# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Chen-Wei Liu' _publ_contact_author_name 'Chen-Wei Liu' _publ_contact_author_email chenwei@mail.ndhu.edu.tw data_1 _database_code_depnum_ccdc_archive 'CCDC 797079' #TrackingRef '- squeezed-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H127 Ag11 N10 O3 S18' _chemical_formula_weight 2836.40 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 20.9216(18) _cell_length_b 20.9216(18) _cell_length_c 21.233(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8048.7(12) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4860 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.84 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 2.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6395 _exptl_absorpt_correction_T_max 0.7999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8891 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5242 _reflns_number_gt 4843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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. Bond constrains are: DFIX 1.54 0.01 C12 C13 C13 C14 C12 C13' C13' C14' DFIX 1.54 0.01 C19 C20 C19 C20' C20 C21 C20' C21' DFIX 2.55 0.01 C12 C14 C12 C14' ; _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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 5242 _refine_ls_number_parameters 311 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.6667 0.3333 -0.10253(4) 0.03860(18) Uani 1 3 d S . . Ag2 Ag 0.6667 0.3333 0.10896(4) 0.04302(19) Uani 1 3 d S . . Ag3 Ag 0.70888(3) 0.28132(3) 0.00344(2) 0.04322(12) Uani 1 1 d . . . Ag4 Ag 0.57241(3) 0.17824(3) -0.07845(3) 0.05171(14) Uani 1 1 d . . . Ag5 Ag 0.82566(3) 0.41364(3) 0.08357(3) 0.05915(16) Uani 1 1 d . . . S1 S 0.67445(10) 0.23116(9) -0.16544(8) 0.0464(4) Uani 1 1 d . . . S2 S 0.80109(10) 0.26515(10) -0.07545(9) 0.0517(4) Uani 1 1 d . . . S3 S 0.55362(11) 0.24012(11) 0.17344(9) 0.0590(5) Uani 1 1 d . . . S4 S 0.71310(11) 0.18456(11) 0.08332(10) 0.0590(5) Uani 1 1 d . . . S5 S 0.92793(11) 0.39417(12) 0.05125(11) 0.0649(5) Uani 1 1 d . . . S6 S 0.93062(10) 0.50631(10) -0.03920(10) 0.0619(5) Uani 1 1 d . . . N1 N 0.7368(4) 0.1494(3) -0.1508(3) 0.0592(16) Uani 1 1 d . . . N2 N 0.4091(4) 0.1670(5) 0.1557(5) 0.103(3) Uani 1 1 d . B . N3 N 1.0411(3) 0.4817(4) -0.0199(3) 0.0621(16) Uani 1 1 d . D . N4 N 1.3333 0.6667 -0.308(5) 0.44(6) Uani 1 3 d SDU . . O1 O 1.2607(5) 0.6275(15) -0.3049(9) 0.323(13) Uani 1 1 d DU . . C1 C 0.7376(4) 0.2104(4) -0.1318(3) 0.0456(15) Uani 1 1 d . . . C2 C 0.7913(4) 0.1281(4) -0.1315(4) 0.064(2) Uani 1 1 d . . . H2A H 0.8377 0.1721 -0.1216 0.076 Uiso 1 1 calc R . . H2B H 0.7998 0.1031 -0.1662 0.076 Uiso 1 1 calc R . . C3 C 0.7647(6) 0.0775(5) -0.0743(5) 0.082(3) Uani 1 1 d . . . H3A H 0.7647 0.1053 -0.0377 0.099 Uiso 1 1 calc R . . H3B H 0.7144 0.0382 -0.0814 0.099 Uiso 1 1 calc R . . C4 C 0.8122(6) 0.0453(6) -0.0619(6) 0.094(3) Uani 1 1 d . . . H4A H 0.8143 0.0200 -0.0989 0.141 Uiso 1 1 calc R . . H4B H 0.7921 0.0110 -0.0276 0.141 Uiso 1 1 calc R . . H4C H 0.8610 0.0839 -0.0513 0.141 Uiso 1 1 calc R . . C5 C 0.6751(5) 0.0921(5) -0.1901(4) 0.070(2) Uani 1 1 d . . . H5A H 0.6658 0.0435 -0.1779 0.084 Uiso 1 1 calc R . . H5B H 0.6305 0.0942 -0.1823 0.084 Uiso 1 1 calc R . . C6 C 0.6926(6) 0.1031(6) -0.2575(5) 0.097(3) Uani 1 1 d . . . H6A H 0.7397 0.1059 -0.2648 0.116 Uiso 1 1 calc R . . H6B H 0.6969 0.1495 -0.2707 0.116 Uiso 1 1 calc R . . C7 C 0.6315(7) 0.0387(7) -0.2975(6) 0.118(5) Uani 1 1 d . . . H7A H 0.6182 -0.0077 -0.2778 0.176 Uiso 1 1 calc R . . H7B H 0.6501 0.0397 -0.3391 0.176 Uiso 1 1 calc R . . H7C H 0.5889 0.0444 -0.3001 0.176 Uiso 1 1 calc R . . C8 C 0.4731(5) 0.2290(5) 0.1391(5) 0.074(2) Uani 1 1 d . . . C9 C 0.4068(7) 0.1108(6) 0.1989(7) 0.117(5) Uani 1 1 d . . . H9A H 0.4495 0.1054 0.1914 0.141 Uiso 1 1 calc R . . H9B H 0.3630 0.0638 0.1900 0.141 Uiso 1 1 calc R . . C10 C 0.4058(7) 0.1296(8) 0.2664(7) 0.123(5) Uani 1 1 d . . . H10A H 0.3573 0.1217 0.2772 0.148 Uiso 1 1 calc R . . H10B H 0.4415 0.1812 0.2733 0.148 Uiso 1 1 calc R . . C11 C 0.4240(8) 0.0823(8) 0.3081(7) 0.131(5) Uani 1 1 d . . . H11A H 0.3887 0.0311 0.3011 0.196 Uiso 1 1 calc R . . H11B H 0.4223 0.0944 0.3514 0.196 Uiso 1 1 calc R . . H11C H 0.4726 0.0912 0.2982 0.196 Uiso 1 1 calc R . . C12 C 0.3382(8) 0.1416(8) 0.1122(7) 0.135(5) Uani 1 1 d D . . H12A H 0.3498 0.1780 0.0793 0.162 Uiso 0.70 1 calc PR A 1 H12B H 0.3256 0.0951 0.0921 0.162 Uiso 0.70 1 calc PR A 1 H12C H 0.3070 0.0889 0.1112 0.162 Uiso 0.30 1 d PR A 2 H12D H 0.3492 0.1610 0.0701 0.162 Uiso 0.30 1 d PR A 2 C13 C 0.2720(10) 0.1323(13) 0.1497(15) 0.191(12) Uiso 0.70 1 d PD B 1 H13A H 0.2549 0.0902 0.1776 0.230 Uiso 0.70 1 calc PR B 1 H13B H 0.2321 0.1229 0.1210 0.230 Uiso 0.70 1 calc PR B 1 C14 C 0.2921(15) 0.2020(15) 0.1887(13) 0.192(11) Uiso 0.70 1 d PD B 1 H14A H 0.2506 0.1936 0.2140 0.289 Uiso 0.70 1 calc PR B 1 H14B H 0.3052 0.2429 0.1610 0.289 Uiso 0.70 1 calc PR B 1 H14C H 0.3332 0.2128 0.2157 0.289 Uiso 0.70 1 calc PR B 1 C13' C 0.299(3) 0.175(4) 0.149(3) 0.191(12) Uiso 0.30 1 d PD B 2 H13C H 0.3288 0.2288 0.1479 0.230 Uiso 0.30 1 calc PR B 2 H13D H 0.2935 0.1598 0.1927 0.230 Uiso 0.30 1 calc PR B 2 C14' C 0.222(2) 0.151(4) 0.120(3) 0.192(11) Uiso 0.30 1 d PD B 2 H14D H 0.1986 0.1726 0.1439 0.289 Uiso 0.30 1 calc PR B 2 H14E H 0.1924 0.0980 0.1223 0.289 Uiso 0.30 1 calc PR B 2 H14F H 0.2276 0.1667 0.0774 0.289 Uiso 0.30 1 calc PR B 2 C15 C 0.9724(4) 0.4623(4) -0.0037(4) 0.0548(17) Uani 1 1 d . . . C16 C 1.0779(5) 0.4431(5) 0.0069(4) 0.074(2) Uani 1 1 d . . . H16A H 1.1124 0.4432 -0.0237 0.089 Uiso 1 1 calc R . . H16B H 1.0412 0.3921 0.0155 0.089 Uiso 1 1 calc R . . C17 C 1.1183(6) 0.4787(6) 0.0663(6) 0.101(4) Uani 1 1 d . . . H17A H 1.0849 0.4815 0.0964 0.122 Uiso 1 1 calc R . . H17B H 1.1579 0.5284 0.0576 0.122 Uiso 1 1 calc R . . C18 C 1.1516(10) 0.4299(10) 0.0951(8) 0.176(9) Uani 1 1 d . . . H18A H 1.1182 0.3963 0.1260 0.264 Uiso 1 1 calc R . . H18B H 1.1984 0.4619 0.1145 0.264 Uiso 1 1 calc R . . H18C H 1.1581 0.4025 0.0619 0.264 Uiso 1 1 calc R . . C19 C 1.0821(6) 0.5352(6) -0.0691(5) 0.090(3) Uani 1 1 d D . . H19A H 1.1324 0.5674 -0.0552 0.108 Uiso 0.50 1 calc PR C 1 H19B H 1.0597 0.5654 -0.0769 0.108 Uiso 0.50 1 calc PR C 1 H19C H 1.1338 0.5561 -0.0609 0.108 Uiso 0.50 1 d PR C 2 H19D H 1.0707 0.5741 -0.0644 0.108 Uiso 0.50 1 d PR C 2 C20 C 1.0829(18) 0.4965(15) -0.1311(9) 0.121(7) Uiso 0.50 1 d PD D 1 H20A H 1.1179 0.4790 -0.1291 0.145 Uiso 0.50 1 calc PR D 1 H20B H 1.0343 0.4555 -0.1410 0.145 Uiso 0.50 1 calc PR D 1 C21 C 1.107(3) 0.560(2) -0.1791(19) 0.170(10) Uiso 0.50 1 d PD D 1 H21A H 1.1053 0.5409 -0.2208 0.256 Uiso 0.50 1 calc PR D 1 H21B H 1.1566 0.5976 -0.1698 0.256 Uiso 0.50 1 calc PR D 1 H21C H 1.0746 0.5793 -0.1766 0.256 Uiso 0.50 1 calc PR D 1 C20' C 1.0590(16) 0.5025(16) -0.1361(8) 0.121(7) Uiso 0.50 1 d PD D 2 H20C H 1.0553 0.4544 -0.1345 0.145 Uiso 0.50 1 calc PR D 2 H20D H 1.0091 0.4933 -0.1419 0.145 Uiso 0.50 1 calc PR D 2 C21' C 1.100(3) 0.538(2) -0.1976(17) 0.170(10) Uiso 0.50 1 d PD D 2 H21D H 1.0705 0.5097 -0.2328 0.256 Uiso 0.50 1 calc PR D 2 H21E H 1.1463 0.5395 -0.1981 0.256 Uiso 0.50 1 calc PR D 2 H21F H 1.1079 0.5875 -0.2005 0.256 Uiso 0.50 1 calc PR D 2 H1 H 0.6667 0.3333 0.020(9) 0.12(7) Uiso 1 3 d S . . 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 0.0362(3) 0.0362(3) 0.0434(4) 0.000 0.000 0.01809(13) Ag2 0.0419(3) 0.0419(3) 0.0453(4) 0.000 0.000 0.02094(14) Ag3 0.0463(3) 0.0458(3) 0.0431(2) 0.0002(2) -0.0011(2) 0.0272(2) Ag4 0.0496(3) 0.0378(3) 0.0653(3) 0.0050(2) -0.0017(2) 0.0201(2) Ag5 0.0439(3) 0.0585(3) 0.0724(4) -0.0013(3) -0.0037(3) 0.0236(3) S1 0.0521(9) 0.0454(9) 0.0464(9) -0.0048(7) -0.0024(7) 0.0278(8) S2 0.0530(10) 0.0541(10) 0.0580(10) -0.0091(8) -0.0066(8) 0.0344(8) S3 0.0568(11) 0.0619(11) 0.0572(11) 0.0095(9) 0.0115(9) 0.0287(9) S4 0.0634(11) 0.0560(11) 0.0669(12) 0.0033(9) -0.0028(9) 0.0368(10) S5 0.0556(11) 0.0637(12) 0.0806(14) 0.0153(10) 0.0028(10) 0.0337(10) S6 0.0499(10) 0.0450(10) 0.0815(14) 0.0019(9) -0.0182(10) 0.0168(8) N1 0.069(4) 0.055(4) 0.067(4) -0.008(3) 0.001(3) 0.041(3) N2 0.052(4) 0.097(6) 0.148(9) 0.048(6) 0.027(5) 0.027(4) N3 0.048(3) 0.071(4) 0.069(4) 0.003(3) 0.001(3) 0.030(3) N4 0.28(2) 0.28(2) 0.76(17) 0.000 0.000 0.141(12) O1 0.26(2) 0.39(3) 0.23(2) -0.02(2) -0.099(19) 0.10(2) C1 0.048(4) 0.044(4) 0.049(4) 0.001(3) 0.007(3) 0.026(3) C2 0.067(5) 0.064(5) 0.073(5) -0.010(4) 0.004(4) 0.042(4) C3 0.090(7) 0.068(6) 0.103(7) 0.005(5) -0.001(6) 0.049(5) C4 0.094(7) 0.090(7) 0.126(9) 0.029(6) 0.012(7) 0.066(6) C5 0.072(5) 0.059(5) 0.075(6) -0.010(4) 0.006(4) 0.029(4) C6 0.099(8) 0.083(7) 0.096(8) -0.012(6) 0.032(6) 0.036(6) C7 0.108(9) 0.102(8) 0.110(9) -0.058(7) 0.005(7) 0.028(7) C8 0.050(5) 0.079(6) 0.094(6) 0.009(5) 0.027(4) 0.031(4) C9 0.080(7) 0.073(7) 0.182(14) 0.027(8) 0.049(8) 0.025(6) C10 0.102(9) 0.134(11) 0.123(10) 0.041(9) 0.045(8) 0.052(8) C11 0.121(10) 0.145(11) 0.138(12) 0.058(10) 0.052(9) 0.076(9) C12 0.131(12) 0.096(9) 0.177(16) 0.007(9) 0.007(11) 0.055(9) C15 0.044(4) 0.054(4) 0.060(4) 0.001(3) -0.005(3) 0.019(3) C16 0.064(5) 0.081(6) 0.084(6) -0.013(5) -0.003(4) 0.043(5) C17 0.083(7) 0.099(8) 0.131(9) -0.053(7) -0.048(7) 0.053(6) C18 0.208(17) 0.166(15) 0.205(18) -0.079(13) -0.142(16) 0.132(14) C19 0.078(6) 0.086(7) 0.096(7) 0.016(6) 0.017(5) 0.033(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. ; 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 S1 2.5938(17) . ? Ag1 S1 2.5938(17) 2_655 ? Ag1 S1 2.5938(17) 3_665 ? Ag1 Ag3 2.8262(8) . ? Ag1 Ag3 2.8262(8) 2_655 ? Ag1 Ag3 2.8262(8) 3_665 ? Ag1 Ag4 2.8775(5) . ? Ag1 Ag4 2.8775(5) 2_655 ? Ag1 Ag4 2.8775(5) 3_665 ? Ag2 S3 2.5804(19) 2_655 ? Ag2 S3 2.5804(19) . ? Ag2 S3 2.5804(19) 3_665 ? Ag2 Ag3 2.8187(8) . ? Ag2 Ag3 2.8187(8) 3_665 ? Ag2 Ag3 2.8187(8) 2_655 ? Ag2 Ag5 2.9309(6) 3_665 ? Ag2 Ag5 2.9309(6) . ? Ag2 Ag5 2.9309(6) 2_655 ? Ag2 H1 1.88(19) . ? Ag3 S4 2.6760(19) . ? Ag3 S2 2.7008(19) . ? Ag3 Ag4 2.9325(8) 2_655 ? Ag3 Ag5 2.9396(8) 3_665 ? Ag3 Ag3 2.9623(8) 3_665 ? Ag3 Ag3 2.9623(8) 2_655 ? Ag3 Ag4 3.1094(8) . ? Ag3 Ag5 3.1249(8) . ? Ag3 H1 1.75(4) . ? Ag4 S6 2.4582(19) 3_665 ? Ag4 S2 2.5121(19) 3_665 ? Ag4 S1 2.6135(18) . ? Ag4 Ag3 2.9325(8) 3_665 ? Ag5 S5 2.467(2) . ? Ag5 S4 2.518(2) 2_655 ? Ag5 S3 2.653(2) 2_655 ? Ag5 Ag3 2.9396(8) 2_655 ? S1 C1 1.737(7) . ? S2 C1 1.728(7) . ? S2 Ag4 2.5121(18) 2_655 ? S3 C8 1.741(10) . ? S3 Ag5 2.653(2) 3_665 ? S4 C8 1.707(10) 2_655 ? S4 Ag5 2.518(2) 3_665 ? S5 C15 1.712(8) . ? S6 C15 1.727(8) . ? S6 Ag4 2.4582(19) 2_655 ? N1 C1 1.331(9) . ? N1 C2 1.475(10) . ? N1 C5 1.501(11) . ? N2 C8 1.365(11) . ? N2 C9 1.472(16) . ? N2 C12 1.596(17) . ? N3 C15 1.331(10) . ? N3 C19 1.456(12) . ? N3 C16 1.480(11) . ? N4 O1 1.319(9) 3_775 ? N4 O1 1.319(9) . ? N4 O1 1.319(10) 2_755 ? C2 C3 1.522(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.477(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.465(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.565(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 S4 1.707(10) 3_665 ? C9 C10 1.488(19) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.512(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.524(10) . ? C12 C13' 1.538(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9600 . ? C12 H12D 0.9599 . ? C13 C14 1.541(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13' C14' 1.548(10) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C16 C17 1.493(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.617(18) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20' 1.547(10) . ? C19 C20 1.550(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9600 . ? C19 H19D 0.9601 . ? C20 C21 1.538(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C20' C21' 1.533(10) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? 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 S1 Ag1 S1 95.87(5) . 2_655 ? S1 Ag1 S1 95.87(5) . 3_665 ? S1 Ag1 S1 95.87(5) 2_655 3_665 ? S1 Ag1 Ag3 86.11(4) . . ? S1 Ag1 Ag3 118.28(4) 2_655 . ? S1 Ag1 Ag3 145.47(4) 3_665 . ? S1 Ag1 Ag3 145.47(4) . 2_655 ? S1 Ag1 Ag3 86.11(4) 2_655 2_655 ? S1 Ag1 Ag3 118.28(4) 3_665 2_655 ? Ag3 Ag1 Ag3 63.21(2) . 2_655 ? S1 Ag1 Ag3 118.28(4) . 3_665 ? S1 Ag1 Ag3 145.47(4) 2_655 3_665 ? S1 Ag1 Ag3 86.11(4) 3_665 3_665 ? Ag3 Ag1 Ag3 63.21(2) . 3_665 ? Ag3 Ag1 Ag3 63.21(2) 2_655 3_665 ? S1 Ag1 Ag4 56.78(4) . . ? S1 Ag1 Ag4 152.60(4) 2_655 . ? S1 Ag1 Ag4 86.24(4) 3_665 . ? Ag3 Ag1 Ag4 66.063(18) . . ? Ag3 Ag1 Ag4 116.93(3) 2_655 . ? Ag3 Ag1 Ag4 61.872(18) 3_665 . ? S1 Ag1 Ag4 86.24(4) . 2_655 ? S1 Ag1 Ag4 56.78(4) 2_655 2_655 ? S1 Ag1 Ag4 152.60(4) 3_665 2_655 ? Ag3 Ag1 Ag4 61.872(18) . 2_655 ? Ag3 Ag1 Ag4 66.063(18) 2_655 2_655 ? Ag3 Ag1 Ag4 116.93(3) 3_665 2_655 ? Ag4 Ag1 Ag4 116.914(12) . 2_655 ? S1 Ag1 Ag4 152.60(4) . 3_665 ? S1 Ag1 Ag4 86.24(4) 2_655 3_665 ? S1 Ag1 Ag4 56.78(4) 3_665 3_665 ? Ag3 Ag1 Ag4 116.93(3) . 3_665 ? Ag3 Ag1 Ag4 61.872(18) 2_655 3_665 ? Ag3 Ag1 Ag4 66.063(18) 3_665 3_665 ? Ag4 Ag1 Ag4 116.914(12) . 3_665 ? Ag4 Ag1 Ag4 116.914(12) 2_655 3_665 ? S3 Ag2 S3 94.46(7) 2_655 . ? S3 Ag2 S3 94.46(7) 2_655 3_665 ? S3 Ag2 S3 94.46(7) . 3_665 ? S3 Ag2 Ag3 87.24(5) 2_655 . ? S3 Ag2 Ag3 118.40(5) . . ? S3 Ag2 Ag3 146.90(5) 3_665 . ? S3 Ag2 Ag3 146.90(5) 2_655 3_665 ? S3 Ag2 Ag3 87.24(5) . 3_665 ? S3 Ag2 Ag3 118.40(5) 3_665 3_665 ? Ag3 Ag2 Ag3 63.40(2) . 3_665 ? S3 Ag2 Ag3 118.40(5) 2_655 2_655 ? S3 Ag2 Ag3 146.90(5) . 2_655 ? S3 Ag2 Ag3 87.24(5) 3_665 2_655 ? Ag3 Ag2 Ag3 63.40(2) . 2_655 ? Ag3 Ag2 Ag3 63.40(2) 3_665 2_655 ? S3 Ag2 Ag5 87.47(5) 2_655 3_665 ? S3 Ag2 Ag5 57.14(5) . 3_665 ? S3 Ag2 Ag5 151.58(5) 3_665 3_665 ? Ag3 Ag2 Ag5 61.461(19) . 3_665 ? Ag3 Ag2 Ag5 65.812(19) 3_665 3_665 ? Ag3 Ag2 Ag5 116.68(3) 2_655 3_665 ? S3 Ag2 Ag5 57.14(5) 2_655 . ? S3 Ag2 Ag5 151.58(5) . . ? S3 Ag2 Ag5 87.47(5) 3_665 . ? Ag3 Ag2 Ag5 65.812(19) . . ? Ag3 Ag2 Ag5 116.68(3) 3_665 . ? Ag3 Ag2 Ag5 61.461(19) 2_655 . ? Ag5 Ag2 Ag5 116.697(13) 3_665 . ? S3 Ag2 Ag5 151.58(5) 2_655 2_655 ? S3 Ag2 Ag5 87.47(5) . 2_655 ? S3 Ag2 Ag5 57.14(5) 3_665 2_655 ? Ag3 Ag2 Ag5 116.68(3) . 2_655 ? Ag3 Ag2 Ag5 61.461(19) 3_665 2_655 ? Ag3 Ag2 Ag5 65.812(19) 2_655 2_655 ? Ag5 Ag2 Ag5 116.697(13) 3_665 2_655 ? Ag5 Ag2 Ag5 116.697(13) . 2_655 ? S3 Ag2 H1 122.04(5) 2_655 . ? S3 Ag2 H1 122.04(5) . . ? S3 Ag2 H1 122.04(5) 3_665 . ? Ag3 Ag2 H1 37.356(15) . . ? Ag3 Ag2 H1 37.356(15) 3_665 . ? Ag3 Ag2 H1 37.356(15) 2_655 . ? Ag5 Ag2 H1 79.40(2) 3_665 . ? Ag5 Ag2 H1 79.40(2) . . ? Ag5 Ag2 H1 79.40(2) 2_655 . ? S4 Ag3 S2 90.14(6) . . ? S4 Ag3 Ag2 85.61(5) . . ? S2 Ag3 Ag2 157.31(4) . . ? S4 Ag3 Ag1 158.55(5) . . ? S2 Ag3 Ag1 86.26(4) . . ? Ag2 Ag3 Ag1 105.40(2) . . ? S4 Ag3 Ag4 131.83(5) . 2_655 ? S2 Ag3 Ag4 52.77(4) . 2_655 ? Ag2 Ag3 Ag4 116.24(2) . 2_655 ? Ag1 Ag3 Ag4 59.924(15) . 2_655 ? S4 Ag3 Ag5 53.02(5) . 3_665 ? S2 Ag3 Ag5 131.31(4) . 3_665 ? Ag2 Ag3 Ag5 61.149(16) . 3_665 ? Ag1 Ag3 Ag5 116.00(2) . 3_665 ? Ag4 Ag3 Ag5 175.02(2) 2_655 3_665 ? S4 Ag3 Ag3 116.73(5) . 3_665 ? S2 Ag3 Ag3 141.45(4) . 3_665 ? Ag2 Ag3 Ag3 58.300(12) . 3_665 ? Ag1 Ag3 Ag3 58.394(12) . 3_665 ? Ag4 Ag3 Ag3 111.115(17) 2_655 3_665 ? Ag5 Ag3 Ag3 63.94(2) 3_665 3_665 ? S4 Ag3 Ag3 140.34(5) . 2_655 ? S2 Ag3 Ag3 116.39(5) . 2_655 ? Ag2 Ag3 Ag3 58.300(12) . 2_655 ? Ag1 Ag3 Ag3 58.394(12) . 2_655 ? Ag4 Ag3 Ag3 63.67(2) 2_655 2_655 ? Ag5 Ag3 Ag3 112.042(18) 3_665 2_655 ? Ag3 Ag3 Ag3 60.0 3_665 2_655 ? S4 Ag3 Ag4 101.30(5) . . ? S2 Ag3 Ag4 91.83(4) . . ? Ag2 Ag3 Ag4 110.85(2) . . ? Ag1 Ag3 Ag4 57.761(13) . . ? Ag4 Ag3 Ag4 108.51(3) 2_655 . ? Ag5 Ag3 Ag4 69.73(2) 3_665 . ? Ag3 Ag3 Ag4 57.699(19) 3_665 . ? Ag3 Ag3 Ag4 106.364(17) 2_655 . ? S4 Ag3 Ag5 91.04(5) . . ? S2 Ag3 Ag5 99.07(4) . . ? Ag2 Ag3 Ag5 58.821(15) . . ? Ag1 Ag3 Ag5 110.41(2) . . ? Ag4 Ag3 Ag5 69.60(2) 2_655 . ? Ag5 Ag3 Ag5 110.69(3) 3_665 . ? Ag3 Ag3 Ag5 106.997(17) 3_665 . ? Ag3 Ag3 Ag5 57.68(2) 2_655 . ? Ag4 Ag3 Ag5 163.54(2) . . ? S4 Ag3 H1 124(6) . . ? S2 Ag3 H1 145(5) . . ? Ag2 Ag3 H1 41(6) . . ? Ag1 Ag3 H1 65(6) . . ? Ag4 Ag3 H1 94(4) 2_655 . ? Ag5 Ag3 H1 81(3) 3_665 . ? Ag3 Ag3 H1 32(2) 3_665 . ? Ag3 Ag3 H1 32(2) 2_655 . ? Ag4 Ag3 H1 88(4) . . ? Ag5 Ag3 H1 76(3) . . ? S6 Ag4 S2 126.62(6) 3_665 3_665 ? S6 Ag4 S1 103.70(6) 3_665 . ? S2 Ag4 S1 124.14(6) 3_665 . ? S6 Ag4 Ag1 141.64(5) 3_665 . ? S2 Ag4 Ag1 88.80(4) 3_665 . ? S1 Ag4 Ag1 56.13(4) . . ? S6 Ag4 Ag3 123.80(6) 3_665 3_665 ? S2 Ag4 Ag3 58.88(5) 3_665 3_665 ? S1 Ag4 Ag3 113.99(4) . 3_665 ? Ag1 Ag4 Ag3 58.204(19) . 3_665 ? S6 Ag4 Ag3 90.67(6) 3_665 . ? S2 Ag4 Ag3 117.46(5) 3_665 . ? S1 Ag4 Ag3 80.16(4) . . ? Ag1 Ag4 Ag3 56.176(18) . . ? Ag3 Ag4 Ag3 58.63(2) 3_665 . ? S5 Ag5 S4 130.68(7) . 2_655 ? S5 Ag5 S3 102.71(7) . 2_655 ? S4 Ag5 S3 119.82(7) 2_655 2_655 ? S5 Ag5 Ag2 141.81(5) . . ? S4 Ag5 Ag2 86.21(5) 2_655 . ? S3 Ag5 Ag2 54.77(4) 2_655 . ? S5 Ag5 Ag3 128.42(6) . 2_655 ? S4 Ag5 Ag3 58.11(5) 2_655 2_655 ? S3 Ag5 Ag3 111.99(5) 2_655 2_655 ? Ag2 Ag5 Ag3 57.390(19) . 2_655 ? S5 Ag5 Ag3 93.48(6) . . ? S4 Ag5 Ag3 116.27(5) 2_655 . ? S3 Ag5 Ag3 79.92(5) 2_655 . ? Ag2 Ag5 Ag3 55.367(19) . . ? Ag3 Ag5 Ag3 58.38(2) 2_655 . ? C1 S1 Ag1 111.3(2) . . ? C1 S1 Ag4 99.5(2) . . ? Ag1 S1 Ag4 67.09(4) . . ? C1 S2 Ag4 110.9(2) . 2_655 ? C1 S2 Ag3 98.7(2) . . ? Ag4 S2 Ag3 68.35(5) 2_655 . ? C8 S3 Ag2 109.8(3) . . ? C8 S3 Ag5 97.1(3) . 3_665 ? Ag2 S3 Ag5 68.09(5) . 3_665 ? C8 S4 Ag5 112.9(3) 2_655 3_665 ? C8 S4 Ag3 99.6(3) 2_655 . ? Ag5 S4 Ag3 68.87(5) 3_665 . ? C15 S5 Ag5 101.9(3) . . ? C15 S6 Ag4 96.5(3) . 2_655 ? C1 N1 C2 124.3(7) . . ? C1 N1 C5 122.0(6) . . ? C2 N1 C5 113.5(6) . . ? C8 N2 C9 123.0(9) . . ? C8 N2 C12 118.3(10) . . ? C9 N2 C12 116.2(9) . . ? C15 N3 C19 123.5(7) . . ? C15 N3 C16 120.7(7) . . ? C19 N3 C16 115.4(7) . . ? O1 N4 O1 119.8(7) 3_775 . ? O1 N4 O1 119.8(7) 3_775 2_755 ? O1 N4 O1 119.8(7) . 2_755 ? N1 C1 S2 118.9(5) . . ? N1 C1 S1 117.9(5) . . ? S2 C1 S1 123.2(4) . . ? N1 C2 C3 111.3(7) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 111.3(9) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N1 111.7(8) . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? N1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.2(9) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 S4 119.7(7) . 3_665 ? N2 C8 S3 116.3(7) . . ? S4 C8 S3 123.8(5) 3_665 . ? N2 C9 C10 112.9(11) . . ? N2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 110.5(13) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.6 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C13' 30(3) . . ? C13 C12 N2 112.0(16) . . ? C13' C12 N2 99.9(18) . . ? C13 C12 H12A 109.2 . . ? C13' C12 H12A 89.2 . . ? N2 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C13' C12 H12B 138.2 . . ? N2 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C13 C12 H12C 79.2 . . ? C13' C12 H12C 109.1 . . ? N2 C12 H12C 112.3 . . ? H12A C12 H12C 130.3 . . ? H12B C12 H12C 32.0 . . ? C13 C12 H12D 123.3 . . ? C13' C12 H12D 110.4 . . ? N2 C12 H12D 114.3 . . ? H12A C12 H12D 24.0 . . ? H12B C12 H12D 84.4 . . ? H12C C12 H12D 110.4 . . ? C12 C13 C14 111.1(10) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13' C14' 110.6(10) . . ? C12 C13' H13C 109.5 . . ? C14' C13' H13C 109.5 . . ? C12 C13' H13D 109.5 . . ? C14' C13' H13D 109.5 . . ? H13C C13' H13D 108.1 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? N3 C15 S5 119.0(6) . . ? N3 C15 S6 118.8(6) . . ? S5 C15 S6 122.2(4) . . ? N3 C16 C17 111.9(7) . . ? N3 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N3 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 108.7(9) . . ? C16 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? C16 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20' 112.7(13) . . ? N3 C19 C20 111.3(13) . . ? C20' C19 C20 21.7(18) . . ? N3 C19 H19A 109.4 . . ? C20' C19 H19A 125.4 . . ? C20 C19 H19A 109.4 . . ? N3 C19 H19B 109.4 . . ? C20' C19 H19B 89.3 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N3 C19 H19C 108.3 . . ? C20' C19 H19C 113.7 . . ? C20 C19 H19C 95.1 . . ? H19A C19 H19C 16.8 . . ? H19B C19 H19C 122.5 . . ? N3 C19 H19D 106.0 . . ? C20' C19 H19D 108.5 . . ? C20 C19 H19D 127.2 . . ? H19A C19 H19D 91.2 . . ? H19B C19 H19D 20.2 . . ? H19C C19 H19D 107.3 . . ? C21 C20 C19 101(2) . . ? C21 C20 H20A 111.5 . . ? C19 C20 H20A 111.5 . . ? C21 C20 H20B 111.5 . . ? C19 C20 H20B 111.5 . . ? H20A C20 H20B 109.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21' C20' C19 126(3) . . ? C21' C20' H20C 105.7 . . ? C19 C20' H20C 105.7 . . ? C21' C20' H20D 105.7 . . ? C19 C20' H20D 105.7 . . ? H20C C20' H20D 106.2 . . ? C20' C21' H21D 109.5 . . ? C20' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C20' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.729 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.085