# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jan Cvengros' _publ_contact_author_email cvengros@inorg.chem.ethz.ch _publ_section_title ; Synthesis and characterization of novel S,N and Se,N homodimetallic Ag(I)-complexes ; loop_ _publ_author_name J.Cvengros E.Mannel N.Santschi # Attachment '- 2c.cif' data_JC142 _database_code_depnum_ccdc_archive 'CCDC 865869' #TrackingRef '- 2c.cif' # This structure was measured, # solved and refined by: # Elli Maennel _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 N2 Se2' _chemical_formula_sum 'C29 H26 N2 Se2' _chemical_formula_weight 560.44 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.42720(10) _cell_length_b 10.0394(2) _cell_length_c 13.2179(2) _cell_angle_alpha 81.9990(10) _cell_angle_beta 83.0590(10) _cell_angle_gamma 79.7370(10) _cell_volume 1213.05(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5613 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.56 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 3.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5804 _exptl_absorpt_correction_T_max 0.8093 _exptl_absorpt_process_details SADABS-2004/1 _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 15184 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 29.13 _reflns_number_total 6444 _reflns_number_gt 5178 _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^)+(0.0269P)^2^+0.5139P] 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 none _refine_ls_number_reflns 6444 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Se1 Se 0.134597(19) 0.060369(19) 0.370466(15) 0.01758(5) Uani 1 1 d . . . Se2 Se 0.99351(2) -0.20806(2) 0.224891(15) 0.01995(6) Uani 1 1 d . . . N1 N 0.69507(16) -0.15682(16) 0.33720(11) 0.0140(3) Uani 1 1 d . . . N2 N 0.43163(16) -0.10378(15) 0.36269(12) 0.0139(3) Uani 1 1 d . . . C1 C 0.44095(19) 0.03866(18) 0.35276(13) 0.0127(3) Uani 1 1 d . . . C2 C 0.31221(19) 0.13413(19) 0.35260(14) 0.0139(4) Uani 1 1 d . . . C3 C 0.3182(2) 0.27252(19) 0.34208(14) 0.0147(4) Uani 1 1 d . . . H3 H 0.2311 0.3366 0.3395 0.018 Uiso 1 1 calc R . . C4 C 0.4510(2) 0.31898(19) 0.33517(14) 0.0152(4) Uani 1 1 d . . . C5 C 0.5770(2) 0.22374(19) 0.33927(14) 0.0154(4) Uani 1 1 d . . . H5 H 0.6673 0.2542 0.3371 0.018 Uiso 1 1 calc R . . C6 C 0.57412(19) 0.08408(19) 0.34656(14) 0.0141(4) Uani 1 1 d . . . C7 C 0.4543(2) 0.4698(2) 0.32464(17) 0.0239(4) Uani 1 1 d . . . H7A H 0.4468 0.4993 0.3930 0.036 Uiso 1 1 calc R . . H7B H 0.3728 0.5194 0.2880 0.036 Uiso 1 1 calc R . . H7C H 0.5456 0.4887 0.2861 0.036 Uiso 1 1 calc R . . C8 C 0.0048(2) 0.2307(2) 0.37084(16) 0.0186(4) Uani 1 1 d . . . C9 C -0.0400(2) 0.2837(2) 0.46288(19) 0.0282(5) Uani 1 1 d . . . H9 H -0.0136 0.2327 0.5259 0.034 Uiso 1 1 calc R . . C10 C -0.1240(3) 0.4128(3) 0.4619(2) 0.0412(7) Uani 1 1 d . . . H10 H -0.1565 0.4497 0.5246 0.049 Uiso 1 1 calc R . . C11 C -0.1604(2) 0.4872(3) 0.3699(3) 0.0450(8) Uani 1 1 d . . . H11 H -0.2142 0.5768 0.3695 0.054 Uiso 1 1 calc R . . C12 C -0.1192(2) 0.4324(3) 0.2789(2) 0.0388(6) Uani 1 1 d . . . H12 H -0.1472 0.4831 0.2162 0.047 Uiso 1 1 calc R . . C13 C -0.0371(2) 0.3037(2) 0.27874(18) 0.0267(5) Uani 1 1 d . . . H13 H -0.0095 0.2653 0.2161 0.032 Uiso 1 1 calc R . . C14 C 0.71379(19) -0.01779(19) 0.35114(15) 0.0155(4) Uani 1 1 d . . . H14A H 0.7870 0.0133 0.2970 0.019 Uiso 1 1 calc R . . H14B H 0.7511 -0.0203 0.4184 0.019 Uiso 1 1 calc R . . C15 C 0.56267(19) -0.18639(19) 0.40107(14) 0.0150(4) Uani 1 1 d . . . H15A H 0.5566 -0.2841 0.4028 0.018 Uiso 1 1 calc R . . H15B H 0.5683 -0.1688 0.4722 0.018 Uiso 1 1 calc R . . C16 C 0.4125(2) -0.14797(19) 0.26386(14) 0.0152(4) Uani 1 1 d . . . H16A H 0.3407 -0.0787 0.2284 0.018 Uiso 1 1 calc R . . H16B H 0.3734 -0.2347 0.2774 0.018 Uiso 1 1 calc R . . C17 C 0.68613(19) -0.17290(18) 0.23167(13) 0.0132(3) Uani 1 1 d . . . C18 C 0.8140(2) -0.19660(19) 0.16586(14) 0.0155(4) Uani 1 1 d . . . C19 C 0.8075(2) -0.2104(2) 0.06327(15) 0.0177(4) Uani 1 1 d . . . H19 H 0.8946 -0.2261 0.0192 0.021 Uiso 1 1 calc R . . C20 C 0.6747(2) -0.2013(2) 0.02441(15) 0.0191(4) Uani 1 1 d . . . C21 C 0.5486(2) -0.1832(2) 0.09105(15) 0.0187(4) Uani 1 1 d . . . H21 H 0.4578 -0.1809 0.0660 0.022 Uiso 1 1 calc R . . C22 C 0.5529(2) -0.16828(19) 0.19394(14) 0.0148(4) Uani 1 1 d . . . C23 C 0.6687(2) -0.2094(2) -0.08837(16) 0.0264(5) Uani 1 1 d . . . H23A H 0.6724 -0.3046 -0.0993 0.040 Uiso 1 1 calc R . . H23B H 0.7515 -0.1740 -0.1283 0.040 Uiso 1 1 calc R . . H23C H 0.5784 -0.1548 -0.1107 0.040 Uiso 1 1 calc R . . C24 C 1.1229(2) -0.2468(2) 0.10469(15) 0.0185(4) Uani 1 1 d . . . C25 C 1.1568(2) -0.1411(2) 0.03128(16) 0.0223(4) Uani 1 1 d . . . H25 H 1.1205 -0.0492 0.0422 0.027 Uiso 1 1 calc R . . C26 C 1.2439(2) -0.1698(2) -0.05813(16) 0.0252(5) Uani 1 1 d . . . H26 H 1.2664 -0.0975 -0.1086 0.030 Uiso 1 1 calc R . . C27 C 1.2975(2) -0.3029(2) -0.07357(17) 0.0289(5) Uani 1 1 d . . . H27 H 1.3565 -0.3224 -0.1350 0.035 Uiso 1 1 calc R . . C28 C 1.2658(3) -0.4090(2) 0.00016(18) 0.0340(5) Uani 1 1 d . . . H28 H 1.3041 -0.5007 -0.0104 0.041 Uiso 1 1 calc R . . C29 C 1.1778(2) -0.3810(2) 0.08958(17) 0.0271(5) Uani 1 1 d . . . H29 H 1.1555 -0.4534 0.1400 0.032 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 Se1 0.01305(9) 0.01320(10) 0.02648(11) -0.00413(8) -0.00111(7) -0.00132(7) Se2 0.01458(10) 0.02649(12) 0.01897(10) -0.00799(8) -0.00009(7) -0.00087(8) N1 0.0155(7) 0.0142(8) 0.0115(7) -0.0033(6) 0.0000(6) -0.0002(6) N2 0.0161(7) 0.0096(7) 0.0156(8) -0.0018(6) -0.0007(6) -0.0012(6) C1 0.0159(8) 0.0118(9) 0.0095(8) -0.0013(7) 0.0001(6) -0.0007(7) C2 0.0141(8) 0.0149(9) 0.0128(8) -0.0024(7) -0.0012(7) -0.0023(7) C3 0.0162(9) 0.0128(9) 0.0138(9) -0.0016(7) -0.0011(7) 0.0013(7) C4 0.0191(9) 0.0112(9) 0.0148(9) -0.0015(7) 0.0007(7) -0.0031(7) C5 0.0171(9) 0.0155(9) 0.0139(9) -0.0023(7) 0.0012(7) -0.0051(7) C6 0.0150(8) 0.0153(9) 0.0113(8) -0.0022(7) 0.0013(6) -0.0013(7) C7 0.0229(10) 0.0127(10) 0.0359(12) -0.0038(9) 0.0004(9) -0.0035(8) C8 0.0121(8) 0.0136(9) 0.0293(11) -0.0030(8) 0.0010(7) -0.0017(7) C9 0.0240(11) 0.0247(12) 0.0350(12) -0.0077(10) 0.0051(9) -0.0038(9) C10 0.0284(12) 0.0293(14) 0.0661(19) -0.0236(13) 0.0157(12) -0.0049(10) C11 0.0166(11) 0.0174(12) 0.096(2) -0.0019(14) -0.0002(13) 0.0025(9) C12 0.0200(11) 0.0265(13) 0.0656(18) 0.0150(12) -0.0096(11) -0.0043(9) C13 0.0163(9) 0.0289(12) 0.0337(12) 0.0041(10) -0.0037(8) -0.0059(9) C14 0.0153(9) 0.0139(9) 0.0173(9) -0.0037(7) -0.0011(7) -0.0010(7) C15 0.0166(9) 0.0110(9) 0.0151(9) -0.0004(7) 0.0006(7) 0.0013(7) C16 0.0159(9) 0.0128(9) 0.0172(9) -0.0044(7) -0.0020(7) -0.0009(7) C17 0.0172(9) 0.0094(9) 0.0125(9) -0.0016(7) -0.0017(7) -0.0005(7) C18 0.0146(8) 0.0145(9) 0.0166(9) -0.0025(7) -0.0005(7) -0.0010(7) C19 0.0192(9) 0.0153(10) 0.0175(9) -0.0041(7) 0.0023(7) -0.0010(7) C20 0.0245(10) 0.0177(10) 0.0143(9) -0.0024(8) -0.0020(7) -0.0011(8) C21 0.0188(9) 0.0185(10) 0.0190(10) -0.0041(8) -0.0043(7) -0.0007(8) C22 0.0171(9) 0.0107(9) 0.0159(9) -0.0018(7) -0.0009(7) -0.0005(7) C23 0.0287(11) 0.0326(13) 0.0175(10) -0.0055(9) -0.0022(8) -0.0017(9) C24 0.0143(9) 0.0230(11) 0.0175(9) -0.0034(8) 0.0016(7) -0.0021(8) C25 0.0176(9) 0.0196(11) 0.0284(11) 0.0007(9) -0.0034(8) -0.0013(8) C26 0.0203(10) 0.0314(12) 0.0216(11) 0.0076(9) -0.0021(8) -0.0067(9) C27 0.0270(11) 0.0373(14) 0.0208(11) -0.0049(10) 0.0054(9) -0.0056(10) C28 0.0424(14) 0.0234(12) 0.0321(13) -0.0082(10) 0.0118(10) -0.0012(10) C29 0.0325(12) 0.0213(11) 0.0237(11) -0.0008(9) 0.0069(9) -0.0024(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 0.8891 (0.0073) x - 9.7245 (0.0020) y + 1.3870 (0.0103) z = 1.4085 (0.0052) * -0.0158 (0.0013) C17 * 0.0097 (0.0013) C18 * 0.0069 (0.0014) C19 * -0.0174 (0.0014) C20 * 0.0113 (0.0014) C21 * 0.0053 (0.0013) C22 Rms deviation of fitted atoms = 0.0119 0.3795 (0.0070) x + 0.8184 (0.0073) y + 13.1614 (0.0009) z = 4.8526 (0.0039) Angle to previous plane (with approximate esd) = 80.93 ( 0.06 ) * -0.0108 (0.0012) C1 * 0.0164 (0.0012) C2 * -0.0065 (0.0013) C3 * -0.0091 (0.0013) C4 * 0.0148 (0.0013) C5 * -0.0047 (0.0012) C6 Rms deviation of fitted atoms = 0.0112 ; 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 Se1 C8 1.9177(19) . ? Se1 C2 1.9249(17) . ? Se2 C24 1.9230(19) . ? Se2 C18 1.9263(19) . ? N1 C17 1.440(2) . ? N1 C15 1.472(2) . ? N1 C14 1.477(2) . ? N2 C1 1.435(2) . ? N2 C15 1.463(2) . ? N2 C16 1.477(2) . ? C1 C6 1.400(2) . ? C1 C2 1.406(3) . ? C2 C3 1.388(3) . ? C3 C4 1.400(2) . ? C4 C5 1.388(3) . ? C4 C7 1.506(3) . ? C5 C6 1.397(3) . ? C6 C14 1.518(3) . ? C8 C9 1.385(3) . ? C8 C13 1.393(3) . ? C9 C10 1.392(3) . ? C10 C11 1.382(4) . ? C11 C12 1.378(4) . ? C12 C13 1.383(3) . ? C16 C22 1.519(2) . ? C17 C22 1.397(2) . ? C17 C18 1.403(2) . ? C18 C19 1.392(3) . ? C19 C20 1.393(3) . ? C20 C21 1.391(3) . ? C20 C23 1.512(3) . ? C21 C22 1.395(3) . ? C24 C29 1.387(3) . ? C24 C25 1.389(3) . ? C25 C26 1.389(3) . ? C26 C27 1.377(3) . ? C27 C28 1.388(3) . ? C28 C29 1.392(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 C8 Se1 C2 97.08(8) . . ? C24 Se2 C18 97.75(8) . . ? C17 N1 C15 110.53(14) . . ? C17 N1 C14 112.97(14) . . ? C15 N1 C14 107.46(14) . . ? C1 N2 C15 110.65(14) . . ? C1 N2 C16 112.01(14) . . ? C15 N2 C16 108.20(14) . . ? C6 C1 C2 119.52(17) . . ? C6 C1 N2 121.67(16) . . ? C2 C1 N2 118.78(16) . . ? C3 C2 C1 119.94(16) . . ? C3 C2 Se1 123.88(14) . . ? C1 C2 Se1 116.16(13) . . ? C2 C3 C4 120.90(17) . . ? C5 C4 C3 118.68(17) . . ? C5 C4 C7 121.49(17) . . ? C3 C4 C7 119.82(17) . . ? C4 C5 C6 121.45(17) . . ? C5 C6 C1 119.42(17) . . ? C5 C6 C14 120.28(16) . . ? C1 C6 C14 120.28(16) . . ? C9 C8 C13 120.5(2) . . ? C9 C8 Se1 119.26(16) . . ? C13 C8 Se1 120.14(16) . . ? C8 C9 C10 119.1(2) . . ? C11 C10 C9 120.2(2) . . ? C12 C11 C10 120.5(2) . . ? C11 C12 C13 120.0(2) . . ? C12 C13 C8 119.7(2) . . ? N1 C14 C6 112.90(15) . . ? N2 C15 N1 112.30(15) . . ? N2 C16 C22 112.70(15) . . ? C22 C17 C18 119.24(16) . . ? C22 C17 N1 121.39(16) . . ? C18 C17 N1 119.35(16) . . ? C19 C18 C17 120.18(17) . . ? C19 C18 Se2 123.08(14) . . ? C17 C18 Se2 116.74(13) . . ? C18 C19 C20 120.79(17) . . ? C21 C20 C19 118.69(18) . . ? C21 C20 C23 121.06(18) . . ? C19 C20 C23 120.25(18) . . ? C20 C21 C22 121.31(18) . . ? C21 C22 C17 119.70(17) . . ? C21 C22 C16 119.53(17) . . ? C17 C22 C16 120.76(16) . . ? C29 C24 C25 120.06(18) . . ? C29 C24 Se2 119.77(15) . . ? C25 C24 Se2 120.13(15) . . ? C24 C25 C26 120.0(2) . . ? C27 C26 C25 119.9(2) . . ? C26 C27 C28 120.3(2) . . ? C27 C28 C29 120.0(2) . . ? C24 C29 C28 119.6(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 C15 N2 C1 C6 20.1(2) . . . . ? C16 N2 C1 C6 -100.70(19) . . . . ? C15 N2 C1 C2 -157.82(16) . . . . ? C16 N2 C1 C2 81.35(19) . . . . ? C6 C1 C2 C3 2.6(3) . . . . ? N2 C1 C2 C3 -179.36(16) . . . . ? C6 C1 C2 Se1 -176.07(13) . . . . ? N2 C1 C2 Se1 1.9(2) . . . . ? C8 Se1 C2 C3 -1.46(17) . . . . ? C8 Se1 C2 C1 177.19(14) . . . . ? C1 C2 C3 C4 -2.3(3) . . . . ? Se1 C2 C3 C4 176.34(14) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C2 C3 C4 C7 -179.51(17) . . . . ? C3 C4 C5 C6 2.2(3) . . . . ? C7 C4 C5 C6 -178.45(18) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C4 C5 C6 C14 -179.88(17) . . . . ? C2 C1 C6 C5 -0.6(3) . . . . ? N2 C1 C6 C5 -178.58(16) . . . . ? C2 C1 C6 C14 177.43(16) . . . . ? N2 C1 C6 C14 -0.5(3) . . . . ? C2 Se1 C8 C9 -89.25(16) . . . . ? C2 Se1 C8 C13 87.11(16) . . . . ? C13 C8 C9 C10 -1.8(3) . . . . ? Se1 C8 C9 C10 174.51(16) . . . . ? C8 C9 C10 C11 -0.8(3) . . . . ? C9 C10 C11 C12 2.8(4) . . . . ? C10 C11 C12 C13 -2.0(3) . . . . ? C11 C12 C13 C8 -0.7(3) . . . . ? C9 C8 C13 C12 2.6(3) . . . . ? Se1 C8 C13 C12 -173.70(15) . . . . ? C17 N1 C14 C6 77.23(18) . . . . ? C15 N1 C14 C6 -44.96(19) . . . . ? C5 C6 C14 N1 -168.16(16) . . . . ? C1 C6 C14 N1 13.8(2) . . . . ? C1 N2 C15 N1 -55.03(19) . . . . ? C16 N2 C15 N1 68.03(18) . . . . ? C17 N1 C15 N2 -55.08(19) . . . . ? C14 N1 C15 N2 68.60(18) . . . . ? C1 N2 C16 C22 78.11(19) . . . . ? C15 N2 C16 C22 -44.13(19) . . . . ? C15 N1 C17 C22 20.7(2) . . . . ? C14 N1 C17 C22 -99.74(19) . . . . ? C15 N1 C17 C18 -157.92(16) . . . . ? C14 N1 C17 C18 81.6(2) . . . . ? C22 C17 C18 C19 2.3(3) . . . . ? N1 C17 C18 C19 -179.03(17) . . . . ? C22 C17 C18 Se2 -177.83(13) . . . . ? N1 C17 C18 Se2 0.8(2) . . . . ? C24 Se2 C18 C19 -2.21(18) . . . . ? C24 Se2 C18 C17 177.93(15) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? Se2 C18 C19 C20 179.97(15) . . . . ? C18 C19 C20 C21 -2.4(3) . . . . ? C18 C19 C20 C23 176.95(19) . . . . ? C19 C20 C21 C22 2.8(3) . . . . ? C23 C20 C21 C22 -176.51(19) . . . . ? C20 C21 C22 C17 -0.7(3) . . . . ? C20 C21 C22 C16 179.66(18) . . . . ? C18 C17 C22 C21 -1.9(3) . . . . ? N1 C17 C22 C21 179.48(17) . . . . ? C18 C17 C22 C16 177.77(17) . . . . ? N1 C17 C22 C16 -0.9(3) . . . . ? N2 C16 C22 C21 -167.27(17) . . . . ? N2 C16 C22 C17 13.1(2) . . . . ? C18 Se2 C24 C29 -93.60(18) . . . . ? C18 Se2 C24 C25 83.91(17) . . . . ? C29 C24 C25 C26 1.1(3) . . . . ? Se2 C24 C25 C26 -176.46(15) . . . . ? C24 C25 C26 C27 -0.5(3) . . . . ? C25 C26 C27 C28 -0.4(3) . . . . ? C26 C27 C28 C29 0.9(4) . . . . ? C25 C24 C29 C28 -0.6(3) . . . . ? Se2 C24 C29 C28 176.90(18) . . . . ? C27 C28 C29 C24 -0.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.475 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.073 # Attachment '- 2a.cif' data_nis811 _database_code_depnum_ccdc_archive 'CCDC 865870' #TrackingRef '- 2a.cif' # This structure was measured, # solved and refined by: # Elli Maennel _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H34 N2 S2' _chemical_formula_sum 'C25 H34 N2 S2' _chemical_formula_weight 426.66 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3248(2) _cell_length_b 11.8592(3) _cell_length_c 12.5893(2) _cell_angle_alpha 81.4160(10) _cell_angle_beta 85.7680(10) _cell_angle_gamma 69.8820(10) _cell_volume 1153.64(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2215 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.35 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.245 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9637 _exptl_absorpt_correction_T_max 0.9826 _exptl_absorpt_process_details SADABS-2004/1 _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 13892 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.1232 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.40 _reflns_number_total 5743 _reflns_number_gt 3508 _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^)+(0.0225P)^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 none _refine_ls_number_reflns 5743 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.005 _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 S1 S 0.33149(6) 0.89975(4) 0.49157(4) 0.01795(12) Uani 1 1 d . . . S2 S -0.05053(6) 0.69226(5) 0.02882(4) 0.02224(13) Uani 1 1 d . . . N1 N 0.30369(18) 0.77938(13) 0.31444(11) 0.0152(3) Uani 1 1 d . . . N2 N 0.18364(19) 0.75144(13) 0.15326(12) 0.0166(3) Uani 1 1 d . . . C1 C 0.1958(2) 0.97463(17) 0.38275(14) 0.0153(4) Uani 1 1 d . . . C2 C 0.0917(2) 1.09556(17) 0.37256(14) 0.0177(4) Uani 1 1 d . . . H2 H 0.0887 1.1425 0.4280 0.021 Uiso 1 1 calc R . . C3 C -0.0083(2) 1.14929(17) 0.28252(15) 0.0181(4) Uani 1 1 d . . . C4 C -0.0005(2) 1.08033(17) 0.20097(15) 0.0182(4) Uani 1 1 d . . . H4 H -0.0651 1.1170 0.1382 0.022 Uiso 1 1 calc R . . C5 C 0.1009(2) 0.95782(17) 0.20961(14) 0.0163(4) Uani 1 1 d . . . C6 C 0.1978(2) 0.90521(16) 0.30068(14) 0.0146(4) Uani 1 1 d . . . C7 C -0.1262(2) 1.27949(17) 0.27631(16) 0.0243(5) Uani 1 1 d . . . H7A H -0.1615 1.3102 0.2019 0.036 Uiso 1 1 calc R . . H7B H -0.0661 1.3288 0.3003 0.036 Uiso 1 1 calc R . . H7C H -0.2276 1.2839 0.3226 0.036 Uiso 1 1 calc R . . C8 C 0.1064(2) 0.88346(16) 0.12037(14) 0.0187(4) Uani 1 1 d . . . H8A H -0.0116 0.9015 0.0965 0.022 Uiso 1 1 calc R . . H8B H 0.1730 0.9080 0.0584 0.022 Uiso 1 1 calc R . . C9 C 0.3395(2) 0.73131(17) 0.21138(14) 0.0182(4) Uani 1 1 d . . . H9A H 0.4035 0.6433 0.2243 0.022 Uiso 1 1 calc R . . H9B H 0.4132 0.7703 0.1661 0.022 Uiso 1 1 calc R . . C10 C 0.2184(2) 0.70535(16) 0.38616(14) 0.0169(4) Uani 1 1 d . . . H10A H 0.1698 0.7466 0.4499 0.020 Uiso 1 1 calc R . . H10B H 0.3047 0.6261 0.4114 0.020 Uiso 1 1 calc R . . C11 C 0.0773(2) 0.68419(16) 0.33192(14) 0.0154(4) Uani 1 1 d . . . C12 C 0.0671(2) 0.70358(16) 0.22049(14) 0.0153(4) Uani 1 1 d . . . C13 C -0.0556(2) 0.67344(16) 0.17088(14) 0.0165(4) Uani 1 1 d . . . C14 C -0.1722(2) 0.63035(16) 0.23435(14) 0.0166(4) Uani 1 1 d . . . H14 H -0.2555 0.6102 0.2009 0.020 Uiso 1 1 calc R . . C15 C -0.1682(2) 0.61642(16) 0.34652(14) 0.0158(4) Uani 1 1 d . . . C16 C -0.0416(2) 0.64149(16) 0.39358(14) 0.0162(4) Uani 1 1 d . . . H16 H -0.0353 0.6294 0.4697 0.019 Uiso 1 1 calc R . . C17 C -0.3040(2) 0.57902(17) 0.41362(14) 0.0197(4) Uani 1 1 d . . . H17A H -0.2671 0.5533 0.4882 0.029 Uiso 1 1 calc R . . H17B H -0.3216 0.5117 0.3852 0.029 Uiso 1 1 calc R . . H17C H -0.4114 0.6478 0.4111 0.029 Uiso 1 1 calc R . . C18 C -0.2251(2) 0.64615(18) -0.00396(14) 0.0230(5) Uani 1 1 d . . . H18A H -0.2109 0.5634 0.0324 0.028 Uiso 1 1 calc R . . H18B H -0.3355 0.7021 0.0207 0.028 Uiso 1 1 calc R . . C19 C -0.2239(2) 0.64868(18) -0.12493(15) 0.0238(5) Uani 1 1 d . . . H19A H -0.1120 0.5937 -0.1484 0.029 Uiso 1 1 calc R . . H19B H -0.2366 0.7317 -0.1600 0.029 Uiso 1 1 calc R . . C20 C -0.3656(3) 0.61100(19) -0.16197(16) 0.0297(5) Uani 1 1 d . . . H20A H -0.4779 0.6664 -0.1395 0.036 Uiso 1 1 calc R . . H20B H -0.3536 0.5281 -0.1271 0.036 Uiso 1 1 calc R . . C21 C -0.3594(3) 0.61385(19) -0.28394(16) 0.0312(5) Uani 1 1 d . . . H21A H -0.3744 0.6964 -0.3186 0.047 Uiso 1 1 calc R . . H21B H -0.4513 0.5884 -0.3051 0.047 Uiso 1 1 calc R . . H21C H -0.2486 0.5586 -0.3063 0.047 Uiso 1 1 calc R . . C22 C 0.2848(2) 1.01342(16) 0.58171(14) 0.0177(4) Uani 1 1 d . . . H22A H 0.3111 1.0852 0.5453 0.021 Uiso 1 1 calc R . . H22B H 0.1620 1.0394 0.6030 0.021 Uiso 1 1 calc R . . C23 C 0.3935(2) 0.95892(16) 0.68023(14) 0.0178(4) Uani 1 1 d . . . H23A H 0.5156 0.9276 0.6577 0.021 Uiso 1 1 calc R . . H23B H 0.3618 0.8901 0.7184 0.021 Uiso 1 1 calc R . . C24 C 0.3688(2) 1.05273(17) 0.75600(15) 0.0220(4) Uani 1 1 d . . . H24A H 0.4144 1.1161 0.7204 0.026 Uiso 1 1 calc R . . H24B H 0.2448 1.0920 0.7698 0.026 Uiso 1 1 calc R . . C25 C 0.4560(3) 0.99961(19) 0.86222(15) 0.0288(5) Uani 1 1 d . . . H25A H 0.4133 0.9356 0.8973 0.043 Uiso 1 1 calc R . . H25B H 0.4312 1.0633 0.9085 0.043 Uiso 1 1 calc R . . H25C H 0.5798 0.9655 0.8496 0.043 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 S1 0.0176(3) 0.0192(3) 0.0175(2) -0.0038(2) -0.0025(2) -0.0058(2) S2 0.0257(3) 0.0297(3) 0.0160(2) -0.0049(2) 0.0001(2) -0.0147(2) N1 0.0149(8) 0.0147(9) 0.0161(8) -0.0019(6) 0.0001(6) -0.0054(7) N2 0.0167(8) 0.0173(9) 0.0173(8) -0.0014(7) 0.0003(7) -0.0082(7) C1 0.0136(9) 0.0187(11) 0.0139(9) 0.0016(8) 0.0003(7) -0.0075(8) C2 0.0167(10) 0.0194(11) 0.0199(10) -0.0052(8) 0.0022(8) -0.0091(9) C3 0.0170(10) 0.0161(11) 0.0212(10) 0.0009(8) 0.0008(8) -0.0072(9) C4 0.0186(10) 0.0187(11) 0.0171(9) 0.0029(8) -0.0008(8) -0.0083(9) C5 0.0151(10) 0.0194(11) 0.0160(9) -0.0007(8) 0.0016(8) -0.0089(9) C6 0.0130(9) 0.0137(10) 0.0166(9) -0.0001(8) 0.0019(8) -0.0050(8) C7 0.0246(11) 0.0196(12) 0.0262(11) 0.0000(9) -0.0018(9) -0.0053(9) C8 0.0215(10) 0.0197(11) 0.0155(9) 0.0011(8) -0.0001(8) -0.0093(9) C9 0.0183(10) 0.0190(11) 0.0194(10) -0.0048(8) 0.0022(8) -0.0085(9) C10 0.0179(10) 0.0155(10) 0.0180(10) -0.0007(8) -0.0007(8) -0.0070(9) C11 0.0134(9) 0.0115(10) 0.0202(10) -0.0027(8) -0.0018(8) -0.0023(8) C12 0.0157(10) 0.0125(10) 0.0171(9) -0.0032(8) 0.0014(8) -0.0037(8) C13 0.0170(10) 0.0157(10) 0.0153(9) -0.0027(8) -0.0008(8) -0.0032(8) C14 0.0148(10) 0.0140(10) 0.0213(10) -0.0040(8) -0.0025(8) -0.0039(8) C15 0.0141(10) 0.0106(10) 0.0204(10) -0.0009(8) 0.0002(8) -0.0019(8) C16 0.0182(10) 0.0131(10) 0.0148(9) -0.0001(7) -0.0022(8) -0.0026(8) C17 0.0165(10) 0.0212(11) 0.0217(10) -0.0004(8) -0.0009(8) -0.0078(9) C18 0.0231(11) 0.0320(13) 0.0188(10) -0.0054(9) -0.0007(9) -0.0146(10) C19 0.0251(11) 0.0246(12) 0.0233(10) -0.0066(9) -0.0015(9) -0.0087(10) C20 0.0293(12) 0.0316(13) 0.0300(12) -0.0100(10) -0.0051(10) -0.0091(10) C21 0.0351(13) 0.0264(13) 0.0307(12) -0.0101(10) -0.0117(10) -0.0038(11) C22 0.0186(10) 0.0159(10) 0.0193(10) -0.0053(8) 0.0004(8) -0.0056(9) C23 0.0159(10) 0.0177(11) 0.0194(10) -0.0027(8) -0.0007(8) -0.0049(8) C24 0.0226(11) 0.0233(12) 0.0210(10) -0.0049(9) 0.0001(9) -0.0084(9) C25 0.0360(13) 0.0316(13) 0.0214(11) -0.0040(9) -0.0056(10) -0.0134(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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 2.6129 (0.0055) x + 9.2906 (0.0051) y + 1.5135 (0.0090) z = 6.6715 (0.0043) * -0.0145 (0.0012) C11 * 0.0235 (0.0013) C12 * -0.0109 (0.0013) C13 * -0.0105 (0.0013) C14 * 0.0195 (0.0012) C15 * -0.0072 (0.0012) C16 Rms deviation of fitted atoms = 0.0154 7.2418 (0.0027) x + 5.7771 (0.0066) y - 4.4692 (0.0077) z = 5.3279 (0.0080) Angle to previous plane (with approximate esd) = 84.76 ( 0.05 ) * 0.0098 (0.0011) C1 * 0.0006 (0.0012) C2 * -0.0112 (0.0012) C3 * 0.0115 (0.0012) C4 * -0.0009 (0.0012) C5 * -0.0097 (0.0012) C6 Rms deviation of fitted atoms = 0.0087 ; 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 S1 C1 1.7655(19) . ? S1 C22 1.8131(17) . ? S2 C13 1.7682(18) . ? S2 C18 1.8124(18) . ? N1 C6 1.440(2) . ? N1 C9 1.464(2) . ? N1 C10 1.479(2) . ? N2 C12 1.447(2) . ? N2 C9 1.466(2) . ? N2 C8 1.480(2) . ? C1 C2 1.389(2) . ? C1 C6 1.410(2) . ? C2 C3 1.394(3) . ? C3 C4 1.390(2) . ? C3 C7 1.512(2) . ? C4 C5 1.399(2) . ? C5 C6 1.390(2) . ? C5 C8 1.517(2) . ? C10 C11 1.511(2) . ? C11 C12 1.391(2) . ? C11 C16 1.397(2) . ? C12 C13 1.405(2) . ? C13 C14 1.395(2) . ? C14 C15 1.399(2) . ? C15 C16 1.382(2) . ? C15 C17 1.510(2) . ? C18 C19 1.518(2) . ? C19 C20 1.521(3) . ? C20 C21 1.528(3) . ? C22 C23 1.516(2) . ? C23 C24 1.523(2) . ? C24 C25 1.513(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 C1 S1 C22 103.40(9) . . ? C13 S2 C18 103.68(8) . . ? C6 N1 C9 111.02(14) . . ? C6 N1 C10 111.03(13) . . ? C9 N1 C10 107.53(14) . . ? C12 N2 C9 110.43(14) . . ? C12 N2 C8 111.65(13) . . ? C9 N2 C8 107.38(14) . . ? C2 C1 C6 118.98(17) . . ? C2 C1 S1 124.63(14) . . ? C6 C1 S1 116.38(14) . . ? C1 C2 C3 121.27(17) . . ? C4 C3 C2 118.87(18) . . ? C4 C3 C7 121.21(18) . . ? C2 C3 C7 119.91(17) . . ? C3 C4 C5 121.21(18) . . ? C6 C5 C4 119.14(17) . . ? C6 C5 C8 120.32(17) . . ? C4 C5 C8 120.54(17) . . ? C5 C6 C1 120.49(17) . . ? C5 C6 N1 121.67(16) . . ? C1 C6 N1 117.84(16) . . ? N2 C8 C5 113.11(15) . . ? N1 C9 N2 112.73(14) . . ? N1 C10 C11 112.84(14) . . ? C12 C11 C16 119.42(17) . . ? C12 C11 C10 120.57(15) . . ? C16 C11 C10 119.98(15) . . ? C11 C12 C13 119.85(16) . . ? C11 C12 N2 121.54(16) . . ? C13 C12 N2 118.59(15) . . ? C14 C13 C12 119.45(16) . . ? C14 C13 S2 123.80(14) . . ? C12 C13 S2 116.75(13) . . ? C13 C14 C15 120.95(17) . . ? C16 C15 C14 118.59(16) . . ? C16 C15 C17 121.30(16) . . ? C14 C15 C17 120.07(17) . . ? C15 C16 C11 121.59(16) . . ? C19 C18 S2 108.34(12) . . ? C18 C19 C20 113.01(16) . . ? C19 C20 C21 111.48(17) . . ? C23 C22 S1 108.47(13) . . ? C22 C23 C24 111.03(15) . . ? C25 C24 C23 113.28(16) . . ? 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 C22 S1 C1 C2 4.20(16) . . . . ? C22 S1 C1 C6 -176.92(13) . . . . ? C6 C1 C2 C3 -0.8(2) . . . . ? S1 C1 C2 C3 178.08(13) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? C1 C2 C3 C7 177.20(15) . . . . ? C2 C3 C4 C5 2.2(3) . . . . ? C7 C3 C4 C5 -176.13(15) . . . . ? C3 C4 C5 C6 -1.3(2) . . . . ? C3 C4 C5 C8 179.30(16) . . . . ? C4 C5 C6 C1 -0.7(2) . . . . ? C8 C5 C6 C1 178.67(15) . . . . ? C4 C5 C6 N1 179.59(14) . . . . ? C8 C5 C6 N1 -1.0(2) . . . . ? C2 C1 C6 C5 1.8(2) . . . . ? S1 C1 C6 C5 -177.19(13) . . . . ? C2 C1 C6 N1 -178.57(14) . . . . ? S1 C1 C6 N1 2.5(2) . . . . ? C9 N1 C6 C5 19.3(2) . . . . ? C10 N1 C6 C5 -100.24(18) . . . . ? C9 N1 C6 C1 -160.34(15) . . . . ? C10 N1 C6 C1 80.10(18) . . . . ? C12 N2 C8 C5 75.79(19) . . . . ? C9 N2 C8 C5 -45.40(18) . . . . ? C6 C5 C8 N2 14.9(2) . . . . ? C4 C5 C8 N2 -165.73(15) . . . . ? C6 N1 C9 N2 -53.72(19) . . . . ? C10 N1 C9 N2 67.93(18) . . . . ? C12 N2 C9 N1 -54.33(19) . . . . ? C8 N2 C9 N1 67.62(17) . . . . ? C6 N1 C10 C11 75.48(18) . . . . ? C9 N1 C10 C11 -46.16(19) . . . . ? N1 C10 C11 C12 16.9(2) . . . . ? N1 C10 C11 C16 -164.95(15) . . . . ? C16 C11 C12 C13 -3.7(3) . . . . ? C10 C11 C12 C13 174.44(16) . . . . ? C16 C11 C12 N2 177.94(16) . . . . ? C10 C11 C12 N2 -3.9(3) . . . . ? C9 N2 C12 C11 21.3(2) . . . . ? C8 N2 C12 C11 -98.06(19) . . . . ? C9 N2 C12 C13 -156.99(16) . . . . ? C8 N2 C12 C13 83.61(19) . . . . ? C11 C12 C13 C14 3.4(3) . . . . ? N2 C12 C13 C14 -178.22(15) . . . . ? C11 C12 C13 S2 -176.16(14) . . . . ? N2 C12 C13 S2 2.2(2) . . . . ? C18 S2 C13 C14 0.85(18) . . . . ? C18 S2 C13 C12 -179.59(14) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? S2 C13 C14 C15 179.35(14) . . . . ? C13 C14 C15 C16 -2.6(3) . . . . ? C13 C14 C15 C17 175.22(16) . . . . ? C14 C15 C16 C11 2.3(3) . . . . ? C17 C15 C16 C11 -175.51(16) . . . . ? C12 C11 C16 C15 0.9(3) . . . . ? C10 C11 C16 C15 -177.34(16) . . . . ? C13 S2 C18 C19 -175.36(14) . . . . ? S2 C18 C19 C20 179.82(14) . . . . ? C18 C19 C20 C21 -179.61(17) . . . . ? C1 S1 C22 C23 179.39(12) . . . . ? S1 C22 C23 C24 176.28(12) . . . . ? C22 C23 C24 C25 172.46(15) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.326 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.081 # Attachment '- 3b.cif' data_nis818 _database_code_depnum_ccdc_archive 'CCDC 865871' #TrackingRef '- 3b.cif' # This structure was measured, # solved and refined by: # Elli Maennel _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_properties_physical 'light sensitive' _chemical_formula_moiety '2 (C40 H48 Ag2 N2 O3 S2), 4 (Cl O4)' _chemical_formula_sum 'C80 H96 Ag4 Cl4 N4 O22 S4' _chemical_formula_weight 2167.13 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' Ag Ag -0.8971 1.1015 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6111(3) _cell_length_b 11.8157(3) _cell_length_c 18.9074(5) _cell_angle_alpha 86.053(2) _cell_angle_beta 89.515(2) _cell_angle_gamma 64.611(2) _cell_volume 2135.95(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3945 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.22 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7934 _exptl_absorpt_correction_T_max 0.8883 _exptl_absorpt_process_details SADABS-2004/1 _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 23087 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.10 _reflns_number_total 9403 _reflns_number_gt 6477 _reflns_threshold_expression >2sigma(I) _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^)+(0.0494P)^2^+3.9520P] 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 9403 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ag1 Ag 0.67639(4) 0.66712(4) 0.38413(2) 0.02808(11) Uani 1 1 d . . . Ag2 Ag 0.38681(4) 0.88328(4) 0.06901(2) 0.03073(12) Uani 1 1 d . . . S1 S 0.46957(13) 0.69920(12) 0.47196(6) 0.0265(3) Uani 1 1 d . A . S2 S 0.14829(13) 0.87703(11) 0.08033(6) 0.0233(3) Uani 1 1 d . . . Cl20 Cl 0.53906(13) 1.07886(12) 0.10417(7) 0.0280(3) Uani 1 1 d . . . Cl1A Cl 0.8109(6) 0.4198(5) 0.2840(3) 0.0271(9) Uani 0.734(11) 1 d P A 1 Cl1B Cl 0.838(2) 0.4051(19) 0.2990(10) 0.048(4) Uani 0.266(11) 1 d P A 2 O11 O 0.5887(5) 0.6847(5) 0.0944(2) 0.0574(12) Uani 1 1 d . . . O12 O 0.4445(5) 1.0367(6) 0.1345(3) 0.0711(16) Uani 1 1 d . . . O13 O 0.7734(6) 0.7936(5) 0.3289(3) 0.0683(15) Uani 1 1 d . A . O14 O 0.8397(5) 0.6175(5) 0.4879(2) 0.0549(12) Uani 1 1 d . A . O1A O 0.7753(7) 0.4276(7) 0.3603(4) 0.0404(19) Uiso 0.734(11) 1 d P A 1 O2A O 0.8014(7) 0.5386(6) 0.2604(4) 0.0484(18) Uiso 0.734(11) 1 d P A 1 O3A O 0.7145(6) 0.3857(6) 0.2497(3) 0.047(2) Uiso 0.734(11) 1 d P A 1 O4A O 0.9509(6) 0.3273(5) 0.2759(3) 0.0352(16) Uiso 0.734(11) 1 d P A 1 O20A O 0.4720(10) 1.1441(9) 0.0365(5) 0.067(3) Uiso 0.545(11) 1 d P . 1 O21A O 0.6711(11) 0.9878(10) 0.0917(6) 0.070(3) Uiso 0.545(11) 1 d P . 1 O22A O 0.5424(10) 1.1740(10) 0.1449(5) 0.065(3) Uiso 0.545(11) 1 d P . 1 O1B O 0.795(2) 0.4519(18) 0.3641(10) 0.037(5) Uiso 0.266(11) 1 d P A 2 O2B O 0.986(2) 0.354(2) 0.2970(13) 0.073(7) Uiso 0.266(11) 1 d P A 2 O3B O 0.797(2) 0.312(2) 0.2821(11) 0.065(7) Uiso 0.266(11) 1 d P A 2 O4B O 0.7748(18) 0.5219(16) 0.2401(10) 0.040(5) Uiso 0.266(11) 1 d P A 2 O20B O 0.6327(17) 1.0783(16) 0.1590(8) 0.103(6) Uiso 0.455(11) 1 d P . 2 O21B O 0.4910(18) 1.2017(17) 0.0766(10) 0.116(6) Uiso 0.455(11) 1 d P . 2 O22B O 0.6203(15) 1.0026(13) 0.0494(8) 0.084(5) Uiso 0.455(11) 1 d P . 2 N1 N 0.4553(4) 0.7390(4) 0.3137(2) 0.0199(8) Uani 1 1 d . A . N2 N 0.3412(4) 0.8328(4) 0.2000(2) 0.0198(8) Uani 1 1 d . A . C1 C 0.2411(5) 0.9394(4) 0.3099(2) 0.0205(10) Uani 1 1 d . A . C3 C 0.4723(5) 0.7850(4) 0.2418(2) 0.0204(10) Uani 1 1 d . . . H3A H 0.5458 0.7159 0.2178 0.024 Uiso 1 1 calc R A . H3B H 0.5027 0.8530 0.2447 0.024 Uiso 1 1 calc R . . C4 C 0.3399(5) 0.8323(4) 0.4228(2) 0.0216(10) Uani 1 1 d . . . C5 C 0.0839(5) 0.8341(4) 0.0046(2) 0.0228(10) Uani 1 1 d . . . C6 C 0.4873(5) 0.7625(5) 0.5520(3) 0.0270(11) Uani 1 1 d . . . C7 C 0.3433(5) 0.8371(4) 0.3482(2) 0.0196(10) Uani 1 1 d . A . C8 C 0.2372(5) 0.9294(5) 0.4570(3) 0.0255(11) Uani 1 1 d . A . H8 H 0.2358 0.9245 0.5074 0.031 Uiso 1 1 calc R . . C9 C 0.1368(5) 1.0335(5) 0.4188(3) 0.0276(11) Uani 1 1 d . . . C10 C 0.1403(5) 1.0364(5) 0.3449(3) 0.0258(11) Uani 1 1 d . A . H10 H 0.0721 1.1062 0.3179 0.031 Uiso 1 1 calc R . . C11 C 0.4373(6) 0.7292(5) 0.6138(3) 0.0310(12) Uani 1 1 d . A . H11 H 0.3901 0.6768 0.6130 0.037 Uiso 1 1 calc R . . C12 C 0.5244(6) 0.8508(6) 0.6787(3) 0.0401(14) Uani 1 1 d . A . H12 H 0.5382 0.8806 0.7221 0.048 Uiso 1 1 calc R . . C13 C 0.5713(6) 0.8843(6) 0.6163(3) 0.0424(15) Uani 1 1 d . . . H13 H 0.6165 0.9384 0.6168 0.051 Uiso 1 1 calc R A . C14 C 0.5539(6) 0.8408(5) 0.5532(3) 0.0347(13) Uani 1 1 d . A . H14 H 0.5874 0.8644 0.5106 0.042 Uiso 1 1 calc R . . C15 C -0.0497(5) 0.8393(5) 0.0062(3) 0.0319(12) Uani 1 1 d . . . H15 H -0.1044 0.8620 0.0474 0.038 Uiso 1 1 calc R . . C16 C 0.1085(7) 0.7789(5) -0.1157(3) 0.0410(15) Uani 1 1 d . . . H16 H 0.1609 0.7606 -0.1578 0.049 Uiso 1 1 calc R . . C17 C 0.1634(6) 0.8045(5) -0.0556(3) 0.0316(12) Uani 1 1 d . . . H17 H 0.2542 0.8018 -0.0558 0.038 Uiso 1 1 calc R . . C18 C 0.4568(6) 0.7733(6) 0.6777(3) 0.0369(13) Uani 1 1 d . . . H18 H 0.4236 0.7501 0.7205 0.044 Uiso 1 1 calc R A . C19 C -0.0223(8) 0.7800(6) -0.1142(3) 0.0508(19) Uani 1 1 d . . . H19 H -0.0581 0.7596 -0.1549 0.061 Uiso 1 1 calc R . . C20 C -0.1013(7) 0.8104(5) -0.0542(4) 0.0449(17) Uani 1 1 d . . . H20 H -0.1914 0.8116 -0.0540 0.054 Uiso 1 1 calc R . . C21 C 0.0290(6) 1.1408(5) 0.4554(3) 0.0372(13) Uani 1 1 d . A . H21A H 0.0661 1.2014 0.4646 0.056 Uiso 1 1 calc R . . H21B H 0.0056 1.1088 0.5004 0.056 Uiso 1 1 calc R . . H21C H -0.0551 1.1820 0.4250 0.056 Uiso 1 1 calc R . . C22 C 0.2410(5) 0.9501(4) 0.2294(2) 0.0222(10) Uani 1 1 d . . . H22A H 0.1460 0.9707 0.2110 0.027 Uiso 1 1 calc R A . H22B H 0.2650 1.0197 0.2131 0.027 Uiso 1 1 calc R . . C23 C 0.2910(5) 0.7366(4) 0.1978(2) 0.0194(10) Uani 1 1 d . . . C24 C 0.3350(5) 0.6354(4) 0.2479(2) 0.0212(10) Uani 1 1 d . A . C25 C 0.4324(5) 0.6247(4) 0.3089(3) 0.0243(11) Uani 1 1 d . . . H25A H 0.3929 0.6079 0.3539 0.029 Uiso 1 1 calc R A . H25B H 0.5234 0.5523 0.3030 0.029 Uiso 1 1 calc R . . C26 C 0.2089(5) 0.5432(5) 0.1849(3) 0.0270(11) Uani 1 1 d . A . C27 C 0.1618(5) 0.6459(5) 0.1355(3) 0.0233(10) Uani 1 1 d . . . H27 H 0.1008 0.6506 0.0978 0.028 Uiso 1 1 calc R A . C28 C 0.2034(5) 0.7422(4) 0.1409(2) 0.0197(10) Uani 1 1 d . A . C31 C 0.1678(6) 0.4358(6) 0.1774(3) 0.0393(14) Uani 1 1 d . . . H31A H 0.0890 0.4631 0.1436 0.059 Uiso 1 1 calc R A . H31B H 0.1408 0.4114 0.2236 0.059 Uiso 1 1 calc R . . H31C H 0.2472 0.3637 0.1600 0.059 Uiso 1 1 calc R . . C32 C 0.8466(7) 0.5474(7) 0.5399(4) 0.0520(17) Uani 1 1 d . . . C33 C 0.8964(8) 0.5640(9) 0.6089(4) 0.071(2) Uani 1 1 d . A . H33A H 0.9215 0.6349 0.6042 0.107 Uiso 1 1 calc R . . H33B H 0.9784 0.4874 0.6249 0.107 Uiso 1 1 calc R . . H33C H 0.8224 0.5809 0.6435 0.107 Uiso 1 1 calc R . . C34 C 0.8021(7) 0.4430(6) 0.5375(4) 0.0519(17) Uani 1 1 d . A . H34A H 0.7064 0.4714 0.5542 0.078 Uiso 1 1 calc R . . H34B H 0.8647 0.3704 0.5680 0.078 Uiso 1 1 calc R . . H34C H 0.8061 0.4190 0.4886 0.078 Uiso 1 1 calc R . . C40 C 0.2949(5) 0.5387(5) 0.2411(3) 0.0269(11) Uani 1 1 d . . . H40 H 0.3268 0.4689 0.2752 0.032 Uiso 1 1 calc R A . C54 C 0.8071(9) 0.8697(9) 0.3686(5) 0.075(2) Uani 1 1 d . . . H54A H 0.8845 0.8196 0.4026 0.090 Uiso 1 1 calc R A 1 H54B H 0.7256 0.9254 0.3950 0.090 Uiso 1 1 calc R A 1 C55 C 0.8350(9) 0.7873(8) 0.2585(4) 0.068(2) Uani 1 1 d . . . H55A H 0.8918 0.6988 0.2482 0.081 Uiso 1 1 calc R A 1 H55B H 0.7610 0.8273 0.2213 0.081 Uiso 1 1 calc R A 1 C82 C 0.5752(7) 0.5738(6) 0.0722(4) 0.0538(18) Uani 1 1 d . . . H82A H 0.6054 0.5063 0.1110 0.065 Uiso 1 1 calc R . . H82B H 0.4774 0.5952 0.0584 0.065 Uiso 1 1 calc R . . C83 C 0.6655(9) 0.5346(7) 0.0119(4) 0.067(2) Uani 1 1 d . . . H83A H 0.6196 0.5854 -0.0322 0.080 Uiso 1 1 calc R . . H83B H 0.6948 0.4446 0.0050 0.080 Uiso 1 1 calc R . . C84 C 0.7925(9) 0.5601(7) 0.0352(6) 0.089(3) Uani 1 1 d . . . H84A H 0.8639 0.4859 0.0623 0.107 Uiso 1 1 calc R . . H84B H 0.8362 0.5833 -0.0063 0.107 Uiso 1 1 calc R . . C85 C 0.7256(8) 0.6661(9) 0.0802(4) 0.074(3) Uani 1 1 d . . . H85A H 0.7797 0.6485 0.1252 0.089 Uiso 1 1 calc R . . H85B H 0.7249 0.7432 0.0557 0.089 Uiso 1 1 calc R . . C56A C 0.922(2) 0.854(2) 0.2607(9) 0.072(5) Uiso 0.60(3) 1 d P A 1 H56A H 0.9264 0.8925 0.2131 0.087 Uiso 0.60(3) 1 calc PR A 1 H56B H 1.0176 0.7965 0.2775 0.087 Uiso 0.60(3) 1 calc PR A 1 C57B C 0.914(2) 0.897(2) 0.3339(11) 0.049(6) Uiso 0.40(3) 1 d P A 2 H57A H 1.0081 0.8291 0.3438 0.058 Uiso 0.40(3) 1 calc PR A 2 H57B H 0.9111 0.9778 0.3476 0.058 Uiso 0.40(3) 1 calc PR A 2 C57A C 0.854(2) 0.950(2) 0.3102(10) 0.075(5) Uiso 0.60(3) 1 d P A 1 H57C H 0.7729 1.0231 0.2881 0.090 Uiso 0.60(3) 1 calc PR A 1 H57D H 0.9199 0.9791 0.3306 0.090 Uiso 0.60(3) 1 calc PR A 1 C56B C 0.867(3) 0.906(3) 0.2544(11) 0.058(6) Uiso 0.40(3) 1 d P A 2 H56C H 0.9422 0.8982 0.2212 0.070 Uiso 0.40(3) 1 calc PR A 2 H56D H 0.7824 0.9849 0.2415 0.070 Uiso 0.40(3) 1 calc PR A 2 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 Ag1 0.0241(2) 0.0324(2) 0.0246(2) -0.00152(17) -0.00342(16) -0.00918(17) Ag2 0.0391(2) 0.0371(3) 0.0217(2) 0.00307(17) 0.00008(17) -0.0226(2) S1 0.0356(7) 0.0256(7) 0.0185(6) 0.0029(5) -0.0054(5) -0.0138(6) S2 0.0312(6) 0.0205(6) 0.0191(6) 0.0018(5) -0.0062(5) -0.0122(5) Cl20 0.0304(6) 0.0324(7) 0.0247(6) 0.0004(5) 0.0043(5) -0.0173(5) Cl1A 0.0288(17) 0.023(2) 0.0263(17) -0.0027(16) -0.0016(11) -0.0074(15) Cl1B 0.042(8) 0.031(4) 0.056(10) 0.019(6) 0.025(6) -0.004(5) O11 0.051(3) 0.067(3) 0.045(3) -0.014(2) 0.010(2) -0.015(2) O12 0.075(3) 0.117(5) 0.053(3) 0.000(3) 0.014(3) -0.073(4) O13 0.094(4) 0.085(4) 0.059(3) -0.024(3) 0.026(3) -0.068(3) O14 0.052(3) 0.067(3) 0.042(3) 0.007(2) -0.006(2) -0.022(2) N1 0.0215(19) 0.019(2) 0.018(2) 0.0011(16) -0.0030(16) -0.0072(16) N2 0.0217(19) 0.017(2) 0.021(2) 0.0006(16) -0.0003(16) -0.0093(16) C1 0.024(2) 0.022(3) 0.020(2) 0.001(2) -0.0006(19) -0.014(2) C3 0.024(2) 0.022(2) 0.018(2) 0.0023(19) -0.0009(19) -0.012(2) C4 0.027(2) 0.022(3) 0.020(2) 0.000(2) -0.001(2) -0.014(2) C5 0.033(3) 0.019(2) 0.017(2) 0.002(2) -0.007(2) -0.012(2) C6 0.031(3) 0.031(3) 0.020(3) 0.000(2) -0.002(2) -0.015(2) C7 0.018(2) 0.021(2) 0.020(2) -0.0022(19) 0.0000(18) -0.0083(19) C8 0.033(3) 0.032(3) 0.015(2) -0.001(2) 0.004(2) -0.016(2) C9 0.026(3) 0.030(3) 0.027(3) -0.008(2) 0.011(2) -0.011(2) C10 0.024(2) 0.019(3) 0.031(3) 0.001(2) 0.002(2) -0.006(2) C11 0.043(3) 0.035(3) 0.021(3) 0.009(2) -0.005(2) -0.024(3) C12 0.048(3) 0.054(4) 0.023(3) -0.009(3) 0.001(3) -0.025(3) C13 0.049(3) 0.061(4) 0.035(3) -0.009(3) 0.000(3) -0.040(3) C14 0.046(3) 0.045(4) 0.024(3) 0.001(3) 0.005(2) -0.030(3) C15 0.033(3) 0.028(3) 0.036(3) 0.008(2) -0.009(2) -0.016(2) C16 0.074(4) 0.024(3) 0.023(3) -0.002(2) -0.006(3) -0.019(3) C17 0.044(3) 0.024(3) 0.027(3) 0.001(2) -0.004(2) -0.015(2) C18 0.047(3) 0.045(4) 0.018(3) 0.004(2) 0.003(2) -0.021(3) C19 0.089(5) 0.030(3) 0.042(4) 0.008(3) -0.036(4) -0.034(3) C20 0.053(4) 0.035(3) 0.054(4) 0.016(3) -0.031(3) -0.027(3) C21 0.043(3) 0.031(3) 0.033(3) -0.004(3) 0.013(3) -0.012(3) C22 0.026(2) 0.019(2) 0.020(2) 0.003(2) -0.006(2) -0.009(2) C23 0.020(2) 0.019(2) 0.020(2) -0.0014(19) 0.0029(19) -0.0091(19) C24 0.027(2) 0.020(2) 0.015(2) 0.0018(19) 0.0018(19) -0.009(2) C25 0.032(3) 0.020(3) 0.022(2) 0.004(2) -0.004(2) -0.014(2) C26 0.035(3) 0.024(3) 0.028(3) -0.005(2) 0.006(2) -0.017(2) C27 0.027(2) 0.026(3) 0.019(2) 0.002(2) -0.003(2) -0.014(2) C28 0.020(2) 0.021(2) 0.018(2) -0.0013(19) 0.0023(18) -0.0086(19) C31 0.058(4) 0.041(4) 0.033(3) 0.002(3) -0.007(3) -0.035(3) C32 0.041(3) 0.056(4) 0.050(4) 0.002(4) 0.006(3) -0.013(3) C33 0.063(5) 0.104(7) 0.045(4) 0.005(4) -0.005(4) -0.036(5) C34 0.056(4) 0.047(4) 0.053(4) -0.004(3) 0.009(3) -0.022(3) C40 0.035(3) 0.028(3) 0.020(3) 0.001(2) 0.000(2) -0.016(2) C54 0.077(6) 0.090(7) 0.077(6) -0.027(5) 0.019(5) -0.050(5) C55 0.097(6) 0.088(6) 0.050(4) -0.013(4) 0.018(4) -0.069(5) C82 0.053(4) 0.044(4) 0.066(5) -0.011(4) 0.006(4) -0.021(3) C83 0.090(6) 0.039(4) 0.061(5) -0.004(4) 0.016(4) -0.017(4) C84 0.074(6) 0.040(5) 0.140(9) -0.002(5) 0.058(6) -0.015(4) C85 0.059(5) 0.130(8) 0.035(4) -0.013(5) 0.012(3) -0.041(5) _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 9.3559 (0.0094) x + 9.5026 (0.0132) y + 0.9056 (0.0356) z = 11.4726 (0.0172) * -0.0091 (0.0031) C1 * 0.0094 (0.0031) C7 * -0.0010 (0.0032) C4 * -0.0075 (0.0033) C8 * 0.0077 (0.0034) C9 * 0.0006 (0.0033) C10 Rms deviation of fitted atoms = 0.0069 - 6.9571 (0.0158) x + 2.2378 (0.0232) y + 10.9153 (0.0305) z = 1.7878 (0.0196) Angle to previous plane (with approximate esd) = 70.80 ( 0.13 ) * -0.0057 (0.0033) C23 * 0.0094 (0.0034) C24 * -0.0029 (0.0036) C40 * -0.0072 (0.0036) C26 * 0.0109 (0.0035) C27 * -0.0044 (0.0033) C28 Rms deviation of fitted atoms = 0.0073 ; 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 Ag1 O13 2.339(5) . ? Ag1 O1B 2.361(19) . ? Ag1 N1 2.488(4) . ? Ag1 O14 2.495(4) . ? Ag1 O1A 2.634(7) . ? Ag1 S1 2.6514(14) . ? Ag2 O11 2.425(5) . ? Ag2 O20A 2.440(10) 2_675 ? Ag2 O22B 2.517(15) 2_675 ? Ag2 O12 2.543(5) . ? Ag2 S2 2.5702(13) . ? Ag2 N2 2.597(4) . ? S1 C6 1.779(5) . ? S1 C4 1.788(5) . ? S2 C28 1.775(5) . ? S2 C5 1.785(4) . ? Cl20 O21B 1.380(18) . ? Cl20 O21A 1.383(10) . ? Cl20 O12 1.400(4) . ? Cl20 O22A 1.418(10) . ? Cl20 O20B 1.440(15) . ? Cl20 O22B 1.441(14) . ? Cl20 O20A 1.465(10) . ? Cl1A O2A 1.404(9) . ? Cl1A O3A 1.424(8) . ? Cl1A O4A 1.432(8) . ? Cl1A O1A 1.488(10) . ? Cl1B O1B 1.38(3) . ? Cl1B O3B 1.40(3) . ? Cl1B O2B 1.42(3) . ? Cl1B O4B 1.61(2) . ? O11 C85 1.400(8) . ? O11 C82 1.467(8) . ? O13 C54 1.369(8) . ? O13 C55 1.470(8) . ? O14 C32 1.224(8) . ? O20A Ag2 2.440(10) 2_675 ? O22B Ag2 2.517(15) 2_675 ? N1 C7 1.446(6) . ? N1 C3 1.468(6) . ? N1 C25 1.480(6) . ? N2 C23 1.450(6) . ? N2 C3 1.471(6) . ? N2 C22 1.481(6) . ? C1 C7 1.390(6) . ? C1 C10 1.392(7) . ? C1 C22 1.518(6) . ? C4 C8 1.393(7) . ? C4 C7 1.408(6) . ? C5 C17 1.384(7) . ? C5 C15 1.392(7) . ? C6 C11 1.381(7) . ? C6 C14 1.386(7) . ? C8 C9 1.392(7) . ? C9 C10 1.395(7) . ? C9 C21 1.503(7) . ? C11 C18 1.399(7) . ? C12 C13 1.376(8) . ? C12 C18 1.385(8) . ? C13 C14 1.374(7) . ? C15 C20 1.396(7) . ? C16 C19 1.383(9) . ? C16 C17 1.390(7) . ? C19 C20 1.379(10) . ? C23 C24 1.385(6) . ? C23 C28 1.407(6) . ? C24 C40 1.393(7) . ? C24 C25 1.517(6) . ? C26 C27 1.388(7) . ? C26 C40 1.389(7) . ? C26 C31 1.524(7) . ? C27 C28 1.395(6) . ? C32 C33 1.467(9) . ? C32 C34 1.502(9) . ? C54 C57B 1.446(18) . ? C54 C57A 1.619(18) . ? C55 C56A 1.448(16) . ? C55 C56B 1.58(2) . ? C82 C83 1.451(10) . ? C83 C84 1.573(12) . ? C84 C85 1.473(11) . ? C56A C57A 1.46(3) . ? C57B C56B 1.57(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 O13 Ag1 O1B 114.5(5) . . ? O13 Ag1 N1 100.62(17) . . ? O1B Ag1 N1 103.7(5) . . ? O13 Ag1 O14 90.43(17) . . ? O1B Ag1 O14 86.0(5) . . ? N1 Ag1 O14 160.38(14) . . ? O13 Ag1 O1A 120.4(2) . . ? O1B Ag1 O1A 7.8(5) . . ? N1 Ag1 O1A 97.07(18) . . ? O14 Ag1 O1A 91.10(19) . . ? O13 Ag1 S1 136.37(14) . . ? O1B Ag1 S1 109.0(5) . . ? N1 Ag1 S1 71.13(9) . . ? O14 Ag1 S1 89.67(11) . . ? O1A Ag1 S1 103.26(16) . . ? O11 Ag2 O20A 75.4(3) . 2_675 ? O11 Ag2 O22B 116.5(3) . 2_675 ? O20A Ag2 O22B 41.0(4) 2_675 2_675 ? O11 Ag2 O12 103.25(17) . . ? O20A Ag2 O12 102.4(3) 2_675 . ? O22B Ag2 O12 92.3(3) 2_675 . ? O11 Ag2 S2 115.78(12) . . ? O20A Ag2 S2 127.8(2) 2_675 . ? O22B Ag2 S2 105.9(3) 2_675 . ? O12 Ag2 S2 121.46(12) . . ? O11 Ag2 N2 79.79(14) . . ? O20A Ag2 N2 154.6(2) 2_675 . ? O22B Ag2 N2 162.7(3) 2_675 . ? O12 Ag2 N2 77.59(13) . . ? S2 Ag2 N2 69.06(8) . . ? C6 S1 C4 102.8(2) . . ? C6 S1 Ag1 112.56(17) . . ? C4 S1 Ag1 96.31(16) . . ? C28 S2 C5 104.4(2) . . ? C28 S2 Ag2 96.81(15) . . ? C5 S2 Ag2 116.71(17) . . ? O21B Cl20 O21A 122.8(8) . . ? O21B Cl20 O12 119.4(7) . . ? O21A Cl20 O12 116.6(5) . . ? O21B Cl20 O22A 58.6(8) . . ? O21A Cl20 O22A 112.4(6) . . ? O12 Cl20 O22A 108.6(5) . . ? O21B Cl20 O20B 99.9(10) . . ? O21A Cl20 O20B 71.7(8) . . ? O12 Cl20 O20B 108.7(7) . . ? O22A Cl20 O20B 47.0(7) . . ? O21B Cl20 O22B 105.9(9) . . ? O21A Cl20 O22B 38.4(6) . . ? O12 Cl20 O22B 113.2(6) . . ? O22A Cl20 O22B 137.3(7) . . ? O20B Cl20 O22B 108.7(8) . . ? O21B Cl20 O20A 46.5(7) . . ? O21A Cl20 O20A 109.1(6) . . ? O12 Cl20 O20A 104.1(4) . . ? O22A Cl20 O20A 105.0(6) . . ? O20B Cl20 O20A 142.3(8) . . ? O22B Cl20 O20A 73.5(7) . . ? O2A Cl1A O3A 114.1(5) . . ? O2A Cl1A O4A 109.3(6) . . ? O3A Cl1A O4A 110.4(5) . . ? O2A Cl1A O1A 105.8(5) . . ? O3A Cl1A O1A 106.8(6) . . ? O4A Cl1A O1A 110.2(5) . . ? O1B Cl1B O3B 114.6(18) . . ? O1B Cl1B O2B 109.1(16) . . ? O3B Cl1B O2B 108.4(19) . . ? O1B Cl1B O4B 107.2(16) . . ? O3B Cl1B O4B 109.3(17) . . ? O2B Cl1B O4B 108.0(16) . . ? C85 O11 C82 106.5(6) . . ? C85 O11 Ag2 123.5(5) . . ? C82 O11 Ag2 115.3(4) . . ? Cl20 O12 Ag2 118.5(3) . . ? C54 O13 C55 109.7(5) . . ? C54 O13 Ag1 119.4(5) . . ? C55 O13 Ag1 129.5(4) . . ? C32 O14 Ag1 125.5(4) . . ? Cl1A O1A Ag1 105.9(4) . . ? Cl20 O20A Ag2 119.3(5) . 2_675 ? Cl1B O1B Ag1 125.1(14) . . ? Cl20 O22B Ag2 116.1(8) . 2_675 ? C7 N1 C3 110.1(4) . . ? C7 N1 C25 113.0(4) . . ? C3 N1 C25 108.5(4) . . ? C7 N1 Ag1 110.1(3) . . ? C3 N1 Ag1 110.2(3) . . ? C25 N1 Ag1 104.7(3) . . ? C23 N2 C3 110.5(4) . . ? C23 N2 C22 114.2(4) . . ? C3 N2 C22 108.3(3) . . ? C23 N2 Ag2 105.4(3) . . ? C3 N2 Ag2 109.6(3) . . ? C22 N2 Ag2 108.8(3) . . ? C7 C1 C10 120.3(4) . . ? C7 C1 C22 120.7(4) . . ? C10 C1 C22 118.9(4) . . ? N1 C3 N2 111.3(4) . . ? C8 C4 C7 120.4(4) . . ? C8 C4 S1 121.1(4) . . ? C7 C4 S1 118.5(4) . . ? C17 C5 C15 121.5(5) . . ? C17 C5 S2 119.6(4) . . ? C15 C5 S2 118.8(4) . . ? C11 C6 C14 120.1(5) . . ? C11 C6 S1 118.9(4) . . ? C14 C6 S1 121.0(4) . . ? C1 C7 C4 118.6(4) . . ? C1 C7 N1 121.8(4) . . ? C4 C7 N1 119.6(4) . . ? C9 C8 C4 121.1(4) . . ? C8 C9 C10 117.9(5) . . ? C8 C9 C21 121.4(5) . . ? C10 C9 C21 120.6(5) . . ? C1 C10 C9 121.6(5) . . ? C6 C11 C18 119.5(5) . . ? C13 C12 C18 119.3(5) . . ? C14 C13 C12 121.1(5) . . ? C13 C14 C6 119.8(5) . . ? C5 C15 C20 118.4(6) . . ? C19 C16 C17 120.0(6) . . ? C5 C17 C16 119.1(5) . . ? C12 C18 C11 120.2(5) . . ? C20 C19 C16 120.6(5) . . ? C19 C20 C15 120.4(6) . . ? N2 C22 C1 112.4(4) . . ? C24 C23 C28 119.6(4) . . ? C24 C23 N2 121.2(4) . . ? C28 C23 N2 119.1(4) . . ? C23 C24 C40 120.0(4) . . ? C23 C24 C25 121.0(4) . . ? C40 C24 C25 118.9(4) . . ? N1 C25 C24 113.0(4) . . ? C27 C26 C40 119.4(4) . . ? C27 C26 C31 120.3(4) . . ? C40 C26 C31 120.3(5) . . ? C26 C27 C28 120.5(4) . . ? C27 C28 C23 119.7(4) . . ? C27 C28 S2 123.6(3) . . ? C23 C28 S2 116.6(3) . . ? O14 C32 C33 120.9(7) . . ? O14 C32 C34 122.5(6) . . ? C33 C32 C34 116.7(7) . . ? C26 C40 C24 120.8(5) . . ? O13 C54 C57B 110.0(9) . . ? O13 C54 C57A 103.7(8) . . ? C57B C54 C57A 29.0(8) . . ? C56A C55 O13 106.3(8) . . ? C56A C55 C56B 24.3(9) . . ? O13 C55 C56B 101.6(9) . . ? C83 C82 O11 105.1(6) . . ? C82 C83 C84 101.6(6) . . ? C85 C84 C83 102.2(6) . . ? O11 C85 C84 110.2(7) . . ? C55 C56A C57A 104.9(13) . . ? C54 C57B C56B 99.8(15) . . ? C56A C57A C54 99.1(14) . . ? C57B C56B C55 97.9(16) . . ? 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 O13 Ag1 S1 C6 -56.8(3) . . . . ? O1B Ag1 S1 C6 119.1(5) . . . . ? N1 Ag1 S1 C6 -142.4(2) . . . . ? O14 Ag1 S1 C6 33.5(2) . . . . ? O1A Ag1 S1 C6 124.5(2) . . . . ? O13 Ag1 S1 C4 49.9(2) . . . . ? O1B Ag1 S1 C4 -134.2(5) . . . . ? N1 Ag1 S1 C4 -35.69(17) . . . . ? O14 Ag1 S1 C4 140.21(19) . . . . ? O1A Ag1 S1 C4 -128.7(2) . . . . ? O11 Ag2 S2 C28 24.7(2) . . . . ? O20A Ag2 S2 C28 115.9(3) 2_675 . . . ? O22B Ag2 S2 C28 155.4(4) 2_675 . . . ? O12 Ag2 S2 C28 -101.8(2) . . . . ? N2 Ag2 S2 C28 -42.02(18) . . . . ? O11 Ag2 S2 C5 -85.2(2) . . . . ? O20A Ag2 S2 C5 6.0(4) 2_675 . . . ? O22B Ag2 S2 C5 45.5(4) 2_675 . . . ? O12 Ag2 S2 C5 148.4(2) . . . . ? N2 Ag2 S2 C5 -151.9(2) . . . . ? O20A Ag2 O11 C85 44.1(5) 2_675 . . . ? O22B Ag2 O11 C85 44.0(6) 2_675 . . . ? O12 Ag2 O11 C85 -55.4(5) . . . . ? S2 Ag2 O11 C85 169.4(4) . . . . ? N2 Ag2 O11 C85 -130.0(5) . . . . ? O20A Ag2 O11 C82 -89.5(5) 2_675 . . . ? O22B Ag2 O11 C82 -89.7(6) 2_675 . . . ? O12 Ag2 O11 C82 170.9(4) . . . . ? S2 Ag2 O11 C82 35.8(4) . . . . ? N2 Ag2 O11 C82 96.4(4) . . . . ? O21B Cl20 O12 Ag2 109.3(9) . . . . ? O21A Cl20 O12 Ag2 -58.7(6) . . . . ? O22A Cl20 O12 Ag2 173.1(5) . . . . ? O20B Cl20 O12 Ag2 -137.2(8) . . . . ? O22B Cl20 O12 Ag2 -16.3(8) . . . . ? O20A Cl20 O12 Ag2 61.5(5) . . . . ? O11 Ag2 O12 Cl20 77.5(4) . . . . ? O20A Ag2 O12 Cl20 -0.2(4) 2_675 . . . ? O22B Ag2 O12 Cl20 -40.4(5) 2_675 . . . ? S2 Ag2 O12 Cl20 -150.5(3) . . . . ? N2 Ag2 O12 Cl20 153.8(4) . . . . ? O1B Ag1 O13 C54 -126.2(8) . . . . ? N1 Ag1 O13 C54 123.3(6) . . . . ? O14 Ag1 O13 C54 -40.4(6) . . . . ? O1A Ag1 O13 C54 -132.0(6) . . . . ? S1 Ag1 O13 C54 49.5(7) . . . . ? O1B Ag1 O13 C55 38.7(9) . . . . ? N1 Ag1 O13 C55 -71.8(7) . . . . ? O14 Ag1 O13 C55 124.5(7) . . . . ? O1A Ag1 O13 C55 32.9(7) . . . . ? S1 Ag1 O13 C55 -145.6(6) . . . . ? O13 Ag1 O14 C32 -178.2(6) . . . . ? O1B Ag1 O14 C32 -63.7(7) . . . . ? N1 Ag1 O14 C32 57.0(8) . . . . ? O1A Ag1 O14 C32 -57.8(6) . . . . ? S1 Ag1 O14 C32 45.4(6) . . . . ? O2A Cl1A O1A Ag1 10.6(6) . . . . ? O3A Cl1A O1A Ag1 -111.4(4) . . . . ? O4A Cl1A O1A Ag1 128.7(4) . . . . ? O13 Ag1 O1A Cl1A -37.6(5) . . . . ? O1B Ag1 O1A Cl1A -80(4) . . . . ? N1 Ag1 O1A Cl1A 69.1(4) . . . . ? O14 Ag1 O1A Cl1A -128.8(4) . . . . ? S1 Ag1 O1A Cl1A 141.3(4) . . . . ? O21B Cl20 O20A Ag2 103.8(12) . . . 2_675 ? O21A Cl20 O20A Ag2 -13.7(8) . . . 2_675 ? O12 Cl20 O20A Ag2 -138.9(5) . . . 2_675 ? O22A Cl20 O20A Ag2 107.0(6) . . . 2_675 ? O20B Cl20 O20A Ag2 70.9(13) . . . 2_675 ? O22B Cl20 O20A Ag2 -28.5(7) . . . 2_675 ? O3B Cl1B O1B Ag1 -128.7(17) . . . . ? O2B Cl1B O1B Ag1 109.5(17) . . . . ? O4B Cl1B O1B Ag1 -7(2) . . . . ? O13 Ag1 O1B Cl1B -46.9(17) . . . . ? N1 Ag1 O1B Cl1B 61.8(16) . . . . ? O14 Ag1 O1B Cl1B -135.5(16) . . . . ? O1A Ag1 O1B Cl1B 93(5) . . . . ? S1 Ag1 O1B Cl1B 136.3(15) . . . . ? O21B Cl20 O22B Ag2 -7.2(11) . . . 2_675 ? O21A Cl20 O22B Ag2 -130.5(15) . . . 2_675 ? O12 Cl20 O22B Ag2 125.3(6) . . . 2_675 ? O22A Cl20 O22B Ag2 -67.8(13) . . . 2_675 ? O20B Cl20 O22B Ag2 -113.8(9) . . . 2_675 ? O20A Cl20 O22B Ag2 26.7(6) . . . 2_675 ? O13 Ag1 N1 C7 -93.8(3) . . . . ? O1B Ag1 N1 C7 147.5(6) . . . . ? O14 Ag1 N1 C7 29.5(6) . . . . ? O1A Ag1 N1 C7 143.4(3) . . . . ? S1 Ag1 N1 C7 41.8(3) . . . . ? O13 Ag1 N1 C3 27.8(3) . . . . ? O1B Ag1 N1 C3 -90.9(6) . . . . ? O14 Ag1 N1 C3 151.1(4) . . . . ? O1A Ag1 N1 C3 -95.0(3) . . . . ? S1 Ag1 N1 C3 163.4(3) . . . . ? O13 Ag1 N1 C25 144.4(3) . . . . ? O1B Ag1 N1 C25 25.7(6) . . . . ? O14 Ag1 N1 C25 -92.4(5) . . . . ? O1A Ag1 N1 C25 21.6(3) . . . . ? S1 Ag1 N1 C25 -80.1(3) . . . . ? O11 Ag2 N2 C23 -76.2(3) . . . . ? O20A Ag2 N2 C23 -89.5(6) 2_675 . . . ? O22B Ag2 N2 C23 122.5(11) 2_675 . . . ? O12 Ag2 N2 C23 177.7(3) . . . . ? S2 Ag2 N2 C23 46.7(2) . . . . ? O11 Ag2 N2 C3 42.8(3) . . . . ? O20A Ag2 N2 C3 29.4(7) 2_675 . . . ? O22B Ag2 N2 C3 -118.6(11) 2_675 . . . ? O12 Ag2 N2 C3 -63.4(3) . . . . ? S2 Ag2 N2 C3 165.6(3) . . . . ? O11 Ag2 N2 C22 161.0(3) . . . . ? O20A Ag2 N2 C22 147.6(6) 2_675 . . . ? O22B Ag2 N2 C22 -0.4(12) 2_675 . . . ? O12 Ag2 N2 C22 54.8(3) . . . . ? S2 Ag2 N2 C22 -76.2(3) . . . . ? C7 N1 C3 N2 -56.1(5) . . . . ? C25 N1 C3 N2 68.1(5) . . . . ? Ag1 N1 C3 N2 -177.7(3) . . . . ? C23 N2 C3 N1 -56.4(5) . . . . ? C22 N2 C3 N1 69.3(5) . . . . ? Ag2 N2 C3 N1 -172.1(3) . . . . ? C6 S1 C4 C8 -29.5(4) . . . . ? Ag1 S1 C4 C8 -144.4(4) . . . . ? C6 S1 C4 C7 150.6(4) . . . . ? Ag1 S1 C4 C7 35.7(4) . . . . ? C28 S2 C5 C17 -104.4(4) . . . . ? Ag2 S2 C5 C17 1.0(5) . . . . ? C28 S2 C5 C15 79.7(4) . . . . ? Ag2 S2 C5 C15 -174.8(3) . . . . ? C4 S1 C6 C11 109.3(4) . . . . ? Ag1 S1 C6 C11 -148.2(4) . . . . ? C4 S1 C6 C14 -72.8(5) . . . . ? Ag1 S1 C6 C14 29.7(5) . . . . ? C10 C1 C7 C4 1.8(7) . . . . ? C22 C1 C7 C4 179.2(4) . . . . ? C10 C1 C7 N1 -175.6(4) . . . . ? C22 C1 C7 N1 1.8(6) . . . . ? C8 C4 C7 C1 -1.0(7) . . . . ? S1 C4 C7 C1 178.9(3) . . . . ? C8 C4 C7 N1 176.5(4) . . . . ? S1 C4 C7 N1 -3.6(6) . . . . ? C3 N1 C7 C1 20.2(5) . . . . ? C25 N1 C7 C1 -101.3(5) . . . . ? Ag1 N1 C7 C1 141.9(4) . . . . ? C3 N1 C7 C4 -157.2(4) . . . . ? C25 N1 C7 C4 81.3(5) . . . . ? Ag1 N1 C7 C4 -35.5(5) . . . . ? C7 C4 C8 C9 -0.6(7) . . . . ? S1 C4 C8 C9 179.5(4) . . . . ? C4 C8 C9 C10 1.4(7) . . . . ? C4 C8 C9 C21 -177.8(5) . . . . ? C7 C1 C10 C9 -1.0(7) . . . . ? C22 C1 C10 C9 -178.5(4) . . . . ? C8 C9 C10 C1 -0.6(7) . . . . ? C21 C9 C10 C1 178.5(5) . . . . ? C14 C6 C11 C18 -1.1(8) . . . . ? S1 C6 C11 C18 176.8(4) . . . . ? C18 C12 C13 C14 -0.9(10) . . . . ? C12 C13 C14 C6 0.4(10) . . . . ? C11 C6 C14 C13 0.6(9) . . . . ? S1 C6 C14 C13 -177.3(5) . . . . ? C17 C5 C15 C20 1.8(8) . . . . ? S2 C5 C15 C20 177.5(4) . . . . ? C15 C5 C17 C16 -0.3(8) . . . . ? S2 C5 C17 C16 -176.0(4) . . . . ? C19 C16 C17 C5 -1.7(8) . . . . ? C13 C12 C18 C11 0.3(9) . . . . ? C6 C11 C18 C12 0.7(9) . . . . ? C17 C16 C19 C20 2.2(9) . . . . ? C16 C19 C20 C15 -0.6(9) . . . . ? C5 C15 C20 C19 -1.3(8) . . . . ? C23 N2 C22 C1 79.9(5) . . . . ? C3 N2 C22 C1 -43.6(5) . . . . ? Ag2 N2 C22 C1 -162.6(3) . . . . ? C7 C1 C22 N2 10.5(6) . . . . ? C10 C1 C22 N2 -172.1(4) . . . . ? C3 N2 C23 C24 20.5(6) . . . . ? C22 N2 C23 C24 -101.9(5) . . . . ? Ag2 N2 C23 C24 138.8(4) . . . . ? C3 N2 C23 C28 -155.3(4) . . . . ? C22 N2 C23 C28 82.4(5) . . . . ? Ag2 N2 C23 C28 -36.9(5) . . . . ? C28 C23 C24 C40 1.4(7) . . . . ? N2 C23 C24 C40 -174.3(4) . . . . ? C28 C23 C24 C25 178.5(4) . . . . ? N2 C23 C24 C25 2.7(7) . . . . ? C7 N1 C25 C24 80.7(5) . . . . ? C3 N1 C25 C24 -41.7(5) . . . . ? Ag1 N1 C25 C24 -159.4(3) . . . . ? C23 C24 C25 N1 8.4(7) . . . . ? C40 C24 C25 N1 -174.5(4) . . . . ? C40 C26 C27 C28 1.8(8) . . . . ? C31 C26 C27 C28 -177.6(5) . . . . ? C26 C27 C28 C23 -1.5(7) . . . . ? C26 C27 C28 S2 -179.9(4) . . . . ? C24 C23 C28 C27 -0.1(7) . . . . ? N2 C23 C28 C27 175.7(4) . . . . ? C24 C23 C28 S2 178.4(4) . . . . ? N2 C23 C28 S2 -5.8(6) . . . . ? C5 S2 C28 C27 -17.4(5) . . . . ? Ag2 S2 C28 C27 -137.3(4) . . . . ? C5 S2 C28 C23 164.2(4) . . . . ? Ag2 S2 C28 C23 44.3(4) . . . . ? Ag1 O14 C32 C33 -153.1(5) . . . . ? Ag1 O14 C32 C34 25.4(9) . . . . ? C27 C26 C40 C24 -0.5(8) . . . . ? C31 C26 C40 C24 179.0(5) . . . . ? C23 C24 C40 C26 -1.1(8) . . . . ? C25 C24 C40 C26 -178.3(5) . . . . ? C55 O13 C54 C57B -11.5(14) . . . . ? Ag1 O13 C54 C57B 156.2(12) . . . . ? C55 O13 C54 C57A 18.1(12) . . . . ? Ag1 O13 C54 C57A -174.2(9) . . . . ? C54 O13 C55 C56A 6.1(13) . . . . ? Ag1 O13 C55 C56A -159.9(10) . . . . ? C54 O13 C55 C56B -18.4(14) . . . . ? Ag1 O13 C55 C56B 175.5(12) . . . . ? C85 O11 C82 C83 -32.7(7) . . . . ? Ag2 O11 C82 C83 108.3(5) . . . . ? O11 C82 C83 C84 37.9(7) . . . . ? C82 C83 C84 C85 -29.8(8) . . . . ? C82 O11 C85 C84 12.3(9) . . . . ? Ag2 O11 C85 C84 -124.6(7) . . . . ? C83 C84 C85 O11 10.8(9) . . . . ? O13 C55 C56A C57A -31(2) . . . . ? C56B C55 C56A C57A 51(3) . . . . ? O13 C54 C57B C56B 36(2) . . . . ? C57A C54 C57B C56B -46(2) . . . . ? C55 C56A C57A C54 39(2) . . . . ? O13 C54 C57A C56A -35.5(18) . . . . ? C57B C54 C57A C56A 71(2) . . . . ? C54 C57B C56B C55 -44(2) . . . . ? C56A C55 C56B C57B -66(3) . . . . ? O13 C55 C56B C57B 37.8(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.207 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.125 # Attachment '- 3c.cif' data_NIS823 _database_code_depnum_ccdc_archive 'CCDC 865872' #TrackingRef '- 3c.cif' # This structure was measured, # solved and refined by: # Elli Maennel _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point 'not measured' _chemical_properties_physical 'light sensitive' _chemical_formula_moiety 'C62 H58 Ag2 N6 Se4,2(Cl O4),0.38(C4 H8 O), 0.62(C2 H3 N)' _chemical_formula_sum 'C64.76 H62.90 Ag2 Cl2 N6.62 O8.38 Se4' _chemical_formula_weight 1670.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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_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 13.9683(3) _cell_length_b 21.6538(4) _cell_length_c 21.3918(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.7900(10) _cell_angle_gamma 90.00 _cell_volume 6447.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.61 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3524 _exptl_absorpt_coefficient_mu 3.016 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5326 _exptl_absorpt_correction_T_max 0.7504 _exptl_absorpt_process_details SADABS-2004/1 _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77242 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.70 _reflns_number_total 16635 _reflns_number_gt 11450 _reflns_threshold_expression >2sigma(I) _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^)+(0.0408P)^2^+19.6243P] 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 'not measured' _refine_ls_number_reflns 16635 _refine_ls_number_parameters 947 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.37137(2) 0.382952(17) 0.254320(16) 0.03925(9) Uani 1 1 d . . . Ag2 Ag 0.85880(3) 0.410470(18) 0.247689(17) 0.04469(10) Uani 1 1 d . . . Se1 Se 0.32908(3) 0.47148(2) 0.34025(2) 0.03642(11) Uani 1 1 d . . . Se2 Se 0.42714(3) 0.38391(2) 0.13655(2) 0.04302(12) Uani 1 1 d . A . Se3 Se -0.15533(3) 0.41057(3) 0.12541(2) 0.04958(14) Uani 1 1 d . . . Se4 Se 0.90204(3) 0.48751(2) 0.33998(2) 0.03967(11) Uani 1 1 d . . . Cl1 Cl 0.38385(8) 0.60577(6) 0.14954(6) 0.0442(3) Uani 1 1 d . . . Cl2 Cl 0.13781(9) 0.70180(6) 0.51719(5) 0.0440(3) Uani 1 1 d . . . O1 O 0.3318(3) 0.63204(18) 0.09565(18) 0.0604(10) Uani 1 1 d . . . O2 O 0.3265(3) 0.6041(2) 0.2016(2) 0.0788(13) Uani 1 1 d . . . O3 O 0.4103(3) 0.54318(17) 0.13590(18) 0.0552(9) Uani 1 1 d . . . O4 O 0.4674(3) 0.64150(18) 0.1671(2) 0.0642(11) Uani 1 1 d . . . N1 N 0.2233(2) 0.39292(16) 0.17964(15) 0.0302(7) Uani 1 1 d . . . N2 N 0.0493(3) 0.38394(17) 0.17062(15) 0.0343(8) Uani 1 1 d . . . N3 N 0.5263(2) 0.44501(15) 0.29788(14) 0.0252(7) Uani 1 1 d . . . N4 N 0.7004(2) 0.44048(15) 0.30833(14) 0.0254(7) Uani 1 1 d . . . N5 N 0.4253(3) 0.30440(19) 0.3215(2) 0.0485(10) Uani 1 1 d . . . N6 N 0.8507(5) 0.3121(3) 0.2787(3) 0.0761(16) Uani 1 1 d . . . C1 C 0.0440(3) 0.43988(19) 0.13410(17) 0.0278(8) Uani 1 1 d . . . C2 C 0.1244(3) 0.47611(18) 0.12624(17) 0.0248(8) Uani 1 1 d . . . C3 C 0.1150(3) 0.53174(19) 0.09366(17) 0.0286(8) Uani 1 1 d . . . H3 H 0.1704 0.5562 0.0890 0.034 Uiso 1 1 calc R . . C4 C 0.0261(3) 0.5520(2) 0.06791(18) 0.0335(9) Uani 1 1 d . . . C5 C -0.0544(3) 0.5155(2) 0.07643(19) 0.0354(10) Uani 1 1 d . . . H5 H -0.1159 0.5285 0.0590 0.043 Uiso 1 1 calc R . . C6 C -0.0461(3) 0.4615(2) 0.10940(18) 0.0327(9) Uani 1 1 d . . . C7 C 0.0171(4) 0.6125(2) 0.0324(2) 0.0505(13) Uani 1 1 d . . . H7A H 0.0151 0.6467 0.0622 0.076 Uiso 1 1 calc R . . H7B H -0.0421 0.6123 0.0044 0.076 Uiso 1 1 calc R . . H7C H 0.0725 0.6176 0.0076 0.076 Uiso 1 1 calc R . . C8 C 0.2221(3) 0.45714(18) 0.15604(19) 0.0290(8) Uani 1 1 d . . . H8A H 0.2700 0.4613 0.1247 0.035 Uiso 1 1 calc R . . H8B H 0.2411 0.4854 0.1913 0.035 Uiso 1 1 calc R . . C9 C 0.1358(3) 0.3838(2) 0.21321(19) 0.0355(9) Uani 1 1 d . . . H9A H 0.1407 0.3439 0.2360 0.043 Uiso 1 1 calc R . . H9B H 0.1316 0.4171 0.2446 0.043 Uiso 1 1 calc R . . C10 C 0.0497(3) 0.3271(2) 0.1315(2) 0.0420(11) Uani 1 1 d . A . H10A H 0.0008 0.3312 0.0955 0.050 Uiso 1 1 calc R . . H10B H 0.0319 0.2913 0.1568 0.050 Uiso 1 1 calc R . . C11 C 0.2277(3) 0.3483(2) 0.1301(2) 0.0374(10) Uani 1 1 d . A . C12 C 0.3160(4) 0.3373(2) 0.1054(2) 0.0476(13) Uani 1 1 d . . . C13A C 0.3251(8) 0.2953(7) 0.0568(7) 0.062(3) Uani 0.81(3) 1 d P A 1 H13A H 0.3851 0.2901 0.0395 0.074 Uiso 0.81(3) 1 calc PR A 1 C14A C 0.2459(9) 0.2612(8) 0.0340(9) 0.082(5) Uani 0.81(3) 1 d P A 1 C15A C 0.1578(10) 0.2723(7) 0.0583(8) 0.063(3) Uani 0.81(3) 1 d P A 1 H15A H 0.1030 0.2501 0.0414 0.075 Uiso 0.81(3) 1 calc PR A 1 C17A C 0.2582(9) 0.2102(11) -0.0144(12) 0.148(10) Uani 0.81(3) 1 d P A 1 H17A H 0.3258 0.2078 -0.0232 0.222 Uiso 0.81(3) 1 calc PR A 1 H17B H 0.2186 0.2198 -0.0531 0.222 Uiso 0.81(3) 1 calc PR A 1 H17C H 0.2380 0.1706 0.0023 0.222 Uiso 0.81(3) 1 calc PR A 1 C13B C 0.311(3) 0.2785(17) 0.0746(16) 0.025(7) Uani 0.19(3) 1 d PU A 2 H13B H 0.3704 0.2612 0.0650 0.031 Uiso 0.19(3) 1 calc PR A 2 C14B C 0.231(3) 0.2445(18) 0.0572(15) 0.034(8) Uani 0.19(3) 1 d P A 2 C15B C 0.147(3) 0.260(2) 0.0793(16) 0.033(8) Uani 0.19(3) 1 d P A 2 H15B H 0.0923 0.2334 0.0755 0.040 Uiso 0.19(3) 1 calc PR A 2 C17B C 0.243(2) 0.1855(14) 0.0202(16) 0.040(9) Uani 0.19(3) 1 d PU A 2 H17D H 0.2601 0.1515 0.0492 0.060 Uiso 0.19(3) 1 calc PR A 2 H17E H 0.2934 0.1912 -0.0082 0.060 Uiso 0.19(3) 1 calc PR A 2 H17F H 0.1821 0.1757 -0.0042 0.060 Uiso 0.19(3) 1 calc PR A 2 C16 C 0.1464(4) 0.3153(2) 0.1073(2) 0.0476(12) Uani 1 1 d . . . C18 C -0.2554(3) 0.4683(3) 0.0973(2) 0.0594(17) Uani 1 1 d . . . C19 C -0.2946(4) 0.4651(4) 0.0352(2) 0.079(2) Uani 1 1 d . . . H19 H -0.2729 0.4349 0.0075 0.095 Uiso 1 1 calc R . . C20 C -0.3659(4) 0.5068(5) 0.0144(3) 0.098(3) Uani 1 1 d . . . H20 H -0.3930 0.5052 -0.0278 0.117 Uiso 1 1 calc R . . C21 C -0.3974(4) 0.5506(5) 0.0547(3) 0.094(3) Uani 1 1 d . . . H21 H -0.4456 0.5793 0.0399 0.113 Uiso 1 1 calc R . . C22 C -0.3593(4) 0.5532(4) 0.1169(3) 0.077(2) Uani 1 1 d . . . H22 H -0.3819 0.5829 0.1448 0.092 Uiso 1 1 calc R . . C23 C -0.2878(3) 0.5116(3) 0.1375(2) 0.0601(17) Uani 1 1 d . . . H23 H -0.2610 0.5132 0.1797 0.072 Uiso 1 1 calc R . . C24 C 0.5252(4) 0.3222(3) 0.1296(2) 0.0528(14) Uani 1 1 d . . . C25 C 0.5829(4) 0.3275(3) 0.0800(3) 0.0594(15) Uani 1 1 d . A . H25 H 0.5719 0.3596 0.0499 0.071 Uiso 1 1 calc R . . C26 C 0.6566(4) 0.2855(3) 0.0749(3) 0.0710(19) Uani 1 1 d . . . H26 H 0.6963 0.2886 0.0411 0.085 Uiso 1 1 calc R A . C27 C 0.6722(5) 0.2396(4) 0.1184(3) 0.083(2) Uani 1 1 d . A . H27 H 0.7230 0.2110 0.1147 0.099 Uiso 1 1 calc R . . C28 C 0.6144(5) 0.2343(3) 0.1678(3) 0.076(2) Uani 1 1 d . . . H28 H 0.6253 0.2018 0.1974 0.091 Uiso 1 1 calc R A . C29 C 0.5407(4) 0.2763(3) 0.1744(3) 0.0592(16) Uani 1 1 d . A . H29 H 0.5020 0.2737 0.2088 0.071 Uiso 1 1 calc R . . C30 C 0.4672(4) 0.2840(2) 0.3644(2) 0.0425(11) Uani 1 1 d . . . C31 C 0.5207(4) 0.2582(2) 0.4197(2) 0.0530(13) Uani 1 1 d . . . H31A H 0.5095 0.2833 0.4565 0.080 Uiso 1 1 calc R . . H31B H 0.5894 0.2580 0.4136 0.080 Uiso 1 1 calc R . . H31C H 0.4991 0.2158 0.4263 0.080 Uiso 1 1 calc R . . C32 C 0.5262(3) 0.43759(17) 0.36511(17) 0.0239(7) Uani 1 1 d . B . C33 C 0.4399(3) 0.44474(19) 0.39333(19) 0.0290(8) Uani 1 1 d . . . C34 C 0.4367(3) 0.43283(19) 0.45675(19) 0.0329(9) Uani 1 1 d . . . H34 H 0.3781 0.4385 0.4757 0.039 Uiso 1 1 calc R . . C35 C 0.5177(3) 0.41272(18) 0.49297(18) 0.0326(9) Uani 1 1 d . . . C36 C 0.6035(3) 0.40704(18) 0.46529(18) 0.0292(8) Uani 1 1 d . B . H36 H 0.6596 0.3939 0.4900 0.035 Uiso 1 1 calc R . . C37 C 0.6092(3) 0.42022(17) 0.40179(17) 0.0242(7) Uani 1 1 d . . . C38 C 0.5112(4) 0.3968(2) 0.5613(2) 0.0460(12) Uani 1 1 d . . . H38A H 0.4606 0.4215 0.5781 0.069 Uiso 1 1 calc R . . H38B H 0.5728 0.4056 0.5849 0.069 Uiso 1 1 calc R . . H38C H 0.4961 0.3528 0.5651 0.069 Uiso 1 1 calc R . . C39 C 0.7046(3) 0.41478(19) 0.37293(17) 0.0271(8) Uani 1 1 d . B . H39A H 0.7546 0.4369 0.3997 0.033 Uiso 1 1 calc R . . H39B H 0.7233 0.3707 0.3718 0.033 Uiso 1 1 calc R . . C40 C 0.6125(3) 0.41656(19) 0.27511(17) 0.0257(8) Uani 1 1 d . B . H40A H 0.6097 0.3713 0.2810 0.031 Uiso 1 1 calc R . . H40B H 0.6137 0.4249 0.2297 0.031 Uiso 1 1 calc R . . C41 C 0.5243(3) 0.51013(19) 0.27709(18) 0.0291(8) Uani 1 1 d . . . H41A H 0.4745 0.5327 0.2983 0.035 Uiso 1 1 calc R . . H41B H 0.5063 0.5117 0.2314 0.035 Uiso 1 1 calc R . . C42 C 0.7020(3) 0.50696(18) 0.30720(16) 0.0259(8) Uani 1 1 d . B . C43 C 0.7895(3) 0.5383(2) 0.31932(19) 0.0337(9) Uani 1 1 d . B . C44 C 0.7936(4) 0.6017(2) 0.3162(2) 0.0459(12) Uani 1 1 d . . . H44 H 0.8531 0.6222 0.3258 0.055 Uiso 1 1 calc R B . C45 C 0.7116(4) 0.6361(2) 0.2994(3) 0.0498(12) Uani 1 1 d . B . C46 C 0.6255(4) 0.6054(2) 0.2870(2) 0.0402(10) Uani 1 1 d . . . H46 H 0.5690 0.6285 0.2753 0.048 Uiso 1 1 calc R B . C47 C 0.6195(3) 0.54160(19) 0.29112(17) 0.0290(8) Uani 1 1 d . B . C48 C 0.7148(6) 0.7059(3) 0.2954(4) 0.088(2) Uani 1 1 d . . . H48A H 0.6780 0.7196 0.2569 0.132 Uiso 1 1 calc R B . H48B H 0.7816 0.7196 0.2949 0.132 Uiso 1 1 calc R . . H48C H 0.6868 0.7238 0.3318 0.132 Uiso 1 1 calc R . . C49 C 0.2276(3) 0.4506(3) 0.3914(2) 0.0478(13) Uani 1 1 d . . . C50 C 0.1711(3) 0.3993(2) 0.3775(2) 0.0386(10) Uani 1 1 d . . . H50 H 0.1866 0.3721 0.3450 0.046 Uiso 1 1 calc R . . C51 C 0.0917(3) 0.3873(3) 0.4107(2) 0.0513(13) Uani 1 1 d . . . H51 H 0.0516 0.3528 0.4002 0.062 Uiso 1 1 calc R . . C52 C 0.0721(4) 0.4261(4) 0.4591(3) 0.078(2) Uani 1 1 d . . . H52 H 0.0193 0.4175 0.4831 0.093 Uiso 1 1 calc R . . C53 C 0.1286(4) 0.4771(4) 0.4729(3) 0.100(3) Uani 1 1 d . . . H53 H 0.1144 0.5036 0.5063 0.120 Uiso 1 1 calc R . . C54 C 0.2061(4) 0.4906(4) 0.4387(3) 0.087(3) Uani 1 1 d . . . H54 H 0.2437 0.5265 0.4476 0.104 Uiso 1 1 calc R . . C55A C 0.9999(15) 0.5463(14) 0.3168(12) 0.037(5) Uani 0.63(3) 1 d P B 1 C56A C 1.0255(10) 0.5957(10) 0.3618(6) 0.049(4) Uani 0.63(3) 1 d P B 1 H56A H 0.9937 0.5996 0.3992 0.059 Uiso 0.63(3) 1 calc PR B 1 C57A C 1.0977(9) 0.6370(10) 0.3486(6) 0.056(4) Uani 0.63(3) 1 d P B 1 H57A H 1.1139 0.6708 0.3757 0.067 Uiso 0.63(3) 1 calc PR B 1 C58A C 1.1434(15) 0.6280(12) 0.2972(11) 0.072(7) Uani 0.63(3) 1 d P B 1 H58A H 1.1917 0.6566 0.2877 0.087 Uiso 0.63(3) 1 calc PR B 1 C59A C 1.1223(14) 0.5761(7) 0.2552(8) 0.029(3) Uani 0.63(3) 1 d P B 1 H59A H 1.1608 0.5686 0.2214 0.035 Uiso 0.63(3) 1 calc PR B 1 C60A C 1.0442(14) 0.5371(9) 0.2649(8) 0.022(3) Uani 0.63(3) 1 d P B 1 H60A H 1.0241 0.5056 0.2358 0.027 Uiso 0.63(3) 1 calc PR B 1 C55B C 1.003(4) 0.540(3) 0.329(2) 0.046(10) Uani 0.37(3) 1 d P B 2 C56B C 1.0533(17) 0.5691(11) 0.3735(9) 0.040(4) Uani 0.37(3) 1 d P B 2 H56B H 1.0353 0.5654 0.4153 0.048 Uiso 0.37(3) 1 calc PR B 2 C57B C 1.1307(18) 0.6049(11) 0.3628(8) 0.043(5) Uani 0.37(3) 1 d P B 2 H57B H 1.1619 0.6284 0.3960 0.052 Uiso 0.37(3) 1 calc PR B 2 C58B C 1.166(2) 0.6073(13) 0.3001(13) 0.041(5) Uani 0.37(3) 1 d P B 2 H58B H 1.2266 0.6245 0.2933 0.049 Uiso 0.37(3) 1 calc PR B 2 C59B C 1.107(3) 0.583(2) 0.252(2) 0.086(15) Uani 0.37(3) 1 d P B 2 H59B H 1.1196 0.5910 0.2094 0.103 Uiso 0.37(3) 1 calc PR B 2 C60B C 1.035(4) 0.5513(19) 0.263(2) 0.058(13) Uani 0.37(3) 1 d P B 2 H60B H 0.9979 0.5330 0.2287 0.070 Uiso 0.37(3) 1 calc PR B 2 C61 C 0.8398(7) 0.2700(4) 0.3028(4) 0.094(3) Uani 1 1 d . B . C62 C 0.8377(10) 0.2088(6) 0.3358(6) 0.169(5) Uani 1 1 d U . . H62A H 0.8822 0.1802 0.3177 0.253 Uiso 1 1 calc R B . H62B H 0.7725 0.1918 0.3306 0.253 Uiso 1 1 calc R . . H62C H 0.8569 0.2144 0.3805 0.253 Uiso 1 1 calc R . . O5A O 0.2304(3) 0.7202(2) 0.54518(19) 0.0531(12) Uani 0.867(7) 1 d P C 1 O6A O 0.1370(4) 0.6361(2) 0.5067(2) 0.0647(16) Uani 0.867(7) 1 d P C 1 O7A O 0.0648(4) 0.7166(3) 0.5592(3) 0.0832(19) Uani 0.867(7) 1 d P C 1 O8A O 0.1148(4) 0.7348(2) 0.4616(2) 0.0685(15) Uani 0.867(7) 1 d P C 1 O5B O 0.1126(17) 0.6734(11) 0.5695(10) 0.035(6) Uiso 0.133(7) 1 d P C 2 O6B O 0.1965(19) 0.6578(12) 0.4779(12) 0.045(7) Uiso 0.133(7) 1 d P C 2 O7B O 0.196(3) 0.761(2) 0.5259(19) 0.088(12) Uiso 0.133(7) 1 d P C 2 O8B O 0.057(3) 0.7211(16) 0.4748(16) 0.065(9) Uiso 0.133(7) 1 d P C 2 N7 N 0.0954(18) 0.2533(7) 0.3139(11) 0.110(7) Uani 0.621(12) 1 d P D 1 C63 C 0.122(2) 0.2114(9) 0.3303(12) 0.122(9) Uani 0.621(12) 1 d P D 1 C64 C 0.1725(18) 0.1556(12) 0.3559(11) 0.156(9) Uani 0.621(12) 1 d PU D 1 H64A H 0.1441 0.1188 0.3351 0.234 Uiso 0.621(12) 1 calc PR D 1 H64B H 0.1660 0.1529 0.4011 0.234 Uiso 0.621(12) 1 calc PR D 1 H64C H 0.2407 0.1581 0.3486 0.234 Uiso 0.621(12) 1 calc PR D 1 O9 O 0.1644(12) 0.2594(5) 0.3106(6) 0.067(4) Uani 0.379(12) 1 d P D 2 C65 C 0.0766(19) 0.222(2) 0.2930(15) 0.090(9) Uani 0.379(12) 1 d P D 2 H65A H 0.0684 0.2135 0.2474 0.107 Uiso 0.379(12) 1 calc PR D 2 H65B H 0.0179 0.2417 0.3065 0.107 Uiso 0.379(12) 1 calc PR D 2 C66 C 0.1039(17) 0.1590(9) 0.3333(7) 0.080(7) Uani 0.379(12) 1 d P D 2 H66A H 0.0460 0.1393 0.3482 0.096 Uiso 0.379(12) 1 calc PR D 2 H66B H 0.1381 0.1288 0.3085 0.096 Uiso 0.379(12) 1 calc PR D 2 C67 C 0.170(2) 0.1850(11) 0.3882(10) 0.108(10) Uani 0.379(12) 1 d P D 2 H67A H 0.1328 0.2056 0.4197 0.130 Uiso 0.379(12) 1 calc PR D 2 H67B H 0.2110 0.1525 0.4090 0.130 Uiso 0.379(12) 1 calc PR D 2 C68 C 0.2247(15) 0.2280(11) 0.3561(10) 0.091(7) Uani 0.379(12) 1 d P D 2 H68A H 0.2556 0.2580 0.3863 0.110 Uiso 0.379(12) 1 calc PR D 2 H68B H 0.2759 0.2061 0.3357 0.110 Uiso 0.379(12) 1 calc PR D 2 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 Ag1 0.03348(18) 0.0458(2) 0.03599(17) -0.01167(15) -0.01160(13) 0.00802(15) Ag2 0.0440(2) 0.0488(2) 0.03902(19) -0.00516(16) -0.00966(15) 0.00718(17) Se1 0.01888(19) 0.0489(3) 0.0416(2) -0.0160(2) 0.00291(17) 0.00074(17) Se2 0.0334(2) 0.0526(3) 0.0406(2) -0.0203(2) -0.01135(19) 0.0172(2) Se3 0.0266(2) 0.0836(4) 0.0397(3) -0.0215(3) 0.00978(19) -0.0151(2) Se4 0.0215(2) 0.0611(3) 0.0359(2) -0.0084(2) -0.00077(17) -0.00414(19) Cl1 0.0299(5) 0.0539(7) 0.0477(6) 0.0146(5) -0.0032(5) -0.0058(5) Cl2 0.0468(7) 0.0477(7) 0.0367(6) -0.0037(5) -0.0008(5) -0.0033(5) O1 0.061(2) 0.057(2) 0.059(2) 0.0121(19) -0.0215(19) 0.0071(19) O2 0.073(3) 0.098(4) 0.069(3) -0.004(3) 0.027(2) -0.004(3) O3 0.053(2) 0.048(2) 0.064(2) 0.0167(18) 0.0013(18) 0.0036(17) O4 0.039(2) 0.063(2) 0.086(3) 0.027(2) -0.0207(19) -0.0145(18) N1 0.0320(18) 0.0323(18) 0.0246(16) -0.0051(14) -0.0085(13) 0.0034(14) N2 0.037(2) 0.042(2) 0.0232(16) -0.0005(15) -0.0039(14) -0.0095(16) N3 0.0204(15) 0.0330(18) 0.0221(15) -0.0007(13) 0.0018(12) 0.0041(13) N4 0.0199(15) 0.0338(18) 0.0226(15) 0.0005(13) 0.0028(12) 0.0023(13) N5 0.055(3) 0.037(2) 0.051(2) -0.0043(19) -0.008(2) 0.0020(19) N6 0.103(5) 0.048(3) 0.076(4) 0.004(3) -0.002(3) -0.012(3) C1 0.028(2) 0.036(2) 0.0192(17) -0.0059(15) 0.0002(15) 0.0003(16) C2 0.0216(18) 0.032(2) 0.0209(17) -0.0087(15) 0.0004(14) 0.0035(15) C3 0.029(2) 0.033(2) 0.0232(18) -0.0099(16) 0.0036(15) 0.0047(16) C4 0.038(2) 0.042(2) 0.0203(18) -0.0099(17) -0.0018(16) 0.0125(19) C5 0.024(2) 0.053(3) 0.028(2) -0.0138(19) -0.0043(16) 0.0122(19) C6 0.0229(19) 0.050(3) 0.0252(19) -0.0131(18) 0.0037(15) 0.0012(18) C7 0.074(4) 0.044(3) 0.033(2) -0.003(2) -0.005(2) 0.022(3) C8 0.025(2) 0.031(2) 0.030(2) -0.0103(16) -0.0010(16) 0.0023(16) C9 0.043(2) 0.035(2) 0.0264(19) 0.0002(17) -0.0068(17) -0.0049(19) C10 0.048(3) 0.033(2) 0.042(3) -0.0025(19) -0.010(2) -0.012(2) C11 0.040(2) 0.035(2) 0.035(2) -0.0131(18) -0.0144(19) 0.0075(19) C12 0.047(3) 0.045(3) 0.047(3) -0.022(2) -0.020(2) 0.013(2) C13A 0.052(5) 0.071(8) 0.061(7) -0.039(6) 0.001(5) 0.005(5) C14A 0.066(6) 0.089(10) 0.090(10) -0.069(8) 0.002(7) 0.000(6) C15A 0.068(6) 0.055(7) 0.062(8) -0.036(6) -0.009(6) -0.007(5) C17A 0.118(10) 0.161(17) 0.165(18) -0.146(16) 0.019(10) -0.023(10) C13B 0.025(10) 0.030(10) 0.022(10) -0.006(7) 0.001(7) 0.004(7) C14B 0.05(2) 0.035(15) 0.019(14) -0.007(11) 0.004(12) -0.007(13) C15B 0.037(16) 0.047(18) 0.015(14) 0.007(12) -0.005(12) -0.006(12) C17B 0.047(12) 0.038(11) 0.036(11) -0.016(8) 0.011(8) -0.001(8) C16 0.051(3) 0.038(3) 0.050(3) -0.015(2) -0.017(2) 0.004(2) C18 0.021(2) 0.126(5) 0.031(2) -0.003(3) 0.0020(18) -0.003(3) C19 0.028(3) 0.181(8) 0.028(2) -0.004(3) 0.004(2) -0.020(4) C20 0.032(3) 0.226(10) 0.034(3) 0.027(4) -0.008(2) -0.014(4) C21 0.031(3) 0.197(9) 0.055(4) 0.049(5) 0.007(3) 0.017(4) C22 0.034(3) 0.148(7) 0.050(3) 0.026(4) 0.010(2) 0.026(4) C23 0.027(2) 0.127(5) 0.027(2) 0.014(3) 0.0037(18) 0.015(3) C24 0.041(3) 0.068(4) 0.047(3) -0.025(3) -0.013(2) 0.028(3) C25 0.047(3) 0.079(4) 0.050(3) -0.021(3) -0.007(2) 0.024(3) C26 0.048(3) 0.100(5) 0.065(4) -0.030(4) 0.001(3) 0.030(3) C27 0.063(4) 0.108(6) 0.074(4) -0.033(4) -0.008(3) 0.055(4) C28 0.079(4) 0.082(4) 0.063(4) -0.015(3) -0.013(3) 0.055(4) C29 0.052(3) 0.074(4) 0.050(3) -0.020(3) -0.008(2) 0.032(3) C30 0.052(3) 0.033(2) 0.043(3) -0.008(2) 0.005(2) -0.003(2) C31 0.082(4) 0.036(3) 0.040(3) -0.002(2) 0.001(3) 0.010(3) C32 0.0250(19) 0.0237(18) 0.0229(17) -0.0026(14) 0.0014(14) -0.0024(15) C33 0.0235(19) 0.031(2) 0.033(2) -0.0072(16) 0.0053(16) -0.0006(16) C34 0.036(2) 0.032(2) 0.033(2) -0.0097(17) 0.0170(18) -0.0106(18) C35 0.048(3) 0.025(2) 0.0252(19) -0.0055(16) 0.0102(18) -0.0088(18) C36 0.038(2) 0.027(2) 0.0227(18) 0.0004(15) 0.0015(16) 0.0000(17) C37 0.0266(19) 0.0225(18) 0.0237(17) 0.0000(14) 0.0027(14) 0.0004(15) C38 0.071(4) 0.043(3) 0.026(2) -0.0015(19) 0.015(2) -0.010(2) C39 0.0237(19) 0.033(2) 0.0241(18) 0.0019(16) -0.0006(15) 0.0032(16) C40 0.0204(18) 0.035(2) 0.0221(17) -0.0016(16) 0.0028(14) 0.0026(15) C41 0.0251(19) 0.036(2) 0.0254(18) 0.0025(16) -0.0010(15) 0.0058(16) C42 0.028(2) 0.032(2) 0.0172(16) -0.0013(15) 0.0024(14) -0.0004(16) C43 0.031(2) 0.044(2) 0.027(2) -0.0047(18) 0.0041(16) -0.0046(18) C44 0.051(3) 0.041(3) 0.046(3) -0.006(2) 0.004(2) -0.016(2) C45 0.060(3) 0.035(3) 0.054(3) 0.002(2) 0.007(3) -0.009(2) C46 0.049(3) 0.036(2) 0.035(2) 0.0051(19) 0.005(2) 0.005(2) C47 0.032(2) 0.034(2) 0.0214(18) 0.0023(16) 0.0045(15) 0.0023(17) C48 0.098(6) 0.036(3) 0.129(7) 0.005(4) 0.006(5) -0.019(3) C49 0.022(2) 0.078(4) 0.044(3) -0.031(3) 0.0065(19) -0.006(2) C50 0.026(2) 0.061(3) 0.028(2) 0.001(2) -0.0003(17) -0.001(2) C51 0.023(2) 0.090(4) 0.040(3) 0.011(3) -0.0005(19) -0.003(2) C52 0.029(3) 0.158(7) 0.049(3) -0.015(4) 0.015(2) 0.000(4) C53 0.037(3) 0.190(9) 0.076(4) -0.081(5) 0.023(3) -0.007(4) C54 0.028(3) 0.141(6) 0.092(5) -0.084(5) 0.017(3) -0.017(3) C55A 0.015(5) 0.070(10) 0.026(11) -0.020(9) 0.002(6) -0.019(6) C56A 0.032(6) 0.085(11) 0.031(5) -0.027(6) 0.004(4) -0.013(6) C57A 0.037(6) 0.084(11) 0.048(6) -0.028(7) 0.012(4) -0.023(6) C58A 0.044(9) 0.101(16) 0.077(9) -0.059(11) 0.037(7) -0.038(9) C59A 0.022(6) 0.038(5) 0.027(5) -0.002(4) 0.006(4) -0.001(4) C60A 0.016(6) 0.027(6) 0.024(5) -0.009(4) 0.002(4) 0.003(5) C55B 0.044(14) 0.086(17) 0.010(11) 0.007(9) 0.008(8) 0.000(11) C56B 0.034(10) 0.052(11) 0.032(7) -0.008(7) 0.000(7) -0.012(8) C57B 0.053(11) 0.049(11) 0.027(7) -0.017(7) 0.009(7) -0.020(9) C58B 0.042(13) 0.050(12) 0.034(8) -0.022(8) 0.027(8) -0.016(9) C59B 0.032(15) 0.16(3) 0.07(2) -0.06(2) 0.019(13) -0.006(17) C60B 0.031(12) 0.07(2) 0.08(2) -0.041(16) 0.004(10) 0.018(14) C61 0.148(8) 0.068(5) 0.067(4) -0.032(4) 0.027(5) -0.039(5) C62 0.197(7) 0.151(6) 0.160(6) -0.003(4) 0.024(5) -0.019(5) O5A 0.048(2) 0.059(3) 0.050(2) 0.004(2) -0.0078(19) -0.012(2) O6A 0.073(3) 0.050(3) 0.065(3) -0.010(2) -0.030(3) 0.001(2) O7A 0.080(4) 0.073(4) 0.104(4) -0.011(3) 0.054(3) -0.019(3) O8A 0.073(4) 0.071(3) 0.058(3) 0.022(2) -0.016(3) 0.013(3) N7 0.122(15) 0.082(11) 0.133(14) -0.011(11) 0.055(12) -0.030(12) C63 0.18(3) 0.078(14) 0.126(18) 0.030(11) 0.094(19) -0.003(13) C64 0.161(10) 0.155(10) 0.153(10) 0.006(5) 0.016(5) -0.002(5) O9 0.077(10) 0.040(6) 0.087(9) 0.007(5) 0.019(7) -0.010(6) C65 0.063(13) 0.10(2) 0.10(2) 0.05(2) 0.000(13) -0.001(15) C66 0.132(19) 0.071(12) 0.042(8) 0.003(8) 0.030(10) -0.067(12) C67 0.18(3) 0.078(14) 0.061(12) 0.004(11) -0.009(14) -0.065(16) C68 0.068(13) 0.116(18) 0.091(15) 0.029(13) 0.011(11) -0.019(12) _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 2.8782 (0.0218) x + 20.6666 (0.0104) y + 4.2358 (0.0327) z = 12.1221 (0.0129) * -0.0176 (0.0027) C32 * 0.0014 (0.0028) C33 * 0.0146 (0.0028) C34 * -0.0142 (0.0028) C35 * -0.0020 (0.0028) C36 * 0.0178 (0.0027) C37 Rms deviation of fitted atoms = 0.0132 - 3.5410 (0.0236) x + 1.5135 (0.0393) y + 21.0197 (0.0070) z = 4.7387 (0.0285) Angle to previous plane (with approximate esd) = 77.12 ( 0.14 ) * -0.0001 (0.0026) C42 * -0.0079 (0.0029) C43 * 0.0092 (0.0034) C44 * -0.0025 (0.0035) C45 * -0.0054 (0.0032) C46 * 0.0067 (0.0028) C47 Rms deviation of fitted atoms = 0.0061 ; 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 Ag1 N5 2.312(4) . ? Ag1 N1 2.514(3) . ? Ag1 N3 2.649(3) . ? Ag1 Se2 2.6984(6) . ? Ag1 Se1 2.7539(5) . ? Ag2 N6 2.237(6) . ? Ag2 Se3 2.6068(6) 1_655 ? Ag2 Se4 2.6165(6) . ? Ag2 N4 2.735(3) . ? Se1 C49 1.915(5) . ? Se1 C33 1.930(4) . ? Se2 C12 1.924(5) . ? Se2 C24 1.928(5) . ? Se3 C18 1.933(6) . ? Se3 C6 1.936(4) . ? Se3 Ag2 2.6067(6) 1_455 ? Se4 C55B 1.84(4) . ? Se4 C43 1.939(4) . ? Se4 C55A 1.96(2) . ? Cl1 O4 1.424(4) . ? Cl1 O2 1.425(4) . ? Cl1 O1 1.429(4) . ? Cl1 O3 1.441(4) . ? Cl2 O5B 1.35(2) . ? Cl2 O8A 1.401(5) . ? Cl2 O5A 1.436(4) . ? Cl2 O6A 1.439(5) . ? Cl2 O7A 1.450(5) . ? Cl2 O8B 1.45(4) . ? Cl2 O7B 1.53(4) . ? Cl2 O6B 1.55(3) . ? N1 C11 1.438(5) . ? N1 C8 1.479(5) . ? N1 C9 1.482(6) . ? N2 C1 1.440(5) . ? N2 C9 1.451(5) . ? N2 C10 1.488(6) . ? N3 C32 1.447(5) . ? N3 C40 1.472(5) . ? N3 C41 1.478(5) . ? N4 C42 1.440(5) . ? N4 C40 1.461(5) . ? N4 C39 1.486(5) . ? N5 C30 1.135(6) . ? N6 C61 1.065(9) . ? C1 C2 1.391(5) . ? C1 C6 1.405(6) . ? C2 C3 1.392(6) . ? C2 C8 1.515(5) . ? C3 C4 1.386(6) . ? C4 C5 1.399(6) . ? C4 C7 1.515(6) . ? C5 C6 1.364(6) . ? C10 C16 1.508(7) . ? C11 C16 1.395(6) . ? C11 C12 1.402(7) . ? C12 C13A 1.395(10) . ? C12 C13B 1.43(4) . ? C13A C14A 1.384(15) . ? C14A C15A 1.396(17) . ? C14A C17A 1.532(13) . ? C15A C16 1.421(13) . ? C13B C14B 1.36(6) . ? C14B C15B 1.34(7) . ? C14B C17B 1.52(5) . ? C15B C16 1.35(5) . ? C18 C23 1.375(8) . ? C18 C19 1.396(7) . ? C19 C20 1.389(11) . ? C20 C21 1.378(12) . ? C21 C22 1.391(9) . ? C22 C23 1.388(8) . ? C24 C29 1.386(8) . ? C24 C25 1.389(8) . ? C25 C26 1.385(7) . ? C26 C27 1.366(10) . ? C27 C28 1.387(10) . ? C28 C29 1.391(7) . ? C30 C31 1.458(7) . ? C32 C37 1.397(5) . ? C32 C33 1.401(5) . ? C33 C34 1.385(6) . ? C34 C35 1.388(6) . ? C35 C36 1.386(6) . ? C35 C38 1.512(6) . ? C36 C37 1.397(5) . ? C37 C39 1.518(5) . ? C41 C47 1.502(6) . ? C42 C47 1.395(6) . ? C42 C43 1.403(6) . ? C43 C44 1.376(6) . ? C44 C45 1.388(8) . ? C45 C46 1.381(7) . ? C45 C48 1.516(7) . ? C46 C47 1.387(6) . ? C49 C50 1.380(7) . ? C49 C54 1.382(7) . ? C50 C51 1.390(6) . ? C51 C52 1.379(8) . ? C52 C53 1.376(10) . ? C53 C54 1.387(9) . ? C55A C60A 1.33(3) . ? C55A C56A 1.46(3) . ? C56A C57A 1.393(16) . ? C57A C58A 1.33(2) . ? C58A C59A 1.45(3) . ? C59A C60A 1.41(2) . ? C55B C56B 1.31(5) . ? C55B C60B 1.53(7) . ? C56B C57B 1.37(2) . ? C57B C58B 1.47(3) . ? C58B C59B 1.37(6) . ? C59B C60B 1.26(6) . ? C61 C62 1.503(14) . ? N7 C63 1.03(3) . ? C63 C64 1.48(3) . ? O9 C68 1.41(2) . ? O9 C65 1.49(3) . ? C65 C66 1.64(4) . ? C66 C67 1.54(3) . ? C67 C68 1.42(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 N5 Ag1 N1 131.75(13) . . ? N5 Ag1 N3 86.59(13) . . ? N1 Ag1 N3 141.63(11) . . ? N5 Ag1 Se2 118.81(11) . . ? N1 Ag1 Se2 72.08(8) . . ? N3 Ag1 Se2 91.92(7) . . ? N5 Ag1 Se1 100.01(11) . . ? N1 Ag1 Se1 98.83(8) . . ? N3 Ag1 Se1 68.07(7) . . ? Se2 Ag1 Se1 135.45(2) . . ? N6 Ag2 Se3 107.26(15) . 1_655 ? N6 Ag2 Se4 113.44(15) . . ? Se3 Ag2 Se4 138.59(2) 1_655 . ? N6 Ag2 N4 91.31(18) . . ? Se3 Ag2 N4 118.64(7) 1_655 . ? Se4 Ag2 N4 68.63(7) . . ? C49 Se1 C33 100.9(2) . . ? C49 Se1 Ag1 115.30(15) . . ? C33 Se1 Ag1 88.72(11) . . ? C12 Se2 C24 99.6(2) . . ? C12 Se2 Ag1 91.82(16) . . ? C24 Se2 Ag1 109.23(17) . . ? C18 Se3 C6 97.8(2) . . ? C18 Se3 Ag2 107.75(14) . 1_455 ? C6 Se3 Ag2 100.55(12) . 1_455 ? C55B Se4 C43 103.8(19) . . ? C55B Se4 C55A 8(2) . . ? C43 Se4 C55A 98.2(9) . . ? C55B Se4 Ag2 115.1(16) . . ? C43 Se4 Ag2 93.31(12) . . ? C55A Se4 Ag2 110.2(7) . . ? O4 Cl1 O2 108.0(3) . . ? O4 Cl1 O1 110.3(2) . . ? O2 Cl1 O1 111.0(3) . . ? O4 Cl1 O3 110.2(2) . . ? O2 Cl1 O3 107.8(3) . . ? O1 Cl1 O3 109.5(2) . . ? O5B Cl2 O8A 151.5(10) . . ? O5B Cl2 O5A 94.0(10) . . ? O8A Cl2 O5A 110.3(3) . . ? O5B Cl2 O6A 71.4(10) . . ? O8A Cl2 O6A 111.9(3) . . ? O5A Cl2 O6A 109.5(3) . . ? O5B Cl2 O7A 48.8(10) . . ? O8A Cl2 O7A 106.8(4) . . ? O5A Cl2 O7A 109.6(3) . . ? O6A Cl2 O7A 108.6(3) . . ? O5B Cl2 O8B 113.9(18) . . ? O8A Cl2 O8B 37.9(14) . . ? O5A Cl2 O8B 144.0(15) . . ? O6A Cl2 O8B 101.0(14) . . ? O7A Cl2 O8B 76.8(14) . . ? O5B Cl2 O7B 117.2(18) . . ? O8A Cl2 O7B 75.8(16) . . ? O5A Cl2 O7B 42.6(16) . . ? O6A Cl2 O7B 148.2(16) . . ? O7A Cl2 O7B 97.6(15) . . ? O8B Cl2 O7B 102(2) . . ? O5B Cl2 O6B 110.9(14) . . ? O8A Cl2 O6B 87.0(10) . . ? O5A Cl2 O6B 84.2(10) . . ? O6A Cl2 O6B 46.0(10) . . ? O7A Cl2 O6B 154.6(11) . . ? O8B Cl2 O6B 104.9(17) . . ? O7B Cl2 O6B 106.6(18) . . ? C11 N1 C8 112.3(3) . . ? C11 N1 C9 110.8(3) . . ? C8 N1 C9 107.7(3) . . ? C11 N1 Ag1 109.1(2) . . ? C8 N1 Ag1 106.4(2) . . ? C9 N1 Ag1 110.4(2) . . ? C1 N2 C9 110.2(3) . . ? C1 N2 C10 113.2(3) . . ? C9 N2 C10 108.0(4) . . ? C32 N3 C40 110.6(3) . . ? C32 N3 C41 113.8(3) . . ? C40 N3 C41 107.2(3) . . ? C32 N3 Ag1 103.0(2) . . ? C40 N3 Ag1 109.8(2) . . ? C41 N3 Ag1 112.6(2) . . ? C42 N4 C40 111.1(3) . . ? C42 N4 C39 113.0(3) . . ? C40 N4 C39 106.6(3) . . ? C42 N4 Ag2 102.4(2) . . ? C40 N4 Ag2 111.4(2) . . ? C39 N4 Ag2 112.4(2) . . ? C30 N5 Ag1 155.2(4) . . ? C61 N6 Ag2 166.3(6) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 N2 122.3(4) . . ? C6 C1 N2 119.3(4) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 C8 120.3(4) . . ? C3 C2 C8 119.3(4) . . ? C4 C3 C2 121.0(4) . . ? C3 C4 C5 118.2(4) . . ? C3 C4 C7 120.4(4) . . ? C5 C4 C7 121.3(4) . . ? C6 C5 C4 121.1(4) . . ? C5 C6 C1 121.0(4) . . ? C5 C6 Se3 123.0(3) . . ? C1 C6 Se3 116.0(3) . . ? N1 C8 C2 112.5(3) . . ? N2 C9 N1 111.9(3) . . ? N2 C10 C16 112.2(4) . . ? C16 C11 C12 119.8(4) . . ? C16 C11 N1 121.2(4) . . ? C12 C11 N1 119.0(4) . . ? C13A C12 C11 122.0(7) . . ? C13A C12 C13B 23.3(11) . . ? C11 C12 C13B 108.3(16) . . ? C13A C12 Se2 118.6(6) . . ? C11 C12 Se2 119.3(3) . . ? C13B C12 Se2 129.3(15) . . ? C14A C13A C12 119.4(9) . . ? C13A C14A C15A 118.7(9) . . ? C13A C14A C17A 119.4(10) . . ? C15A C14A C17A 121.8(10) . . ? C14A C15A C16 123.0(10) . . ? C14B C13B C12 128(3) . . ? C15B C14B C13B 120(4) . . ? C15B C14B C17B 122(4) . . ? C13B C14B C17B 118(4) . . ? C14B C15B C16 114(4) . . ? C15B C16 C11 125(2) . . ? C15B C16 C15A 23.0(12) . . ? C11 C16 C15A 117.1(7) . . ? C15B C16 C10 110(2) . . ? C11 C16 C10 121.3(4) . . ? C15A C16 C10 121.5(7) . . ? C23 C18 C19 120.3(6) . . ? C23 C18 Se3 121.0(4) . . ? C19 C18 Se3 118.7(5) . . ? C20 C19 C18 119.1(7) . . ? C21 C20 C19 120.3(5) . . ? C20 C21 C22 120.6(7) . . ? C23 C22 C21 119.0(7) . . ? C18 C23 C22 120.6(5) . . ? C29 C24 C25 121.4(5) . . ? C29 C24 Se2 120.9(4) . . ? C25 C24 Se2 117.6(4) . . ? C26 C25 C24 119.2(6) . . ? C27 C26 C25 120.1(6) . . ? C26 C27 C28 120.6(5) . . ? C27 C28 C29 120.4(6) . . ? C24 C29 C28 118.2(6) . . ? N5 C30 C31 179.5(6) . . ? C37 C32 C33 119.5(3) . . ? C37 C32 N3 121.2(3) . . ? C33 C32 N3 119.2(3) . . ? C34 C33 C32 120.1(4) . . ? C34 C33 Se1 122.8(3) . . ? C32 C33 Se1 117.1(3) . . ? C33 C34 C35 120.9(4) . . ? C36 C35 C34 118.9(4) . . ? C36 C35 C38 121.1(4) . . ? C34 C35 C38 120.0(4) . . ? C35 C36 C37 121.3(4) . . ? C36 C37 C32 119.3(4) . . ? C36 C37 C39 120.2(3) . . ? C32 C37 C39 120.5(3) . . ? N4 C39 C37 112.4(3) . . ? N4 C40 N3 111.6(3) . . ? N3 C41 C47 112.2(3) . . ? C47 C42 C43 118.4(4) . . ? C47 C42 N4 121.8(4) . . ? C43 C42 N4 119.7(4) . . ? C44 C43 C42 120.8(4) . . ? C44 C43 Se4 122.8(4) . . ? C42 C43 Se4 116.4(3) . . ? C43 C44 C45 120.8(5) . . ? C46 C45 C44 118.5(4) . . ? C46 C45 C48 119.9(5) . . ? C44 C45 C48 121.5(5) . . ? C45 C46 C47 121.6(5) . . ? C46 C47 C42 119.8(4) . . ? C46 C47 C41 119.8(4) . . ? C42 C47 C41 120.4(4) . . ? C50 C49 C54 120.4(5) . . ? C50 C49 Se1 120.2(3) . . ? C54 C49 Se1 119.1(4) . . ? C49 C50 C51 120.4(5) . . ? C52 C51 C50 119.2(5) . . ? C53 C52 C51 120.2(5) . . ? C52 C53 C54 121.0(6) . . ? C49 C54 C53 118.8(6) . . ? C60A C55A C56A 123.6(17) . . ? C60A C55A Se4 119.7(17) . . ? C56A C55A Se4 116.4(15) . . ? C57A C56A C55A 118.4(12) . . ? C58A C57A C56A 118.8(13) . . ? C57A C58A C59A 122.4(18) . . ? C60A C59A C58A 119.5(17) . . ? C55A C60A C59A 117.0(18) . . ? C56B C55B C60B 114(4) . . ? C56B C55B Se4 125(3) . . ? C60B C55B Se4 121(3) . . ? C55B C56B C57B 123(2) . . ? C56B C57B C58B 120.2(18) . . ? C59B C58B C57B 117(3) . . ? C60B C59B C58B 120(4) . . ? C59B C60B C55B 125(5) . . ? N6 C61 C62 172.6(11) . . ? N7 C63 C64 173(4) . . ? C68 O9 C65 110.0(18) . . ? O9 C65 C66 99.8(17) . . ? C67 C66 C65 101.3(17) . . ? C68 C67 C66 100.6(16) . . ? O9 C68 C67 109.6(19) . . ? 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 N5 Ag1 Se1 C49 -64.4(2) . . . . ? N1 Ag1 Se1 C49 71.0(2) . . . . ? N3 Ag1 Se1 C49 -146.6(2) . . . . ? Se2 Ag1 Se1 C49 144.34(18) . . . . ? N5 Ag1 Se1 C33 37.04(16) . . . . ? N1 Ag1 Se1 C33 172.42(14) . . . . ? N3 Ag1 Se1 C33 -45.13(14) . . . . ? Se2 Ag1 Se1 C33 -114.20(12) . . . . ? N5 Ag1 Se2 C12 91.66(19) . . . . ? N1 Ag1 Se2 C12 -36.72(16) . . . . ? N3 Ag1 Se2 C12 178.83(16) . . . . ? Se1 Ag1 Se2 C12 -121.07(14) . . . . ? N5 Ag1 Se2 C24 -9.2(2) . . . . ? N1 Ag1 Se2 C24 -137.6(2) . . . . ? N3 Ag1 Se2 C24 77.97(19) . . . . ? Se1 Ag1 Se2 C24 138.07(18) . . . . ? N6 Ag2 Se4 C55B 128(2) . . . . ? Se3 Ag2 Se4 C55B -41(2) 1_655 . . . ? N4 Ag2 Se4 C55B -150(2) . . . . ? N6 Ag2 Se4 C43 -124.9(2) . . . . ? Se3 Ag2 Se4 C43 66.38(13) 1_655 . . . ? N4 Ag2 Se4 C43 -43.16(14) . . . . ? N6 Ag2 Se4 C55A 135.0(10) . . . . ? Se3 Ag2 Se4 C55A -33.6(10) 1_655 . . . ? N4 Ag2 Se4 C55A -143.2(10) . . . . ? N5 Ag1 N1 C11 -66.1(3) . . . . ? N3 Ag1 N1 C11 116.3(3) . . . . ? Se2 Ag1 N1 C11 46.9(3) . . . . ? Se1 Ag1 N1 C11 -178.1(3) . . . . ? N5 Ag1 N1 C8 172.5(2) . . . . ? N3 Ag1 N1 C8 -5.1(3) . . . . ? Se2 Ag1 N1 C8 -74.6(2) . . . . ? Se1 Ag1 N1 C8 60.5(2) . . . . ? N5 Ag1 N1 C9 55.8(3) . . . . ? N3 Ag1 N1 C9 -121.8(3) . . . . ? Se2 Ag1 N1 C9 168.8(3) . . . . ? Se1 Ag1 N1 C9 -56.2(3) . . . . ? N5 Ag1 N3 C32 -47.4(2) . . . . ? N1 Ag1 N3 C32 130.9(2) . . . . ? Se2 Ag1 N3 C32 -166.1(2) . . . . ? Se1 Ag1 N3 C32 54.9(2) . . . . ? N5 Ag1 N3 C40 70.4(2) . . . . ? N1 Ag1 N3 C40 -111.4(3) . . . . ? Se2 Ag1 N3 C40 -48.3(2) . . . . ? Se1 Ag1 N3 C40 172.6(2) . . . . ? N5 Ag1 N3 C41 -170.3(3) . . . . ? N1 Ag1 N3 C41 7.9(3) . . . . ? Se2 Ag1 N3 C41 70.9(2) . . . . ? Se1 Ag1 N3 C41 -68.1(2) . . . . ? N6 Ag2 N4 C42 167.6(3) . . . . ? Se3 Ag2 N4 C42 -81.9(2) 1_655 . . . ? Se4 Ag2 N4 C42 52.8(2) . . . . ? N6 Ag2 N4 C40 -73.6(3) . . . . ? Se3 Ag2 N4 C40 36.9(3) 1_655 . . . ? Se4 Ag2 N4 C40 171.7(3) . . . . ? N6 Ag2 N4 C39 46.0(3) . . . . ? Se3 Ag2 N4 C39 156.5(2) 1_655 . . . ? Se4 Ag2 N4 C39 -68.7(2) . . . . ? N1 Ag1 N5 C30 -154.9(9) . . . . ? N3 Ag1 N5 C30 23.6(10) . . . . ? Se2 Ag1 N5 C30 113.9(10) . . . . ? Se1 Ag1 N5 C30 -43.4(10) . . . . ? Se3 Ag2 N6 C61 -151(3) 1_655 . . . ? Se4 Ag2 N6 C61 37(3) . . . . ? N4 Ag2 N6 C61 -30(3) . . . . ? C9 N2 C1 C2 20.1(5) . . . . ? C10 N2 C1 C2 -101.0(4) . . . . ? C9 N2 C1 C6 -154.9(4) . . . . ? C10 N2 C1 C6 84.1(5) . . . . ? C6 C1 C2 C3 -1.2(5) . . . . ? N2 C1 C2 C3 -176.2(3) . . . . ? C6 C1 C2 C8 175.5(3) . . . . ? N2 C1 C2 C8 0.5(5) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C8 C2 C3 C4 -177.4(3) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? C2 C3 C4 C7 -179.8(4) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C7 C4 C5 C6 -178.8(4) . . . . ? C4 C5 C6 C1 -2.1(6) . . . . ? C4 C5 C6 Se3 177.7(3) . . . . ? C2 C1 C6 C5 2.6(6) . . . . ? N2 C1 C6 C5 177.7(4) . . . . ? C2 C1 C6 Se3 -177.3(3) . . . . ? N2 C1 C6 Se3 -2.1(5) . . . . ? C18 Se3 C6 C5 -10.5(4) . . . . ? Ag2 Se3 C6 C5 -120.3(3) 1_455 . . . ? C18 Se3 C6 C1 169.3(3) . . . . ? Ag2 Se3 C6 C1 59.5(3) 1_455 . . . ? C11 N1 C8 C2 77.8(4) . . . . ? C9 N1 C8 C2 -44.5(4) . . . . ? Ag1 N1 C8 C2 -162.9(2) . . . . ? C1 C2 C8 N1 12.7(5) . . . . ? C3 C2 C8 N1 -170.6(3) . . . . ? C1 N2 C9 N1 -55.2(4) . . . . ? C10 N2 C9 N1 68.8(4) . . . . ? C11 N1 C9 N2 -54.1(5) . . . . ? C8 N1 C9 N2 69.1(4) . . . . ? Ag1 N1 C9 N2 -175.1(3) . . . . ? C1 N2 C10 C16 77.4(5) . . . . ? C9 N2 C10 C16 -44.8(5) . . . . ? C8 N1 C11 C16 -103.1(5) . . . . ? C9 N1 C11 C16 17.4(6) . . . . ? Ag1 N1 C11 C16 139.1(4) . . . . ? C8 N1 C11 C12 78.0(5) . . . . ? C9 N1 C11 C12 -161.4(4) . . . . ? Ag1 N1 C11 C12 -39.7(5) . . . . ? C16 C11 C12 C13A 2.0(12) . . . . ? N1 C11 C12 C13A -179.1(10) . . . . ? C16 C11 C12 C13B -18.9(15) . . . . ? N1 C11 C12 C13B 160.0(14) . . . . ? C16 C11 C12 Se2 179.2(4) . . . . ? N1 C11 C12 Se2 -1.9(6) . . . . ? C24 Se2 C12 C13A -36.1(10) . . . . ? Ag1 Se2 C12 C13A -145.9(9) . . . . ? C24 Se2 C12 C11 146.6(4) . . . . ? Ag1 Se2 C12 C11 36.8(4) . . . . ? C24 Se2 C12 C13B -11.0(18) . . . . ? Ag1 Se2 C12 C13B -120.8(18) . . . . ? C11 C12 C13A C14A -3.1(15) . . . . ? C13B C12 C13A C14A 56(4) . . . . ? Se2 C12 C13A C14A 179.7(9) . . . . ? C12 C13A C14A C15A 3.3(19) . . . . ? C12 C13A C14A C17A -173.6(12) . . . . ? C13A C14A C15A C16 -3(2) . . . . ? C17A C14A C15A C16 174.1(12) . . . . ? C13A C12 C13B C14B -115(6) . . . . ? C11 C12 C13B C14B 15(3) . . . . ? Se2 C12 C13B C14B 175(2) . . . . ? C12 C13B C14B C15B -13(5) . . . . ? C12 C13B C14B C17B 175(3) . . . . ? C13B C14B C15B C16 12(5) . . . . ? C17B C14B C15B C16 -176(3) . . . . ? C14B C15B C16 C11 -19(3) . . . . ? C14B C15B C16 C15A 57(5) . . . . ? C14B C15B C16 C10 -179(2) . . . . ? C12 C11 C16 C15B 24.0(19) . . . . ? N1 C11 C16 C15B -154.8(18) . . . . ? C12 C11 C16 C15A -1.2(11) . . . . ? N1 C11 C16 C15A 180.0(9) . . . . ? C12 C11 C16 C10 -178.3(5) . . . . ? N1 C11 C16 C10 2.8(7) . . . . ? C14A C15A C16 C15B -116(7) . . . . ? C14A C15A C16 C11 1.6(16) . . . . ? C14A C15A C16 C10 178.7(10) . . . . ? N2 C10 C16 C15B 172.0(16) . . . . ? N2 C10 C16 C11 11.3(7) . . . . ? N2 C10 C16 C15A -165.7(10) . . . . ? C6 Se3 C18 C23 -87.0(5) . . . . ? Ag2 Se3 C18 C23 16.7(5) 1_455 . . . ? C6 Se3 C18 C19 93.0(5) . . . . ? Ag2 Se3 C18 C19 -163.2(4) 1_455 . . . ? C23 C18 C19 C20 0.8(9) . . . . ? Se3 C18 C19 C20 -179.3(5) . . . . ? C18 C19 C20 C21 -0.1(10) . . . . ? C19 C20 C21 C22 -0.8(11) . . . . ? C20 C21 C22 C23 1.1(11) . . . . ? C19 C18 C23 C22 -0.5(9) . . . . ? Se3 C18 C23 C22 179.6(5) . . . . ? C21 C22 C23 C18 -0.4(10) . . . . ? C12 Se2 C24 C29 -80.0(5) . . . . ? Ag1 Se2 C24 C29 15.4(5) . . . . ? C12 Se2 C24 C25 103.5(5) . . . . ? Ag1 Se2 C24 C25 -161.1(4) . . . . ? C29 C24 C25 C26 0.9(9) . . . . ? Se2 C24 C25 C26 177.4(4) . . . . ? C24 C25 C26 C27 -0.2(9) . . . . ? C25 C26 C27 C28 0.3(11) . . . . ? C26 C27 C28 C29 -1.1(11) . . . . ? C25 C24 C29 C28 -1.7(9) . . . . ? Se2 C24 C29 C28 -178.0(5) . . . . ? C27 C28 C29 C24 1.7(10) . . . . ? Ag1 N5 C30 C31 57(86) . . . . ? C40 N3 C32 C37 15.0(5) . . . . ? C41 N3 C32 C37 -105.6(4) . . . . ? Ag1 N3 C32 C37 132.2(3) . . . . ? C40 N3 C32 C33 -161.5(3) . . . . ? C41 N3 C32 C33 77.9(4) . . . . ? Ag1 N3 C32 C33 -44.3(4) . . . . ? C37 C32 C33 C34 -1.9(6) . . . . ? N3 C32 C33 C34 174.7(3) . . . . ? C37 C32 C33 Se1 178.0(3) . . . . ? N3 C32 C33 Se1 -5.4(5) . . . . ? C49 Se1 C33 C34 -16.5(4) . . . . ? Ag1 Se1 C33 C34 -132.0(3) . . . . ? C49 Se1 C33 C32 163.6(3) . . . . ? Ag1 Se1 C33 C32 48.1(3) . . . . ? C32 C33 C34 C35 -1.1(6) . . . . ? Se1 C33 C34 C35 178.9(3) . . . . ? C33 C34 C35 C36 2.6(6) . . . . ? C33 C34 C35 C38 -176.7(4) . . . . ? C34 C35 C36 C37 -1.0(6) . . . . ? C38 C35 C36 C37 178.3(4) . . . . ? C35 C36 C37 C32 -2.0(6) . . . . ? C35 C36 C37 C39 178.8(4) . . . . ? C33 C32 C37 C36 3.5(6) . . . . ? N3 C32 C37 C36 -173.1(3) . . . . ? C33 C32 C37 C39 -177.4(4) . . . . ? N3 C32 C37 C39 6.1(5) . . . . ? C42 N4 C39 C37 76.1(4) . . . . ? C40 N4 C39 C37 -46.2(4) . . . . ? Ag2 N4 C39 C37 -168.5(2) . . . . ? C36 C37 C39 N4 -170.4(3) . . . . ? C32 C37 C39 N4 10.5(5) . . . . ? C42 N4 C40 N3 -52.3(4) . . . . ? C39 N4 C40 N3 71.2(4) . . . . ? Ag2 N4 C40 N3 -165.8(2) . . . . ? C32 N3 C40 N4 -54.7(4) . . . . ? C41 N3 C40 N4 69.8(4) . . . . ? Ag1 N3 C40 N4 -167.7(2) . . . . ? C32 N3 C41 C47 74.5(4) . . . . ? C40 N3 C41 C47 -48.1(4) . . . . ? Ag1 N3 C41 C47 -168.8(2) . . . . ? C40 N4 C42 C47 15.5(5) . . . . ? C39 N4 C42 C47 -104.2(4) . . . . ? Ag2 N4 C42 C47 134.6(3) . . . . ? C40 N4 C42 C43 -161.0(3) . . . . ? C39 N4 C42 C43 79.2(4) . . . . ? Ag2 N4 C42 C43 -42.0(4) . . . . ? C47 C42 C43 C44 0.9(6) . . . . ? N4 C42 C43 C44 177.6(4) . . . . ? C47 C42 C43 Se4 -179.0(3) . . . . ? N4 C42 C43 Se4 -2.2(5) . . . . ? C55B Se4 C43 C44 -16.5(15) . . . . ? C55A Se4 C43 C44 -22.4(8) . . . . ? Ag2 Se4 C43 C44 -133.4(4) . . . . ? C55B Se4 C43 C42 163.3(15) . . . . ? C55A Se4 C43 C42 157.4(8) . . . . ? Ag2 Se4 C43 C42 46.4(3) . . . . ? C42 C43 C44 C45 -1.8(7) . . . . ? Se4 C43 C44 C45 178.0(4) . . . . ? C43 C44 C45 C46 1.2(8) . . . . ? C43 C44 C45 C48 -179.6(5) . . . . ? C44 C45 C46 C47 0.2(7) . . . . ? C48 C45 C46 C47 -179.0(5) . . . . ? C45 C46 C47 C42 -1.1(7) . . . . ? C45 C46 C47 C41 -179.9(4) . . . . ? C43 C42 C47 C46 0.5(6) . . . . ? N4 C42 C47 C46 -176.1(4) . . . . ? C43 C42 C47 C41 179.4(3) . . . . ? N4 C42 C47 C41 2.8(5) . . . . ? N3 C41 C47 C46 -166.6(4) . . . . ? N3 C41 C47 C42 14.6(5) . . . . ? C33 Se1 C49 C50 -104.0(4) . . . . ? Ag1 Se1 C49 C50 -10.2(5) . . . . ? C33 Se1 C49 C54 81.8(5) . . . . ? Ag1 Se1 C49 C54 175.6(5) . . . . ? C54 C49 C50 C51 0.3(8) . . . . ? Se1 C49 C50 C51 -173.8(4) . . . . ? C49 C50 C51 C52 -2.3(8) . . . . ? C50 C51 C52 C53 2.2(10) . . . . ? C51 C52 C53 C54 -0.1(12) . . . . ? C50 C49 C54 C53 1.8(11) . . . . ? Se1 C49 C54 C53 176.0(6) . . . . ? C52 C53 C54 C49 -1.9(13) . . . . ? C55B Se4 C55A C60A 119(21) . . . . ? C43 Se4 C55A C60A -107(2) . . . . ? Ag2 Se4 C55A C60A -10(3) . . . . ? C55B Se4 C55A C56A -56(19) . . . . ? C43 Se4 C55A C56A 78.3(18) . . . . ? Ag2 Se4 C55A C56A 175.0(15) . . . . ? C60A C55A C56A C57A 3(3) . . . . ? Se4 C55A C56A C57A 177.3(13) . . . . ? C55A C56A C57A C58A -3(2) . . . . ? C56A C57A C58A C59A -1(3) . . . . ? C57A C58A C59A C60A 7(3) . . . . ? C56A C55A C60A C59A 3(4) . . . . ? Se4 C55A C60A C59A -171.8(15) . . . . ? C58A C59A C60A C55A -7(3) . . . . ? C43 Se4 C55B C56B 99(5) . . . . ? C55A Se4 C55B C56B 146(25) . . . . ? Ag2 Se4 C55B C56B -160(4) . . . . ? C43 Se4 C55B C60B -81(4) . . . . ? C55A Se4 C55B C60B -34(17) . . . . ? Ag2 Se4 C55B C60B 19(5) . . . . ? C60B C55B C56B C57B -3(6) . . . . ? Se4 C55B C56B C57B 177(3) . . . . ? C55B C56B C57B C58B -5(4) . . . . ? C56B C57B C58B C59B 13(4) . . . . ? C57B C58B C59B C60B -13(5) . . . . ? C58B C59B C60B C55B 4(6) . . . . ? C56B C55B C60B C59B 4(7) . . . . ? Se4 C55B C60B C59B -176(4) . . . . ? Ag2 N6 C61 C62 -129(6) . . . . ? C68 O9 C65 C66 -5(2) . . . . ? O9 C65 C66 C67 28(2) . . . . ? C65 C66 C67 C68 -41(3) . . . . ? C65 O9 C68 C67 -23(3) . . . . ? C66 C67 C68 O9 41(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.881 _refine_diff_density_min -2.155 _refine_diff_density_rms 0.106