5) 1_445 . . . ? O8 Cd2 N1 C2 45.2(4) . . . . ? O7 Cd2 N1 C2 -149.4(3) 2_666 . . . ? O1W Cd2 N1 C2 124.6(3) . . . . ? O1 Cd2 N1 C2 12.5(3) . . . . ? O5 Cd2 N1 C2 -74.7(3) 1_445 . . . ? N1 C5 N2 C3 -0.3(5) . . . . ? C6 C5 N2 C3 -179.0(4) . . . . ? N1 C5 N2 Cd1 -173.1(4) . . . . ? C6 C5 N2 Cd1 8.3(8) . . . . ? C2 C3 N2 C5 0.2(5) . . . . ? C4 C3 N2 C5 -178.6(4) . . . . ? C2 C3 N2 Cd1 175.8(3) . . . . ? C4 C3 N2 Cd1 -3.0(5) . . . . ? O4 Cd1 N2 C5 -3.8(5) 2_557 . . . ? O4 Cd1 N2 C5 176.2(5) . . . . ? O2W Cd1 N2 C5 -91.9(5) 2_557 . . . ? O2W Cd1 N2 C5 88.1(5) . . . . ? N2 Cd1 N2 C5 170(100) 2_557 . . . ? O4 Cd1 N2 C3 -176.3(3) 2_557 . . . ? O4 Cd1 N2 C3 3.7(3) . . . . ? O2W Cd1 N2 C3 95.6(3) 2_557 . . . ? O2W Cd1 N2 C3 -84.4(3) . . . . ? N2 Cd1 N2 C3 -3(100) 2_557 . . . ? C10 C9 N3 C8 -1.4(7) . . . . ? C7 C8 N3 C9 1.3(7) . . . . ? O2 C1 O1 Cd2 -167.5(4) . . . . ? C2 C1 O1 Cd2 12.7(5) . . . . ? O8 Cd2 O1 C1 -176.0(3) . . . . ? O7 Cd2 O1 C1 89.1(5) 2_666 . . . ? O1W Cd2 O1 C1 -94.1(3) . . . . ? N1 Cd2 O1 C1 -13.8(3) . . . . ? O5 Cd2 O1 C1 68.9(3) 1_445 . . . ? O3 C4 O4 Cd1 -174.4(3) . . . . ? C3 C4 O4 Cd1 4.7(6) . . . . ? O4 Cd1 O4 C4 23(100) 2_557 . . . ? O2W Cd1 O4 C4 -91.3(4) 2_557 . . . ? O2W Cd1 O4 C4 88.7(4) . . . . ? N2 Cd1 O4 C4 -4.6(3) . . . . ? N2 Cd1 O4 C4 175.4(3) 2_557 . . . ? O6 C11 O5 Cd2 126.8(4) . . . 1_665 ? C12 C11 O5 Cd2 -54.7(5) . . . 1_665 ? O8 C15 O7 Cd2 -104.5(4) . . . 2_666 ? C14 C15 O7 Cd2 79.2(4) . . . 2_666 ? O7 C15 O8 Cd2 14.8(5) . . . . ? C14 C15 O8 Cd2 -168.8(3) . . . . ? O7 Cd2 O8 C15 53.2(3) 2_666 . . . ? O1W Cd2 O8 C15 139.6(3) . . . . ? N1 Cd2 O8 C15 -140.7(3) . . . . ? O1 Cd2 O8 C15 -109.1(3) . . . . ? O5 Cd2 O8 C15 -29.8(3) 1_445 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O6 0.839(19) 1.86(2) 2.697(5) 174(6) 1_545 O1W H1B O3 0.84(2) 2.00(3) 2.782(5) 155(5) 2_667 O2W H2A O1 0.84(2) 1.92(2) 2.764(5) 179(7) 2_667 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.732 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.131 data_3 _database_code_depnum_ccdc_archive 'CCDC 837791' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H9 Cd2 Cl N3 O7, H2O' _chemical_formula_sum 'C14 H11 Cd2 Cl N3 O8' _chemical_formula_weight 609.48 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' Cl Cl 0.1484 0.1585 '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 8.743(5) _cell_length_b 9.887(5) _cell_length_c 11.655(1) _cell_angle_alpha 71.127(9) _cell_angle_beta 72.770(1) _cell_angle_gamma 65.701(5) _cell_volume 853.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.585 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4306 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2956 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The restraint command 'ISOR' was used to refine the oxygen atom of water mocule O2W. 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. H atoms of coordination water molecule were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1A...H1B was restrained to 1.35+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.4671P] 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 2956 _refine_ls_number_parameters 261 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.129 _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 0.57993(4) 1.30751(3) 0.11959(3) 0.01997(10) Uani 1 1 d . . . Cd2 Cd 0.56009(4) 0.58746(3) 0.32407(3) 0.02314(11) Uani 1 1 d . . . C1 C 0.2547(5) 1.2313(5) 0.2482(4) 0.0243(9) Uani 1 1 d . . . C2 C 0.3864(5) 1.0823(5) 0.2314(4) 0.0200(8) Uani 1 1 d . . . C3 C 0.3782(5) 0.9370(4) 0.2681(4) 0.0179(8) Uani 1 1 d . . . C4 C 0.2370(5) 0.8799(5) 0.3317(4) 0.0225(9) Uani 1 1 d . . . C5 C 0.6353(5) 0.9210(4) 0.1791(4) 0.0181(8) Uani 1 1 d . . . C6 C 0.8165(5) 0.8579(4) 0.1195(4) 0.0195(8) Uani 1 1 d . . . C7 C 0.9445(5) 0.8837(5) 0.1462(4) 0.0255(9) Uani 1 1 d . . . H7 H 0.9197 0.9379 0.2054 0.031 Uiso 1 1 calc R . . C8 C 1.1098(5) 0.8278(5) 0.0836(4) 0.0267(9) Uani 1 1 d . . . H8 H 1.1957 0.8448 0.1023 0.032 Uiso 1 1 calc R . . C9 C 0.8612(6) 0.7719(5) 0.0341(4) 0.0318(11) Uani 1 1 d . . . H9 H 0.7789 0.7486 0.0168 0.038 Uiso 1 1 calc R . . C10 C 1.0283(6) 0.7211(5) -0.0249(4) 0.0319(11) Uani 1 1 d . . . H10 H 1.0566 0.6642 -0.0828 0.038 Uiso 1 1 calc R . . C11 C 0.5549(6) 0.2861(5) 0.4021(4) 0.0247(9) Uani 1 1 d . . . C12 C 0.5266(6) 0.1382(5) 0.4555(4) 0.0224(9) Uani 1 1 d . . . C13 C 0.6604(5) 0.0034(5) 0.4377(4) 0.0230(9) Uani 1 1 d . . . H13 H 0.7680 0.0060 0.3958 0.028 Uiso 1 1 calc R . . C14 C 0.6336(6) -0.1339(5) 0.4819(4) 0.0239(9) Uani 1 1 d . . . H14 H 0.7231 -0.2237 0.4697 0.029 Uiso 1 1 calc R . . Cl1 Cl 0.53771(15) 1.59197(12) 0.09295(10) 0.0292(2) Uani 1 1 d . . . N1 N 0.5505(4) 1.0715(4) 0.1751(3) 0.0183(7) Uani 1 1 d . . . N2 N 0.5371(4) 0.8357(4) 0.2347(3) 0.0182(7) Uani 1 1 d . . . N3 N 1.1513(4) 0.7500(4) -0.0028(3) 0.0241(8) Uani 1 1 d . . . O1 O 0.2991(4) 1.3445(3) 0.2186(3) 0.0310(7) Uani 1 1 d . . . O2 O 0.1027(4) 1.2347(3) 0.2935(3) 0.0348(8) Uani 1 1 d . . . O3 O 0.0847(4) 0.9778(4) 0.3535(3) 0.0352(8) Uani 1 1 d . . . O4 O 0.2649(4) 0.7414(3) 0.3603(3) 0.0308(7) Uani 1 1 d . . . O5 O 0.4758(4) 0.3927(3) 0.4587(3) 0.0298(7) Uani 1 1 d . . . O6 O 0.6554(4) 0.3036(4) 0.2993(3) 0.0332(8) Uani 1 1 d . . . O1W O 0.8421(4) 0.5090(4) 0.3061(4) 0.0470(10) Uani 1 1 d D . . O2W O 0.0556(8) 0.5816(7) 0.3765(6) 0.1053(19) Uani 1 1 d U . . H1A H 0.874(9) 0.414(2) 0.338(7) 0.10(3) Uiso 1 1 d D . . H1B H 0.900(7) 0.542(6) 0.330(6) 0.06(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01931(17) 0.01784(17) 0.02233(17) -0.00678(12) 0.00050(12) -0.00749(12) Cd2 0.02432(18) 0.01538(17) 0.02846(19) -0.00405(13) -0.00284(13) -0.00796(13) C1 0.021(2) 0.021(2) 0.028(2) -0.0043(18) -0.0060(18) -0.0044(17) C2 0.020(2) 0.019(2) 0.022(2) -0.0054(16) -0.0024(16) -0.0090(17) C3 0.0176(19) 0.017(2) 0.021(2) -0.0048(16) -0.0044(16) -0.0067(16) C4 0.017(2) 0.027(2) 0.027(2) -0.0104(18) -0.0018(17) -0.0089(17) C5 0.0139(18) 0.019(2) 0.021(2) -0.0077(16) -0.0020(16) -0.0032(16) C6 0.017(2) 0.017(2) 0.021(2) -0.0042(16) 0.0009(16) -0.0060(16) C7 0.024(2) 0.029(2) 0.026(2) -0.0131(19) -0.0019(18) -0.0088(18) C8 0.021(2) 0.034(3) 0.029(2) -0.012(2) -0.0044(18) -0.0093(19) C9 0.025(2) 0.040(3) 0.041(3) -0.022(2) -0.001(2) -0.016(2) C10 0.028(2) 0.040(3) 0.037(3) -0.027(2) 0.004(2) -0.013(2) C11 0.039(2) 0.021(2) 0.022(2) 0.0032(18) -0.0145(19) -0.0178(19) C12 0.036(2) 0.019(2) 0.017(2) -0.0038(16) -0.0057(18) -0.0143(18) C13 0.025(2) 0.025(2) 0.021(2) -0.0077(17) 0.0014(17) -0.0128(18) C14 0.033(2) 0.018(2) 0.022(2) -0.0075(17) -0.0038(18) -0.0091(18) Cl1 0.0416(6) 0.0188(5) 0.0330(6) -0.0059(4) -0.0180(5) -0.0085(4) N1 0.0157(16) 0.0165(17) 0.0213(17) -0.0068(14) 0.0008(13) -0.0054(13) N2 0.0172(16) 0.0175(17) 0.0198(17) -0.0061(14) -0.0021(14) -0.0057(14) N3 0.0160(17) 0.0255(19) 0.0278(19) -0.0099(16) 0.0017(14) -0.0057(14) O1 0.0232(16) 0.0169(15) 0.049(2) -0.0097(14) 0.0033(14) -0.0084(13) O2 0.0167(15) 0.0241(17) 0.058(2) -0.0134(15) 0.0003(15) -0.0032(13) O3 0.0172(15) 0.0271(17) 0.059(2) -0.0165(16) 0.0034(15) -0.0083(13) O4 0.0244(16) 0.0207(16) 0.046(2) -0.0063(14) -0.0011(14) -0.0113(13) O5 0.0430(19) 0.0169(15) 0.0338(18) -0.0065(13) -0.0092(15) -0.0127(14) O6 0.051(2) 0.0359(19) 0.0234(17) 0.0016(14) -0.0088(15) -0.0302(16) O1W 0.0269(18) 0.029(2) 0.089(3) -0.021(2) -0.0176(19) -0.0033(15) O2W 0.118(4) 0.096(3) 0.136(4) 0.013(3) -0.067(3) -0.071(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 Cd1 N3 2.281(4) 2_775 ? Cd1 N1 2.313(3) . ? Cd1 O1 2.313(3) . ? Cd1 O6 2.360(3) 1_565 ? Cd1 Cl1 2.6059(18) . ? Cd1 Cl1 2.6939(15) 2_685 ? Cd2 O1W 2.225(4) . ? Cd2 N2 2.283(3) . ? Cd2 O5 2.290(3) . ? Cd2 O4 2.386(3) . ? Cd2 O5 2.520(3) 2_666 ? Cd2 Cl1 2.7430(16) 1_545 ? C1 O1 1.246(5) . ? C1 O2 1.267(5) . ? C1 C2 1.480(6) . ? C2 N1 1.364(5) . ? C2 C3 1.386(6) . ? C3 N2 1.368(5) . ? C3 C4 1.467(6) . ? C4 O4 1.234(5) . ? C4 O3 1.294(5) . ? C5 N2 1.334(5) . ? C5 N1 1.355(5) . ? C5 C6 1.482(5) . ? C6 C7 1.380(6) . ? C6 C9 1.382(6) . ? C7 C8 1.380(6) . ? C7 H7 0.9300 . ? C8 N3 1.339(6) . ? C8 H8 0.9300 . ? C9 C10 1.372(6) . ? C9 H9 0.9300 . ? C10 N3 1.331(6) . ? C10 H10 0.9300 . ? C11 O5 1.266(5) . ? C11 O6 1.267(5) . ? C11 C12 1.485(6) . ? C12 C14 1.385(6) 2_656 ? C12 C13 1.393(6) . ? C13 C14 1.379(6) . ? C13 H13 0.9300 . ? C14 C12 1.385(6) 2_656 ? C14 H14 0.9300 . ? Cl1 Cd1 2.6939(15) 2_685 ? Cl1 Cd2 2.7430(16) 1_565 ? N3 Cd1 2.281(4) 2_775 ? O5 Cd2 2.520(3) 2_666 ? O6 Cd1 2.360(3) 1_545 ? O1W H1A 0.847(11) . ? O1W H1B 0.848(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N1 99.75(12) 2_775 . ? N3 Cd1 O1 170.26(12) 2_775 . ? N1 Cd1 O1 73.81(11) . . ? N3 Cd1 O6 96.91(13) 2_775 1_565 ? N1 Cd1 O6 100.29(11) . 1_565 ? O1 Cd1 O6 91.51(12) . 1_565 ? N3 Cd1 Cl1 94.69(9) 2_775 . ? N1 Cd1 Cl1 165.54(8) . . ? O1 Cd1 Cl1 91.97(8) . . ? O6 Cd1 Cl1 76.98(8) 1_565 . ? N3 Cd1 Cl1 87.19(10) 2_775 2_685 ? N1 Cd1 Cl1 96.51(9) . 2_685 ? O1 Cd1 Cl1 86.32(10) . 2_685 ? O6 Cd1 Cl1 161.74(8) 1_565 2_685 ? Cl1 Cd1 Cl1 84.98(3) . 2_685 ? O1W Cd2 N2 93.17(13) . . ? O1W Cd2 O5 106.45(14) . . ? N2 Cd2 O5 155.83(12) . . ? O1W Cd2 O4 160.51(12) . . ? N2 Cd2 O4 72.08(11) . . ? O5 Cd2 O4 85.43(11) . . ? O1W Cd2 O5 89.34(14) . 2_666 ? N2 Cd2 O5 95.35(11) . 2_666 ? O5 Cd2 O5 71.42(11) . 2_666 ? O4 Cd2 O5 79.73(11) . 2_666 ? O1W Cd2 Cl1 100.66(12) . 1_545 ? N2 Cd2 Cl1 82.46(9) . 1_545 ? O5 Cd2 Cl1 106.92(8) . 1_545 ? O4 Cd2 Cl1 90.18(9) . 1_545 ? O5 Cd2 Cl1 169.85(8) 2_666 1_545 ? O1 C1 O2 124.0(4) . . ? O1 C1 C2 118.7(4) . . ? O2 C1 C2 117.2(4) . . ? N1 C2 C3 108.2(3) . . ? N1 C2 C1 120.7(3) . . ? C3 C2 C1 131.1(4) . . ? N2 C3 C2 108.7(3) . . ? N2 C3 C4 119.0(4) . . ? C2 C3 C4 132.3(4) . . ? O4 C4 O3 121.7(4) . . ? O4 C4 C3 119.8(4) . . ? O3 C4 C3 118.4(4) . . ? N2 C5 N1 113.6(3) . . ? N2 C5 C6 122.9(3) . . ? N1 C5 C6 123.4(3) . . ? C7 C6 C9 118.2(4) . . ? C7 C6 C5 121.6(4) . . ? C9 C6 C5 120.2(4) . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N3 C8 C7 122.7(4) . . ? N3 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C10 C9 C6 119.4(4) . . ? C10 C9 H9 120.3 . . ? C6 C9 H9 120.3 . . ? N3 C10 C9 122.7(4) . . ? N3 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? O5 C11 O6 121.5(4) . . ? O5 C11 C12 119.5(4) . . ? O6 C11 C12 119.0(4) . . ? C14 C12 C13 119.8(4) 2_656 . ? C14 C12 C11 120.5(4) 2_656 . ? C13 C12 C11 119.6(4) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C12 120.0(4) . 2_656 ? C13 C14 H14 120.0 . . ? C12 C14 H14 120.0 2_656 . ? Cd1 Cl1 Cd1 95.02(3) . 2_685 ? Cd1 Cl1 Cd2 100.82(4) . 1_565 ? Cd1 Cl1 Cd2 158.64(5) 2_685 1_565 ? C5 N1 C2 104.8(3) . . ? C5 N1 Cd1 144.5(3) . . ? C2 N1 Cd1 110.7(2) . . ? C5 N2 C3 104.8(3) . . ? C5 N2 Cd2 140.3(3) . . ? C3 N2 Cd2 113.0(3) . . ? C10 N3 C8 118.0(4) . . ? C10 N3 Cd1 122.1(3) . 2_775 ? C8 N3 Cd1 119.6(3) . 2_775 ? C1 O1 Cd1 115.8(3) . . ? C4 O4 Cd2 114.3(3) . . ? C11 O5 Cd2 101.9(3) . . ? C11 O5 Cd2 134.2(3) . 2_666 ? Cd2 O5 Cd2 108.58(11) . 2_666 ? C11 O6 Cd1 119.3(3) . 1_545 ? Cd2 O1W H1A 106(5) . . ? Cd2 O1W H1B 129(4) . . ? H1A O1W H1B 105.5(18) . . ? 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 N1 -5.4(6) . . . . ? O2 C1 C2 N1 175.3(4) . . . . ? O1 C1 C2 C3 171.9(4) . . . . ? O2 C1 C2 C3 -7.5(7) . . . . ? N1 C2 C3 N2 0.0(4) . . . . ? C1 C2 C3 N2 -177.6(4) . . . . ? N1 C2 C3 C4 -179.9(4) . . . . ? C1 C2 C3 C4 2.6(8) . . . . ? N2 C3 C4 O4 4.1(6) . . . . ? C2 C3 C4 O4 -176.1(4) . . . . ? N2 C3 C4 O3 -174.2(4) . . . . ? C2 C3 C4 O3 5.6(7) . . . . ? N2 C5 C6 C7 -128.7(4) . . . . ? N1 C5 C6 C7 55.9(6) . . . . ? N2 C5 C6 C9 51.9(6) . . . . ? N1 C5 C6 C9 -123.5(5) . . . . ? C9 C6 C7 C8 2.3(6) . . . . ? C5 C6 C7 C8 -177.1(4) . . . . ? C6 C7 C8 N3 0.4(7) . . . . ? C7 C6 C9 C10 -2.9(7) . . . . ? C5 C6 C9 C10 176.6(4) . . . . ? C6 C9 C10 N3 0.6(8) . . . . ? O5 C11 C12 C14 35.9(6) . . . 2_656 ? O6 C11 C12 C14 -142.6(4) . . . 2_656 ? O5 C11 C12 C13 -147.0(4) . . . . ? O6 C11 C12 C13 34.5(6) . . . . ? C14 C12 C13 C14 0.1(7) 2_656 . . . ? C11 C12 C13 C14 -177.0(4) . . . . ? C12 C13 C14 C12 -0.1(7) . . . 2_656 ? N3 Cd1 Cl1 Cd1 86.76(10) 2_775 . . 2_685 ? N1 Cd1 Cl1 Cd1 -96.6(3) . . . 2_685 ? O1 Cd1 Cl1 Cd1 -86.13(10) . . . 2_685 ? O6 Cd1 Cl1 Cd1 -177.23(9) 1_565 . . 2_685 ? Cl1 Cd1 Cl1 Cd1 0.0 2_685 . . 2_685 ? N3 Cd1 Cl1 Cd2 -107.63(10) 2_775 . . 1_565 ? N1 Cd1 Cl1 Cd2 69.0(3) . . . 1_565 ? O1 Cd1 Cl1 Cd2 79.48(9) . . . 1_565 ? O6 Cd1 Cl1 Cd2 -11.61(9) 1_565 . . 1_565 ? Cl1 Cd1 Cl1 Cd2 165.61(6) 2_685 . . 1_565 ? N2 C5 N1 C2 -0.5(5) . . . . ? C6 C5 N1 C2 175.2(4) . . . . ? N2 C5 N1 Cd1 175.2(3) . . . . ? C6 C5 N1 Cd1 -9.0(7) . . . . ? C3 C2 N1 C5 0.3(4) . . . . ? C1 C2 N1 C5 178.2(4) . . . . ? C3 C2 N1 Cd1 -177.0(3) . . . . ? C1 C2 N1 Cd1 0.8(5) . . . . ? N3 Cd1 N1 C5 13.7(5) 2_775 . . . ? O1 Cd1 N1 C5 -173.8(5) . . . . ? O6 Cd1 N1 C5 -85.2(5) 1_565 . . . ? Cl1 Cd1 N1 C5 -162.9(3) . . . . ? Cl1 Cd1 N1 C5 101.9(5) 2_685 . . . ? N3 Cd1 N1 C2 -170.7(3) 2_775 . . . ? O1 Cd1 N1 C2 1.8(3) . . . . ? O6 Cd1 N1 C2 90.4(3) 1_565 . . . ? Cl1 Cd1 N1 C2 12.7(5) . . . . ? Cl1 Cd1 N1 C2 -82.4(3) 2_685 . . . ? N1 C5 N2 C3 0.5(5) . . . . ? C6 C5 N2 C3 -175.3(4) . . . . ? N1 C5 N2 Cd2 -161.7(3) . . . . ? C6 C5 N2 Cd2 22.4(6) . . . . ? C2 C3 N2 C5 -0.3(4) . . . . ? C4 C3 N2 C5 179.6(4) . . . . ? C2 C3 N2 Cd2 167.5(3) . . . . ? C4 C3 N2 Cd2 -12.6(4) . . . . ? O1W Cd2 N2 C5 5.4(4) . . . . ? O5 Cd2 N2 C5 150.1(4) . . . . ? O4 Cd2 N2 C5 172.4(4) . . . . ? O5 Cd2 N2 C5 95.1(4) 2_666 . . . ? Cl1 Cd2 N2 C5 -94.9(4) 1_545 . . . ? O1W Cd2 N2 C3 -155.9(3) . . . . ? O5 Cd2 N2 C3 -11.2(4) . . . . ? O4 Cd2 N2 C3 11.1(2) . . . . ? O5 Cd2 N2 C3 -66.3(3) 2_666 . . . ? Cl1 Cd2 N2 C3 103.7(3) 1_545 . . . ? C9 C10 N3 C8 2.1(7) . . . . ? C9 C10 N3 Cd1 -171.6(4) . . . 2_775 ? C7 C8 N3 C10 -2.7(7) . . . . ? C7 C8 N3 Cd1 171.3(3) . . . 2_775 ? O2 C1 O1 Cd1 -173.8(3) . . . . ? C2 C1 O1 Cd1 6.9(5) . . . . ? N3 Cd1 O1 C1 44.7(9) 2_775 . . . ? N1 Cd1 O1 C1 -4.8(3) . . . . ? O6 Cd1 O1 C1 -105.1(3) 1_565 . . . ? Cl1 Cd1 O1 C1 177.9(3) . . . . ? Cl1 Cd1 O1 C1 93.0(3) 2_685 . . . ? O3 C4 O4 Cd2 -175.2(3) . . . . ? C3 C4 O4 Cd2 6.6(5) . . . . ? O1W Cd2 O4 C4 32.7(6) . . . . ? N2 Cd2 O4 C4 -9.6(3) . . . . ? O5 Cd2 O4 C4 161.4(3) . . . . ? O5 Cd2 O4 C4 89.5(3) 2_666 . . . ? Cl1 Cd2 O4 C4 -91.6(3) 1_545 . . . ? O6 C11 O5 Cd2 2.3(5) . . . . ? C12 C11 O5 Cd2 -176.2(3) . . . . ? O6 C11 O5 Cd2 -129.0(4) . . . 2_666 ? C12 C11 O5 Cd2 52.5(6) . . . 2_666 ? O1W Cd2 O5 C11 -61.8(3) . . . . ? N2 Cd2 O5 C11 155.2(3) . . . . ? O4 Cd2 O5 C11 133.9(3) . . . . ? O5 Cd2 O5 C11 -145.4(3) 2_666 . . . ? Cl1 Cd2 O5 C11 45.1(3) 1_545 . . . ? O1W Cd2 O5 Cd2 83.57(16) . . . 2_666 ? N2 Cd2 O5 Cd2 -59.4(3) . . . 2_666 ? O4 Cd2 O5 Cd2 -80.68(13) . . . 2_666 ? O5 Cd2 O5 Cd2 0.0 2_666 . . 2_666 ? Cl1 Cd2 O5 Cd2 -169.48(8) 1_545 . . 2_666 ? O5 C11 O6 Cd1 -111.7(4) . . . 1_545 ? C12 C11 O6 Cd1 66.7(5) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.566 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.123 data_4 _database_code_depnum_ccdc_archive 'CCDC 837792' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H11 Cd2 N3 O8' _chemical_formula_sum 'C12 H11 Cd2 N3 O8' _chemical_formula_weight 550.04 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 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.562(6) _cell_length_b 6.941(2) _cell_length_c 16.190(1) _cell_angle_alpha 90 _cell_angle_beta 102.243(3) _cell_angle_gamma 90 _cell_volume 1489.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1250 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.475 _exptl_absorpt_correction_T_max 0.546 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 7183 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2618 _reflns_number_gt 2119 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. H atoms of coordination water molecule and lattice water molecule were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1A...H1B and the distance of H2A...H2B were restrained to 1.35+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.9638P] 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 2618 _refine_ls_number_parameters 243 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.935 _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 0.79417(2) 1.34721(5) -0.14056(2) 0.01870(11) Uani 1 1 d . . . Cd2 Cd 0.71563(2) 0.53954(5) 0.15073(2) 0.02581(12) Uani 1 1 d . . . C1 C 0.8839(3) 0.2956(7) 0.2659(3) 0.0222(11) Uani 1 1 d . . . C2 C 0.9396(3) 0.4232(6) 0.2178(3) 0.0168(10) Uani 1 1 d . . . C3 C 1.0394(3) 0.4462(6) 0.2119(3) 0.0162(10) Uani 1 1 d . . . C4 C 1.1343(3) 0.3580(6) 0.2587(3) 0.0203(10) Uani 1 1 d . . . C5 C 0.9479(3) 0.6445(6) 0.1249(3) 0.0176(10) Uani 1 1 d . . . C6 C 0.9131(3) 0.7940(6) 0.0614(3) 0.0199(10) Uani 1 1 d . . . C7 C 0.8546(4) 0.9448(7) 0.0806(3) 0.0342(13) Uani 1 1 d . . . H7 H 0.8383 0.9517 0.1336 0.041 Uiso 1 1 calc R . . C8 C 0.8212(4) 1.0831(8) 0.0213(4) 0.0350(14) Uani 1 1 d . . . H8 H 0.7834 1.1847 0.0357 0.042 Uiso 1 1 calc R . . C9 C 0.9324(3) 0.7888(7) -0.0187(3) 0.0227(11) Uani 1 1 d . . . H9 H 0.9712 0.6899 -0.0340 0.027 Uiso 1 1 calc R . . C10 C 0.8938(3) 0.9316(7) -0.0764(3) 0.0249(11) Uani 1 1 d . . . H10 H 0.9057 0.9240 -0.1308 0.030 Uiso 1 1 calc R . . C11 C 0.6719(4) 0.6200(7) -0.0380(3) 0.0238(11) Uani 1 1 d . . . C12 C 0.6180(4) 0.7093(8) -0.1197(3) 0.0342(13) Uani 1 1 d . . . H12A H 0.6642 0.7238 -0.1568 0.051 Uiso 1 1 calc R . . H12B H 0.5923 0.8333 -0.1087 0.051 Uiso 1 1 calc R . . H12C H 0.5631 0.6277 -0.1460 0.051 Uiso 1 1 calc R . . H1A H 0.617(5) 0.206(10) 0.070(2) 0.10(3) Uiso 1 1 d D . . H2A H 0.510(3) 0.785(12) 0.029(5) 0.13(4) Uiso 1 1 d D . . H1B H 0.657(7) 0.145(7) 0.151(4) 0.14(4) Uiso 1 1 d D . . H2B H 0.448(5) 0.774(11) 0.085(3) 0.10(3) Uiso 1 1 d D . . N1 N 0.8829(3) 0.5523(5) 0.1643(2) 0.0204(9) Uani 1 1 d . . . N2 N 1.0442(3) 0.5859(5) 0.1533(2) 0.0176(8) Uani 1 1 d . . . N3 N 0.8401(3) 1.0798(6) -0.0568(3) 0.0243(9) Uani 1 1 d . . . O1 O 0.7986(2) 0.3566(5) 0.2753(2) 0.0332(9) Uani 1 1 d . . . O2 O 0.9174(2) 0.1347(5) 0.2916(2) 0.0298(8) Uani 1 1 d . . . O3 O 1.1309(2) 0.2352(5) 0.3148(2) 0.0260(8) Uani 1 1 d . . . O4 O 1.2161(2) 0.4089(5) 0.2398(2) 0.0240(8) Uani 1 1 d . . . O5 O 0.6409(3) 0.6671(5) 0.0281(2) 0.0376(9) Uani 1 1 d . . . O6 O 0.7435(2) 0.5037(5) -0.0353(2) 0.0263(8) Uani 1 1 d . . . O1W O 0.6526(3) 0.2406(6) 0.1177(3) 0.0446(10) Uani 1 1 d D . . O2W O 0.4535(3) 0.8226(7) 0.0377(3) 0.0510(11) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01413(18) 0.02086(19) 0.0207(2) 0.00429(15) 0.00275(13) -0.00163(14) Cd2 0.0179(2) 0.0345(2) 0.0251(2) -0.00221(17) 0.00463(15) 0.00614(16) C1 0.021(3) 0.031(3) 0.013(3) -0.002(2) 0.001(2) -0.004(2) C2 0.017(2) 0.021(2) 0.013(2) 0.0012(19) 0.0038(18) 0.0006(19) C3 0.021(2) 0.013(2) 0.015(2) 0.0006(19) 0.0055(19) 0.0001(19) C4 0.019(2) 0.016(2) 0.025(3) 0.001(2) 0.003(2) 0.0003(19) C5 0.018(2) 0.017(2) 0.019(3) 0.001(2) 0.0070(19) 0.0020(19) C6 0.017(2) 0.020(3) 0.022(3) 0.001(2) 0.004(2) -0.0011(19) C7 0.042(3) 0.035(3) 0.030(3) 0.010(3) 0.018(3) 0.012(3) C8 0.035(3) 0.035(3) 0.038(3) 0.012(3) 0.017(3) 0.016(2) C9 0.024(2) 0.018(3) 0.025(3) -0.003(2) 0.004(2) -0.001(2) C10 0.030(3) 0.025(3) 0.019(3) 0.000(2) 0.004(2) -0.004(2) C11 0.026(3) 0.020(3) 0.027(3) -0.001(2) 0.008(2) -0.003(2) C12 0.037(3) 0.036(3) 0.029(3) 0.007(2) 0.004(2) 0.013(2) N1 0.019(2) 0.022(2) 0.020(2) 0.0049(18) 0.0025(17) 0.0050(17) N2 0.0122(19) 0.023(2) 0.018(2) 0.0039(17) 0.0043(16) 0.0001(16) N3 0.023(2) 0.026(2) 0.024(2) 0.0108(19) 0.0043(18) 0.0006(18) O1 0.0183(18) 0.045(2) 0.040(2) 0.0151(19) 0.0138(16) 0.0063(16) O2 0.0279(19) 0.0253(19) 0.037(2) 0.0138(17) 0.0092(16) 0.0023(15) O3 0.0173(16) 0.0289(19) 0.031(2) 0.0131(17) 0.0039(14) 0.0029(14) O4 0.0139(16) 0.0274(19) 0.031(2) 0.0089(15) 0.0054(15) 0.0008(14) O5 0.038(2) 0.053(2) 0.022(2) 0.0039(18) 0.0056(17) 0.0143(18) O6 0.0244(18) 0.0271(19) 0.026(2) -0.0020(16) 0.0025(15) 0.0052(15) O1W 0.051(3) 0.040(2) 0.041(3) -0.001(2) 0.004(2) -0.002(2) O2W 0.042(3) 0.071(3) 0.041(3) 0.007(2) 0.011(2) 0.009(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 2.248(3) 1_565 ? Cd1 O3 2.253(3) 4_575 ? Cd1 N2 2.292(4) 3_775 ? Cd1 N3 2.305(4) . ? Cd1 O4 2.318(3) 3_775 ? Cd2 O5 2.214(4) . ? Cd2 N1 2.235(4) . ? Cd2 O1W 2.265(4) . ? Cd2 O2 2.297(3) 2_655 ? Cd2 O1 2.446(3) . ? Cd2 O1 2.533(4) 2_655 ? Cd2 C1 2.752(5) 2_655 ? C1 O2 1.243(5) . ? C1 O1 1.270(5) . ? C1 C2 1.489(6) . ? C1 Cd2 2.752(5) 2_645 ? C2 N1 1.364(5) . ? C2 C3 1.385(6) . ? C3 N2 1.367(6) . ? C3 C4 1.481(6) . ? C4 O3 1.253(6) . ? C4 O4 1.262(5) . ? C5 N2 1.353(5) . ? C5 N1 1.353(6) . ? C5 C6 1.467(6) . ? C6 C9 1.376(7) . ? C6 C7 1.388(7) . ? C7 C8 1.366(7) . ? C7 H7 0.9300 . ? C8 N3 1.342(7) . ? C8 H8 0.9300 . ? C9 C10 1.386(6) . ? C9 H9 0.9300 . ? C10 N3 1.338(6) . ? C10 H10 0.9300 . ? C11 O6 1.256(5) . ? C11 O5 1.271(6) . ? C11 C12 1.504(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 Cd1 2.292(4) 3_775 ? O1 Cd2 2.533(4) 2_645 ? O2 Cd2 2.297(3) 2_645 ? O3 Cd1 2.253(3) 4_676 ? O4 Cd1 2.318(3) 3_775 ? O6 Cd1 2.248(3) 1_545 ? O1W H1A 0.848(10) . ? O1W H1B 0.846(10) . ? O2W H2A 0.848(10) . ? O2W H2B 0.847(10) . ? 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 O6 Cd1 O3 85.88(12) 1_565 4_575 ? O6 Cd1 N2 115.00(12) 1_565 3_775 ? O3 Cd1 N2 156.36(13) 4_575 3_775 ? O6 Cd1 N3 91.78(14) 1_565 . ? O3 Cd1 N3 96.24(13) 4_575 . ? N2 Cd1 N3 94.15(13) 3_775 . ? O6 Cd1 O4 100.91(12) 1_565 3_775 ? O3 Cd1 O4 92.99(12) 4_575 3_775 ? N2 Cd1 O4 73.01(12) 3_775 3_775 ? N3 Cd1 O4 164.81(13) . 3_775 ? O5 Cd2 N1 109.52(14) . . ? O5 Cd2 O1W 94.41(16) . . ? N1 Cd2 O1W 112.59(15) . . ? O5 Cd2 O2 90.00(13) . 2_655 ? N1 Cd2 O2 144.82(13) . 2_655 ? O1W Cd2 O2 93.99(14) . 2_655 ? O5 Cd2 O1 171.99(13) . . ? N1 Cd2 O1 70.09(12) . . ? O1W Cd2 O1 78.67(15) . . ? O2 Cd2 O1 94.48(12) 2_655 . ? O5 Cd2 O1 90.59(13) . 2_655 ? N1 Cd2 O1 95.57(12) . 2_655 ? O1W Cd2 O1 147.66(14) . 2_655 ? O2 Cd2 O1 54.02(11) 2_655 2_655 ? O1 Cd2 O1 97.42(6) . 2_655 ? O5 Cd2 C1 90.16(14) . 2_655 ? N1 Cd2 C1 121.31(14) . 2_655 ? O1W Cd2 C1 120.50(16) . 2_655 ? O2 Cd2 C1 26.61(12) 2_655 2_655 ? O1 Cd2 C1 96.81(13) . 2_655 ? O1 Cd2 C1 27.41(12) 2_655 2_655 ? O2 C1 O1 122.5(4) . . ? O2 C1 C2 121.3(4) . . ? O1 C1 C2 116.1(4) . . ? O2 C1 Cd2 55.8(2) . 2_645 ? O1 C1 Cd2 66.6(3) . 2_645 ? C2 C1 Cd2 176.3(3) . 2_645 ? N1 C2 C3 108.0(4) . . ? N1 C2 C1 116.3(4) . . ? C3 C2 C1 135.8(4) . . ? N2 C3 C2 108.7(4) . . ? N2 C3 C4 118.9(4) . . ? C2 C3 C4 132.3(4) . . ? O3 C4 O4 122.4(4) . . ? O3 C4 C3 119.4(4) . . ? O4 C4 C3 118.3(4) . . ? N2 C5 N1 112.1(4) . . ? N2 C5 C6 126.5(4) . . ? N1 C5 C6 121.3(4) . . ? C9 C6 C7 117.6(4) . . ? C9 C6 C5 123.0(4) . . ? C7 C6 C5 119.3(4) . . ? C8 C7 C6 119.5(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? N3 C8 C7 123.3(5) . . ? N3 C8 H8 118.3 . . ? C7 C8 H8 118.3 . . ? C6 C9 C10 119.7(4) . . ? C6 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N3 C10 C9 122.4(5) . . ? N3 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? O6 C11 O5 121.8(5) . . ? O6 C11 C12 121.5(5) . . ? O5 C11 C12 116.7(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N1 C2 105.9(4) . . ? C5 N1 Cd2 136.2(3) . . ? C2 N1 Cd2 117.4(3) . . ? C5 N2 C3 105.3(4) . . ? C5 N2 Cd1 141.4(3) . 3_775 ? C3 N2 Cd1 113.2(3) . 3_775 ? C10 N3 C8 117.4(4) . . ? C10 N3 Cd1 124.9(3) . . ? C8 N3 Cd1 117.3(3) . . ? C1 O1 Cd2 110.2(3) . . ? C1 O1 Cd2 85.9(3) . 2_645 ? Cd2 O1 Cd2 140.63(15) . 2_645 ? C1 O2 Cd2 97.5(3) . 2_645 ? C4 O3 Cd1 102.7(3) . 4_676 ? C4 O4 Cd1 116.5(3) . 3_775 ? C11 O5 Cd2 118.8(3) . . ? C11 O6 Cd1 130.0(3) . 1_545 ? Cd2 O1W H1A 126(5) . . ? Cd2 O1W H1B 127(5) . . ? H1A O1W H1B 108(3) . . ? H2A O2W H2B 106(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 154.1(4) . . . . ? O1 C1 C2 N1 -22.6(6) . . . . ? Cd2 C1 C2 N1 115(5) 2_645 . . . ? O2 C1 C2 C3 -25.2(8) . . . . ? O1 C1 C2 C3 158.1(5) . . . . ? Cd2 C1 C2 C3 -64(5) 2_645 . . . ? N1 C2 C3 N2 -1.5(5) . . . . ? C1 C2 C3 N2 177.8(5) . . . . ? N1 C2 C3 C4 174.8(5) . . . . ? C1 C2 C3 C4 -5.9(9) . . . . ? N2 C3 C4 O3 177.2(4) . . . . ? C2 C3 C4 O3 1.3(8) . . . . ? N2 C3 C4 O4 -3.3(7) . . . . ? C2 C3 C4 O4 -179.3(5) . . . . ? N2 C5 C6 C9 56.2(7) . . . . ? N1 C5 C6 C9 -126.0(5) . . . . ? N2 C5 C6 C7 -126.4(5) . . . . ? N1 C5 C6 C7 51.5(6) . . . . ? C9 C6 C7 C8 -1.7(7) . . . . ? C5 C6 C7 C8 -179.3(5) . . . . ? C6 C7 C8 N3 1.4(9) . . . . ? C7 C6 C9 C10 0.1(7) . . . . ? C5 C6 C9 C10 177.6(4) . . . . ? C6 C9 C10 N3 2.0(7) . . . . ? N2 C5 N1 C2 -2.6(5) . . . . ? C6 C5 N1 C2 179.3(4) . . . . ? N2 C5 N1 Cd2 -173.8(3) . . . . ? C6 C5 N1 Cd2 8.1(7) . . . . ? C3 C2 N1 C5 2.4(5) . . . . ? C1 C2 N1 C5 -177.1(4) . . . . ? C3 C2 N1 Cd2 175.5(3) . . . . ? C1 C2 N1 Cd2 -3.9(5) . . . . ? O5 Cd2 N1 C5 14.0(5) . . . . ? O1W Cd2 N1 C5 117.6(4) . . . . ? O2 Cd2 N1 C5 -106.2(5) 2_655 . . . ? O1 Cd2 N1 C5 -174.5(5) . . . . ? O1 Cd2 N1 C5 -78.6(5) 2_655 . . . ? C1 Cd2 N1 C5 -88.7(5) 2_655 . . . ? O5 Cd2 N1 C2 -156.5(3) . . . . ? O1W Cd2 N1 C2 -52.9(4) . . . . ? O2 Cd2 N1 C2 83.3(4) 2_655 . . . ? O1 Cd2 N1 C2 15.0(3) . . . . ? O1 Cd2 N1 C2 110.9(3) 2_655 . . . ? C1 Cd2 N1 C2 100.8(3) 2_655 . . . ? N1 C5 N2 C3 1.7(5) . . . . ? C6 C5 N2 C3 179.6(4) . . . . ? N1 C5 N2 Cd1 -174.2(3) . . . 3_775 ? C6 C5 N2 Cd1 3.8(8) . . . 3_775 ? C2 C3 N2 C5 -0.1(5) . . . . ? C4 C3 N2 C5 -176.9(4) . . . . ? C2 C3 N2 Cd1 177.1(3) . . . 3_775 ? C4 C3 N2 Cd1 0.3(5) . . . 3_775 ? C9 C10 N3 C8 -2.3(7) . . . . ? C9 C10 N3 Cd1 169.9(3) . . . . ? C7 C8 N3 C10 0.5(8) . . . . ? C7 C8 N3 Cd1 -172.2(4) . . . . ? O6 Cd1 N3 C10 -168.7(4) 1_565 . . . ? O3 Cd1 N3 C10 105.2(4) 4_575 . . . ? N2 Cd1 N3 C10 -53.5(4) 3_775 . . . ? O4 Cd1 N3 C10 -21.9(7) 3_775 . . . ? O6 Cd1 N3 C8 3.5(4) 1_565 . . . ? O3 Cd1 N3 C8 -82.6(4) 4_575 . . . ? N2 Cd1 N3 C8 118.7(4) 3_775 . . . ? O4 Cd1 N3 C8 150.3(5) 3_775 . . . ? O2 C1 O1 Cd2 -142.5(4) . . . . ? C2 C1 O1 Cd2 34.1(5) . . . . ? Cd2 C1 O1 Cd2 -143.1(2) 2_645 . . . ? O2 C1 O1 Cd2 0.6(4) . . . 2_645 ? C2 C1 O1 Cd2 177.3(4) . . . 2_645 ? O5 Cd2 O1 C1 62.0(10) . . . . ? N1 Cd2 O1 C1 -26.7(3) . . . . ? O1W Cd2 O1 C1 92.6(3) . . . . ? O2 Cd2 O1 C1 -174.2(3) 2_655 . . . ? O1 Cd2 O1 C1 -120.0(3) 2_655 . . . ? C1 Cd2 O1 C1 -147.6(3) 2_655 . . . ? O5 Cd2 O1 Cd2 -47.3(10) . . . 2_645 ? N1 Cd2 O1 Cd2 -136.0(3) . . . 2_645 ? O1W Cd2 O1 Cd2 -16.7(2) . . . 2_645 ? O2 Cd2 O1 Cd2 76.5(2) 2_655 . . 2_645 ? O1 Cd2 O1 Cd2 130.7(3) 2_655 . . 2_645 ? C1 Cd2 O1 Cd2 103.1(2) 2_655 . . 2_645 ? O1 C1 O2 Cd2 -0.7(5) . . . 2_645 ? C2 C1 O2 Cd2 -177.2(4) . . . 2_645 ? O4 C4 O3 Cd1 -0.6(5) . . . 4_676 ? C3 C4 O3 Cd1 178.8(3) . . . 4_676 ? O3 C4 O4 Cd1 -176.0(4) . . . 3_775 ? C3 C4 O4 Cd1 4.6(5) . . . 3_775 ? O6 C11 O5 Cd2 -0.1(6) . . . . ? C12 C11 O5 Cd2 179.5(3) . . . . ? N1 Cd2 O5 C11 45.7(4) . . . . ? O1W Cd2 O5 C11 -70.2(4) . . . . ? O2 Cd2 O5 C11 -164.2(4) 2_655 . . . ? O1 Cd2 O5 C11 -40.1(11) . . . . ? O1 Cd2 O5 C11 141.8(4) 2_655 . . . ? C1 Cd2 O5 C11 169.2(4) 2_655 . . . ? O5 C11 O6 Cd1 166.0(3) . . . 1_545 ? C12 C11 O6 Cd1 -13.6(7) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.442 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.129 data_5 _database_code_depnum_ccdc_archive 'CCDC 837793' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 N3 O10 Zn2' _chemical_formula_sum 'C12 H8 N3 O10 Zn2' _chemical_formula_weight 484.95 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.259(8) _cell_length_b 10.892(1) _cell_length_c 16.450(9) _cell_angle_alpha 90 _cell_angle_beta 98.025(8) _cell_angle_gamma 90 _cell_volume 1465.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 3.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_T_max 0.360 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3608 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1287 _reflns_number_gt 1103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms of coordination water molecule were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1A...H1B was restrained to 1.35+-0.02 \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+13.8947P] 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 1287 _refine_ls_number_parameters 124 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.984 _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 0.51797(8) 0.37921(6) 0.05836(4) 0.0267(3) Uani 1 1 d . . . C1 C 0.5047(8) 0.6083(5) 0.1433(4) 0.0295(14) Uani 1 1 d . . . C2 C 0.5094(7) 0.5113(5) 0.2081(3) 0.0211(12) Uani 1 1 d . . . C3 C 0.5000 0.3235(7) 0.2500 0.0227(16) Uani 1 2 d S . . C4 C 0.5000 0.1887(7) 0.2500 0.0186(15) Uani 1 2 d S . . C5 C 0.5861(7) 0.1219(5) 0.1972(4) 0.0275(13) Uani 1 1 d U . . H7 H 0.6457 0.1631 0.1618 0.033 Uiso 1 1 calc R . . C6 C 0.5829(8) -0.0037(6) 0.1976(4) 0.0343(15) Uani 1 1 d U . . H8 H 0.6383 -0.0473 0.1614 0.041 Uiso 1 1 calc R . . C7 C 0.3095(7) 0.1939(5) -0.0033(3) 0.0254(12) Uani 1 1 d . . . N1 N 0.5194(6) 0.3919(4) 0.1845(3) 0.0199(10) Uani 1 1 d . . . N2 N 0.5000 -0.0648(7) 0.2500 0.0370(18) Uani 1 2 d S . . O1 O 0.5181(5) 0.5676(4) 0.0730(2) 0.0302(10) Uani 1 1 d . . . O2 O 0.4884(8) 0.7174(4) 0.1597(3) 0.0577(16) Uani 1 1 d . . . O3 O 0.4543(5) 0.2057(4) 0.0261(2) 0.0274(9) Uani 1 1 d . . . O4 O 0.2461(5) 0.1005(4) -0.0389(3) 0.0312(10) Uani 1 1 d . . . O1W O 0.7662(5) 0.3734(4) 0.0567(3) 0.0429(12) Uani 1 1 d . . . H1A H 0.8380 0.3252 0.0735 0.064 Uiso 1 1 d R . . H1B H 0.8047 0.4307 0.0330 0.064 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0420(5) 0.0201(4) 0.0184(4) -0.0021(3) 0.0056(3) 0.0030(3) C1 0.051(4) 0.014(3) 0.026(3) 0.001(2) 0.012(3) 0.000(2) C2 0.034(3) 0.019(3) 0.009(2) -0.002(2) -0.001(2) 0.001(2) C3 0.036(4) 0.011(4) 0.022(4) 0.000 0.009(3) 0.000 C4 0.022(4) 0.015(4) 0.019(4) 0.000 0.001(3) 0.000 C5 0.037(3) 0.025(3) 0.021(3) 0.002(2) 0.007(2) 0.002(2) C6 0.051(4) 0.026(3) 0.025(3) -0.006(2) 0.005(3) 0.005(3) C7 0.036(3) 0.021(3) 0.021(3) 0.005(2) 0.012(2) 0.002(3) N1 0.032(2) 0.015(2) 0.012(2) -0.0004(17) 0.0005(18) -0.0028(18) N2 0.046(5) 0.022(4) 0.045(5) 0.000 0.012(4) 0.000 O1 0.059(3) 0.020(2) 0.0127(19) 0.0017(15) 0.0089(18) 0.0027(19) O2 0.131(5) 0.016(2) 0.033(3) 0.0003(19) 0.031(3) 0.006(3) O3 0.032(2) 0.025(2) 0.024(2) -0.0011(16) 0.0001(17) 0.0021(17) O4 0.039(2) 0.025(2) 0.029(2) -0.0074(17) 0.0007(18) 0.0042(18) O1W 0.036(3) 0.054(3) 0.040(3) 0.009(2) 0.010(2) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.013(4) . ? Zn1 O1W 2.055(4) . ? Zn1 O1 2.066(4) . ? Zn1 N1 2.078(4) . ? Zn1 O4 2.171(4) 7 ? Zn1 O1 2.216(4) 5_665 ? C1 O2 1.231(7) . ? C1 O1 1.258(7) . ? C1 C2 1.498(8) . ? C2 N1 1.363(7) . ? C2 C2 1.407(10) 2_655 ? C3 N1 1.338(6) 2_655 ? C3 N1 1.338(6) . ? C3 C4 1.468(10) . ? C4 C5 1.400(7) . ? C4 C5 1.400(7) 2_655 ? C5 C6 1.369(8) . ? C5 H7 0.9300 . ? C6 N2 1.348(7) . ? C6 H8 0.9300 . ? C7 O3 1.232(7) . ? C7 O4 1.251(7) . ? C7 C7 1.582(11) 7 ? N2 C6 1.348(7) 2_655 ? O1 Zn1 2.216(4) 5_665 ? O4 Zn1 2.171(4) 7 ? O1W H1A 0.8119 . ? O1W H1B 0.8224 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1W 101.07(17) . . ? O3 Zn1 O1 163.54(16) . . ? O1W Zn1 O1 92.75(18) . . ? O3 Zn1 N1 106.87(16) . . ? O1W Zn1 N1 98.58(18) . . ? O1 Zn1 N1 79.52(15) . . ? O3 Zn1 O4 80.59(15) . 7 ? O1W Zn1 O4 169.95(17) . 7 ? O1 Zn1 O4 84.27(16) . 7 ? N1 Zn1 O4 90.34(17) . 7 ? O3 Zn1 O1 89.66(15) . 5_665 ? O1W Zn1 O1 89.61(17) . 5_665 ? O1 Zn1 O1 81.46(16) . 5_665 ? N1 Zn1 O1 159.60(16) . 5_665 ? O4 Zn1 O1 80.46(16) 7 5_665 ? O2 C1 O1 124.7(6) . . ? O2 C1 C2 121.2(5) . . ? O1 C1 C2 114.2(5) . . ? N1 C2 C2 107.4(3) . 2_655 ? N1 C2 C1 117.8(5) . . ? C2 C2 C1 134.5(3) 2_655 . ? N1 C3 N1 112.4(6) 2_655 . ? N1 C3 C4 123.8(3) 2_655 . ? N1 C3 C4 123.8(3) . . ? C5 C4 C5 117.4(7) . 2_655 ? C5 C4 C3 121.3(4) . . ? C5 C4 C3 121.3(4) 2_655 . ? C6 C5 C4 120.3(6) . . ? C6 C5 H7 119.8 . . ? C4 C5 H7 119.8 . . ? N2 C6 C5 120.5(6) . . ? N2 C6 H8 119.7 . . ? C5 C6 H8 119.7 . . ? O3 C7 O4 126.0(5) . . ? O3 C7 C7 118.1(6) . 7 ? O4 C7 C7 115.9(6) . 7 ? C3 N1 C2 106.4(4) . . ? C3 N1 Zn1 141.5(4) . . ? C2 N1 Zn1 110.9(3) . . ? C6 N2 C6 120.9(8) 2_655 . ? C1 O1 Zn1 117.3(3) . . ? C1 O1 Zn1 141.9(4) . 5_665 ? Zn1 O1 Zn1 98.54(16) . 5_665 ? C7 O3 Zn1 113.9(3) . . ? C7 O4 Zn1 109.4(4) . 7 ? Zn1 O1W H1A 134.3 . . ? Zn1 O1W H1B 115.8 . . ? H1A O1W H1B 109.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 176.7(6) . . . . ? O1 C1 C2 N1 -3.0(8) . . . . ? O2 C1 C2 C2 3.9(13) . . . 2_655 ? O1 C1 C2 C2 -175.8(8) . . . 2_655 ? N1 C3 C4 C5 -152.2(4) 2_655 . . . ? N1 C3 C4 C5 27.8(4) . . . . ? N1 C3 C4 C5 27.8(4) 2_655 . . 2_655 ? N1 C3 C4 C5 -152.2(4) . . . 2_655 ? C5 C4 C5 C6 0.7(4) 2_655 . . . ? C3 C4 C5 C6 -179.3(4) . . . . ? C4 C5 C6 N2 -1.5(9) . . . . ? N1 C3 N1 C2 -1.0(3) 2_655 . . . ? C4 C3 N1 C2 179.0(3) . . . . ? N1 C3 N1 Zn1 -166.3(6) 2_655 . . . ? C4 C3 N1 Zn1 13.7(6) . . . . ? C2 C2 N1 C3 2.6(7) 2_655 . . . ? C1 C2 N1 C3 -172.0(4) . . . . ? C2 C2 N1 Zn1 172.8(5) 2_655 . . . ? C1 C2 N1 Zn1 -1.8(6) . . . . ? O3 Zn1 N1 C3 4.2(5) . . . . ? O1W Zn1 N1 C3 -100.2(5) . . . . ? O1 Zn1 N1 C3 168.6(5) . . . . ? O4 Zn1 N1 C3 84.5(5) 7 . . . ? O1 Zn1 N1 C3 147.1(4) 5_665 . . . ? O3 Zn1 N1 C2 -160.6(4) . . . . ? O1W Zn1 N1 C2 95.0(4) . . . . ? O1 Zn1 N1 C2 3.8(4) . . . . ? O4 Zn1 N1 C2 -80.4(4) 7 . . . ? O1 Zn1 N1 C2 -17.7(7) 5_665 . . . ? C5 C6 N2 C6 0.8(5) . . . 2_655 ? O2 C1 O1 Zn1 -173.3(6) . . . . ? C2 C1 O1 Zn1 6.5(7) . . . . ? O2 C1 O1 Zn1 -15.0(12) . . . 5_665 ? C2 C1 O1 Zn1 164.7(4) . . . 5_665 ? O3 Zn1 O1 C1 108.6(6) . . . . ? O1W Zn1 O1 C1 -104.2(5) . . . . ? N1 Zn1 O1 C1 -5.9(5) . . . . ? O4 Zn1 O1 C1 85.5(5) 7 . . . ? O1 Zn1 O1 C1 166.6(5) 5_665 . . . ? O3 Zn1 O1 Zn1 -58.0(6) . . . 5_665 ? O1W Zn1 O1 Zn1 89.19(18) . . . 5_665 ? N1 Zn1 O1 Zn1 -172.58(19) . . . 5_665 ? O4 Zn1 O1 Zn1 -81.18(17) 7 . . 5_665 ? O1 Zn1 O1 Zn1 0.0 5_665 . . 5_665 ? O4 C7 O3 Zn1 168.6(5) . . . . ? C7 C7 O3 Zn1 -10.8(7) 7 . . . ? O1W Zn1 O3 C7 -157.5(4) . . . . ? O1 Zn1 O3 C7 -10.9(7) . . . . ? N1 Zn1 O3 C7 99.9(4) . . . . ? O4 Zn1 O3 C7 12.4(4) 7 . . . ? O1 Zn1 O3 C7 -67.9(4) 5_665 . . . ? O3 C7 O4 Zn1 170.2(4) . . . 7 ? C7 C7 O4 Zn1 -10.4(7) 7 . . 7 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.657 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.119 data_6 _database_code_depnum_ccdc_archive 'CCDC 837794' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H7 Eu N3 O7, 2(H2O)' _chemical_formula_sum 'C11 H11 Eu N3 O9' _chemical_formula_weight 481.14 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.301(6) _cell_length_b 14.878(5) _cell_length_c 11.575(4) _cell_angle_alpha 90 _cell_angle_beta 90.854(9) _cell_angle_gamma 90 _cell_volume 1429.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 4.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.150 _exptl_absorpt_correction_T_max 0.235 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8609 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3371 _reflns_number_gt 2640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atom of imidazole ring were located in difference Fourier maps and refined isotropically with distance restraints of N---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(N). ; _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^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3371 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.004 _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 Eu1 Eu 0.78023(3) 1.132097(14) 0.932320(19) 0.01507(8) Uani 1 1 d . . . C1 C 0.9642(6) 0.9359(3) 0.8540(4) 0.0215(11) Uani 1 1 d . . . C2 C 0.9925(6) 0.8746(3) 0.7542(4) 0.0190(10) Uani 1 1 d . . . C3 C 1.0701(6) 0.7942(3) 0.7393(4) 0.0173(10) Uani 1 1 d . . . C4 C 1.1784(6) 0.7391(3) 0.8157(4) 0.0173(10) Uani 1 1 d . . . C5 C 0.9363(6) 0.8208(3) 0.5814(4) 0.0234(11) Uani 1 1 d . . . C6 C 0.8492(6) 0.8119(3) 0.4697(4) 0.0245(11) Uani 1 1 d . . . C7 C 0.8533(7) 0.8783(4) 0.3856(5) 0.0333(13) Uani 1 1 d . . . H7 H 0.9156 0.9297 0.3964 0.040 Uiso 1 1 calc R . . C8 C 0.7639(8) 0.8667(4) 0.2866(5) 0.0383(14) Uani 1 1 d . . . H8 H 0.7691 0.9110 0.2301 0.046 Uiso 1 1 calc R . . C9 C 0.7552(6) 0.7372(4) 0.4478(5) 0.0313(13) Uani 1 1 d . . . H9 H 0.7512 0.6903 0.5008 0.038 Uiso 1 1 calc R . . C10 C 0.6678(7) 0.7334(4) 0.3463(5) 0.0383(14) Uani 1 1 d . . . H10 H 0.6029 0.6833 0.3334 0.046 Uiso 1 1 calc R . . C11 C 0.4733(6) 0.9972(3) 0.9363(4) 0.0245(11) Uani 1 1 d . . . H1 H 0.848(8) 0.941(4) 0.639(5) 0.05(2) Uiso 1 1 d . . . N1 N 0.9124(5) 0.8910(3) 0.6520(3) 0.0230(9) Uani 1 1 d . . . N2 N 1.0338(5) 0.7604(3) 0.6305(3) 0.0196(9) Uani 1 1 d . . . N3 N 0.6699(6) 0.7960(4) 0.2662(4) 0.0376(12) Uani 1 1 d . . . O1 O 0.8913(5) 1.0076(2) 0.8298(3) 0.0388(11) Uani 1 1 d . . . O2 O 1.0039(4) 0.9108(2) 0.9524(3) 0.0260(8) Uani 1 1 d . . . O3 O 1.2171(4) 0.7638(2) 0.9135(3) 0.0231(8) Uani 1 1 d . . . O4 O 1.2244(4) 0.6667(2) 0.7703(3) 0.0222(8) Uani 1 1 d . . . O5 O 0.5511(5) 1.0430(3) 0.8660(3) 0.0368(10) Uani 1 1 d . . . O6 O 0.3546(5) 0.9480(2) 0.9123(3) 0.0309(9) Uani 1 1 d . . . O1W O 0.5593(4) 1.2353(2) 0.9013(3) 0.0325(9) Uani 1 1 d . . . O2W O 0.3058(5) 0.5281(3) 0.9154(3) 0.0401(10) Uani 1 1 d . . . O3W O 0.5793(6) 0.4253(3) 0.8537(4) 0.0536(13) 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 Eu1 0.02194(13) 0.01292(12) 0.01028(12) 0.00054(10) -0.00176(8) -0.00196(10) C1 0.028(3) 0.019(2) 0.017(2) -0.0074(19) -0.007(2) 0.004(2) C2 0.026(3) 0.015(2) 0.016(2) 0.0010(19) -0.0052(19) 0.001(2) C3 0.021(3) 0.021(2) 0.010(2) -0.0017(18) -0.0040(18) -0.0020(19) C4 0.018(2) 0.017(2) 0.016(2) -0.0025(19) 0.0037(19) -0.0043(19) C5 0.031(3) 0.024(3) 0.015(2) 0.000(2) 0.002(2) 0.006(2) C6 0.023(3) 0.034(3) 0.016(3) -0.004(2) -0.002(2) 0.008(2) C7 0.042(3) 0.032(3) 0.026(3) 0.000(2) -0.007(2) 0.004(3) C8 0.047(4) 0.043(4) 0.024(3) 0.005(3) -0.010(3) 0.004(3) C9 0.029(3) 0.039(3) 0.025(3) 0.006(2) -0.001(2) 0.002(2) C10 0.033(3) 0.048(4) 0.034(3) -0.003(3) -0.008(3) -0.005(3) C11 0.031(3) 0.020(3) 0.023(3) -0.001(2) -0.003(2) -0.004(2) N1 0.032(3) 0.020(2) 0.016(2) -0.0029(17) -0.0075(18) 0.0073(19) N2 0.026(2) 0.020(2) 0.013(2) -0.0036(16) -0.0041(17) 0.0068(17) N3 0.036(3) 0.052(3) 0.025(3) -0.005(2) -0.012(2) 0.004(2) O1 0.067(3) 0.027(2) 0.022(2) -0.0099(16) -0.0189(19) 0.026(2) O2 0.037(2) 0.0241(19) 0.0169(18) -0.0057(15) -0.0083(15) 0.0093(16) O3 0.031(2) 0.0184(18) 0.0198(18) -0.0051(14) -0.0094(15) 0.0067(15) O4 0.038(2) 0.0173(17) 0.0115(17) -0.0035(13) -0.0020(14) 0.0085(15) O5 0.050(3) 0.044(2) 0.0158(19) 0.0081(16) -0.0049(17) -0.029(2) O6 0.038(2) 0.038(2) 0.0167(19) 0.0028(15) -0.0049(16) -0.0208(18) O1W 0.027(2) 0.042(2) 0.029(2) -0.0117(17) -0.0096(16) 0.0112(17) O2W 0.055(3) 0.028(2) 0.037(2) 0.0071(17) -0.018(2) -0.0111(19) O3W 0.073(4) 0.042(3) 0.045(3) 0.006(2) -0.013(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.308(4) 3_777 ? Eu1 O3 2.362(3) 3_777 ? Eu1 O1 2.391(3) . ? Eu1 O4 2.401(3) 2_756 ? Eu1 O1W 2.415(4) . ? Eu1 O5 2.433(4) . ? Eu1 O6 2.443(3) 3_677 ? Eu1 N2 2.567(4) 2_756 ? Eu1 C11 3.246(5) 3_677 ? Eu1 C11 3.245(5) . ? C1 O2 1.238(6) . ? C1 O1 1.257(6) . ? C1 C2 1.492(6) . ? C2 C3 1.371(6) . ? C2 N1 1.371(6) . ? C3 N2 1.385(6) . ? C3 C4 1.496(7) . ? C4 O3 1.229(5) . ? C4 O4 1.261(5) . ? C5 N2 1.331(6) . ? C5 N1 1.342(6) . ? C5 C6 1.478(7) . ? C6 C9 1.379(7) . ? C6 C7 1.388(7) . ? C7 C8 1.366(8) . ? C7 H7 0.9300 . ? C8 N3 1.328(7) . ? C8 H8 0.9300 . ? C9 C10 1.373(7) . ? C9 H9 0.9300 . ? C10 N3 1.315(7) . ? C10 H10 0.9300 . ? C11 O5 1.249(6) . ? C11 O6 1.255(6) . ? C11 C11 1.536(10) 3_677 ? C11 Eu1 3.246(5) 3_677 ? N1 H1 0.93(6) . ? N2 Eu1 2.567(4) 2_746 ? O2 Eu1 2.308(3) 3_777 ? O3 Eu1 2.362(3) 3_777 ? O4 Eu1 2.401(3) 2_746 ? O6 Eu1 2.443(3) 3_677 ? 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 Eu1 O3 75.29(12) 3_777 3_777 ? O2 Eu1 O1 76.77(12) 3_777 . ? O3 Eu1 O1 152.00(13) 3_777 . ? O2 Eu1 O4 128.67(13) 3_777 2_756 ? O3 Eu1 O4 126.66(11) 3_777 2_756 ? O1 Eu1 O4 71.46(12) . 2_756 ? O2 Eu1 O1W 147.47(12) 3_777 . ? O3 Eu1 O1W 72.18(12) 3_777 . ? O1 Eu1 O1W 135.74(12) . . ? O4 Eu1 O1W 73.58(12) 2_756 . ? O2 Eu1 O5 128.92(13) 3_777 . ? O3 Eu1 O5 126.43(13) 3_777 . ? O1 Eu1 O5 74.15(15) . . ? O4 Eu1 O5 78.92(12) 2_756 . ? O1W Eu1 O5 73.22(15) . . ? O2 Eu1 O6 78.47(13) 3_777 3_677 ? O3 Eu1 O6 76.27(12) 3_777 3_677 ? O1 Eu1 O6 99.91(14) . 3_677 ? O4 Eu1 O6 145.39(12) 2_756 3_677 ? O1W Eu1 O6 93.68(14) . 3_677 ? O5 Eu1 O6 66.54(12) . 3_677 ? O2 Eu1 N2 84.49(13) 3_777 2_756 ? O3 Eu1 N2 74.20(12) 3_777 2_756 ? O1 Eu1 N2 101.38(15) . 2_756 ? O4 Eu1 N2 64.20(12) 2_756 2_756 ? O1W Eu1 N2 86.78(14) . 2_756 ? O5 Eu1 N2 141.86(12) . 2_756 ? O6 Eu1 N2 148.79(12) 3_677 2_756 ? O2 Eu1 C11 93.94(13) 3_777 3_677 ? O3 Eu1 C11 91.91(12) 3_777 3_677 ? O1 Eu1 C11 91.78(14) . 3_677 ? O4 Eu1 C11 125.71(12) 2_756 3_677 ? O1W Eu1 C11 87.14(14) . 3_677 ? O5 Eu1 C11 46.81(12) . 3_677 ? O6 Eu1 C11 19.73(12) 3_677 3_677 ? N2 Eu1 C11 165.98(12) 2_756 3_677 ? O2 Eu1 C11 115.08(13) 3_777 . ? O3 Eu1 C11 113.16(13) 3_777 . ? O1 Eu1 C11 80.59(15) . . ? O4 Eu1 C11 98.36(12) 2_756 . ? O1W Eu1 C11 78.50(14) . . ? O5 Eu1 C11 19.45(12) . . ? O6 Eu1 C11 47.10(12) 3_677 . ? N2 Eu1 C11 160.03(13) 2_756 . ? C11 Eu1 C11 27.37(17) 3_677 . ? O2 C1 O1 125.5(4) . . ? O2 C1 C2 119.0(4) . . ? O1 C1 C2 115.3(4) . . ? C3 C2 N1 105.6(4) . . ? C3 C2 C1 135.3(4) . . ? N1 C2 C1 118.7(4) . . ? C2 C3 N2 109.6(4) . . ? C2 C3 C4 133.0(4) . . ? N2 C3 C4 117.3(4) . . ? O3 C4 O4 124.3(4) . . ? O3 C4 C3 121.9(4) . . ? O4 C4 C3 113.9(4) . . ? N2 C5 N1 111.1(4) . . ? N2 C5 C6 126.8(5) . . ? N1 C5 C6 121.8(4) . . ? C9 C6 C7 117.7(5) . . ? C9 C6 C5 120.1(5) . . ? C7 C6 C5 122.2(5) . . ? C8 C7 C6 118.6(5) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? N3 C8 C7 124.0(5) . . ? N3 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? C10 C9 C6 118.8(5) . . ? C10 C9 H9 120.6 . . ? C6 C9 H9 120.6 . . ? N3 C10 C9 124.1(6) . . ? N3 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? O5 C11 O6 125.9(5) . . ? O5 C11 C11 116.8(6) . 3_677 ? O6 C11 C11 117.4(5) . 3_677 ? O5 C11 Eu1 166.9(4) . 3_677 ? O6 C11 Eu1 41.1(2) . 3_677 ? C11 C11 Eu1 76.3(4) 3_677 3_677 ? O5 C11 Eu1 40.5(2) . . ? O6 C11 Eu1 166.3(3) . . ? C11 C11 Eu1 76.3(4) 3_677 . ? Eu1 C11 Eu1 152.63(17) 3_677 . ? C5 N1 C2 108.3(4) . . ? C5 N1 H1 128(4) . . ? C2 N1 H1 124(4) . . ? C5 N2 C3 105.4(4) . . ? C5 N2 Eu1 138.2(3) . 2_746 ? C3 N2 Eu1 113.8(3) . 2_746 ? C10 N3 C8 116.8(5) . . ? C1 O1 Eu1 137.3(3) . . ? C1 O2 Eu1 143.9(4) . 3_777 ? C4 O3 Eu1 153.1(3) . 3_777 ? C4 O4 Eu1 126.1(3) . 2_746 ? C11 O5 Eu1 120.1(3) . . ? C11 O6 Eu1 119.2(3) . 3_677 ? 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 -7.7(9) . . . . ? O1 C1 C2 C3 176.6(5) . . . . ? O2 C1 C2 N1 163.0(5) . . . . ? O1 C1 C2 N1 -12.7(7) . . . . ? N1 C2 C3 N2 -1.9(5) . . . . ? C1 C2 C3 N2 169.6(5) . . . . ? N1 C2 C3 C4 179.3(5) . . . . ? C1 C2 C3 C4 -9.2(10) . . . . ? C2 C3 C4 O3 -1.2(8) . . . . ? N2 C3 C4 O3 -180.0(4) . . . . ? C2 C3 C4 O4 178.8(5) . . . . ? N2 C3 C4 O4 0.0(6) . . . . ? N2 C5 C6 C9 51.9(8) . . . . ? N1 C5 C6 C9 -121.7(6) . . . . ? N2 C5 C6 C7 -130.5(6) . . . . ? N1 C5 C6 C7 55.9(7) . . . . ? C9 C6 C7 C8 0.5(8) . . . . ? C5 C6 C7 C8 -177.2(5) . . . . ? C6 C7 C8 N3 1.3(9) . . . . ? C7 C6 C9 C10 -1.8(8) . . . . ? C5 C6 C9 C10 176.0(5) . . . . ? C6 C9 C10 N3 1.5(9) . . . . ? O2 Eu1 C11 O5 -139.3(4) 3_777 . . . ? O3 Eu1 C11 O5 136.7(4) 3_777 . . . ? O1 Eu1 C11 O5 -68.8(4) . . . . ? O4 Eu1 C11 O5 0.7(4) 2_756 . . . ? O1W Eu1 C11 O5 72.0(4) . . . . ? O6 Eu1 C11 O5 178.2(5) 3_677 . . . ? N2 Eu1 C11 O5 28.7(6) 2_756 . . . ? C11 Eu1 C11 O5 178.4(7) 3_677 . . . ? O2 Eu1 C11 O6 -136.3(16) 3_777 . . . ? O3 Eu1 C11 O6 139.7(16) 3_777 . . . ? O1 Eu1 C11 O6 -65.8(16) . . . . ? O4 Eu1 C11 O6 3.7(16) 2_756 . . . ? O1W Eu1 C11 O6 74.9(16) . . . . ? O5 Eu1 C11 O6 2.9(14) . . . . ? O6 Eu1 C11 O6 -178.9(16) 3_677 . . . ? N2 Eu1 C11 O6 31.6(18) 2_756 . . . ? C11 Eu1 C11 O6 -179(2) 3_677 . . . ? O2 Eu1 C11 C11 42.4(4) 3_777 . . 3_677 ? O3 Eu1 C11 C11 -41.6(4) 3_777 . . 3_677 ? O1 Eu1 C11 C11 112.9(4) . . . 3_677 ? O4 Eu1 C11 C11 -177.6(4) 2_756 . . 3_677 ? O1W Eu1 C11 C11 -106.4(4) . . . 3_677 ? O5 Eu1 C11 C11 -178.4(7) . . . 3_677 ? O6 Eu1 C11 C11 -0.2(3) 3_677 . . 3_677 ? N2 Eu1 C11 C11 -149.7(3) 2_756 . . 3_677 ? O2 Eu1 C11 Eu1 42.4(4) 3_777 . . 3_677 ? O3 Eu1 C11 Eu1 -41.6(4) 3_777 . . 3_677 ? O1 Eu1 C11 Eu1 112.9(4) . . . 3_677 ? O4 Eu1 C11 Eu1 -177.6(4) 2_756 . . 3_677 ? O1W Eu1 C11 Eu1 -106.4(4) . . . 3_677 ? O5 Eu1 C11 Eu1 -178.4(7) . . . 3_677 ? O6 Eu1 C11 Eu1 -0.2(3) 3_677 . . 3_677 ? N2 Eu1 C11 Eu1 -149.7(3) 2_756 . . 3_677 ? C11 Eu1 C11 Eu1 0.0 3_677 . . 3_677 ? N2 C5 N1 C2 -2.5(6) . . . . ? C6 C5 N1 C2 172.0(5) . . . . ? C3 C2 N1 C5 2.6(6) . . . . ? C1 C2 N1 C5 -170.6(4) . . . . ? N1 C5 N2 C3 1.3(6) . . . . ? C6 C5 N2 C3 -172.9(5) . . . . ? N1 C5 N2 Eu1 -158.2(4) . . . 2_746 ? C6 C5 N2 Eu1 27.6(9) . . . 2_746 ? C2 C3 N2 C5 0.5(5) . . . . ? C4 C3 N2 C5 179.5(4) . . . . ? C2 C3 N2 Eu1 165.7(3) . . . 2_746 ? C4 C3 N2 Eu1 -15.3(5) . . . 2_746 ? C9 C10 N3 C8 0.2(9) . . . . ? C7 C8 N3 C10 -1.6(9) . . . . ? O2 C1 O1 Eu1 -1.9(10) . . . . ? C2 C1 O1 Eu1 173.5(4) . . . . ? O2 Eu1 O1 C1 31.5(6) 3_777 . . . ? O3 Eu1 O1 C1 35.3(7) 3_777 . . . ? O4 Eu1 O1 C1 170.6(6) 2_756 . . . ? O1W Eu1 O1 C1 -149.8(5) . . . . ? O5 Eu1 O1 C1 -106.0(6) . . . . ? O6 Eu1 O1 C1 -44.0(6) 3_677 . . . ? N2 Eu1 O1 C1 113.0(6) 2_756 . . . ? C11 Eu1 O1 C1 -62.1(6) 3_677 . . . ? C11 Eu1 O1 C1 -87.2(6) . . . . ? O1 C1 O2 Eu1 -123.0(6) . . . 3_777 ? C2 C1 O2 Eu1 61.8(8) . . . 3_777 ? O4 C4 O3 Eu1 176.4(4) . . . 3_777 ? C3 C4 O3 Eu1 -3.6(10) . . . 3_777 ? O3 C4 O4 Eu1 -161.4(3) . . . 2_746 ? C3 C4 O4 Eu1 18.6(6) . . . 2_746 ? O6 C11 O5 Eu1 -179.1(4) . . . . ? C11 C11 O5 Eu1 1.8(8) 3_677 . . . ? Eu1 C11 O5 Eu1 176.7(14) 3_677 . . . ? O2 Eu1 O5 C11 49.4(5) 3_777 . . . ? O3 Eu1 O5 C11 -51.5(5) 3_777 . . . ? O1 Eu1 O5 C11 107.1(4) . . . . ? O4 Eu1 O5 C11 -179.3(4) 2_756 . . . ? O1W Eu1 O5 C11 -103.2(4) . . . . ? O6 Eu1 O5 C11 -1.5(4) 3_677 . . . ? N2 Eu1 O5 C11 -164.6(4) 2_756 . . . ? C11 Eu1 O5 C11 -1.0(4) 3_677 . . . ? O5 C11 O6 Eu1 -178.6(4) . . . 3_677 ? C11 C11 O6 Eu1 0.5(8) 3_677 . . 3_677 ? Eu1 C11 O6 Eu1 179.1(14) . . . 3_677 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.772 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.181 data_7 _database_code_depnum_ccdc_archive 'CCDC 837795' #TrackingRef '1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H7 N3 O7 Tb, 2(H2O)' _chemical_formula_sum 'C11 H11 N3 O9 Tb' _chemical_formula_weight 488.12 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.321(9) _cell_length_b 14.724(1) _cell_length_c 11.522(3) _cell_angle_alpha 90 _cell_angle_beta 90.797(7) _cell_angle_gamma 90 _cell_volume 1411.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1286 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 5.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 0.212 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6981 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2479 _reflns_number_gt 1947 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. H atoms of coordination water molecule were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1A...H1B was restrained to 1.35+-0.02 \%A. H atom of imidazole ring was located in difference Fourier maps and refined isotropically with distance restraints of N---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(N). ; _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^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2479 _refine_ls_number_parameters 229 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Tb1 Tb 0.77765(4) 0.132268(19) 0.93312(2) 0.01475(11) Uani 1 1 d . . . C1 C 0.8173(7) 0.2393(4) 0.6861(5) 0.0150(14) Uani 1 1 d . . . C2 C 0.9270(8) 0.2944(4) 0.7603(5) 0.0191(15) Uani 1 1 d . . . C3 C 1.0055(8) 0.3748(4) 0.7449(5) 0.0203(14) Uani 1 1 d . . . C4 C 1.0357(8) 0.4357(4) 0.6455(5) 0.0222(16) Uani 1 1 d . . . C5 C 1.0601(9) 0.3202(5) 0.9192(6) 0.0271(17) Uani 1 1 d . . . C6 C 1.1467(8) 0.3124(5) 1.0306(5) 0.0249(16) Uani 1 1 d . . . C7 C 1.2433(9) 0.2376(5) 1.0514(6) 0.0340(18) Uani 1 1 d . . . H7 H 1.2487 0.1910 0.9971 0.041 Uiso 1 1 calc R . . C8 C 1.3311(10) 0.2328(6) 1.1529(7) 0.042(2) Uani 1 1 d . . . H8 H 1.3969 0.1825 1.1648 0.050 Uiso 1 1 calc R . . C9 C 1.1421(9) 0.3788(5) 1.1167(6) 0.0327(18) Uani 1 1 d . . . H9 H 1.0780 0.4301 1.1067 0.039 Uiso 1 1 calc R . . C10 C 1.2329(10) 0.3683(5) 1.2167(6) 0.042(2) Uani 1 1 d . . . H10 H 1.2280 0.4134 1.2731 0.050 Uiso 1 1 calc R . . C11 C 0.4742(9) -0.0026(5) 0.9356(5) 0.0245(16) Uani 1 1 d . . . H1 H 1.161(9) 0.442(5) 0.849(6) 0.04(2) Uiso 1 1 d . . . H1A H 0.561(9) 0.2897(14) 0.899(6) 0.06(3) Uiso 1 1 d D . . H1B H 0.490(6) 0.212(4) 0.858(5) 0.03(2) Uiso 1 1 d D . . N1 N 1.0874(7) 0.3906(4) 0.8474(4) 0.0237(13) Uani 1 1 d . . . N2 N 0.9610(6) 0.2602(3) 0.8705(4) 0.0189(12) Uani 1 1 d . . . N3 N 1.3273(8) 0.2969(5) 1.2365(5) 0.0389(17) Uani 1 1 d . . . O1 O 0.7704(5) 0.1663(3) 0.7318(3) 0.0233(11) Uani 1 1 d . . . O2 O 0.7787(5) 0.2626(3) 0.5855(3) 0.0218(10) Uani 1 1 d . . . O3 O 0.9909(6) 0.4106(3) 0.5459(4) 0.0288(11) Uani 1 1 d . . . O4 O 1.1127(6) 0.5071(3) 0.6671(4) 0.0347(13) Uani 1 1 d . . . O5 O 0.5541(6) 0.0425(3) 0.8662(4) 0.0307(12) Uani 1 1 d . . . O6 O 0.3562(6) -0.0529(3) 0.9120(3) 0.0300(12) Uani 1 1 d . . . O1W O 0.5594(6) 0.2330(4) 0.9043(4) 0.0327(12) Uani 1 1 d D . . O2W O 0.6923(6) 0.0273(3) 0.5847(4) 0.0383(13) Uani 1 1 d . . . O3W O 0.5821(7) 0.4253(3) 0.8546(4) 0.0482(15) 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 Tb1 0.02010(18) 0.01419(17) 0.00991(15) 0.00031(14) -0.00152(11) -0.00199(15) C1 0.017(4) 0.017(3) 0.011(3) -0.001(3) 0.000(3) 0.004(3) C2 0.025(4) 0.021(4) 0.011(3) 0.003(3) -0.001(3) 0.001(3) C3 0.022(4) 0.020(3) 0.018(3) -0.001(3) -0.007(3) -0.004(3) C4 0.032(4) 0.021(4) 0.014(3) 0.005(3) -0.010(3) -0.003(3) C5 0.033(5) 0.029(4) 0.019(3) -0.001(3) -0.005(3) -0.001(3) C6 0.027(4) 0.031(4) 0.017(3) 0.005(3) 0.003(3) -0.009(3) C7 0.031(5) 0.038(4) 0.034(4) -0.002(4) -0.002(3) -0.003(4) C8 0.036(5) 0.044(5) 0.045(5) 0.010(4) -0.008(4) 0.003(4) C9 0.044(5) 0.029(4) 0.025(4) 0.004(3) -0.012(3) -0.008(4) C10 0.050(5) 0.038(5) 0.035(4) -0.007(4) -0.018(4) -0.012(4) C11 0.035(4) 0.020(4) 0.019(4) -0.001(3) -0.001(3) -0.005(3) N1 0.031(4) 0.024(3) 0.015(3) 0.002(2) -0.007(2) -0.011(3) N2 0.018(3) 0.022(3) 0.017(3) -0.002(2) -0.003(2) -0.007(2) N3 0.034(4) 0.052(4) 0.030(4) 0.006(3) -0.014(3) -0.010(3) O1 0.032(3) 0.024(2) 0.014(2) 0.006(2) -0.005(2) -0.007(2) O2 0.027(3) 0.023(3) 0.015(2) 0.0037(19) -0.0081(19) -0.006(2) O3 0.033(3) 0.029(3) 0.024(3) 0.003(2) -0.002(2) -0.011(2) O4 0.059(4) 0.024(3) 0.020(2) 0.012(2) -0.012(2) -0.023(3) O5 0.033(3) 0.042(3) 0.016(2) 0.004(2) 0.000(2) -0.025(2) O6 0.036(3) 0.039(3) 0.014(2) 0.000(2) -0.002(2) -0.021(2) O1W 0.031(3) 0.038(4) 0.028(3) -0.011(3) -0.014(2) 0.006(3) O2W 0.048(4) 0.029(3) 0.037(3) -0.010(2) -0.017(3) 0.010(2) O3W 0.063(4) 0.040(3) 0.041(3) 0.007(3) -0.016(3) 0.005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Tb1 O3 2.274(5) 4_566 ? Tb1 O2 2.341(4) 4_566 ? Tb1 O4 2.364(4) 2_746 ? Tb1 O1W 2.365(5) . ? Tb1 O1 2.373(4) . ? Tb1 O5 2.400(4) . ? Tb1 O6 2.418(4) 3_657 ? Tb1 N2 2.536(5) . ? C1 O2 1.246(6) . ? C1 O1 1.261(7) . ? C1 C2 1.483(8) . ? C2 C3 1.365(9) . ? C2 N2 1.391(7) . ? C3 N1 1.375(7) . ? C3 C4 1.479(8) . ? C4 O3 1.258(7) . ? C4 O4 1.254(7) . ? C5 N2 1.327(8) . ? C5 N1 1.347(8) . ? C5 C6 1.468(9) . ? C6 C7 1.382(10) . ? C6 C9 1.395(9) . ? C7 C8 1.373(10) . ? C7 H7 0.9300 . ? C8 N3 1.349(10) . ? C8 H8 0.9300 . ? C9 C10 1.377(10) . ? C9 H9 0.9300 . ? C10 N3 1.331(10) . ? C10 H10 0.9300 . ? C11 O5 1.240(7) . ? C11 O6 1.257(8) . ? C11 C11 1.541(12) 3_657 ? N1 H1 0.98(7) . ? O2 Tb1 2.341(4) 4_565 ? O3 Tb1 2.274(5) 4_565 ? O4 Tb1 2.364(4) 2_756 ? O6 Tb1 2.418(4) 3_657 ? O1W H1A 0.84(2) . ? O1W H1B 0.83(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O2 76.14(15) 4_566 4_566 ? O3 Tb1 O4 76.06(16) 4_566 2_746 ? O2 Tb1 O4 152.15(16) 4_566 2_746 ? O3 Tb1 O1W 147.78(17) 4_566 . ? O2 Tb1 O1W 71.65(16) 4_566 . ? O4 Tb1 O1W 136.17(17) 2_746 . ? O3 Tb1 O1 128.77(16) 4_566 . ? O2 Tb1 O1 126.38(15) 4_566 . ? O4 Tb1 O1 72.08(15) 2_746 . ? O1W Tb1 O1 73.81(17) . . ? O3 Tb1 O5 128.73(17) 4_566 . ? O2 Tb1 O5 126.88(16) 4_566 . ? O4 Tb1 O5 73.53(18) 2_746 . ? O1W Tb1 O5 73.16(19) . . ? O1 Tb1 O5 78.07(15) . . ? O3 Tb1 O6 78.91(17) 4_566 3_657 ? O2 Tb1 O6 76.29(15) 4_566 3_657 ? O4 Tb1 O6 99.70(17) 2_746 3_657 ? O1W Tb1 O6 92.65(19) . 3_657 ? O1 Tb1 O6 144.88(15) . 3_657 ? O5 Tb1 O6 66.95(14) . 3_657 ? O3 Tb1 N2 84.31(17) 4_566 . ? O2 Tb1 N2 74.09(16) 4_566 . ? O4 Tb1 N2 101.68(18) 2_746 . ? O1W Tb1 N2 87.59(19) . . ? O1 Tb1 N2 64.67(15) . . ? O5 Tb1 N2 141.68(16) . . ? O6 Tb1 N2 148.67(15) 3_657 . ? O2 C1 O1 123.0(6) . . ? O2 C1 C2 122.3(6) . . ? O1 C1 C2 114.6(5) . . ? C3 C2 N2 109.9(5) . . ? C3 C2 C1 133.7(6) . . ? N2 C2 C1 116.4(5) . . ? C2 C3 N1 105.5(5) . . ? C2 C3 C4 135.5(6) . . ? N1 C3 C4 118.4(5) . . ? O3 C4 O4 124.8(6) . . ? O3 C4 C3 118.5(6) . . ? O4 C4 C3 116.5(5) . . ? N2 C5 N1 111.2(6) . . ? N2 C5 C6 127.7(6) . . ? N1 C5 C6 120.8(6) . . ? C7 C6 C9 117.2(6) . . ? C7 C6 C5 119.4(6) . . ? C9 C6 C5 123.3(6) . . ? C8 C7 C6 119.4(7) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? N3 C8 C7 123.7(7) . . ? N3 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? C10 C9 C6 119.7(7) . . ? C10 C9 H9 120.1 . . ? C6 C9 H9 120.1 . . ? N3 C10 C9 123.2(7) . . ? N3 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? O5 C11 O6 126.9(6) . . ? O5 C11 C11 116.7(8) . 3_657 ? O6 C11 C11 116.4(7) . 3_657 ? C5 N1 C3 108.1(5) . . ? C5 N1 H1 134(4) . . ? C3 N1 H1 117(4) . . ? C5 N2 C2 105.2(5) . . ? C5 N2 Tb1 138.3(4) . . ? C2 N2 Tb1 114.4(4) . . ? C10 N3 C8 116.7(6) . . ? C1 O1 Tb1 125.8(4) . . ? C1 O2 Tb1 151.3(4) . 4_565 ? C4 O3 Tb1 145.3(5) . 4_565 ? C4 O4 Tb1 139.1(4) . 2_756 ? C11 O5 Tb1 120.5(4) . . ? C11 O6 Tb1 119.4(4) . 3_657 ? Tb1 O1W H1A 129(5) . . ? Tb1 O1W H1B 113(5) . . ? H1A O1W H1B 109(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 0.8(11) . . . . ? O1 C1 C2 C3 178.9(7) . . . . ? O2 C1 C2 N2 -179.6(5) . . . . ? O1 C1 C2 N2 -1.4(8) . . . . ? N2 C2 C3 N1 -0.6(7) . . . . ? C1 C2 C3 N1 179.1(7) . . . . ? N2 C2 C3 C4 169.8(7) . . . . ? C1 C2 C3 C4 -10.5(13) . . . . ? C2 C3 C4 O3 -5.2(12) . . . . ? N1 C3 C4 O3 164.2(6) . . . . ? C2 C3 C4 O4 178.4(7) . . . . ? N1 C3 C4 O4 -12.1(9) . . . . ? N2 C5 C6 C7 54.4(11) . . . . ? N1 C5 C6 C7 -119.2(8) . . . . ? N2 C5 C6 C9 -128.2(8) . . . . ? N1 C5 C6 C9 58.2(10) . . . . ? C9 C6 C7 C8 -1.2(10) . . . . ? C5 C6 C7 C8 176.4(7) . . . . ? C6 C7 C8 N3 1.2(12) . . . . ? C7 C6 C9 C10 0.6(10) . . . . ? C5 C6 C9 C10 -176.9(7) . . . . ? C6 C9 C10 N3 0.1(12) . . . . ? N2 C5 N1 C3 -1.7(8) . . . . ? C6 C5 N1 C3 172.8(6) . . . . ? C2 C3 N1 C5 1.4(7) . . . . ? C4 C3 N1 C5 -171.0(6) . . . . ? N1 C5 N2 C2 1.3(8) . . . . ? C6 C5 N2 C2 -172.8(7) . . . . ? N1 C5 N2 Tb1 -160.3(5) . . . . ? C6 C5 N2 Tb1 25.6(12) . . . . ? C3 C2 N2 C5 -0.5(7) . . . . ? C1 C2 N2 C5 179.8(6) . . . . ? C3 C2 N2 Tb1 166.2(4) . . . . ? C1 C2 N2 Tb1 -13.5(7) . . . . ? O3 Tb1 N2 C5 -46.2(7) 4_566 . . . ? O2 Tb1 N2 C5 31.0(7) 4_566 . . . ? O4 Tb1 N2 C5 -120.7(7) 2_746 . . . ? O1W Tb1 N2 C5 102.6(7) . . . . ? O1 Tb1 N2 C5 175.8(7) . . . . ? O5 Tb1 N2 C5 161.2(6) . . . . ? O6 Tb1 N2 C5 11.4(9) 3_657 . . . ? O3 Tb1 N2 C2 153.3(4) 4_566 . . . ? O2 Tb1 N2 C2 -129.5(4) 4_566 . . . ? O4 Tb1 N2 C2 78.9(4) 2_746 . . . ? O1W Tb1 N2 C2 -57.9(4) . . . . ? O1 Tb1 N2 C2 15.3(4) . . . . ? O5 Tb1 N2 C2 0.7(6) . . . . ? O6 Tb1 N2 C2 -149.1(4) 3_657 . . . ? C9 C10 N3 C8 -0.2(12) . . . . ? C7 C8 N3 C10 -0.5(12) . . . . ? O2 C1 O1 Tb1 -163.1(4) . . . . ? C2 C1 O1 Tb1 18.7(7) . . . . ? O3 Tb1 O1 C1 -77.7(5) 4_566 . . . ? O2 Tb1 O1 C1 24.4(6) 4_566 . . . ? O4 Tb1 O1 C1 -131.9(5) 2_746 . . . ? O1W Tb1 O1 C1 76.0(5) . . . . ? O5 Tb1 O1 C1 151.7(5) . . . . ? O6 Tb1 O1 C1 146.8(4) 3_657 . . . ? N2 Tb1 O1 C1 -19.1(5) . . . . ? O1 C1 O2 Tb1 174.9(5) . . . 4_565 ? C2 C1 O2 Tb1 -7.0(12) . . . 4_565 ? O4 C4 O3 Tb1 -125.1(7) . . . 4_565 ? C3 C4 O3 Tb1 58.9(11) . . . 4_565 ? O3 C4 O4 Tb1 -0.4(12) . . . 2_756 ? C3 C4 O4 Tb1 175.7(5) . . . 2_756 ? O6 C11 O5 Tb1 -179.2(6) . . . . ? C11 C11 O5 Tb1 0.0(10) 3_657 . . . ? O3 Tb1 O5 C11 52.1(6) 4_566 . . . ? O2 Tb1 O5 C11 -50.5(6) 4_566 . . . ? O4 Tb1 O5 C11 108.1(5) 2_746 . . . ? O1W Tb1 O5 C11 -100.9(5) . . . . ? O1 Tb1 O5 C11 -177.3(5) . . . . ? O6 Tb1 O5 C11 -0.4(5) 3_657 . . . ? N2 Tb1 O5 C11 -163.9(5) . . . . ? O5 C11 O6 Tb1 -179.7(6) . . . 3_657 ? C11 C11 O6 Tb1 1.1(10) 3_657 . . 3_657 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.735 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.165