# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lu, Jianmei' _publ_contact_author_email lujm@suda.edu.cn _publ_section_title ; Hydrothermal Synthesis, Structure, and Luminescent Properties of Selected Zn(II)/Cd(II) Coordination Polymers Constructed from 3,5-bis(x-pyridyl)- 1,2,4-triazole( x = 3, 4) ; loop_ _publ_author_name 'Qingfeng Xu' 'Jianfeng Ge' 'Qiu-Xuan Zhou' 'Jianmei Lu' 'Shun-Jun Ji' ; Lihua Wang ; 'Yong Zhang' 'Xue-Ming Jin' 'Bing Wu' # Attachment '- Zn-6.cif' data_shelxl6 _database_code_depnum_ccdc_archive 'CCDC 666420' #TrackingRef '- Zn-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 N5 O5 S Zn2' _chemical_formula_sum 'C12 H9 N5 O5 S Zn2' _chemical_formula_weight 466.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.293(7) _cell_length_b 15.308(13) _cell_length_c 13.087(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.46(3) _cell_angle_gamma 90.00 _cell_volume 1432(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4197 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 3.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.392 _exptl_absorpt_correction_T_max 0.493 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6738 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2611 _reflns_number_gt 2154 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The hydrogen atom of OH group was found in Fourier maps, and its coordinates and isotropic temperature factors were refined. O-H distance was constrained. 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^)+(0.0301P)^2^+1.6088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2611 _refine_ls_number_parameters 231 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.71824(7) 0.41009(3) 0.59876(4) 0.02073(16) Uani 1 1 d . . . Zn2 Zn 0.93322(7) 0.47476(3) 0.23300(4) 0.01851(15) Uani 1 1 d . . . S1 S 0.65399(15) 0.49901(7) 0.38304(8) 0.0199(3) Uani 1 1 d . . . O1 O 0.7843(4) 0.46679(19) 0.4767(2) 0.0235(7) Uani 1 1 d . . . O2 O 0.7687(5) 0.5342(2) 0.3114(3) 0.0339(8) Uani 1 1 d . . . O3 O 0.5504(4) 0.57471(19) 0.4145(2) 0.0247(7) Uani 1 1 d . . . O4 O 0.5298(5) 0.4310(2) 0.3367(3) 0.0368(9) Uani 1 1 d . . . O5 O 0.8532(4) 0.4484(2) 0.7317(2) 0.0233(7) Uani 1 1 d D . . H5A H 0.779(6) 0.451(3) 0.771(3) 0.038(16) Uiso 1 1 d D . . N1 N 0.7350(5) 0.2823(2) 0.5647(3) 0.0240(9) Uani 1 1 d . . . N2 N 1.0018(5) -0.3557(2) 0.6998(3) 0.0220(8) Uani 1 1 d . . . N3 N 0.6885(5) -0.0341(2) 0.4173(3) 0.0197(8) Uani 1 1 d . . . N4 N 0.7298(5) -0.1201(2) 0.4389(3) 0.0222(8) Uani 1 1 d . . . N5 N 0.8255(5) -0.0426(2) 0.5850(3) 0.0204(8) Uani 1 1 d . . . C1 C 0.8213(7) 0.2250(3) 0.6362(4) 0.0306(12) Uani 1 1 d . . . H1 H 0.8794 0.2460 0.7013 0.037 Uiso 1 1 calc R . . C2 C 0.8273(7) 0.1381(3) 0.6178(4) 0.0286(11) Uani 1 1 d . . . H2 H 0.8903 0.1009 0.6692 0.034 Uiso 1 1 calc R . . C3 C 0.7391(6) 0.1043(3) 0.5216(3) 0.0199(10) Uani 1 1 d . . . C4 C 0.6518(6) 0.1628(3) 0.4477(4) 0.0261(11) Uani 1 1 d . . . H4 H 0.5924 0.1434 0.3821 0.031 Uiso 1 1 calc R . . C5 C 0.6534(6) 0.2502(3) 0.4721(4) 0.0276(11) Uani 1 1 d . . . H5B H 0.5945 0.2889 0.4213 0.033 Uiso 1 1 calc R . . C6 C 0.8904(7) -0.3570(3) 0.6050(4) 0.0315(12) Uani 1 1 d . . . H6 H 0.8539 -0.4109 0.5747 0.038 Uiso 1 1 calc R . . C7 C 0.8279(7) -0.2825(3) 0.5504(4) 0.0292(11) Uani 1 1 d . . . H7 H 0.7520 -0.2864 0.4845 0.035 Uiso 1 1 calc R . . C8 C 0.8781(6) -0.2023(3) 0.5939(3) 0.0201(10) Uani 1 1 d . . . C9 C 0.9968(7) -0.2008(3) 0.6909(3) 0.0272(11) Uani 1 1 d . . . H9 H 1.0371 -0.1478 0.7223 0.033 Uiso 1 1 calc R . . C10 C 1.0538(7) -0.2774(3) 0.7400(3) 0.0266(11) Uani 1 1 d . . . H10 H 1.1333 -0.2750 0.8050 0.032 Uiso 1 1 calc R . . C11 C 0.7475(6) 0.0098(3) 0.5063(3) 0.0168(9) Uani 1 1 d . . . C12 C 0.8123(6) -0.1220(3) 0.5389(3) 0.0176(9) 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 Zn1 0.0249(3) 0.0151(3) 0.0202(3) -0.0011(2) -0.0004(2) 0.0006(2) Zn2 0.0239(3) 0.0143(3) 0.0155(3) -0.0001(2) -0.0005(2) 0.0004(2) S1 0.0256(6) 0.0177(5) 0.0152(6) -0.0006(4) 0.0013(4) 0.0026(5) O1 0.0239(16) 0.0244(17) 0.0197(17) 0.0029(13) -0.0015(13) 0.0023(14) O2 0.047(2) 0.0295(18) 0.032(2) 0.0131(15) 0.0241(16) 0.0113(16) O3 0.0256(17) 0.0204(16) 0.0281(19) -0.0056(13) 0.0055(14) 0.0035(14) O4 0.047(2) 0.0239(18) 0.031(2) -0.0048(15) -0.0125(16) -0.0061(17) O5 0.0207(16) 0.0284(18) 0.0191(18) -0.0031(14) 0.0002(14) -0.0021(15) N1 0.029(2) 0.0160(19) 0.026(2) -0.0042(16) 0.0042(17) 0.0012(17) N2 0.027(2) 0.0155(19) 0.021(2) 0.0015(15) 0.0012(16) 0.0032(17) N3 0.027(2) 0.0127(18) 0.017(2) 0.0031(15) -0.0005(15) 0.0007(16) N4 0.031(2) 0.0140(18) 0.019(2) 0.0002(15) -0.0003(16) 0.0008(17) N5 0.026(2) 0.0176(19) 0.016(2) 0.0010(15) 0.0022(16) -0.0011(17) C1 0.040(3) 0.023(3) 0.025(3) -0.002(2) -0.004(2) 0.003(2) C2 0.043(3) 0.018(2) 0.021(3) 0.0015(19) -0.005(2) 0.005(2) C3 0.022(2) 0.015(2) 0.022(2) 0.0001(18) 0.0021(18) 0.0009(19) C4 0.035(3) 0.020(2) 0.019(3) -0.0008(19) -0.005(2) -0.001(2) C5 0.031(3) 0.019(2) 0.027(3) 0.003(2) -0.007(2) 0.005(2) C6 0.042(3) 0.015(2) 0.030(3) -0.002(2) -0.011(2) -0.005(2) C7 0.036(3) 0.020(2) 0.024(3) -0.001(2) -0.012(2) 0.002(2) C8 0.027(2) 0.015(2) 0.018(2) 0.0029(18) 0.0036(18) -0.002(2) C9 0.039(3) 0.015(2) 0.022(3) -0.0022(19) -0.006(2) -0.001(2) C10 0.038(3) 0.019(2) 0.016(2) -0.0019(19) -0.009(2) 0.002(2) C11 0.022(2) 0.014(2) 0.014(2) 0.0004(17) 0.0033(17) 0.0012(19) C12 0.022(2) 0.013(2) 0.017(2) 0.0012(17) 0.0026(18) 0.0001(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.913(3) . ? Zn1 O3 1.946(4) 3_666 ? Zn1 O1 1.960(3) . ? Zn1 N1 2.015(4) . ? Zn2 O5 1.933(3) 3_766 ? Zn2 O2 1.951(3) . ? Zn2 N3 1.996(4) 2_655 ? Zn2 N2 2.037(4) 3_756 ? S1 O4 1.434(3) . ? S1 O2 1.477(3) . ? S1 O1 1.479(3) . ? S1 O3 1.486(3) . ? O3 Zn1 1.946(4) 3_666 ? O5 Zn2 1.933(3) 3_766 ? O5 H5A 0.818(10) . ? N1 C5 1.334(6) . ? N1 C1 1.345(6) . ? N2 C10 1.333(6) . ? N2 C6 1.342(6) . ? N2 Zn2 2.037(4) 3_756 ? N3 C11 1.340(5) . ? N3 N4 1.368(5) . ? N3 Zn2 1.996(4) 2_645 ? N4 C12 1.327(5) . ? N5 C11 1.339(5) . ? N5 C12 1.351(5) . ? C1 C2 1.355(6) . ? C1 H1 0.9300 . ? C2 C3 1.394(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 C11 1.464(6) . ? C4 C5 1.375(6) . ? C4 H4 0.9300 . ? C5 H5B 0.9300 . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C7 C8 1.372(6) . ? C7 H7 0.9300 . ? C8 C9 1.388(6) . ? C8 C12 1.458(6) . ? C9 C10 1.362(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 Zn1 O3 111.81(14) . 3_666 ? O5 Zn1 O1 116.10(14) . . ? O3 Zn1 O1 106.27(13) 3_666 . ? O5 Zn1 N1 117.13(14) . . ? O3 Zn1 N1 101.57(14) 3_666 . ? O1 Zn1 N1 102.35(14) . . ? O5 Zn2 O2 98.10(15) 3_766 . ? O5 Zn2 N3 117.14(14) 3_766 2_655 ? O2 Zn2 N3 110.51(15) . 2_655 ? O5 Zn2 N2 109.48(15) 3_766 3_756 ? O2 Zn2 N2 107.76(14) . 3_756 ? N3 Zn2 N2 112.61(14) 2_655 3_756 ? O4 S1 O2 112.8(2) . . ? O4 S1 O1 110.87(19) . . ? O2 S1 O1 107.2(2) . . ? O4 S1 O3 111.7(2) . . ? O2 S1 O3 105.97(19) . . ? O1 S1 O3 107.97(18) . . ? S1 O1 Zn1 126.99(19) . . ? S1 O2 Zn2 130.4(2) . . ? S1 O3 Zn1 128.82(19) . 3_666 ? Zn1 O5 Zn2 130.42(18) . 3_766 ? Zn1 O5 H5A 107(4) . . ? Zn2 O5 H5A 115(4) 3_766 . ? C5 N1 C1 117.1(4) . . ? C5 N1 Zn1 121.6(3) . . ? C1 N1 Zn1 121.3(3) . . ? C10 N2 C6 116.8(4) . . ? C10 N2 Zn2 127.6(3) . 3_756 ? C6 N2 Zn2 115.6(3) . 3_756 ? C11 N3 N4 106.5(3) . . ? C11 N3 Zn2 145.7(3) . 2_645 ? N4 N3 Zn2 107.8(2) . 2_645 ? C12 N4 N3 105.2(3) . . ? C11 N5 C12 102.3(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.9(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 117.4(4) . . ? C4 C3 C11 124.9(4) . . ? C2 C3 C11 117.7(4) . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.5(4) . . ? N1 C5 H5B 118.3 . . ? C4 C5 H5B 118.3 . . ? N2 C6 C7 123.1(4) . . ? N2 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C8 C7 C6 119.6(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 117.5(4) . . ? C7 C8 C12 121.1(4) . . ? C9 C8 C12 121.5(4) . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 123.5(4) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N5 C11 N3 112.5(4) . . ? N5 C11 C3 120.7(4) . . ? N3 C11 C3 126.8(4) . . ? N4 C12 N5 113.5(4) . . ? N4 C12 C8 123.0(4) . . ? N5 C12 C8 123.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Zn1 -54.9(3) . . . . ? O2 S1 O1 Zn1 -178.4(2) . . . . ? O3 S1 O1 Zn1 67.8(3) . . . . ? O5 Zn1 O1 S1 -136.1(2) . . . . ? O3 Zn1 O1 S1 -11.1(3) 3_666 . . . ? N1 Zn1 O1 S1 95.1(2) . . . . ? O4 S1 O2 Zn2 -54.4(3) . . . . ? O1 S1 O2 Zn2 68.0(3) . . . . ? O3 S1 O2 Zn2 -176.9(2) . . . . ? O5 Zn2 O2 S1 -132.6(3) 3_766 . . . ? N3 Zn2 O2 S1 104.4(3) 2_655 . . . ? N2 Zn2 O2 S1 -19.1(3) 3_756 . . . ? O4 S1 O3 Zn1 0.4(3) . . . 3_666 ? O2 S1 O3 Zn1 123.6(2) . . . 3_666 ? O1 S1 O3 Zn1 -121.8(2) . . . 3_666 ? O3 Zn1 O5 Zn2 -130.3(2) 3_666 . . 3_766 ? O1 Zn1 O5 Zn2 -8.1(3) . . . 3_766 ? N1 Zn1 O5 Zn2 113.1(2) . . . 3_766 ? O5 Zn1 N1 C5 -176.7(3) . . . . ? O3 Zn1 N1 C5 61.2(4) 3_666 . . . ? O1 Zn1 N1 C5 -48.5(4) . . . . ? O5 Zn1 N1 C1 6.6(4) . . . . ? O3 Zn1 N1 C1 -115.4(4) 3_666 . . . ? O1 Zn1 N1 C1 134.8(4) . . . . ? C11 N3 N4 C12 -0.6(5) . . . . ? Zn2 N3 N4 C12 179.2(3) 2_645 . . . ? C5 N1 C1 C2 -0.2(7) . . . . ? Zn1 N1 C1 C2 176.7(4) . . . . ? N1 C1 C2 C3 -1.0(8) . . . . ? C1 C2 C3 C4 1.4(7) . . . . ? C1 C2 C3 C11 -179.1(4) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C11 C3 C4 C5 179.8(4) . . . . ? C1 N1 C5 C4 0.9(7) . . . . ? Zn1 N1 C5 C4 -175.9(4) . . . . ? C3 C4 C5 N1 -0.4(8) . . . . ? C10 N2 C6 C7 -1.1(7) . . . . ? Zn2 N2 C6 C7 177.6(4) 3_756 . . . ? N2 C6 C7 C8 -0.7(8) . . . . ? C6 C7 C8 C9 2.1(7) . . . . ? C6 C7 C8 C12 -179.1(4) . . . . ? C7 C8 C9 C10 -1.8(7) . . . . ? C12 C8 C9 C10 179.5(4) . . . . ? C6 N2 C10 C9 1.5(7) . . . . ? Zn2 N2 C10 C9 -177.1(4) 3_756 . . . ? C8 C9 C10 N2 0.0(8) . . . . ? C12 N5 C11 N3 0.4(5) . . . . ? C12 N5 C11 C3 -177.6(4) . . . . ? N4 N3 C11 N5 0.1(5) . . . . ? Zn2 N3 C11 N5 -179.5(4) 2_645 . . . ? N4 N3 C11 C3 178.0(4) . . . . ? Zn2 N3 C11 C3 -1.6(8) 2_645 . . . ? C4 C3 C11 N5 -175.7(4) . . . . ? C2 C3 C11 N5 4.8(6) . . . . ? C4 C3 C11 N3 6.5(7) . . . . ? C2 C3 C11 N3 -172.9(4) . . . . ? N3 N4 C12 N5 0.9(5) . . . . ? N3 N4 C12 C8 179.6(4) . . . . ? C11 N5 C12 N4 -0.8(5) . . . . ? C11 N5 C12 C8 -179.5(4) . . . . ? C7 C8 C12 N4 -12.2(7) . . . . ? C9 C8 C12 N4 166.5(4) . . . . ? C7 C8 C12 N5 166.4(4) . . . . ? C9 C8 C12 N5 -14.9(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A N5 0.818(10) 2.17(2) 2.952(5) 159(5) 2_656 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.432 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.112 # Attachment '- Zn-1.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 686453' #TrackingRef '- Zn-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 Cl2 N5 O Zn2' _chemical_formula_weight 440.88 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.334(3) _cell_length_b 7.8400(16) _cell_length_c 15.597(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.620(5) _cell_angle_gamma 90.00 _cell_volume 1477.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2726 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 3.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_correction_T_max 0.485 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6870 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.34 _reflns_number_total 1351 _reflns_number_gt 1272 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0257P)^2^+2.9284P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1351 _refine_ls_number_parameters 104 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.096 _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 Zn1 Zn 0.55628(3) 0.17250(4) 0.664715(17) 0.02317(12) Uani 1 1 d . . . Cl1 Cl 0.72888(6) 0.16689(10) 0.64551(5) 0.0409(2) Uani 1 1 d . . . O1 O 0.5000 0.3036(3) 0.7500 0.0306(6) Uani 1 2 d SD . . H1A H 0.5000 0.4080(14) 0.7500 0.060(17) Uiso 1 2 d SD . . N1 N 0.46320(18) 0.2508(3) 0.54634(13) 0.0233(5) Uani 1 1 d . . . N2 N 0.5000 0.3278(3) 0.2500 0.0205(6) Uani 1 2 d S . . N3 N 0.48388(19) 0.0570(3) 0.28973(13) 0.0247(5) Uani 1 1 d . . . C1 C 0.3807(2) 0.3635(3) 0.54393(17) 0.0269(6) Uani 1 1 d . . . H1B H 0.3593 0.3922 0.5959 0.032 Uiso 1 1 calc R . . C2 C 0.3268(2) 0.4380(4) 0.46739(17) 0.0304(6) Uani 1 1 d . . . H2 H 0.2712 0.5177 0.4682 0.036 Uiso 1 1 calc R . . C3 C 0.3556(2) 0.3938(3) 0.38938(17) 0.0264(6) Uani 1 1 d . . . H3 H 0.3197 0.4426 0.3370 0.032 Uiso 1 1 calc R . . C4 C 0.4398(2) 0.2742(3) 0.39067(15) 0.0211(5) Uani 1 1 d . . . C5 C 0.4917(2) 0.2088(3) 0.47028(16) 0.0237(6) Uani 1 1 d . . . H5 H 0.5494 0.1318 0.4715 0.028 Uiso 1 1 calc R . . C6 C 0.4747(2) 0.2209(3) 0.31004(15) 0.0211(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 Zn1 0.0354(2) 0.02011(19) 0.01560(18) 0.00134(11) 0.00896(13) 0.00090(12) Cl1 0.0329(4) 0.0471(5) 0.0441(4) 0.0059(3) 0.0112(3) 0.0082(3) O1 0.0581(19) 0.0162(14) 0.0225(14) 0.000 0.0200(13) 0.000 N1 0.0334(12) 0.0220(12) 0.0158(10) -0.0008(9) 0.0083(9) 0.0005(10) N2 0.0290(16) 0.0163(15) 0.0159(14) 0.000 0.0041(12) 0.000 N3 0.0411(13) 0.0201(12) 0.0156(10) -0.0002(9) 0.0118(9) 0.0012(9) C1 0.0351(15) 0.0275(14) 0.0210(13) -0.0033(11) 0.0122(12) -0.0001(12) C2 0.0312(15) 0.0316(15) 0.0297(14) -0.0014(12) 0.0094(12) 0.0083(12) C3 0.0331(15) 0.0250(14) 0.0210(13) 0.0018(11) 0.0050(11) 0.0029(11) C4 0.0292(14) 0.0173(12) 0.0176(12) -0.0023(10) 0.0068(10) -0.0047(10) C5 0.0313(14) 0.0216(13) 0.0188(12) -0.0007(10) 0.0065(11) 0.0025(11) C6 0.0261(13) 0.0214(13) 0.0150(11) 0.0000(10) 0.0024(10) 0.0009(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 Zn1 O1 1.9184(14) . ? Zn1 N3 2.032(2) 5_656 ? Zn1 N1 2.062(2) . ? Zn1 Cl1 2.2092(9) . ? O1 Zn1 1.9184(14) 2_656 ? O1 H1A 0.819(10) . ? N1 C1 1.342(3) . ? N1 C5 1.345(3) . ? N2 C6 1.340(3) . ? N2 C6 1.340(3) 2_655 ? N3 C6 1.334(3) . ? N3 N3 1.376(4) 2_655 ? N3 Zn1 2.032(2) 5_656 ? C1 C2 1.374(4) . ? C1 H1B 0.9300 . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.396(4) . ? C3 H3 0.9300 . ? C4 C5 1.377(3) . ? C4 C6 1.470(3) . ? C5 H5 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N3 94.83(9) . 5_656 ? O1 Zn1 N1 104.33(7) . . ? N3 Zn1 N1 116.48(9) 5_656 . ? O1 Zn1 Cl1 126.71(4) . . ? N3 Zn1 Cl1 109.83(7) 5_656 . ? N1 Zn1 Cl1 105.22(6) . . ? Zn1 O1 Zn1 115.19(13) 2_656 . ? Zn1 O1 H1A 122.41(6) 2_656 . ? Zn1 O1 H1A 122.41(6) . . ? C1 N1 C5 117.9(2) . . ? C1 N1 Zn1 120.22(16) . . ? C5 N1 Zn1 121.32(17) . . ? C6 N2 C6 102.6(3) . 2_655 ? C6 N3 N3 105.54(13) . 2_655 ? C6 N3 Zn1 137.02(17) . 5_656 ? N3 N3 Zn1 116.75(6) 2_655 5_656 ? N1 C1 C2 122.4(2) . . ? N1 C1 H1B 118.8 . . ? C2 C1 H1B 118.8 . . ? C1 C2 C3 119.6(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 118.6(2) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.2(2) . . ? C5 C4 C6 120.2(2) . . ? C3 C4 C6 121.6(2) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N3 C6 N2 113.2(2) . . ? N3 C6 C4 122.1(2) . . ? N2 C6 C4 124.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zn1 O1 Zn1 2.84(6) 5_656 . . 2_656 ? N1 Zn1 O1 Zn1 121.75(6) . . . 2_656 ? Cl1 Zn1 O1 Zn1 -116.36(5) . . . 2_656 ? O1 Zn1 N1 C1 -3.2(2) . . . . ? N3 Zn1 N1 C1 99.8(2) 5_656 . . . ? Cl1 Zn1 N1 C1 -138.34(19) . . . . ? O1 Zn1 N1 C5 168.12(19) . . . . ? N3 Zn1 N1 C5 -88.9(2) 5_656 . . . ? Cl1 Zn1 N1 C5 33.0(2) . . . . ? C5 N1 C1 C2 -1.1(4) . . . . ? Zn1 N1 C1 C2 170.5(2) . . . . ? N1 C1 C2 C3 1.6(4) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C2 C3 C4 C6 179.9(2) . . . . ? C1 N1 C5 C4 -0.7(4) . . . . ? Zn1 N1 C5 C4 -172.23(19) . . . . ? C3 C4 C5 N1 2.0(4) . . . . ? C6 C4 C5 N1 -179.3(2) . . . . ? N3 N3 C6 N2 -0.8(3) 2_655 . . . ? Zn1 N3 C6 N2 -170.39(16) 5_656 . . . ? N3 N3 C6 C4 179.1(2) 2_655 . . . ? Zn1 N3 C6 C4 9.5(4) 5_656 . . . ? C6 N2 C6 N3 0.32(13) 2_655 . . . ? C6 N2 C6 C4 -179.6(3) 2_655 . . . ? C5 C4 C6 N3 51.3(4) . . . . ? C3 C4 C6 N3 -130.0(3) . . . . ? C5 C4 C6 N2 -128.8(3) . . . . ? C3 C4 C6 N2 49.9(4) . . . . ? 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 C1 H1B Cl1 0.93 2.89 3.588(3) 133.3 3_455 O1 H1A N2 0.819(10) 2.071(11) 2.890(4) 180.000(2) 5_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.445 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.069 # Attachment '- Zn-2-new.cif' data_Zn-2-new _database_code_depnum_ccdc_archive 'CCDC 803353' #TrackingRef '- Zn-2-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 N10 O11 S Zn2, O4 S, 5(H2 O)' _chemical_formula_sum 'C24 H42 N10 O20 S2 Zn2' _chemical_formula_weight 985.54 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2947(13) _cell_length_b 17.4730(18) _cell_length_c 16.5991(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.015(3) _cell_angle_gamma 90.00 _cell_volume 3841.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16683 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.390 _exptl_absorpt_correction_T_max 0.577 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36308 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8755 _reflns_number_gt 8046 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; There are seven coordinated water molecules and five water solvates. Two water solvates were disordered. One was disordered over two positions; another was disordered over three positions, O20a, O20b, and O20c, their temperature factors are constrained as the same. The hydrogen atoms of disordered water haven¡¯t been defined. Other hydrogen atoms of water molecules were found in Fourier maps, and their coordinates and isotropic temperature factors were refined. Their O-H and H-H distances were constrained. 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^)+(0.0609P)^2^+5.0905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8755 _refine_ls_number_parameters 584 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.74203(3) 0.36087(2) 0.72624(2) 0.02368(11) Uani 1 1 d . . . Zn2 Zn 0.25132(3) 0.62047(2) 0.76061(2) 0.02122(11) Uani 1 1 d . . . S1 S 0.56604(6) 0.50261(5) 0.71165(5) 0.02406(18) Uani 1 1 d . . . S2 S 0.10378(6) 0.36433(4) 0.71760(5) 0.02142(17) Uani 1 1 d . . . O1 O 0.64554(17) 0.45221(15) 0.74868(15) 0.0337(6) Uani 1 1 d . . . O2 O 0.53488(17) 0.55440(15) 0.77542(14) 0.0315(5) Uani 1 1 d . . . O3 O 0.47771(17) 0.45585(15) 0.68164(15) 0.0337(6) Uani 1 1 d . . . O4 O 0.6007(2) 0.54669(17) 0.64522(16) 0.0414(6) Uani 1 1 d . . . O5 O 0.83955(19) 0.44036(15) 0.68099(17) 0.0358(6) Uani 1 1 d D . . H5C H 0.827(2) 0.4858(9) 0.672(3) 0.043 Uiso 1 1 d D . . H5D H 0.9009(9) 0.437(2) 0.690(3) 0.043 Uiso 1 1 d D . . O6 O 0.85406(16) 0.27241(14) 0.71692(14) 0.0265(5) Uani 1 1 d D . . H6C H 0.861(2) 0.249(2) 0.6753(14) 0.032 Uiso 1 1 d D . . H6D H 0.9111(13) 0.285(2) 0.7353(19) 0.032 Uiso 1 1 d D . . O7 O 0.63641(18) 0.28166(16) 0.77509(16) 0.0352(6) Uani 1 1 d D . . H7C H 0.5780(12) 0.2938(19) 0.780(3) 0.042 Uiso 1 1 d D . . H7D H 0.638(3) 0.2357(7) 0.767(3) 0.042 Uiso 1 1 d D . . O8 O 0.20157(17) 0.72906(13) 0.79986(15) 0.0278(5) Uani 1 1 d D . . H8C H 0.1507(15) 0.7513(17) 0.781(2) 0.033 Uiso 1 1 d D . . H8D H 0.2420(19) 0.7617(14) 0.818(2) 0.033 Uiso 1 1 d D . . O9 O 0.39105(16) 0.66262(13) 0.73084(14) 0.0242(5) Uani 1 1 d D . . H9C H 0.414(2) 0.7064(8) 0.736(2) 0.029 Uiso 1 1 d D . . H9D H 0.4368(18) 0.6333(13) 0.745(2) 0.029 Uiso 1 1 d D . . O10 O 0.29578(17) 0.51336(13) 0.72018(15) 0.0264(5) Uani 1 1 d D . . H10C H 0.3519(13) 0.4994(17) 0.709(2) 0.032 Uiso 1 1 d D . . H10D H 0.264(2) 0.4749(12) 0.730(2) 0.032 Uiso 1 1 d D . . O11 O 0.11525(17) 0.57003(14) 0.79196(15) 0.0280(5) Uani 1 1 d D . . H11C H 0.0539(12) 0.5867(17) 0.780(2) 0.034 Uiso 1 1 d D . . H11D H 0.107(2) 0.5245(7) 0.800(2) 0.034 Uiso 1 1 d D . . O12 O 0.1930(2) 0.39461(17) 0.76486(16) 0.0422(7) Uani 1 1 d . . . O13 O 0.0385(2) 0.42506(16) 0.6840(2) 0.0486(8) Uani 1 1 d . . . O14 O 0.1358(2) 0.31685(15) 0.65163(15) 0.0370(6) Uani 1 1 d . . . O15 O 0.04863(16) 0.31493(13) 0.77296(13) 0.0263(5) Uani 1 1 d . . . O16 O 0.4388(2) 0.33471(17) 0.78537(17) 0.0410(6) Uani 1 1 d D . . H16C H 0.439(4) 0.3730(14) 0.7562(19) 0.049 Uiso 1 1 d D . . H16D H 0.424(3) 0.350(2) 0.8296(12) 0.049 Uiso 1 1 d D . . O17A O 0.7107(5) 0.1439(4) 0.0043(4) 0.0483(15) Uiso 0.50 1 d P A 1 O17B O 0.6835(5) 0.1051(4) 0.0088(4) 0.0480(14) Uiso 0.50 1 d P B 2 O18 O 0.7037(2) 0.0934(3) 0.8496(2) 0.0698(11) Uani 1 1 d D . . H18C H 0.7633(13) 0.084(3) 0.847(4) 0.084 Uiso 1 1 d D . . H18D H 0.696(4) 0.1398(8) 0.847(4) 0.084 Uiso 1 1 d D . . O19 O 0.5814(3) 0.1323(2) 0.7208(2) 0.0630(9) Uani 1 1 d D . . H19C H 0.626(3) 0.112(3) 0.752(2) 0.076 Uiso 1 1 d D . . H19D H 0.600(4) 0.123(3) 0.6752(12) 0.076 Uiso 1 1 d D . . O20A O 0.3816(8) 0.4406(6) 0.5257(6) 0.0504(13) Uiso 0.33 1 d P C 1 O20B O 0.3898(8) 0.4099(6) 0.5247(6) 0.0504(13) Uiso 0.33 1 d P D 2 O20C O 0.3168(7) 0.3970(6) 0.5399(6) 0.0504(13) Uiso 0.33 1 d P E 3 N1 N 0.80897(19) 0.37155(15) 0.84621(16) 0.0230(5) Uani 1 1 d . . . N2 N 0.86803(19) 0.59452(16) 0.94551(15) 0.0239(6) Uani 1 1 d . . . N3 N 0.89924(19) 0.54237(16) 1.06980(16) 0.0242(6) Uani 1 1 d . . . N4 N 0.9027(2) 0.61949(15) 1.07414(15) 0.0234(5) Uani 1 1 d . . . H4 H 0.9155 0.6458 1.1191 0.028 Uiso 1 1 calc R . . N5 N 0.8223(2) 0.83126(17) 0.89053(16) 0.0266(6) Uani 1 1 d . . . N6 N 0.32029(19) 0.59705(16) 0.88195(15) 0.0226(5) Uani 1 1 d . . . N7 N 0.36115(19) 0.36591(14) 0.95239(15) 0.0195(5) Uani 1 1 d . . . N8 N 0.38926(19) 0.39539(15) 1.08114(15) 0.0207(5) Uani 1 1 d . . . H8 H 0.3987 0.4231 1.1255 0.025 Uiso 1 1 calc R . . N9 N 0.39007(19) 0.31771(15) 1.07845(15) 0.0221(5) Uani 1 1 d . . . N10 N 0.3211(2) 0.14083(16) 0.85760(16) 0.0246(6) Uani 1 1 d . . . C1 C 0.8257(2) 0.30995(19) 0.8940(2) 0.0256(7) Uani 1 1 d . . . H1 H 0.8134 0.2605 0.8714 0.031 Uiso 1 1 calc R . . C2 C 0.8602(2) 0.3159(2) 0.9746(2) 0.0265(7) Uani 1 1 d . . . H2 H 0.8709 0.2713 1.0069 0.032 Uiso 1 1 calc R . . C3 C 0.8790(2) 0.3878(2) 1.00785(19) 0.0253(7) Uani 1 1 d . . . H3 H 0.9023 0.3931 1.0633 0.030 Uiso 1 1 calc R . . C4 C 0.8633(2) 0.45215(18) 0.95895(18) 0.0218(6) Uani 1 1 d . . . C5 C 0.8283(2) 0.44082(18) 0.87834(18) 0.0213(6) Uani 1 1 d . . . H5A H 0.8176 0.4844 0.8445 0.026 Uiso 1 1 calc R . . C6 C 0.8779(2) 0.52962(19) 0.99122(18) 0.0214(6) Uani 1 1 d . . . C7 C 0.8837(2) 0.65043(19) 1.00010(18) 0.0213(6) Uani 1 1 d . . . C8 C 0.8778(2) 0.73240(19) 0.98435(18) 0.0221(6) Uani 1 1 d . . . C9 C 0.9069(3) 0.7874(2) 1.04257(19) 0.0284(7) Uani 1 1 d . . . H9A H 0.9373 0.7726 1.0942 0.034 Uiso 1 1 calc R . . C10 C 0.8908(3) 0.8636(2) 1.0239(2) 0.0324(8) Uani 1 1 d . . . H10A H 0.9089 0.9020 1.0631 0.039 Uiso 1 1 calc R . . C11 C 0.8480(3) 0.8838(2) 0.9477(2) 0.0310(7) Uani 1 1 d . . . H11A H 0.8365 0.9363 0.9356 0.037 Uiso 1 1 calc R . . C12 C 0.8366(2) 0.75779(19) 0.90913(19) 0.0240(6) Uani 1 1 d . . . H12 H 0.8176 0.7206 0.8689 0.029 Uiso 1 1 calc R . . C13 C 0.3524(2) 0.65232(19) 0.93489(19) 0.0234(6) Uani 1 1 d . . . H13 H 0.3501 0.7040 0.9169 0.028 Uiso 1 1 calc R . . C14 C 0.3885(2) 0.63752(18) 1.0139(2) 0.0237(6) Uani 1 1 d . . . H14 H 0.4084 0.6783 1.0497 0.028 Uiso 1 1 calc R . . C15 C 0.3951(2) 0.56246(18) 1.04015(18) 0.0213(6) Uani 1 1 d . . . H15 H 0.4189 0.5506 1.0943 0.026 Uiso 1 1 calc R . . C16 C 0.3660(2) 0.50476(17) 0.98534(18) 0.0192(6) Uani 1 1 d . . . C17 C 0.3281(2) 0.52480(18) 0.90759(18) 0.0215(6) Uani 1 1 d . . . H17 H 0.3068 0.4851 0.8709 0.026 Uiso 1 1 calc R . . C18 C 0.3719(2) 0.42355(17) 1.00607(17) 0.0186(6) Uani 1 1 d . . . C19 C 0.3735(2) 0.30263(17) 0.99988(17) 0.0190(6) Uani 1 1 d . . . C20 C 0.3707(2) 0.22484(18) 0.96823(18) 0.0212(6) Uani 1 1 d . . . C21 C 0.4147(3) 0.1641(2) 1.0120(2) 0.0295(7) Uani 1 1 d . . . H21 H 0.4475 0.1720 1.0646 0.035 Uiso 1 1 calc R . . C22 C 0.4101(3) 0.0922(2) 0.9781(2) 0.0377(9) Uani 1 1 d . . . H22 H 0.4381 0.0495 1.0077 0.045 Uiso 1 1 calc R . . C23 C 0.3647(3) 0.0826(2) 0.9008(2) 0.0328(8) Uani 1 1 d . . . H23 H 0.3641 0.0331 0.8772 0.039 Uiso 1 1 calc R . . C24 C 0.3233(2) 0.20999(18) 0.89177(18) 0.0218(6) Uani 1 1 d . . . H24 H 0.2910 0.2511 0.8624 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02205(19) 0.0280(2) 0.0205(2) -0.00371(14) -0.00065(14) -0.00008(14) Zn2 0.02271(19) 0.0204(2) 0.02034(19) 0.00294(13) 0.00088(13) 0.00053(13) S1 0.0218(4) 0.0294(4) 0.0207(4) -0.0034(3) 0.0003(3) 0.0024(3) S2 0.0225(4) 0.0192(4) 0.0227(4) -0.0013(3) 0.0025(3) -0.0013(3) O1 0.0283(12) 0.0381(15) 0.0337(13) -0.0041(11) -0.0033(10) 0.0123(10) O2 0.0311(12) 0.0364(14) 0.0258(12) -0.0093(10) -0.0048(9) 0.0118(10) O3 0.0256(12) 0.0420(15) 0.0330(13) -0.0112(11) -0.0011(10) -0.0019(10) O4 0.0445(15) 0.0488(17) 0.0320(14) 0.0035(12) 0.0083(11) -0.0028(12) O5 0.0310(13) 0.0324(15) 0.0438(15) 0.0064(12) 0.0030(11) -0.0025(10) O6 0.0234(11) 0.0305(13) 0.0252(11) -0.0097(10) 0.0007(9) 0.0013(9) O7 0.0310(13) 0.0415(16) 0.0334(13) -0.0017(12) 0.0057(11) -0.0097(11) O8 0.0282(12) 0.0220(12) 0.0322(13) -0.0015(10) -0.0026(10) 0.0026(9) O9 0.0230(11) 0.0216(12) 0.0280(12) 0.0028(9) 0.0019(9) -0.0005(8) O10 0.0253(11) 0.0201(12) 0.0347(13) -0.0010(10) 0.0072(10) -0.0001(9) O11 0.0255(11) 0.0244(12) 0.0348(13) 0.0052(10) 0.0059(10) -0.0033(9) O12 0.0437(15) 0.0511(18) 0.0315(13) -0.0018(12) 0.0014(11) -0.0269(13) O13 0.0379(14) 0.0314(15) 0.079(2) 0.0247(14) 0.0211(14) 0.0099(11) O14 0.0528(16) 0.0325(14) 0.0262(12) -0.0052(10) 0.0073(11) 0.0023(11) O15 0.0269(11) 0.0264(12) 0.0254(11) 0.0011(9) 0.0016(9) -0.0061(9) O16 0.0350(14) 0.0474(18) 0.0417(16) 0.0032(13) 0.0100(12) -0.0043(12) O18 0.0373(17) 0.118(3) 0.054(2) -0.033(2) 0.0017(15) -0.0030(18) O19 0.067(2) 0.071(3) 0.051(2) 0.0023(18) 0.0074(17) 0.0049(18) N1 0.0225(13) 0.0240(14) 0.0222(13) -0.0046(10) 0.0010(10) 0.0021(10) N2 0.0206(12) 0.0304(15) 0.0204(13) -0.0049(11) -0.0005(10) 0.0013(10) N3 0.0252(13) 0.0257(15) 0.0218(13) -0.0044(11) 0.0023(10) 0.0005(10) N4 0.0274(13) 0.0252(15) 0.0171(12) -0.0044(10) -0.0004(10) 0.0011(10) N5 0.0249(13) 0.0326(16) 0.0218(13) 0.0026(11) -0.0006(10) -0.0013(11) N6 0.0229(12) 0.0233(14) 0.0221(13) 0.0044(10) 0.0048(10) 0.0013(10) N7 0.0218(12) 0.0191(13) 0.0169(12) 0.0018(9) -0.0015(9) -0.0015(9) N8 0.0272(13) 0.0186(13) 0.0161(12) -0.0002(10) 0.0005(10) -0.0013(10) N9 0.0270(13) 0.0191(13) 0.0197(12) 0.0021(10) -0.0011(10) -0.0011(10) N10 0.0261(13) 0.0249(15) 0.0223(13) -0.0029(11) -0.0014(10) 0.0033(10) C1 0.0265(15) 0.0238(17) 0.0268(16) -0.0026(13) 0.0042(12) 0.0024(12) C2 0.0238(15) 0.0292(18) 0.0262(16) 0.0049(13) 0.0013(12) 0.0011(12) C3 0.0204(14) 0.0357(19) 0.0197(15) 0.0006(13) 0.0010(11) 0.0004(12) C4 0.0159(13) 0.0265(17) 0.0230(15) -0.0042(12) 0.0026(11) 0.0004(11) C5 0.0190(13) 0.0231(16) 0.0217(14) -0.0029(12) 0.0006(11) 0.0018(11) C6 0.0162(13) 0.0269(17) 0.0210(14) -0.0038(12) 0.0014(11) 0.0019(11) C7 0.0166(13) 0.0288(17) 0.0183(14) -0.0021(12) 0.0002(11) 0.0017(11) C8 0.0192(14) 0.0281(17) 0.0190(14) -0.0019(12) 0.0011(11) 0.0017(11) C9 0.0341(17) 0.0304(19) 0.0201(15) -0.0011(13) -0.0011(13) 0.0017(13) C10 0.042(2) 0.030(2) 0.0234(17) -0.0060(14) -0.0019(14) -0.0017(14) C11 0.0376(19) 0.0279(18) 0.0270(17) 0.0013(14) 0.0011(14) 0.0014(14) C12 0.0218(14) 0.0295(18) 0.0204(15) -0.0019(12) -0.0001(11) -0.0025(12) C13 0.0233(15) 0.0199(16) 0.0270(16) 0.0023(12) 0.0019(12) -0.0010(11) C14 0.0224(15) 0.0208(16) 0.0277(16) -0.0030(12) 0.0012(12) -0.0029(11) C15 0.0193(14) 0.0250(16) 0.0195(14) -0.0001(12) 0.0018(11) -0.0002(11) C16 0.0166(13) 0.0219(15) 0.0196(14) 0.0024(11) 0.0039(10) 0.0005(10) C17 0.0229(14) 0.0228(16) 0.0190(14) 0.0018(12) 0.0038(11) 0.0004(11) C18 0.0180(13) 0.0207(15) 0.0168(13) 0.0019(11) 0.0004(10) 0.0013(10) C19 0.0183(13) 0.0202(15) 0.0182(14) 0.0009(11) 0.0004(10) -0.0004(10) C20 0.0204(14) 0.0219(16) 0.0211(14) -0.0003(12) 0.0003(11) -0.0009(11) C21 0.0358(18) 0.0279(18) 0.0234(16) -0.0011(13) -0.0047(13) 0.0067(14) C22 0.051(2) 0.0269(19) 0.0330(19) 0.0007(15) -0.0104(16) 0.0134(16) C23 0.0421(19) 0.0246(18) 0.0304(18) -0.0036(14) -0.0039(15) 0.0089(14) C24 0.0220(14) 0.0211(16) 0.0217(15) 0.0004(12) -0.0006(11) 0.0000(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.084(2) . ? Zn1 O1 2.101(2) . ? Zn1 N5 2.114(3) 2_646 ? Zn1 N1 2.117(3) . ? Zn1 O6 2.161(2) . ? Zn1 O7 2.178(2) . ? Zn2 O10 2.091(2) . ? Zn2 O9 2.097(2) . ? Zn2 O11 2.118(2) . ? Zn2 O8 2.130(2) . ? Zn2 N10 2.138(3) 2_556 ? Zn2 N6 2.178(3) . ? S1 O4 1.453(3) . ? S1 O1 1.469(2) . ? S1 O2 1.479(2) . ? S1 O3 1.481(2) . ? S2 O13 1.451(3) . ? S2 O12 1.463(3) . ? S2 O14 1.466(3) . ? S2 O15 1.498(2) . ? O5 H5C 0.822(10) . ? O5 H5D 0.819(10) . ? O6 H6C 0.821(10) . ? O6 H6D 0.824(10) . ? O7 H7C 0.815(10) . ? O7 H7D 0.814(10) . ? O8 H8C 0.819(10) . ? O8 H8D 0.821(10) . ? O9 H9C 0.825(10) . ? O9 H9D 0.815(10) . ? O10 H10C 0.820(10) . ? O10 H10D 0.818(10) . ? O11 H11C 0.873(10) . ? O11 H11D 0.816(10) . ? O16 H16C 0.827(10) . ? O16 H16D 0.824(10) . ? O18 H18C 0.812(10) . ? O18 H18D 0.817(10) . ? O19 H19C 0.833(10) . ? O19 H19D 0.831(10) . ? N1 C5 1.339(4) . ? N1 C1 1.344(4) . ? N2 C7 1.337(4) . ? N2 C6 1.364(4) . ? N3 C6 1.329(4) . ? N3 N4 1.350(4) . ? N4 C7 1.346(4) . ? N4 H4 0.8800 . ? N5 C12 1.330(4) . ? N5 C11 1.342(5) . ? N5 Zn1 2.114(3) 2_656 ? N6 C17 1.333(4) . ? N6 C13 1.350(4) . ? N7 C18 1.344(4) . ? N7 C19 1.359(4) . ? N8 C18 1.341(4) . ? N8 N9 1.358(4) . ? N8 H8 0.8800 . ? N9 C19 1.330(4) . ? N10 C24 1.334(4) . ? N10 C23 1.346(4) . ? N10 Zn2 2.138(3) 2_546 ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 C6 1.463(4) . ? C5 H5A 0.9500 . ? C7 C8 1.457(5) . ? C8 C12 1.391(4) . ? C8 C9 1.393(4) . ? C9 C10 1.380(5) . ? C9 H9A 0.9500 . ? C10 C11 1.387(5) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.381(5) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 C17 1.389(4) . ? C16 C18 1.461(4) . ? C17 H17 0.9500 . ? C19 C20 1.457(4) . ? C20 C21 1.387(4) . ? C20 C24 1.391(4) . ? C21 C22 1.377(5) . ? C21 H21 0.9500 . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24 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 O5 Zn1 O1 88.08(11) . . ? O5 Zn1 N5 92.72(11) . 2_646 ? O1 Zn1 N5 98.28(10) . 2_646 ? O5 Zn1 N1 93.25(11) . . ? O1 Zn1 N1 88.81(10) . . ? N5 Zn1 N1 170.88(11) 2_646 . ? O5 Zn1 O6 89.80(10) . . ? O1 Zn1 O6 172.34(9) . . ? N5 Zn1 O6 89.18(10) 2_646 . ? N1 Zn1 O6 83.95(9) . . ? O5 Zn1 O7 177.67(11) . . ? O1 Zn1 O7 89.61(11) . . ? N5 Zn1 O7 87.90(10) 2_646 . ? N1 Zn1 O7 86.42(10) . . ? O6 Zn1 O7 92.46(10) . . ? O10 Zn2 O9 87.57(9) . . ? O10 Zn2 O11 88.73(9) . . ? O9 Zn2 O11 175.84(9) . . ? O10 Zn2 O8 178.23(9) . . ? O9 Zn2 O8 93.69(9) . . ? O11 Zn2 O8 90.04(9) . . ? O10 Zn2 N10 88.37(10) . 2_556 ? O9 Zn2 N10 93.57(9) . 2_556 ? O11 Zn2 N10 88.23(10) . 2_556 ? O8 Zn2 N10 90.32(10) . 2_556 ? O10 Zn2 N6 91.18(10) . . ? O9 Zn2 N6 88.51(9) . . ? O11 Zn2 N6 89.67(9) . . ? O8 Zn2 N6 90.08(10) . . ? N10 Zn2 N6 177.86(10) 2_556 . ? O4 S1 O1 111.77(16) . . ? O4 S1 O2 110.25(16) . . ? O1 S1 O2 107.67(14) . . ? O4 S1 O3 109.42(16) . . ? O1 S1 O3 109.30(16) . . ? O2 S1 O3 108.35(14) . . ? O13 S2 O12 111.77(18) . . ? O13 S2 O14 109.26(18) . . ? O12 S2 O14 109.29(17) . . ? O13 S2 O15 110.41(14) . . ? O12 S2 O15 107.27(14) . . ? O14 S2 O15 108.77(15) . . ? S1 O1 Zn1 144.04(16) . . ? Zn1 O5 H5C 126(3) . . ? Zn1 O5 H5D 122(3) . . ? H5C O5 H5D 106.5(17) . . ? Zn1 O6 H6C 124(3) . . ? Zn1 O6 H6D 113(2) . . ? H6C O6 H6D 106.2(16) . . ? Zn1 O7 H7C 121(3) . . ? Zn1 O7 H7D 122(3) . . ? H7C O7 H7D 108.5(17) . . ? Zn2 O8 H8C 125(2) . . ? Zn2 O8 H8D 121(2) . . ? H8C O8 H8D 107.5(17) . . ? Zn2 O9 H9C 129(2) . . ? Zn2 O9 H9D 111(2) . . ? H9C O9 H9D 107.0(17) . . ? Zn2 O10 H10C 129(2) . . ? Zn2 O10 H10D 120(2) . . ? H10C O10 H10D 107.2(17) . . ? Zn2 O11 H11C 127(2) . . ? Zn2 O11 H11D 126(2) . . ? H11C O11 H11D 102.6(15) . . ? H16C O16 H16D 105.7(17) . . ? H18C O18 H18D 108.2(18) . . ? H19C O19 H19D 103.9(15) . . ? C5 N1 C1 118.2(3) . . ? C5 N1 Zn1 120.3(2) . . ? C1 N1 Zn1 121.2(2) . . ? C7 N2 C6 103.2(3) . . ? C6 N3 N4 102.9(3) . . ? C7 N4 N3 110.5(3) . . ? C7 N4 H4 124.8 . . ? N3 N4 H4 124.8 . . ? C12 N5 C11 118.3(3) . . ? C12 N5 Zn1 119.2(2) . 2_656 ? C11 N5 Zn1 122.6(2) . 2_656 ? C17 N6 C13 117.3(3) . . ? C17 N6 Zn2 119.2(2) . . ? C13 N6 Zn2 123.5(2) . . ? C18 N7 C19 103.0(2) . . ? C18 N8 N9 109.7(2) . . ? C18 N8 H8 125.1 . . ? N9 N8 H8 125.1 . . ? C19 N9 N8 103.2(2) . . ? C24 N10 C23 117.7(3) . . ? C24 N10 Zn2 122.2(2) . 2_546 ? C23 N10 Zn2 120.1(2) . 2_546 ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C6 120.4(3) . . ? C3 C4 C6 121.7(3) . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? N3 C6 N2 114.1(3) . . ? N3 C6 C4 121.6(3) . . ? N2 C6 C4 124.2(3) . . ? N2 C7 N4 109.3(3) . . ? N2 C7 C8 126.4(3) . . ? N4 C7 C8 124.2(3) . . ? C12 C8 C9 117.8(3) . . ? C12 C8 C7 119.0(3) . . ? C9 C8 C7 123.1(3) . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? N5 C11 C10 122.0(3) . . ? N5 C11 H11A 119.0 . . ? C10 C11 H11A 119.0 . . ? N5 C12 C8 123.6(3) . . ? N5 C12 H12 118.2 . . ? C8 C12 H12 118.2 . . ? N6 C13 C14 123.2(3) . . ? N6 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 118.4(3) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 118.9(3) . . ? C17 C16 C18 118.1(3) . . ? C15 C16 C18 123.0(3) . . ? N6 C17 C16 123.2(3) . . ? N6 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? N8 C18 N7 109.9(3) . . ? N8 C18 C16 125.2(3) . . ? N7 C18 C16 124.8(3) . . ? N9 C19 N7 114.1(3) . . ? N9 C19 C20 122.4(3) . . ? N7 C19 C20 123.5(3) . . ? C21 C20 C24 118.2(3) . . ? C21 C20 C19 121.9(3) . . ? C24 C20 C19 119.9(3) . . ? C22 C21 C20 118.9(3) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 119.4(3) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N10 C23 C22 122.5(3) . . ? N10 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? N10 C24 C20 123.2(3) . . ? N10 C24 H24 118.4 . . ? C20 C24 H24 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Zn1 -60.0(3) . . . . ? O2 S1 O1 Zn1 178.7(3) . . . . ? O3 S1 O1 Zn1 61.2(3) . . . . ? O5 Zn1 O1 S1 82.5(3) . . . . ? N5 Zn1 O1 S1 -10.0(3) 2_646 . . . ? N1 Zn1 O1 S1 175.8(3) . . . . ? O6 Zn1 O1 S1 156.7(6) . . . . ? O7 Zn1 O1 S1 -97.8(3) . . . . ? O5 Zn1 N1 C5 46.7(2) . . . . ? O1 Zn1 N1 C5 -41.4(2) . . . . ? N5 Zn1 N1 C5 177.6(5) 2_646 . . . ? O6 Zn1 N1 C5 136.1(2) . . . . ? O7 Zn1 N1 C5 -131.0(2) . . . . ? O5 Zn1 N1 C1 -138.6(2) . . . . ? O1 Zn1 N1 C1 133.4(2) . . . . ? N5 Zn1 N1 C1 -7.6(8) 2_646 . . . ? O6 Zn1 N1 C1 -49.1(2) . . . . ? O7 Zn1 N1 C1 43.7(2) . . . . ? C6 N3 N4 C7 0.1(3) . . . . ? O10 Zn2 N6 C17 -27.8(2) . . . . ? O9 Zn2 N6 C17 -115.4(2) . . . . ? O11 Zn2 N6 C17 60.9(2) . . . . ? O8 Zn2 N6 C17 150.9(2) . . . . ? N10 Zn2 N6 C17 50(3) 2_556 . . . ? O10 Zn2 N6 C13 155.0(2) . . . . ? O9 Zn2 N6 C13 67.4(2) . . . . ? O11 Zn2 N6 C13 -116.3(2) . . . . ? O8 Zn2 N6 C13 -26.3(2) . . . . ? N10 Zn2 N6 C13 -127(3) 2_556 . . . ? C18 N8 N9 C19 0.4(3) . . . . ? C5 N1 C1 C2 1.1(4) . . . . ? Zn1 N1 C1 C2 -173.7(2) . . . . ? N1 C1 C2 C3 -0.4(5) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C2 C3 C4 C6 177.6(3) . . . . ? C1 N1 C5 C4 -1.1(4) . . . . ? Zn1 N1 C5 C4 173.8(2) . . . . ? C3 C4 C5 N1 0.2(4) . . . . ? C6 C4 C5 N1 -176.8(3) . . . . ? N4 N3 C6 N2 0.2(3) . . . . ? N4 N3 C6 C4 -177.7(3) . . . . ? C7 N2 C6 N3 -0.4(3) . . . . ? C7 N2 C6 C4 177.4(3) . . . . ? C3 C4 C6 N3 -5.4(4) . . . . ? C5 C4 C6 N3 171.6(3) . . . . ? C3 C4 C6 N2 177.0(3) . . . . ? C5 C4 C6 N2 -6.1(4) . . . . ? C6 N2 C7 N4 0.4(3) . . . . ? C6 N2 C7 C8 -177.2(3) . . . . ? N3 N4 C7 N2 -0.3(3) . . . . ? N3 N4 C7 C8 177.4(3) . . . . ? N2 C7 C8 C12 11.2(5) . . . . ? N4 C7 C8 C12 -166.1(3) . . . . ? N2 C7 C8 C9 -172.0(3) . . . . ? N4 C7 C8 C9 10.7(5) . . . . ? C12 C8 C9 C10 2.0(5) . . . . ? C7 C8 C9 C10 -174.8(3) . . . . ? C8 C9 C10 C11 -1.2(5) . . . . ? C12 N5 C11 C10 1.7(5) . . . . ? Zn1 N5 C11 C10 -179.6(3) 2_656 . . . ? C9 C10 C11 N5 -0.6(6) . . . . ? C11 N5 C12 C8 -0.9(5) . . . . ? Zn1 N5 C12 C8 -179.6(2) 2_656 . . . ? C9 C8 C12 N5 -1.0(5) . . . . ? C7 C8 C12 N5 175.9(3) . . . . ? C17 N6 C13 C14 -2.7(4) . . . . ? Zn2 N6 C13 C14 174.5(2) . . . . ? N6 C13 C14 C15 1.9(5) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C17 -2.3(4) . . . . ? C14 C15 C16 C18 178.7(3) . . . . ? C13 N6 C17 C16 0.9(4) . . . . ? Zn2 N6 C17 C16 -176.4(2) . . . . ? C15 C16 C17 N6 1.6(4) . . . . ? C18 C16 C17 N6 -179.4(3) . . . . ? N9 N8 C18 N7 -0.1(3) . . . . ? N9 N8 C18 C16 -179.8(3) . . . . ? C19 N7 C18 N8 -0.2(3) . . . . ? C19 N7 C18 C16 179.5(3) . . . . ? C17 C16 C18 N8 -167.5(3) . . . . ? C15 C16 C18 N8 11.5(4) . . . . ? C17 C16 C18 N7 12.9(4) . . . . ? C15 C16 C18 N7 -168.1(3) . . . . ? N8 N9 C19 N7 -0.6(3) . . . . ? N8 N9 C19 C20 178.4(3) . . . . ? C18 N7 C19 N9 0.5(3) . . . . ? C18 N7 C19 C20 -178.5(3) . . . . ? N9 C19 C20 C21 -20.5(4) . . . . ? N7 C19 C20 C21 158.5(3) . . . . ? N9 C19 C20 C24 160.0(3) . . . . ? N7 C19 C20 C24 -21.1(4) . . . . ? C24 C20 C21 C22 0.2(5) . . . . ? C19 C20 C21 C22 -179.3(3) . . . . ? C20 C21 C22 C23 1.9(6) . . . . ? C24 N10 C23 C22 0.4(5) . . . . ? Zn2 N10 C23 C22 -178.3(3) 2_546 . . . ? C21 C22 C23 N10 -2.3(6) . . . . ? C23 N10 C24 C20 1.9(5) . . . . ? Zn2 N10 C24 C20 -179.4(2) 2_546 . . . ? C21 C20 C24 N10 -2.2(5) . . . . ? C19 C20 C24 N10 177.3(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 O5 H5C O18 0.822(10) 1.953(11) 2.774(5) 179(4) 2_656 O5 H5D O13 0.819(10) 1.851(15) 2.654(4) 166(4) 1_655 O5 H5D S2 0.819(10) 2.977(14) 3.754(3) 159(3) 1_655 O6 H6C N9 0.820(10) 2.044(11) 2.861(3) 174(4) 4_665 O6 H6D O15 0.824(10) 1.950(11) 2.772(3) 176(3) 1_655 O6 H6D S2 0.824(10) 2.95(2) 3.687(2) 149(3) 1_655 O7 H7C O16 0.816(10) 1.991(11) 2.804(4) 174(4) . O7 H7D O19 0.813(10) 2.07(2) 2.829(5) 156(4) . O8 H8C O16 0.819(10) 2.125(17) 2.905(4) 159(3) 2_556 O8 H8D O14 0.820(10) 1.919(13) 2.715(4) 163(3) 2_556 O8 H8D S2 0.820(10) 2.83(2) 3.536(2) 146(3) 2_556 O9 H9C O15 0.825(10) 1.973(12) 2.782(3) 167(3) 2_556 O9 H9C S2 0.825(10) 2.873(17) 3.626(2) 153(3) 2_556 O9 H9D O2 0.815(10) 1.934(10) 2.745(3) 173(3) . O9 H9D S1 0.815(10) 2.940(19) 3.669(2) 150(3) . O10 H10C O3 0.819(10) 1.930(11) 2.746(3) 174(3) . O10 H10C S1 0.819(10) 2.846(16) 3.613(2) 157(3) . O10 H10D O12 0.817(10) 1.815(11) 2.626(3) 172(4) . O10 H10D S2 0.817(10) 2.867(15) 3.645(2) 160(3) . O11 H11C O19 0.868(10) 1.989(14) 2.839(4) 166(4) 2_556 O11 H11D O12 0.817(10) 2.62(2) 3.278(4) 138(3) . O16 H16C O3 0.827(10) 1.989(13) 2.803(4) 168(4) . O16 H16C S1 0.827(10) 2.93(3) 3.649(3) 147(4) . O16 H16D N7 0.824(10) 2.290(14) 3.091(4) 164(4) . O18 H18D O19 0.826(10) 2.43(6) 2.643(6) 95(5) . O18 H18D O17A 0.826(10) 2.64(7) 2.709(7) 86(5) 1_556 O19 H19C O11 0.866(10) 1.977(13) 2.839(4) 173(6) 2_546 O16 H16D N7 0.824(10) 2.290(14) 3.091(4) 164(4) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.763 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.100 # Attachment '- Cd-3.cif' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 701506' #TrackingRef '- Cd-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 Cd N5 O4 S' _chemical_formula_sum 'C12 H9 Cd N5 O4 S' _chemical_formula_weight 431.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 6.7324(12) _cell_length_b 21.804(4) _cell_length_c 9.5103(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.592(3) _cell_angle_gamma 90.00 _cell_volume 1351.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3352 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5913 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.49 _reflns_number_total 2496 _reflns_number_gt 2187 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2496 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Cd1 Cd 0.75128(3) 0.906601(8) 1.05654(2) 0.01095(7) Uani 1 1 d . . . S1 S 0.25412(9) 0.94644(3) 1.05713(7) 0.01082(14) Uani 1 1 d . . . O1 O 0.4205(2) 0.90037(7) 1.0770(2) 0.0153(4) Uani 1 1 d . . . O2 O 0.2733(2) 0.98860(8) 0.9369(2) 0.0149(4) Uani 1 1 d . . . O3 O 0.0586(3) 0.91294(7) 1.0078(2) 0.0165(4) Uani 1 1 d . . . O4 O 0.2641(3) 0.98116(8) 1.1877(2) 0.0209(4) Uani 1 1 d . . . N1 N 0.8362(3) 0.69849(9) 0.6063(3) 0.0160(5) Uani 1 1 d . . . N2 N -0.1492(3) 0.91519(9) 0.3141(2) 0.0156(5) Uani 1 1 d . . . N3 N 0.5794(3) 0.87827(9) 0.8060(2) 0.0142(5) Uani 1 1 d . . . N4 N 0.4002(3) 0.90952(10) 0.7552(3) 0.0147(5) Uani 1 1 d . . . H4A H 0.363(4) 0.9394(13) 0.808(3) 0.022(8) Uiso 1 1 d . . . N5 N 0.4054(3) 0.84106(9) 0.5872(2) 0.0159(5) Uani 1 1 d . . . C1 C 0.6930(4) 0.73950(12) 0.6207(3) 0.0175(6) Uani 1 1 d . . . H1 H 0.5549 0.7313 0.5745 0.021 Uiso 1 1 calc R . . C2 C 0.7390(4) 0.79312(11) 0.7001(3) 0.0149(6) Uani 1 1 d . . . C3 C 0.9425(4) 0.80377(12) 0.7752(3) 0.0164(6) Uani 1 1 d . . . H3 H 0.9781 0.8381 0.8362 0.020 Uiso 1 1 calc R . . C4 C 1.0909(4) 0.76235(12) 0.7576(3) 0.0186(6) Uani 1 1 d . . . H4B H 1.2297 0.7688 0.8050 0.022 Uiso 1 1 calc R . . C5 C 1.0333(4) 0.71202(11) 0.6707(3) 0.0166(6) Uani 1 1 d . . . H5 H 1.1363 0.6857 0.6552 0.020 Uiso 1 1 calc R . . C6 C 0.0376(4) 0.90029(11) 0.3971(3) 0.0159(6) Uani 1 1 d . . . H6 H 0.1339 0.8836 0.3513 0.019 Uiso 1 1 calc R . . C7 C 0.0955(4) 0.90821(11) 0.5460(3) 0.0136(6) Uani 1 1 d . . . C8 C -0.0422(4) 0.93580(12) 0.6147(3) 0.0152(6) Uani 1 1 d . . . H8 H -0.0054 0.9439 0.7151 0.018 Uiso 1 1 calc R . . C9 C -0.2345(4) 0.95075(12) 0.5297(3) 0.0179(6) Uani 1 1 d . . . H9 H -0.3321 0.9688 0.5722 0.022 Uiso 1 1 calc R . . C10 C -0.2832(4) 0.93920(12) 0.3824(3) 0.0182(6) Uani 1 1 d . . . H10 H -0.4164 0.9486 0.3272 0.022 Uiso 1 1 calc R . . C11 C 0.5755(4) 0.83758(11) 0.7009(3) 0.0140(6) Uani 1 1 d . . . C12 C 0.2987(4) 0.88652(11) 0.6275(3) 0.0132(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 Cd1 0.00951(11) 0.01168(10) 0.01148(11) 0.00006(8) 0.00230(7) 0.00030(8) S1 0.0089(3) 0.0119(3) 0.0119(3) -0.0007(3) 0.0029(2) 0.0000(3) O1 0.0104(9) 0.0164(9) 0.0200(11) 0.0034(8) 0.0055(8) 0.0031(7) O2 0.0176(9) 0.0123(9) 0.0167(10) 0.0019(8) 0.0076(8) 0.0008(7) O3 0.0088(9) 0.0175(10) 0.0245(11) -0.0017(8) 0.0066(8) -0.0027(7) O4 0.0222(10) 0.0262(10) 0.0142(11) -0.0068(9) 0.0043(8) 0.0004(8) N1 0.0168(11) 0.0134(11) 0.0171(13) -0.0024(10) 0.0031(10) 0.0010(9) N2 0.0147(11) 0.0181(12) 0.0124(12) -0.0025(10) 0.0002(9) -0.0008(9) N3 0.0118(11) 0.0148(11) 0.0146(13) 0.0009(10) 0.0009(9) 0.0047(9) N4 0.0139(11) 0.0156(11) 0.0137(12) -0.0021(10) 0.0016(9) 0.0063(9) N5 0.0149(11) 0.0170(11) 0.0150(13) -0.0030(10) 0.0026(9) 0.0013(9) C1 0.0153(13) 0.0180(14) 0.0179(16) -0.0026(12) 0.0019(11) -0.0003(11) C2 0.0173(13) 0.0159(13) 0.0120(14) 0.0016(11) 0.0046(11) 0.0029(11) C3 0.0197(13) 0.0144(13) 0.0149(15) -0.0033(11) 0.0043(11) -0.0017(11) C4 0.0125(13) 0.0193(14) 0.0228(16) 0.0009(13) 0.0020(11) 0.0012(11) C5 0.0145(13) 0.0153(13) 0.0213(16) 0.0007(12) 0.0065(12) 0.0018(11) C6 0.0150(13) 0.0175(13) 0.0143(15) -0.0014(11) 0.0021(11) 0.0020(11) C7 0.0137(13) 0.0123(13) 0.0139(14) 0.0004(11) 0.0017(11) -0.0008(10) C8 0.0160(13) 0.0179(13) 0.0106(14) -0.0009(11) 0.0015(11) 0.0001(11) C9 0.0173(14) 0.0190(14) 0.0189(17) -0.0014(12) 0.0071(12) 0.0017(11) C10 0.0130(13) 0.0225(15) 0.0174(15) -0.0004(12) 0.0010(11) 0.0023(11) C11 0.0161(13) 0.0130(13) 0.0132(15) 0.0005(11) 0.0039(11) -0.0009(11) C12 0.0138(13) 0.0158(12) 0.0100(14) 0.0010(11) 0.0032(11) -0.0002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.2356(18) 1_655 ? Cd1 O1 2.2879(17) . ? Cd1 O2 2.2929(17) 3_677 ? Cd1 N2 2.378(2) 1_656 ? Cd1 N1 2.380(2) 4_576 ? Cd1 N3 2.451(2) . ? S1 O4 1.4418(19) . ? S1 O3 1.4749(17) . ? S1 O1 1.4805(17) . ? S1 O2 1.4981(19) . ? O2 Cd1 2.2929(17) 3_677 ? O3 Cd1 2.2356(17) 1_455 ? N1 C5 1.347(3) . ? N1 C1 1.347(3) . ? N1 Cd1 2.380(2) 4_575 ? N2 C10 1.344(3) . ? N2 C6 1.346(3) . ? N2 Cd1 2.378(2) 1_454 ? N3 C11 1.332(3) . ? N3 N4 1.364(3) . ? N4 C12 1.332(3) . ? N4 H4A 0.90(3) . ? N5 C12 1.335(3) . ? N5 C11 1.364(3) . ? C1 C2 1.384(4) . ? C1 H1 0.9400 . ? C2 C3 1.396(3) . ? C2 C11 1.468(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9400 . ? C4 C5 1.370(4) . ? C4 H4B 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.381(4) . ? C6 H6 0.9400 . ? C7 C8 1.398(4) . ? C7 C12 1.470(3) . ? C8 C9 1.382(3) . ? C8 H8 0.9400 . ? C9 C10 1.379(4) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O1 173.14(7) 1_655 . ? O3 Cd1 O2 91.20(6) 1_655 3_677 ? O1 Cd1 O2 88.76(6) . 3_677 ? O3 Cd1 N2 99.99(7) 1_655 1_656 ? O1 Cd1 N2 86.84(7) . 1_656 ? O2 Cd1 N2 84.08(7) 3_677 1_656 ? O3 Cd1 N1 84.97(7) 1_655 4_576 ? O1 Cd1 N1 96.67(7) . 4_576 ? O2 Cd1 N1 165.77(7) 3_677 4_576 ? N2 Cd1 N1 83.10(7) 1_656 4_576 ? O3 Cd1 N3 92.80(7) 1_655 . ? O1 Cd1 N3 80.59(7) . . ? O2 Cd1 N3 104.96(7) 3_677 . ? N2 Cd1 N3 164.24(7) 1_656 . ? N1 Cd1 N3 88.94(7) 4_576 . ? O4 S1 O3 112.20(11) . . ? O4 S1 O1 112.14(11) . . ? O3 S1 O1 106.88(10) . . ? O4 S1 O2 109.96(11) . . ? O3 S1 O2 107.62(11) . . ? O1 S1 O2 107.81(11) . . ? S1 O1 Cd1 132.08(10) . . ? S1 O2 Cd1 124.75(11) . 3_677 ? S1 O3 Cd1 139.75(11) . 1_455 ? C5 N1 C1 117.2(2) . . ? C5 N1 Cd1 117.46(16) . 4_575 ? C1 N1 Cd1 121.15(17) . 4_575 ? C10 N2 C6 116.9(2) . . ? C10 N2 Cd1 118.67(17) . 1_454 ? C6 N2 Cd1 124.36(18) . 1_454 ? C11 N3 N4 102.6(2) . . ? C11 N3 Cd1 144.38(17) . . ? N4 N3 Cd1 112.19(15) . . ? C12 N4 N3 109.9(2) . . ? C12 N4 H4A 129.5(18) . . ? N3 N4 H4A 120.6(18) . . ? C12 N5 C11 102.7(2) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.4(2) . . ? C1 C2 C11 119.7(2) . . ? C3 C2 C11 121.9(2) . . ? C4 C3 C2 118.3(2) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4B 120.3 . . ? C3 C4 H4B 120.3 . . ? N1 C5 C4 123.1(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C7 123.5(3) . . ? N2 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C6 C7 C8 119.0(2) . . ? C6 C7 C12 119.0(2) . . ? C8 C7 C12 122.0(2) . . ? C9 C8 C7 117.5(3) . . ? C9 C8 H8 121.3 . . ? C7 C8 H8 121.3 . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 123.1(2) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N3 C11 N5 114.3(2) . . ? N3 C11 C2 124.7(2) . . ? N5 C11 C2 120.9(2) . . ? N4 C12 N5 110.6(2) . . ? N4 C12 C7 123.7(2) . . ? N5 C12 C7 125.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Cd1 -86.21(17) . . . . ? O3 S1 O1 Cd1 150.43(14) . . . . ? O2 S1 O1 Cd1 34.97(18) . . . . ? O3 Cd1 O1 S1 -74.4(5) 1_655 . . . ? O2 Cd1 O1 S1 15.38(15) 3_677 . . . ? N2 Cd1 O1 S1 99.52(16) 1_656 . . . ? N1 Cd1 O1 S1 -177.81(15) 4_576 . . . ? N3 Cd1 O1 S1 -90.00(16) . . . . ? O4 S1 O2 Cd1 -12.72(14) . . . 3_677 ? O3 S1 O2 Cd1 109.78(12) . . . 3_677 ? O1 S1 O2 Cd1 -135.26(11) . . . 3_677 ? O4 S1 O3 Cd1 9.4(2) . . . 1_455 ? O1 S1 O3 Cd1 132.76(16) . . . 1_455 ? O2 S1 O3 Cd1 -111.66(17) . . . 1_455 ? O3 Cd1 N3 C11 57.8(3) 1_655 . . . ? O1 Cd1 N3 C11 -124.0(3) . . . . ? O2 Cd1 N3 C11 149.8(3) 3_677 . . . ? N2 Cd1 N3 C11 -86.5(4) 1_656 . . . ? N1 Cd1 N3 C11 -27.1(3) 4_576 . . . ? O3 Cd1 N3 N4 -135.48(16) 1_655 . . . ? O1 Cd1 N3 N4 42.67(16) . . . . ? O2 Cd1 N3 N4 -43.49(17) 3_677 . . . ? N2 Cd1 N3 N4 80.1(3) 1_656 . . . ? N1 Cd1 N3 N4 139.61(17) 4_576 . . . ? C11 N3 N4 C12 0.9(3) . . . . ? Cd1 N3 N4 C12 -171.20(17) . . . . ? C5 N1 C1 C2 -1.6(4) . . . . ? Cd1 N1 C1 C2 154.8(2) 4_575 . . . ? N1 C1 C2 C3 -3.4(4) . . . . ? N1 C1 C2 C11 175.3(3) . . . . ? C1 C2 C3 C4 4.8(4) . . . . ? C11 C2 C3 C4 -173.8(3) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? C1 N1 C5 C4 5.2(4) . . . . ? Cd1 N1 C5 C4 -152.1(2) 4_575 . . . ? C3 C4 C5 N1 -3.7(4) . . . . ? C10 N2 C6 C7 0.3(4) . . . . ? Cd1 N2 C6 C7 176.97(19) 1_454 . . . ? N2 C6 C7 C8 -3.2(4) . . . . ? N2 C6 C7 C12 175.9(2) . . . . ? C6 C7 C8 C9 3.4(4) . . . . ? C12 C7 C8 C9 -175.7(2) . . . . ? C7 C8 C9 C10 -1.0(4) . . . . ? C6 N2 C10 C9 2.3(4) . . . . ? Cd1 N2 C10 C9 -174.5(2) 1_454 . . . ? C8 C9 C10 N2 -2.0(4) . . . . ? N4 N3 C11 N5 -0.1(3) . . . . ? Cd1 N3 C11 N5 167.3(2) . . . . ? N4 N3 C11 C2 178.1(2) . . . . ? Cd1 N3 C11 C2 -14.5(4) . . . . ? C12 N5 C11 N3 -0.7(3) . . . . ? C12 N5 C11 C2 -179.0(2) . . . . ? C1 C2 C11 N3 155.5(3) . . . . ? C3 C2 C11 N3 -25.9(4) . . . . ? C1 C2 C11 N5 -26.4(4) . . . . ? C3 C2 C11 N5 152.2(3) . . . . ? N3 N4 C12 N5 -1.4(3) . . . . ? N3 N4 C12 C7 177.4(2) . . . . ? C11 N5 C12 N4 1.2(3) . . . . ? C11 N5 C12 C7 -177.6(2) . . . . ? C6 C7 C12 N4 155.0(3) . . . . ? C8 C7 C12 N4 -25.9(4) . . . . ? C6 C7 C12 N5 -26.3(4) . . . . ? C8 C7 C12 N5 152.7(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 N4 H4A O2 0.90(3) 1.84(3) 2.727(3) 169(3) . N4 H4A S1 0.90(3) 2.65(3) 3.359(2) 136(2) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.472 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.085 # Attachment '- Zn-5.cif' data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 701507' #TrackingRef '- Zn-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Cl N5 Zn' _chemical_formula_sum 'C12 H8 Cl N5 Zn' _chemical_formula_weight 323.05 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 14.900(3) _cell_length_b 7.6852(14) _cell_length_c 23.142(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2649.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6235 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8497 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3016 _reflns_number_gt 2617 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0554P)^2^+1.3619P] 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 3016 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.56586(3) 0.09418(5) 0.370418(17) 0.02677(15) Uani 1 1 d . . . Cl1 Cl 0.61077(8) -0.16939(13) 0.34446(5) 0.0494(3) Uani 1 1 d . . . N1 N 0.39598(18) -0.2424(4) 0.19587(12) 0.0294(6) Uani 1 1 d . . . N2 N 0.13770(18) 0.3239(4) 0.56065(13) 0.0295(6) Uani 1 1 d . . . N3 N 0.43487(18) 0.1175(4) 0.37985(13) 0.0299(7) Uani 1 1 d . . . N4 N 0.40183(19) 0.1906(4) 0.42931(12) 0.0300(7) Uani 1 1 d . . . N5 N 0.28825(18) 0.0602(4) 0.38133(12) 0.0278(6) Uani 1 1 d . . . C1 C 0.3416(3) -0.2972(5) 0.23812(18) 0.0454(11) Uani 1 1 d . . . H1 H 0.3106 -0.4026 0.2328 0.054 Uiso 1 1 calc R . . C2 C 0.3286(3) -0.2082(6) 0.28846(17) 0.0461(11) Uani 1 1 d . . . H2 H 0.2895 -0.2520 0.3168 0.055 Uiso 1 1 calc R . . C3 C 0.3736(2) -0.0531(5) 0.29752(14) 0.0278(7) Uani 1 1 d . . . C4 C 0.4269(2) 0.0084(5) 0.25284(15) 0.0323(8) Uani 1 1 d . . . H4 H 0.4565 0.1158 0.2563 0.039 Uiso 1 1 calc R . . C5 C 0.4361(2) -0.0896(5) 0.20319(16) 0.0315(8) Uani 1 1 d . . . H5 H 0.4724 -0.0462 0.1732 0.038 Uiso 1 1 calc R . . C6 C 0.2271(2) 0.3403(5) 0.56558(16) 0.0325(8) Uani 1 1 d . . . H6 H 0.2506 0.3908 0.5993 0.039 Uiso 1 1 calc R . . C7 C 0.2854(2) 0.2867(4) 0.52351(15) 0.0309(8) Uani 1 1 d . . . H7 H 0.3475 0.3002 0.5288 0.037 Uiso 1 1 calc R . . C8 C 0.2531(2) 0.2129(4) 0.47330(14) 0.0271(7) Uani 1 1 d . . . C9 C 0.1603(2) 0.1966(5) 0.46761(16) 0.0350(8) Uani 1 1 d . . . H9 H 0.1352 0.1480 0.4340 0.042 Uiso 1 1 calc R . . C10 C 0.1058(2) 0.2530(5) 0.51198(16) 0.0368(8) Uani 1 1 d . . . H10 H 0.0434 0.2410 0.5079 0.044 Uiso 1 1 calc R . . C11 C 0.3650(2) 0.0408(5) 0.35270(14) 0.0269(7) Uani 1 1 d . . . C12 C 0.3144(2) 0.1543(4) 0.42769(14) 0.0271(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 Zn1 0.0279(2) 0.0321(3) 0.0203(2) -0.00042(16) -0.00088(15) 0.00011(16) Cl1 0.0660(7) 0.0372(5) 0.0452(6) -0.0106(5) -0.0185(5) 0.0156(5) N1 0.0281(14) 0.0373(16) 0.0227(14) -0.0018(13) 0.0045(11) -0.0029(13) N2 0.0291(14) 0.0342(16) 0.0251(15) -0.0022(13) 0.0010(11) 0.0021(13) N3 0.0268(14) 0.0403(18) 0.0225(15) -0.0046(13) 0.0026(11) -0.0001(13) N4 0.0304(14) 0.0379(17) 0.0216(15) -0.0047(13) 0.0040(11) 0.0012(13) N5 0.0269(14) 0.0324(15) 0.0241(15) -0.0025(12) -0.0001(11) 0.0041(13) C1 0.044(2) 0.052(3) 0.040(2) -0.0154(19) 0.0169(17) -0.024(2) C2 0.042(2) 0.059(3) 0.037(2) -0.0130(19) 0.0188(17) -0.023(2) C3 0.0250(16) 0.0375(19) 0.0209(16) -0.0009(14) -0.0003(13) 0.0034(14) C4 0.044(2) 0.0271(18) 0.0258(18) 0.0013(15) -0.0002(15) -0.0041(16) C5 0.038(2) 0.036(2) 0.0203(17) 0.0052(14) 0.0047(14) -0.0032(16) C6 0.0349(19) 0.036(2) 0.0263(18) -0.0044(15) -0.0016(14) 0.0028(16) C7 0.0276(17) 0.0358(19) 0.0291(18) 0.0003(15) -0.0009(13) 0.0038(15) C8 0.0324(16) 0.0285(17) 0.0205(15) 0.0037(14) 0.0029(13) 0.0058(15) C9 0.0311(18) 0.050(2) 0.0241(18) -0.0074(16) -0.0005(14) -0.0029(17) C10 0.0285(18) 0.050(2) 0.032(2) -0.0102(18) 0.0029(14) -0.0004(17) C11 0.0268(16) 0.0333(18) 0.0208(16) 0.0014(14) -0.0018(13) 0.0024(15) C12 0.0277(16) 0.0322(18) 0.0215(17) 0.0015(14) 0.0030(13) 0.0031(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 Zn1 N3 1.972(3) . ? Zn1 N2 2.022(3) 6_666 ? Zn1 N1 2.062(3) 7_666 ? Zn1 Cl1 2.2162(11) . ? N1 C5 1.329(5) . ? N1 C1 1.338(4) . ? N1 Zn1 2.062(3) 7_656 ? N2 C10 1.338(5) . ? N2 C6 1.343(4) . ? N2 Zn1 2.022(3) 6_566 ? N3 C11 1.351(4) . ? N3 N4 1.367(4) . ? N4 C12 1.333(4) . ? N5 C11 1.330(4) . ? N5 C12 1.351(4) . ? C1 C2 1.365(5) . ? C1 H1 0.9400 . ? C2 C3 1.383(5) . ? C2 H2 0.9400 . ? C3 C4 1.387(5) . ? C3 C11 1.472(4) . ? C4 C5 1.380(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.368(5) . ? C6 H6 0.9400 . ? C7 C8 1.380(5) . ? C7 H7 0.9400 . ? C8 C9 1.394(5) . ? C8 C12 1.467(4) . ? C9 C10 1.378(5) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N2 114.10(12) . 6_666 ? N3 Zn1 N1 107.45(12) . 7_666 ? N2 Zn1 N1 104.56(12) 6_666 7_666 ? N3 Zn1 Cl1 114.32(10) . . ? N2 Zn1 Cl1 109.80(9) 6_666 . ? N1 Zn1 Cl1 105.76(9) 7_666 . ? C5 N1 C1 117.2(3) . . ? C5 N1 Zn1 120.6(2) . 7_656 ? C1 N1 Zn1 121.3(3) . 7_656 ? C10 N2 C6 117.5(3) . . ? C10 N2 Zn1 127.1(2) . 6_566 ? C6 N2 Zn1 115.4(2) . 6_566 ? C11 N3 N4 106.9(3) . . ? C11 N3 Zn1 132.2(2) . . ? N4 N3 Zn1 119.1(2) . . ? C12 N4 N3 104.0(3) . . ? C11 N5 C12 102.0(3) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 117.2(3) . . ? C2 C3 C11 120.8(3) . . ? C4 C3 C11 122.0(3) . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 122.7(3) . . ? N2 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C6 C7 C8 120.1(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 117.5(3) . . ? C7 C8 C12 121.0(3) . . ? C9 C8 C12 121.5(3) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 123.1(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N5 C11 N3 112.4(3) . . ? N5 C11 C3 124.2(3) . . ? N3 C11 C3 123.4(3) . . ? N4 C12 N5 114.6(3) . . ? N4 C12 C8 121.6(3) . . ? N5 C12 C8 123.8(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 N2 Zn1 N3 C11 -160.2(3) 6_666 . . . ? N1 Zn1 N3 C11 84.4(3) 7_666 . . . ? Cl1 Zn1 N3 C11 -32.6(4) . . . . ? N2 Zn1 N3 N4 2.4(3) 6_666 . . . ? N1 Zn1 N3 N4 -113.0(3) 7_666 . . . ? Cl1 Zn1 N3 N4 130.0(2) . . . . ? C11 N3 N4 C12 -0.8(4) . . . . ? Zn1 N3 N4 C12 -167.4(2) . . . . ? C5 N1 C1 C2 -2.8(6) . . . . ? Zn1 N1 C1 C2 166.4(3) 7_656 . . . ? N1 C1 C2 C3 -0.3(7) . . . . ? C1 C2 C3 C4 3.1(6) . . . . ? C1 C2 C3 C11 -176.5(4) . . . . ? C2 C3 C4 C5 -2.9(5) . . . . ? C11 C3 C4 C5 176.6(3) . . . . ? C1 N1 C5 C4 2.9(5) . . . . ? Zn1 N1 C5 C4 -166.3(3) 7_656 . . . ? C3 C4 C5 N1 -0.1(6) . . . . ? C10 N2 C6 C7 -0.5(5) . . . . ? Zn1 N2 C6 C7 178.2(3) 6_566 . . . ? N2 C6 C7 C8 0.3(6) . . . . ? C6 C7 C8 C9 0.2(5) . . . . ? C6 C7 C8 C12 -179.9(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? C12 C8 C9 C10 179.6(4) . . . . ? C6 N2 C10 C9 0.2(6) . . . . ? Zn1 N2 C10 C9 -178.3(3) 6_566 . . . ? C8 C9 C10 N2 0.3(6) . . . . ? C12 N5 C11 N3 0.3(4) . . . . ? C12 N5 C11 C3 -179.5(3) . . . . ? N4 N3 C11 N5 0.3(4) . . . . ? Zn1 N3 C11 N5 164.5(3) . . . . ? N4 N3 C11 C3 -179.9(3) . . . . ? Zn1 N3 C11 C3 -15.7(5) . . . . ? C2 C3 C11 N5 -41.6(5) . . . . ? C4 C3 C11 N5 138.8(4) . . . . ? C2 C3 C11 N3 138.6(4) . . . . ? C4 C3 C11 N3 -41.0(5) . . . . ? N3 N4 C12 N5 1.1(4) . . . . ? N3 N4 C12 C8 -179.1(3) . . . . ? C11 N5 C12 N4 -0.9(4) . . . . ? C11 N5 C12 C8 179.3(3) . . . . ? C7 C8 C12 N4 -9.1(5) . . . . ? C9 C8 C12 N4 170.7(3) . . . . ? C7 C8 C12 N5 170.7(3) . . . . ? C9 C8 C12 N5 -9.5(5) . . . . ? 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 C2 H2 N5 0.94 2.38 3.289(5) 163.3 2_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.378 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.074 # Attachment '- Cd-4.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 722455' #TrackingRef '- Cd-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 Cd N5 O7 S, 2(H2 O)' _chemical_formula_sum 'C12 H19 Cd N5 O9 S' _chemical_formula_weight 521.78 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' S S 0.1246 0.1234 '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' _symmetry_Int_Tables_number 14 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 7.9223(15) _cell_length_b 14.721(3) _cell_length_c 15.965(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.897(3) _cell_angle_gamma 90.00 _cell_volume 1815.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3732 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7403 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3362 _reflns_number_gt 3051 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _refine_special_details ; All hydrogen atoms of water molecules were found in Fourier maps, and their coordinates and isotropic temperature factors were refined. 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^)+(0.0303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3362 _refine_ls_number_parameters 284 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.24907(3) 0.136805(15) 0.716399(13) 0.02084(8) Uani 1 1 d . . . S1 S 0.43776(10) -0.07179(5) 0.68786(5) 0.02074(17) Uani 1 1 d . . . O1 O 0.3112(3) -0.01291(16) 0.71727(14) 0.0379(6) Uani 1 1 d . . . O2 O 0.3911(3) -0.16578(16) 0.69908(17) 0.0442(7) Uani 1 1 d . . . O3 O 0.6137(3) -0.05497(17) 0.74062(14) 0.0369(6) Uani 1 1 d . . . O4 O 0.4375(3) -0.05324(18) 0.59859(13) 0.0416(7) Uani 1 1 d . . . O5 O 0.5117(3) 0.18717(18) 0.70051(16) 0.0388(6) Uani 1 1 d D . . H5A H 0.565(4) 0.167(2) 0.667(2) 0.047 Uiso 1 1 d D . . H5B H 0.563(4) 0.2299(18) 0.727(2) 0.047 Uiso 1 1 d D . . O6 O 0.1913(3) 0.28761(16) 0.74280(16) 0.0307(5) Uani 1 1 d D . . H6A H 0.250(4) 0.3343(15) 0.751(2) 0.037 Uiso 1 1 d D . . H6B H 0.092(2) 0.308(2) 0.730(2) 0.037 Uiso 1 1 d D . . O7 O -0.0356(3) 0.1045(2) 0.71926(14) 0.0359(6) Uani 1 1 d D . . H7A H -0.112(3) 0.101(3) 0.6756(14) 0.043 Uiso 1 1 d D . . H7B H -0.064(5) 0.109(2) 0.7649(13) 0.043 Uiso 1 1 d D . . O8 O 0.6702(3) 0.08758(18) 0.58279(15) 0.0344(6) Uani 1 1 d D . . H8A H 0.651(5) 0.089(3) 0.5303(7) 0.041 Uiso 1 1 d D . . H8B H 0.608(4) 0.0445(16) 0.589(2) 0.041 Uiso 1 1 d D . . O9 O 0.8570(4) 0.3431(2) 0.68642(16) 0.0558(9) Uani 1 1 d D . . H9A H 0.837(6) 0.368(3) 0.6391(13) 0.067 Uiso 1 1 d D . . H9B H 0.807(5) 0.375(2) 0.715(2) 0.067 Uiso 1 1 d D . . N1 N 0.1357(3) 0.15879(17) 0.57116(15) 0.0227(6) Uani 1 1 d . . . N2 N -0.3213(3) 0.63033(16) 0.63348(15) 0.0217(6) Uani 1 1 d . . . N3 N -0.1729(3) 0.37903(17) 0.36903(15) 0.0223(6) Uani 1 1 d . . . N4 N -0.2480(3) 0.45909(17) 0.38203(14) 0.0220(6) Uani 1 1 d . . . H4 H -0.2977 0.4962 0.3416 0.026 Uiso 1 1 calc R . . N5 N -0.1513(3) 0.40242(17) 0.51043(14) 0.0205(6) Uani 1 1 d . . . C1 C 0.1468(5) 0.1005(2) 0.50794(19) 0.0289(8) Uani 1 1 d . . . H1 H 0.2055 0.0451 0.5221 0.035 Uiso 1 1 calc R . . C2 C 0.0746(5) 0.1193(2) 0.4231(2) 0.0370(9) Uani 1 1 d . . . H2 H 0.0853 0.0774 0.3802 0.044 Uiso 1 1 calc R . . C3 C -0.0124(4) 0.1989(2) 0.40122(19) 0.0279(8) Uani 1 1 d . . . H3 H -0.0624 0.2121 0.3434 0.033 Uiso 1 1 calc R . . C4 C -0.0259(4) 0.2597(2) 0.46552(17) 0.0197(7) Uani 1 1 d . . . C5 C 0.0512(4) 0.2366(2) 0.54868(18) 0.0250(7) Uani 1 1 d . . . H5 H 0.0440 0.2782 0.5924 0.030 Uiso 1 1 calc R . . C6 C -0.4166(4) 0.6939(2) 0.58546(19) 0.0258(7) Uani 1 1 d . . . H6 H -0.4578 0.7428 0.6132 0.031 Uiso 1 1 calc R . . C7 C -0.4575(4) 0.6912(2) 0.49670(19) 0.0269(7) Uani 1 1 d . . . H7 H -0.5247 0.7374 0.4648 0.032 Uiso 1 1 calc R . . C8 C -0.3978(4) 0.6195(2) 0.4556(2) 0.0254(7) Uani 1 1 d . . . H8 H -0.4232 0.6167 0.3953 0.030 Uiso 1 1 calc R . . C9 C -0.3007(4) 0.5520(2) 0.50368(17) 0.0184(6) Uani 1 1 d . . . C10 C -0.2646(4) 0.5611(2) 0.59327(18) 0.0225(7) Uani 1 1 d . . . H10 H -0.1969 0.5162 0.6268 0.027 Uiso 1 1 calc R . . C11 C -0.1170(4) 0.3471(2) 0.44737(17) 0.0185(6) Uani 1 1 d . . . C12 C -0.2345(4) 0.4726(2) 0.46628(17) 0.0199(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 Cd1 0.02452(14) 0.02049(14) 0.01762(12) 0.00277(9) 0.00493(9) 0.00294(11) S1 0.0250(4) 0.0187(4) 0.0188(3) -0.0009(3) 0.0054(3) 0.0023(3) O1 0.0425(15) 0.0248(13) 0.0519(15) -0.0010(12) 0.0220(13) 0.0101(12) O2 0.0447(17) 0.0198(13) 0.0686(18) 0.0112(13) 0.0137(14) 0.0046(12) O3 0.0287(13) 0.0459(16) 0.0314(12) -0.0145(11) -0.0034(10) 0.0004(12) O4 0.0394(15) 0.0648(19) 0.0203(11) 0.0058(12) 0.0060(11) -0.0007(14) O5 0.0327(15) 0.0457(17) 0.0416(15) -0.0191(13) 0.0157(12) -0.0142(13) O6 0.0283(14) 0.0222(13) 0.0374(12) -0.0029(11) -0.0014(12) 0.0030(11) O7 0.0236(13) 0.0620(17) 0.0233(12) -0.0053(13) 0.0077(10) -0.0057(13) O8 0.0379(15) 0.0382(15) 0.0276(12) -0.0057(12) 0.0085(12) -0.0066(13) O9 0.062(2) 0.079(2) 0.0317(15) 0.0230(15) 0.0225(14) 0.0433(18) N1 0.0266(15) 0.0228(14) 0.0188(12) 0.0036(11) 0.0054(11) 0.0049(12) N2 0.0303(15) 0.0173(14) 0.0178(12) -0.0016(11) 0.0060(11) 0.0000(12) N3 0.0236(14) 0.0230(15) 0.0206(13) -0.0009(11) 0.0056(11) 0.0060(12) N4 0.0268(15) 0.0223(14) 0.0162(12) 0.0048(11) 0.0032(11) 0.0076(12) N5 0.0234(14) 0.0212(14) 0.0170(12) -0.0008(11) 0.0049(11) 0.0044(12) C1 0.039(2) 0.0205(17) 0.0268(16) 0.0000(14) 0.0061(15) 0.0103(16) C2 0.053(2) 0.031(2) 0.0247(16) -0.0086(15) 0.0040(16) 0.0139(19) C3 0.0315(19) 0.0302(19) 0.0189(15) -0.0036(14) -0.0008(14) 0.0070(16) C4 0.0187(16) 0.0214(16) 0.0200(14) -0.0013(13) 0.0062(13) 0.0007(14) C5 0.0331(19) 0.0256(18) 0.0159(14) -0.0011(13) 0.0045(13) 0.0106(16) C6 0.0331(19) 0.0197(17) 0.0259(16) -0.0050(14) 0.0091(15) 0.0029(15) C7 0.0290(19) 0.0243(18) 0.0260(16) 0.0044(14) 0.0034(14) 0.0080(16) C8 0.0304(18) 0.0250(18) 0.0213(15) 0.0019(13) 0.0068(14) 0.0035(15) C9 0.0180(16) 0.0176(16) 0.0185(14) 0.0010(12) 0.0021(12) 0.0001(13) C10 0.0274(18) 0.0205(16) 0.0194(14) 0.0020(13) 0.0050(13) 0.0018(15) C11 0.0186(15) 0.0205(16) 0.0165(14) -0.0004(12) 0.0040(12) 0.0003(14) C12 0.0208(16) 0.0219(16) 0.0169(14) 0.0002(13) 0.0038(12) -0.0022(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 Cd1 O1 2.258(2) . ? Cd1 O5 2.275(2) . ? Cd1 N1 2.315(2) . ? Cd1 O7 2.316(2) . ? Cd1 O6 2.324(2) . ? Cd1 N2 2.339(2) 2_546 ? S1 O4 1.451(2) . ? S1 O2 1.454(2) . ? S1 O1 1.479(2) . ? S1 O3 1.479(2) . ? O5 H5A 0.814(10) . ? O5 H5B 0.813(10) . ? O6 H6A 0.822(10) . ? O6 H6B 0.824(10) . ? O7 H7A 0.815(10) . ? O7 H7B 0.812(10) . ? O8 H8A 0.818(10) . ? O8 H8B 0.821(10) . ? O9 H9A 0.820(10) . ? O9 H9B 0.818(10) . ? N1 C5 1.335(4) . ? N1 C1 1.343(4) . ? N2 C6 1.333(4) . ? N2 C10 1.334(4) . ? N2 Cd1 2.339(2) 2_556 ? N3 C11 1.317(4) . ? N3 N4 1.357(3) . ? N4 C12 1.340(3) . ? N4 H4 0.8700 . ? N5 C12 1.338(4) . ? N5 C11 1.369(3) . ? C1 C2 1.375(5) . ? C1 H1 0.9400 . ? C2 C3 1.364(4) . ? C2 H2 0.9400 . ? C3 C4 1.385(4) . ? C3 H3 0.9400 . ? C4 C5 1.375(4) . ? C4 C11 1.472(4) . ? C5 H5 0.9400 . ? C6 C7 1.382(4) . ? C6 H6 0.9400 . ? C7 C8 1.381(4) . ? C7 H7 0.9400 . ? C8 C9 1.380(4) . ? C8 H8 0.9400 . ? C9 C10 1.401(4) . ? C9 C12 1.463(4) . ? C10 H10 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O5 96.61(9) . . ? O1 Cd1 N1 100.25(9) . . ? O5 Cd1 N1 90.15(9) . . ? O1 Cd1 O7 90.65(10) . . ? O5 Cd1 O7 171.11(10) . . ? N1 Cd1 O7 83.50(8) . . ? O1 Cd1 O6 169.37(8) . . ? O5 Cd1 O6 86.04(9) . . ? N1 Cd1 O6 90.01(9) . . ? O7 Cd1 O6 87.75(10) . . ? O1 Cd1 N2 87.18(8) . 2_546 ? O5 Cd1 N2 96.13(9) . 2_546 ? N1 Cd1 N2 169.69(9) . 2_546 ? O7 Cd1 N2 89.32(8) . 2_546 ? O6 Cd1 N2 82.31(8) . 2_546 ? O4 S1 O2 110.84(15) . . ? O4 S1 O1 110.44(14) . . ? O2 S1 O1 108.04(14) . . ? O4 S1 O3 108.80(14) . . ? O2 S1 O3 108.82(16) . . ? O1 S1 O3 109.89(14) . . ? S1 O1 Cd1 137.11(14) . . ? Cd1 O5 H5A 125(3) . . ? Cd1 O5 H5B 124(3) . . ? H5A O5 H5B 110(4) . . ? Cd1 O6 H6A 134(3) . . ? Cd1 O6 H6B 121(3) . . ? H6A O6 H6B 102(3) . . ? Cd1 O7 H7A 122(3) . . ? Cd1 O7 H7B 118(3) . . ? H7A O7 H7B 118(4) . . ? H8A O8 H8B 99(3) . . ? H9A O9 H9B 104(4) . . ? C5 N1 C1 117.3(3) . . ? C5 N1 Cd1 116.65(19) . . ? C1 N1 Cd1 126.0(2) . . ? C6 N2 C10 117.9(2) . . ? C6 N2 Cd1 122.59(19) . 2_556 ? C10 N2 Cd1 119.5(2) . 2_556 ? C11 N3 N4 103.3(2) . . ? C12 N4 N3 110.1(2) . . ? C12 N4 H4 125.0 . . ? N3 N4 H4 125.0 . . ? C12 N5 C11 103.1(2) . . ? N1 C1 C2 121.9(3) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 117.7(3) . . ? C5 C4 C11 120.0(3) . . ? C3 C4 C11 122.4(3) . . ? N1 C5 C4 124.1(3) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? N2 C6 C7 122.9(3) . . ? N2 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C8 C7 C6 118.8(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 117.4(3) . . ? C8 C9 C12 123.7(3) . . ? C10 C9 C12 118.9(3) . . ? N2 C10 C9 123.4(3) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N3 C11 N5 114.0(3) . . ? N3 C11 C4 123.0(3) . . ? N5 C11 C4 123.0(2) . . ? N5 C12 N4 109.5(3) . . ? N5 C12 C9 125.5(2) . . ? N4 C12 C9 124.9(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 O4 S1 O1 Cd1 -51.4(3) . . . . ? O2 S1 O1 Cd1 -172.7(2) . . . . ? O3 S1 O1 Cd1 68.7(2) . . . . ? O5 Cd1 O1 S1 -21.2(2) . . . . ? N1 Cd1 O1 S1 70.1(2) . . . . ? O7 Cd1 O1 S1 153.6(2) . . . . ? O6 Cd1 O1 S1 -125.2(4) . . . . ? N2 Cd1 O1 S1 -117.1(2) 2_546 . . . ? O1 Cd1 N1 C5 166.5(2) . . . . ? O5 Cd1 N1 C5 -96.8(2) . . . . ? O7 Cd1 N1 C5 77.0(2) . . . . ? O6 Cd1 N1 C5 -10.7(2) . . . . ? N2 Cd1 N1 C5 30.9(6) 2_546 . . . ? O1 Cd1 N1 C1 -13.2(3) . . . . ? O5 Cd1 N1 C1 83.5(3) . . . . ? O7 Cd1 N1 C1 -102.7(3) . . . . ? O6 Cd1 N1 C1 169.5(3) . . . . ? N2 Cd1 N1 C1 -148.8(4) 2_546 . . . ? C11 N3 N4 C12 0.2(3) . . . . ? C5 N1 C1 C2 0.1(5) . . . . ? Cd1 N1 C1 C2 179.8(3) . . . . ? N1 C1 C2 C3 -0.5(6) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C2 C3 C4 C11 179.8(3) . . . . ? C1 N1 C5 C4 0.7(5) . . . . ? Cd1 N1 C5 C4 -179.0(2) . . . . ? C3 C4 C5 N1 -1.0(5) . . . . ? C11 C4 C5 N1 179.7(3) . . . . ? C10 N2 C6 C7 -0.4(5) . . . . ? Cd1 N2 C6 C7 179.0(2) 2_556 . . . ? N2 C6 C7 C8 0.2(5) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? C7 C8 C9 C10 -1.2(4) . . . . ? C7 C8 C9 C12 178.8(3) . . . . ? C6 N2 C10 C9 -0.3(4) . . . . ? Cd1 N2 C10 C9 -179.6(2) 2_556 . . . ? C8 C9 C10 N2 1.1(5) . . . . ? C12 C9 C10 N2 -179.0(3) . . . . ? N4 N3 C11 N5 -0.2(3) . . . . ? N4 N3 C11 C4 179.7(3) . . . . ? C12 N5 C11 N3 0.1(3) . . . . ? C12 N5 C11 C4 -179.7(3) . . . . ? C5 C4 C11 N3 170.4(3) . . . . ? C3 C4 C11 N3 -8.8(5) . . . . ? C5 C4 C11 N5 -9.7(4) . . . . ? C3 C4 C11 N5 171.1(3) . . . . ? C11 N5 C12 N4 0.0(3) . . . . ? C11 N5 C12 C9 -180.0(3) . . . . ? N3 N4 C12 N5 -0.1(3) . . . . ? N3 N4 C12 C9 179.9(3) . . . . ? C8 C9 C12 N5 -174.6(3) . . . . ? C10 C9 C12 N5 5.4(5) . . . . ? C8 C9 C12 N4 5.4(5) . . . . ? C10 C9 C12 N4 -174.6(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 N4 H4 O3 0.87 1.83 2.681(3) 166.9 4_465 O9 H9B S1 0.818(10) 2.848(19) 3.625(3) 159(4) 2_656 O9 H9B O2 0.818(10) 2.38(3) 2.970(3) 130(4) 2_656 O9 H9B O1 0.818(10) 2.283(13) 3.090(3) 169(4) 2_656 O9 H9A N5 0.820(10) 2.138(17) 2.929(3) 162(4) 1_655 O8 H8B S1 0.821(10) 2.865(18) 3.618(3) 153(3) . O8 H8B O4 0.821(10) 2.004(11) 2.822(4) 175(4) . O8 H8A O4 0.818(10) 2.086(15) 2.875(3) 162(4) 3_656 O7 H7B N3 0.812(10) 2.044(12) 2.850(3) 171(4) 4_566 O7 H7A O8 0.815(10) 2.020(13) 2.824(4) 169(4) 1_455 O6 H6B O9 0.824(10) 1.908(12) 2.726(4) 171(4) 1_455 O6 H6A S1 0.822(10) 2.816(19) 3.563(3) 152(3) 2_656 O6 H6A O3 0.822(10) 1.945(11) 2.765(4) 176(4) 2_656 O5 H5B O2 0.813(10) 1.925(16) 2.702(3) 159(4) 2_656 O5 H5A O8 0.814(10) 2.084(13) 2.883(3) 167(4) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.381 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.078