Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 #============================================================ data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _publ_contact_author_name 'Professor Hans-Conrad zur Loye' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina 29208 USA ; _publ_contact_author_phone '803 777 6916' _publ_contact_author_fax '803 777 8508' _publ_contact_author_email zurloye@sc.edu loop_ _publ_author_name 'Hans-Conrad Zur Loye' 'Delia M. Ciurtin' 'Mark D. Smith' _publ_section_title ; Structural diversity in the Cu(pyrazinecarboxylate)2 / CdCl2 system: new one-, two- and three-dimensional mixed metal coordination polymers ; data_cmpd1 _database_code_CSD 188220 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H12 Cd Cl2 Cu N4 O7' _chemical_formula_weight 547.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 7.2898(7) _cell_length_b 11.0148(10) _cell_length_c 11.3154(11) _cell_angle_alpha 68.462(2) _cell_angle_beta 88.051(2) _cell_angle_gamma 84.854(2) _cell_volume 841.73(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5007 _cell_measurement_theta_min 2.806 _cell_measurement_theta_max 26.378 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 2.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6987 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7776 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3441 _reflns_number_gt 2875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^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 3441 _refine_ls_number_parameters 250 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.010 _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 Cu Cu 0.39983(6) 0.31792(4) 0.45829(4) 0.03135(12) Uani 1 1 d . . . Cd Cd -0.07416(3) 0.84747(2) -0.03339(2) 0.02848(8) Uani 1 1 d . . . Cl1 Cl -0.15744(12) 0.96444(8) 0.12328(8) 0.0337(2) Uani 1 1 d . . . Cl2 Cl -0.32455(13) 0.69301(9) 0.03051(9) 0.0441(2) Uani 1 1 d . . . C1 C 0.2171(5) 0.5609(3) 0.3334(3) 0.0285(7) Uani 1 1 d . . . C2 C 0.1259(5) 0.6659(3) 0.2421(3) 0.0301(8) Uani 1 1 d . . . H2 H 0.0569 0.7283 0.2660 0.036 Uiso 1 1 calc R . . C3 C 0.2322(5) 0.5879(3) 0.0908(3) 0.0355(8) Uani 1 1 d . . . H3 H 0.2429 0.5960 0.0062 0.043 Uiso 1 1 calc R . . C4 C 0.3197(5) 0.4794(3) 0.1829(3) 0.0356(8) Uani 1 1 d . . . H4 H 0.3846 0.4150 0.1595 0.043 Uiso 1 1 calc R . . C5 C 0.2214(5) 0.5407(3) 0.4732(3) 0.0307(8) Uani 1 1 d . . . C6 C 0.6414(4) 0.1039(3) 0.5846(3) 0.0272(7) Uani 1 1 d . . . C7 C 0.7418(5) 0.0079(3) 0.6785(3) 0.0325(8) Uani 1 1 d . . . H7 H 0.8211 -0.0525 0.6581 0.039 Uiso 1 1 calc R . . C8 C 0.6103(4) 0.0859(3) 0.8255(3) 0.0307(8) Uani 1 1 d . . . H8 H 0.5973 0.0819 0.9089 0.037 Uiso 1 1 calc R . . C9 C 0.5070(4) 0.1817(3) 0.7316(3) 0.0294(8) Uani 1 1 d . . . H9 H 0.4243 0.2402 0.7522 0.035 Uiso 1 1 calc R . . C10 C 0.6534(5) 0.1249(3) 0.4448(3) 0.0312(8) Uani 1 1 d . . . N1 N 0.3117(4) 0.4664(3) 0.3036(2) 0.0298(6) Uani 1 1 d . . . N2 N 0.1339(4) 0.6807(3) 0.1191(2) 0.0311(7) Uani 1 1 d . . . N3 N 0.5254(4) 0.1905(3) 0.6117(2) 0.0269(6) Uani 1 1 d . . . N4 N 0.7273(4) -0.0003(3) 0.8006(2) 0.0308(7) Uani 1 1 d . . . O1 O 0.3002(3) 0.4340(2) 0.5446(2) 0.0367(6) Uani 1 1 d . . . O2 O 0.1516(4) 0.6283(2) 0.5071(2) 0.0423(6) Uani 1 1 d . . . O3 O 0.5484(3) 0.2196(2) 0.3736(2) 0.0379(6) Uani 1 1 d . . . O4 O 0.7599(4) 0.0534(2) 0.4093(2) 0.0439(7) Uani 1 1 d . . . O5 O 0.1533(4) 0.2106(3) 0.4789(3) 0.0481(7) Uani 1 1 d D . . H5A H 0.058(4) 0.249(4) 0.496(4) 0.053(13) Uiso 1 1 d D . . H5B H 0.149(6) 0.135(2) 0.529(3) 0.059(14) Uiso 1 1 d D . . O6 O 0.0703(4) 0.7853(3) -0.1845(3) 0.0441(7) Uani 1 1 d D . . H6A H 0.139(6) 0.840(4) -0.227(4) 0.082(18) Uiso 1 1 d D . . H6B H 0.065(6) 0.717(3) -0.198(4) 0.054(13) Uiso 1 1 d D . . O7 O 0.1187(5) 0.5630(3) 0.7725(3) 0.0548(8) Uani 1 1 d D . . H7A H 0.148(6) 0.573(4) 0.698(2) 0.058(15) Uiso 1 1 d D . . H7B H 0.204(5) 0.508(4) 0.813(4) 0.10(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 Cu 0.0405(3) 0.0264(2) 0.0216(2) -0.00460(18) -0.00557(18) 0.00943(19) Cd 0.03639(15) 0.02443(14) 0.02104(13) -0.00493(10) -0.00429(10) 0.00267(10) Cl1 0.0402(5) 0.0336(5) 0.0296(4) -0.0139(4) 0.0045(4) -0.0063(4) Cl2 0.0506(6) 0.0416(5) 0.0402(5) -0.0132(4) 0.0004(4) -0.0112(4) C1 0.0364(19) 0.0229(17) 0.0247(17) -0.0072(14) -0.0032(15) -0.0006(14) C2 0.0347(19) 0.0258(18) 0.0284(18) -0.0092(15) -0.0040(15) 0.0036(15) C3 0.042(2) 0.039(2) 0.0194(17) -0.0042(15) -0.0030(15) 0.0025(17) C4 0.044(2) 0.034(2) 0.0284(19) -0.0136(16) -0.0015(16) 0.0062(17) C5 0.0321(19) 0.0283(19) 0.0297(18) -0.0087(16) -0.0019(15) 0.0004(15) C6 0.0328(19) 0.0259(17) 0.0209(16) -0.0063(14) -0.0039(14) 0.0003(14) C7 0.035(2) 0.0281(19) 0.0292(18) -0.0058(15) -0.0040(15) 0.0061(15) C8 0.0339(19) 0.035(2) 0.0201(17) -0.0061(15) 0.0011(14) -0.0040(15) C9 0.0317(19) 0.0303(18) 0.0246(17) -0.0089(15) 0.0006(14) 0.0009(15) C10 0.039(2) 0.0266(18) 0.0241(17) -0.0054(15) -0.0019(15) 0.0012(16) N1 0.0369(16) 0.0248(15) 0.0237(15) -0.0054(12) -0.0044(12) 0.0056(12) N2 0.0384(17) 0.0269(15) 0.0248(15) -0.0062(12) -0.0034(13) 0.0013(13) N3 0.0291(15) 0.0257(15) 0.0212(14) -0.0039(12) -0.0013(12) 0.0009(12) N4 0.0347(16) 0.0285(16) 0.0232(15) -0.0033(12) -0.0046(12) 0.0021(13) O1 0.0507(15) 0.0320(13) 0.0220(12) -0.0068(11) -0.0060(11) 0.0131(11) O2 0.0598(17) 0.0354(14) 0.0321(14) -0.0159(12) -0.0059(12) 0.0123(12) O3 0.0502(15) 0.0356(14) 0.0206(12) -0.0057(11) -0.0047(11) 0.0160(12) O4 0.0612(18) 0.0347(14) 0.0281(13) -0.0076(11) 0.0030(12) 0.0175(13) O5 0.0412(17) 0.0312(17) 0.067(2) -0.0134(15) -0.0006(15) 0.0043(14) O6 0.066(2) 0.0310(16) 0.0349(15) -0.0131(13) 0.0113(14) -0.0015(15) O7 0.088(2) 0.0366(17) 0.0394(18) -0.0149(15) 0.0049(18) -0.0016(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O3 1.935(2) . ? Cu O1 1.954(2) . ? Cu N3 1.977(3) . ? Cu N1 1.984(3) . ? Cu O5 2.198(3) . ? Cd O6 2.260(3) . ? Cd N4 2.424(3) 1_464 ? Cd N2 2.450(3) . ? Cd Cl2 2.5126(10) . ? Cd Cl1 2.5758(9) . ? Cd Cl1 2.6722(9) 2_575 ? Cl1 Cd 2.6722(9) 2_575 ? C1 N1 1.336(4) . ? C1 C2 1.370(4) . ? C1 C5 1.516(4) . ? C2 N2 1.340(4) . ? C3 N2 1.324(4) . ? C3 C4 1.384(4) . ? C4 N1 1.320(4) . ? C5 O2 1.228(4) . ? C5 O1 1.256(4) . ? C6 N3 1.331(4) . ? C6 C7 1.368(4) . ? C6 C10 1.514(4) . ? C7 N4 1.352(4) . ? C8 N4 1.321(4) . ? C8 C9 1.378(4) . ? C9 N3 1.327(4) . ? C10 O4 1.219(4) . ? C10 O3 1.267(4) . ? N4 Cd 2.424(3) 1_646 ? 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 Cu O1 167.44(11) . . ? O3 Cu N3 83.12(10) . . ? O1 Cu N3 93.97(10) . . ? O3 Cu N1 97.35(10) . . ? O1 Cu N1 83.25(10) . . ? N3 Cu N1 169.27(11) . . ? O3 Cu O5 95.92(11) . . ? O1 Cu O5 96.52(11) . . ? N3 Cu O5 95.60(11) . . ? N1 Cu O5 95.02(11) . . ? O6 Cd N4 87.65(10) . 1_464 ? O6 Cd N2 86.57(10) . . ? N4 Cd N2 173.82(9) 1_464 . ? O6 Cd Cl2 100.37(9) . . ? N4 Cd Cl2 89.27(7) 1_464 . ? N2 Cd Cl2 89.64(7) . . ? O6 Cd Cl1 162.40(8) . . ? N4 Cd Cl1 93.65(7) 1_464 . ? N2 Cd Cl1 92.52(7) . . ? Cl2 Cd Cl1 97.20(3) . . ? O6 Cd Cl1 80.37(8) . 2_575 ? N4 Cd Cl1 82.80(7) 1_464 2_575 ? N2 Cd Cl1 98.36(7) . 2_575 ? Cl2 Cd Cl1 172.00(3) . 2_575 ? Cl1 Cd Cl1 82.38(3) . 2_575 ? Cd Cl1 Cd 97.62(3) . 2_575 ? N1 C1 C2 121.1(3) . . ? N1 C1 C5 114.4(3) . . ? C2 C1 C5 124.5(3) . . ? N2 C2 C1 121.5(3) . . ? N2 C3 C4 122.3(3) . . ? N1 C4 C3 120.5(3) . . ? O2 C5 O1 125.6(3) . . ? O2 C5 C1 118.6(3) . . ? O1 C5 C1 115.7(3) . . ? N3 C6 C7 120.7(3) . . ? N3 C6 C10 114.3(3) . . ? C7 C6 C10 124.9(3) . . ? N4 C7 C6 120.8(3) . . ? N4 C8 C9 121.9(3) . . ? N3 C9 C8 120.1(3) . . ? O4 C10 O3 125.5(3) . . ? O4 C10 C6 119.6(3) . . ? O3 C10 C6 114.9(3) . . ? C4 N1 C1 118.0(3) . . ? C4 N1 Cu 130.5(2) . . ? C1 N1 Cu 111.3(2) . . ? C3 N2 C2 116.6(3) . . ? C3 N2 Cd 122.6(2) . . ? C2 N2 Cd 119.7(2) . . ? C9 N3 C6 119.0(3) . . ? C9 N3 Cu 129.0(2) . . ? C6 N3 Cu 112.0(2) . . ? C8 N4 C7 117.5(3) . . ? C8 N4 Cd 120.1(2) . 1_646 ? C7 N4 Cd 122.2(2) . 1_646 ? C5 O1 Cu 114.8(2) . . ? C10 O3 Cu 115.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cd Cl1 Cd 11.5(3) . . . 2_575 ? N4 Cd Cl1 Cd -82.22(7) 1_464 . . 2_575 ? N2 Cd Cl1 Cd 98.10(7) . . . 2_575 ? Cl2 Cd Cl1 Cd -171.94(3) . . . 2_575 ? Cl1 Cd Cl1 Cd 0.0 2_575 . . 2_575 ? N1 C1 C2 N2 -2.7(5) . . . . ? C5 C1 C2 N2 177.2(3) . . . . ? N2 C3 C4 N1 -1.8(6) . . . . ? N1 C1 C5 O2 173.8(3) . . . . ? C2 C1 C5 O2 -6.2(5) . . . . ? N1 C1 C5 O1 -5.3(4) . . . . ? C2 C1 C5 O1 174.8(3) . . . . ? N3 C6 C7 N4 -0.8(5) . . . . ? C10 C6 C7 N4 177.4(3) . . . . ? N4 C8 C9 N3 -1.1(5) . . . . ? N3 C6 C10 O4 177.7(3) . . . . ? C7 C6 C10 O4 -0.5(5) . . . . ? N3 C6 C10 O3 -1.7(4) . . . . ? C7 C6 C10 O3 -180.0(3) . . . . ? C3 C4 N1 C1 0.0(5) . . . . ? C3 C4 N1 Cu 173.5(3) . . . . ? C2 C1 N1 C4 2.2(5) . . . . ? C5 C1 N1 C4 -177.7(3) . . . . ? C2 C1 N1 Cu -172.6(3) . . . . ? C5 C1 N1 Cu 7.5(4) . . . . ? O3 Cu N1 C4 12.7(3) . . . . ? O1 Cu N1 C4 -179.9(3) . . . . ? N3 Cu N1 C4 104.5(6) . . . . ? O5 Cu N1 C4 -83.9(3) . . . . ? O3 Cu N1 C1 -173.4(2) . . . . ? O1 Cu N1 C1 -6.0(2) . . . . ? N3 Cu N1 C1 -81.6(6) . . . . ? O5 Cu N1 C1 90.0(2) . . . . ? C4 C3 N2 C2 1.4(5) . . . . ? C4 C3 N2 Cd -166.5(3) . . . . ? C1 C2 N2 C3 0.8(5) . . . . ? C1 C2 N2 Cd 169.1(2) . . . . ? O6 Cd N2 C3 -14.7(3) . . . . ? N4 Cd N2 C3 5.9(10) 1_464 . . . ? Cl2 Cd N2 C3 85.7(3) . . . . ? Cl1 Cd N2 C3 -177.1(3) . . . . ? Cl1 Cd N2 C3 -94.5(3) 2_575 . . . ? O6 Cd N2 C2 177.7(3) . . . . ? N4 Cd N2 C2 -161.6(8) 1_464 . . . ? Cl2 Cd N2 C2 -81.9(2) . . . . ? Cl1 Cd N2 C2 15.3(2) . . . . ? Cl1 Cd N2 C2 98.0(2) 2_575 . . . ? C8 C9 N3 C6 1.6(5) . . . . ? C8 C9 N3 Cu -179.0(2) . . . . ? C7 C6 N3 C9 -0.7(5) . . . . ? C10 C6 N3 C9 -179.0(3) . . . . ? C7 C6 N3 Cu 179.8(3) . . . . ? C10 C6 N3 Cu 1.4(4) . . . . ? O3 Cu N3 C9 179.8(3) . . . . ? O1 Cu N3 C9 12.1(3) . . . . ? N1 Cu N3 C9 86.6(7) . . . . ? O5 Cu N3 C9 -84.9(3) . . . . ? O3 Cu N3 C6 -0.7(2) . . . . ? O1 Cu N3 C6 -168.5(2) . . . . ? N1 Cu N3 C6 -93.9(6) . . . . ? O5 Cu N3 C6 94.6(2) . . . . ? C9 C8 N4 C7 -0.4(5) . . . . ? C9 C8 N4 Cd 174.0(2) . . . 1_646 ? C6 C7 N4 C8 1.3(5) . . . . ? C6 C7 N4 Cd -173.0(2) . . . 1_646 ? O2 C5 O1 Cu -178.9(3) . . . . ? C1 C5 O1 Cu 0.0(4) . . . . ? O3 Cu O1 C5 96.8(4) . . . . ? N3 Cu O1 C5 172.8(2) . . . . ? N1 Cu O1 C5 3.2(2) . . . . ? O5 Cu O1 C5 -91.1(2) . . . . ? O4 C10 O3 Cu -178.3(3) . . . . ? C6 C10 O3 Cu 1.0(4) . . . . ? O1 Cu O3 C10 77.0(5) . . . . ? N3 Cu O3 C10 -0.2(3) . . . . ? N1 Cu O3 C10 169.0(3) . . . . ? O5 Cu O3 C10 -95.2(3) . . . . ? 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 O7 H7A O2 0.829(18) 2.02(2) 2.827(4) 164(4) . O5 H5A O2 0.833(18) 1.94(2) 2.755(4) 165(4) 2_566 O7 H7B Cl2 0.841(19) 2.39(3) 3.166(3) 154(5) 2_566 O5 H5B O4 0.824(18) 1.99(3) 2.735(4) 151(4) 2_656 O6 H6A O4 0.824(19) 2.10(3) 2.832(4) 147(4) 2_665 O6 H6A Cl1 0.824(19) 2.82(5) 3.198(3) 110(4) 2_575 O6 H6B O7 0.826(19) 1.85(2) 2.658(4) 165(4) 1_554 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.598 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.097 #===END data_cmpd2 _database_code_CSD 188221 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [Cu(C5H3N2O2)2 (H2O)2 Cd2 Cl4 (H2O)2] ; _chemical_formula_sum 'C10 H14 Cd2 Cl4 Cu N4 O8' _chemical_formula_weight 748.39 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 6.7082(11) _cell_length_b 8.1416(13) _cell_length_c 10.3645(17) _cell_angle_alpha 76.568(3) _cell_angle_beta 75.419(3) _cell_angle_gamma 86.280(3) _cell_volume 532.83(15) _cell_formula_units_Z 1 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 2806 _cell_measurement_theta_min 2.572 _cell_measurement_theta_max 26.400 _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 359 _exptl_absorpt_coefficient_mu 3.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7776 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4887 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.43 _reflns_number_total 2190 _reflns_number_gt 1820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(0.60(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0240P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 2190 _refine_ls_number_parameters 149 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _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 Cu Cu 0.0000 0.0000 0.5000 0.01969(17) Uani 1 2 d S . . Cd Cd 0.28607(4) 0.49119(4) 0.91442(3) 0.01752(10) Uani 1 1 d . . . Cl1 Cl 0.40589(15) 0.69474(13) 1.04165(11) 0.0231(2) Uani 1 1 d . . . Cl2 Cl 0.01970(15) 0.30668(13) 1.11826(10) 0.0206(2) Uani 1 1 d . . . C1 C -0.0010(6) 0.2556(5) 0.6370(4) 0.0159(8) Uani 1 1 d . . . C2 C 0.0476(6) 0.3552(5) 0.7173(4) 0.0177(9) Uani 1 1 d . . . H2 H -0.0263 0.4573 0.7256 0.021 Uiso 1 1 calc R . . C3 C 0.2958(6) 0.1618(5) 0.7716(4) 0.0243(10) Uani 1 1 d . . . H3 H 0.4015 0.1256 0.8181 0.029 Uiso 1 1 calc R . . C4 C 0.2452(7) 0.0620(5) 0.6927(4) 0.0257(10) Uani 1 1 d . . . H4 H 0.3155 -0.0421 0.6869 0.031 Uiso 1 1 calc R . . C5 C -0.1608(6) 0.3064(5) 0.5534(4) 0.0166(8) Uani 1 1 d . . . N1 N 0.0988(5) 0.1108(4) 0.6248(3) 0.0187(7) Uani 1 1 d . . . N2 N 0.1976(5) 0.3083(4) 0.7830(3) 0.0180(7) Uani 1 1 d . . . O1 O -0.1693(4) 0.2094(3) 0.4744(3) 0.0201(6) Uani 1 1 d . . . O2 O -0.2627(4) 0.4366(4) 0.5623(3) 0.0245(7) Uani 1 1 d . . . O3 O 0.2861(5) 0.1017(4) 0.3129(3) 0.0307(8) Uani 1 1 d D . . H3A H 0.352(6) 0.186(4) 0.310(5) 0.028(14) Uiso 1 1 d D . . H3B H 0.238(10) 0.143(8) 0.243(5) 0.10(3) Uiso 1 1 d D . . O4 O 0.4505(5) 0.6389(4) 0.6862(3) 0.0208(6) Uani 1 1 d D . . H4A H 0.525(6) 0.565(4) 0.652(4) 0.022(12) Uiso 1 1 d D . . H4B H 0.364(6) 0.665(7) 0.640(5) 0.050(17) 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 Cu 0.0223(4) 0.0178(4) 0.0268(4) -0.0119(3) -0.0150(3) 0.0049(3) Cd 0.01534(16) 0.02145(17) 0.01920(16) -0.00800(12) -0.00748(12) 0.00076(12) Cl1 0.0194(5) 0.0259(6) 0.0309(6) -0.0141(5) -0.0128(5) 0.0038(4) Cl2 0.0174(5) 0.0221(5) 0.0216(5) -0.0029(4) -0.0061(4) 0.0024(4) C1 0.014(2) 0.017(2) 0.018(2) -0.0057(17) -0.0032(16) -0.0013(16) C2 0.015(2) 0.021(2) 0.018(2) -0.0073(17) -0.0028(17) 0.0003(16) C3 0.023(2) 0.024(2) 0.033(2) -0.010(2) -0.018(2) 0.0054(19) C4 0.027(2) 0.022(2) 0.037(3) -0.015(2) -0.019(2) 0.0072(19) C5 0.016(2) 0.021(2) 0.0133(19) -0.0044(17) -0.0042(16) 0.0001(17) N1 0.0189(18) 0.0191(18) 0.0210(18) -0.0074(15) -0.0072(15) -0.0004(15) N2 0.0155(18) 0.0214(18) 0.0194(18) -0.0050(15) -0.0074(14) -0.0021(14) O1 0.0239(16) 0.0180(15) 0.0247(15) -0.0098(13) -0.0144(13) 0.0062(12) O2 0.0257(16) 0.0253(17) 0.0274(17) -0.0131(14) -0.0119(13) 0.0132(13) O3 0.0282(18) 0.030(2) 0.0335(19) 0.0013(16) -0.0128(15) -0.0056(15) O4 0.0214(16) 0.0221(16) 0.0221(16) -0.0094(13) -0.0086(13) 0.0046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O1 1.989(3) . ? Cu O1 1.989(3) 2_556 ? Cu N1 1.994(3) . ? Cu N1 1.994(3) 2_556 ? Cu O3 2.391(3) 2_556 ? Cu O3 2.391(3) . ? Cd O4 2.407(3) . ? Cd N2 2.427(3) . ? Cd Cl1 2.5528(11) 2_667 ? Cd Cl2 2.5851(11) 2_567 ? Cd Cl1 2.6179(10) . ? Cd Cl2 2.6241(11) . ? Cl1 Cd 2.5528(11) 2_667 ? Cl2 Cd 2.5851(11) 2_567 ? C1 N1 1.334(5) . ? C1 C2 1.393(5) . ? C1 C5 1.521(5) . ? C2 N2 1.340(5) . ? C3 N2 1.340(5) . ? C3 C4 1.388(5) . ? C4 N1 1.336(5) . ? C5 O2 1.232(5) . ? C5 O1 1.276(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 O1 Cu O1 180.00(16) . 2_556 ? O1 Cu N1 82.89(12) . . ? O1 Cu N1 97.11(12) 2_556 . ? O1 Cu N1 97.11(12) . 2_556 ? O1 Cu N1 82.89(12) 2_556 2_556 ? N1 Cu N1 180.0 . 2_556 ? O1 Cu O3 84.03(11) . 2_556 ? O1 Cu O3 95.97(11) 2_556 2_556 ? N1 Cu O3 87.63(13) . 2_556 ? N1 Cu O3 92.37(13) 2_556 2_556 ? O1 Cu O3 95.97(11) . . ? O1 Cu O3 84.03(11) 2_556 . ? N1 Cu O3 92.37(13) . . ? N1 Cu O3 87.63(13) 2_556 . ? O3 Cu O3 180.0 2_556 . ? O4 Cd N2 79.78(10) . . ? O4 Cd Cl1 96.63(8) . 2_667 ? N2 Cd Cl1 91.75(8) . 2_667 ? O4 Cd Cl2 84.44(8) . 2_567 ? N2 Cd Cl2 92.62(8) . 2_567 ? Cl1 Cd Cl2 175.63(3) 2_667 2_567 ? O4 Cd Cl1 96.49(7) . . ? N2 Cd Cl1 175.78(8) . . ? Cl1 Cd Cl1 86.69(3) 2_667 . ? Cl2 Cd Cl1 88.97(3) 2_567 . ? O4 Cd Cl2 160.53(7) . . ? N2 Cd Cl2 83.77(8) . . ? Cl1 Cd Cl2 94.19(4) 2_667 . ? Cl2 Cd Cl2 86.00(4) 2_567 . ? Cl1 Cd Cl2 100.25(3) . . ? Cd Cl1 Cd 93.31(3) 2_667 . ? Cd Cl2 Cd 94.00(3) 2_567 . ? N1 C1 C2 120.9(3) . . ? N1 C1 C5 115.8(3) . . ? C2 C1 C5 123.2(3) . . ? N2 C2 C1 120.6(4) . . ? N2 C3 C4 121.0(4) . . ? N1 C4 C3 120.8(4) . . ? O2 C5 O1 125.9(4) . . ? O2 C5 C1 119.4(3) . . ? O1 C5 C1 114.7(3) . . ? C1 N1 C4 118.5(3) . . ? C1 N1 Cu 111.6(3) . . ? C4 N1 Cu 129.9(3) . . ? C3 N2 C2 118.2(3) . . ? C3 N2 Cd 122.3(3) . . ? C2 N2 Cd 119.5(3) . . ? C5 O1 Cu 114.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cd Cl1 Cd -96.30(8) . . . 2_667 ? N2 Cd Cl1 Cd -68.4(11) . . . 2_667 ? Cl1 Cd Cl1 Cd 0.0 2_667 . . 2_667 ? Cl2 Cd Cl1 Cd 179.41(4) 2_567 . . 2_667 ? Cl2 Cd Cl1 Cd 93.67(4) . . . 2_667 ? O4 Cd Cl2 Cd -60.7(2) . . . 2_567 ? N2 Cd Cl2 Cd -93.08(8) . . . 2_567 ? Cl1 Cd Cl2 Cd 175.62(3) 2_667 . . 2_567 ? Cl2 Cd Cl2 Cd 0.0 2_567 . . 2_567 ? Cl1 Cd Cl2 Cd 88.23(3) . . . 2_567 ? N1 C1 C2 N2 0.7(6) . . . . ? C5 C1 C2 N2 -176.4(3) . . . . ? N2 C3 C4 N1 0.8(7) . . . . ? N1 C1 C5 O2 178.2(4) . . . . ? C2 C1 C5 O2 -4.5(6) . . . . ? N1 C1 C5 O1 -4.7(5) . . . . ? C2 C1 C5 O1 172.6(4) . . . . ? C2 C1 N1 C4 0.8(6) . . . . ? C5 C1 N1 C4 178.1(4) . . . . ? C2 C1 N1 Cu -178.6(3) . . . . ? C5 C1 N1 Cu -1.3(4) . . . . ? C3 C4 N1 C1 -1.5(6) . . . . ? C3 C4 N1 Cu 177.7(3) . . . . ? O1 Cu N1 C1 4.2(3) . . . . ? O1 Cu N1 C1 -175.8(3) 2_556 . . . ? N1 Cu N1 C1 134(100) 2_556 . . . ? O3 Cu N1 C1 -80.0(3) 2_556 . . . ? O3 Cu N1 C1 100.0(3) . . . . ? O1 Cu N1 C4 -175.0(4) . . . . ? O1 Cu N1 C4 5.0(4) 2_556 . . . ? N1 Cu N1 C4 -45(100) 2_556 . . . ? O3 Cu N1 C4 100.7(4) 2_556 . . . ? O3 Cu N1 C4 -79.3(4) . . . . ? C4 C3 N2 C2 0.7(6) . . . . ? C4 C3 N2 Cd -178.3(3) . . . . ? C1 C2 N2 C3 -1.4(6) . . . . ? C1 C2 N2 Cd 177.6(3) . . . . ? O4 Cd N2 C3 102.3(3) . . . . ? Cl1 Cd N2 C3 5.9(3) 2_667 . . . ? Cl2 Cd N2 C3 -173.8(3) 2_567 . . . ? Cl1 Cd N2 C3 74.1(12) . . . . ? Cl2 Cd N2 C3 -88.2(3) . . . . ? O4 Cd N2 C2 -76.7(3) . . . . ? Cl1 Cd N2 C2 -173.1(3) 2_667 . . . ? Cl2 Cd N2 C2 7.2(3) 2_567 . . . ? Cl1 Cd N2 C2 -104.9(11) . . . . ? Cl2 Cd N2 C2 92.9(3) . . . . ? O2 C5 O1 Cu -174.9(3) . . . . ? C1 C5 O1 Cu 8.2(4) . . . . ? O1 Cu O1 C5 -123(100) 2_556 . . . ? N1 Cu O1 C5 -7.1(3) . . . . ? N1 Cu O1 C5 172.9(3) 2_556 . . . ? O3 Cu O1 C5 81.2(3) 2_556 . . . ? O3 Cu O1 C5 -98.8(3) . . . . ? 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 O3 H3A O4 0.830(19) 2.02(2) 2.843(4) 169(5) 2_666 O3 H3B Cl2 0.86(2) 2.34(3) 3.148(4) 157(6) 1_554 O4 H4A O2 0.844(19) 1.89(2) 2.718(4) 167(4) 1_655 O4 H4B O1 0.831(19) 2.05(2) 2.860(4) 165(5) 2_566 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.849 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.125 #===END data_3 _database_code_CSD 188222 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Cd2 Cl4 Cu N4 O10' _chemical_formula_weight 784.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 6.5901(6) _cell_length_b 9.2936(8) _cell_length_c 19.4373(17) _cell_angle_alpha 82.778(2) _cell_angle_beta 86.121(2) _cell_angle_gamma 72.191(2) _cell_volume 1123.88(17) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 5442 _cell_measurement_theta_min 2.316 _cell_measurement_theta_max 26.371 _exptl_crystal_description bar _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 3.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6233 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10342 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4592 _reflns_number_gt 3510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^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 4592 _refine_ls_number_parameters 322 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.53653(9) 0.96771(6) 0.75681(3) 0.02149(14) Uani 1 1 d . . . Cd1 Cd 0.79016(5) 1.40084(3) 0.996425(16) 0.01615(8) Uani 1 1 d . . . Cd2 Cd 0.21129(5) 0.60206(3) 0.503481(16) 0.01705(8) Uani 1 1 d . . . Cl1 Cl 0.89621(16) 1.55565(12) 1.08278(5) 0.0205(2) Uani 1 1 d . . . Cl2 Cl 0.47398(16) 1.36968(11) 1.07416(5) 0.0195(2) Uani 1 1 d . . . Cl3 Cl 0.11168(16) 0.43509(12) 0.42107(5) 0.0209(2) Uani 1 1 d . . . Cl4 Cl 0.52875(16) 0.63246(12) 0.42587(5) 0.0213(2) Uani 1 1 d . . . C1 C 0.5287(6) 1.0962(4) 0.8776(2) 0.0159(9) Uani 1 1 d . . . C2 C 0.5735(6) 1.1766(4) 0.9269(2) 0.0166(9) Uani 1 1 d . . . H2 H 0.4917 1.1861 0.9691 0.020 Uiso 1 1 calc R . . C3 C 0.8428(7) 1.2226(5) 0.8564(2) 0.0200(10) Uani 1 1 d . . . H3 H 0.9561 1.2664 0.8477 0.024 Uiso 1 1 calc R . . C4 C 0.8003(7) 1.1418(5) 0.8067(2) 0.0213(10) Uani 1 1 d . . . H4 H 0.8845 1.1299 0.7650 0.026 Uiso 1 1 calc R . . C5 C 0.3508(6) 1.0232(4) 0.8846(2) 0.0172(9) Uani 1 1 d . . . C6 C 0.4905(6) 0.8872(4) 0.6283(2) 0.0162(9) Uani 1 1 d . . . C7 C 0.4267(6) 0.8237(4) 0.5763(2) 0.0174(9) Uani 1 1 d . . . H7 H 0.4892 0.8315 0.5310 0.021 Uiso 1 1 calc R . . C8 C 0.1910(6) 0.7477(5) 0.6521(2) 0.0221(10) Uani 1 1 d . . . H8 H 0.0836 0.6987 0.6619 0.027 Uiso 1 1 calc R . . C9 C 0.2509(7) 0.8128(5) 0.7044(2) 0.0225(10) Uani 1 1 d . . . H9 H 0.1830 0.8097 0.7490 0.027 Uiso 1 1 calc R . . C10 C 0.6639(6) 0.9630(5) 0.6197(2) 0.0188(9) Uani 1 1 d . . . N1 N 0.6404(5) 1.0808(4) 0.81785(18) 0.0178(8) Uani 1 1 d . . . N2 N 0.7302(5) 1.2409(4) 0.91587(17) 0.0168(8) Uani 1 1 d . . . N3 N 0.4034(5) 0.8798(4) 0.69229(18) 0.0185(8) Uani 1 1 d . . . N4 N 0.2788(5) 0.7513(4) 0.58830(18) 0.0181(8) Uani 1 1 d . . . O1 O 0.3252(4) 0.9654(3) 0.83131(14) 0.0199(7) Uani 1 1 d . . . O2 O 0.2428(4) 1.0243(3) 0.93908(15) 0.0209(7) Uani 1 1 d . . . O3 O 0.7078(4) 1.0075(3) 0.67504(14) 0.0219(7) Uani 1 1 d . . . O4 O 0.7543(4) 0.9769(3) 0.56254(14) 0.0206(7) Uani 1 1 d . . . O5 O 0.8122(6) 0.7525(4) 0.7927(2) 0.0363(9) Uani 1 1 d D . . H5A H 0.801(7) 0.673(3) 0.778(2) 0.014(12) Uiso 1 1 d D . . H5B H 0.811(10) 0.739(7) 0.8359(11) 0.07(2) Uiso 1 1 d D . . O6 O 1.0147(5) 1.1733(3) 1.05022(17) 0.0210(7) Uani 1 1 d D . . H6A H 1.087(6) 1.136(5) 1.0162(17) 0.031(15) Uiso 1 1 d D . . H6B H 0.939(5) 1.118(4) 1.062(2) 0.014(12) Uiso 1 1 d D . . O7 O -0.0079(5) 0.8285(3) 0.45164(17) 0.0220(7) Uani 1 1 d D . . H7A H -0.086(5) 0.862(4) 0.4852(15) 0.015(12) Uiso 1 1 d D . . H7B H 0.059(8) 0.893(5) 0.444(3) 0.07(2) Uiso 1 1 d D . . O8 O 0.7903(8) 0.4947(5) 0.7363(2) 0.0547(11) Uani 1 1 d D . . H8A H 0.654(4) 0.500(7) 0.739(3) 0.06(2) Uiso 1 1 d D . . H8B H 0.811(9) 0.502(8) 0.6920(12) 0.10(3) Uiso 1 1 d D . . O9 O 0.4095(7) 0.4622(5) 0.7782(3) 0.0665(13) Uani 1 1 d . . . H9A H 0.3331 0.4294 0.7530 0.13(4) Uiso 1 1 d R . . H9B H 0.3288 0.4911 0.8133 0.17(5) Uiso 1 1 d R . . O10 O 0.2179(9) 0.2769(6) 0.7180(3) 0.0705(14) Uani 1 1 d D . . H10A H 0.249(10) 0.241(7) 0.6793(19) 0.07(3) Uiso 1 1 d D . . H10B H 0.092(4) 0.327(6) 0.723(3) 0.046(19) 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 Cu 0.0257(3) 0.0325(3) 0.0151(3) -0.0086(2) 0.0050(2) -0.0205(3) Cd1 0.01478(16) 0.01898(17) 0.01705(17) -0.00409(13) 0.00061(13) -0.00795(13) Cd2 0.01591(16) 0.02029(17) 0.01773(18) -0.00462(13) 0.00060(13) -0.00878(13) Cl1 0.0191(5) 0.0280(6) 0.0198(6) -0.0087(5) 0.0037(4) -0.0134(5) Cl2 0.0180(5) 0.0217(5) 0.0186(6) -0.0003(4) 0.0027(4) -0.0072(5) Cl3 0.0193(5) 0.0290(6) 0.0199(6) -0.0091(5) 0.0040(4) -0.0139(5) Cl4 0.0188(5) 0.0247(6) 0.0201(6) -0.0008(5) 0.0034(4) -0.0077(5) C1 0.012(2) 0.016(2) 0.018(2) -0.0019(17) -0.0011(18) -0.0028(18) C2 0.015(2) 0.019(2) 0.016(2) -0.0028(18) 0.0010(18) -0.0041(18) C3 0.019(2) 0.024(2) 0.021(2) -0.0046(19) 0.0037(19) -0.0125(19) C4 0.022(2) 0.029(2) 0.019(2) -0.0031(19) 0.0051(19) -0.016(2) C5 0.016(2) 0.015(2) 0.021(3) -0.0016(18) -0.0017(19) -0.0040(18) C6 0.015(2) 0.017(2) 0.017(2) -0.0017(17) 0.0019(18) -0.0063(18) C7 0.018(2) 0.019(2) 0.016(2) -0.0022(18) 0.0023(18) -0.0076(19) C8 0.017(2) 0.032(3) 0.022(3) -0.008(2) 0.0038(19) -0.013(2) C9 0.027(2) 0.030(3) 0.016(2) -0.0066(19) 0.0085(19) -0.017(2) C10 0.018(2) 0.019(2) 0.020(3) 0.0008(18) 0.0010(19) -0.0085(19) N1 0.0197(18) 0.0197(19) 0.017(2) -0.0031(15) 0.0025(15) -0.0098(16) N2 0.0156(18) 0.0202(19) 0.015(2) -0.0012(15) -0.0031(15) -0.0060(15) N3 0.0193(18) 0.0237(19) 0.016(2) -0.0076(15) 0.0031(15) -0.0107(16) N4 0.0193(19) 0.0183(19) 0.018(2) -0.0032(15) -0.0013(16) -0.0069(16) O1 0.0220(16) 0.0308(17) 0.0133(16) -0.0060(13) 0.0040(13) -0.0171(14) O2 0.0215(16) 0.0254(17) 0.0174(17) -0.0039(13) 0.0056(13) -0.0103(14) O3 0.0264(17) 0.0326(17) 0.0147(16) -0.0059(13) 0.0034(13) -0.0203(15) O4 0.0259(16) 0.0241(16) 0.0152(16) -0.0032(13) 0.0042(13) -0.0134(14) O5 0.040(2) 0.035(2) 0.031(2) 0.0023(18) 0.0048(18) -0.0095(18) O6 0.0199(17) 0.0240(18) 0.0196(19) -0.0017(14) 0.0040(14) -0.0087(15) O7 0.0228(17) 0.0238(17) 0.0211(19) -0.0039(14) 0.0045(15) -0.0100(15) O8 0.074(3) 0.059(3) 0.035(3) 0.000(2) 0.012(2) -0.031(3) O9 0.069(3) 0.075(3) 0.042(3) 0.000(2) 0.028(3) -0.010(3) O10 0.070(4) 0.073(4) 0.054(4) 0.016(3) 0.017(3) -0.014(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 Cu O1 1.943(3) . ? Cu O3 1.950(3) . ? Cu N1 1.961(3) . ? Cu N3 1.963(3) . ? Cu O5 2.321(4) . ? Cd1 O6 2.344(3) . ? Cd1 N2 2.418(3) . ? Cd1 Cl2 2.5576(10) . ? Cd1 Cl1 2.5941(11) 2_787 ? Cd1 Cl1 2.5993(11) . ? Cd1 Cl2 2.6033(10) 2_687 ? Cd2 O7 2.310(3) . ? Cd2 N4 2.428(3) . ? Cd2 Cl4 2.5613(11) . ? Cd2 Cl3 2.5884(11) 2_566 ? Cd2 Cl3 2.6068(11) . ? Cd2 Cl4 2.6178(11) 2_666 ? Cl1 Cd1 2.5941(11) 2_787 ? Cl2 Cd1 2.6033(10) 2_687 ? Cl3 Cd2 2.5884(11) 2_566 ? Cl4 Cd2 2.6178(11) 2_666 ? C1 N1 1.332(5) . ? C1 C2 1.384(5) . ? C1 C5 1.515(5) . ? C2 N2 1.336(5) . ? C3 N2 1.331(5) . ? C3 C4 1.386(6) . ? C4 N1 1.334(5) . ? C5 O2 1.235(5) . ? C5 O1 1.268(5) . ? C6 N3 1.337(5) . ? C6 C7 1.381(5) . ? C6 C10 1.506(5) . ? C7 N4 1.337(5) . ? C8 N4 1.333(5) . ? C8 C9 1.382(6) . ? C9 N3 1.329(5) . ? C10 O4 1.236(5) . ? C10 O3 1.280(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu O3 168.67(12) . . ? O1 Cu N1 83.47(13) . . ? O3 Cu N1 96.34(13) . . ? O1 Cu N3 95.06(13) . . ? O3 Cu N3 83.64(13) . . ? N1 Cu N3 172.45(13) . . ? O1 Cu O5 101.39(13) . . ? O3 Cu O5 89.92(13) . . ? N1 Cu O5 88.65(14) . . ? N3 Cu O5 98.89(14) . . ? O6 Cd1 N2 84.53(11) . . ? O6 Cd1 Cl2 91.06(8) . . ? N2 Cd1 Cl2 91.62(8) . . ? O6 Cd1 Cl1 90.99(8) . 2_787 ? N2 Cd1 Cl1 89.68(8) . 2_787 ? Cl2 Cd1 Cl1 177.67(3) . 2_787 ? O6 Cd1 Cl1 90.87(8) . . ? N2 Cd1 Cl1 174.00(8) . . ? Cl2 Cd1 Cl1 92.32(3) . . ? Cl1 Cd1 Cl1 86.54(3) 2_787 . ? O6 Cd1 Cl2 172.14(8) . 2_687 ? N2 Cd1 Cl2 87.67(8) . 2_687 ? Cl2 Cd1 Cl2 88.26(3) . 2_687 ? Cl1 Cd1 Cl2 89.86(3) 2_787 2_687 ? Cl1 Cd1 Cl2 96.97(3) . 2_687 ? O7 Cd2 N4 86.33(11) . . ? O7 Cd2 Cl4 91.11(9) . . ? N4 Cd2 Cl4 92.35(9) . . ? O7 Cd2 Cl3 89.18(9) . 2_566 ? N4 Cd2 Cl3 89.70(9) . 2_566 ? Cl4 Cd2 Cl3 177.95(4) . 2_566 ? O7 Cd2 Cl3 94.45(8) . . ? N4 Cd2 Cl3 174.43(9) . . ? Cl4 Cd2 Cl3 93.15(3) . . ? Cl3 Cd2 Cl3 84.80(3) 2_566 . ? O7 Cd2 Cl4 172.24(8) . 2_666 ? N4 Cd2 Cl4 85.91(8) . 2_666 ? Cl4 Cd2 Cl4 88.87(3) . 2_666 ? Cl3 Cd2 Cl4 91.11(3) 2_566 2_666 ? Cl3 Cd2 Cl4 93.30(3) . 2_666 ? Cd1 Cl1 Cd1 93.46(3) 2_787 . ? Cd1 Cl2 Cd1 91.74(3) . 2_687 ? Cd2 Cl3 Cd2 95.20(3) 2_566 . ? Cd2 Cl4 Cd2 91.13(3) . 2_666 ? N1 C1 C2 121.0(4) . . ? N1 C1 C5 114.3(4) . . ? C2 C1 C5 124.7(4) . . ? N2 C2 C1 120.9(4) . . ? N2 C3 C4 122.2(4) . . ? N1 C4 C3 119.7(4) . . ? O2 C5 O1 125.1(4) . . ? O2 C5 C1 120.0(4) . . ? O1 C5 C1 114.9(4) . . ? N3 C6 C7 120.7(4) . . ? N3 C6 C10 114.8(4) . . ? C7 C6 C10 124.4(4) . . ? N4 C7 C6 121.3(4) . . ? N4 C8 C9 122.3(4) . . ? N3 C9 C8 120.0(4) . . ? O4 C10 O3 124.7(4) . . ? O4 C10 C6 120.3(4) . . ? O3 C10 C6 115.0(4) . . ? C1 N1 C4 118.7(4) . . ? C1 N1 Cu 112.2(3) . . ? C4 N1 Cu 129.1(3) . . ? C3 N2 C2 117.5(3) . . ? C3 N2 Cd1 120.9(3) . . ? C2 N2 Cd1 121.4(3) . . ? C9 N3 C6 118.6(4) . . ? C9 N3 Cu 129.5(3) . . ? C6 N3 Cu 111.9(3) . . ? C8 N4 C7 117.0(4) . . ? C8 N4 Cd2 121.1(3) . . ? C7 N4 Cd2 121.3(3) . . ? C5 O1 Cu 114.9(3) . . ? C10 O3 Cu 114.6(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 O6 Cd1 Cl1 Cd1 90.94(8) . . . 2_787 ? N2 Cd1 Cl1 Cd1 51.1(8) . . . 2_787 ? Cl2 Cd1 Cl1 Cd1 -177.97(4) . . . 2_787 ? Cl1 Cd1 Cl1 Cd1 0.0 2_787 . . 2_787 ? Cl2 Cd1 Cl1 Cd1 -89.44(3) 2_687 . . 2_787 ? O6 Cd1 Cl2 Cd1 -172.17(8) . . . 2_687 ? N2 Cd1 Cl2 Cd1 -87.62(8) . . . 2_687 ? Cl1 Cd1 Cl2 Cd1 36.3(9) 2_787 . . 2_687 ? Cl1 Cd1 Cl2 Cd1 96.91(3) . . . 2_687 ? Cl2 Cd1 Cl2 Cd1 0.0 2_687 . . 2_687 ? O7 Cd2 Cl3 Cd2 -88.77(9) . . . 2_566 ? N4 Cd2 Cl3 Cd2 9.0(8) . . . 2_566 ? Cl4 Cd2 Cl3 Cd2 179.87(4) . . . 2_566 ? Cl3 Cd2 Cl3 Cd2 0.0 2_566 . . 2_566 ? Cl4 Cd2 Cl3 Cd2 90.81(4) 2_666 . . 2_566 ? O7 Cd2 Cl4 Cd2 172.24(8) . . . 2_666 ? N4 Cd2 Cl4 Cd2 85.86(8) . . . 2_666 ? Cl3 Cd2 Cl4 Cd2 -89.5(10) 2_566 . . 2_666 ? Cl3 Cd2 Cl4 Cd2 -93.25(3) . . . 2_666 ? Cl4 Cd2 Cl4 Cd2 0.0 2_666 . . 2_666 ? N1 C1 C2 N2 -0.1(6) . . . . ? C5 C1 C2 N2 -178.2(3) . . . . ? N2 C3 C4 N1 0.6(6) . . . . ? N1 C1 C5 O2 176.7(3) . . . . ? C2 C1 C5 O2 -5.0(6) . . . . ? N1 C1 C5 O1 -3.8(5) . . . . ? C2 C1 C5 O1 174.5(4) . . . . ? N3 C6 C7 N4 -0.9(6) . . . . ? C10 C6 C7 N4 176.7(4) . . . . ? N4 C8 C9 N3 -1.2(6) . . . . ? N3 C6 C10 O4 -179.5(4) . . . . ? C7 C6 C10 O4 2.8(6) . . . . ? N3 C6 C10 O3 1.4(5) . . . . ? C7 C6 C10 O3 -176.3(4) . . . . ? C2 C1 N1 C4 1.4(6) . . . . ? C5 C1 N1 C4 179.8(3) . . . . ? C2 C1 N1 Cu -178.1(3) . . . . ? C5 C1 N1 Cu 0.3(4) . . . . ? C3 C4 N1 C1 -1.7(6) . . . . ? C3 C4 N1 Cu 177.7(3) . . . . ? O1 Cu N1 C1 1.9(3) . . . . ? O3 Cu N1 C1 170.5(3) . . . . ? N3 Cu N1 C1 81.1(12) . . . . ? O5 Cu N1 C1 -99.7(3) . . . . ? O1 Cu N1 C4 -177.5(4) . . . . ? O3 Cu N1 C4 -8.9(4) . . . . ? N3 Cu N1 C4 -98.4(12) . . . . ? O5 Cu N1 C4 80.9(4) . . . . ? C4 C3 N2 C2 0.7(6) . . . . ? C4 C3 N2 Cd1 -174.6(3) . . . . ? C1 C2 N2 C3 -1.0(5) . . . . ? C1 C2 N2 Cd1 174.3(3) . . . . ? O6 Cd1 N2 C3 -95.2(3) . . . . ? Cl2 Cd1 N2 C3 173.9(3) . . . . ? Cl1 Cd1 N2 C3 -4.1(3) 2_787 . . . ? Cl1 Cd1 N2 C3 -55.1(9) . . . . ? Cl2 Cd1 N2 C3 85.7(3) 2_687 . . . ? O6 Cd1 N2 C2 89.7(3) . . . . ? Cl2 Cd1 N2 C2 -1.2(3) . . . . ? Cl1 Cd1 N2 C2 -179.3(3) 2_787 . . . ? Cl1 Cd1 N2 C2 129.8(7) . . . . ? Cl2 Cd1 N2 C2 -89.4(3) 2_687 . . . ? C8 C9 N3 C6 2.4(6) . . . . ? C8 C9 N3 Cu -175.0(3) . . . . ? C7 C6 N3 C9 -1.4(6) . . . . ? C10 C6 N3 C9 -179.2(3) . . . . ? C7 C6 N3 Cu 176.4(3) . . . . ? C10 C6 N3 Cu -1.4(4) . . . . ? O1 Cu N3 C9 -12.9(4) . . . . ? O3 Cu N3 C9 178.4(4) . . . . ? N1 Cu N3 C9 -91.3(12) . . . . ? O5 Cu N3 C9 89.4(4) . . . . ? O1 Cu N3 C6 169.6(3) . . . . ? O3 Cu N3 C6 0.9(3) . . . . ? N1 Cu N3 C6 91.2(12) . . . . ? O5 Cu N3 C6 -88.1(3) . . . . ? C9 C8 N4 C7 -1.1(6) . . . . ? C9 C8 N4 Cd2 170.1(3) . . . . ? C6 C7 N4 C8 2.1(6) . . . . ? C6 C7 N4 Cd2 -169.0(3) . . . . ? O7 Cd2 N4 C8 105.3(3) . . . . ? Cl4 Cd2 N4 C8 -163.8(3) . . . . ? Cl3 Cd2 N4 C8 16.1(3) 2_566 . . . ? Cl3 Cd2 N4 C8 7.1(10) . . . . ? Cl4 Cd2 N4 C8 -75.1(3) 2_666 . . . ? O7 Cd2 N4 C7 -83.9(3) . . . . ? Cl4 Cd2 N4 C7 7.1(3) . . . . ? Cl3 Cd2 N4 C7 -173.1(3) 2_566 . . . ? Cl3 Cd2 N4 C7 177.9(7) . . . . ? Cl4 Cd2 N4 C7 95.8(3) 2_666 . . . ? O2 C5 O1 Cu -175.1(3) . . . . ? C1 C5 O1 Cu 5.4(4) . . . . ? O3 Cu O1 C5 -94.0(7) . . . . ? N1 Cu O1 C5 -4.3(3) . . . . ? N3 Cu O1 C5 -176.8(3) . . . . ? O5 Cu O1 C5 83.0(3) . . . . ? O4 C10 O3 Cu -179.7(3) . . . . ? C6 C10 O3 Cu -0.6(4) . . . . ? O1 Cu O3 C10 -84.1(7) . . . . ? N1 Cu O3 C10 -172.5(3) . . . . ? N3 Cu O3 C10 -0.1(3) . . . . ? O5 Cu O3 C10 98.9(3) . . . . ? 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 O5 H5A O8 0.847(18) 1.96(2) 2.803(6) 174(4) . O8 H8A O9 0.881(19) 1.85(3) 2.680(7) 156(5) . O9 H9A O10 0.87 2.01 2.822(8) 156.9 . O5 H5B Cl2 0.83(2) 2.80(5) 3.384(4) 128(5) 2_677 O6 H6B O2 0.822(19) 2.04(2) 2.839(4) 162(4) 2_677 O9 H9B Cl1 0.85 2.50 3.277(4) 152.3 2_677 O6 H6A O2 0.836(19) 1.98(2) 2.808(4) 172(5) 1_655 O7 H7A O4 0.835(19) 2.00(2) 2.824(4) 168(4) 1_455 O10 H10B O8 0.825(19) 2.14(2) 2.953(7) 168(5) 1_455 O7 H7B O4 0.84(2) 1.96(2) 2.793(4) 170(6) 2_676 O8 H8B Cl3 0.859(19) 2.27(2) 3.112(4) 168(6) 2_666 O10 H10A Cl4 0.85(2) 2.78(6) 3.310(5) 121(5) 2_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.833 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.121 #===END data_4 _database_code_CSD 188223 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; Cu(C5H3N2O2)2(CdCl2)2 ; _chemical_formula_sum 'C10 H6 Cd2 Cl4 Cu N4 O4' _chemical_formula_weight 676.33 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.2485(11) _cell_length_b 9.0948(7) _cell_length_c 13.5787(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.0960(10) _cell_angle_gamma 90.00 _cell_volume 1841.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5557 _cell_measurement_theta_min 2.624 _cell_measurement_theta_max 28.300 _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 4.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4775 _exptl_absorpt_correction_T_max 0.6471 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8027 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2281 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.624 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^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 2281 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Cu Cu 0.2500 0.7500 0.5000 0.02376(11) Uani 1 2 d S . . Cd Cd 0.053557(14) 0.08602(2) 0.635349(14) 0.02378(7) Uani 1 1 d . . . Cl1 Cl -0.09193(5) 0.10951(8) 0.48911(5) 0.03241(16) Uani 1 1 d . . . Cl2 Cl 0.0000 0.28423(10) 0.7500 0.0278(2) Uani 1 2 d S . . Cl3 Cl 0.0000 -0.10871(10) 0.7500 0.0380(3) Uani 1 2 d S . . C1 C 0.21079(18) 0.5066(3) 0.60618(19) 0.0216(5) Uani 1 1 d . . . C2 C 0.1758(2) 0.3759(3) 0.6335(2) 0.0275(6) Uani 1 1 d . . . H2 H 0.1901 0.3454 0.7003 0.033 Uiso 1 1 calc R . . C3 C 0.1035(2) 0.3395(3) 0.4691(2) 0.0349(7) Uani 1 1 d . . . H3 H 0.0666 0.2833 0.4201 0.042 Uiso 1 1 calc R . . C4 C 0.1387(2) 0.4705(3) 0.4411(2) 0.0322(7) Uani 1 1 d . . . H4 H 0.1253 0.5001 0.3741 0.039 Uiso 1 1 calc R . . C5 C 0.27110(18) 0.6055(3) 0.68030(19) 0.0229(5) Uani 1 1 d . . . N1 N 0.19165(15) 0.5541(2) 0.51026(16) 0.0231(5) Uani 1 1 d . . . N2 N 0.12104(17) 0.2921(2) 0.56452(17) 0.0292(5) Uani 1 1 d . . . O1 O 0.28789(13) 0.72992(18) 0.64534(13) 0.0245(4) Uani 1 1 d . . . O2 O 0.29895(14) 0.5606(2) 0.76765(14) 0.0313(5) 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 Cu 0.0290(3) 0.0204(2) 0.0201(2) 0.00207(17) 0.0010(2) -0.00653(19) Cd 0.02576(12) 0.02359(10) 0.02082(11) -0.00060(7) 0.00222(8) -0.00258(8) Cl1 0.0245(4) 0.0410(4) 0.0284(4) -0.0110(3) -0.0019(3) 0.0092(3) Cl2 0.0290(5) 0.0260(4) 0.0280(5) 0.000 0.0049(4) 0.000 Cl3 0.0636(8) 0.0247(5) 0.0297(5) 0.000 0.0191(5) 0.000 C1 0.0190(14) 0.0232(12) 0.0203(13) 0.0020(10) -0.0008(11) -0.0003(10) C2 0.0313(17) 0.0255(13) 0.0227(14) 0.0036(10) -0.0010(12) -0.0046(12) C3 0.041(2) 0.0332(15) 0.0250(15) -0.0020(12) -0.0045(14) -0.0147(14) C4 0.0408(19) 0.0320(14) 0.0198(14) 0.0006(11) -0.0031(13) -0.0112(13) C5 0.0193(14) 0.0267(13) 0.0215(13) -0.0006(10) 0.0018(11) -0.0009(11) N1 0.0241(13) 0.0219(10) 0.0218(11) 0.0004(8) 0.0013(10) -0.0037(9) N2 0.0335(14) 0.0247(11) 0.0266(12) 0.0007(9) -0.0002(11) -0.0086(10) O1 0.0292(11) 0.0221(8) 0.0202(9) 0.0007(7) 0.0004(8) -0.0053(8) O2 0.0333(12) 0.0330(10) 0.0227(10) 0.0060(8) -0.0057(9) -0.0068(9) _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 Cu O1 1.9453(17) 7_566 ? Cu O1 1.9453(17) . ? Cu N1 2.009(2) 7_566 ? Cu N1 2.009(2) . ? Cu Cl1 2.7593(7) 5_566 ? Cu Cl1 2.7593(7) 3 ? Cd O2 2.368(2) 4_546 ? Cd N2 2.432(2) . ? Cd Cl3 2.6000(6) . ? Cd Cl1 2.6029(7) 5_556 ? Cd Cl2 2.6217(6) . ? Cd Cl1 2.6579(8) . ? Cl1 Cd 2.6029(7) 5_556 ? Cl1 Cu 2.7593(7) 3_445 ? Cl2 Cd 2.6217(6) 2_556 ? Cl3 Cd 2.6000(6) 2_556 ? C1 N1 1.345(3) . ? C1 C2 1.385(3) . ? C1 C5 1.510(4) . ? C2 N2 1.352(3) . ? C3 N2 1.338(4) . ? C3 C4 1.392(4) . ? C4 N1 1.340(3) . ? C5 O2 1.242(3) . ? C5 O1 1.274(3) . ? O2 Cd 2.368(2) 4_556 ? 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 Cu O1 180.0 7_566 . ? O1 Cu N1 83.57(8) 7_566 7_566 ? O1 Cu N1 96.43(8) . 7_566 ? O1 Cu N1 96.43(8) 7_566 . ? O1 Cu N1 83.57(8) . . ? N1 Cu N1 180.0 7_566 . ? O1 Cu Cl1 86.21(6) 7_566 5_566 ? O1 Cu Cl1 93.79(6) . 5_566 ? N1 Cu Cl1 89.86(7) 7_566 5_566 ? N1 Cu Cl1 90.14(7) . 5_566 ? O1 Cu Cl1 93.79(6) 7_566 3 ? O1 Cu Cl1 86.21(6) . 3 ? N1 Cu Cl1 90.14(7) 7_566 3 ? N1 Cu Cl1 89.86(7) . 3 ? Cl1 Cu Cl1 180.0 5_566 3 ? O2 Cd N2 82.18(8) 4_546 . ? O2 Cd Cl3 88.93(5) 4_546 . ? N2 Cd Cl3 166.91(6) . . ? O2 Cd Cl1 88.73(5) 4_546 5_556 ? N2 Cd Cl1 95.66(6) . 5_556 ? Cl3 Cd Cl1 93.72(2) . 5_556 ? O2 Cd Cl2 96.58(4) 4_546 . ? N2 Cd Cl2 85.13(6) . . ? Cl3 Cd Cl2 86.38(2) . . ? Cl1 Cd Cl2 174.686(18) 5_556 . ? O2 Cd Cl1 166.02(5) 4_546 . ? N2 Cd Cl1 89.92(6) . . ? Cl3 Cd Cl1 100.626(19) . . ? Cl1 Cd Cl1 80.55(2) 5_556 . ? Cl2 Cd Cl1 94.204(16) . . ? Cd Cl1 Cd 99.45(2) 5_556 . ? Cd Cl1 Cu 131.98(3) 5_556 3_445 ? Cd Cl1 Cu 126.79(3) . 3_445 ? Cd Cl2 Cd 93.12(3) . 2_556 ? Cd Cl3 Cd 94.13(3) 2_556 . ? N1 C1 C2 121.1(2) . . ? N1 C1 C5 115.6(2) . . ? C2 C1 C5 123.2(2) . . ? N2 C2 C1 121.0(2) . . ? N2 C3 C4 122.0(3) . . ? N1 C4 C3 120.3(3) . . ? O2 C5 O1 126.3(2) . . ? O2 C5 C1 118.7(2) . . ? O1 C5 C1 115.0(2) . . ? C4 N1 C1 118.2(2) . . ? C4 N1 Cu 131.72(18) . . ? C1 N1 Cu 110.03(17) . . ? C3 N2 C2 117.3(2) . . ? C3 N2 Cd 128.01(19) . . ? C2 N2 Cd 114.32(17) . . ? C5 O1 Cu 114.92(16) . . ? C5 O2 Cd 126.44(18) . 4_556 ? 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 Cd Cl1 Cd 40.4(2) 4_546 . . 5_556 ? N2 Cd Cl1 Cd 95.75(6) . . . 5_556 ? Cl3 Cd Cl1 Cd -92.05(3) . . . 5_556 ? Cl1 Cd Cl1 Cd 0.0 5_556 . . 5_556 ? Cl2 Cd Cl1 Cd -179.14(2) . . . 5_556 ? O2 Cd Cl1 Cu -153.36(19) 4_546 . . 3_445 ? N2 Cd Cl1 Cu -98.03(6) . . . 3_445 ? Cl3 Cd Cl1 Cu 74.18(4) . . . 3_445 ? Cl1 Cd Cl1 Cu 166.22(5) 5_556 . . 3_445 ? Cl2 Cd Cl1 Cu -12.92(4) . . . 3_445 ? O2 Cd Cl2 Cd -88.50(5) 4_546 . . 2_556 ? N2 Cd Cl2 Cd -170.03(6) . . . 2_556 ? Cl3 Cd Cl2 Cd 0.0 . . . 2_556 ? Cl1 Cd Cl2 Cd 91.2(2) 5_556 . . 2_556 ? Cl1 Cd Cl2 Cd 100.406(19) . . . 2_556 ? O2 Cd Cl3 Cd 96.66(4) 4_546 . . 2_556 ? N2 Cd Cl3 Cd 49.6(3) . . . 2_556 ? Cl1 Cd Cl3 Cd -174.676(19) 5_556 . . 2_556 ? Cl2 Cd Cl3 Cd 0.0 . . . 2_556 ? Cl1 Cd Cl3 Cd -93.603(16) . . . 2_556 ? N1 C1 C2 N2 -0.2(4) . . . . ? C5 C1 C2 N2 179.1(3) . . . . ? N2 C3 C4 N1 -0.3(5) . . . . ? N1 C1 C5 O2 -172.4(2) . . . . ? C2 C1 C5 O2 8.3(4) . . . . ? N1 C1 C5 O1 7.9(3) . . . . ? C2 C1 C5 O1 -171.3(3) . . . . ? C3 C4 N1 C1 1.2(4) . . . . ? C3 C4 N1 Cu -177.3(2) . . . . ? C2 C1 N1 C4 -0.9(4) . . . . ? C5 C1 N1 C4 179.8(2) . . . . ? C2 C1 N1 Cu 177.8(2) . . . . ? C5 C1 N1 Cu -1.5(3) . . . . ? O1 Cu N1 C4 -4.4(3) 7_566 . . . ? O1 Cu N1 C4 175.6(3) . . . . ? N1 Cu N1 C4 122(100) 7_566 . . . ? Cl1 Cu N1 C4 81.8(3) 5_566 . . . ? Cl1 Cu N1 C4 -98.2(3) 3 . . . ? O1 Cu N1 C1 177.04(18) 7_566 . . . ? O1 Cu N1 C1 -2.96(18) . . . . ? N1 Cu N1 C1 -57(100) 7_566 . . . ? Cl1 Cu N1 C1 -96.76(17) 5_566 . . . ? Cl1 Cu N1 C1 83.24(17) 3 . . . ? C4 C3 N2 C2 -0.8(4) . . . . ? C4 C3 N2 Cd 171.6(2) . . . . ? C1 C2 N2 C3 1.0(4) . . . . ? C1 C2 N2 Cd -172.4(2) . . . . ? O2 Cd N2 C3 143.6(3) 4_546 . . . ? Cl3 Cd N2 C3 -168.8(2) . . . . ? Cl1 Cd N2 C3 55.6(3) 5_556 . . . ? Cl2 Cd N2 C3 -119.1(3) . . . . ? Cl1 Cd N2 C3 -24.9(3) . . . . ? O2 Cd N2 C2 -43.85(19) 4_546 . . . ? Cl3 Cd N2 C2 3.8(4) . . . . ? Cl1 Cd N2 C2 -131.78(19) 5_556 . . . ? Cl2 Cd N2 C2 53.50(19) . . . . ? Cl1 Cd N2 C2 147.72(19) . . . . ? O2 C5 O1 Cu 170.0(2) . . . . ? C1 C5 O1 Cu -10.4(3) . . . . ? O1 Cu O1 C5 -18(100) 7_566 . . . ? N1 Cu O1 C5 -172.26(19) 7_566 . . . ? N1 Cu O1 C5 7.74(19) . . . . ? Cl1 Cu O1 C5 97.46(18) 5_566 . . . ? Cl1 Cu O1 C5 -82.54(18) 3 . . . ? O1 C5 O2 Cd -43.1(4) . . . 4_556 ? C1 C5 O2 Cd 137.3(2) . . . 4_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.738 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.103 #===END