# Electronic SUpplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'En-Qing Gao' _publ_contact_author_email EQGAO@CHEM.ECNU.EDU.CN _publ_section_title ; Syntheses, Structures and Luminescence Properties of Cadmium (II) Coordination Polymers with In Situ Formed Oxalate and Bis(chelating) Bridging Ligands ; loop_ _publ_author_name 'En-Qing Gao.' 'Ai-Ling Cheng.' 'Qin-Xiang Jia.' 'Qi Yue.' 'Jian-Yong Zhang.' # Attachment 'B807165A-675255-revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 675255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cd3 N4 O14' _chemical_formula_weight 795.46 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 tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+3/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+1/4' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' '-y, -x, -z+1/2' _cell_length_a 9.4587(13) _cell_length_b 9.4587(13) _cell_length_c 21.123(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1889.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 956 _cell_measurement_theta_min 2.195 _cell_measurement_theta_max 27.094 _exptl_crystal_description diamond _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 3.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4803 _exptl_absorpt_correction_T_max 0.6266 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9160 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2079 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The water hydrogen atoms H7A and H7B were located from the difference Fourier map. To obtain a reasonable H-O-H geometry, the H-O and H...H distances were restrained to 0.85 and 1.38 \%A, respectively. And to avoid close H...H contacts between lattice water hydrogens and the framework hydrogens, the relevant distances were also restrained to 2.3 \%A using DFIX. DFIX 0.85 0.04 o7 h7a o7 h7b DFIX 1.38 0.04 h7a h7b EQIV $1 1-y, 1-x,1.5-z DFIX 2.3 0.04 H5a H7B H7b H7B_$1 ; _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^)+(0.0176P)^2^+5.2445P] 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 0.02(5) _refine_ls_number_reflns 2079 _refine_ls_number_parameters 166 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.269 _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 0.96553(4) -0.03447(4) 1.0000 0.02603(13) Uani 1 2 d S . . Cd2 Cd 0.72449(4) 0.09685(4) 0.824021(17) 0.02046(9) Uani 1 1 d . . . C1 C 0.5215(6) -0.1527(6) 0.7907(3) 0.0279(11) Uani 1 1 d . . . C2 C 0.6629(6) -0.2230(6) 0.8001(2) 0.0233(10) Uani 1 1 d . . . C3 C 0.7969(7) -0.4240(6) 0.8002(3) 0.0328(12) Uani 1 1 d . . . H3A H 0.8045 -0.5215 0.7958 0.039 Uiso 1 1 calc R . . C4 C 0.9135(8) -0.3479(7) 0.8152(3) 0.0420(15) Uani 1 1 d . . . H4A H 1.0014 -0.3912 0.8188 0.050 Uiso 1 1 calc R . . C5 C 0.8983(7) -0.2041(6) 0.8249(3) 0.0361(12) Uani 1 1 d . . . H5A H 0.9762 -0.1499 0.8362 0.043 Uiso 1 1 calc RD . . C6 C 1.0045(5) 0.1718(5) 0.8962(2) 0.0208(9) Uani 1 1 d . . . C7 C 1.0070(5) 0.2635(5) 0.8350(2) 0.0196(9) Uani 1 1 d . . . N1 N 0.7707(5) -0.1424(5) 0.8179(2) 0.0269(9) Uani 1 1 d . . . N2 N 0.6700(5) -0.3619(5) 0.7916(2) 0.0275(10) Uani 1 1 d . . . O1 O 0.5145(4) -0.0232(4) 0.8028(2) 0.0308(8) Uani 1 1 d . . . O2 O 0.4237(5) -0.2282(4) 0.7721(2) 0.0392(10) Uani 1 1 d . . . O3 O 0.9119(4) 0.0772(4) 0.90044(16) 0.0248(7) Uani 1 1 d . . . O4 O 1.0949(4) 0.1969(4) 0.93744(17) 0.0263(7) Uani 1 1 d . . . O5 O 0.9115(4) 0.2391(4) 0.79454(15) 0.0230(7) Uani 1 1 d . . . O6 O 1.1028(4) 0.3514(4) 0.83068(18) 0.0308(8) Uani 1 1 d . . . O7 O 1.1896(11) -0.041(2) 0.8090(6) 0.235(9) Uani 1 1 d D . . H7B H 1.129(5) 0.001(4) 0.7855(18) 0.352 Uiso 1 1 d D . . H7A H 1.268(10) -0.04(3) 0.787(7) 0.352 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 0.02721(17) 0.02721(17) 0.0237(2) 0.00008(15) -0.00008(15) 0.0090(2) Cd2 0.01977(17) 0.01688(16) 0.02473(16) -0.00123(15) 0.00111(14) -0.00037(13) C1 0.023(3) 0.030(3) 0.031(3) -0.002(2) 0.001(2) -0.003(2) C2 0.031(3) 0.019(2) 0.020(2) 0.0052(19) -0.003(2) -0.002(2) C3 0.043(3) 0.023(3) 0.033(3) -0.003(2) -0.007(2) 0.003(2) C4 0.048(4) 0.034(3) 0.044(4) -0.002(3) -0.007(3) 0.013(3) C5 0.034(3) 0.033(3) 0.041(3) -0.004(3) -0.011(3) -0.003(2) C6 0.020(2) 0.020(2) 0.022(2) -0.0035(19) 0.0019(18) 0.0006(16) C7 0.019(2) 0.018(2) 0.021(2) -0.0005(18) 0.0003(17) 0.0021(17) N1 0.030(2) 0.021(2) 0.030(2) -0.0016(18) -0.009(2) 0.0010(17) N2 0.034(2) 0.021(2) 0.027(2) 0.0019(17) -0.0039(19) -0.0014(18) O1 0.026(2) 0.0227(19) 0.044(2) -0.0033(18) -0.0007(17) 0.0008(16) O2 0.035(2) 0.027(2) 0.056(3) -0.0054(19) -0.0009(19) -0.0032(17) O3 0.0262(18) 0.0225(18) 0.0257(16) 0.0032(14) -0.0028(15) -0.0069(14) O4 0.0296(18) 0.0265(18) 0.0229(17) 0.0011(14) -0.0100(15) -0.0056(15) O5 0.0240(17) 0.0256(18) 0.0193(15) 0.0040(13) -0.0037(14) -0.0027(15) O6 0.0294(19) 0.036(2) 0.0267(18) 0.0030(16) -0.0057(17) -0.0138(17) O7 0.079(7) 0.47(3) 0.158(10) 0.153(14) 0.045(7) 0.073(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.327(4) 7_545 ? Cd1 O2 2.327(4) 2_546 ? Cd1 N2 2.340(5) 7_545 ? Cd1 N2 2.340(5) 2_546 ? Cd1 O3 2.407(3) 5_647 ? Cd1 O3 2.407(3) . ? Cd1 O4 2.834(4) . ? Cd2 N1 2.308(4) . ? Cd2 O5 2.308(4) . ? Cd2 O4 2.317(4) 2_456 ? Cd2 O1 2.331(4) . ? Cd2 O6 2.370(4) 2_456 ? Cd2 O3 2.405(4) . ? Cd2 O5 2.529(3) 8_666 ? C1 O2 1.232(7) . ? C1 O1 1.254(7) . ? C1 C2 1.507(8) . ? C2 N2 1.327(7) . ? C2 N1 1.328(7) . ? C3 N2 1.349(7) . ? C3 C4 1.354(10) . ? C3 H3A 0.9300 . ? C4 C5 1.383(9) . ? C4 H4A 0.9300 . ? C5 N1 1.349(7) . ? C5 H5A 0.9300 . ? C6 O4 1.243(6) . ? C6 O3 1.255(6) . ? C6 C7 1.557(7) . ? C7 O6 1.234(6) . ? C7 O5 1.264(6) . ? N2 Cd1 2.340(5) 2_446 ? O2 Cd1 2.327(4) 2_446 ? O4 Cd2 2.317(4) 2_556 ? O5 Cd2 2.529(3) 8_666 ? O6 Cd2 2.370(4) 2_556 ? O7 H7B 0.86(4) . ? O7 H7A 0.88(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 73.3(2) 7_545 2_546 ? O2 Cd1 N2 70.17(15) 7_545 7_545 ? O2 Cd1 N2 143.29(17) 2_546 7_545 ? O2 Cd1 N2 143.29(17) 7_545 2_546 ? O2 Cd1 N2 70.17(15) 2_546 2_546 ? N2 Cd1 N2 146.5(2) 7_545 2_546 ? O2 Cd1 O3 102.26(14) 7_545 5_647 ? O2 Cd1 O3 92.68(15) 2_546 5_647 ? N2 Cd1 O3 91.69(15) 7_545 5_647 ? N2 Cd1 O3 82.97(15) 2_546 5_647 ? O2 Cd1 O3 92.68(15) 7_545 . ? O2 Cd1 O3 102.26(14) 2_546 . ? N2 Cd1 O3 82.97(15) 7_545 . ? N2 Cd1 O3 91.69(15) 2_546 . ? O3 Cd1 O3 161.42(17) 5_647 . ? O2 Cd1 O4 129.89(14) 7_545 . ? O2 Cd1 O4 136.45(13) 2_546 . ? N2 Cd1 O4 73.62(15) 7_545 . ? N2 Cd1 O4 77.96(14) 2_546 . ? O3 Cd1 O4 112.36(12) 5_647 . ? O3 Cd1 O4 49.06(11) . . ? N1 Cd2 O5 114.28(15) . . ? N1 Cd2 O4 156.90(15) . 2_456 ? O5 Cd2 O4 83.49(13) . 2_456 ? N1 Cd2 O1 70.92(16) . . ? O5 Cd2 O1 152.25(13) . . ? O4 Cd2 O1 86.51(14) 2_456 . ? N1 Cd2 O6 109.98(15) . 2_456 ? O5 Cd2 O6 118.76(14) . 2_456 ? O4 Cd2 O6 70.00(13) 2_456 2_456 ? O1 Cd2 O6 81.38(15) . 2_456 ? N1 Cd2 O3 79.76(14) . . ? O5 Cd2 O3 70.19(12) . . ? O4 Cd2 O3 121.69(13) 2_456 . ? O1 Cd2 O3 136.01(13) . . ? O6 Cd2 O3 78.68(13) 2_456 . ? N1 Cd2 O5 83.59(14) . 8_666 ? O5 Cd2 O5 69.30(14) . 8_666 ? O4 Cd2 O5 89.71(12) 2_456 8_666 ? O1 Cd2 O5 84.87(13) . 8_666 ? O6 Cd2 O5 156.03(13) 2_456 8_666 ? O3 Cd2 O5 124.17(12) . 8_666 ? O2 C1 O1 126.3(5) . . ? O2 C1 C2 116.9(5) . . ? O1 C1 C2 116.8(5) . . ? N2 C2 N1 124.6(5) . . ? N2 C2 C1 117.6(5) . . ? N1 C2 C1 117.8(5) . . ? N2 C3 C4 121.7(5) . . ? N2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C3 C4 C5 118.2(6) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? N1 C5 C4 120.2(6) . . ? N1 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? O4 C6 O3 124.4(5) . . ? O4 C6 C7 117.7(4) . . ? O3 C6 C7 117.8(4) . . ? O6 C7 O5 126.7(5) . . ? O6 C7 C6 116.6(4) . . ? O5 C7 C6 116.7(4) . . ? C2 N1 C5 118.0(5) . . ? C2 N1 Cd2 115.7(4) . . ? C5 N1 Cd2 126.0(4) . . ? C2 N2 C3 117.3(5) . . ? C2 N2 Cd1 115.1(4) . 2_446 ? C3 N2 Cd1 127.1(4) . 2_446 ? C1 O1 Cd2 118.1(4) . . ? C1 O2 Cd1 119.7(4) . 2_446 ? C6 O3 Cd2 114.3(3) . . ? C6 O3 Cd1 103.2(3) . . ? Cd2 O3 Cd1 140.85(16) . . ? C6 O4 Cd2 116.8(3) . 2_556 ? C6 O4 Cd1 83.3(3) . . ? Cd2 O4 Cd1 158.03(15) 2_556 . ? C7 O5 Cd2 118.1(3) . . ? C7 O5 Cd2 131.8(3) . 8_666 ? Cd2 O5 Cd2 108.82(13) . 8_666 ? C7 O6 Cd2 115.7(3) . 2_556 ? H7B O7 H7A 105(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N2 -4.0(8) . . . . ? O1 C1 C2 N2 175.5(5) . . . . ? O2 C1 C2 N1 177.6(5) . . . . ? O1 C1 C2 N1 -2.8(8) . . . . ? N2 C3 C4 C5 3.4(10) . . . . ? C3 C4 C5 N1 -1.6(10) . . . . ? O4 C6 C7 O6 2.9(7) . . . . ? O3 C6 C7 O6 -176.8(5) . . . . ? O4 C6 C7 O5 -177.9(4) . . . . ? O3 C6 C7 O5 2.4(7) . . . . ? N2 C2 N1 C5 3.5(8) . . . . ? C1 C2 N1 C5 -178.3(5) . . . . ? N2 C2 N1 Cd2 177.4(4) . . . . ? C1 C2 N1 Cd2 -4.4(6) . . . . ? C4 C5 N1 C2 -1.7(9) . . . . ? C4 C5 N1 Cd2 -174.9(5) . . . . ? O5 Cd2 N1 C2 -144.5(3) . . . . ? O4 Cd2 N1 C2 -6.7(6) 2_456 . . . ? O1 Cd2 N1 C2 6.1(4) . . . . ? O6 Cd2 N1 C2 79.0(4) 2_456 . . . ? O3 Cd2 N1 C2 152.8(4) . . . . ? O5 Cd2 N1 C2 -80.7(4) 8_666 . . . ? O5 Cd2 N1 C5 28.8(5) . . . . ? O4 Cd2 N1 C5 166.6(4) 2_456 . . . ? O1 Cd2 N1 C5 179.5(5) . . . . ? O6 Cd2 N1 C5 -107.7(5) 2_456 . . . ? O3 Cd2 N1 C5 -33.8(5) . . . . ? O5 Cd2 N1 C5 92.7(5) 8_666 . . . ? N1 C2 N2 C3 -1.8(8) . . . . ? C1 C2 N2 C3 180.0(5) . . . . ? N1 C2 N2 Cd1 -173.9(4) . . . 2_446 ? C1 C2 N2 Cd1 7.9(6) . . . 2_446 ? C4 C3 N2 C2 -1.8(9) . . . . ? C4 C3 N2 Cd1 169.2(5) . . . 2_446 ? O2 C1 O1 Cd2 -171.9(5) . . . . ? C2 C1 O1 Cd2 8.6(7) . . . . ? N1 Cd2 O1 C1 -8.0(4) . . . . ? O5 Cd2 O1 C1 98.1(5) . . . . ? O4 Cd2 O1 C1 167.0(4) 2_456 . . . ? O6 Cd2 O1 C1 -122.7(4) 2_456 . . . ? O3 Cd2 O1 C1 -59.0(5) . . . . ? O5 Cd2 O1 C1 76.9(4) 8_666 . . . ? O1 C1 O2 Cd1 178.2(5) . . . 2_446 ? C2 C1 O2 Cd1 -2.2(7) . . . 2_446 ? O4 C6 O3 Cd2 166.1(4) . . . . ? C7 C6 O3 Cd2 -14.2(5) . . . . ? O4 C6 O3 Cd1 -2.3(6) . . . . ? C7 C6 O3 Cd1 177.4(3) . . . . ? N1 Cd2 O3 C6 135.2(4) . . . . ? O5 Cd2 O3 C6 14.5(3) . . . . ? O4 Cd2 O3 C6 -54.1(4) 2_456 . . . ? O1 Cd2 O3 C6 -176.6(3) . . . . ? O6 Cd2 O3 C6 -111.9(3) 2_456 . . . ? O5 Cd2 O3 C6 60.2(4) 8_666 . . . ? N1 Cd2 O3 Cd1 -62.9(3) . . . . ? O5 Cd2 O3 Cd1 176.5(3) . . . . ? O4 Cd2 O3 Cd1 107.9(3) 2_456 . . . ? O1 Cd2 O3 Cd1 -14.6(4) . . . . ? O6 Cd2 O3 Cd1 50.1(3) 2_456 . . . ? O5 Cd2 O3 Cd1 -137.8(2) 8_666 . . . ? O2 Cd1 O3 C6 145.1(3) 7_545 . . . ? O2 Cd1 O3 C6 -141.4(3) 2_546 . . . ? N2 Cd1 O3 C6 75.5(3) 7_545 . . . ? N2 Cd1 O3 C6 -71.3(3) 2_546 . . . ? O3 Cd1 O3 C6 1.4(3) 5_647 . . . ? O4 Cd1 O3 C6 1.1(3) . . . . ? O2 Cd1 O3 Cd2 -18.0(3) 7_545 . . . ? O2 Cd1 O3 Cd2 55.4(3) 2_546 . . . ? N2 Cd1 O3 Cd2 -87.7(3) 7_545 . . . ? N2 Cd1 O3 Cd2 125.5(3) 2_546 . . . ? O3 Cd1 O3 Cd2 -161.8(3) 5_647 . . . ? O4 Cd1 O3 Cd2 -162.1(3) . . . . ? O3 C6 O4 Cd2 -168.7(4) . . . 2_556 ? C7 C6 O4 Cd2 11.6(6) . . . 2_556 ? O3 C6 O4 Cd1 1.9(5) . . . . ? C7 C6 O4 Cd1 -177.7(4) . . . . ? O2 Cd1 O4 C6 -51.0(3) 7_545 . . . ? O2 Cd1 O4 C6 58.6(4) 2_546 . . . ? N2 Cd1 O4 C6 -96.0(3) 7_545 . . . ? N2 Cd1 O4 C6 101.9(3) 2_546 . . . ? O3 Cd1 O4 C6 179.0(3) 5_647 . . . ? O3 Cd1 O4 C6 -1.1(3) . . . . ? O2 Cd1 O4 Cd2 106.2(5) 7_545 . . 2_556 ? O2 Cd1 O4 Cd2 -144.3(4) 2_546 . . 2_556 ? N2 Cd1 O4 Cd2 61.1(5) 7_545 . . 2_556 ? N2 Cd1 O4 Cd2 -101.0(5) 2_546 . . 2_556 ? O3 Cd1 O4 Cd2 -23.9(5) 5_647 . . 2_556 ? O3 Cd1 O4 Cd2 156.0(6) . . . 2_556 ? O6 C7 O5 Cd2 -169.2(4) . . . . ? C6 C7 O5 Cd2 11.7(5) . . . . ? O6 C7 O5 Cd2 25.1(8) . . . 8_666 ? C6 C7 O5 Cd2 -154.0(3) . . . 8_666 ? N1 Cd2 O5 C7 -82.0(4) . . . . ? O4 Cd2 O5 C7 113.4(3) 2_456 . . . ? O1 Cd2 O5 C7 -177.0(3) . . . . ? O6 Cd2 O5 C7 50.5(4) 2_456 . . . ? O3 Cd2 O5 C7 -13.7(3) . . . . ? O5 Cd2 O5 C7 -154.4(3) 8_666 . . . ? N1 Cd2 O5 Cd2 86.79(17) . . . 8_666 ? O4 Cd2 O5 Cd2 -77.83(14) 2_456 . . 8_666 ? O1 Cd2 O5 Cd2 -8.2(4) . . . 8_666 ? O6 Cd2 O5 Cd2 -140.74(14) 2_456 . . 8_666 ? O3 Cd2 O5 Cd2 155.08(17) . . . 8_666 ? O5 Cd2 O5 Cd2 14.34(17) 8_666 . . 8_666 ? O5 C7 O6 Cd2 165.6(4) . . . 2_556 ? C6 C7 O6 Cd2 -15.3(6) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.684 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.118 # Attachment 'B807165A-675256-revised.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 675256' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Cd2 N12 O5' _chemical_formula_weight 625.10 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)/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 10.391(3) _cell_length_b 16.868(5) _cell_length_c 11.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.251(3) _cell_angle_gamma 90.00 _cell_volume 1787.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3762 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.45 _exptl_crystal_description rod _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 2.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6411 _exptl_absorpt_correction_T_max 0.7924 _exptl_absorpt_process_details 'SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _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_% ? _diffrn_reflns_number 9881 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3506 _reflns_number_gt 2723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The water hydrogen atoms H5b and H5c were located from the difference Fourier map. To obtain a reasonable H-O-H geometry, the H-O and H...H distances were restrained to 0.85 and 1.38 \%A, respectively. A DFIX constraint was applied on C11-C12 of oxalate to avoid too long C-C distance. The last DFIX constraint on N9(tetrazole)...H5c(water) was applied to make the water O-H properly orientated for hydrogen bonding. DFIX 1.54 C12 C11 DFIX 0.85 0.03 O5 H5b O5 H5c DFIX 1.38 0.03 H5b H5c DFIX 2.1 N9 H5c ; _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^)+(0.0285P)^2^+0.6283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00032(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3506 _refine_ls_number_parameters 287 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.33214(3) 0.812603(15) 0.90127(3) 0.02830(10) Uani 1 1 d . . . Cd2 Cd -0.28900(3) 0.688126(15) 0.65014(3) 0.02839(10) Uani 1 1 d . . . C1 C 0.0055(4) 0.7737(2) 0.7516(4) 0.0290(8) Uani 1 1 d . . . C2 C 0.0583(4) 0.7009(2) 0.8262(4) 0.0283(8) Uani 1 1 d . . . C3 C 0.0129(5) 0.5775(2) 0.8766(4) 0.0400(10) Uani 1 1 d . . . H3A H -0.0501 0.5365 0.8690 0.048 Uiso 1 1 calc R . . C4 C 0.1538(5) 0.5672(2) 0.9561(4) 0.0430(10) Uani 1 1 d . . . H4A H 0.1873 0.5196 1.0003 0.052 Uiso 1 1 calc R . . C5 C 0.2447(4) 0.6288(2) 0.9691(4) 0.0401(10) Uani 1 1 d . . . H5A H 0.3410 0.6232 1.0242 0.048 Uiso 1 1 calc R . . C6 C 0.3299(4) 0.99988(19) 0.8713(4) 0.0311(9) Uani 1 1 d . . . C7 C 0.2670(4) 1.0022(2) 0.9642(4) 0.0328(9) Uani 1 1 d . . . C8 C 0.1805(5) 1.0741(3) 1.0807(5) 0.0529(12) Uani 1 1 d . . . H8A H 0.1514 1.1222 1.1016 0.063 Uiso 1 1 calc R . . C9 C 0.1734(6) 1.0073(3) 1.1471(5) 0.0634(15) Uani 1 1 d . . . H9A H 0.1427 1.0096 1.2134 0.076 Uiso 1 1 calc R . . C10 C 0.2134(5) 0.9367(3) 1.1119(5) 0.0565(13) Uani 1 1 d . . . H10A H 0.2069 0.8902 1.1535 0.068 Uiso 1 1 calc R . . C11 C 0.4513(4) 0.73848(19) 0.7127(3) 0.0274(8) Uani 1 1 d D . . C12 C 0.5890(4) 0.7567(2) 0.8397(4) 0.0289(8) Uani 1 1 d D . . N1 N 0.0876(3) 0.83510(18) 0.7598(3) 0.0344(8) Uani 1 1 d . . . N2 N -0.0001(4) 0.8889(2) 0.6775(4) 0.0485(9) Uani 1 1 d . . . N3 N -0.1305(4) 0.8604(2) 0.6228(4) 0.0465(9) Uani 1 1 d . . . N4 N -0.1287(3) 0.78562(18) 0.6691(3) 0.0340(8) Uani 1 1 d . . . N5 N -0.0383(3) 0.64469(18) 0.8086(3) 0.0312(7) Uani 1 1 d . . . N6 N 0.1973(3) 0.69694(17) 0.9039(3) 0.0320(7) Uani 1 1 d . . . N7 N 0.3792(3) 0.93500(17) 0.8388(3) 0.0345(7) Uani 1 1 d . . . N8 N 0.4332(4) 0.9588(2) 0.7563(4) 0.0455(9) Uani 1 1 d . . . N9 N 0.4163(4) 1.0355(2) 0.7402(3) 0.0443(9) Uani 1 1 d D . . N10 N 0.3502(3) 1.06317(18) 0.8116(3) 0.0352(7) Uani 1 1 d . . . N11 N 0.2269(4) 1.07309(19) 0.9885(3) 0.0394(8) Uani 1 1 d . . . N12 N 0.2611(4) 0.93318(19) 1.0199(3) 0.0412(8) Uani 1 1 d . . . O1 O 0.4728(3) 0.71483(15) 0.6172(2) 0.0325(6) Uani 1 1 d . . . O2 O 0.3339(3) 0.74876(15) 0.7148(2) 0.0356(6) Uani 1 1 d . . . O3 O 0.5676(3) 0.78317(15) 0.9343(2) 0.0345(6) Uani 1 1 d . . . O4 O 0.7060(3) 0.74438(16) 0.8390(2) 0.0374(6) Uani 1 1 d . . . O5 O 0.4516(9) 1.0851(7) 0.5040(11) 0.221(4) Uani 1 1 d D . . H5C H 0.470(8) 1.065(10) 0.585(7) 0.331 Uiso 1 1 d D . . H5B H 0.359(3) 1.086(10) 0.466(10) 0.331 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 0.02148(16) 0.03033(16) 0.03048(17) 0.00093(11) 0.00859(13) -0.00157(11) Cd2 0.02116(16) 0.03050(16) 0.03097(17) -0.00017(11) 0.00869(13) -0.00125(11) C1 0.022(2) 0.034(2) 0.031(2) -0.0030(16) 0.0114(17) -0.0016(16) C2 0.024(2) 0.033(2) 0.026(2) -0.0076(15) 0.0087(17) -0.0037(16) C3 0.041(3) 0.036(2) 0.041(2) 0.0010(19) 0.016(2) -0.010(2) C4 0.042(3) 0.035(2) 0.042(3) 0.0082(19) 0.009(2) 0.004(2) C5 0.032(2) 0.043(2) 0.036(2) 0.0045(19) 0.0070(19) 0.003(2) C6 0.020(2) 0.028(2) 0.034(2) 0.0005(16) 0.0000(17) -0.0018(16) C7 0.026(2) 0.030(2) 0.034(2) -0.0017(16) 0.0050(19) -0.0010(16) C8 0.058(3) 0.047(3) 0.055(3) -0.013(2) 0.025(3) 0.001(2) C9 0.079(4) 0.067(4) 0.060(3) -0.001(3) 0.045(3) -0.001(3) C10 0.064(3) 0.054(3) 0.052(3) 0.011(2) 0.026(3) -0.003(3) C11 0.029(2) 0.0220(18) 0.033(2) 0.0025(15) 0.0148(18) -0.0018(16) C12 0.030(2) 0.0261(19) 0.029(2) 0.0030(15) 0.0114(18) 0.0005(16) N1 0.0289(18) 0.0297(16) 0.043(2) 0.0038(15) 0.0132(16) -0.0013(15) N2 0.039(2) 0.040(2) 0.062(3) 0.0063(18) 0.018(2) 0.0003(18) N3 0.035(2) 0.041(2) 0.055(2) 0.0098(18) 0.0115(18) 0.0038(18) N4 0.0277(19) 0.0329(17) 0.0366(19) 0.0060(14) 0.0091(16) -0.0038(15) N5 0.0255(17) 0.0338(17) 0.0322(18) -0.0011(14) 0.0105(15) -0.0041(14) N6 0.0243(17) 0.0343(18) 0.0313(18) 0.0010(14) 0.0061(14) -0.0040(14) N7 0.0322(19) 0.0283(16) 0.042(2) -0.0039(15) 0.0147(16) -0.0011(15) N8 0.046(2) 0.041(2) 0.050(2) -0.0092(17) 0.0211(19) -0.0042(18) N9 0.042(2) 0.045(2) 0.047(2) 0.0002(17) 0.0190(18) -0.0018(18) N10 0.0286(18) 0.0327(17) 0.043(2) 0.0034(15) 0.0138(16) 0.0022(15) N11 0.037(2) 0.0347(18) 0.042(2) -0.0056(15) 0.0128(17) 0.0003(16) N12 0.041(2) 0.0362(19) 0.039(2) 0.0027(16) 0.0106(17) -0.0019(16) O1 0.0273(15) 0.0427(15) 0.0267(14) -0.0068(12) 0.0106(12) 0.0009(12) O2 0.0241(14) 0.0449(15) 0.0364(15) -0.0058(12) 0.0116(12) -0.0009(12) O3 0.0325(16) 0.0429(15) 0.0286(15) -0.0027(12) 0.0134(13) 0.0033(13) O4 0.0243(15) 0.0502(16) 0.0356(16) -0.0075(13) 0.0108(12) -0.0004(13) O5 0.191(8) 0.219(9) 0.281(11) 0.041(8) 0.129(8) -0.011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.289(3) 4_576 ? Cd1 N7 2.300(3) . ? Cd1 O3 2.366(3) . ? Cd1 O2 2.369(3) . ? Cd1 N1 2.384(3) . ? Cd1 N6 2.410(3) . ? Cd2 N4 2.285(3) . ? Cd2 N10 2.295(3) 2_546 ? Cd2 O3 2.298(3) 4_475 ? Cd2 O4 2.352(3) 1_455 ? Cd2 O1 2.384(3) 1_455 ? Cd2 N5 2.559(3) . ? C1 N1 1.320(4) . ? C1 N4 1.320(5) . ? C1 C2 1.457(5) . ? C2 N5 1.333(4) . ? C2 N6 1.334(5) . ? C3 N5 1.345(5) . ? C3 C4 1.363(6) . ? C3 H3A 0.9300 . ? C4 C5 1.369(5) . ? C4 H4A 0.9300 . ? C5 N6 1.340(5) . ? C5 H5A 0.9300 . ? C6 N7 1.324(4) . ? C6 N10 1.326(4) . ? C6 C7 1.452(5) . ? C7 N11 1.332(4) . ? C7 N12 1.337(5) . ? C8 N11 1.319(5) . ? C8 C9 1.373(6) . ? C8 H8A 0.9300 . ? C9 C10 1.375(6) . ? C9 H9A 0.9300 . ? C10 N12 1.328(5) . ? C10 H10A 0.9300 . ? C11 O2 1.242(4) . ? C11 O1 1.255(4) . ? C11 C12 1.564(5) . ? C12 O4 1.236(4) . ? C12 O3 1.260(4) . ? N1 N2 1.340(4) . ? N2 N3 1.316(5) . ? N3 N4 1.362(4) . ? N7 N8 1.336(4) . ? N8 N9 1.309(5) . ? N9 N10 1.345(4) . ? N10 Cd2 2.295(3) 2_556 ? O1 Cd1 2.289(2) 4_575 ? O1 Cd2 2.384(3) 1_655 ? O3 Cd2 2.298(3) 4_676 ? O4 Cd2 2.352(3) 1_655 ? O5 H5C 0.91(3) . ? O5 H5B 0.87(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N7 112.59(10) 4_576 . ? O1 Cd1 O3 69.01(9) 4_576 . ? N7 Cd1 O3 84.03(10) . . ? O1 Cd1 O2 127.47(9) 4_576 . ? N7 Cd1 O2 93.06(10) . . ? O3 Cd1 O2 69.20(9) . . ? O1 Cd1 N1 139.32(10) 4_576 . ? N7 Cd1 N1 87.55(11) . . ? O3 Cd1 N1 150.94(10) . . ? O2 Cd1 N1 83.59(10) . . ? O1 Cd1 N6 86.22(10) 4_576 . ? N7 Cd1 N6 158.62(11) . . ? O3 Cd1 N6 113.33(10) . . ? O2 Cd1 N6 82.40(10) . . ? N1 Cd1 N6 71.21(10) . . ? N4 Cd2 N10 153.22(11) . 2_546 ? N4 Cd2 O3 93.71(10) . 4_475 ? N10 Cd2 O3 106.62(10) 2_546 4_475 ? N4 Cd2 O4 85.52(10) . 1_455 ? N10 Cd2 O4 94.92(10) 2_546 1_455 ? O3 Cd2 O4 128.24(9) 4_475 1_455 ? N4 Cd2 O1 123.07(10) . 1_455 ? N10 Cd2 O1 81.41(10) 2_546 1_455 ? O3 Cd2 O1 68.54(9) 4_475 1_455 ? O4 Cd2 O1 69.05(8) 1_455 1_455 ? N4 Cd2 N5 69.89(11) . . ? N10 Cd2 N5 83.51(10) 2_546 . ? O3 Cd2 N5 143.78(9) 4_475 . ? O4 Cd2 N5 83.83(9) 1_455 . ? O1 Cd2 N5 147.49(9) 1_455 . ? N1 C1 N4 112.8(3) . . ? N1 C1 C2 123.2(3) . . ? N4 C1 C2 124.0(3) . . ? N5 C2 N6 126.7(3) . . ? N5 C2 C1 116.1(3) . . ? N6 C2 C1 117.2(3) . . ? N5 C3 C4 122.3(4) . . ? N5 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? C3 C4 C5 118.2(4) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? N6 C5 C4 121.1(4) . . ? N6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? N7 C6 N10 111.2(4) . . ? N7 C6 C7 124.6(3) . . ? N10 C6 C7 124.2(3) . . ? N11 C7 N12 127.2(4) . . ? N11 C7 C6 116.7(3) . . ? N12 C7 C6 116.1(3) . . ? N11 C8 C9 122.8(4) . . ? N11 C8 H8A 118.6 . . ? C9 C8 H8A 118.6 . . ? C8 C9 C10 117.4(5) . . ? C8 C9 H9A 121.3 . . ? C10 C9 H9A 121.3 . . ? N12 C10 C9 121.6(4) . . ? N12 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? O2 C11 O1 126.6(4) . . ? O2 C11 C12 118.6(3) . . ? O1 C11 C12 114.8(3) . . ? O4 C12 O3 126.4(4) . . ? O4 C12 C11 118.7(3) . . ? O3 C12 C11 114.9(3) . . ? C1 N1 N2 104.7(3) . . ? C1 N1 Cd1 113.2(2) . . ? N2 N1 Cd1 142.0(2) . . ? N3 N2 N1 109.7(3) . . ? N2 N3 N4 108.4(3) . . ? C1 N4 N3 104.4(3) . . ? C1 N4 Cd2 117.7(2) . . ? N3 N4 Cd2 137.8(3) . . ? C2 N5 C3 115.2(3) . . ? C2 N5 Cd2 112.2(2) . . ? C3 N5 Cd2 132.6(3) . . ? C2 N6 C5 116.4(3) . . ? C2 N6 Cd1 115.0(2) . . ? C5 N6 Cd1 128.5(3) . . ? C6 N7 N8 105.7(3) . . ? C6 N7 Cd1 120.0(3) . . ? N8 N7 Cd1 133.6(2) . . ? N9 N8 N7 108.8(3) . . ? N8 N9 N10 109.4(3) . . ? C6 N10 N9 104.9(3) . . ? C6 N10 Cd2 121.9(3) . 2_556 ? N9 N10 Cd2 133.1(2) . 2_556 ? C8 N11 C7 115.1(4) . . ? C10 N12 C7 115.8(4) . . ? C11 O1 Cd1 135.2(2) . 4_575 ? C11 O1 Cd2 118.7(2) . 1_655 ? Cd1 O1 Cd2 106.09(9) 4_575 1_655 ? C11 O2 Cd1 117.4(2) . . ? C12 O3 Cd2 134.6(2) . 4_676 ? C12 O3 Cd1 119.0(2) . . ? Cd2 O3 Cd1 106.38(10) 4_676 . ? C12 O4 Cd2 118.4(2) . 1_655 ? H5C O5 H5B 103(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N5 179.0(3) . . . . ? N4 C1 C2 N5 -0.9(5) . . . . ? N1 C1 C2 N6 -1.4(5) . . . . ? N4 C1 C2 N6 178.8(3) . . . . ? N5 C3 C4 C5 1.8(6) . . . . ? C3 C4 C5 N6 -1.1(6) . . . . ? N7 C6 C7 N11 178.0(4) . . . . ? N10 C6 C7 N11 0.5(6) . . . . ? N7 C6 C7 N12 0.6(6) . . . . ? N10 C6 C7 N12 -176.8(4) . . . . ? N11 C8 C9 C10 -1.7(8) . . . . ? C8 C9 C10 N12 1.9(8) . . . . ? O2 C11 C12 O4 178.0(3) . . . . ? O1 C11 C12 O4 -2.4(5) . . . . ? O2 C11 C12 O3 -2.0(5) . . . . ? O1 C11 C12 O3 177.6(3) . . . . ? N4 C1 N1 N2 0.0(4) . . . . ? C2 C1 N1 N2 -179.9(3) . . . . ? N4 C1 N1 Cd1 -177.5(2) . . . . ? C2 C1 N1 Cd1 2.6(4) . . . . ? O1 Cd1 N1 C1 -61.8(3) 4_576 . . . ? N7 Cd1 N1 C1 175.5(3) . . . . ? O3 Cd1 N1 C1 102.4(3) . . . . ? O2 Cd1 N1 C1 82.1(2) . . . . ? N6 Cd1 N1 C1 -2.0(2) . . . . ? O1 Cd1 N1 N2 122.1(4) 4_576 . . . ? N7 Cd1 N1 N2 -0.6(4) . . . . ? O3 Cd1 N1 N2 -73.6(5) . . . . ? O2 Cd1 N1 N2 -93.9(4) . . . . ? N6 Cd1 N1 N2 -178.1(4) . . . . ? C1 N1 N2 N3 0.4(4) . . . . ? Cd1 N1 N2 N3 176.7(3) . . . . ? N1 N2 N3 N4 -0.6(5) . . . . ? N1 C1 N4 N3 -0.3(4) . . . . ? C2 C1 N4 N3 179.5(3) . . . . ? N1 C1 N4 Cd2 -176.8(2) . . . . ? C2 C1 N4 Cd2 3.0(5) . . . . ? N2 N3 N4 C1 0.6(4) . . . . ? N2 N3 N4 Cd2 176.0(3) . . . . ? N10 Cd2 N4 C1 -9.5(4) 2_546 . . . ? O3 Cd2 N4 C1 -149.4(3) 4_475 . . . ? O4 Cd2 N4 C1 82.5(3) 1_455 . . . ? O1 Cd2 N4 C1 143.9(2) 1_455 . . . ? N5 Cd2 N4 C1 -2.6(3) . . . . ? N10 Cd2 N4 N3 175.5(3) 2_546 . . . ? O3 Cd2 N4 N3 35.6(4) 4_475 . . . ? O4 Cd2 N4 N3 -92.4(4) 1_455 . . . ? O1 Cd2 N4 N3 -31.1(4) 1_455 . . . ? N5 Cd2 N4 N3 -177.5(4) . . . . ? N6 C2 N5 C3 -0.7(5) . . . . ? C1 C2 N5 C3 178.9(3) . . . . ? N6 C2 N5 Cd2 178.9(3) . . . . ? C1 C2 N5 Cd2 -1.5(4) . . . . ? C4 C3 N5 C2 -0.9(6) . . . . ? C4 C3 N5 Cd2 179.5(3) . . . . ? N4 Cd2 N5 C2 2.1(2) . . . . ? N10 Cd2 N5 C2 179.0(2) 2_546 . . . ? O3 Cd2 N5 C2 69.6(3) 4_475 . . . ? O4 Cd2 N5 C2 -85.4(2) 1_455 . . . ? O1 Cd2 N5 C2 -118.3(2) 1_455 . . . ? N4 Cd2 N5 C3 -178.3(4) . . . . ? N10 Cd2 N5 C3 -1.5(3) 2_546 . . . ? O3 Cd2 N5 C3 -110.9(3) 4_475 . . . ? O4 Cd2 N5 C3 94.2(3) 1_455 . . . ? O1 Cd2 N5 C3 61.2(4) 1_455 . . . ? N5 C2 N6 C5 1.3(6) . . . . ? C1 C2 N6 C5 -178.3(3) . . . . ? N5 C2 N6 Cd1 178.9(3) . . . . ? C1 C2 N6 Cd1 -0.7(4) . . . . ? C4 C5 N6 C2 -0.3(6) . . . . ? C4 C5 N6 Cd1 -177.5(3) . . . . ? O1 Cd1 N6 C2 147.0(3) 4_576 . . . ? N7 Cd1 N6 C2 -5.5(5) . . . . ? O3 Cd1 N6 C2 -147.8(2) . . . . ? O2 Cd1 N6 C2 -84.4(3) . . . . ? N1 Cd1 N6 C2 1.4(2) . . . . ? O1 Cd1 N6 C5 -35.7(3) 4_576 . . . ? N7 Cd1 N6 C5 171.7(3) . . . . ? O3 Cd1 N6 C5 29.5(3) . . . . ? O2 Cd1 N6 C5 92.9(3) . . . . ? N1 Cd1 N6 C5 178.6(3) . . . . ? N10 C6 N7 N8 0.4(4) . . . . ? C7 C6 N7 N8 -177.3(4) . . . . ? N10 C6 N7 Cd1 -171.1(2) . . . . ? C7 C6 N7 Cd1 11.1(5) . . . . ? O1 Cd1 N7 C6 -77.6(3) 4_576 . . . ? O3 Cd1 N7 C6 -141.9(3) . . . . ? O2 Cd1 N7 C6 149.4(3) . . . . ? N1 Cd1 N7 C6 66.0(3) . . . . ? N6 Cd1 N7 C6 72.5(4) . . . . ? O1 Cd1 N7 N8 113.7(3) 4_576 . . . ? O3 Cd1 N7 N8 49.4(3) . . . . ? O2 Cd1 N7 N8 -19.3(4) . . . . ? N1 Cd1 N7 N8 -102.8(4) . . . . ? N6 Cd1 N7 N8 -96.2(4) . . . . ? C6 N7 N8 N9 -0.1(4) . . . . ? Cd1 N7 N8 N9 169.8(3) . . . . ? N7 N8 N9 N10 -0.3(4) . . . . ? N7 C6 N10 N9 -0.6(4) . . . . ? C7 C6 N10 N9 177.1(4) . . . . ? N7 C6 N10 Cd2 -177.1(2) . . . 2_556 ? C7 C6 N10 Cd2 0.7(5) . . . 2_556 ? N8 N9 N10 C6 0.5(4) . . . . ? N8 N9 N10 Cd2 176.4(3) . . . 2_556 ? C9 C8 N11 C7 -0.1(7) . . . . ? N12 C7 N11 C8 2.1(6) . . . . ? C6 C7 N11 C8 -174.9(4) . . . . ? C9 C10 N12 C7 -0.2(7) . . . . ? N11 C7 N12 C10 -1.9(6) . . . . ? C6 C7 N12 C10 175.1(4) . . . . ? O2 C11 O1 Cd1 5.8(6) . . . 4_575 ? C12 C11 O1 Cd1 -173.8(2) . . . 4_575 ? O2 C11 O1 Cd2 -173.7(3) . . . 1_655 ? C12 C11 O1 Cd2 6.7(4) . . . 1_655 ? O1 C11 O2 Cd1 -170.8(3) . . . . ? C12 C11 O2 Cd1 8.7(4) . . . . ? O1 Cd1 O2 C11 -47.7(3) 4_576 . . . ? N7 Cd1 O2 C11 74.1(3) . . . . ? O3 Cd1 O2 C11 -8.4(2) . . . . ? N1 Cd1 O2 C11 161.2(3) . . . . ? N6 Cd1 O2 C11 -126.9(3) . . . . ? O4 C12 O3 Cd2 -6.5(6) . . . 4_676 ? C11 C12 O3 Cd2 173.5(2) . . . 4_676 ? O4 C12 O3 Cd1 174.1(3) . . . . ? C11 C12 O3 Cd1 -5.9(4) . . . . ? O1 Cd1 O3 C12 154.8(3) 4_576 . . . ? N7 Cd1 O3 C12 -88.2(3) . . . . ? O2 Cd1 O3 C12 7.4(2) . . . . ? N1 Cd1 O3 C12 -14.2(4) . . . . ? N6 Cd1 O3 C12 78.9(3) . . . . ? O1 Cd1 O3 Cd2 -24.71(10) 4_576 . . 4_676 ? N7 Cd1 O3 Cd2 92.28(12) . . . 4_676 ? O2 Cd1 O3 Cd2 -172.14(13) . . . 4_676 ? N1 Cd1 O3 Cd2 166.22(15) . . . 4_676 ? N6 Cd1 O3 Cd2 -100.69(12) . . . 4_676 ? O3 C12 O4 Cd2 176.8(3) . . . 1_655 ? C11 C12 O4 Cd2 -3.2(4) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.769 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.090