# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Carmen R. Maldonado' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; M.Quiros ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; 'Juan M. Salas' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email mquiros@ugr.es _publ_contact_author_fax 34-58-248526 _publ_contact_author_phone 34-58-240441 #TrackingRef '- Compound1.cif' _publ_contact_author_name 'Miguel Quiros' _publ_section_title ; H-bond superstructures built by aquacomplexes and an azapurine derivative: A case of molecular recognition ; data_mnax44 _database_code_depnum_ccdc_archive 'CCDC 827852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N2, H12 Mn O6 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C22 H32 Mn N12 O10' _chemical_formula_weight 679.54 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' 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 8.5570(12) _cell_length_b 9.1663(13) _cell_length_c 10.9500(15) _cell_angle_alpha 108.647(2) _cell_angle_beta 108.125(2) _cell_angle_gamma 101.431(2) _cell_volume 729.93(18) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4227 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.8 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 353 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 176 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.1 _diffrn_reflns_number 8537 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.20 _reflns_number_total 3306 _reflns_number_gt 2984 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3306 _refine_ls_number_parameters 231 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Mn Mn 0.5000 0.5000 0.5000 0.03291(13) Uani 1 2 d S . . O1W O 0.38415(17) 0.24176(16) 0.34578(14) 0.0437(3) Uani 1 1 d D . . H11W H 0.315(2) 0.230(3) 0.2675(14) 0.053(6) Uiso 1 1 d D . . H12W H 0.460(3) 0.205(3) 0.327(3) 0.087(9) Uiso 1 1 d D . . O2W O 0.58027(17) 0.42212(19) 0.67057(15) 0.0484(3) Uani 1 1 d D . . H21W H 0.533(3) 0.405(3) 0.723(2) 0.072(8) Uiso 1 1 d D . . H22W H 0.6796(19) 0.413(3) 0.702(3) 0.074(8) Uiso 1 1 d D . . O3W O 0.25331(16) 0.48602(19) 0.51155(15) 0.0465(3) Uani 1 1 d D . . H31W H 0.174(2) 0.511(3) 0.463(2) 0.056(6) Uiso 1 1 d D . . H32W H 0.220(3) 0.472(3) 0.572(2) 0.065(7) Uiso 1 1 d D . . N1 N 0.13923(19) 0.4375(2) 0.71109(16) 0.0412(3) Uani 1 1 d . . . N2 N -0.01977(19) 0.4426(2) 0.68268(16) 0.0453(4) Uani 1 1 d . . . N3 N -0.09668(19) 0.3791(2) 0.75466(16) 0.0411(3) Uani 1 1 d . . . C3A C 0.0236(2) 0.3338(2) 0.83089(17) 0.0335(3) Uani 1 1 d . . . N4 N 0.01147(17) 0.26468(18) 0.92315(15) 0.0356(3) Uani 1 1 d . . . C4 C -0.1471(2) 0.2294(3) 0.9486(2) 0.0476(4) Uani 1 1 d . . . H41 H -0.1921 0.1099 0.9276 0.057 Uiso 1 1 d R . . H42 H -0.2360 0.2577 0.8869 0.057 Uiso 1 1 d R . . H43 H -0.1212 0.2972 1.0480 0.057 Uiso 1 1 d R . . C5 C 0.1524(2) 0.23112(19) 0.99522(17) 0.0338(3) Uani 1 1 d . . . O5 O 0.14973(16) 0.17507(17) 1.08119(14) 0.0452(3) Uani 1 1 d . . . N6 N 0.29924(17) 0.26195(17) 0.96334(14) 0.0343(3) Uani 1 1 d . . . C6 C 0.4448(2) 0.2179(3) 1.0371(2) 0.0471(4) Uani 1 1 d . . . H61 H 0.5147 0.1937 0.9804 0.057 Uiso 1 1 d R . . H62 H 0.3967 0.1182 1.0508 0.057 Uiso 1 1 d R . . H63 H 0.5201 0.3117 1.1299 0.057 Uiso 1 1 d R . . C7 C 0.3211(2) 0.3330(2) 0.87202(17) 0.0331(3) Uani 1 1 d . . . O7 O 0.45824(15) 0.35773(17) 0.85600(13) 0.0437(3) Uani 1 1 d . . . C7A C 0.1708(2) 0.3689(2) 0.80528(17) 0.0333(3) Uani 1 1 d . . . N1P N 0.6319(2) 0.0869(2) 0.3182(2) 0.0594(5) Uani 1 1 d . . . C2P C 0.6219(3) -0.0061(3) 0.3895(3) 0.0592(5) Uani 1 1 d . . . H2P H 0.5100 -0.0490 0.3906 0.071 Uiso 1 1 d R . . C3P C 0.7617(3) -0.0416(3) 0.4620(2) 0.0520(5) Uani 1 1 d . . . H3P H 0.7452 -0.1060 0.5140 0.062 Uiso 1 1 d R . . C4P C 0.9226(2) 0.0166(2) 0.46071(19) 0.0402(4) Uani 1 1 d . . . C5P C 0.9315(3) 0.1081(3) 0.3824(2) 0.0537(5) Uani 1 1 d . . . H5P H 1.0400 0.1476 0.3749 0.064 Uiso 1 1 d R . . C6P C 0.7862(3) 0.1408(3) 0.3152(3) 0.0613(6) Uani 1 1 d . . . H6P H 0.7988 0.2058 0.2631 0.074 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 Mn 0.02829(19) 0.0474(2) 0.0355(2) 0.02583(16) 0.01584(14) 0.01805(15) O1W 0.0434(7) 0.0529(7) 0.0383(7) 0.0225(6) 0.0126(6) 0.0230(6) O2W 0.0376(7) 0.0851(10) 0.0548(8) 0.0526(8) 0.0267(6) 0.0326(7) O3W 0.0349(6) 0.0806(10) 0.0538(8) 0.0478(7) 0.0269(6) 0.0311(6) N1 0.0376(8) 0.0643(10) 0.0401(8) 0.0348(7) 0.0196(6) 0.0252(7) N2 0.0384(8) 0.0721(11) 0.0467(9) 0.0404(8) 0.0204(7) 0.0294(8) N3 0.0328(7) 0.0631(9) 0.0429(8) 0.0334(7) 0.0171(6) 0.0246(7) C3A 0.0314(8) 0.0430(9) 0.0326(8) 0.0205(7) 0.0140(6) 0.0155(6) N4 0.0278(6) 0.0498(8) 0.0380(7) 0.0268(6) 0.0144(6) 0.0140(6) C4 0.0334(9) 0.0659(12) 0.0557(11) 0.0361(10) 0.0225(8) 0.0149(8) C5 0.0297(8) 0.0375(8) 0.0329(8) 0.0175(7) 0.0094(6) 0.0086(6) O5 0.0372(6) 0.0595(8) 0.0442(7) 0.0354(6) 0.0120(5) 0.0105(6) N6 0.0290(7) 0.0473(8) 0.0346(7) 0.0241(6) 0.0124(5) 0.0175(6) C6 0.0375(9) 0.0692(12) 0.0525(11) 0.0404(10) 0.0172(8) 0.0292(9) C7 0.0314(8) 0.0438(9) 0.0299(7) 0.0184(7) 0.0137(6) 0.0163(6) O7 0.0335(6) 0.0709(9) 0.0438(7) 0.0328(6) 0.0222(5) 0.0257(6) C7A 0.0306(8) 0.0451(9) 0.0330(8) 0.0223(7) 0.0147(6) 0.0166(6) N1P 0.0567(11) 0.0600(11) 0.0615(11) 0.0252(9) 0.0148(9) 0.0332(9) C2P 0.0462(11) 0.0735(14) 0.0640(13) 0.0296(11) 0.0233(10) 0.0282(10) C3P 0.0463(11) 0.0626(12) 0.0577(12) 0.0324(10) 0.0229(9) 0.0235(9) C4P 0.0411(9) 0.0349(8) 0.0422(9) 0.0151(7) 0.0126(7) 0.0155(7) C5P 0.0483(11) 0.0536(11) 0.0662(13) 0.0360(10) 0.0188(10) 0.0187(9) C6P 0.0623(14) 0.0580(12) 0.0689(14) 0.0385(11) 0.0168(11) 0.0252(10) _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 Mn O3W 2.1349(12) . ? Mn O3W 2.1349(12) 2_666 ? Mn O2W 2.1722(12) 2_666 ? Mn O2W 2.1722(12) . ? Mn O1W 2.2158(14) 2_666 ? Mn O1W 2.2158(14) . ? O1W H11W 0.835(10) . ? O1W H12W 0.835(10) . ? O2W H21W 0.830(10) . ? O2W H22W 0.845(10) . ? O3W H31W 0.840(10) . ? O3W H32W 0.831(10) . ? N1 N2 1.312(2) . ? N1 C7A 1.356(2) . ? N2 N3 1.363(2) . ? N3 C3A 1.336(2) . ? C3A N4 1.372(2) . ? C3A C7A 1.373(2) . ? N4 C5 1.372(2) . ? N4 C4 1.463(2) . ? C4 H41 1.0093 . ? C4 H42 0.9860 . ? C4 H43 0.9912 . ? C5 O5 1.2120(19) . ? C5 N6 1.405(2) . ? N6 C7 1.394(2) . ? N6 C6 1.466(2) . ? C6 H61 0.9937 . ? C6 H62 1.0019 . ? C6 H63 1.0010 . ? C7 O7 1.2274(19) . ? C7 C7A 1.426(2) . ? N1P C6P 1.329(3) . ? N1P C2P 1.335(3) . ? C2P C3P 1.378(3) . ? C2P H2P 0.9656 . ? C3P C4P 1.381(3) . ? C3P H3P 0.9610 . ? C4P C5P 1.386(3) . ? C4P C4P 1.485(3) 2_756 ? C5P C6P 1.378(3) . ? C5P H5P 0.9653 . ? C6P H6P 0.9608 . ? 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 O3W Mn O3W 179.999(2) . 2_666 ? O3W Mn O2W 88.78(5) . 2_666 ? O3W Mn O2W 91.22(5) 2_666 2_666 ? O3W Mn O2W 91.22(5) . . ? O3W Mn O2W 88.78(5) 2_666 . ? O2W Mn O2W 180.00(7) 2_666 . ? O3W Mn O1W 91.50(5) . 2_666 ? O3W Mn O1W 88.50(5) 2_666 2_666 ? O2W Mn O1W 89.98(6) 2_666 2_666 ? O2W Mn O1W 90.02(6) . 2_666 ? O3W Mn O1W 88.50(5) . . ? O3W Mn O1W 91.50(5) 2_666 . ? O2W Mn O1W 90.02(6) 2_666 . ? O2W Mn O1W 89.98(6) . . ? O1W Mn O1W 179.999(1) 2_666 . ? Mn O1W H11W 112.6(16) . . ? Mn O1W H12W 111(2) . . ? H11W O1W H12W 103(3) . . ? Mn O2W H21W 131.5(19) . . ? Mn O2W H22W 122.2(19) . . ? H21W O2W H22W 106(3) . . ? Mn O3W H31W 126.6(16) . . ? Mn O3W H32W 129.0(17) . . ? H31W O3W H32W 104(2) . . ? N2 N1 C7A 106.49(13) . . ? N1 N2 N3 112.10(13) . . ? C3A N3 N2 104.79(13) . . ? N3 C3A N4 127.92(15) . . ? N3 C3A C7A 109.30(14) . . ? N4 C3A C7A 122.77(14) . . ? C3A N4 C5 119.17(13) . . ? C3A N4 C4 121.42(14) . . ? C5 N4 C4 119.39(14) . . ? N4 C4 H41 110.0 . . ? N4 C4 H42 109.0 . . ? H41 C4 H42 109.6 . . ? N4 C4 H43 109.4 . . ? H41 C4 H43 110.3 . . ? H42 C4 H43 108.6 . . ? O5 C5 N4 121.51(15) . . ? O5 C5 N6 121.37(15) . . ? N4 C5 N6 117.12(14) . . ? C7 N6 C5 126.67(13) . . ? C7 N6 C6 117.36(13) . . ? C5 N6 C6 115.95(14) . . ? N6 C6 H61 110.2 . . ? N6 C6 H62 108.7 . . ? H61 C6 H62 109.1 . . ? N6 C6 H63 108.7 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 110.7 . . ? O7 C7 N6 120.47(14) . . ? O7 C7 C7A 127.13(15) . . ? N6 C7 C7A 112.40(13) . . ? N1 C7A C3A 107.32(14) . . ? N1 C7A C7 130.94(14) . . ? C3A C7A C7 121.74(14) . . ? C6P N1P C2P 116.14(18) . . ? N1P C2P C3P 123.7(2) . . ? N1P C2P H2P 117.4 . . ? C3P C2P H2P 118.9 . . ? C2P C3P C4P 120.0(2) . . ? C2P C3P H3P 118.9 . . ? C4P C3P H3P 121.1 . . ? C3P C4P C5P 116.28(17) . . ? C3P C4P C4P 121.8(2) . 2_756 ? C5P C4P C4P 121.9(2) . 2_756 ? C6P C5P C4P 120.0(2) . . ? C6P C5P H5P 120.6 . . ? C4P C5P H5P 119.4 . . ? N1P C6P C5P 123.8(2) . . ? N1P C6P H6P 119.1 . . ? C5P C6P H6P 117.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H12W N1P 0.835(10) 2.003(13) 2.814(2) 164(3) . O1W H11W O5 0.835(10) 1.918(10) 2.7489(18) 173(2) 1_554 O2W H21W O7 0.830(10) 1.899(11) 2.7207(17) 170(3) . O2W H22W N3 0.845(10) 1.937(10) 2.7795(19) 174(3) 1_655 O3W H32W N1 0.831(10) 1.944(10) 2.7752(19) 179(3) . O3W H31W N2 0.840(10) 1.957(11) 2.7767(19) 165(2) 2_566 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.347 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.113 # Attachment '- Compound2.cif' data_znax44 _database_code_depnum_ccdc_archive 'CCDC 827853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N2, H12 O6 Zn 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C22 H32 N12 O10 Zn' _chemical_formula_weight 689.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4575(7) _cell_length_b 8.9798(11) _cell_length_c 10.8612(8) _cell_angle_alpha 109.345(1) _cell_angle_beta 107.577(1) _cell_angle_gamma 101.978(1) _cell_volume 697.24(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3253 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description irregular _exptl_crystal_colour white _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 218 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 4421 _diffrn_reflns_av_R_equivalents 0.0107 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2992 _reflns_number_gt 2921 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997a). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXS97. Program for the Solution of Crystal Structures. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2992 _refine_ls_number_parameters 231 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 Zn Zn 0.5000 0.5000 0.5000 0.01169(9) Uani 1 2 d S . . O1W O 0.38378(15) 0.24507(15) 0.35005(12) 0.0153(2) Uani 1 1 d D . . H11W H 0.314(2) 0.229(3) 0.2703(14) 0.021(5) Uiso 1 1 d D . . H12W H 0.457(3) 0.203(3) 0.330(3) 0.036(7) Uiso 1 1 d D . . O2W O 0.57401(16) 0.42449(16) 0.66574(13) 0.0174(2) Uani 1 1 d D . . H21W H 0.521(3) 0.410(3) 0.717(2) 0.036(7) Uiso 1 1 d D . . H22W H 0.673(2) 0.416(4) 0.701(3) 0.055(9) Uiso 1 1 d D . . O3W O 0.26128(15) 0.48944(16) 0.51272(13) 0.0170(2) Uani 1 1 d D . . H31W H 0.182(2) 0.511(3) 0.460(2) 0.034(7) Uiso 1 1 d D . . H32W H 0.229(3) 0.474(3) 0.5746(19) 0.031(6) Uiso 1 1 d D . . N1 N 0.13862(18) 0.43603(18) 0.70940(14) 0.0152(3) Uani 1 1 d . . . N2 N -0.02244(18) 0.44126(18) 0.68012(15) 0.0162(3) Uani 1 1 d . . . N3 N -0.10230(18) 0.37891(18) 0.75335(15) 0.0153(3) Uani 1 1 d . . . C3A C 0.0181(2) 0.33386(19) 0.83121(16) 0.0126(3) Uani 1 1 d . . . N4 N 0.00421(17) 0.26603(17) 0.92563(14) 0.0132(3) Uani 1 1 d . . . C4 C -0.1568(2) 0.2311(2) 0.95194(18) 0.0176(3) Uani 1 1 d . . . H41 H -0.2191 0.1095 0.9074 0.021 Uiso 1 1 d R . . H42 H -0.2332 0.2858 0.9110 0.021 Uiso 1 1 d R . . H43 H -0.1257 0.2746 1.0548 0.021 Uiso 1 1 d R . . C5 C 0.1458(2) 0.23333(19) 0.99956(16) 0.0127(3) Uani 1 1 d . . . O5 O 0.14213(15) 0.18016(15) 1.08861(12) 0.0158(2) Uani 1 1 d . . . N6 N 0.29492(17) 0.26211(17) 0.96685(14) 0.0127(3) Uani 1 1 d . . . C6 C 0.4406(2) 0.2172(2) 1.04165(18) 0.0172(3) Uani 1 1 d . . . H61 H 0.5146 0.1997 0.9878 0.021 Uiso 1 1 d R . . H62 H 0.3924 0.1137 1.0501 0.021 Uiso 1 1 d R . . H63 H 0.5118 0.3082 1.1369 0.021 Uiso 1 1 d R . . C7 C 0.3196(2) 0.33226(19) 0.87352(16) 0.0125(3) Uani 1 1 d . . . O7 O 0.45875(15) 0.35604(15) 0.85680(12) 0.0156(2) Uani 1 1 d . . . C7A C 0.1682(2) 0.36781(19) 0.80540(16) 0.0129(3) Uani 1 1 d . . . N1P N 0.6307(2) 0.08720(18) 0.31354(16) 0.0200(3) Uani 1 1 d . . . C2P C 0.6178(2) -0.0054(2) 0.38704(19) 0.0199(3) Uani 1 1 d . . . H2P H 0.5059 -0.0483 0.3881 0.024 Uiso 1 1 d R . . C3P C 0.7577(2) -0.0416(2) 0.46210(18) 0.0183(3) Uani 1 1 d . . . H3P H 0.7412 -0.1059 0.5141 0.022 Uiso 1 1 d R . . C4P C 0.9228(2) 0.01736(19) 0.45994(17) 0.0148(3) Uani 1 1 d . . . C5P C 0.9356(2) 0.1088(2) 0.37961(19) 0.0187(3) Uani 1 1 d . . . H5P H 1.0441 0.1483 0.3721 0.022 Uiso 1 1 d R . . C6P C 0.7891(2) 0.1416(2) 0.31066(19) 0.0205(4) Uani 1 1 d . . . H6P H 0.8016 0.2067 0.2585 0.025 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 Zn 0.00986(14) 0.01677(15) 0.01311(14) 0.00909(11) 0.00603(10) 0.00676(10) O1W 0.0147(6) 0.0199(6) 0.0145(5) 0.0090(5) 0.0057(5) 0.0093(5) O2W 0.0140(6) 0.0308(7) 0.0201(6) 0.0188(5) 0.0108(5) 0.0128(5) O3W 0.0124(6) 0.0307(7) 0.0202(6) 0.0182(5) 0.0104(5) 0.0126(5) N1 0.0144(7) 0.0224(7) 0.0144(6) 0.0110(6) 0.0068(5) 0.0099(5) N2 0.0138(7) 0.0250(7) 0.0173(7) 0.0136(6) 0.0084(5) 0.0098(6) N3 0.0137(7) 0.0225(7) 0.0162(7) 0.0120(6) 0.0076(5) 0.0097(5) C3A 0.0130(7) 0.0144(7) 0.0118(7) 0.0058(6) 0.0055(6) 0.0058(6) N4 0.0092(6) 0.0198(7) 0.0150(6) 0.0105(6) 0.0059(5) 0.0063(5) C4 0.0120(8) 0.0249(8) 0.0216(8) 0.0135(7) 0.0095(6) 0.0069(6) C5 0.0103(7) 0.0130(7) 0.0129(7) 0.0050(6) 0.0036(6) 0.0029(6) O5 0.0128(5) 0.0217(6) 0.0156(5) 0.0118(5) 0.0053(4) 0.0051(4) N6 0.0102(6) 0.0175(6) 0.0139(6) 0.0089(5) 0.0053(5) 0.0072(5) C6 0.0143(8) 0.0249(8) 0.0200(8) 0.0150(7) 0.0074(6) 0.0115(7) C7 0.0133(7) 0.0146(7) 0.0105(7) 0.0049(6) 0.0055(6) 0.0058(6) O7 0.0124(6) 0.0237(6) 0.0158(6) 0.0103(5) 0.0080(4) 0.0091(5) C7A 0.0122(7) 0.0152(7) 0.0129(7) 0.0064(6) 0.0059(6) 0.0059(6) N1P 0.0212(7) 0.0200(7) 0.0195(7) 0.0075(6) 0.0065(6) 0.0121(6) C2P 0.0170(8) 0.0234(8) 0.0209(8) 0.0087(7) 0.0088(7) 0.0094(7) C3P 0.0187(8) 0.0211(8) 0.0197(8) 0.0110(7) 0.0092(7) 0.0094(7) C4P 0.0152(8) 0.0130(7) 0.0143(7) 0.0043(6) 0.0046(6) 0.0059(6) C5P 0.0171(8) 0.0195(8) 0.0219(8) 0.0113(7) 0.0076(7) 0.0070(6) C6P 0.0223(9) 0.0196(8) 0.0225(8) 0.0125(7) 0.0072(7) 0.0092(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O3W 2.0499(11) . ? Zn O3W 2.0499(11) 2_666 ? Zn O2W 2.0967(11) . ? Zn O2W 2.0968(11) 2_666 ? Zn O1W 2.1186(12) . ? Zn O1W 2.1186(12) 2_666 ? O1W H11W 0.831(10) . ? O1W H12W 0.832(10) . ? O2W H21W 0.838(10) . ? O2W H22W 0.843(10) . ? O3W H31W 0.840(10) . ? O3W H32W 0.839(10) . ? N1 N2 1.3167(19) . ? N1 C7A 1.362(2) . ? N2 N3 1.3656(18) . ? N3 C3A 1.339(2) . ? C3A C7A 1.376(2) . ? C3A N4 1.376(2) . ? N4 C5 1.374(2) . ? N4 C4 1.467(2) . ? C4 H41 0.9800 . ? C4 H42 0.9800 . ? C4 H43 0.9800 . ? C5 O5 1.2176(19) . ? C5 N6 1.407(2) . ? N6 C7 1.401(2) . ? N6 C6 1.4693(19) . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? C7 O7 1.230(2) . ? C7 C7A 1.429(2) . ? N1P C2P 1.340(2) . ? N1P C6P 1.341(2) . ? C2P C3P 1.387(2) . ? C2P H2P 0.9500 . ? C3P C4P 1.397(2) . ? C3P H3P 0.9500 . ? C4P C5P 1.394(2) . ? C4P C4P 1.491(3) 2_756 ? C5P C6P 1.386(2) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? 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 O3W Zn O3W 180.0 . 2_666 ? O3W Zn O2W 90.85(5) . . ? O3W Zn O2W 89.15(5) 2_666 . ? O3W Zn O2W 89.15(5) . 2_666 ? O3W Zn O2W 90.85(5) 2_666 2_666 ? O2W Zn O2W 180.0 . 2_666 ? O3W Zn O1W 88.69(5) . . ? O3W Zn O1W 91.31(5) 2_666 . ? O2W Zn O1W 89.92(5) . . ? O2W Zn O1W 90.08(5) 2_666 . ? O3W Zn O1W 91.31(5) . 2_666 ? O3W Zn O1W 88.69(5) 2_666 2_666 ? O2W Zn O1W 90.08(5) . 2_666 ? O2W Zn O1W 89.92(5) 2_666 2_666 ? O1W Zn O1W 180.0 . 2_666 ? Zn O1W H11W 114.4(15) . . ? Zn O1W H12W 113.4(18) . . ? H11W O1W H12W 102(2) . . ? Zn O2W H21W 128.8(18) . . ? Zn O2W H22W 125(2) . . ? H21W O2W H22W 106(3) . . ? Zn O3W H31W 124.5(17) . . ? Zn O3W H32W 127.6(16) . . ? H31W O3W H32W 108(2) . . ? N2 N1 C7A 106.34(13) . . ? N1 N2 N3 112.23(13) . . ? C3A N3 N2 104.70(13) . . ? N3 C3A C7A 109.46(14) . . ? N3 C3A N4 128.03(14) . . ? C7A C3A N4 122.51(14) . . ? C5 N4 C3A 119.30(13) . . ? C5 N4 C4 118.98(13) . . ? C3A N4 C4 121.71(13) . . ? N4 C4 H41 109.5 . . ? N4 C4 H42 109.3 . . ? H41 C4 H42 109.5 . . ? N4 C4 H43 109.6 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.5 . . ? O5 C5 N4 121.55(14) . . ? O5 C5 N6 121.32(14) . . ? N4 C5 N6 117.13(13) . . ? C7 N6 C5 126.74(13) . . ? C7 N6 C6 117.26(13) . . ? C5 N6 C6 115.98(13) . . ? N6 C6 H61 109.5 . . ? N6 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N6 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? O7 C7 N6 120.78(14) . . ? O7 C7 C7A 127.12(14) . . ? N6 C7 C7A 112.10(13) . . ? N1 C7A C3A 107.28(14) . . ? N1 C7A C7 130.65(14) . . ? C3A C7A C7 122.07(14) . . ? C2P N1P C6P 116.35(15) . . ? N1P C2P C3P 124.07(16) . . ? N1P C2P H2P 117.9 . . ? C3P C2P H2P 118.1 . . ? C2P C3P C4P 119.18(16) . . ? C2P C3P H3P 120.3 . . ? C4P C3P H3P 120.5 . . ? C5P C4P C3P 117.04(15) . . ? C5P C4P C4P 121.96(19) . 2_756 ? C3P C4P C4P 121.00(18) . 2_756 ? C6P C5P C4P 119.53(16) . . ? C6P C5P H5P 120.2 . . ? C4P C5P H5P 120.2 . . ? N1P C6P C5P 123.78(16) . . ? N1P C6P H6P 118.1 . . ? C5P C6P H6P 118.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H12W N1P 0.832(10) 1.988(11) 2.8080(19) 169(2) . O1W H11W O5 0.831(10) 1.906(10) 2.7357(16) 175(2) 1_554 O2W H21W O7 0.838(10) 1.919(12) 2.7299(16) 162(3) . O2W H22W N3 0.843(10) 1.942(11) 2.7780(18) 171(3) 1_655 O3W H32W N1 0.839(10) 1.933(10) 2.7713(18) 176(2) . O3W H31W N2 0.840(10) 1.940(11) 2.7721(18) 171(2) 2_566 _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.488 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.081 # Attachment '- Compound3.cif' data_cdax44 _database_code_depnum_ccdc_archive 'CCDC 827854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N2, Cd H12 O6 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C22 H32 Cd N12 O10' _chemical_formula_weight 737.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5931(4) _cell_length_b 9.0396(4) _cell_length_c 10.9308(5) _cell_angle_alpha 109.292(1) _cell_angle_beta 107.638(1) _cell_angle_gamma 101.821(1) _cell_volume 718.50(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6828 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.2 _exptl_crystal_description laminae _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 255 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 8412 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.32 _reflns_number_total 3265 _reflns_number_gt 3249 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997a). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXS97. Program for the Solution of Crystal Structures. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3265 _refine_ls_number_parameters 225 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Cd Cd 0.5000 0.5000 0.5000 0.01314(6) Uani 1 2 d S . . O1W O 0.46315(16) 0.61624(16) 0.33923(13) 0.0181(2) Uani 1 1 d D . . H11W H 0.453(3) 0.547(2) 0.2634(15) 0.022 Uiso 1 1 d D . . H12W H 0.3710(18) 0.635(3) 0.324(2) 0.022 Uiso 1 1 d D . . O2W O 0.40275(16) 0.24307(16) 0.31931(14) 0.0221(3) Uani 1 1 d D . . H21W H 0.2999(16) 0.180(2) 0.271(2) 0.027 Uiso 1 1 d D . . H22W H 0.466(3) 0.197(3) 0.287(2) 0.027 Uiso 1 1 d D . . O3W O 0.76846(16) 0.52666(16) 0.51070(14) 0.0216(3) Uani 1 1 d D . . H31W H 0.8601(19) 0.599(2) 0.5728(19) 0.026 Uiso 1 1 d D . . H32W H 0.795(3) 0.452(2) 0.461(2) 0.026 Uiso 1 1 d D . . N1 N 0.92618(18) 0.22141(18) 0.28711(15) 0.0167(3) Uani 1 1 d . . . N2 N 0.79603(18) 0.25600(18) 0.31636(15) 0.0178(3) Uani 1 1 d . . . N3 N 0.64619(18) 0.12198(18) 0.24361(15) 0.0170(3) Uani 1 1 d . . . C3A C 0.6884(2) 0.0002(2) 0.16681(17) 0.0140(3) Uani 1 1 d . . . N4 N 0.58234(18) -0.16017(18) 0.07393(15) 0.0150(3) Uani 1 1 d . . . C4 C 0.3989(2) -0.2203(2) 0.0488(2) 0.0192(3) Uani 1 1 d . . . H41 H 0.3284 -0.2785 -0.0532 0.023 Uiso 1 1 d R . . H42 H 0.3637 -0.1257 0.0899 0.023 Uiso 1 1 d R . . H43 H 0.3819 -0.2972 0.0930 0.023 Uiso 1 1 d R . . C5 C 0.6499(2) -0.2665(2) 0.00167(17) 0.0141(3) Uani 1 1 d . . . O5 O 0.55900(16) -0.40869(15) -0.08491(13) 0.0179(2) Uani 1 1 d . . . N6 N 0.82737(18) -0.20628(17) 0.03219(15) 0.0143(3) Uani 1 1 d . . . C6 C 0.8967(2) -0.3253(2) -0.04288(19) 0.0189(3) Uani 1 1 d . . . H61 H 0.8483 -0.4343 -0.0444 0.023 Uiso 1 1 d R . . H62 H 1.0235 -0.2853 0.0059 0.023 Uiso 1 1 d R . . H63 H 0.8647 -0.3358 -0.1401 0.023 Uiso 1 1 d R . . C7 C 0.9433(2) -0.0447(2) 0.12453(17) 0.0143(3) Uani 1 1 d . . . O7 O 1.09625(15) -0.00578(15) 0.14063(13) 0.0177(2) Uani 1 1 d . . . C7A C 0.8616(2) 0.0591(2) 0.19210(17) 0.0147(3) Uani 1 1 d . . . N1P N 0.1852(2) 0.7336(2) 0.31515(17) 0.0228(3) Uani 1 1 d . . . C2P C 0.2687(3) 0.8977(2) 0.3896(2) 0.0234(4) Uani 1 1 d . . . H2P H 0.3801 0.9426 0.3917 0.028 Uiso 1 1 d R . . C3P C 0.2026(2) 1.0062(2) 0.4640(2) 0.0209(4) Uani 1 1 d . . . H3P H 0.2689 1.1214 0.5168 0.025 Uiso 1 1 d R . . C4P C 0.0380(2) 0.9443(2) 0.46034(18) 0.0171(3) Uani 1 1 d . . . C5P C -0.0518(2) 0.7742(2) 0.3793(2) 0.0212(4) Uani 1 1 d . . . H5P H -0.1660 0.7264 0.3708 0.025 Uiso 1 1 d R . . C6P C 0.0268(3) 0.6752(2) 0.3110(2) 0.0241(4) Uani 1 1 d . . . H6P H -0.0356 0.5592 0.2582 0.029 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 Cd 0.01041(9) 0.01224(9) 0.01404(9) 0.00251(7) 0.00503(6) 0.00340(6) O1W 0.0192(6) 0.0173(6) 0.0153(6) 0.0034(5) 0.0067(5) 0.0075(5) O2W 0.0124(6) 0.0170(6) 0.0256(7) -0.0025(5) 0.0076(5) 0.0021(5) O3W 0.0114(6) 0.0170(6) 0.0256(7) -0.0021(5) 0.0071(5) 0.0026(5) N1 0.0134(6) 0.0152(7) 0.0156(7) 0.0010(6) 0.0045(6) 0.0045(5) N2 0.0136(7) 0.0163(7) 0.0185(7) 0.0019(6) 0.0061(6) 0.0049(6) N3 0.0142(7) 0.0159(7) 0.0163(7) 0.0020(6) 0.0057(6) 0.0047(5) C3A 0.0137(7) 0.0148(8) 0.0127(7) 0.0050(6) 0.0046(6) 0.0056(6) N4 0.0126(6) 0.0139(7) 0.0151(7) 0.0027(5) 0.0061(5) 0.0028(5) C4 0.0132(8) 0.0192(8) 0.0225(9) 0.0055(7) 0.0090(7) 0.0030(6) C5 0.0143(7) 0.0156(8) 0.0128(7) 0.0063(6) 0.0060(6) 0.0045(6) O5 0.0191(6) 0.0136(6) 0.0166(6) 0.0019(5) 0.0088(5) 0.0017(5) N6 0.0140(6) 0.0132(6) 0.0143(6) 0.0027(5) 0.0072(5) 0.0050(5) C6 0.0177(8) 0.0158(8) 0.0210(8) 0.0023(7) 0.0096(7) 0.0076(7) C7 0.0146(7) 0.0144(8) 0.0122(7) 0.0047(6) 0.0042(6) 0.0051(6) O7 0.0118(5) 0.0191(6) 0.0170(6) 0.0029(5) 0.0047(5) 0.0046(5) C7A 0.0128(7) 0.0155(8) 0.0134(7) 0.0041(6) 0.0046(6) 0.0049(6) N1P 0.0290(8) 0.0233(8) 0.0214(8) 0.0105(7) 0.0116(7) 0.0153(7) C2P 0.0217(9) 0.0273(10) 0.0239(9) 0.0108(8) 0.0105(8) 0.0114(8) C3P 0.0201(8) 0.0196(9) 0.0222(9) 0.0076(7) 0.0083(7) 0.0071(7) C4P 0.0208(8) 0.0170(8) 0.0161(8) 0.0083(7) 0.0075(7) 0.0090(7) C5P 0.0246(9) 0.0173(8) 0.0238(9) 0.0087(7) 0.0123(8) 0.0072(7) C6P 0.0317(10) 0.0168(9) 0.0237(9) 0.0070(7) 0.0114(8) 0.0101(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd O3W 2.2324(12) . ? Cd O3W 2.2325(12) 2_666 ? Cd O2W 2.2731(13) . ? Cd O2W 2.2731(13) 2_666 ? Cd O1W 2.3047(13) 2_666 ? Cd O1W 2.3047(13) . ? O1W H11W 0.823(10) . ? O1W H12W 0.823(10) . ? O2W H21W 0.835(10) . ? O2W H22W 0.839(10) . ? O3W H31W 0.825(10) . ? O3W H32W 0.834(10) . ? N1 N2 1.321(2) . ? N1 C7A 1.360(2) . ? N2 N3 1.365(2) . ? N3 C3A 1.336(2) . ? C3A N4 1.374(2) . ? C3A C7A 1.380(2) . ? N4 C5 1.374(2) . ? N4 C4 1.464(2) . ? C4 H41 0.9800 . ? C4 H42 0.9800 . ? C4 H43 0.9800 . ? C5 O5 1.223(2) . ? C5 N6 1.402(2) . ? N6 C7 1.402(2) . ? N6 C6 1.471(2) . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? C7 O7 1.229(2) . ? C7 C7A 1.430(2) . ? N1P C6P 1.336(3) . ? N1P C2P 1.337(3) . ? C2P C3P 1.388(3) . ? C2P H2P 0.9500 . ? C3P C4P 1.393(3) . ? C3P H3P 0.9500 . ? C4P C5P 1.394(3) . ? C4P C4P 1.494(3) 2_576 ? C5P C6P 1.388(3) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? 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 O3W Cd O3W 180.0 . 2_666 ? O3W Cd O2W 89.13(5) . . ? O3W Cd O2W 90.87(5) 2_666 . ? O3W Cd O2W 90.87(5) . 2_666 ? O3W Cd O2W 89.12(5) 2_666 2_666 ? O2W Cd O2W 180.0 . 2_666 ? O3W Cd O1W 91.95(5) . 2_666 ? O3W Cd O1W 88.05(5) 2_666 2_666 ? O2W Cd O1W 90.29(5) . 2_666 ? O2W Cd O1W 89.71(5) 2_666 2_666 ? O3W Cd O1W 88.05(5) . . ? O3W Cd O1W 91.95(5) 2_666 . ? O2W Cd O1W 89.70(5) . . ? O2W Cd O1W 90.29(5) 2_666 . ? O1W Cd O1W 179.999(2) 2_666 . ? Cd O1W H11W 108.7(16) . . ? Cd O1W H12W 109.5(16) . . ? H11W O1W H12W 106(2) . . ? Cd O2W H21W 127.3(17) . . ? Cd O2W H22W 124.9(17) . . ? H21W O2W H22W 108(2) . . ? Cd O3W H31W 127.5(17) . . ? Cd O3W H32W 124.3(17) . . ? H31W O3W H32W 107(2) . . ? N2 N1 C7A 106.37(13) . . ? N1 N2 N3 112.07(13) . . ? C3A N3 N2 104.90(13) . . ? N3 C3A N4 127.93(15) . . ? N3 C3A C7A 109.45(15) . . ? N4 C3A C7A 122.61(15) . . ? C3A N4 C5 119.12(14) . . ? C3A N4 C4 121.76(14) . . ? C5 N4 C4 119.12(14) . . ? N4 C4 H41 109.5 . . ? N4 C4 H42 109.5 . . ? H41 C4 H42 109.5 . . ? N4 C4 H43 109.4 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.5 . . ? O5 C5 N4 121.27(15) . . ? O5 C5 N6 121.25(15) . . ? N4 C5 N6 117.47(14) . . ? C7 N6 C5 126.68(14) . . ? C7 N6 C6 117.28(14) . . ? C5 N6 C6 116.03(14) . . ? N6 C6 H61 109.4 . . ? N6 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N6 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? O7 C7 N6 120.65(15) . . ? O7 C7 C7A 127.16(15) . . ? N6 C7 C7A 112.20(14) . . ? N1 C7A C3A 107.21(14) . . ? N1 C7A C7 130.96(15) . . ? C3A C7A C7 121.84(15) . . ? C6P N1P C2P 116.47(16) . . ? N1P C2P C3P 123.99(18) . . ? N1P C2P H2P 118.0 . . ? C3P C2P H2P 118.0 . . ? C2P C3P C4P 119.27(17) . . ? C2P C3P H3P 120.4 . . ? C4P C3P H3P 120.4 . . ? C3P C4P C5P 116.96(16) . . ? C3P C4P C4P 121.3(2) . 2_576 ? C5P C4P C4P 121.8(2) . 2_576 ? C6P C5P C4P 119.48(17) . . ? C6P C5P H5P 120.2 . . ? C4P C5P H5P 120.3 . . ? N1P C6P C5P 123.77(17) . . ? N1P C6P H6P 118.1 . . ? C5P C6P H6P 118.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H12W N1P 0.823(10) 1.974(11) 2.783(2) 167(2) . O1W H11W O5 0.823(10) 1.895(10) 2.7149(17) 174(2) 2_655 O2W H21W O7 0.835(10) 1.901(12) 2.7136(17) 164(2) 1_455 O2W H22W N3 0.839(10) 1.936(11) 2.7654(19) 170(2) . O3W H31W N1 0.825(10) 1.945(10) 2.7690(19) 176(2) 2_766 O3W H32W N2 0.834(10) 1.952(11) 2.7682(19) 166(2) . _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.70 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.536 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.073 # Attachment '- Compound4.cif' data_mnaxes _database_code_depnum_ccdc_archive 'CCDC 827855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2, H12 Mn O6 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C24 H36 Mn N12 O10' _chemical_formula_weight 707.59 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' 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 8.5542(6) _cell_length_b 10.5222(7) _cell_length_c 10.7110(7) _cell_angle_alpha 65.084(1) _cell_angle_beta 71.622(1) _cell_angle_gamma 67.507(1) _cell_volume 794.06(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5385 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.8 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 369 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 184 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 9279 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3583 _reflns_number_gt 3319 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3583 _refine_ls_number_parameters 234 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Mn Mn 0.5000 0.5000 0.5000 0.03419(11) Uani 1 2 d S . . O1W O 0.26454(14) 0.47948(15) 0.49319(13) 0.0469(3) Uani 1 1 d D . . H11W H 0.1714(18) 0.506(2) 0.5480(19) 0.056 Uiso 1 1 d D . . H12W H 0.237(3) 0.469(2) 0.4293(17) 0.056 Uiso 1 1 d D . . O2W O 0.42107(14) 0.73674(13) 0.37362(12) 0.0438(3) Uani 1 1 d D . . H21W H 0.3202(15) 0.776(2) 0.355(2) 0.053 Uiso 1 1 d D . . H22W H 0.484(2) 0.759(2) 0.2929(13) 0.053 Uiso 1 1 d D . . O3W O 0.62451(14) 0.45494(15) 0.30491(13) 0.0462(3) Uani 1 1 d D . . H31W H 0.578(2) 0.428(2) 0.266(2) 0.055 Uiso 1 1 d D . . H32W H 0.7333(13) 0.430(2) 0.275(2) 0.055 Uiso 1 1 d D . . N1 N 0.18303(17) 0.43177(17) 0.28659(14) 0.0432(3) Uani 1 1 d . . . N2 N 0.01936(17) 0.44038(18) 0.31152(15) 0.0474(3) Uani 1 1 d . . . N3 N -0.01641(17) 0.38826(17) 0.23031(15) 0.0446(3) Uani 1 1 d . . . C3A C 0.13510(18) 0.34462(17) 0.15217(15) 0.0359(3) Uani 1 1 d . . . N4 N 0.17073(16) 0.28221(15) 0.05223(13) 0.0387(3) Uani 1 1 d . . . C4 C 0.0353(2) 0.2610(2) 0.01335(19) 0.0482(4) Uani 1 1 d . . . H41 H 0.0428 0.3043 -0.0864 0.058 Uiso 1 1 d R . . H42 H -0.0756 0.3066 0.0586 0.058 Uiso 1 1 d R . . H43 H 0.0502 0.1581 0.0419 0.058 Uiso 1 1 d R . . C5 C 0.3367(2) 0.24103(18) -0.01459(15) 0.0377(3) Uani 1 1 d . . . O5 O 0.37523(15) 0.18548(15) -0.10351(12) 0.0495(3) Uani 1 1 d . . . N6 N 0.46325(16) 0.26413(16) 0.02449(14) 0.0405(3) Uani 1 1 d . . . C6 C 0.6420(2) 0.2131(3) -0.0442(2) 0.0627(5) Uani 1 1 d . . . H61 H 0.6553 0.1309 -0.0682 0.075 Uiso 1 1 d R . . H62 H 0.7184 0.1845 0.0183 0.075 Uiso 1 1 d R . . H63 H 0.6689 0.2910 -0.1277 0.075 Uiso 1 1 d R . . C7 C 0.43619(19) 0.33357(17) 0.11828(15) 0.0366(3) Uani 1 1 d . . . O7 O 0.55678(14) 0.35358(15) 0.13857(13) 0.0485(3) Uani 1 1 d . . . C7A C 0.26033(18) 0.37034(17) 0.18463(15) 0.0363(3) Uani 1 1 d . . . N1P N 0.08037(18) 0.87722(17) 0.32332(16) 0.0507(4) Uani 1 1 d . . . C2P C -0.0222(3) 0.8088(2) 0.3236(2) 0.0606(5) Uani 1 1 d . . . H2P H 0.0284 0.7219 0.3045 0.073 Uiso 1 1 d R . . C3P C -0.1989(2) 0.8596(2) 0.3495(2) 0.0589(5) Uani 1 1 d . . . H3P H -0.2643 0.8084 0.3461 0.071 Uiso 1 1 d R . . C4P C -0.2787(2) 0.98765(19) 0.38007(17) 0.0445(4) Uani 1 1 d . . . C5P C -0.1733(2) 1.0614(2) 0.3761(2) 0.0506(4) Uani 1 1 d . . . H5P H -0.2205 1.1493 0.3934 0.061 Uiso 1 1 d R . . C6P C 0.0031(2) 1.0031(2) 0.34694(19) 0.0503(4) Uani 1 1 d . . . H6P H 0.0720 1.0552 0.3435 0.060 Uiso 1 1 d R . . C7P C -0.4709(2) 1.0398(2) 0.4222(2) 0.0558(5) Uani 1 1 d . . . H71P H -0.5261 1.0232 0.3662 0.067 Uiso 1 1 d R . . H72P H -0.5065 1.1442 0.4045 0.067 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 Mn 0.02314(16) 0.0486(2) 0.03929(18) -0.02497(14) -0.00389(12) -0.00951(12) O1W 0.0271(5) 0.0785(8) 0.0535(7) -0.0416(6) -0.0017(5) -0.0177(5) O2W 0.0307(5) 0.0531(7) 0.0452(6) -0.0205(5) -0.0039(5) -0.0082(5) O3W 0.0309(5) 0.0732(8) 0.0508(7) -0.0412(6) -0.0016(5) -0.0142(5) N1 0.0315(6) 0.0654(9) 0.0438(7) -0.0327(7) -0.0014(5) -0.0142(6) N2 0.0318(7) 0.0729(10) 0.0508(8) -0.0384(7) 0.0003(6) -0.0159(6) N3 0.0304(6) 0.0669(9) 0.0476(7) -0.0329(7) 0.0000(5) -0.0165(6) C3A 0.0290(7) 0.0477(8) 0.0352(7) -0.0176(6) -0.0035(5) -0.0136(6) N4 0.0322(6) 0.0556(8) 0.0394(6) -0.0246(6) -0.0029(5) -0.0178(6) C4 0.0409(9) 0.0707(11) 0.0490(9) -0.0270(8) -0.0090(7) -0.0248(8) C5 0.0352(7) 0.0510(8) 0.0349(7) -0.0207(6) -0.0024(6) -0.0174(6) O5 0.0457(7) 0.0741(8) 0.0469(6) -0.0392(6) 0.0042(5) -0.0255(6) N6 0.0303(6) 0.0608(8) 0.0409(7) -0.0294(6) -0.0017(5) -0.0146(6) C6 0.0324(8) 0.1043(16) 0.0703(12) -0.0600(12) 0.0048(8) -0.0170(9) C7 0.0309(7) 0.0513(8) 0.0334(7) -0.0188(6) -0.0047(5) -0.0143(6) O7 0.0316(6) 0.0795(8) 0.0516(7) -0.0366(6) -0.0050(5) -0.0201(5) C7A 0.0293(7) 0.0502(8) 0.0368(7) -0.0211(6) -0.0048(6) -0.0133(6) N1P 0.0314(7) 0.0613(9) 0.0502(8) -0.0214(7) -0.0018(6) -0.0059(6) C2P 0.0468(10) 0.0581(11) 0.0783(13) -0.0375(10) -0.0084(9) -0.0032(8) C3P 0.0433(10) 0.0580(11) 0.0811(14) -0.0282(10) -0.0137(9) -0.0139(8) C4P 0.0307(7) 0.0478(9) 0.0415(8) -0.0085(7) -0.0057(6) -0.0059(6) C5P 0.0415(9) 0.0456(9) 0.0581(10) -0.0204(8) -0.0053(7) -0.0061(7) C6P 0.0403(9) 0.0562(10) 0.0526(10) -0.0166(8) -0.0045(7) -0.0176(8) C7P 0.0309(8) 0.0600(11) 0.0541(10) -0.0071(8) -0.0065(7) -0.0052(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O1W 2.1325(11) . ? Mn O1W 2.1326(11) 2_666 ? Mn O3W 2.1841(11) 2_666 ? Mn O3W 2.1842(11) . ? Mn O2W 2.2230(12) 2_666 ? Mn O2W 2.2230(12) . ? O1W H11W 0.854(9) . ? O1W H12W 0.850(9) . ? O2W H21W 0.848(9) . ? O2W H22W 0.849(9) . ? O3W H31W 0.836(9) . ? O3W H32W 0.857(9) . ? N1 N2 1.3143(19) . ? N1 C7A 1.3639(19) . ? N2 N3 1.3599(18) . ? N3 C3A 1.3325(19) . ? C3A C7A 1.370(2) . ? C3A N4 1.3797(19) . ? N4 C5 1.366(2) . ? N4 C4 1.4653(19) . ? C4 H41 0.9601 . ? C4 H42 0.9601 . ? C4 H43 0.9601 . ? C5 O5 1.2170(18) . ? C5 N6 1.4067(19) . ? N6 C7 1.3926(19) . ? N6 C6 1.470(2) . ? C6 H61 0.9601 . ? C6 H62 0.9600 . ? C6 H63 0.9601 . ? C7 O7 1.2254(18) . ? C7 C7A 1.425(2) . ? N1P C6P 1.328(2) . ? N1P C2P 1.329(3) . ? C2P C3P 1.374(3) . ? C2P H2P 0.9300 . ? C3P C4P 1.384(3) . ? C3P H3P 0.9300 . ? C4P C5P 1.378(3) . ? C4P C7P 1.503(2) . ? C5P C6P 1.381(2) . ? C5P H5P 0.9300 . ? C6P H6P 0.9300 . ? C7P C7P 1.531(4) 2_476 ? C7P H71P 0.9700 . ? C7P H72P 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Mn O1W 180.0 . 2_666 ? O1W Mn O3W 88.70(4) . 2_666 ? O1W Mn O3W 91.30(4) 2_666 2_666 ? O1W Mn O3W 91.30(4) . . ? O1W Mn O3W 88.70(4) 2_666 . ? O3W Mn O3W 180.0 2_666 . ? O1W Mn O2W 89.74(5) . 2_666 ? O1W Mn O2W 90.26(5) 2_666 2_666 ? O3W Mn O2W 88.42(5) 2_666 2_666 ? O3W Mn O2W 91.57(5) . 2_666 ? O1W Mn O2W 90.26(5) . . ? O1W Mn O2W 89.74(5) 2_666 . ? O3W Mn O2W 91.58(5) 2_666 . ? O3W Mn O2W 88.42(5) . . ? O2W Mn O2W 180.000(1) 2_666 . ? Mn O1W H11W 121.1(15) . . ? Mn O1W H12W 129.6(15) . . ? H11W O1W H12W 107(2) . . ? Mn O2W H21W 119.2(14) . . ? Mn O2W H22W 113.5(14) . . ? H21W O2W H22W 102.4(19) . . ? Mn O3W H31W 122.7(15) . . ? Mn O3W H32W 125.4(14) . . ? H31W O3W H32W 108(2) . . ? N2 N1 C7A 105.64(12) . . ? N1 N2 N3 112.81(12) . . ? C3A N3 N2 104.44(12) . . ? N3 C3A C7A 109.71(13) . . ? N3 C3A N4 128.09(13) . . ? C7A C3A N4 122.20(13) . . ? C5 N4 C3A 119.28(12) . . ? C5 N4 C4 118.70(13) . . ? C3A N4 C4 122.01(13) . . ? N4 C4 H41 109.3 . . ? N4 C4 H42 109.8 . . ? H41 C4 H42 109.5 . . ? N4 C4 H43 109.4 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.5 . . ? O5 C5 N4 121.97(14) . . ? O5 C5 N6 120.84(14) . . ? N4 C5 N6 117.19(12) . . ? C7 N6 C5 126.77(13) . . ? C7 N6 C6 116.87(13) . . ? C5 N6 C6 116.33(13) . . ? N6 C6 H61 109.6 . . ? N6 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N6 C6 H63 109.3 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? O7 C7 N6 120.65(14) . . ? O7 C7 C7A 127.30(14) . . ? N6 C7 C7A 112.03(12) . . ? N1 C7A C3A 107.38(13) . . ? N1 C7A C7 130.28(13) . . ? C3A C7A C7 122.33(13) . . ? C6P N1P C2P 116.27(15) . . ? N1P C2P C3P 123.84(18) . . ? N1P C2P H2P 118.2 . . ? C3P C2P H2P 118.0 . . ? C2P C3P C4P 119.62(18) . . ? C2P C3P H3P 120.1 . . ? C4P C3P H3P 120.2 . . ? C5P C4P C3P 116.86(16) . . ? C5P C4P C7P 121.67(17) . . ? C3P C4P C7P 121.41(17) . . ? C4P C5P C6P 119.46(17) . . ? C4P C5P H5P 120.3 . . ? C6P C5P H5P 120.2 . . ? N1P C6P C5P 123.87(17) . . ? N1P C6P H6P 118.0 . . ? C5P C6P H6P 118.1 . . ? C4P C7P C7P 110.98(18) . 2_476 ? C4P C7P H71P 109.7 . . ? C7P C7P H71P 109.7 2_476 . ? C4P C7P H72P 109.3 . . ? C7P C7P H72P 109.2 2_476 . ? H71P C7P H72P 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W N2 0.854(9) 1.926(10) 2.7749(17) 172(2) 2_566 O1W H12W N1 0.850(9) 1.946(10) 2.7948(17) 177(2) . O2W H21W N1P 0.848(9) 1.981(10) 2.8270(18) 175(2) . O2W H22W O5 0.849(9) 1.978(10) 2.8273(16) 179(2) 2_665 O3W H31W O7 0.836(9) 1.920(12) 2.7152(15) 159(2) . O3W H32W N3 0.857(9) 1.953(10) 2.8003(17) 170(2) 1_655 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 26.90 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.237 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.079 # Attachment '- Compound5.cif' data_znaxss _database_code_depnum_ccdc_archive 'CCDC 827856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 N4 O4 S2 Zn 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C32 H36 N14 O8 S2 Zn' _chemical_formula_weight 874.24 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3460(8) _cell_length_b 10.1959(10) _cell_length_c 11.7050(11) _cell_angle_alpha 100.431(1) _cell_angle_beta 97.247(2) _cell_angle_gamma 94.369(1) _cell_volume 966.73(16) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5301 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 216 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.2 _diffrn_reflns_number 11323 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.21 _reflns_number_total 4383 _reflns_number_gt 4013 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4383 _refine_ls_number_parameters 273 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 Zn Zn 0.5000 0.5000 0.5000 0.03322(10) Uani 1 2 d S . . O1W O 0.24590(14) 0.46875(13) 0.46191(13) 0.0402(3) Uani 1 1 d D . . H11W H 0.191(2) 0.5322(17) 0.480(2) 0.048 Uiso 1 1 d D . . H12W H 0.198(2) 0.4060(17) 0.4850(19) 0.048 Uiso 1 1 d D . . O2W O 0.49865(15) 0.30196(13) 0.53214(14) 0.0444(3) Uani 1 1 d D . . H21W H 0.5897(16) 0.272(2) 0.538(2) 0.053 Uiso 1 1 d D . . H22W H 0.437(2) 0.259(2) 0.5664(18) 0.053 Uiso 1 1 d D . . N1P N 0.51543(18) 0.42066(15) 0.31925(14) 0.0401(3) Uani 1 1 d . . . C2P C 0.4081(2) 0.31927(19) 0.25813(18) 0.0424(4) Uani 1 1 d . . . H2P H 0.3198 0.2897 0.2914 0.051 Uiso 1 1 d R . . C3P C 0.4175(2) 0.2570(2) 0.14639(19) 0.0494(5) Uani 1 1 d . . . H3P H 0.3391 0.1833 0.1043 0.059 Uiso 1 1 d R . . C4P C 0.5438(3) 0.2996(2) 0.09016(18) 0.0538(5) Uani 1 1 d . . . C5P C 0.6522(3) 0.4058(2) 0.15034(19) 0.0537(5) Uani 1 1 d . . . H5P H 0.7382 0.4405 0.1174 0.064 Uiso 1 1 d R . . C6P C 0.6347(2) 0.4620(2) 0.26290(18) 0.0460(4) Uani 1 1 d . . . H6P H 0.7114 0.5359 0.3067 0.055 Uiso 1 1 d R . . S S 0.55145(11) 0.21488(11) -0.05327(6) 0.1029(4) Uani 1 1 d . . . N1Q N 1.0287(3) 0.3841(3) -0.1417(2) 0.0835(7) Uani 1 1 d . . . C2Q C 0.8907(4) 0.4189(3) -0.1828(3) 0.0826(9) Uani 1 1 d . . . H2Q H 0.8885 0.4817 -0.2334 0.099 Uiso 1 1 d R . . C3Q C 0.7427(4) 0.3724(3) -0.1574(2) 0.0692(7) Uani 1 1 d . . . H3Q H 0.6428 0.3977 -0.1926 0.083 Uiso 1 1 d R . . C4Q C 0.7406(3) 0.2831(3) -0.08425(19) 0.0588(6) Uani 1 1 d . . . C5Q C 0.8841(4) 0.2423(3) -0.0405(3) 0.0785(8) Uani 1 1 d . . . H5Q H 0.8899 0.1799 0.0105 0.094 Uiso 1 1 d R . . C6Q C 1.0252(4) 0.2967(4) -0.0725(3) 0.0874(9) Uani 1 1 d . . . H6Q H 1.1268 0.2730 -0.0389 0.105 Uiso 1 1 d R . . N1 N 0.05956(18) 0.27227(15) 0.53431(15) 0.0414(4) Uani 1 1 d . . . N2 N -0.09247(19) 0.29654(16) 0.50877(17) 0.0477(4) Uani 1 1 d . . . N3 N -0.19704(18) 0.21281(16) 0.54980(16) 0.0432(4) Uani 1 1 d . . . C3A C -0.1037(2) 0.13507(16) 0.60234(16) 0.0347(4) Uani 1 1 d . . . N4 N -0.15071(17) 0.03717(15) 0.66119(14) 0.0382(3) Uani 1 1 d . . . C4 C -0.3224(2) 0.0057(2) 0.6692(2) 0.0497(5) Uani 1 1 d . . . H41 H -0.3713 -0.0800 0.6159 0.060 Uiso 1 1 d R . . H42 H -0.3837 0.0791 0.6497 0.060 Uiso 1 1 d R . . H43 H -0.3251 -0.0016 0.7506 0.060 Uiso 1 1 d R . . C5 C -0.0358(2) -0.02791(19) 0.71575(17) 0.0409(4) Uani 1 1 d . . . O5 O -0.07024(18) -0.11075(16) 0.77385(15) 0.0588(4) Uani 1 1 d . . . N6 N 0.12710(17) 0.00532(16) 0.70240(15) 0.0406(3) Uani 1 1 d . . . C6 C 0.2469(3) -0.0725(2) 0.7551(2) 0.0576(6) Uani 1 1 d . . . H61 H 0.3384 -0.0731 0.7135 0.069 Uiso 1 1 d R . . H62 H 0.1946 -0.1655 0.7452 0.069 Uiso 1 1 d R . . H63 H 0.2869 -0.0343 0.8387 0.069 Uiso 1 1 d R . . C7 C 0.1836(2) 0.10492(18) 0.64499(17) 0.0379(4) Uani 1 1 d . . . O7 O 0.32954(15) 0.12901(15) 0.64310(15) 0.0533(4) Uani 1 1 d . . . C7A C 0.05620(19) 0.16917(17) 0.59338(16) 0.0353(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02514(15) 0.03221(16) 0.04552(18) 0.01308(11) 0.00948(11) 0.00232(10) O1W 0.0274(6) 0.0347(6) 0.0639(8) 0.0189(6) 0.0131(5) 0.0039(5) O2W 0.0302(6) 0.0382(7) 0.0733(9) 0.0265(6) 0.0154(6) 0.0068(5) N1P 0.0347(7) 0.0386(8) 0.0494(9) 0.0120(7) 0.0119(6) 0.0003(6) C2P 0.0362(9) 0.0402(9) 0.0535(11) 0.0158(8) 0.0103(8) -0.0024(7) C3P 0.0441(10) 0.0473(11) 0.0537(11) 0.0087(9) 0.0061(9) -0.0102(8) C4P 0.0509(11) 0.0628(13) 0.0447(11) 0.0057(9) 0.0106(9) -0.0077(10) C5P 0.0480(11) 0.0601(13) 0.0522(12) 0.0090(10) 0.0172(9) -0.0123(9) C6P 0.0414(10) 0.0453(10) 0.0508(11) 0.0095(8) 0.0124(8) -0.0082(8) S 0.0936(6) 0.1334(8) 0.0585(4) -0.0276(4) 0.0309(4) -0.0568(5) N1Q 0.0722(16) 0.0990(19) 0.0750(15) 0.0038(14) 0.0239(13) -0.0107(14) C2Q 0.102(2) 0.083(2) 0.0651(16) 0.0233(15) 0.0193(16) -0.0094(17) C3Q 0.0719(16) 0.0788(17) 0.0578(14) 0.0173(12) 0.0048(12) 0.0109(13) C4Q 0.0662(14) 0.0647(14) 0.0410(11) 0.0002(10) 0.0133(10) -0.0073(11) C5Q 0.093(2) 0.0799(19) 0.0661(16) 0.0262(14) 0.0076(15) 0.0078(16) C6Q 0.0608(17) 0.105(2) 0.093(2) 0.0126(19) 0.0040(15) 0.0156(16) N1 0.0310(7) 0.0368(8) 0.0632(10) 0.0215(7) 0.0135(7) 0.0060(6) N2 0.0349(8) 0.0404(8) 0.0767(12) 0.0273(8) 0.0152(8) 0.0093(6) N3 0.0302(7) 0.0378(8) 0.0680(10) 0.0210(7) 0.0138(7) 0.0071(6) C3A 0.0283(8) 0.0286(8) 0.0492(10) 0.0091(7) 0.0113(7) 0.0024(6) N4 0.0279(7) 0.0350(7) 0.0566(9) 0.0169(7) 0.0144(6) 0.0012(5) C4 0.0301(9) 0.0477(11) 0.0753(14) 0.0182(10) 0.0174(9) -0.0016(7) C5 0.0340(9) 0.0388(9) 0.0535(11) 0.0163(8) 0.0113(8) -0.0007(7) O5 0.0452(8) 0.0611(9) 0.0825(11) 0.0439(8) 0.0153(7) -0.0003(7) N6 0.0296(7) 0.0418(8) 0.0562(9) 0.0233(7) 0.0079(6) 0.0037(6) C6 0.0379(10) 0.0652(14) 0.0787(15) 0.0415(12) 0.0016(10) 0.0064(9) C7 0.0297(8) 0.0373(9) 0.0505(10) 0.0156(8) 0.0103(7) 0.0022(7) O7 0.0246(6) 0.0635(9) 0.0819(10) 0.0381(8) 0.0117(6) 0.0037(6) C7A 0.0267(8) 0.0334(8) 0.0498(10) 0.0131(7) 0.0125(7) 0.0036(6) _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 Zn O1W 2.0988(12) 2_666 ? Zn O1W 2.0988(12) . ? Zn O2W 2.1192(13) . ? Zn O2W 2.1193(13) 2_666 ? Zn N1P 2.1475(16) 2_666 ? Zn N1P 2.1475(16) . ? O1W H11W 0.831(10) . ? O1W H12W 0.833(9) . ? O2W H21W 0.839(10) . ? O2W H22W 0.837(10) . ? N1P C6P 1.344(2) . ? N1P C2P 1.346(2) . ? C2P C3P 1.361(3) . ? C2P H2P 0.9307 . ? C3P C4P 1.394(3) . ? C3P H3P 0.9715 . ? C4P C5P 1.379(3) . ? C4P S 1.755(2) . ? C5P C6P 1.369(3) . ? C5P H5P 0.9319 . ? C6P H6P 0.9719 . ? S C4Q 1.782(2) . ? N1Q C2Q 1.292(4) . ? N1Q C6Q 1.309(4) . ? C2Q C3Q 1.377(4) . ? C2Q H2Q 0.9474 . ? C3Q C4Q 1.359(4) . ? C3Q H3Q 0.9567 . ? C4Q C5Q 1.367(4) . ? C5Q C6Q 1.386(4) . ? C5Q H5Q 0.9480 . ? C6Q H6Q 0.9562 . ? N1 N2 1.319(2) . ? N1 C7A 1.359(2) . ? N2 N3 1.365(2) . ? N3 C3A 1.328(2) . ? C3A N4 1.372(2) . ? C3A C7A 1.375(2) . ? N4 C5 1.366(2) . ? N4 C4 1.463(2) . ? C4 H41 1.0010 . ? C4 H42 0.9820 . ? C4 H43 0.9720 . ? C5 O5 1.216(2) . ? C5 N6 1.410(2) . ? N6 C7 1.400(2) . ? N6 C6 1.467(2) . ? C6 H61 0.9563 . ? C6 H62 0.9934 . ? C6 H63 0.9897 . ? C7 O7 1.228(2) . ? C7 C7A 1.418(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Zn O1W 179.999(1) 2_666 . ? O1W Zn O2W 91.70(5) 2_666 . ? O1W Zn O2W 88.30(5) . . ? O1W Zn O2W 88.30(5) 2_666 2_666 ? O1W Zn O2W 91.70(5) . 2_666 ? O2W Zn O2W 180.0 . 2_666 ? O1W Zn N1P 89.31(6) 2_666 2_666 ? O1W Zn N1P 90.69(6) . 2_666 ? O2W Zn N1P 91.61(6) . 2_666 ? O2W Zn N1P 88.39(6) 2_666 2_666 ? O1W Zn N1P 90.69(6) 2_666 . ? O1W Zn N1P 89.31(6) . . ? O2W Zn N1P 88.39(6) . . ? O2W Zn N1P 91.61(6) 2_666 . ? N1P Zn N1P 179.999(2) 2_666 . ? Zn O1W H11W 119.5(16) . . ? Zn O1W H12W 118.5(16) . . ? H11W O1W H12W 103(2) . . ? Zn O2W H21W 115.3(16) . . ? Zn O2W H22W 131.3(17) . . ? H21W O2W H22W 108(2) . . ? C6P N1P C2P 116.31(17) . . ? C6P N1P Zn 123.23(13) . . ? C2P N1P Zn 120.36(12) . . ? N1P C2P C3P 123.72(17) . . ? N1P C2P H2P 119.9 . . ? C3P C2P H2P 116.3 . . ? C2P C3P C4P 119.12(18) . . ? C2P C3P H3P 122.2 . . ? C4P C3P H3P 118.7 . . ? C5P C4P C3P 117.90(19) . . ? C5P C4P S 124.80(16) . . ? C3P C4P S 117.29(16) . . ? C6P C5P C4P 119.18(18) . . ? C6P C5P H5P 118.5 . . ? C4P C5P H5P 122.3 . . ? N1P C6P C5P 123.74(18) . . ? N1P C6P H6P 116.3 . . ? C5P C6P H6P 120.0 . . ? C4P S C4Q 102.96(10) . . ? C2Q N1Q C6Q 116.8(3) . . ? N1Q C2Q C3Q 124.6(3) . . ? N1Q C2Q H2Q 119.2 . . ? C3Q C2Q H2Q 116.2 . . ? C4Q C3Q C2Q 118.0(3) . . ? C4Q C3Q H3Q 120.0 . . ? C2Q C3Q H3Q 122.0 . . ? C3Q C4Q C5Q 118.9(3) . . ? C3Q C4Q S 119.7(2) . . ? C5Q C4Q S 121.3(2) . . ? C4Q C5Q C6Q 117.6(3) . . ? C4Q C5Q H5Q 122.6 . . ? C6Q C5Q H5Q 119.9 . . ? N1Q C6Q C5Q 124.0(3) . . ? N1Q C6Q H6Q 117.6 . . ? C5Q C6Q H6Q 118.4 . . ? N2 N1 C7A 106.55(14) . . ? N1 N2 N3 111.61(14) . . ? C3A N3 N2 105.19(14) . . ? N3 C3A N4 127.84(15) . . ? N3 C3A C7A 109.60(15) . . ? N4 C3A C7A 122.53(16) . . ? C5 N4 C3A 119.60(14) . . ? C5 N4 C4 119.99(15) . . ? C3A N4 C4 120.37(15) . . ? N4 C4 H41 113.0 . . ? N4 C4 H42 109.5 . . ? H41 C4 H42 108.8 . . ? N4 C4 H43 104.9 . . ? H41 C4 H43 110.1 . . ? H42 C4 H43 110.5 . . ? O5 C5 N4 122.25(16) . . ? O5 C5 N6 120.74(17) . . ? N4 C5 N6 117.01(15) . . ? C7 N6 C5 126.23(15) . . ? C7 N6 C6 117.87(15) . . ? C5 N6 C6 115.89(15) . . ? N6 C6 H61 108.6 . . ? N6 C6 H62 107.1 . . ? H61 C6 H62 109.4 . . ? N6 C6 H63 113.0 . . ? H61 C6 H63 107.5 . . ? H62 C6 H63 111.2 . . ? O7 C7 N6 120.56(16) . . ? O7 C7 C7A 126.76(16) . . ? N6 C7 C7A 112.68(14) . . ? N1 C7A C3A 107.05(15) . . ? N1 C7A C7 131.07(15) . . ? C3A C7A C7 121.81(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W N2 0.831(10) 1.977(11) 2.786(2) 164(2) 2_566 O1W H12W N1 0.833(9) 1.933(10) 2.7609(19) 172(2) . O2W H21W N3 0.839(10) 1.920(10) 2.758(2) 177(2) 1_655 O2W H22W O7 0.837(10) 1.953(11) 2.7751(18) 167(2) . _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.80 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.437 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.056 # Attachment '- Compound6.cif' data_cdaxss _database_code_depnum_ccdc_archive 'CCDC 827857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Cd N4 O4 S2 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C32 H36 Cd N14 O8 S2' _chemical_formula_weight 921.27 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4223(6) _cell_length_b 10.1249(7) _cell_length_c 11.7854(8) _cell_angle_alpha 100.942(1) _cell_angle_beta 99.816(1) _cell_angle_gamma 94.821(1) _cell_volume 965.22(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7611 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.2 _exptl_crystal_description laminae _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 system' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 280 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 11246 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.25 _reflns_number_total 4355 _reflns_number_gt 4228 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _publ_section_references ; Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Winsconsin, USA. Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western Australia, Perth, Australia. Sheldrick, G.M. (1997a). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXS97. Program for the Solution of Crystal Structures. University of G\"ottingen, Germany. ; _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. Hydrogen atoms of the heterocycles were placed in ideal positions. Hydrogen atoms of water molecules were located in \DF maps and then refined with restrained (SHELX-97 DFIX command) O-H distances (0.84 \%A). An isotropic thermal parameter fixed to 1.2 times the Uiso of their parent atoms was used for all hydrogen atoms. A relatively high residual peak (~1.2 e/\%A^3^ ) remains in the final \DF map, close to the sulphur atom, suggesting high thermal motion or even disorder in this region of the structure. Attempts to find a model to account for this hypothethical disorder did not yield reasonable results. ; _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^)+(0.0500P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4355 _refine_ls_number_parameters 273 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.058 _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 Cd Cd 0.5000 0.5000 0.5000 0.01387(8) Uani 1 2 d S . . O1W O 0.22244(17) 0.45967(15) 0.44931(14) 0.0181(3) Uani 1 1 d D . . H11W H 0.177(3) 0.5259(18) 0.473(2) 0.022 Uiso 1 1 d D . . H12W H 0.180(3) 0.402(2) 0.480(2) 0.022 Uiso 1 1 d D . . O2W O 0.49681(18) 0.28203(15) 0.52953(14) 0.0196(3) Uani 1 1 d D . . H21W H 0.5874(18) 0.254(3) 0.541(2) 0.023 Uiso 1 1 d D . . H22W H 0.438(3) 0.247(3) 0.569(2) 0.023 Uiso 1 1 d D . . N1P N 0.5148(2) 0.41641(17) 0.30690(16) 0.0182(3) Uani 1 1 d . . . C2P C 0.4056(3) 0.3130(2) 0.24269(19) 0.0191(4) Uani 1 1 d . . . H2P H 0.3173 0.2835 0.2760 0.023 Uiso 1 1 d R . . C3P C 0.4161(3) 0.2485(2) 0.13089(19) 0.0213(4) Uani 1 1 d . . . H3P H 0.3377 0.1748 0.0888 0.026 Uiso 1 1 d R . . C4P C 0.5434(3) 0.2924(2) 0.08013(19) 0.0229(4) Uani 1 1 d . . . C5P C 0.6534(3) 0.4021(2) 0.14405(19) 0.0221(4) Uani 1 1 d . . . H5P H 0.7394 0.4367 0.1112 0.026 Uiso 1 1 d R . . C6P C 0.6354(3) 0.4593(2) 0.25622(19) 0.0195(4) Uani 1 1 d . . . H6P H 0.7122 0.5332 0.3001 0.023 Uiso 1 1 d R . . S S 0.55248(9) 0.20445(8) -0.06205(6) 0.04056(18) Uani 1 1 d . . . N1Q N 1.0248(3) 0.3924(2) -0.1360(2) 0.0347(5) Uani 1 1 d . . . C2Q C 0.8822(3) 0.4245(3) -0.1822(2) 0.0325(5) Uani 1 1 d . . . H2Q H 0.8801 0.4873 -0.2328 0.039 Uiso 1 1 d R . . C3Q C 0.7350(3) 0.3707(2) -0.1606(2) 0.0298(5) Uani 1 1 d . . . H3Q H 0.6351 0.3960 -0.1958 0.036 Uiso 1 1 d R . . C4Q C 0.7387(3) 0.2805(2) -0.0873(2) 0.0260(5) Uani 1 1 d . . . C5Q C 0.8859(3) 0.2449(3) -0.0377(2) 0.0323(5) Uani 1 1 d . . . H5Q H 0.8916 0.1825 0.0134 0.039 Uiso 1 1 d R . . C6Q C 1.0251(3) 0.3044(3) -0.0654(2) 0.0364(6) Uani 1 1 d . . . H6Q H 1.1268 0.2807 -0.0318 0.044 Uiso 1 1 d R . . N1 N 0.0605(2) 0.26743(17) 0.54071(16) 0.0176(3) Uani 1 1 d . . . N2 N -0.0913(2) 0.29462(17) 0.51868(17) 0.0194(4) Uani 1 1 d . . . N3 N -0.1932(2) 0.21145(17) 0.56012(16) 0.0180(3) Uani 1 1 d . . . C3A C -0.0982(2) 0.13079(19) 0.60988(17) 0.0152(4) Uani 1 1 d . . . N4 N -0.1425(2) 0.03203(17) 0.66792(16) 0.0169(3) Uani 1 1 d . . . C4 C -0.3110(2) 0.0029(2) 0.6807(2) 0.0209(4) Uani 1 1 d . . . H41 H -0.3602 -0.0821 0.6266 0.025 Uiso 1 1 d R . . H42 H -0.3719 0.0769 0.6622 0.025 Uiso 1 1 d R . . H43 H -0.3135 -0.0055 0.7619 0.025 Uiso 1 1 d R . . C5 C -0.0256(2) -0.0368(2) 0.71831(18) 0.0182(4) Uani 1 1 d . . . O5 O -0.05697(18) -0.12111(16) 0.77554(15) 0.0242(3) Uani 1 1 d . . . N6 N 0.1340(2) -0.00652(17) 0.70155(16) 0.0172(3) Uani 1 1 d . . . C6 C 0.2534(3) -0.0891(2) 0.7499(2) 0.0231(4) Uani 1 1 d . . . H61 H 0.3492 -0.0824 0.7134 0.028 Uiso 1 1 d R . . H62 H 0.2051 -0.1838 0.7332 0.028 Uiso 1 1 d R . . H63 H 0.2855 -0.0560 0.8352 0.028 Uiso 1 1 d R . . C7 C 0.1888(2) 0.0941(2) 0.64530(18) 0.0166(4) Uani 1 1 d . . . O7 O 0.33266(17) 0.11534(15) 0.64023(14) 0.0215(3) Uani 1 1 d . . . C7A C 0.0594(2) 0.16294(19) 0.59840(18) 0.0153(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.01380(11) 0.01060(11) 0.01926(12) 0.00551(7) 0.00578(7) 0.00230(7) O1W 0.0173(7) 0.0128(7) 0.0281(8) 0.0096(6) 0.0084(6) 0.0033(5) O2W 0.0156(7) 0.0152(7) 0.0326(8) 0.0124(6) 0.0079(6) 0.0041(5) N1P 0.0193(8) 0.0140(8) 0.0231(9) 0.0059(7) 0.0065(7) 0.0020(6) C2P 0.0188(10) 0.0152(9) 0.0259(11) 0.0087(8) 0.0059(8) 0.0026(7) C3P 0.0223(10) 0.0169(10) 0.0236(11) 0.0057(8) 0.0020(8) -0.0028(8) C4P 0.0265(11) 0.0224(11) 0.0193(10) 0.0034(8) 0.0059(8) -0.0003(9) C5P 0.0239(10) 0.0198(10) 0.0235(11) 0.0055(8) 0.0085(8) -0.0026(8) C6P 0.0196(10) 0.0154(9) 0.0232(10) 0.0047(8) 0.0047(8) -0.0012(8) S 0.0420(4) 0.0461(4) 0.0254(3) -0.0088(3) 0.0139(3) -0.0189(3) N1Q 0.0334(11) 0.0361(12) 0.0334(12) 0.0016(9) 0.0130(9) -0.0026(9) C2Q 0.0448(15) 0.0287(12) 0.0250(12) 0.0080(10) 0.0085(10) -0.0001(11) C3Q 0.0362(13) 0.0272(12) 0.0243(11) 0.0048(9) -0.0002(10) 0.0072(10) C4Q 0.0329(12) 0.0233(11) 0.0195(10) -0.0004(9) 0.0075(9) -0.0030(9) C5Q 0.0404(14) 0.0285(12) 0.0283(12) 0.0100(10) 0.0027(10) 0.0040(10) C6Q 0.0290(13) 0.0361(14) 0.0416(15) 0.0049(12) 0.0013(11) 0.0074(11) N1 0.0163(8) 0.0131(8) 0.0258(9) 0.0081(7) 0.0063(7) 0.0025(6) N2 0.0176(8) 0.0141(8) 0.0302(10) 0.0100(7) 0.0083(7) 0.0035(6) N3 0.0173(8) 0.0130(8) 0.0267(9) 0.0084(7) 0.0070(7) 0.0030(6) C3A 0.0165(9) 0.0106(8) 0.0197(9) 0.0045(7) 0.0057(7) 0.0017(7) N4 0.0151(8) 0.0131(8) 0.0255(9) 0.0085(7) 0.0071(6) 0.0013(6) C4 0.0160(9) 0.0169(10) 0.0325(11) 0.0080(8) 0.0097(8) 0.0000(7) C5 0.0186(10) 0.0148(9) 0.0224(10) 0.0061(8) 0.0054(8) 0.0007(7) O5 0.0214(7) 0.0222(8) 0.0346(9) 0.0177(7) 0.0080(6) 0.0017(6) N6 0.0149(8) 0.0146(8) 0.0252(9) 0.0106(7) 0.0043(7) 0.0032(6) C6 0.0183(10) 0.0205(10) 0.0339(12) 0.0150(9) 0.0030(8) 0.0043(8) C7 0.0179(9) 0.0130(9) 0.0203(10) 0.0057(7) 0.0048(7) 0.0014(7) O7 0.0149(7) 0.0218(8) 0.0316(8) 0.0137(6) 0.0060(6) 0.0028(6) C7A 0.0152(9) 0.0110(9) 0.0213(10) 0.0061(7) 0.0047(7) 0.0013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd O1W 2.2933(15) . ? Cd O1W 2.2933(15) 2_666 ? Cd O2W 2.2972(14) 2_666 ? Cd O2W 2.2973(14) . ? Cd N1P 2.3009(18) . ? Cd N1P 2.3009(18) 2_666 ? O1W H11W 0.828(10) . ? O1W H12W 0.831(10) . ? O2W H21W 0.836(10) . ? O2W H22W 0.836(10) . ? N1P C6P 1.345(3) . ? N1P C2P 1.347(3) . ? C2P C3P 1.376(3) . ? C2P H2P 0.9500 . ? C3P C4P 1.395(3) . ? C3P H3P 0.9500 . ? C4P C5P 1.389(3) . ? C4P S 1.759(2) . ? C5P C6P 1.378(3) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? S C4Q 1.785(2) . ? N1Q C2Q 1.325(4) . ? N1Q C6Q 1.329(4) . ? C2Q C3Q 1.395(4) . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.369(3) . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.384(4) . ? C5Q C6Q 1.390(4) . ? C5Q H5Q 0.9500 . ? C6Q H6Q 0.9500 . ? N1 N2 1.323(2) . ? N1 C7A 1.362(3) . ? N2 N3 1.365(2) . ? N3 C3A 1.335(3) . ? C3A N4 1.375(3) . ? C3A C7A 1.376(3) . ? N4 C5 1.371(3) . ? N4 C4 1.464(3) . ? C4 H41 0.9800 . ? C4 H42 0.9800 . ? C4 H43 0.9800 . ? C5 O5 1.223(3) . ? C5 N6 1.409(3) . ? N6 C7 1.404(3) . ? N6 C6 1.470(2) . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? C7 O7 1.226(2) . ? C7 C7A 1.431(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 O1W Cd O1W 180.0 . 2_666 ? O1W Cd O2W 92.55(5) . 2_666 ? O1W Cd O2W 87.45(5) 2_666 2_666 ? O1W Cd O2W 87.45(5) . . ? O1W Cd O2W 92.55(5) 2_666 . ? O2W Cd O2W 180.0 2_666 . ? O1W Cd N1P 89.07(6) . . ? O1W Cd N1P 90.93(6) 2_666 . ? O2W Cd N1P 91.93(6) 2_666 . ? O2W Cd N1P 88.07(6) . . ? O1W Cd N1P 90.93(6) . 2_666 ? O1W Cd N1P 89.07(6) 2_666 2_666 ? O2W Cd N1P 88.07(6) 2_666 2_666 ? O2W Cd N1P 91.93(6) . 2_666 ? N1P Cd N1P 180.0 . 2_666 ? Cd O1W H11W 113.1(18) . . ? Cd O1W H12W 114.9(18) . . ? H11W O1W H12W 101(3) . . ? Cd O2W H21W 115.6(18) . . ? Cd O2W H22W 125.2(19) . . ? H21W O2W H22W 109(3) . . ? C6P N1P C2P 117.38(19) . . ? C6P N1P Cd 122.96(14) . . ? C2P N1P Cd 119.48(14) . . ? N1P C2P C3P 122.9(2) . . ? N1P C2P H2P 118.6 . . ? C3P C2P H2P 118.5 . . ? C2P C3P C4P 119.1(2) . . ? C2P C3P H3P 120.5 . . ? C4P C3P H3P 120.4 . . ? C5P C4P C3P 118.4(2) . . ? C5P C4P S 124.44(17) . . ? C3P C4P S 117.16(17) . . ? C6P C5P C4P 118.6(2) . . ? C6P C5P H5P 120.7 . . ? C4P C5P H5P 120.7 . . ? N1P C6P C5P 123.50(19) . . ? N1P C6P H6P 118.2 . . ? C5P C6P H6P 118.3 . . ? C4P S C4Q 102.75(11) . . ? C2Q N1Q C6Q 117.3(2) . . ? N1Q C2Q C3Q 123.4(2) . . ? N1Q C2Q H2Q 118.3 . . ? C3Q C2Q H2Q 118.3 . . ? C4Q C3Q C2Q 118.1(2) . . ? C4Q C3Q H3Q 121.1 . . ? C2Q C3Q H3Q 120.9 . . ? C3Q C4Q C5Q 119.9(2) . . ? C3Q C4Q S 119.39(19) . . ? C5Q C4Q S 120.65(19) . . ? C4Q C5Q C6Q 117.2(2) . . ? C4Q C5Q H5Q 121.5 . . ? C6Q C5Q H5Q 121.3 . . ? N1Q C6Q C5Q 124.1(2) . . ? N1Q C6Q H6Q 118.0 . . ? C5Q C6Q H6Q 117.9 . . ? N2 N1 C7A 106.41(16) . . ? N1 N2 N3 111.77(16) . . ? C3A N3 N2 105.07(16) . . ? N3 C3A N4 127.71(18) . . ? N3 C3A C7A 109.55(17) . . ? N4 C3A C7A 122.71(18) . . ? C5 N4 C3A 119.33(17) . . ? C5 N4 C4 119.54(17) . . ? C3A N4 C4 121.09(17) . . ? N4 C4 H41 109.5 . . ? N4 C4 H42 109.5 . . ? H41 C4 H42 109.5 . . ? N4 C4 H43 109.4 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.5 . . ? O5 C5 N4 122.05(19) . . ? O5 C5 N6 120.76(19) . . ? N4 C5 N6 117.19(17) . . ? C7 N6 C5 126.61(17) . . ? C7 N6 C6 117.89(17) . . ? C5 N6 C6 115.49(16) . . ? N6 C6 H61 109.5 . . ? N6 C6 H62 109.4 . . ? H61 C6 H62 109.5 . . ? N6 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? O7 C7 N6 120.93(18) . . ? O7 C7 C7A 126.99(19) . . ? N6 C7 C7A 112.08(17) . . ? N1 C7A C3A 107.18(17) . . ? N1 C7A C7 130.85(18) . . ? C3A C7A C7 121.94(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W N2 0.828(10) 2.002(13) 2.793(2) 159(3) 2_566 O1W H12W N1 0.831(10) 1.939(10) 2.767(2) 174(3) . O2W H21W N3 0.836(10) 1.917(11) 2.747(2) 172(3) 1_655 O2W H22W O7 0.836(10) 1.938(13) 2.742(2) 161(3) . _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 26.70 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.228 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.087