# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Miaoli Zhu' _publ_contact_author_email MIAOLI@SXU.EDU.CN _publ_section_title ; Novel Complexes of [Mi(HjL)k(H2O)l]n Chains (H3L=1-H-1,2,4-triazole-3, 5-dicarboxylic acid) with Topological Ferrimagnetic Behavior of the AF/AF/F Alternating (M=Mn) and AF Regular (M=Co) Sequence and (4,4) Topological Structure (M=Cd) ; loop_ _publ_author_name 'Miaoli Zhu.' 'Sisi Feng.' 'Liping Lu.' 'Qi Ma.' # Attachment '1-Mn_CCDC760033.cif' data_1-Mn _database_code_depnum_ccdc_archive 'CCDC 760033' #TrackingRef '1-Mn_CCDC760033.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Mn3 N6 O16' _chemical_formula_sum 'C8 H16 Mn3 N6 O16' _chemical_formula_weight 617.09 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' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3420(9) _cell_length_b 7.4391(10) _cell_length_c 9.6269(13) _cell_angle_alpha 81.117(1) _cell_angle_beta 87.714(2) _cell_angle_gamma 73.857(1) _cell_volume 499.01(11) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1226 _cell_measurement_theta_min 2.888 _cell_measurement_theta_max 27.164 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 309 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6832 _exptl_absorpt_correction_T_max 0.8913 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 2640 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1739 _reflns_number_gt 1383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1739 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 1.0000 0.5000 0.0246(2) Uani 1 2 d S . . Mn2 Mn 0.28719(6) 0.63777(7) 0.90876(4) 0.02520(17) Uani 1 1 d . . . N1 N 0.2817(3) 0.8175(4) 0.5705(2) 0.0240(6) Uani 1 1 d . . . N2 N 0.3701(3) 0.7154(4) 0.6901(2) 0.0225(6) Uani 1 1 d . . . N3 N 0.5876(3) 0.6963(4) 0.5197(2) 0.0215(6) Uani 1 1 d . . . O1 O 0.1915(3) 1.0038(3) 0.3123(2) 0.0303(6) Uani 1 1 d . . . O2 O 0.4808(3) 0.8797(3) 0.2295(2) 0.0298(6) Uani 1 1 d . . . O3 O 0.6122(3) 0.5066(3) 0.8877(2) 0.0304(6) Uani 1 1 d . . . O4 O 0.8548(3) 0.4632(3) 0.7383(2) 0.0366(6) Uani 1 1 d . . . O5 O -0.0659(3) 0.7583(4) 0.4425(3) 0.0517(8) Uani 1 1 d . . . H5A H 0.0068 0.6714 0.4022 0.062 Uiso 1 1 d R . . H5B H -0.1669 0.7267 0.4658 0.062 Uiso 1 1 d R . . O6 O 0.2120(3) 0.3894(3) 0.8531(2) 0.0312(6) Uani 1 1 d . . . H6A H 0.2937 0.3092 0.8125 0.037 Uiso 1 1 d R . . H6B H 0.1126 0.4269 0.8024 0.037 Uiso 1 1 d R . . O7 O 0.3351(3) 0.8940(3) 0.9613(2) 0.0420(6) Uani 1 1 d . . . H7A H 0.3718 0.8956 1.0436 0.050 Uiso 1 1 d R . . H7B H 0.4004 0.9482 0.9032 0.050 Uiso 1 1 d R . . O8 O -0.0114(3) 0.7634(4) 0.9136(2) 0.0442(7) Uani 1 1 d . . . H8A H -0.0777 0.8382 0.8470 0.053 Uiso 1 1 d R . . H8B H -0.0837 0.7298 0.9774 0.053 Uiso 1 1 d R . . C1 C 0.3619(4) 0.9018(4) 0.3262(3) 0.0234(7) Uani 1 1 d . . . C2 C 0.4153(4) 0.8033(4) 0.4720(3) 0.0203(7) Uani 1 1 d . . . C3 C 0.5500(4) 0.6456(4) 0.6555(3) 0.0207(7) Uani 1 1 d . . . C4 C 0.6874(4) 0.5284(4) 0.7664(3) 0.0237(7) 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 Mn1 0.0152(4) 0.0320(4) 0.0223(4) -0.0020(3) 0.0002(3) -0.0006(3) Mn2 0.0201(3) 0.0324(3) 0.0188(3) 0.0005(2) -0.00007(19) -0.0024(2) N1 0.0190(14) 0.0330(16) 0.0170(13) -0.0002(12) -0.0018(10) -0.0037(12) N2 0.0184(14) 0.0284(15) 0.0159(12) -0.0002(11) -0.0031(10) 0.0001(12) N3 0.0153(13) 0.0284(15) 0.0177(13) -0.0019(11) 0.0006(10) -0.0015(11) O1 0.0206(12) 0.0431(15) 0.0193(11) 0.0030(10) -0.0009(9) 0.0004(11) O2 0.0248(12) 0.0413(15) 0.0184(11) -0.0004(10) 0.0044(9) -0.0040(11) O3 0.0252(12) 0.0404(14) 0.0186(11) 0.0032(10) -0.0011(9) -0.0017(11) O4 0.0184(13) 0.0537(17) 0.0290(12) -0.0072(12) -0.0037(10) 0.0054(11) O5 0.0304(14) 0.0547(18) 0.085(2) -0.0419(16) 0.0300(13) -0.0228(13) O6 0.0209(12) 0.0365(14) 0.0330(13) -0.0069(11) -0.0040(10) -0.0011(10) O7 0.0588(17) 0.0450(16) 0.0265(12) -0.0033(11) -0.0012(11) -0.0223(14) O8 0.0242(13) 0.0618(18) 0.0317(13) 0.0109(12) 0.0019(10) 0.0027(12) C1 0.0221(17) 0.0268(18) 0.0215(16) -0.0026(14) 0.0012(13) -0.0075(14) C2 0.0174(16) 0.0243(17) 0.0195(15) -0.0036(13) 0.0003(12) -0.0060(13) C3 0.0168(16) 0.0250(17) 0.0193(15) -0.0040(13) -0.0021(12) -0.0036(13) C4 0.0211(17) 0.0235(17) 0.0234(16) -0.0034(14) -0.0025(13) -0.0005(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.142(2) 2_576 ? Mn1 O5 2.142(2) . ? Mn1 N1 2.202(2) 2_576 ? Mn1 N1 2.202(2) . ? Mn1 O1 2.247(2) . ? Mn1 O1 2.247(2) 2_576 ? Mn2 O8 2.132(2) . ? Mn2 O3 2.137(2) 2_667 ? Mn2 O7 2.168(2) . ? Mn2 N2 2.203(2) . ? Mn2 O6 2.214(2) . ? Mn2 O3 2.327(2) . ? N1 C2 1.331(4) . ? N1 N2 1.356(3) . ? N2 C3 1.327(4) . ? N3 C3 1.343(4) . ? N3 C2 1.348(3) . ? O1 C1 1.270(3) . ? O2 C1 1.249(3) . ? O3 C4 1.278(4) . ? O3 Mn2 2.137(2) 2_667 ? O4 C4 1.225(3) . ? O5 H5A 0.8499 . ? O5 H5B 0.8499 . ? O6 H6A 0.8500 . ? O6 H6B 0.8499 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? C1 C2 1.492(4) . ? C3 C4 1.492(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 O5 Mn1 O5 180.0 2_576 . ? O5 Mn1 N1 89.01(10) 2_576 2_576 ? O5 Mn1 N1 90.99(10) . 2_576 ? O5 Mn1 N1 90.99(10) 2_576 . ? O5 Mn1 N1 89.01(10) . . ? N1 Mn1 N1 180.000(1) 2_576 . ? O5 Mn1 O1 90.78(9) 2_576 . ? O5 Mn1 O1 89.22(9) . . ? N1 Mn1 O1 106.44(8) 2_576 . ? N1 Mn1 O1 73.56(8) . . ? O5 Mn1 O1 89.22(9) 2_576 2_576 ? O5 Mn1 O1 90.78(9) . 2_576 ? N1 Mn1 O1 73.56(8) 2_576 2_576 ? N1 Mn1 O1 106.44(8) . 2_576 ? O1 Mn1 O1 180.000(1) . 2_576 ? O8 Mn2 O3 110.30(8) . 2_667 ? O8 Mn2 O7 89.92(10) . . ? O3 Mn2 O7 89.68(9) 2_667 . ? O8 Mn2 N2 104.82(8) . . ? O3 Mn2 N2 144.87(9) 2_667 . ? O7 Mn2 N2 89.57(9) . . ? O8 Mn2 O6 85.19(9) . . ? O3 Mn2 O6 92.63(9) 2_667 . ? O7 Mn2 O6 175.07(8) . . ? N2 Mn2 O6 91.05(9) . . ? O8 Mn2 O3 176.26(8) . . ? O3 Mn2 O3 73.42(9) 2_667 . ? O7 Mn2 O3 90.51(9) . . ? N2 Mn2 O3 71.47(8) . . ? O6 Mn2 O3 94.33(8) . . ? C2 N1 N2 105.7(2) . . ? C2 N1 Mn1 114.89(18) . . ? N2 N1 Mn1 139.36(18) . . ? C3 N2 N1 105.9(2) . . ? C3 N2 Mn2 117.50(18) . . ? N1 N2 Mn2 136.51(18) . . ? C3 N3 C2 101.3(2) . . ? C1 O1 Mn1 117.97(17) . . ? C4 O3 Mn2 135.08(19) . 2_667 ? C4 O3 Mn2 118.30(18) . . ? Mn2 O3 Mn2 106.58(8) 2_667 . ? Mn1 O5 H5A 127.1 . . ? Mn1 O5 H5B 124.4 . . ? H5A O5 H5B 108.1 . . ? Mn2 O6 H6A 119.3 . . ? Mn2 O6 H6B 109.3 . . ? H6A O6 H6B 107.6 . . ? Mn2 O7 H7A 119.7 . . ? Mn2 O7 H7B 116.3 . . ? H7A O7 H7B 107.8 . . ? Mn2 O8 H8A 125.8 . . ? Mn2 O8 H8B 123.7 . . ? H8A O8 H8B 109.7 . . ? O2 C1 O1 125.2(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 114.6(2) . . ? N1 C2 N3 113.5(2) . . ? N1 C2 C1 118.8(2) . . ? N3 C2 C1 127.8(3) . . ? N2 C3 N3 113.7(2) . . ? N2 C3 C4 119.2(3) . . ? N3 C3 C4 127.1(3) . . ? O4 C4 O3 125.7(3) . . ? O4 C4 C3 120.9(3) . . ? O3 C4 C3 113.4(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 O5 Mn1 N1 C2 -90.3(2) 2_576 . . . ? O5 Mn1 N1 C2 89.7(2) . . . . ? O1 Mn1 N1 C2 0.3(2) . . . . ? O1 Mn1 N1 C2 -179.7(2) 2_576 . . . ? O5 Mn1 N1 N2 85.8(3) 2_576 . . . ? O5 Mn1 N1 N2 -94.2(3) . . . . ? O1 Mn1 N1 N2 176.4(3) . . . . ? O1 Mn1 N1 N2 -3.6(3) 2_576 . . . ? C2 N1 N2 C3 -0.5(3) . . . . ? Mn1 N1 N2 C3 -176.8(2) . . . . ? C2 N1 N2 Mn2 -178.1(2) . . . . ? Mn1 N1 N2 Mn2 5.6(5) . . . . ? O8 Mn2 N2 C3 -176.4(2) . . . . ? O3 Mn2 N2 C3 5.0(3) 2_667 . . . ? O7 Mn2 N2 C3 93.8(2) . . . . ? O6 Mn2 N2 C3 -91.1(2) . . . . ? O3 Mn2 N2 C3 3.1(2) . . . . ? O8 Mn2 N2 N1 1.0(3) . . . . ? O3 Mn2 N2 N1 -177.6(2) 2_667 . . . ? O7 Mn2 N2 N1 -88.8(3) . . . . ? O6 Mn2 N2 N1 86.3(3) . . . . ? O3 Mn2 N2 N1 -179.5(3) . . . . ? O5 Mn1 O1 C1 93.4(2) 2_576 . . . ? O5 Mn1 O1 C1 -86.6(2) . . . . ? N1 Mn1 O1 C1 -177.4(2) 2_576 . . . ? N1 Mn1 O1 C1 2.6(2) . . . . ? O3 Mn2 O3 C4 178.0(3) 2_667 . . . ? O7 Mn2 O3 C4 -92.4(2) . . . . ? N2 Mn2 O3 C4 -3.1(2) . . . . ? O6 Mn2 O3 C4 86.6(2) . . . . ? O3 Mn2 O3 Mn2 0.0 2_667 . . 2_667 ? O7 Mn2 O3 Mn2 89.51(10) . . . 2_667 ? N2 Mn2 O3 Mn2 178.88(13) . . . 2_667 ? O6 Mn2 O3 Mn2 -91.46(10) . . . 2_667 ? Mn1 O1 C1 O2 175.0(3) . . . . ? Mn1 O1 C1 C2 -4.6(4) . . . . ? N2 N1 C2 N3 0.4(4) . . . . ? Mn1 N1 C2 N3 177.7(2) . . . . ? N2 N1 C2 C1 179.9(3) . . . . ? Mn1 N1 C2 C1 -2.7(4) . . . . ? C3 N3 C2 N1 -0.1(4) . . . . ? C3 N3 C2 C1 -179.6(3) . . . . ? O2 C1 C2 N1 -174.7(3) . . . . ? O1 C1 C2 N1 4.9(4) . . . . ? O2 C1 C2 N3 4.8(5) . . . . ? O1 C1 C2 N3 -175.5(3) . . . . ? N1 N2 C3 N3 0.5(4) . . . . ? Mn2 N2 C3 N3 178.6(2) . . . . ? N1 N2 C3 C4 178.7(3) . . . . ? Mn2 N2 C3 C4 -3.2(4) . . . . ? C2 N3 C3 N2 -0.2(4) . . . . ? C2 N3 C3 C4 -178.3(3) . . . . ? Mn2 O3 C4 O4 -0.4(6) 2_667 . . . ? Mn2 O3 C4 O4 -177.8(3) . . . . ? Mn2 O3 C4 C3 179.8(2) 2_667 . . . ? Mn2 O3 C4 C3 2.5(4) . . . . ? N2 C3 C4 O4 -179.4(3) . . . . ? N3 C3 C4 O4 -1.4(5) . . . . ? N2 C3 C4 O3 0.4(4) . . . . ? N3 C3 C4 O3 178.4(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 _geom_hbond_publ_flag O8 H8B O6 0.85 2.06 2.896(3) 169.0 2_567 y O8 H8A O1 0.85 1.85 2.697(3) 172.1 2_576 y O7 H7B O2 0.85 2.01 2.854(3) 169.6 2_676 y O7 H7A O2 0.85 1.96 2.810(3) 174.1 1_556 y O6 H6B O4 0.85 1.95 2.765(3) 160.9 1_455 y O6 H6A O2 0.85 1.93 2.750(3) 163.2 2_666 y O5 H5B N3 0.85 1.92 2.763(3) 171.1 1_455 y O5 H5A O4 0.85 1.90 2.719(3) 161.8 2_666 y _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.393 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.074 # Attachment '2-Co_CCDC760034.cif' data_2-Co _database_code_depnum_ccdc_archive 'CCDC 760034' #TrackingRef '2-Co_CCDC760034.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H7 Co N3 O7' _chemical_formula_sum 'C4 H7 Co N3 O7' _chemical_formula_weight 268.06 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.762(3) _cell_length_b 6.6490(17) _cell_length_c 13.767(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.472(14) _cell_angle_gamma 90.00 _cell_volume 849.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3102 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 2.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6393 _exptl_absorpt_correction_T_max 0.8214 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4105 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1487 _reflns_number_gt 1358 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0387P)^2^+0.5527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1487 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.27983(3) 0.69165(4) 0.45410(2) 0.01928(13) Uani 1 1 d . . . O1 O 0.06093(17) 0.6390(3) 0.33695(12) 0.0233(4) Uani 1 1 d . . . O2 O -0.16026(17) 0.6417(3) 0.31497(13) 0.0288(4) Uani 1 1 d . . . O3 O 0.33547(17) 0.9309(3) 0.84104(12) 0.0256(4) Uani 1 1 d . . . O4 O 0.45589(18) 0.8817(3) 0.75095(14) 0.0355(4) Uani 1 1 d . . . O5 O 0.31296(17) 0.3975(3) 0.52227(13) 0.0255(4) Uani 1 1 d . . . H5A H 0.2349 0.3397 0.5075 0.031 Uiso 1 1 d R . . H5B H 0.3758 0.3756 0.5909 0.031 Uiso 1 1 d R . . O6 O 0.26631(19) 0.9810(3) 0.39251(13) 0.0328(4) Uani 1 1 d . . . H6A H 0.2230 1.0179 0.3239 0.039 Uiso 1 1 d R . . H6B H 0.3457 1.0446 0.4275 0.039 Uiso 1 1 d R . . O7 O 0.49073(17) 0.7676(3) 0.57682(13) 0.0231(4) Uani 1 1 d . . . H7A H 0.4849 0.8050 0.6334 0.028 Uiso 1 1 d R . . H7B H 0.5426 0.6623 0.5949 0.028 Uiso 1 1 d R . . N1 N 0.1829(2) 0.7751(3) 0.55141(14) 0.0177(4) Uani 1 1 d . . . N2 N -0.0308(2) 0.7736(3) 0.54354(15) 0.0189(4) Uani 1 1 d . . . N3 N 0.0763(2) 0.8302(3) 0.64674(15) 0.0196(4) Uani 1 1 d . . . H3 H 0.0643 0.8622 0.7020 0.024 Uiso 1 1 calc R . . C1 C -0.0296(3) 0.6694(3) 0.36908(18) 0.0196(5) Uani 1 1 d . . . C2 C 0.0392(2) 0.7424(3) 0.48918(17) 0.0173(4) Uani 1 1 d . . . C3 C 0.2037(2) 0.8297(3) 0.65120(17) 0.0176(5) Uani 1 1 d . . . C4 C 0.3439(2) 0.8834(4) 0.75589(18) 0.0214(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 Co1 0.0181(2) 0.0249(2) 0.01545(18) 0.00043(11) 0.00890(15) -0.00019(11) O1 0.0213(9) 0.0358(9) 0.0154(7) -0.0034(7) 0.0113(7) -0.0021(7) O2 0.0158(9) 0.0450(10) 0.0207(8) -0.0083(7) 0.0058(7) -0.0036(7) O3 0.0273(9) 0.0360(10) 0.0161(7) -0.0059(7) 0.0129(7) -0.0090(7) O4 0.0205(9) 0.0636(13) 0.0233(8) -0.0133(8) 0.0118(8) -0.0064(9) O5 0.0203(9) 0.0307(9) 0.0225(8) 0.0030(7) 0.0087(7) -0.0030(7) O6 0.0357(10) 0.0305(10) 0.0217(8) 0.0066(7) 0.0068(7) -0.0076(8) O7 0.0212(9) 0.0284(9) 0.0199(8) -0.0004(7) 0.0105(7) 0.0020(7) N1 0.0187(10) 0.0196(9) 0.0163(9) -0.0010(7) 0.0100(8) -0.0009(8) N2 0.0176(10) 0.0227(10) 0.0162(9) -0.0020(8) 0.0084(8) -0.0008(8) N3 0.0217(10) 0.0254(10) 0.0129(9) -0.0029(7) 0.0097(8) -0.0012(7) C1 0.0231(13) 0.0186(11) 0.0156(10) 0.0007(8) 0.0087(10) -0.0001(9) C2 0.0188(12) 0.0170(10) 0.0155(10) 0.0006(9) 0.0082(9) -0.0004(9) C3 0.0199(12) 0.0198(11) 0.0139(10) 0.0000(8) 0.0090(9) -0.0011(8) C4 0.0208(12) 0.0243(12) 0.0174(11) -0.0016(9) 0.0086(9) -0.0022(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 Co1 O6 2.0778(18) . ? Co1 O7 2.0909(17) . ? Co1 O3 2.0955(15) 4_575 ? Co1 O1 2.1024(17) . ? Co1 O5 2.1197(17) . ? Co1 N1 2.1468(18) . ? O1 C1 1.274(3) . ? O2 C1 1.226(3) . ? O3 C4 1.261(3) . ? O3 Co1 2.0955(15) 4_576 ? O4 C4 1.241(3) . ? O5 H5A 0.8499 . ? O5 H5B 0.8499 . ? O6 H6A 0.8500 . ? O6 H6B 0.8500 . ? O7 H7A 0.8499 . ? O7 H7B 0.8499 . ? N1 C3 1.326(3) . ? N1 C2 1.353(3) . ? N2 C2 1.320(3) . ? N2 N3 1.352(3) . ? N3 C3 1.341(3) . ? N3 H3 0.8600 . ? C1 C2 1.509(3) . ? C3 C4 1.508(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 O6 Co1 O7 85.91(7) . . ? O6 Co1 O3 92.54(7) . 4_575 ? O7 Co1 O3 95.29(7) . 4_575 ? O6 Co1 O1 91.26(7) . . ? O7 Co1 O1 174.28(6) . . ? O3 Co1 O1 89.80(6) 4_575 . ? O6 Co1 O5 175.07(7) . . ? O7 Co1 O5 89.72(6) . . ? O3 Co1 O5 85.57(6) 4_575 . ? O1 Co1 O5 93.29(7) . . ? O6 Co1 N1 93.43(7) . . ? O7 Co1 N1 96.04(7) . . ? O3 Co1 N1 167.54(7) 4_575 . ? O1 Co1 N1 79.15(7) . . ? O5 Co1 N1 89.31(7) . . ? C1 O1 Co1 117.64(14) . . ? C4 O3 Co1 140.84(16) . 4_576 ? Co1 O5 H5A 112.8 . . ? Co1 O5 H5B 120.7 . . ? H5A O5 H5B 108.7 . . ? Co1 O6 H6A 127.3 . . ? Co1 O6 H6B 112.7 . . ? H6A O6 H6B 108.3 . . ? Co1 O7 H7A 104.8 . . ? Co1 O7 H7B 108.7 . . ? H7A O7 H7B 108.4 . . ? C3 N1 C2 103.80(18) . . ? C3 N1 Co1 146.85(16) . . ? C2 N1 Co1 108.95(13) . . ? C2 N2 N3 102.25(17) . . ? C3 N3 N2 110.75(17) . . ? C3 N3 H3 124.6 . . ? N2 N3 H3 124.6 . . ? O2 C1 O1 127.5(2) . . ? O2 C1 C2 119.2(2) . . ? O1 C1 C2 113.3(2) . . ? N2 C2 N1 114.43(18) . . ? N2 C2 C1 124.6(2) . . ? N1 C2 C1 120.93(19) . . ? N1 C3 N3 108.76(19) . . ? N1 C3 C4 128.1(2) . . ? N3 C3 C4 123.16(19) . . ? O4 C4 O3 125.6(2) . . ? O4 C4 C3 118.3(2) . . ? O3 C4 C3 116.0(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 Co1 O1 C1 -94.97(16) . . . . ? O3 Co1 O1 C1 172.50(16) 4_575 . . . ? O5 Co1 O1 C1 86.95(16) . . . . ? N1 Co1 O1 C1 -1.72(16) . . . . ? O6 Co1 N1 C3 -96.2(3) . . . . ? O7 Co1 N1 C3 -10.0(3) . . . . ? O3 Co1 N1 C3 145.3(3) 4_575 . . . ? O1 Co1 N1 C3 173.2(3) . . . . ? O5 Co1 N1 C3 79.7(3) . . . . ? O6 Co1 N1 C2 93.03(15) . . . . ? O7 Co1 N1 C2 179.27(14) . . . . ? O3 Co1 N1 C2 -25.4(4) 4_575 . . . ? O1 Co1 N1 C2 2.40(14) . . . . ? O5 Co1 N1 C2 -91.08(15) . . . . ? C2 N2 N3 C3 -0.5(2) . . . . ? Co1 O1 C1 O2 -177.55(19) . . . . ? Co1 O1 C1 C2 0.6(2) . . . . ? N3 N2 C2 N1 0.2(2) . . . . ? N3 N2 C2 C1 178.1(2) . . . . ? C3 N1 C2 N2 0.1(3) . . . . ? Co1 N1 C2 N2 174.96(15) . . . . ? C3 N1 C2 C1 -177.84(19) . . . . ? Co1 N1 C2 C1 -3.0(2) . . . . ? O2 C1 C2 N2 2.4(3) . . . . ? O1 C1 C2 N2 -176.0(2) . . . . ? O2 C1 C2 N1 -179.9(2) . . . . ? O1 C1 C2 N1 1.8(3) . . . . ? C2 N1 C3 N3 -0.4(2) . . . . ? Co1 N1 C3 N3 -171.4(2) . . . . ? C2 N1 C3 C4 179.3(2) . . . . ? Co1 N1 C3 C4 8.3(4) . . . . ? N2 N3 C3 N1 0.6(2) . . . . ? N2 N3 C3 C4 -179.12(19) . . . . ? Co1 O3 C4 O4 -117.4(3) 4_576 . . . ? Co1 O3 C4 C3 64.2(3) 4_576 . . . ? N1 C3 C4 O4 1.5(4) . . . . ? N3 C3 C4 O4 -178.8(2) . . . . ? N1 C3 C4 O3 180.0(2) . . . . ? N3 C3 C4 O3 -0.3(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 _geom_hbond_publ_flag O5 H5A N2 0.85 2.08 2.923(3) 172.8 3_566 y O5 H5B O4 0.85 2.01 2.841(2) 166.9 2_646 y O6 H6A O2 0.85 1.87 2.701(2) 167.3 2 y O6 H6B O7 0.85 2.18 2.948(2) 149.4 3_676 y O7 H7A O4 0.85 1.87 2.716(2) 175.3 . y O7 H7B O3 0.85 1.92 2.765(2) 171.0 2_646 y N3 H3 O1 0.86 1.88 2.714(2) 164.0 4_576 y _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.349 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.064 # Attachment '3-Cd_CCDC760035.cif' data_3-Cd _database_code_depnum_ccdc_archive 'CCDC 760035' #TrackingRef '3-Cd_CCDC760035.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 Cd N3 O6' _chemical_formula_sum 'C4 H5 Cd N3 O6' _chemical_formula_weight 303.51 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 7.345(3) _cell_length_b 10.222(4) _cell_length_c 10.635(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.502(4) _cell_angle_gamma 90.00 _cell_volume 796.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3433 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 2.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4920 _exptl_absorpt_correction_T_max 0.6088 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2957 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1364 _reflns_number_gt 1353 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0597P)^2^+4.1181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1364 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.585 _refine_ls_restrained_S_all 1.585 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20026(9) 0.89894(6) 0.32177(6) 0.0246(3) Uani 1 1 d . . . N1 N 0.2748(10) 1.0052(7) 0.1448(7) 0.0227(15) Uani 1 1 d . . . N2 N 0.3419(10) 1.1160(7) -0.0207(7) 0.0229(16) Uani 1 1 d . . . H2 H 0.3858 1.1762 -0.0660 0.027 Uiso 1 1 calc R . . N3 N 0.2509(10) 1.0095(7) -0.0657(7) 0.0257(17) Uani 1 1 d . . . C1 C 0.3538(12) 1.1136(8) 0.1073(9) 0.0214(18) Uani 1 1 d . . . C2 C 0.4523(13) 1.2158(9) 0.1888(8) 0.0261(19) Uani 1 1 d . . . C3 C 0.2136(11) 0.9463(8) 0.0335(8) 0.0207(17) Uani 1 1 d . . . C4 C 0.1165(12) 0.8163(8) 0.0341(8) 0.0207(17) Uani 1 1 d . . . O1 O 0.4450(12) 1.2078(7) 0.3003(7) 0.0425(18) Uani 1 1 d . . . O2 O 0.5298(10) 1.3003(7) 0.1259(7) 0.0373(17) Uani 1 1 d . . . O3 O 0.0874(9) 0.7735(6) 0.1470(6) 0.0287(15) Uani 1 1 d . . . O4 O 0.0718(9) 0.7616(6) -0.0633(6) 0.0284(14) Uani 1 1 d . . . O5 O -0.0730(9) 1.0138(6) 0.3107(6) 0.0270(14) Uani 1 1 d . . . H5A H -0.1218 0.9705 0.2524 0.041 Uiso 1 1 d R . . H5B H -0.0584 1.0907 0.2925 0.041 Uiso 1 1 d R . . O6 O 0.2754(11) 1.0311(8) 0.4860(8) 0.046(2) Uani 1 1 d . . . H6A H 0.1973 1.0245 0.5367 0.069 Uiso 1 1 d R . . H6B H 0.3386 1.0970 0.4961 0.069 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0329(5) 0.0193(5) 0.0216(5) 0.0020(2) 0.0018(3) 0.0055(2) N1 0.021(4) 0.014(3) 0.032(4) -0.004(3) -0.001(3) 0.001(3) N2 0.027(4) 0.022(4) 0.020(4) 0.007(3) 0.002(3) -0.002(3) N3 0.026(4) 0.024(4) 0.026(4) -0.004(3) -0.001(3) -0.004(3) C1 0.023(4) 0.014(4) 0.027(5) 0.008(3) 0.004(4) -0.004(3) C2 0.031(5) 0.022(5) 0.024(4) 0.001(4) -0.001(4) 0.002(4) C3 0.022(4) 0.013(4) 0.028(4) -0.006(3) 0.004(3) 0.000(3) C4 0.025(4) 0.010(4) 0.026(4) -0.003(3) -0.002(3) -0.001(3) O1 0.065(5) 0.024(4) 0.038(4) -0.009(3) 0.001(4) -0.007(3) O2 0.037(4) 0.026(4) 0.047(4) 0.005(3) -0.009(3) -0.013(3) O3 0.045(4) 0.012(3) 0.028(3) -0.001(2) 0.000(3) -0.008(3) O4 0.040(4) 0.026(3) 0.018(3) -0.009(3) -0.005(3) -0.001(3) O5 0.035(4) 0.019(3) 0.026(3) 0.002(2) -0.004(3) 0.005(3) O6 0.051(5) 0.049(5) 0.041(4) -0.022(4) 0.014(4) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O6 2.242(7) . ? Cd1 O2 2.255(7) 2_645 ? Cd1 N1 2.277(8) . ? Cd1 O4 2.293(6) 4_576 ? Cd1 O5 2.320(6) . ? Cd1 O3 2.355(6) . ? N1 C1 1.327(11) . ? N1 C3 1.372(11) . ? N2 N3 1.345(10) . ? N2 C1 1.357(12) . ? N2 H2 0.8600 . ? N3 C3 1.285(12) . ? C1 C2 1.506(12) . ? C2 O1 1.194(12) . ? C2 O2 1.256(12) . ? C3 C4 1.508(11) . ? C4 O4 1.200(10) . ? C4 O3 1.311(11) . ? O2 Cd1 2.255(7) 2_655 ? O4 Cd1 2.293(6) 4_575 ? O5 H5A 0.8213 . ? O5 H5B 0.8187 . ? O6 H6A 0.8205 . ? O6 H6B 0.8203 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cd1 O2 85.4(3) . 2_645 ? O6 Cd1 N1 107.2(3) . . ? O2 Cd1 N1 98.8(3) 2_645 . ? O6 Cd1 O4 95.9(3) . 4_576 ? O2 Cd1 O4 86.5(3) 2_645 4_576 ? N1 Cd1 O4 156.6(2) . 4_576 ? O6 Cd1 O5 83.9(3) . . ? O2 Cd1 O5 168.3(2) 2_645 . ? N1 Cd1 O5 88.8(2) . . ? O4 Cd1 O5 89.9(2) 4_576 . ? O6 Cd1 O3 173.1(3) . . ? O2 Cd1 O3 101.5(2) 2_645 . ? N1 Cd1 O3 72.5(2) . . ? O4 Cd1 O3 84.1(2) 4_576 . ? O5 Cd1 O3 89.2(2) . . ? C1 N1 C3 103.2(8) . . ? C1 N1 Cd1 141.8(6) . . ? C3 N1 Cd1 114.8(6) . . ? N3 N2 C1 109.5(7) . . ? N3 N2 H2 125.3 . . ? C1 N2 H2 125.3 . . ? C3 N3 N2 104.3(7) . . ? N1 C1 N2 108.7(8) . . ? N1 C1 C2 127.4(8) . . ? N2 C1 C2 123.7(7) . . ? O1 C2 O2 129.4(9) . . ? O1 C2 C1 117.9(8) . . ? O2 C2 C1 112.8(8) . . ? N3 C3 N1 114.2(8) . . ? N3 C3 C4 125.3(8) . . ? N1 C3 C4 120.4(8) . . ? O4 C4 O3 125.6(8) . . ? O4 C4 C3 120.3(8) . . ? O3 C4 C3 114.1(7) . . ? C2 O2 Cd1 127.1(6) . 2_655 ? C4 O3 Cd1 118.0(5) . . ? C4 O4 Cd1 134.2(6) . 4_575 ? Cd1 O5 H5A 95.2 . . ? Cd1 O5 H5B 111.7 . . ? H5A O5 H5B 113.4 . . ? Cd1 O6 H6A 108.7 . . ? Cd1 O6 H6B 134.4 . . ? H6A O6 H6B 113.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cd1 N1 C1 4.4(10) . . . . ? O2 Cd1 N1 C1 -83.4(10) 2_645 . . . ? O4 Cd1 N1 C1 174.8(8) 4_576 . . . ? O5 Cd1 N1 C1 87.7(10) . . . . ? O3 Cd1 N1 C1 177.2(10) . . . . ? O6 Cd1 N1 C3 -170.9(6) . . . . ? O2 Cd1 N1 C3 101.2(6) 2_645 . . . ? O4 Cd1 N1 C3 -0.6(10) 4_576 . . . ? O5 Cd1 N1 C3 -87.7(6) . . . . ? O3 Cd1 N1 C3 1.8(5) . . . . ? C1 N2 N3 C3 -0.9(10) . . . . ? C3 N1 C1 N2 -1.2(9) . . . . ? Cd1 N1 C1 N2 -176.8(7) . . . . ? C3 N1 C1 C2 -177.6(9) . . . . ? Cd1 N1 C1 C2 6.7(16) . . . . ? N3 N2 C1 N1 1.4(10) . . . . ? N3 N2 C1 C2 178.0(8) . . . . ? N1 C1 C2 O1 -8.3(15) . . . . ? N2 C1 C2 O1 175.8(9) . . . . ? N1 C1 C2 O2 172.8(9) . . . . ? N2 C1 C2 O2 -3.2(13) . . . . ? N2 N3 C3 N1 0.2(10) . . . . ? N2 N3 C3 C4 -178.0(8) . . . . ? C1 N1 C3 N3 0.6(10) . . . . ? Cd1 N1 C3 N3 177.7(6) . . . . ? C1 N1 C3 C4 178.9(8) . . . . ? Cd1 N1 C3 C4 -4.0(10) . . . . ? N3 C3 C4 O4 2.1(14) . . . . ? N1 C3 C4 O4 -176.0(8) . . . . ? N3 C3 C4 O3 -177.4(8) . . . . ? N1 C3 C4 O3 4.5(12) . . . . ? O1 C2 O2 Cd1 37.6(15) . . . 2_655 ? C1 C2 O2 Cd1 -143.6(7) . . . 2_655 ? O4 C4 O3 Cd1 177.9(7) . . . . ? C3 C4 O3 Cd1 -2.6(9) . . . . ? O2 Cd1 O3 C4 -95.2(6) 2_645 . . . ? N1 Cd1 O3 C4 0.5(6) . . . . ? O4 Cd1 O3 C4 179.6(6) 4_576 . . . ? O5 Cd1 O3 C4 89.6(6) . . . . ? O3 C4 O4 Cd1 -84.8(11) . . . 4_575 ? C3 C4 O4 Cd1 95.8(9) . . . 4_575 ? 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 _geom_hbond_publ_flag N2 H2 O1 0.86 1.93 2.769(10) 166.0 4_585 y O5 H5A N3 0.82 2.14 2.832(10) 141.6 3_575 y O5 H5B O3 0.82 1.99 2.696(9) 143.6 2 y O6 H6A O5 0.82 1.96 2.757(10) 162.7 3_576 y O6 H6B O2 0.82 2.16 2.871(10) 144.6 4_586 y O6 H6B O1 0.82 2.55 3.017(11) 117.7 . y _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.460 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.257