Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Paul O'Brian" _publ_contact_author_address ; School of Chemistry The University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email PAUL.OBRIEN@MANCHESTER.AC.UK _publ_section_title ; The N-alkyldithiocarbamato complexes [M(S2CNHR)2] (M = Cd(II) Zn(II); R = C2H5, C4H9, C6H13, C12H25); Their synthesis, thermal decomposition and use to prepare of nano -particles and -rods of CdS. ; loop_ _publ_author_name P.O'Brian 'Mohammad Afzaal' 'Mohammad A. Malik' 'Ashfaq A. Memon' 'Chinh Q. Nguyen' 'Jim Raftery' # Attachment 'Compound7.cif' data_s2062ma _database_code_depnum_ccdc_archive 'CCDC 285987' _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically, except where the ADP becomes NPD or unrealistic. H atoms were included in calculated positions, except where they were largely indeterminate. ; # Insert blank lines between references _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 N4 S8 Zn2' _chemical_formula_weight 835.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5670(5) _cell_length_b 8.3420(6) _cell_length_c 16.5130(12) _cell_angle_alpha 97.5570(10) _cell_angle_beta 91.1570(10) _cell_angle_gamma 113.3540(10) _cell_volume 945.66(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4826 _cell_measurement_theta_min 2.4955 _cell_measurement_theta_max 28.2795 _exptl_crystal_description plate _exptl_crystal_colour white _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5436 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8258 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4308 _reflns_number_gt 3897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR2004 (Burla et al, 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4308 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _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 C1 C 0.2497(3) -1.0152(2) -0.00178(13) 0.0285(5) Uani 1 1 d . . . H1A H 0.3306 -1.0577 0.0287 0.043 Uiso 1 1 calc R . . H1B H 0.2456 -1.0558 -0.0605 0.043 Uiso 1 1 calc R . . H1C H 0.1185 -1.0617 0.0162 0.043 Uiso 1 1 calc R . . C2 C 0.3338(3) -0.8145(2) 0.01409(11) 0.0204(4) Uani 1 1 d . . . H2A H 0.2504 -0.7732 -0.0167 0.025 Uiso 1 1 calc R . . H2B H 0.4629 -0.7691 -0.0074 0.025 Uiso 1 1 calc R . . C3 C 0.3531(3) -0.7368(2) 0.10408(11) 0.0163(4) Uani 1 1 d . . . H3A H 0.4373 -0.7767 0.1352 0.020 Uiso 1 1 calc R . . H3B H 0.2243 -0.7808 0.1260 0.020 Uiso 1 1 calc R . . C4 C 0.4379(3) -0.5356(2) 0.11637(11) 0.0158(4) Uani 1 1 d . . . H4A H 0.5626 -0.4928 0.0911 0.019 Uiso 1 1 calc R . . H4B H 0.3496 -0.4967 0.0874 0.019 Uiso 1 1 calc R . . C5 C 0.4708(3) -0.4512(2) 0.20588(11) 0.0166(4) Uani 1 1 d . . . H5A H 0.5572 -0.4912 0.2355 0.020 Uiso 1 1 calc R . . H5B H 0.3460 -0.4904 0.2311 0.020 Uiso 1 1 calc R . . C6 C 0.5603(3) -0.2504(2) 0.21487(11) 0.0160(4) Uani 1 1 d . . . H6A H 0.6851 -0.2107 0.1896 0.019 Uiso 1 1 calc R . . H6B H 0.4737 -0.2098 0.1858 0.019 Uiso 1 1 calc R . . C7 C 0.6712(2) -0.0023(2) 0.32995(10) 0.0137(3) Uani 1 1 d . . . C8 C 0.7579(2) 0.6204(2) 0.51910(10) 0.0119(3) Uani 1 1 d . . . C9 C 0.7552(3) 0.8291(2) 0.64016(10) 0.0157(4) Uani 1 1 d . . . H9A H 0.8380 0.7854 0.6697 0.019 Uiso 1 1 calc R . . H9B H 0.6258 0.7833 0.6614 0.019 Uiso 1 1 calc R . . C10 C 0.8415(3) 1.0304(2) 0.65638(11) 0.0149(3) Uani 1 1 d . . . H10A H 0.9689 1.0769 0.6335 0.018 Uiso 1 1 calc R . . H10B H 0.7561 1.0746 0.6289 0.018 Uiso 1 1 calc R . . C11 C 0.8645(3) 1.0952(2) 0.74781(11) 0.0151(3) Uani 1 1 d . . . H11A H 0.9462 1.0466 0.7748 0.018 Uiso 1 1 calc R . . H11B H 0.7360 1.0491 0.7699 0.018 Uiso 1 1 calc R . . C12 C 0.9546(3) 1.2958(2) 0.76940(11) 0.0156(3) Uani 1 1 d . . . H12A H 1.0827 1.3423 0.7471 0.019 Uiso 1 1 calc R . . H12B H 0.8723 1.3446 0.7431 0.019 Uiso 1 1 calc R . . C13 C 0.9783(3) 1.3581(2) 0.86136(11) 0.0168(4) Uani 1 1 d . . . H13A H 1.0592 1.3078 0.8876 0.020 Uiso 1 1 calc R . . H13B H 0.8499 1.3121 0.8834 0.020 Uiso 1 1 calc R . . C14 C 1.0702(3) 1.5585(2) 0.88430(12) 0.0205(4) Uani 1 1 d . . . H14A H 1.2000 1.6048 0.8649 0.031 Uiso 1 1 calc R . . H14B H 1.0788 1.5899 0.9440 0.031 Uiso 1 1 calc R . . H14C H 0.9908 1.6096 0.8587 0.031 Uiso 1 1 calc R . . N1 N 0.5913(2) -0.17290(19) 0.30132(9) 0.0159(3) Uani 1 1 d . . . H1 H 0.5535 -0.2462 0.3374 0.019 Uiso 1 1 calc R . . N2 N 0.7384(2) 0.76315(19) 0.55245(9) 0.0143(3) Uani 1 1 d . . . H2 H 0.7125 0.8258 0.5187 0.017 Uiso 1 1 calc R . . S1 S 0.70420(7) 0.06568(6) 0.43462(3) 0.01640(10) Uani 1 1 d . . . S2 S 0.74317(6) 0.15575(6) 0.26673(3) 0.01510(10) Uani 1 1 d . . . S3 S 0.71720(6) 0.56253(6) 0.41423(3) 0.01345(10) Uani 1 1 d . . . S4 S 0.81705(6) 0.48708(5) 0.57760(3) 0.01252(10) Uani 1 1 d . . . Zn1 Zn 0.84693(3) 0.35085(2) 0.400473(12) 0.01319(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 C1 0.0393(12) 0.0117(9) 0.0265(11) -0.0025(8) 0.0034(9) 0.0035(8) C2 0.0271(10) 0.0115(9) 0.0181(9) -0.0003(7) 0.0002(8) 0.0038(7) C3 0.0192(9) 0.0112(8) 0.0169(9) 0.0014(7) 0.0005(7) 0.0047(7) C4 0.0179(9) 0.0120(8) 0.0159(9) 0.0008(7) 0.0006(7) 0.0048(7) C5 0.0201(9) 0.0122(9) 0.0167(9) 0.0007(7) 0.0004(7) 0.0060(7) C6 0.0208(9) 0.0138(8) 0.0123(8) -0.0009(7) -0.0012(7) 0.0067(7) C7 0.0131(8) 0.0149(8) 0.0145(8) 0.0021(7) 0.0008(6) 0.0073(7) C8 0.0099(7) 0.0112(8) 0.0135(8) 0.0015(6) 0.0010(6) 0.0033(6) C9 0.0209(9) 0.0129(9) 0.0130(8) -0.0012(7) 0.0005(7) 0.0074(7) C10 0.0195(9) 0.0121(8) 0.0132(8) 0.0005(6) 0.0008(7) 0.0069(7) C11 0.0181(9) 0.0120(8) 0.0151(9) -0.0001(7) 0.0015(7) 0.0065(7) C12 0.0197(9) 0.0128(8) 0.0142(8) 0.0009(7) 0.0008(7) 0.0070(7) C13 0.0203(9) 0.0134(9) 0.0144(9) 0.0006(7) 0.0007(7) 0.0049(7) C14 0.0250(10) 0.0148(9) 0.0178(9) -0.0011(7) 0.0014(7) 0.0051(7) N1 0.0232(8) 0.0113(7) 0.0119(7) 0.0011(6) -0.0010(6) 0.0059(6) N2 0.0190(7) 0.0123(7) 0.0132(7) 0.0012(6) 0.0006(6) 0.0081(6) S1 0.0256(2) 0.0111(2) 0.0112(2) 0.00065(16) 0.00079(17) 0.00634(18) S2 0.0202(2) 0.0115(2) 0.0122(2) 0.00155(16) 0.00024(16) 0.00509(17) S3 0.0176(2) 0.0129(2) 0.0116(2) -0.00003(16) -0.00067(16) 0.00860(17) S4 0.0140(2) 0.0103(2) 0.0136(2) 0.00219(16) 0.00061(15) 0.00513(16) Zn1 0.01377(11) 0.00972(11) 0.01601(12) 0.00035(8) -0.00045(8) 0.00523(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.520(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.523(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.522(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.461(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.321(2) . ? C7 S2 1.7145(18) . ? C7 S1 1.7275(18) . ? C8 N2 1.309(2) . ? C8 S3 1.7227(17) . ? C8 S4 1.7409(17) . ? C9 N2 1.464(2) . ? C9 C10 1.524(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.517(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.523(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.522(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N1 H1 0.8800 . ? N2 H2 0.8800 . ? S1 Zn1 2.3418(5) . ? S2 Zn1 2.4727(5) . ? S3 Zn1 2.3262(5) . ? S4 Zn1 2.3522(5) 2_766 ? Zn1 S4 2.3522(5) 2_766 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 113.94(16) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 111.69(14) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 113.69(14) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 111.60(15) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C5 110.44(14) . . ? N1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N1 C7 S2 122.30(14) . . ? N1 C7 S1 119.28(13) . . ? S2 C7 S1 118.42(10) . . ? N2 C8 S3 118.09(13) . . ? N2 C8 S4 122.02(13) . . ? S3 C8 S4 119.87(10) . . ? N2 C9 C10 111.25(14) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 110.14(14) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 113.46(15) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 112.69(15) . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 113.51(15) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 N1 C6 125.57(15) . . ? C7 N1 H1 117.2 . . ? C6 N1 H1 117.2 . . ? C8 N2 C9 126.60(15) . . ? C8 N2 H2 116.7 . . ? C9 N2 H2 116.7 . . ? C7 S1 Zn1 84.78(6) . . ? C7 S2 Zn1 81.03(6) . . ? C8 S3 Zn1 97.64(6) . . ? C8 S4 Zn1 99.75(6) . 2_766 ? S3 Zn1 S1 126.310(18) . . ? S3 Zn1 S4 104.923(17) . 2_766 ? S1 Zn1 S4 120.428(17) . 2_766 ? S3 Zn1 S2 112.137(17) . . ? S1 Zn1 S2 75.727(16) . . ? S4 Zn1 S2 113.786(16) 2_766 . ? 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 C1 C2 C3 C4 -179.98(16) . . . . ? C2 C3 C4 C5 -176.71(16) . . . . ? C3 C4 C5 C6 178.57(15) . . . . ? C4 C5 C6 N1 -179.67(14) . . . . ? N2 C9 C10 C11 -177.79(14) . . . . ? C9 C10 C11 C12 178.64(14) . . . . ? C10 C11 C12 C13 -179.43(15) . . . . ? C11 C12 C13 C14 179.41(15) . . . . ? S2 C7 N1 C6 2.5(3) . . . . ? S1 C7 N1 C6 -177.73(13) . . . . ? C5 C6 N1 C7 178.07(16) . . . . ? S3 C8 N2 C9 176.18(14) . . . . ? S4 C8 N2 C9 -2.2(2) . . . . ? C10 C9 N2 C8 146.12(17) . . . . ? N1 C7 S1 Zn1 178.09(14) . . . . ? S2 C7 S1 Zn1 -2.15(9) . . . . ? N1 C7 S2 Zn1 -178.20(15) . . . . ? S1 C7 S2 Zn1 2.05(9) . . . . ? N2 C8 S3 Zn1 167.30(13) . . . . ? S4 C8 S3 Zn1 -14.30(10) . . . . ? N2 C8 S4 Zn1 -80.90(14) . . . 2_766 ? S3 C8 S4 Zn1 100.77(9) . . . 2_766 ? C8 S3 Zn1 S1 74.70(6) . . . . ? C8 S3 Zn1 S4 -73.11(6) . . . 2_766 ? C8 S3 Zn1 S2 162.91(6) . . . . ? C7 S1 Zn1 S3 108.55(6) . . . . ? C7 S1 Zn1 S4 -108.11(6) . . . 2_766 ? C7 S1 Zn1 S2 1.35(6) . . . . ? C7 S2 Zn1 S3 -125.17(6) . . . . ? C7 S2 Zn1 S1 -1.38(6) . . . . ? C7 S2 Zn1 S4 115.94(6) . . . 2_766 ? 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 N1 H1 S3 0.88 2.78 3.4544(15) 134.5 1_545 N2 H2 S1 0.88 2.60 3.4656(15) 167.6 1_565 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.674 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.173 # Attachment 'compound9.cif' data_s2125m _database_code_depnum_ccdc_archive 'CCDC 285988' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the Cd monomer; the monomer grows into a polymeric structure by space group symmetry. H atoms were included in calculated positions. Non H atoms were refined anisotropically. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cd2 N8 O8 S2' _chemical_formula_weight 1049.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0273(15) _cell_length_b 20.111(2) _cell_length_c 17.171(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.398(2) _cell_angle_gamma 90.00 _cell_volume 4056.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2154 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.01 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.215 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7931 _exptl_absorpt_correction_T_max 0.9417 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26140 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.43 _reflns_number_total 8278 _reflns_number_gt 4130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8278 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.724 _refine_ls_restrained_S_all 0.724 _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 0.25272(5) 0.12203(2) 0.23912(3) 0.00933(11) Uani 1 1 d . . . Cd2 Cd -0.24599(5) 0.12149(2) 0.24009(3) 0.00930(11) Uani 1 1 d . . . S1 S 0.00100(12) 0.21923(6) 0.24163(7) 0.0089(3) Uani 1 1 d . . . S2 S 0.50556(12) 0.02410(6) 0.24252(7) 0.0089(3) Uani 1 1 d . . . O1 O 0.1231(3) 0.20236(17) 0.24859(19) 0.0135(9) Uani 1 1 d . . . O2 O -0.0603(3) 0.15699(17) 0.25442(18) 0.0113(8) Uani 1 1 d . . . O3 O -0.0453(3) 0.24554(18) 0.16157(19) 0.0177(9) Uani 1 1 d . . . O4 O -0.0085(3) 0.26762(17) 0.3027(2) 0.0149(9) Uani 1 1 d . . . O5 O 0.3821(3) 0.04189(17) 0.22967(19) 0.0134(9) Uani 1 1 d . . . O6 O 0.5190(3) -0.02550(17) 0.18274(19) 0.0121(8) Uani 1 1 d . . . O7 O 0.5442(3) -0.00152(17) 0.32375(19) 0.0136(9) Uani 1 1 d . . . O8 O 0.5687(3) 0.08564(17) 0.23150(18) 0.0105(8) Uani 1 1 d . . . N1 N 0.2581(4) 0.0915(2) 0.3733(3) 0.0135(11) Uani 1 1 d . . . N2 N 0.1242(4) 0.0372(2) 0.1925(2) 0.0101(10) Uani 1 1 d . . . N3 N 0.2456(4) 0.1582(2) 0.1069(2) 0.0129(11) Uani 1 1 d . . . N4 N 0.3830(4) 0.2061(2) 0.2878(2) 0.0122(11) Uani 1 1 d . . . N5 N -0.1621(4) 0.0176(2) 0.2853(2) 0.0127(11) Uani 1 1 d . . . N6 N -0.2260(4) 0.1451(2) 0.3757(2) 0.0096(10) Uani 1 1 d . . . N7 N -0.3300(4) 0.2258(2) 0.1965(2) 0.0130(11) Uani 1 1 d . . . N8 N -0.2659(4) 0.0964(2) 0.1049(2) 0.0121(11) Uani 1 1 d . . . C1 C 0.3437(5) 0.0548(3) 0.4167(3) 0.0143(13) Uani 1 1 d . . . H1 H 0.3985 0.0356 0.3910 0.017 Uiso 1 1 calc R . . C2 C 0.3534(5) 0.0443(3) 0.4974(3) 0.0129(13) Uani 1 1 d . . . H2 H 0.4142 0.0183 0.5265 0.015 Uiso 1 1 calc R . . C3 C 0.2752(5) 0.0717(3) 0.5353(3) 0.0193(15) Uani 1 1 d . . . H3 H 0.2816 0.0652 0.5909 0.023 Uiso 1 1 calc R . . C4 C 0.1868(5) 0.1087(3) 0.4917(3) 0.0168(14) Uani 1 1 d . . . H4 H 0.1301 0.1271 0.5163 0.020 Uiso 1 1 calc R . . C5 C 0.1827(5) 0.1185(3) 0.4113(3) 0.0145(14) Uani 1 1 d . . . H5 H 0.1238 0.1455 0.3817 0.017 Uiso 1 1 calc R . . C6 C 0.1442(5) -0.0230(3) 0.2257(3) 0.0156(13) Uani 1 1 d . . . H6 H 0.2053 -0.0276 0.2707 0.019 Uiso 1 1 calc R . . C7 C 0.0812(5) -0.0786(3) 0.1983(3) 0.0176(14) Uani 1 1 d . . . H7 H 0.0975 -0.1204 0.2242 0.021 Uiso 1 1 calc R . . C8 C -0.0063(5) -0.0720(3) 0.1321(3) 0.0198(14) Uani 1 1 d . . . H8 H -0.0510 -0.1095 0.1113 0.024 Uiso 1 1 calc R . . C9 C -0.0283(5) -0.0113(3) 0.0968(3) 0.0216(15) Uani 1 1 d . . . H9 H -0.0885 -0.0057 0.0514 0.026 Uiso 1 1 calc R . . C10 C 0.0394(5) 0.0419(3) 0.1287(3) 0.0157(13) Uani 1 1 d . . . H10 H 0.0244 0.0841 0.1037 0.019 Uiso 1 1 calc R . . C11 C 0.1642(5) 0.1991(3) 0.0666(3) 0.0140(13) Uani 1 1 d . . . H11 H 0.1091 0.2165 0.0934 0.017 Uiso 1 1 calc R . . C12 C 0.1580(5) 0.2168(3) -0.0122(3) 0.0179(14) Uani 1 1 d . . . H12 H 0.0994 0.2454 -0.0392 0.021 Uiso 1 1 calc R . . C13 C 0.2385(5) 0.1919(3) -0.0508(3) 0.0193(14) Uani 1 1 d . . . H13 H 0.2364 0.2032 -0.1048 0.023 Uiso 1 1 calc R . . C14 C 0.3216(5) 0.1505(3) -0.0098(3) 0.0199(14) Uani 1 1 d . . . H14 H 0.3776 0.1326 -0.0354 0.024 Uiso 1 1 calc R . . C15 C 0.3234(5) 0.1350(3) 0.0686(3) 0.0137(14) Uani 1 1 d . . . H15 H 0.3821 0.1069 0.0966 0.016 Uiso 1 1 calc R . . C16 C 0.3596(5) 0.2676(3) 0.2594(3) 0.0135(13) Uani 1 1 d . . . H16 H 0.2989 0.2733 0.2144 0.016 Uiso 1 1 calc R . . C17 C 0.4193(5) 0.3236(3) 0.2922(3) 0.0150(13) Uani 1 1 d . . . H17 H 0.4004 0.3665 0.2702 0.018 Uiso 1 1 calc R . . C18 C 0.5073(5) 0.3147(3) 0.3582(4) 0.0264(16) Uani 1 1 d . . . H18 H 0.5501 0.3517 0.3826 0.032 Uiso 1 1 calc R . . C19 C 0.5322(5) 0.2520(3) 0.3881(3) 0.0209(14) Uani 1 1 d . . . H19 H 0.5917 0.2449 0.4336 0.025 Uiso 1 1 calc R . . C20 C 0.4689(5) 0.1992(3) 0.3507(3) 0.0163(13) Uani 1 1 d . . . H20 H 0.4877 0.1557 0.3710 0.020 Uiso 1 1 calc R . . C21 C -0.0689(5) 0.0182(3) 0.3450(3) 0.0151(13) Uani 1 1 d . . . H21 H -0.0408 0.0599 0.3668 0.018 Uiso 1 1 calc R . . C22 C -0.0124(5) -0.0385(3) 0.3761(3) 0.0168(14) Uani 1 1 d . . . H22 H 0.0526 -0.0356 0.4186 0.020 Uiso 1 1 calc R . . C23 C -0.0510(5) -0.0994(3) 0.3452(3) 0.0157(13) Uani 1 1 d . . . H23 H -0.0137 -0.1393 0.3660 0.019 Uiso 1 1 calc R . . C24 C -0.1457(5) -0.1010(3) 0.2830(3) 0.0164(13) Uani 1 1 d . . . H24 H -0.1737 -0.1421 0.2592 0.020 Uiso 1 1 calc R . . C25 C -0.1985(5) -0.0425(3) 0.2562(3) 0.0131(13) Uani 1 1 d . . . H25 H -0.2648 -0.0444 0.2146 0.016 Uiso 1 1 calc R . . C26 C -0.1533(5) 0.1920(3) 0.4140(3) 0.0133(13) Uani 1 1 d . . . H26 H -0.1084 0.2164 0.3846 0.016 Uiso 1 1 calc R . . C27 C -0.1424(5) 0.2053(3) 0.4932(3) 0.0108(13) Uani 1 1 d . . . H27 H -0.0902 0.2383 0.5182 0.013 Uiso 1 1 calc R . . C28 C -0.2071(5) 0.1709(3) 0.5372(3) 0.0131(13) Uani 1 1 d . . . H28 H -0.2020 0.1804 0.5920 0.016 Uiso 1 1 calc R . . C29 C -0.2790(5) 0.1224(3) 0.4990(3) 0.0127(14) Uani 1 1 d . . . H29 H -0.3231 0.0967 0.5277 0.015 Uiso 1 1 calc R . . C30 C -0.2867(5) 0.1111(3) 0.4189(3) 0.0121(14) Uani 1 1 d . . . H30 H -0.3375 0.0777 0.3933 0.015 Uiso 1 1 calc R . . C31 C -0.4210(5) 0.2267(3) 0.1362(3) 0.0175(14) Uani 1 1 d . . . H31 H -0.4461 0.1858 0.1110 0.021 Uiso 1 1 calc R . . C32 C -0.4812(5) 0.2838(3) 0.1082(3) 0.0190(14) Uani 1 1 d . . . H32 H -0.5444 0.2820 0.0642 0.023 Uiso 1 1 calc R . . C33 C -0.4466(5) 0.3435(3) 0.1461(3) 0.0193(14) Uani 1 1 d . . . H33 H -0.4865 0.3835 0.1291 0.023 Uiso 1 1 calc R . . C34 C -0.3531(5) 0.3437(3) 0.2089(3) 0.0167(13) Uani 1 1 d . . . H34 H -0.3281 0.3839 0.2363 0.020 Uiso 1 1 calc R . . C35 C -0.2963(5) 0.2845(3) 0.2313(3) 0.0148(13) Uani 1 1 d . . . H35 H -0.2303 0.2854 0.2732 0.018 Uiso 1 1 calc R . . C36 C -0.3384(5) 0.0491(3) 0.0686(3) 0.0119(13) Uani 1 1 d . . . H36 H -0.3831 0.0259 0.0991 0.014 Uiso 1 1 calc R . . C37 C -0.3504(5) 0.0329(3) -0.0101(3) 0.0141(13) Uani 1 1 d . . . H37 H -0.4034 -0.0001 -0.0339 0.017 Uiso 1 1 calc R . . C38 C -0.2832(5) 0.0658(3) -0.0549(3) 0.0140(13) Uani 1 1 d . . . H38 H -0.2877 0.0544 -0.1092 0.017 Uiso 1 1 calc R . . C39 C -0.2099(5) 0.1154(3) -0.0189(3) 0.0163(13) Uani 1 1 d . . . H39 H -0.1639 0.1389 -0.0481 0.020 Uiso 1 1 calc R . . C40 C -0.2051(5) 0.1298(3) 0.0602(3) 0.0122(15) Uani 1 1 d . . . H40 H -0.1569 0.1649 0.0843 0.015 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 Cd1 0.0089(2) 0.0104(2) 0.0085(2) 0.00019(17) 0.00149(18) -0.00024(17) Cd2 0.0095(2) 0.0104(2) 0.0076(2) -0.00087(16) 0.00104(18) -0.00028(17) S1 0.0074(8) 0.0087(7) 0.0102(7) 0.0006(5) 0.0009(6) -0.0002(6) S2 0.0067(8) 0.0090(7) 0.0107(7) -0.0006(6) 0.0014(6) 0.0005(6) O1 0.008(2) 0.014(2) 0.020(2) 0.0049(16) 0.0037(16) 0.0005(16) O2 0.008(2) 0.014(2) 0.0120(19) 0.0007(15) 0.0024(15) -0.0049(16) O3 0.017(2) 0.020(2) 0.0123(19) 0.0100(16) -0.0048(17) -0.0061(18) O4 0.016(2) 0.014(2) 0.017(2) -0.0015(16) 0.0073(17) 0.0023(18) O5 0.007(2) 0.012(2) 0.020(2) -0.0004(16) -0.0007(16) 0.0008(16) O6 0.012(2) 0.013(2) 0.0119(19) -0.0049(15) 0.0025(16) -0.0027(17) O7 0.014(2) 0.015(2) 0.0100(19) 0.0010(15) -0.0018(16) -0.0065(17) O8 0.008(2) 0.012(2) 0.0102(18) -0.0001(15) 0.0006(15) -0.0043(16) N1 0.010(3) 0.015(3) 0.013(2) -0.001(2) -0.001(2) -0.005(2) N2 0.007(3) 0.016(3) 0.007(2) -0.0017(19) 0.0004(18) 0.000(2) N3 0.013(3) 0.015(3) 0.011(2) -0.001(2) 0.002(2) -0.003(2) N4 0.011(3) 0.016(3) 0.010(2) -0.0006(19) 0.003(2) 0.002(2) N5 0.010(3) 0.018(3) 0.011(2) -0.001(2) 0.006(2) 0.003(2) N6 0.004(2) 0.009(2) 0.015(2) -0.0030(19) 0.0006(19) 0.003(2) N7 0.011(3) 0.018(3) 0.010(2) -0.0011(19) 0.0016(19) -0.001(2) N8 0.010(3) 0.016(3) 0.011(2) 0.0001(19) 0.003(2) 0.000(2) C1 0.014(4) 0.012(3) 0.019(3) -0.002(2) 0.008(3) 0.000(3) C2 0.014(4) 0.010(3) 0.012(3) 0.002(2) -0.004(2) -0.002(3) C3 0.024(4) 0.023(4) 0.011(3) 0.003(3) 0.003(3) -0.003(3) C4 0.017(4) 0.018(3) 0.019(3) 0.001(3) 0.010(3) 0.004(3) C5 0.010(3) 0.018(3) 0.016(3) 0.002(3) 0.002(2) -0.001(3) C6 0.012(3) 0.023(4) 0.011(3) -0.002(2) 0.000(2) -0.002(3) C7 0.021(4) 0.009(3) 0.027(3) -0.001(3) 0.015(3) 0.005(3) C8 0.018(4) 0.019(3) 0.025(3) -0.013(3) 0.009(3) -0.010(3) C9 0.010(4) 0.030(4) 0.021(3) 0.005(3) -0.005(3) -0.001(3) C10 0.012(3) 0.016(3) 0.018(3) 0.005(2) -0.001(2) 0.004(3) C11 0.017(4) 0.014(3) 0.012(3) -0.001(2) 0.004(3) -0.002(3) C12 0.015(4) 0.018(3) 0.019(3) -0.001(3) 0.000(3) -0.002(3) C13 0.021(4) 0.022(4) 0.013(3) -0.001(3) -0.001(3) -0.009(3) C14 0.026(4) 0.019(3) 0.020(3) -0.003(3) 0.017(3) -0.006(3) C15 0.008(3) 0.014(3) 0.018(3) -0.003(2) -0.001(2) -0.003(2) C16 0.007(3) 0.021(3) 0.014(3) 0.001(2) 0.005(2) 0.004(3) C17 0.008(3) 0.015(3) 0.022(3) -0.002(2) 0.002(2) 0.003(3) C18 0.018(4) 0.030(4) 0.033(4) -0.014(3) 0.011(3) -0.012(3) C19 0.011(4) 0.030(4) 0.020(3) -0.001(3) 0.000(3) -0.001(3) C20 0.013(3) 0.009(3) 0.027(3) 0.000(2) 0.003(3) 0.000(3) C21 0.011(3) 0.016(3) 0.017(3) -0.006(2) 0.002(2) -0.007(3) C22 0.010(3) 0.022(4) 0.017(3) 0.004(3) 0.000(2) 0.007(3) C23 0.019(4) 0.012(3) 0.019(3) 0.008(2) 0.012(3) 0.005(3) C24 0.017(4) 0.011(3) 0.023(3) 0.000(2) 0.008(3) -0.002(3) C25 0.007(3) 0.017(3) 0.017(3) 0.002(2) 0.005(2) 0.002(2) C26 0.012(3) 0.010(3) 0.017(3) 0.002(2) 0.001(2) 0.001(3) C27 0.009(3) 0.010(3) 0.013(3) -0.004(2) -0.001(2) -0.002(2) C28 0.012(3) 0.017(3) 0.009(3) 0.000(2) 0.001(2) 0.010(3) C29 0.012(3) 0.015(3) 0.012(3) 0.003(2) 0.005(2) -0.001(3) C30 0.011(3) 0.005(3) 0.020(3) -0.002(2) 0.000(2) 0.004(3) C31 0.018(4) 0.017(3) 0.017(3) -0.006(2) 0.003(3) -0.001(3) C32 0.016(4) 0.021(4) 0.018(3) -0.003(3) 0.000(3) 0.002(3) C33 0.021(4) 0.018(3) 0.022(3) 0.011(3) 0.012(3) 0.008(3) C34 0.017(4) 0.011(3) 0.023(3) -0.002(2) 0.006(3) -0.005(3) C35 0.014(3) 0.017(3) 0.014(3) 0.002(2) 0.004(2) 0.000(3) C36 0.008(3) 0.014(3) 0.014(3) 0.002(2) 0.001(2) 0.001(2) C37 0.012(3) 0.017(3) 0.014(3) -0.003(2) 0.003(2) -0.004(3) C38 0.015(3) 0.016(3) 0.009(3) -0.003(2) -0.002(2) 0.007(3) C39 0.014(3) 0.018(3) 0.019(3) 0.006(3) 0.007(3) 0.006(3) C40 0.009(3) 0.009(3) 0.016(3) -0.002(2) -0.004(2) 0.001(2) _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 O5 2.271(3) . ? Cd1 O1 2.275(4) . ? Cd1 N2 2.327(4) . ? Cd1 N4 2.334(4) . ? Cd1 N3 2.369(4) . ? Cd1 N1 2.372(4) . ? Cd2 O2 2.307(3) . ? Cd2 O8 2.317(3) 1_455 ? Cd2 N8 2.337(4) . ? Cd2 N6 2.339(4) . ? Cd2 N5 2.377(4) . ? Cd2 N7 2.379(4) . ? S1 O4 1.453(3) . ? S1 O3 1.467(3) . ? S1 O1 1.486(4) . ? S1 O2 1.493(3) . ? S2 O6 1.465(3) . ? S2 O7 1.466(3) . ? S2 O8 1.485(3) . ? S2 O5 1.496(4) . ? O8 Cd2 2.317(3) 1_655 ? N1 C5 1.340(7) . ? N1 C1 1.353(7) . ? N2 C10 1.330(6) . ? N2 C6 1.336(6) . ? N3 C15 1.337(7) . ? N3 C11 1.350(7) . ? N4 C20 1.333(6) . ? N4 C16 1.337(6) . ? N5 C25 1.344(6) . ? N5 C21 1.347(6) . ? N6 C30 1.336(7) . ? N6 C26 1.355(6) . ? N7 C31 1.336(6) . ? N7 C35 1.345(6) . ? N8 C40 1.347(7) . ? N8 C36 1.350(6) . ? C1 C2 1.383(7) . ? C1 H1 0.9500 . ? C2 C3 1.369(8) . ? C2 H2 0.9500 . ? C3 C4 1.380(8) . ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.377(7) . ? C6 H6 0.9500 . ? C7 C8 1.379(7) . ? C7 H7 0.9500 . ? C8 C9 1.365(7) . ? C8 H8 0.9500 . ? C9 C10 1.384(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.386(7) . ? C11 H11 0.9500 . ? C12 C13 1.379(8) . ? C12 H12 0.9500 . ? C13 C14 1.374(8) . ? C13 H13 0.9500 . ? C14 C15 1.378(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(7) . ? C16 H16 0.9500 . ? C17 C18 1.387(7) . ? C17 H17 0.9500 . ? C18 C19 1.370(8) . ? C18 H18 0.9500 . ? C19 C20 1.382(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.375(7) . ? C21 H21 0.9500 . ? C22 C23 1.377(7) . ? C22 H22 0.9500 . ? C23 C24 1.385(7) . ? C23 H23 0.9500 . ? C24 C25 1.369(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.365(7) . ? C26 H26 0.9500 . ? C27 C28 1.381(7) . ? C27 H27 0.9500 . ? C28 C29 1.373(7) . ? C28 H28 0.9500 . ? C29 C30 1.376(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.387(7) . ? C31 H31 0.9500 . ? C32 C33 1.386(7) . ? C32 H32 0.9500 . ? C33 C34 1.382(7) . ? C33 H33 0.9500 . ? C34 C35 1.386(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.367(7) . ? C36 H36 0.9500 . ? C37 C38 1.395(7) . ? C37 H37 0.9500 . ? C38 C39 1.385(7) . ? C38 H38 0.9500 . ? C39 C40 1.378(7) . ? C39 H39 0.9500 . ? C40 H40 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 Cd1 O1 179.99(17) . . ? O5 Cd1 N2 82.52(13) . . ? O1 Cd1 N2 97.49(14) . . ? O5 Cd1 N4 97.01(14) . . ? O1 Cd1 N4 82.98(13) . . ? N2 Cd1 N4 179.01(16) . . ? O5 Cd1 N3 91.93(14) . . ? O1 Cd1 N3 88.07(14) . . ? N2 Cd1 N3 90.64(15) . . ? N4 Cd1 N3 90.24(15) . . ? O5 Cd1 N1 90.54(14) . . ? O1 Cd1 N1 89.47(14) . . ? N2 Cd1 N1 91.23(15) . . ? N4 Cd1 N1 87.91(15) . . ? N3 Cd1 N1 177.08(17) . . ? O2 Cd2 O8 177.58(12) . 1_455 ? O2 Cd2 N8 93.63(14) . . ? O8 Cd2 N8 88.71(14) 1_455 . ? O2 Cd2 N6 86.59(14) . . ? O8 Cd2 N6 91.06(13) 1_455 . ? N8 Cd2 N6 179.27(17) . . ? O2 Cd2 N5 84.48(14) . . ? O8 Cd2 N5 94.73(14) 1_455 . ? N8 Cd2 N5 94.62(15) . . ? N6 Cd2 N5 84.71(14) . . ? O2 Cd2 N7 95.54(14) . . ? O8 Cd2 N7 85.22(14) 1_455 . ? N8 Cd2 N7 86.07(15) . . ? N6 Cd2 N7 94.60(14) . . ? N5 Cd2 N7 179.31(15) . . ? O4 S1 O3 111.3(2) . . ? O4 S1 O1 108.9(2) . . ? O3 S1 O1 109.1(2) . . ? O4 S1 O2 109.7(2) . . ? O3 S1 O2 109.9(2) . . ? O1 S1 O2 107.9(2) . . ? O6 S2 O7 111.5(2) . . ? O6 S2 O8 110.0(2) . . ? O7 S2 O8 110.4(2) . . ? O6 S2 O5 108.3(2) . . ? O7 S2 O5 109.0(2) . . ? O8 S2 O5 107.5(2) . . ? S1 O1 Cd1 146.8(2) . . ? S1 O2 Cd2 137.8(2) . . ? S2 O5 Cd1 146.4(2) . . ? S2 O8 Cd2 139.7(2) . 1_655 ? C5 N1 C1 117.9(5) . . ? C5 N1 Cd1 119.2(4) . . ? C1 N1 Cd1 122.3(4) . . ? C10 N2 C6 116.9(5) . . ? C10 N2 Cd1 124.5(4) . . ? C6 N2 Cd1 118.2(3) . . ? C15 N3 C11 117.9(5) . . ? C15 N3 Cd1 118.6(4) . . ? C11 N3 Cd1 123.4(4) . . ? C20 N4 C16 117.2(5) . . ? C20 N4 Cd1 124.0(4) . . ? C16 N4 Cd1 117.9(4) . . ? C25 N5 C21 116.3(5) . . ? C25 N5 Cd2 125.9(4) . . ? C21 N5 Cd2 117.8(3) . . ? C30 N6 C26 117.4(5) . . ? C30 N6 Cd2 119.8(4) . . ? C26 N6 Cd2 122.8(4) . . ? C31 N7 C35 116.8(5) . . ? C31 N7 Cd2 118.6(4) . . ? C35 N7 Cd2 124.5(4) . . ? C40 N8 C36 117.7(5) . . ? C40 N8 Cd2 120.3(4) . . ? C36 N8 Cd2 122.0(4) . . ? N1 C1 C2 121.7(5) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.8(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.4(6) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.0(6) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 123.7(5) . . ? N2 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C6 C7 C8 118.0(5) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.3(5) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 123.6(5) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N3 C11 C12 122.5(5) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 118.7(6) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C12 118.9(5) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.6(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 122.4(6) . . ? N3 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N4 C16 C17 123.6(5) . . ? N4 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C18 C17 C16 117.6(5) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C19 C18 C17 119.5(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 118.6(6) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N4 C20 C19 123.4(5) . . ? N4 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? N5 C21 C22 123.3(5) . . ? N5 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 118.1(5) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 119.0(5) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N5 C25 C24 123.9(5) . . ? N5 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? N6 C26 C27 122.2(5) . . ? N6 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C28 120.1(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 117.8(5) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? C28 C29 C30 119.6(5) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? N6 C30 C29 122.9(5) . . ? N6 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N7 C31 C32 124.1(5) . . ? N7 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C33 C32 C31 118.2(5) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N7 C35 C34 123.2(5) . . ? N7 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N8 C36 C37 123.0(5) . . ? N8 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C36 C37 C38 118.8(5) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 118.9(5) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C40 C39 C38 118.7(5) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? N8 C40 C39 122.9(5) . . ? N8 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Cd1 143.6(3) . . . . ? O3 S1 O1 Cd1 -94.8(4) . . . . ? O2 S1 O1 Cd1 24.6(4) . . . . ? O5 Cd1 O1 S1 153(100) . . . . ? N2 Cd1 O1 S1 4.8(4) . . . . ? N4 Cd1 O1 S1 -174.3(4) . . . . ? N3 Cd1 O1 S1 95.2(4) . . . . ? N1 Cd1 O1 S1 -86.4(4) . . . . ? O4 S1 O2 Cd2 72.5(3) . . . . ? O3 S1 O2 Cd2 -50.1(3) . . . . ? O1 S1 O2 Cd2 -169.0(3) . . . . ? O8 Cd2 O2 S1 -110(3) 1_455 . . . ? N8 Cd2 O2 S1 84.5(3) . . . . ? N6 Cd2 O2 S1 -96.1(3) . . . . ? N5 Cd2 O2 S1 178.8(3) . . . . ? N7 Cd2 O2 S1 -1.8(3) . . . . ? O6 S2 O5 Cd1 -149.3(3) . . . . ? O7 S2 O5 Cd1 89.1(4) . . . . ? O8 S2 O5 Cd1 -30.5(4) . . . . ? O1 Cd1 O5 S2 34(100) . . . . ? N2 Cd1 O5 S2 -177.8(4) . . . . ? N4 Cd1 O5 S2 1.3(4) . . . . ? N3 Cd1 O5 S2 91.8(4) . . . . ? N1 Cd1 O5 S2 -86.7(4) . . . . ? O6 S2 O8 Cd2 -65.4(3) . . . 1_655 ? O7 S2 O8 Cd2 58.1(3) . . . 1_655 ? O5 S2 O8 Cd2 176.9(3) . . . 1_655 ? O5 Cd1 N1 C5 -171.5(4) . . . . ? O1 Cd1 N1 C5 8.5(4) . . . . ? N2 Cd1 N1 C5 -89.0(4) . . . . ? N4 Cd1 N1 C5 91.5(4) . . . . ? N3 Cd1 N1 C5 41(4) . . . . ? O5 Cd1 N1 C1 17.6(4) . . . . ? O1 Cd1 N1 C1 -162.4(4) . . . . ? N2 Cd1 N1 C1 100.1(4) . . . . ? N4 Cd1 N1 C1 -79.4(4) . . . . ? N3 Cd1 N1 C1 -130(3) . . . . ? O5 Cd1 N2 C10 -126.1(4) . . . . ? O1 Cd1 N2 C10 53.9(4) . . . . ? N4 Cd1 N2 C10 173(41) . . . . ? N3 Cd1 N2 C10 -34.3(4) . . . . ? N1 Cd1 N2 C10 143.5(4) . . . . ? O5 Cd1 N2 C6 45.4(4) . . . . ? O1 Cd1 N2 C6 -134.6(4) . . . . ? N4 Cd1 N2 C6 -16(9) . . . . ? N3 Cd1 N2 C6 137.2(4) . . . . ? N1 Cd1 N2 C6 -45.0(4) . . . . ? O5 Cd1 N3 C15 -11.0(4) . . . . ? O1 Cd1 N3 C15 169.0(4) . . . . ? N2 Cd1 N3 C15 -93.5(4) . . . . ? N4 Cd1 N3 C15 86.1(4) . . . . ? N1 Cd1 N3 C15 137(3) . . . . ? O5 Cd1 N3 C11 166.3(4) . . . . ? O1 Cd1 N3 C11 -13.7(4) . . . . ? N2 Cd1 N3 C11 83.8(4) . . . . ? N4 Cd1 N3 C11 -96.7(4) . . . . ? N1 Cd1 N3 C11 -46(4) . . . . ? O5 Cd1 N4 C20 -51.8(4) . . . . ? O1 Cd1 N4 C20 128.2(4) . . . . ? N2 Cd1 N4 C20 9(9) . . . . ? N3 Cd1 N4 C20 -143.8(4) . . . . ? N1 Cd1 N4 C20 38.5(4) . . . . ? O5 Cd1 N4 C16 139.5(4) . . . . ? O1 Cd1 N4 C16 -40.5(4) . . . . ? N2 Cd1 N4 C16 -159(9) . . . . ? N3 Cd1 N4 C16 47.5(4) . . . . ? N1 Cd1 N4 C16 -130.2(4) . . . . ? O2 Cd2 N5 C25 -138.7(4) . . . . ? O8 Cd2 N5 C25 43.6(4) 1_455 . . . ? N8 Cd2 N5 C25 -45.5(4) . . . . ? N6 Cd2 N5 C25 134.2(4) . . . . ? N7 Cd2 N5 C25 130(14) . . . . ? O2 Cd2 N5 C21 40.7(4) . . . . ? O8 Cd2 N5 C21 -137.0(4) 1_455 . . . ? N8 Cd2 N5 C21 134.0(4) . . . . ? N6 Cd2 N5 C21 -46.3(4) . . . . ? N7 Cd2 N5 C21 -51(14) . . . . ? O2 Cd2 N6 C30 -151.5(4) . . . . ? O8 Cd2 N6 C30 27.9(4) 1_455 . . . ? N8 Cd2 N6 C30 -44(13) . . . . ? N5 Cd2 N6 C30 -66.8(4) . . . . ? N7 Cd2 N6 C30 113.2(4) . . . . ? O2 Cd2 N6 C26 27.6(4) . . . . ? O8 Cd2 N6 C26 -153.0(4) 1_455 . . . ? N8 Cd2 N6 C26 135(13) . . . . ? N5 Cd2 N6 C26 112.4(4) . . . . ? N7 Cd2 N6 C26 -67.7(4) . . . . ? O2 Cd2 N7 C31 137.6(4) . . . . ? O8 Cd2 N7 C31 -44.7(4) 1_455 . . . ? N8 Cd2 N7 C31 44.4(4) . . . . ? N6 Cd2 N7 C31 -135.3(4) . . . . ? N5 Cd2 N7 C31 -131(14) . . . . ? O2 Cd2 N7 C35 -46.3(4) . . . . ? O8 Cd2 N7 C35 131.4(4) 1_455 . . . ? N8 Cd2 N7 C35 -139.6(4) . . . . ? N6 Cd2 N7 C35 40.7(4) . . . . ? N5 Cd2 N7 C35 45(15) . . . . ? O2 Cd2 N8 C40 -28.5(4) . . . . ? O8 Cd2 N8 C40 152.1(4) 1_455 . . . ? N6 Cd2 N8 C40 -136(13) . . . . ? N5 Cd2 N8 C40 -113.2(4) . . . . ? N7 Cd2 N8 C40 66.8(4) . . . . ? O2 Cd2 N8 C36 152.1(4) . . . . ? O8 Cd2 N8 C36 -27.3(4) 1_455 . . . ? N6 Cd2 N8 C36 45(13) . . . . ? N5 Cd2 N8 C36 67.4(4) . . . . ? N7 Cd2 N8 C36 -112.6(4) . . . . ? C5 N1 C1 C2 0.7(8) . . . . ? Cd1 N1 C1 C2 171.7(4) . . . . ? N1 C1 C2 C3 -0.1(8) . . . . ? C1 C2 C3 C4 0.7(8) . . . . ? C2 C3 C4 C5 -1.9(9) . . . . ? C1 N1 C5 C4 -2.0(8) . . . . ? Cd1 N1 C5 C4 -173.3(4) . . . . ? C3 C4 C5 N1 2.6(9) . . . . ? C10 N2 C6 C7 -1.2(8) . . . . ? Cd1 N2 C6 C7 -173.3(4) . . . . ? N2 C6 C7 C8 1.1(8) . . . . ? C6 C7 C8 C9 -0.6(8) . . . . ? C7 C8 C9 C10 0.4(9) . . . . ? C6 N2 C10 C9 0.9(8) . . . . ? Cd1 N2 C10 C9 172.5(4) . . . . ? C8 C9 C10 N2 -0.6(9) . . . . ? C15 N3 C11 C12 1.0(8) . . . . ? Cd1 N3 C11 C12 -176.3(4) . . . . ? N3 C11 C12 C13 -0.4(8) . . . . ? C11 C12 C13 C14 0.1(8) . . . . ? C12 C13 C14 C15 -0.4(9) . . . . ? C11 N3 C15 C14 -1.2(8) . . . . ? Cd1 N3 C15 C14 176.2(4) . . . . ? C13 C14 C15 N3 1.0(9) . . . . ? C20 N4 C16 C17 -0.4(8) . . . . ? Cd1 N4 C16 C17 169.0(4) . . . . ? N4 C16 C17 C18 -0.3(8) . . . . ? C16 C17 C18 C19 0.2(8) . . . . ? C17 C18 C19 C20 0.6(9) . . . . ? C16 N4 C20 C19 1.3(8) . . . . ? Cd1 N4 C20 C19 -167.4(4) . . . . ? C18 C19 C20 N4 -1.4(9) . . . . ? C25 N5 C21 C22 -0.2(8) . . . . ? Cd2 N5 C21 C22 -179.7(4) . . . . ? N5 C21 C22 C23 0.5(9) . . . . ? C21 C22 C23 C24 0.4(8) . . . . ? C22 C23 C24 C25 -1.6(8) . . . . ? C21 N5 C25 C24 -1.0(8) . . . . ? Cd2 N5 C25 C24 178.4(4) . . . . ? C23 C24 C25 N5 1.9(8) . . . . ? C30 N6 C26 C27 -0.8(8) . . . . ? Cd2 N6 C26 C27 -180.0(4) . . . . ? N6 C26 C27 C28 -0.4(8) . . . . ? C26 C27 C28 C29 1.8(8) . . . . ? C27 C28 C29 C30 -1.9(8) . . . . ? C26 N6 C30 C29 0.7(8) . . . . ? Cd2 N6 C30 C29 179.9(4) . . . . ? C28 C29 C30 N6 0.7(9) . . . . ? C35 N7 C31 C32 0.1(8) . . . . ? Cd2 N7 C31 C32 176.4(4) . . . . ? N7 C31 C32 C33 -1.5(9) . . . . ? C31 C32 C33 C34 1.0(8) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C31 N7 C35 C34 1.9(8) . . . . ? Cd2 N7 C35 C34 -174.2(4) . . . . ? C33 C34 C35 N7 -2.4(8) . . . . ? C40 N8 C36 C37 1.5(8) . . . . ? Cd2 N8 C36 C37 -179.1(4) . . . . ? N8 C36 C37 C38 1.3(8) . . . . ? C36 C37 C38 C39 -2.4(8) . . . . ? C37 C38 C39 C40 0.7(8) . . . . ? C36 N8 C40 C39 -3.3(8) . . . . ? Cd2 N8 C40 C39 177.3(4) . . . . ? C38 C39 C40 N8 2.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.940 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.113 # Attachment 'Compound10.cif' data_s2126abs _database_code_depnum_ccdc_archive 'CCDC 285989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the Cd monomer with two water molecules; the monomer grows into a polymeric structure by space group symmetry. H atoms bonded to water were included in difference map positions, and refined isotropically; those bonded to C were included in calculated positions. Non H atoms were refined anisotropically. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cd N3 O7 S' _chemical_formula_weight 499.81 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.8209(9) _cell_length_b 9.4590(7) _cell_length_c 16.8494(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.9770(10) _cell_angle_gamma 90.00 _cell_volume 1932.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6573 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7838 _exptl_absorpt_correction_T_max 0.8827 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14934 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3915 _reflns_number_gt 3433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+1.5275P] 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 3915 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.5000 0.5000 0.0000 0.01132(6) Uani 1 2 d S . . Cd2 Cd 1.0000 0.5000 0.0000 0.01079(6) Uani 1 2 d S . . S1 S 0.75830(4) 0.36052(5) 0.02893(3) 0.01081(10) Uani 1 1 d . . . O1 O 0.67933(10) 0.43310(14) 0.06406(8) 0.0157(3) Uani 1 1 d . . . O2 O 0.85349(11) 0.45580(16) 0.04359(9) 0.0196(3) Uani 1 1 d . . . O3 O 0.70579(11) 0.33620(14) -0.06104(8) 0.0169(3) Uani 1 1 d . . . O4 O 0.79377(12) 0.22723(14) 0.07341(8) 0.0212(3) Uani 1 1 d . . . O5 O 0.49589(13) 0.55248(16) 0.13420(9) 0.0185(3) Uani 1 1 d . . . N1 N 0.44517(13) 0.27451(17) 0.02005(10) 0.0157(3) Uani 1 1 d . . . N2 N 1.11231(13) 0.38889(16) 0.11996(10) 0.0151(3) Uani 1 1 d . . . N3 N 1.00257(12) 0.71574(16) 0.07563(10) 0.0145(3) Uani 1 1 d . . . C1 C 0.35086(16) 0.2176(2) -0.03031(12) 0.0180(4) Uani 1 1 d . . . H1 H 0.3059 0.2721 -0.0760 0.022 Uiso 1 1 calc R . . C2 C 0.31651(17) 0.0834(2) -0.01852(13) 0.0208(4) Uani 1 1 d . . . H2 H 0.2496 0.0462 -0.0557 0.025 Uiso 1 1 calc R . . C3 C 0.38117(19) 0.0035(2) 0.04848(14) 0.0212(5) Uani 1 1 d . . . H3 H 0.3593 -0.0891 0.0581 0.025 Uiso 1 1 calc R . . C4 C 0.47813(17) 0.0614(2) 0.10095(13) 0.0199(4) Uani 1 1 d . . . H4 H 0.5237 0.0094 0.1476 0.024 Uiso 1 1 calc R . . C5 C 0.50784(16) 0.1962(2) 0.08455(12) 0.0176(4) Uani 1 1 d . . . H5 H 0.5751 0.2349 0.1203 0.021 Uiso 1 1 calc R . . C6 C 1.07986(16) 0.3700(2) 0.18748(12) 0.0178(4) Uani 1 1 d . . . H6 H 1.0118 0.4099 0.1873 0.021 Uiso 1 1 calc R . . C7 C 1.14176(18) 0.2948(2) 0.25698(13) 0.0217(4) Uani 1 1 d . . . H7 H 1.1174 0.2854 0.3043 0.026 Uiso 1 1 calc R . . C8 C 1.23934(17) 0.2335(2) 0.25706(13) 0.0243(5) Uani 1 1 d . . . H8 H 1.2821 0.1789 0.3036 0.029 Uiso 1 1 calc R . . C9 C 1.27359(17) 0.2530(2) 0.18818(13) 0.0240(5) Uani 1 1 d . . . H9 H 1.3409 0.2129 0.1867 0.029 Uiso 1 1 calc R . . C10 C 1.20845(16) 0.3319(2) 0.12135(13) 0.0199(4) Uani 1 1 d . . . H10 H 1.2329 0.3462 0.0745 0.024 Uiso 1 1 calc R . . C11 C 0.95225(16) 0.7245(2) 0.13449(12) 0.0166(4) Uani 1 1 d . . . H11 H 0.9139 0.6442 0.1446 0.020 Uiso 1 1 calc R . . C12 C 0.95449(17) 0.8462(2) 0.18053(13) 0.0219(4) Uani 1 1 d . . . H12 H 0.9186 0.8488 0.2217 0.026 Uiso 1 1 calc R . . C13 C 1.00943(18) 0.9635(2) 0.16595(13) 0.0231(5) Uani 1 1 d . . . H13 H 1.0116 1.0485 0.1966 0.028 Uiso 1 1 calc R . . C14 C 1.06105(17) 0.9550(2) 0.10602(13) 0.0215(4) Uani 1 1 d . . . H14 H 1.1000 1.0339 0.0950 0.026 Uiso 1 1 calc R . . C15 C 1.05540(16) 0.8301(2) 0.06214(12) 0.0172(4) Uani 1 1 d . . . H15 H 1.0907 0.8255 0.0206 0.021 Uiso 1 1 calc R . . O2S O 0.70855(15) 0.00067(17) 0.26927(11) 0.0284(4) Uani 1 1 d . . . O1S O 0.84866(13) 0.21573(18) 0.24412(10) 0.0241(3) Uani 1 1 d . . . H1O H 0.540(2) 0.606(3) 0.1677(17) 0.037(8) Uiso 1 1 d . . . H4O H 0.835(2) 0.304(3) 0.2545(17) 0.042(8) Uiso 1 1 d . . . H5O H 0.743(2) 0.064(3) 0.2550(19) 0.049(9) Uiso 1 1 d . . . H6O H 0.748(3) -0.017(3) 0.321(2) 0.049(9) Uiso 1 1 d . . . H3O H 0.844(2) 0.217(3) 0.195(2) 0.043(8) Uiso 1 1 d . . . H2O H 0.433(2) 0.592(3) 0.1205(16) 0.033(7) Uiso 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 0.01004(10) 0.01141(11) 0.01199(11) -0.00034(7) 0.00286(8) -0.00104(7) Cd2 0.01095(10) 0.01084(11) 0.01028(11) -0.00001(6) 0.00303(8) -0.00107(7) S1 0.0098(2) 0.0109(2) 0.0115(2) -0.00075(17) 0.00322(16) -0.00100(17) O1 0.0124(6) 0.0209(7) 0.0135(7) -0.0028(5) 0.0038(5) 0.0014(6) O2 0.0163(7) 0.0246(8) 0.0202(7) -0.0047(6) 0.0090(6) -0.0087(6) O3 0.0167(7) 0.0198(7) 0.0127(7) -0.0023(5) 0.0029(5) 0.0006(6) O4 0.0298(8) 0.0147(7) 0.0178(7) 0.0012(6) 0.0057(6) 0.0038(6) O5 0.0165(7) 0.0222(8) 0.0152(7) -0.0032(6) 0.0028(6) 0.0015(7) N1 0.0153(8) 0.0144(8) 0.0170(8) -0.0005(6) 0.0049(7) -0.0008(7) N2 0.0171(8) 0.0134(8) 0.0136(8) -0.0006(6) 0.0034(6) -0.0009(6) N3 0.0124(8) 0.0147(8) 0.0145(8) 0.0002(6) 0.0017(6) 0.0017(6) C1 0.0179(10) 0.0175(10) 0.0166(10) 0.0010(8) 0.0027(8) -0.0009(8) C2 0.0193(10) 0.0183(10) 0.0222(11) -0.0026(8) 0.0032(8) -0.0065(8) C3 0.0284(12) 0.0120(10) 0.0244(12) -0.0016(8) 0.0103(10) -0.0048(8) C4 0.0227(10) 0.0176(10) 0.0193(10) 0.0033(8) 0.0067(8) 0.0027(8) C5 0.0155(9) 0.0193(10) 0.0164(10) -0.0003(8) 0.0028(8) -0.0008(8) C6 0.0194(10) 0.0179(10) 0.0162(10) 0.0002(8) 0.0058(8) -0.0005(8) C7 0.0272(11) 0.0212(11) 0.0154(10) 0.0019(8) 0.0050(9) -0.0044(9) C8 0.0264(11) 0.0191(11) 0.0181(11) 0.0024(8) -0.0054(9) -0.0011(9) C9 0.0160(10) 0.0248(11) 0.0264(12) -0.0026(9) 0.0002(9) 0.0042(9) C10 0.0186(10) 0.0209(10) 0.0195(10) -0.0015(8) 0.0051(8) -0.0002(8) C11 0.0158(9) 0.0166(10) 0.0167(10) 0.0002(8) 0.0044(8) 0.0000(8) C12 0.0243(10) 0.0253(11) 0.0163(10) -0.0022(8) 0.0067(8) 0.0051(9) C13 0.0285(12) 0.0154(10) 0.0215(11) -0.0063(8) 0.0030(9) 0.0021(9) C14 0.0241(11) 0.0134(9) 0.0250(11) 0.0006(8) 0.0050(9) -0.0017(9) C15 0.0171(9) 0.0173(10) 0.0173(10) 0.0021(8) 0.0057(8) 0.0030(8) O2S 0.0303(9) 0.0314(10) 0.0170(9) 0.0064(6) -0.0015(7) -0.0105(7) O1S 0.0283(8) 0.0248(9) 0.0178(8) 0.0055(6) 0.0055(7) 0.0026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.2886(13) . ? Cd1 O1 2.2887(13) 3_665 ? Cd1 N1 2.3048(16) . ? Cd1 N1 2.3048(16) 3_665 ? Cd1 O5 2.3323(14) . ? Cd1 O5 2.3323(14) 3_665 ? Cd2 O2 2.2671(13) 3_765 ? Cd2 O2 2.2672(13) . ? Cd2 N2 2.3174(15) . ? Cd2 N2 2.3174(15) 3_765 ? Cd2 N3 2.4005(16) 3_765 ? Cd2 N3 2.4005(16) . ? S1 O4 1.4617(14) . ? S1 O3 1.4630(13) . ? S1 O2 1.4720(14) . ? S1 O1 1.4954(13) . ? O5 H1O 0.83(3) . ? O5 H2O 0.85(3) . ? N1 C1 1.343(2) . ? N1 C5 1.345(2) . ? N2 C10 1.339(3) . ? N2 C6 1.344(2) . ? N3 C15 1.334(2) . ? N3 C11 1.350(2) . ? C1 C2 1.379(3) . ? C1 H1 0.9500 . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.379(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 C9 1.380(3) . ? C8 H8 0.9500 . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? O2S H5O 0.83(3) . ? O2S H6O 0.87(3) . ? O1S H4O 0.88(3) . ? O1S H3O 0.82(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 180.00(3) . 3_665 ? O1 Cd1 N1 89.00(5) . . ? O1 Cd1 N1 91.00(5) 3_665 . ? O1 Cd1 N1 91.00(5) . 3_665 ? O1 Cd1 N1 89.00(5) 3_665 3_665 ? N1 Cd1 N1 180.0 . 3_665 ? O1 Cd1 O5 86.42(5) . . ? O1 Cd1 O5 93.58(5) 3_665 . ? N1 Cd1 O5 87.18(5) . . ? N1 Cd1 O5 92.82(5) 3_665 . ? O1 Cd1 O5 93.58(5) . 3_665 ? O1 Cd1 O5 86.42(5) 3_665 3_665 ? N1 Cd1 O5 92.82(5) . 3_665 ? N1 Cd1 O5 87.17(5) 3_665 3_665 ? O5 Cd1 O5 180.0 . 3_665 ? O2 Cd2 O2 180.0 3_765 . ? O2 Cd2 N2 91.20(5) 3_765 . ? O2 Cd2 N2 88.80(5) . . ? O2 Cd2 N2 88.80(5) 3_765 3_765 ? O2 Cd2 N2 91.20(5) . 3_765 ? N2 Cd2 N2 179.999(2) . 3_765 ? O2 Cd2 N3 81.64(5) 3_765 3_765 ? O2 Cd2 N3 98.36(5) . 3_765 ? N2 Cd2 N3 88.56(5) . 3_765 ? N2 Cd2 N3 91.44(5) 3_765 3_765 ? O2 Cd2 N3 98.37(5) 3_765 . ? O2 Cd2 N3 81.63(5) . . ? N2 Cd2 N3 91.44(5) . . ? N2 Cd2 N3 88.56(5) 3_765 . ? N3 Cd2 N3 180.00(7) 3_765 . ? O4 S1 O3 110.93(8) . . ? O4 S1 O2 109.84(9) . . ? O3 S1 O2 110.32(8) . . ? O4 S1 O1 109.32(8) . . ? O3 S1 O1 109.86(8) . . ? O2 S1 O1 106.47(8) . . ? S1 O1 Cd1 130.23(7) . . ? S1 O2 Cd2 141.96(9) . . ? Cd1 O5 H1O 124.4(18) . . ? Cd1 O5 H2O 98.5(17) . . ? H1O O5 H2O 107(2) . . ? C1 N1 C5 117.92(17) . . ? C1 N1 Cd1 122.22(13) . . ? C5 N1 Cd1 119.85(13) . . ? C10 N2 C6 117.91(17) . . ? C10 N2 Cd2 120.36(13) . . ? C6 N2 Cd2 121.53(13) . . ? C15 N3 C11 117.74(17) . . ? C15 N3 Cd2 121.24(12) . . ? C11 N3 Cd2 121.00(12) . . ? N1 C1 C2 122.82(18) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.96(18) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.68(18) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.06(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.55(18) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 122.42(19) . . ? N2 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 119.29(19) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 118.65(19) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C10 118.95(19) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.74(19) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 122.40(18) . . ? N3 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 119.25(19) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 118.55(19) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.20(19) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 122.85(18) . . ? N3 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? H5O O2S H6O 104(3) . . ? H4O O1S H3O 103(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 -120.34(10) . . . . ? O3 S1 O1 Cd1 1.60(13) . . . . ? O2 S1 O1 Cd1 121.06(10) . . . . ? O1 Cd1 O1 S1 55(24) 3_665 . . . ? N1 Cd1 O1 S1 84.17(11) . . . . ? N1 Cd1 O1 S1 -95.83(11) 3_665 . . . ? O5 Cd1 O1 S1 171.40(11) . . . . ? O5 Cd1 O1 S1 -8.60(11) 3_665 . . . ? O4 S1 O2 Cd2 80.61(15) . . . . ? O3 S1 O2 Cd2 -41.97(17) . . . . ? O1 S1 O2 Cd2 -161.13(13) . . . . ? O2 Cd2 O2 S1 79(3) 3_765 . . . ? N2 Cd2 O2 S1 -102.31(15) . . . . ? N2 Cd2 O2 S1 77.69(15) 3_765 . . . ? N3 Cd2 O2 S1 -13.94(15) 3_765 . . . ? N3 Cd2 O2 S1 166.06(15) . . . . ? O1 Cd1 N1 C1 -153.38(15) . . . . ? O1 Cd1 N1 C1 26.62(15) 3_665 . . . ? N1 Cd1 N1 C1 -52(4) 3_665 . . . ? O5 Cd1 N1 C1 120.15(15) . . . . ? O5 Cd1 N1 C1 -59.85(15) 3_665 . . . ? O1 Cd1 N1 C5 27.46(14) . . . . ? O1 Cd1 N1 C5 -152.55(14) 3_665 . . . ? N1 Cd1 N1 C5 129(4) 3_665 . . . ? O5 Cd1 N1 C5 -59.01(14) . . . . ? O5 Cd1 N1 C5 120.99(14) 3_665 . . . ? O2 Cd2 N2 C10 -24.37(15) 3_765 . . . ? O2 Cd2 N2 C10 155.63(15) . . . . ? N2 Cd2 N2 C10 -20(4) 3_765 . . . ? N3 Cd2 N2 C10 57.23(15) 3_765 . . . ? N3 Cd2 N2 C10 -122.77(15) . . . . ? O2 Cd2 N2 C6 160.80(14) 3_765 . . . ? O2 Cd2 N2 C6 -19.20(14) . . . . ? N2 Cd2 N2 C6 165(4) 3_765 . . . ? N3 Cd2 N2 C6 -117.60(15) 3_765 . . . ? N3 Cd2 N2 C6 62.40(15) . . . . ? O2 Cd2 N3 C15 18.93(15) 3_765 . . . ? O2 Cd2 N3 C15 -161.07(15) . . . . ? N2 Cd2 N3 C15 110.36(14) . . . . ? N2 Cd2 N3 C15 -69.64(14) 3_765 . . . ? N3 Cd2 N3 C15 136(37) 3_765 . . . ? O2 Cd2 N3 C11 -159.80(14) 3_765 . . . ? O2 Cd2 N3 C11 20.21(14) . . . . ? N2 Cd2 N3 C11 -68.37(14) . . . . ? N2 Cd2 N3 C11 111.63(14) 3_765 . . . ? N3 Cd2 N3 C11 -43(37) 3_765 . . . ? C5 N1 C1 C2 -0.1(3) . . . . ? Cd1 N1 C1 C2 -179.32(15) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C1 N1 C5 C4 -0.7(3) . . . . ? Cd1 N1 C5 C4 178.53(15) . . . . ? C3 C4 C5 N1 1.0(3) . . . . ? C10 N2 C6 C7 0.0(3) . . . . ? Cd2 N2 C6 C7 174.97(15) . . . . ? N2 C6 C7 C8 -1.6(3) . . . . ? C6 C7 C8 C9 1.9(3) . . . . ? C7 C8 C9 C10 -0.7(3) . . . . ? C6 N2 C10 C9 1.3(3) . . . . ? Cd2 N2 C10 C9 -173.74(15) . . . . ? C8 C9 C10 N2 -0.9(3) . . . . ? C15 N3 C11 C12 -0.4(3) . . . . ? Cd2 N3 C11 C12 178.41(14) . . . . ? N3 C11 C12 C13 0.3(3) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C11 N3 C15 C14 0.5(3) . . . . ? Cd2 N3 C15 C14 -178.28(14) . . . . ? C13 C14 C15 N3 -0.6(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 O5 H2O S1 0.85(3) 2.92(3) 3.6093(16) 139(2) 3_665 O5 H2O O3 0.85(3) 1.86(3) 2.691(2) 164(2) 3_665 O1S H3O S1 0.82(3) 2.97(3) 3.6922(16) 148(2) . O1S H3O O4 0.82(3) 1.93(3) 2.732(2) 166(3) . O2S H6O S1 0.87(3) 2.81(3) 3.5440(18) 143(3) 2_645 O2S H6O O1 0.87(3) 1.91(3) 2.781(2) 174(3) 2_645 O2S H5O O1S 0.83(3) 2.02(3) 2.835(2) 169(3) . O1S H4O O2S 0.88(3) 1.95(3) 2.783(2) 158(3) 2_655 O5 H1O O1S 0.83(3) 1.99(3) 2.811(2) 174(3) 2_655 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.355 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.068