# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Haukka, Matti' _publ_contact_author_name 'Haukka, Matti' _publ_contact_author_email matti.haukka@uef.fi _publ_section_title ; Argentophilic interactions in multinuclear Ag complexes of imidazole containing Schiff bases ; # Attachment 'Koskinen.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 855059' #TrackingRef 'Koskinen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Ag2 N12, 2(C F3 O3 S), C H4 O, C2 H3 N' _chemical_formula_sum 'C29 H39 Ag2 F6 N13 O7 S2' _chemical_formula_weight 1075.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0553(3) _cell_length_b 13.5377(3) _cell_length_c 13.8510(4) _cell_angle_alpha 89.426(2) _cell_angle_beta 77.0130(10) _cell_angle_gamma 67.0080(10) _cell_volume 2020.06(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25990 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8121 _exptl_absorpt_correction_T_max 0.8967 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The OH hydrogen atom was located from the difference Fourier map but constrained to ride on its parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.47 \%A from atom C28 and the deepest hole is located 0.43 \%A from atom F4. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40562 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9267 _reflns_number_gt 6977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0551P)^2^+3.5610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9267 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.09075(3) 0.08716(2) 0.79524(2) 0.03626(10) Uani 1 1 d . . . Ag2 Ag 0.08720(3) 0.32693(2) 0.73351(2) 0.03196(10) Uani 1 1 d . . . S1 S 0.49783(9) 0.43032(8) 0.74843(8) 0.0330(2) Uani 1 1 d . . . S2 S 0.20849(10) 0.17190(9) 0.23206(8) 0.0370(2) Uani 1 1 d . . . F1 F 0.4177(3) 0.3236(2) 0.6446(2) 0.0583(8) Uani 1 1 d . . . F2 F 0.6151(3) 0.2629(3) 0.6196(3) 0.0777(11) Uani 1 1 d . . . F3 F 0.5160(3) 0.4109(3) 0.5584(2) 0.0676(9) Uani 1 1 d . . . F4 F 0.1492(5) 0.0193(4) 0.3091(5) 0.1229(19) Uani 1 1 d . . . F5 F 0.3179(4) -0.0366(3) 0.1966(4) 0.1073(16) Uani 1 1 d . . . F6 F 0.1492(5) 0.0337(3) 0.1502(5) 0.138(2) Uani 1 1 d . . . O1 O 0.3874(3) 0.5252(2) 0.7536(2) 0.0456(8) Uani 1 1 d . . . O2 O 0.4872(3) 0.3582(3) 0.8251(2) 0.0500(8) Uani 1 1 d . . . O3 O 0.6119(2) 0.4459(2) 0.7288(2) 0.0350(6) Uani 1 1 d . . . O4 O 0.0799(3) 0.2391(3) 0.2755(3) 0.0540(9) Uani 1 1 d . . . O5 O 0.2914(3) 0.1591(3) 0.2956(3) 0.0522(8) Uani 1 1 d . . . O6 O 0.2530(4) 0.1956(4) 0.1345(3) 0.0887(15) Uani 1 1 d . . . O7 O 0.5061(4) 0.1862(4) 0.1247(3) 0.0726(11) Uani 1 1 d . . . H7O H 0.4238 0.2373 0.1187 0.109 Uiso 1 1 d R . . N1 N 0.1912(3) -0.0891(2) 0.7104(2) 0.0286(7) Uani 1 1 d . . . N2 N 0.3767(3) -0.2237(2) 0.6619(2) 0.0305(7) Uani 1 1 d . . . N3 N 0.3009(3) 0.0483(3) 0.7576(2) 0.0281(7) Uani 1 1 d . . . N4 N 0.1743(3) 0.2679(2) 0.8666(2) 0.0270(7) Uani 1 1 d . . . N5 N -0.0668(3) 0.4229(2) 0.8792(2) 0.0260(7) Uani 1 1 d . . . N6 N -0.1077(3) 0.4358(2) 1.0434(2) 0.0278(7) Uani 1 1 d . . . N7 N -0.0667(3) 0.1516(2) 0.9391(2) 0.0274(7) Uani 1 1 d . . . N8 N -0.2580(3) 0.2710(2) 1.0019(2) 0.0272(7) Uani 1 1 d . . . N9 N -0.0896(3) 0.1957(2) 0.7448(2) 0.0245(6) Uani 1 1 d . . . N10 N 0.0600(3) 0.2739(2) 0.5853(2) 0.0248(6) Uani 1 1 d . . . N11 N 0.1460(3) 0.4344(3) 0.6103(2) 0.0286(7) Uani 1 1 d . . . N12 N 0.1791(3) 0.4548(2) 0.4484(2) 0.0240(6) Uani 1 1 d . . . N13 N 0.3692(7) 0.1330(7) 0.5183(6) 0.116(2) Uani 1 1 d . . . C1 C 0.1775(4) -0.1771(3) 0.6772(3) 0.0308(8) Uani 1 1 d . . . H1 H 0.1007 -0.1803 0.6752 0.037 Uiso 1 1 calc R . . C2 C 0.2913(4) -0.2602(3) 0.6471(3) 0.0328(9) Uani 1 1 d . . . H2 H 0.3075 -0.3304 0.6209 0.039 Uiso 1 1 calc R . . C3 C 0.5115(4) -0.2869(3) 0.6435(4) 0.0441(11) Uani 1 1 d . . . H3A H 0.5528 -0.2734 0.5784 0.066 Uiso 1 1 calc R . . H3B H 0.5281 -0.3638 0.6444 0.066 Uiso 1 1 calc R . . H3C H 0.5433 -0.2657 0.6954 0.066 Uiso 1 1 calc R . . C4 C 0.3135(3) -0.1191(3) 0.7002(3) 0.0274(8) Uani 1 1 d . . . C5 C 0.3695(3) -0.0475(3) 0.7218(3) 0.0287(8) Uani 1 1 d . . . H5 H 0.4572 -0.0722 0.7091 0.034 Uiso 1 1 calc R . . C6 C 0.3616(4) 0.1207(3) 0.7679(3) 0.0332(9) Uani 1 1 d . . . H6A H 0.3574 0.1661 0.7113 0.040 Uiso 1 1 calc R . . H6B H 0.4502 0.0775 0.7652 0.040 Uiso 1 1 calc R . . C7 C 0.3030(4) 0.1929(3) 0.8642(3) 0.0336(9) Uani 1 1 d . . . H7A H 0.3028 0.1480 0.9210 0.040 Uiso 1 1 calc R . . H7B H 0.3528 0.2346 0.8709 0.040 Uiso 1 1 calc R . . C8 C 0.1008(3) 0.3050(3) 0.9514(3) 0.0273(8) Uani 1 1 d . . . H8 H 0.1268 0.2802 1.0102 0.033 Uiso 1 1 calc R . . C9 C -0.0229(3) 0.3854(3) 0.9576(3) 0.0249(7) Uani 1 1 d . . . C10 C -0.1832(4) 0.4999(3) 0.9168(3) 0.0297(8) Uani 1 1 d . . . H10 H -0.2379 0.5413 0.8780 0.036 Uiso 1 1 calc R . . C11 C -0.2091(4) 0.5087(3) 1.0174(3) 0.0319(9) Uani 1 1 d . . . H11 H -0.2835 0.5564 1.0613 0.038 Uiso 1 1 calc R . . C12 C -0.0949(4) 0.4164(4) 1.1460(3) 0.0360(9) Uani 1 1 d . . . H12A H -0.1248 0.4855 1.1854 0.054 Uiso 1 1 calc R . . H12B H -0.0073 0.3750 1.1452 0.054 Uiso 1 1 calc R . . H12C H -0.1438 0.3758 1.1757 0.054 Uiso 1 1 calc R . . C13 C -0.0926(4) 0.1542(3) 1.0402(3) 0.0327(9) Uani 1 1 d . . . H13 H -0.0370 0.1111 1.0776 0.039 Uiso 1 1 calc R . . C14 C -0.2095(4) 0.2277(3) 1.0797(3) 0.0312(8) Uani 1 1 d . . . H14 H -0.2496 0.2453 1.1483 0.037 Uiso 1 1 calc R . . C15 C -0.3834(3) 0.3540(3) 1.0102(3) 0.0367(10) Uani 1 1 d . . . H15A H -0.3779 0.4159 0.9754 0.055 Uiso 1 1 calc R . . H15B H -0.4247 0.3770 1.0805 0.055 Uiso 1 1 calc R . . H15C H -0.4313 0.3243 0.9802 0.055 Uiso 1 1 calc R . . C16 C -0.1687(3) 0.2228(3) 0.9177(3) 0.0239(7) Uani 1 1 d . . . C17 C -0.1828(3) 0.2433(3) 0.8171(3) 0.0253(8) Uani 1 1 d . . . H17 H -0.2599 0.2911 0.8055 0.030 Uiso 1 1 calc R . . C18 C -0.1070(3) 0.2100(3) 0.6440(3) 0.0289(8) Uani 1 1 d . . . H18A H -0.1676 0.2840 0.6411 0.035 Uiso 1 1 calc R . . H18B H -0.1409 0.1589 0.6257 0.035 Uiso 1 1 calc R . . C19 C 0.0149(4) 0.1907(3) 0.5704(3) 0.0301(8) Uani 1 1 d . . . H19A H 0.0777 0.1194 0.5782 0.036 Uiso 1 1 calc R . . H19B H 0.0035 0.1899 0.5019 0.036 Uiso 1 1 calc R . . C20 C 0.0912(3) 0.3199(3) 0.5099(3) 0.0248(8) Uani 1 1 d . . . H20 H 0.0846 0.3008 0.4463 0.030 Uiso 1 1 calc R . . C21 C 0.1371(3) 0.4024(3) 0.5228(3) 0.0225(7) Uani 1 1 d . . . C22 C 0.1950(4) 0.5098(3) 0.5901(3) 0.0324(9) Uani 1 1 d . . . H22 H 0.2117 0.5479 0.6383 0.039 Uiso 1 1 calc R . . C23 C 0.2163(3) 0.5227(3) 0.4910(3) 0.0284(8) Uani 1 1 d . . . H23 H 0.2506 0.5699 0.4581 0.034 Uiso 1 1 calc R . . C24 C 0.1834(4) 0.4429(3) 0.3427(3) 0.0297(8) Uani 1 1 d . . . H24A H 0.2349 0.3680 0.3163 0.045 Uiso 1 1 calc R . . H24B H 0.2191 0.4904 0.3067 0.045 Uiso 1 1 calc R . . H24C H 0.0991 0.4623 0.3341 0.045 Uiso 1 1 calc R . . C25 C 0.5127(4) 0.3519(4) 0.6375(4) 0.0445(11) Uani 1 1 d . . . C26 C 0.2078(6) 0.0383(5) 0.2204(6) 0.076(2) Uani 1 1 d . . . C27 C 0.5701(7) 0.1139(6) 0.0385(5) 0.0793(19) Uani 1 1 d . . . H27A H 0.5492 0.1509 -0.0202 0.119 Uiso 1 1 calc R . . H27B H 0.5456 0.0526 0.0437 0.119 Uiso 1 1 calc R . . H27C H 0.6597 0.0880 0.0322 0.119 Uiso 1 1 calc R . . C28 C 0.3516(6) 0.0543(5) 0.4903(4) 0.0635(15) Uani 1 1 d . . . C29 C 0.3386(7) -0.0314(5) 0.4602(5) 0.081(2) Uani 1 1 d . . . H29A H 0.4147 -0.0954 0.4581 0.122 Uiso 1 1 calc R . . H29B H 0.3229 -0.0233 0.3935 0.122 Uiso 1 1 calc R . . H29C H 0.2686 -0.0394 0.5063 0.122 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 Ag1 0.01873(15) 0.03654(18) 0.0411(2) 0.00330(13) -0.00130(12) -0.00115(12) Ag2 0.03588(17) 0.03991(18) 0.01731(15) 0.00383(11) -0.00503(12) -0.01298(14) S1 0.0248(5) 0.0358(5) 0.0325(5) 0.0024(4) -0.0061(4) -0.0062(4) S2 0.0360(5) 0.0464(6) 0.0309(5) 0.0082(4) -0.0110(4) -0.0174(5) F1 0.0502(16) 0.0611(17) 0.081(2) 0.0094(15) -0.0305(15) -0.0324(15) F2 0.0441(17) 0.065(2) 0.105(3) -0.0459(19) -0.0210(17) 0.0016(15) F3 0.073(2) 0.112(3) 0.0326(15) 0.0125(16) -0.0135(14) -0.052(2) F4 0.111(4) 0.079(3) 0.193(6) 0.051(3) -0.031(4) -0.057(3) F5 0.084(3) 0.061(2) 0.150(4) -0.044(2) -0.065(3) 0.021(2) F6 0.120(4) 0.075(3) 0.232(6) -0.046(3) -0.129(4) -0.005(2) O1 0.0277(15) 0.0420(17) 0.052(2) 0.0023(14) -0.0056(13) 0.0003(13) O2 0.0446(18) 0.069(2) 0.0372(18) 0.0248(16) -0.0114(14) -0.0237(17) O3 0.0299(14) 0.0369(15) 0.0409(17) 0.0046(12) -0.0107(12) -0.0149(12) O4 0.0388(18) 0.056(2) 0.062(2) -0.0057(17) -0.0118(16) -0.0135(16) O5 0.053(2) 0.057(2) 0.060(2) 0.0113(17) -0.0283(17) -0.0282(17) O6 0.077(3) 0.137(4) 0.045(2) 0.043(3) -0.015(2) -0.037(3) O7 0.065(3) 0.092(3) 0.075(3) 0.019(2) -0.017(2) -0.046(2) N1 0.0212(15) 0.0316(17) 0.0293(17) 0.0053(13) -0.0046(13) -0.0076(13) N2 0.0235(16) 0.0267(16) 0.0361(19) 0.0017(14) -0.0026(14) -0.0069(13) N3 0.0210(15) 0.0336(17) 0.0253(16) 0.0041(13) -0.0031(12) -0.0077(14) N4 0.0262(16) 0.0287(16) 0.0239(16) 0.0032(12) -0.0056(13) -0.0088(13) N5 0.0266(16) 0.0299(16) 0.0185(15) 0.0036(12) -0.0027(12) -0.0097(13) N6 0.0317(17) 0.0323(17) 0.0186(15) 0.0014(12) -0.0014(12) -0.0143(14) N7 0.0213(15) 0.0310(16) 0.0276(17) 0.0068(13) -0.0062(13) -0.0081(13) N8 0.0212(15) 0.0317(16) 0.0253(16) -0.0001(13) -0.0021(12) -0.0088(13) N9 0.0204(15) 0.0270(15) 0.0242(16) 0.0053(12) -0.0038(12) -0.0082(13) N10 0.0221(15) 0.0284(15) 0.0197(15) 0.0001(12) -0.0012(12) -0.0076(13) N11 0.0291(16) 0.0391(18) 0.0196(16) 0.0054(13) -0.0049(12) -0.0164(15) N12 0.0198(14) 0.0311(16) 0.0171(15) 0.0042(12) -0.0021(11) -0.0073(13) N13 0.101(5) 0.133(6) 0.090(5) 0.007(5) -0.020(4) -0.025(5) C1 0.0248(19) 0.039(2) 0.030(2) 0.0080(17) -0.0065(15) -0.0146(17) C2 0.034(2) 0.0283(19) 0.034(2) 0.0017(16) -0.0044(17) -0.0112(17) C3 0.023(2) 0.035(2) 0.062(3) -0.005(2) -0.0042(19) -0.0009(17) C4 0.0231(18) 0.0270(18) 0.0266(19) 0.0056(15) -0.0046(15) -0.0049(15) C5 0.0198(17) 0.035(2) 0.0250(19) 0.0080(16) -0.0025(14) -0.0057(16) C6 0.0226(18) 0.034(2) 0.037(2) 0.0011(17) -0.0031(16) -0.0071(16) C7 0.030(2) 0.036(2) 0.034(2) 0.0022(17) -0.0113(17) -0.0102(17) C8 0.032(2) 0.0296(19) 0.0240(19) 0.0057(15) -0.0091(15) -0.0145(16) C9 0.0285(19) 0.0278(18) 0.0194(18) 0.0023(14) -0.0021(14) -0.0142(16) C10 0.0272(19) 0.0300(19) 0.026(2) 0.0040(15) -0.0039(15) -0.0067(16) C11 0.0274(19) 0.032(2) 0.029(2) -0.0022(16) 0.0014(16) -0.0088(17) C12 0.039(2) 0.051(2) 0.0179(19) 0.0022(17) -0.0017(16) -0.021(2) C13 0.034(2) 0.041(2) 0.024(2) 0.0116(16) -0.0083(16) -0.0154(18) C14 0.030(2) 0.041(2) 0.0226(19) 0.0045(16) -0.0050(15) -0.0152(18) C15 0.0203(18) 0.043(2) 0.038(2) -0.0060(18) -0.0018(16) -0.0060(17) C16 0.0191(17) 0.0262(18) 0.0247(18) 0.0025(14) -0.0026(14) -0.0087(14) C17 0.0199(17) 0.0254(18) 0.0275(19) 0.0045(15) -0.0059(14) -0.0059(15) C18 0.0285(19) 0.034(2) 0.0237(19) 0.0039(15) -0.0033(15) -0.0136(17) C19 0.034(2) 0.033(2) 0.0235(19) -0.0006(15) -0.0025(16) -0.0154(17) C20 0.0183(17) 0.0309(19) 0.0192(18) 0.0003(14) -0.0005(13) -0.0055(15) C21 0.0148(16) 0.0284(18) 0.0192(17) 0.0037(14) -0.0007(13) -0.0052(14) C22 0.033(2) 0.045(2) 0.025(2) 0.0039(17) -0.0077(16) -0.0222(19) C23 0.0260(19) 0.0322(19) 0.028(2) 0.0060(15) -0.0064(15) -0.0124(16) C24 0.033(2) 0.039(2) 0.0177(18) 0.0058(15) -0.0043(15) -0.0157(17) C25 0.031(2) 0.050(3) 0.052(3) -0.002(2) -0.012(2) -0.014(2) C26 0.059(4) 0.062(4) 0.105(5) -0.014(4) -0.047(4) -0.007(3) C27 0.102(5) 0.083(4) 0.076(5) 0.012(4) -0.032(4) -0.056(4) C28 0.061(4) 0.063(4) 0.049(3) -0.006(3) -0.009(3) -0.009(3) C29 0.089(5) 0.078(4) 0.060(4) 0.016(3) -0.008(3) -0.023(4) _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 N3 2.311(3) . yes Ag1 N7 2.318(3) . yes Ag1 N9 2.354(3) . yes Ag1 N1 2.387(3) . yes Ag1 Ag2 3.3348(5) . yes Ag2 N4 2.307(3) . yes Ag2 N10 2.313(3) . yes Ag2 N5 2.385(3) . yes Ag2 N11 2.396(3) . yes S1 O1 1.432(3) . ? S1 O3 1.437(3) . ? S1 O2 1.453(3) . ? S1 C25 1.811(5) . ? S2 O6 1.421(4) . ? S2 O5 1.436(3) . ? S2 O4 1.443(3) . ? S2 C26 1.821(7) . ? F1 C25 1.327(5) . ? F2 C25 1.321(5) . ? F3 C25 1.353(6) . ? F4 C26 1.349(9) . ? F5 C26 1.288(7) . ? F6 C26 1.339(7) . ? O7 C27 1.413(8) . ? O7 H7O 0.9843 . ? N1 C4 1.341(5) . ? N1 C1 1.363(5) . ? N2 C2 1.356(5) . ? N2 C4 1.363(5) . ? N2 C3 1.474(5) . ? N3 C5 1.266(5) . ? N3 C6 1.458(5) . ? N4 C8 1.271(5) . ? N4 C7 1.479(5) . ? N5 C9 1.325(5) . ? N5 C10 1.366(5) . ? N6 C11 1.358(5) . ? N6 C9 1.360(5) . ? N6 C12 1.474(5) . ? N7 C16 1.328(5) . ? N7 C13 1.362(5) . ? N8 C16 1.359(5) . ? N8 C14 1.360(5) . ? N8 C15 1.470(5) . ? N9 C17 1.274(5) . ? N9 C18 1.458(5) . ? N10 C20 1.270(5) . ? N10 C19 1.463(5) . ? N11 C21 1.333(5) . ? N11 C22 1.363(5) . ? N12 C23 1.360(5) . ? N12 C21 1.361(5) . ? N12 C24 1.462(5) . ? N13 C28 1.246(10) . ? C1 C2 1.366(5) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.446(6) . ? C5 H5 0.9500 . ? C6 C7 1.514(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.447(5) . ? C8 H8 0.9500 . ? C10 C11 1.354(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.358(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.453(5) . ? C17 H17 0.9500 . ? C18 C19 1.516(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.454(5) . ? C20 H20 0.9500 . ? C22 C23 1.361(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.314(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N7 133.85(11) . . ? N3 Ag1 N9 139.94(11) . . ? N7 Ag1 N9 73.70(10) . . yes N3 Ag1 N1 73.88(11) . . yes N7 Ag1 N1 129.95(11) . . ? N9 Ag1 N1 113.17(11) . . ? N3 Ag1 Ag2 79.85(8) . . ? N7 Ag1 Ag2 96.02(8) . . ? N9 Ag1 Ag2 66.98(7) . . ? N1 Ag1 Ag2 133.24(8) . . ? N4 Ag2 N10 144.84(11) . . ? N4 Ag2 N5 73.56(10) . . yes N10 Ag2 N5 128.61(10) . . ? N4 Ag2 N11 126.07(11) . . ? N10 Ag2 N11 72.99(11) . . yes N5 Ag2 N11 116.20(11) . . ? N4 Ag2 Ag1 66.86(8) . . ? N10 Ag2 Ag1 83.00(8) . . ? N5 Ag2 Ag1 94.23(7) . . ? N11 Ag2 Ag1 148.83(8) . . ? O1 S1 O3 115.95(19) . . ? O1 S1 O2 114.7(2) . . ? O3 S1 O2 114.45(18) . . ? O1 S1 C25 104.0(2) . . ? O3 S1 C25 103.35(19) . . ? O2 S1 C25 101.9(2) . . ? O6 S2 O5 113.4(3) . . ? O6 S2 O4 113.7(2) . . ? O5 S2 O4 115.2(2) . . ? O6 S2 C26 106.6(4) . . ? O5 S2 C26 103.2(2) . . ? O4 S2 C26 103.1(3) . . ? C27 O7 H7O 111.6 . . ? C4 N1 C1 105.8(3) . . ? C4 N1 Ag1 107.0(2) . . ? C1 N1 Ag1 146.7(3) . . ? C2 N2 C4 107.0(3) . . ? C2 N2 C3 126.2(3) . . ? C4 N2 C3 126.8(3) . . ? C5 N3 C6 117.5(3) . . ? C5 N3 Ag1 114.5(3) . . ? C6 N3 Ag1 128.0(2) . . ? C8 N4 C7 117.4(3) . . ? C8 N4 Ag2 114.8(2) . . ? C7 N4 Ag2 127.9(2) . . ? C9 N5 C10 105.5(3) . . ? C9 N5 Ag2 108.0(2) . . ? C10 N5 Ag2 146.5(3) . . ? C11 N6 C9 107.0(3) . . ? C11 N6 C12 125.5(3) . . ? C9 N6 C12 127.5(3) . . ? C16 N7 C13 105.5(3) . . ? C16 N7 Ag1 109.8(2) . . ? C13 N7 Ag1 144.1(3) . . ? C16 N8 C14 106.8(3) . . ? C16 N8 C15 127.9(3) . . ? C14 N8 C15 125.4(3) . . ? C17 N9 C18 118.2(3) . . ? C17 N9 Ag1 113.5(2) . . ? C18 N9 Ag1 128.3(2) . . ? C20 N10 C19 117.8(3) . . ? C20 N10 Ag2 116.0(3) . . ? C19 N10 Ag2 126.1(2) . . ? C21 N11 C22 105.1(3) . . ? C21 N11 Ag2 108.6(2) . . ? C22 N11 Ag2 146.0(3) . . ? C23 N12 C21 106.8(3) . . ? C23 N12 C24 125.5(3) . . ? C21 N12 C24 127.6(3) . . ? N1 C1 C2 109.6(3) . . ? N1 C1 H1 125.2 . . ? C2 C1 H1 125.2 . . ? N2 C2 C1 107.1(3) . . ? N2 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 110.5(3) . . ? N1 C4 C5 124.0(3) . . ? N2 C4 C5 125.3(3) . . ? N3 C5 C4 119.6(3) . . ? N3 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N3 C6 C7 112.7(3) . . ? N3 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N3 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N4 C7 C6 111.0(3) . . ? N4 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C9 119.3(3) . . ? N4 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? N5 C9 N6 110.8(3) . . ? N5 C9 C8 124.0(3) . . ? N6 C9 C8 125.1(3) . . ? C11 C10 N5 110.1(3) . . ? C11 C10 H10 125.0 . . ? N5 C10 H10 125.0 . . ? C10 C11 N6 106.6(3) . . ? C10 C11 H11 126.7 . . ? N6 C11 H11 126.7 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N7 110.0(3) . . ? C14 C13 H13 125.0 . . ? N7 C13 H13 125.0 . . ? C13 C14 N8 106.7(3) . . ? C13 C14 H14 126.7 . . ? N8 C14 H14 126.7 . . ? N8 C15 H15A 109.5 . . ? N8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 111.0(3) . . ? N7 C16 C17 123.8(3) . . ? N8 C16 C17 125.1(3) . . ? N9 C17 C16 118.5(3) . . ? N9 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N9 C18 C19 110.7(3) . . ? N9 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N9 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N10 C19 C18 111.7(3) . . ? N10 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? N10 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? N10 C20 C21 118.8(3) . . ? N10 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N11 C21 N12 111.1(3) . . ? N11 C21 C20 123.5(3) . . ? N12 C21 C20 125.3(3) . . ? C23 C22 N11 110.4(3) . . ? C23 C22 H22 124.8 . . ? N11 C22 H22 124.8 . . ? N12 C23 C22 106.5(3) . . ? N12 C23 H23 126.7 . . ? C22 C23 H23 126.7 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F2 C25 F1 107.6(4) . . ? F2 C25 F3 108.6(4) . . ? F1 C25 F3 107.3(4) . . ? F2 C25 S1 111.4(3) . . ? F1 C25 S1 112.1(3) . . ? F3 C25 S1 109.7(3) . . ? F5 C26 F6 108.1(5) . . ? F5 C26 F4 107.7(6) . . ? F6 C26 F4 110.5(7) . . ? F5 C26 S2 112.6(5) . . ? F6 C26 S2 109.6(5) . . ? F4 C26 S2 108.3(4) . . ? O7 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N13 C28 C29 177.3(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O7 H7O O6 0.98 2.30 2.975(6) 124.6 . yes _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.448 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.110 #===END======================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 855060' #TrackingRef 'Koskinen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Ag2 N12, 2(C F3 O3 S), 0.5(H2 O)' _chemical_formula_sum 'C52 H66 Ag4 F12 N24 O13 S4' _chemical_formula_weight 2023.01 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2630(4) _cell_length_b 12.8443(3) _cell_length_c 13.4111(4) _cell_angle_alpha 95.896(2) _cell_angle_beta 98.347(2) _cell_angle_gamma 107.469(2) _cell_volume 1808.90(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26106 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8193 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008)' _publ_section_exptl_refinement ; One of the CF~3~SO~3~ anions was disordered over two sites with occupancies 0.74/0.26. The S---O, C---F, O...O, and F...F distances in the minor component were restrained to be equal. Furthermore, oxygen atom O4B was restrained so that its U~ij~ components approximate to isotropic behavior. The H~2~O hydrogen atoms were located from the difference Fourier map. The coordinates of these hydrogens were fixed with U~iso~ = 1.5 U~eq~(O7). Other hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.52 \%A from atom F2 and the deepest hole is located 0.76 \%A from atom Ag1. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32947 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8289 _reflns_number_gt 6079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2008)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond v.3.1f (Brandenburg, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0366P)^2^+1.1115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8289 _refine_ls_number_parameters 573 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _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 0.61740(2) 0.41945(2) 0.700086(19) 0.02686(8) Uani 1 1 d . . . Ag2 Ag 0.58819(2) 0.186176(19) 0.773378(17) 0.02562(8) Uani 1 1 d . . . N1 N 0.7182(3) 0.5916(2) 0.8132(2) 0.0257(6) Uani 1 1 d . . . N2 N 0.8888(3) 0.6807(2) 0.9313(2) 0.0280(6) Uani 1 1 d . . . N3 N 0.8210(3) 0.4238(2) 0.7612(2) 0.0235(6) Uani 1 1 d . . . N4 N 0.6824(2) 0.2118(2) 0.63092(19) 0.0217(6) Uani 1 1 d . . . N5 N 0.4273(2) 0.0984(2) 0.62954(19) 0.0200(6) Uani 1 1 d . . . N6 N 0.3810(2) 0.0805(2) 0.46024(19) 0.0210(6) Uani 1 1 d . . . N7 N 0.4582(3) 0.3646(2) 0.5622(2) 0.0233(6) Uani 1 1 d . . . N8 N 0.2509(3) 0.3048(2) 0.5069(2) 0.0250(6) Uani 1 1 d . . . N9 N 0.4244(2) 0.3508(2) 0.76450(19) 0.0199(6) Uani 1 1 d . . . N10 N 0.5658(2) 0.2680(2) 0.92596(18) 0.0192(5) Uani 1 1 d . . . N11 N 0.6556(2) 0.0866(2) 0.90233(19) 0.0232(6) Uani 1 1 d . . . N12 N 0.6556(2) 0.0679(2) 1.06509(19) 0.0202(6) Uani 1 1 d . . . C1 C 0.6977(3) 0.6789(3) 0.8667(3) 0.0298(8) Uani 1 1 d . . . H1 H 0.6225 0.6984 0.8549 0.036 Uiso 1 1 calc R . . C2 C 0.8022(4) 0.7341(3) 0.9400(3) 0.0333(8) Uani 1 1 d . . . H2 H 0.8123 0.7975 0.9878 0.040 Uiso 1 1 calc R . . C3 C 1.0155(4) 0.7121(3) 0.9926(3) 0.0450(10) Uani 1 1 d . . . H3A H 1.0255 0.6500 1.0258 0.067 Uiso 1 1 calc R . . H3B H 1.0278 0.7757 1.0446 0.067 Uiso 1 1 calc R . . H3C H 1.0785 0.7318 0.9486 0.067 Uiso 1 1 calc R . . C4 C 0.8335(3) 0.5939(3) 0.8536(2) 0.0240(7) Uani 1 1 d . . . C5 C 0.8891(3) 0.5097(3) 0.8232(2) 0.0247(7) Uani 1 1 d . . . H5 H 0.9752 0.5189 0.8493 0.030 Uiso 1 1 calc R . . C6 C 0.8772(3) 0.3370(3) 0.7373(3) 0.0265(7) Uani 1 1 d . . . H6A H 0.8663 0.2872 0.7893 0.032 Uiso 1 1 calc R . . H6B H 0.9691 0.3712 0.7398 0.032 Uiso 1 1 calc R . . C7 C 0.8166(3) 0.2703(3) 0.6329(2) 0.0261(7) Uani 1 1 d . . . H7A H 0.8244 0.3200 0.5807 0.031 Uiso 1 1 calc R . . H7B H 0.8607 0.2164 0.6167 0.031 Uiso 1 1 calc R . . C8 C 0.6066(3) 0.1744(2) 0.5457(2) 0.0217(7) Uani 1 1 d . . . H8 H 0.6365 0.1843 0.4835 0.026 Uiso 1 1 calc R . . C9 C 0.4747(3) 0.1170(2) 0.5446(2) 0.0200(7) Uani 1 1 d . . . C10 C 0.2996(3) 0.0488(2) 0.5972(2) 0.0228(7) Uani 1 1 d . . . H10 H 0.2404 0.0255 0.6406 0.027 Uiso 1 1 calc R . . C11 C 0.2698(3) 0.0377(3) 0.4939(3) 0.0250(7) Uani 1 1 d . . . H11 H 0.1877 0.0062 0.4530 0.030 Uiso 1 1 calc R . . C12 C 0.3946(3) 0.0837(3) 0.3541(2) 0.0290(8) Uani 1 1 d . . . H12A H 0.4112 0.1596 0.3400 0.043 Uiso 1 1 calc R . . H12B H 0.3164 0.0357 0.3094 0.043 Uiso 1 1 calc R . . H12C H 0.4654 0.0579 0.3415 0.043 Uiso 1 1 calc R . . C13 C 0.4340(3) 0.3670(2) 0.4594(2) 0.0257(7) Uani 1 1 d . . . H13 H 0.4964 0.3900 0.4186 0.031 Uiso 1 1 calc R . . C14 C 0.3069(3) 0.3312(3) 0.4249(3) 0.0292(8) Uani 1 1 d . . . H14 H 0.2649 0.3256 0.3569 0.035 Uiso 1 1 calc R . . C15 C 0.1146(3) 0.2637(3) 0.5057(3) 0.0367(9) Uani 1 1 d . . . H15A H 0.0684 0.2585 0.4366 0.055 Uiso 1 1 calc R . . H15B H 0.0917 0.3146 0.5530 0.055 Uiso 1 1 calc R . . H15C H 0.0925 0.1904 0.5266 0.055 Uiso 1 1 calc R . . C16 C 0.3463(3) 0.3271(2) 0.5888(2) 0.0214(7) Uani 1 1 d . . . C17 C 0.3276(3) 0.3173(2) 0.6929(2) 0.0212(7) Uani 1 1 d . . . H17 H 0.2452 0.2865 0.7072 0.025 Uiso 1 1 calc R . . C18 C 0.4032(3) 0.3519(3) 0.8695(2) 0.0223(7) Uani 1 1 d . . . H18A H 0.3387 0.2817 0.8750 0.027 Uiso 1 1 calc R . . H18B H 0.3706 0.4132 0.8884 0.027 Uiso 1 1 calc R . . C19 C 0.5252(3) 0.3660(2) 0.9420(2) 0.0221(7) Uani 1 1 d . . . H19A H 0.5922 0.4318 0.9311 0.027 Uiso 1 1 calc R . . H19B H 0.5124 0.3782 1.0133 0.027 Uiso 1 1 calc R . . C20 C 0.5866(3) 0.2209(2) 1.0026(2) 0.0188(6) Uani 1 1 d . . . H20 H 0.5731 0.2474 1.0674 0.023 Uiso 1 1 calc R . . C21 C 0.6310(3) 0.1264(2) 0.9897(2) 0.0204(7) Uani 1 1 d . . . C22 C 0.6986(3) 0.0007(3) 0.9233(3) 0.0269(7) Uani 1 1 d . . . H22 H 0.7246 -0.0436 0.8754 0.032 Uiso 1 1 calc R . . C23 C 0.6986(3) -0.0116(3) 1.0228(2) 0.0247(7) Uani 1 1 d . . . H23 H 0.7238 -0.0653 1.0563 0.030 Uiso 1 1 calc R . . C24 C 0.6420(3) 0.0863(3) 1.1716(2) 0.0276(8) Uani 1 1 d . . . H24A H 0.6222 0.0158 1.1979 0.041 Uiso 1 1 calc R . . H24B H 0.5733 0.1176 1.1763 0.041 Uiso 1 1 calc R . . H24C H 0.7214 0.1377 1.2121 0.041 Uiso 1 1 calc R . . C25 C 0.9843(3) -0.0672(3) 0.7905(3) 0.0403(10) Uani 1 1 d . . . F1 F 0.8668(2) -0.13038(17) 0.74569(19) 0.0512(6) Uani 1 1 d . . . F2 F 1.0631(3) -0.1179(2) 0.7660(3) 0.0854(10) Uani 1 1 d . . . F3 F 0.9908(2) -0.0609(2) 0.8914(2) 0.0690(9) Uani 1 1 d . . . S1 S 1.02096(8) 0.06975(7) 0.75500(6) 0.02579(19) Uani 1 1 d . . . O1 O 0.9193(3) 0.1054(2) 0.7826(2) 0.0485(7) Uani 1 1 d . . . O2 O 1.0167(2) 0.0510(3) 0.64761(18) 0.0507(8) Uani 1 1 d . . . O3 O 1.1450(2) 0.1258(2) 0.81453(19) 0.0434(7) Uani 1 1 d . . . C26 C 0.8286(5) 0.3989(4) 0.3674(4) 0.0343(12) Uani 0.743(3) 1 d P A 1 F4 F 0.7857(5) 0.4496(4) 0.4396(3) 0.0520(11) Uani 0.743(3) 1 d P A 1 F5 F 0.8031(7) 0.2934(5) 0.3789(5) 0.0522(17) Uani 0.743(3) 1 d P A 1 F6 F 0.9533(10) 0.4431(9) 0.3850(6) 0.054(3) Uani 0.743(3) 1 d P A 1 S2 S 0.75837(11) 0.41257(10) 0.24006(10) 0.0280(4) Uani 0.743(3) 1 d P A 1 O4 O 0.8050(7) 0.5296(6) 0.2395(5) 0.0415(16) Uani 0.743(3) 1 d P A 1 O5 O 0.6249(6) 0.3648(5) 0.2375(5) 0.0416(15) Uani 0.743(3) 1 d P A 1 O6 O 0.8105(3) 0.3483(3) 0.1750(2) 0.0306(8) Uani 0.743(3) 1 d P A 1 C26B C 0.8586(12) 0.3523(10) 0.3244(9) 0.027(3) Uani 0.257(3) 1 d PD A 2 F4B F 0.969(3) 0.428(2) 0.3755(17) 0.040(6) Uani 0.257(3) 1 d PD A 2 F6B F 0.8777(8) 0.3171(6) 0.2314(6) 0.036(2) Uani 0.257(3) 1 d PD A 2 F5B F 0.8306(16) 0.2646(12) 0.3752(14) 0.036(4) Uani 0.257(3) 1 d PD A 2 S2B S 0.7306(3) 0.4121(3) 0.3129(3) 0.0322(13) Uani 0.257(3) 1 d PD A 2 O4B O 0.779(2) 0.5029(14) 0.2569(14) 0.040(5) Uani 0.257(3) 1 d PDU A 2 O5B O 0.7233(12) 0.4480(13) 0.4173(10) 0.047(4) Uani 0.257(3) 1 d PD A 2 O6B O 0.6202(18) 0.3229(11) 0.2565(12) 0.037(4) Uani 0.257(3) 1 d PD A 2 O7 O 0.8323(11) 0.4834(11) 0.0566(10) 0.172(5) Uani 0.50 1 d P . . H7O H 0.8233 0.5231 0.1191 0.258 Uiso 0.50 1 d P . . H7P H 0.8299 0.4176 0.0699 0.258 Uiso 0.50 1 d P . . 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 0.02004(14) 0.02515(14) 0.02983(15) 0.00344(11) -0.00123(11) 0.00206(11) Ag2 0.03298(16) 0.02671(14) 0.01422(13) 0.00242(10) 0.00384(11) 0.00573(11) N1 0.0269(16) 0.0240(14) 0.0236(15) 0.0059(11) 0.0066(12) 0.0027(12) N2 0.0319(17) 0.0259(15) 0.0222(15) 0.0002(12) 0.0007(13) 0.0068(13) N3 0.0235(15) 0.0215(14) 0.0222(14) 0.0030(11) 0.0034(12) 0.0030(12) N4 0.0203(14) 0.0221(13) 0.0200(14) 0.0005(11) 0.0030(12) 0.0043(11) N5 0.0189(14) 0.0205(13) 0.0188(14) 0.0012(11) 0.0031(11) 0.0047(11) N6 0.0241(15) 0.0218(13) 0.0154(13) -0.0015(10) -0.0016(11) 0.0089(12) N7 0.0254(16) 0.0186(13) 0.0233(14) 0.0063(11) 0.0012(12) 0.0038(11) N8 0.0264(16) 0.0228(14) 0.0218(15) 0.0041(11) -0.0025(12) 0.0050(12) N9 0.0207(15) 0.0189(13) 0.0190(14) 0.0023(11) 0.0003(11) 0.0066(11) N10 0.0165(14) 0.0203(13) 0.0179(13) 0.0019(10) 0.0004(11) 0.0032(11) N11 0.0236(15) 0.0280(14) 0.0200(14) 0.0060(11) 0.0034(12) 0.0105(12) N12 0.0173(14) 0.0228(13) 0.0183(13) 0.0051(11) 0.0007(11) 0.0037(11) C1 0.031(2) 0.0240(17) 0.034(2) 0.0053(15) 0.0132(16) 0.0046(15) C2 0.045(2) 0.0251(18) 0.0275(19) 0.0018(15) 0.0136(17) 0.0053(17) C3 0.057(3) 0.038(2) 0.029(2) -0.0083(17) -0.0109(19) 0.013(2) C4 0.0267(19) 0.0213(16) 0.0182(16) 0.0027(13) 0.0025(14) 0.0003(14) C5 0.0211(18) 0.0278(18) 0.0218(17) 0.0054(14) 0.0023(14) 0.0030(14) C6 0.0214(18) 0.0245(17) 0.0281(18) -0.0005(14) 0.0007(14) 0.0025(14) C7 0.0195(18) 0.0293(18) 0.0260(18) -0.0008(14) 0.0066(14) 0.0032(14) C8 0.0230(18) 0.0235(16) 0.0188(16) 0.0019(13) 0.0079(14) 0.0062(14) C9 0.0222(17) 0.0187(15) 0.0164(16) -0.0009(12) -0.0005(13) 0.0058(13) C10 0.0204(18) 0.0223(16) 0.0248(17) 0.0030(13) 0.0023(14) 0.0069(14) C11 0.0147(17) 0.0240(17) 0.0325(19) 0.0016(14) -0.0033(14) 0.0051(13) C12 0.033(2) 0.0352(19) 0.0175(17) -0.0011(14) -0.0006(15) 0.0128(16) C13 0.033(2) 0.0188(16) 0.0216(17) 0.0064(13) 0.0017(15) 0.0039(14) C14 0.041(2) 0.0205(16) 0.0209(17) 0.0028(13) -0.0058(16) 0.0070(15) C15 0.025(2) 0.048(2) 0.033(2) 0.0096(17) -0.0024(16) 0.0075(17) C16 0.0226(18) 0.0152(15) 0.0235(17) 0.0037(12) -0.0013(14) 0.0043(13) C17 0.0200(17) 0.0164(15) 0.0260(17) 0.0053(13) 0.0019(14) 0.0044(13) C18 0.0236(18) 0.0214(16) 0.0210(17) 0.0012(13) 0.0059(14) 0.0059(14) C19 0.0269(18) 0.0212(16) 0.0157(16) 0.0005(12) 0.0003(13) 0.0063(14) C20 0.0162(16) 0.0207(15) 0.0148(15) 0.0006(12) 0.0013(12) 0.0004(13) C21 0.0176(16) 0.0234(16) 0.0174(16) 0.0060(13) 0.0015(13) 0.0021(13) C22 0.0246(19) 0.0297(18) 0.0262(18) 0.0017(14) 0.0013(15) 0.0107(15) C23 0.0222(18) 0.0231(16) 0.0267(18) 0.0042(14) -0.0019(14) 0.0070(14) C24 0.0301(19) 0.0324(18) 0.0170(16) 0.0072(14) 0.0001(14) 0.0062(15) C25 0.024(2) 0.031(2) 0.056(3) 0.0047(18) -0.0080(18) 0.0021(16) F1 0.0319(13) 0.0299(11) 0.0716(17) 0.0026(11) -0.0155(12) -0.0063(10) F2 0.0483(17) 0.0406(14) 0.162(3) -0.0039(17) -0.0106(18) 0.0266(13) F3 0.0530(16) 0.0704(17) 0.0573(17) 0.0430(14) -0.0180(13) -0.0167(13) S1 0.0235(5) 0.0257(4) 0.0242(4) 0.0060(3) 0.0002(3) 0.0034(3) O1 0.0481(18) 0.0377(15) 0.0650(19) 0.0020(14) 0.0157(15) 0.0211(13) O2 0.0268(15) 0.092(2) 0.0219(14) 0.0132(14) 0.0000(11) 0.0031(14) O3 0.0353(15) 0.0361(14) 0.0397(15) 0.0143(12) -0.0137(12) -0.0097(12) C26 0.036(3) 0.035(3) 0.028(3) 0.001(2) 0.002(2) 0.009(3) F4 0.063(3) 0.054(2) 0.033(2) -0.0113(16) 0.010(2) 0.016(3) F5 0.082(5) 0.040(3) 0.032(2) 0.014(2) 0.009(3) 0.015(2) F6 0.039(4) 0.073(6) 0.041(3) 0.005(3) -0.015(3) 0.015(3) S2 0.0203(7) 0.0310(7) 0.0281(8) 0.0009(5) -0.0020(5) 0.0056(5) O4 0.032(4) 0.028(3) 0.061(3) 0.012(2) -0.003(3) 0.009(2) O5 0.019(2) 0.050(4) 0.046(3) -0.010(3) 0.005(2) 0.003(3) O6 0.0279(19) 0.0344(18) 0.0282(18) 0.0009(14) 0.0058(15) 0.0092(15) C26B 0.031(8) 0.023(7) 0.035(8) 0.004(6) 0.012(7) 0.015(7) F4B 0.015(8) 0.025(6) 0.066(12) 0.008(6) 0.004(6) -0.011(8) F6B 0.041(5) 0.027(4) 0.045(5) 0.006(4) 0.019(4) 0.016(4) F5B 0.030(6) 0.038(9) 0.044(7) 0.028(7) 0.002(5) 0.011(5) S2B 0.031(2) 0.0287(19) 0.041(3) 0.0040(16) 0.0126(18) 0.0147(16) O4B 0.042(8) 0.024(9) 0.062(8) 0.013(6) 0.025(6) 0.012(6) O5B 0.030(8) 0.064(8) 0.043(9) -0.023(6) 0.007(7) 0.018(8) O6B 0.040(8) 0.030(8) 0.036(8) -0.004(6) -0.001(6) 0.010(7) O7 0.104(8) 0.186(12) 0.199(13) 0.093(10) -0.009(8) 0.004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N7 2.268(3) . yes Ag1 N3 2.302(3) . yes Ag1 N1 2.405(3) . yes Ag1 N9 2.408(3) . yes Ag1 Ag2 3.1873(3) . yes Ag2 N10 2.285(2) . yes Ag2 N4 2.322(3) . yes Ag2 N5 2.364(2) . yes Ag2 N11 2.421(2) . yes N1 C4 1.322(4) . ? N1 C1 1.366(4) . ? N2 C2 1.362(4) . ? N2 C4 1.368(4) . ? N2 C3 1.456(5) . ? N3 C5 1.271(4) . ? N3 C6 1.468(4) . ? N4 C8 1.274(4) . ? N4 C7 1.468(4) . ? N5 C9 1.340(4) . ? N5 C10 1.369(4) . ? N6 C9 1.364(4) . ? N6 C11 1.370(4) . ? N6 C12 1.457(4) . ? N7 C16 1.323(4) . ? N7 C13 1.371(4) . ? N8 C16 1.361(4) . ? N8 C14 1.367(4) . ? N8 C15 1.463(4) . ? N9 C17 1.275(4) . ? N9 C18 1.461(4) . ? N10 C20 1.273(4) . ? N10 C19 1.469(4) . ? N11 C21 1.329(4) . ? N11 C22 1.369(4) . ? N12 C23 1.363(4) . ? N12 C21 1.365(4) . ? N12 C24 1.461(4) . ? C1 C2 1.369(5) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.455(5) . ? C5 H5 0.9500 . ? C6 C7 1.511(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.444(4) . ? C8 H8 0.9500 . ? C10 C11 1.358(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.357(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.454(4) . ? C17 H17 0.9500 . ? C18 C19 1.515(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.449(4) . ? C20 H20 0.9500 . ? C22 C23 1.360(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 F2 1.307(5) . ? C25 F3 1.337(5) . ? C25 F1 1.340(4) . ? C25 S1 1.812(4) . ? S1 O2 1.427(3) . ? S1 O1 1.435(3) . ? S1 O3 1.436(3) . ? C26 F6 1.323(11) . ? C26 F5 1.329(8) . ? C26 F4 1.339(7) . ? C26 S2 1.823(5) . ? S2 O5 1.437(6) . ? S2 O4 1.437(6) . ? S2 O6 1.442(3) . ? C26B F6B 1.351(13) . ? C26B F5B 1.357(16) . ? C26B F4B 1.363(17) . ? C26B S2B 1.821(14) . ? S2B O5B 1.451(13) . ? S2B O6B 1.457(15) . ? S2B O4B 1.462(13) . ? O7 H7O 0.9701 . ? O7 H7P 0.8750 . ? 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 N7 Ag1 N3 144.53(10) . . ? N7 Ag1 N1 133.29(9) . . ? N3 Ag1 N1 73.26(9) . . yes N7 Ag1 N9 73.82(9) . . yes N3 Ag1 N9 131.06(9) . . ? N1 Ag1 N9 100.81(9) . . ? N7 Ag1 Ag2 99.01(6) . . ? N3 Ag1 Ag2 74.91(6) . . ? N1 Ag1 Ag2 122.46(6) . . ? N9 Ag1 Ag2 68.05(6) . . ? N10 Ag2 N4 145.82(9) . . ? N10 Ag2 N5 127.33(9) . . ? N4 Ag2 N5 73.38(9) . . yes N10 Ag2 N11 73.33(9) . . yes N4 Ag2 N11 121.69(9) . . ? N5 Ag2 N11 122.74(9) . . ? N10 Ag2 Ag1 85.91(6) . . ? N4 Ag2 Ag1 65.33(6) . . ? N5 Ag2 Ag1 90.18(6) . . ? N11 Ag2 Ag1 147.06(6) . . ? C4 N1 C1 105.9(3) . . ? C4 N1 Ag1 108.1(2) . . ? C1 N1 Ag1 144.5(2) . . ? C2 N2 C4 106.4(3) . . ? C2 N2 C3 126.0(3) . . ? C4 N2 C3 127.6(3) . . ? C5 N3 C6 117.9(3) . . ? C5 N3 Ag1 115.6(2) . . ? C6 N3 Ag1 126.48(19) . . ? C8 N4 C7 119.7(3) . . ? C8 N4 Ag2 114.8(2) . . ? C7 N4 Ag2 125.40(19) . . ? C9 N5 C10 105.4(3) . . ? C9 N5 Ag2 109.12(19) . . ? C10 N5 Ag2 144.5(2) . . ? C9 N6 C11 106.8(3) . . ? C9 N6 C12 127.4(3) . . ? C11 N6 C12 125.8(3) . . ? C16 N7 C13 105.9(3) . . ? C16 N7 Ag1 111.5(2) . . ? C13 N7 Ag1 142.0(2) . . ? C16 N8 C14 106.6(3) . . ? C16 N8 C15 127.4(3) . . ? C14 N8 C15 126.0(3) . . ? C17 N9 C18 117.9(3) . . ? C17 N9 Ag1 111.7(2) . . ? C18 N9 Ag1 130.18(19) . . ? C20 N10 C19 118.0(3) . . ? C20 N10 Ag2 116.0(2) . . ? C19 N10 Ag2 126.03(18) . . ? C21 N11 C22 105.6(3) . . ? C21 N11 Ag2 107.03(19) . . ? C22 N11 Ag2 147.1(2) . . ? C23 N12 C21 106.7(3) . . ? C23 N12 C24 125.5(3) . . ? C21 N12 C24 127.8(3) . . ? N1 C1 C2 109.6(3) . . ? N1 C1 H1 125.2 . . ? C2 C1 H1 125.2 . . ? N2 C2 C1 106.8(3) . . ? N2 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 111.3(3) . . ? N1 C4 C5 123.6(3) . . ? N2 C4 C5 125.0(3) . . ? N3 C5 C4 119.2(3) . . ? N3 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N3 C6 C7 111.5(3) . . ? N3 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N4 C7 C6 109.7(3) . . ? N4 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N4 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 119.3(3) . . ? N4 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? N5 C9 N6 110.9(3) . . ? N5 C9 C8 123.2(3) . . ? N6 C9 C8 125.9(3) . . ? C11 C10 N5 110.2(3) . . ? C11 C10 H10 124.9 . . ? N5 C10 H10 124.9 . . ? C10 C11 N6 106.8(3) . . ? C10 C11 H11 126.6 . . ? N6 C11 H11 126.6 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N7 109.5(3) . . ? C14 C13 H13 125.2 . . ? N7 C13 H13 125.2 . . ? C13 C14 N8 106.9(3) . . ? C13 C14 H14 126.6 . . ? N8 C14 H14 126.6 . . ? N8 C15 H15A 109.5 . . ? N8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 111.1(3) . . ? N7 C16 C17 124.4(3) . . ? N8 C16 C17 124.5(3) . . ? N9 C17 C16 118.5(3) . . ? N9 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N9 C18 C19 110.5(3) . . ? N9 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N9 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N10 C19 C18 110.9(2) . . ? N10 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? N10 C20 C21 119.1(3) . . ? N10 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N11 C21 N12 111.0(3) . . ? N11 C21 C20 124.0(3) . . ? N12 C21 C20 125.0(3) . . ? C23 C22 N11 109.9(3) . . ? C23 C22 H22 125.0 . . ? N11 C22 H22 125.0 . . ? C22 C23 N12 106.8(3) . . ? C22 C23 H23 126.6 . . ? N12 C23 H23 126.6 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F2 C25 F3 107.2(3) . . ? F2 C25 F1 108.1(3) . . ? F3 C25 F1 107.6(3) . . ? F2 C25 S1 112.4(3) . . ? F3 C25 S1 110.2(3) . . ? F1 C25 S1 111.1(3) . . ? O2 S1 O1 113.71(17) . . ? O2 S1 O3 114.66(16) . . ? O1 S1 O3 116.74(17) . . ? O2 S1 C25 104.09(19) . . ? O1 S1 C25 102.39(18) . . ? O3 S1 C25 102.77(15) . . ? F6 C26 F5 107.0(7) . . ? F6 C26 F4 107.3(7) . . ? F5 C26 F4 108.3(5) . . ? F6 C26 S2 111.5(5) . . ? F5 C26 S2 111.2(4) . . ? F4 C26 S2 111.4(4) . . ? O5 S2 O4 116.8(4) . . ? O5 S2 O6 114.4(3) . . ? O4 S2 O6 114.5(4) . . ? O5 S2 C26 103.0(3) . . ? O4 S2 C26 102.9(3) . . ? O6 S2 C26 102.6(2) . . ? F6B C26B F5B 108.1(11) . . ? F6B C26B F4B 107.8(14) . . ? F5B C26B F4B 108.7(13) . . ? F6B C26B S2B 110.8(8) . . ? F5B C26B S2B 110.5(10) . . ? F4B C26B S2B 110.9(19) . . ? O5B S2B O6B 115.0(8) . . ? O5B S2B O4B 113.8(9) . . ? O6B S2B O4B 114.9(9) . . ? O5B S2B C26B 104.5(7) . . ? O6B S2B C26B 104.8(9) . . ? O4B S2B C26B 101.6(11) . . ? H7O O7 H7P 105.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O7 H7O O4 0.97 1.65 2.548(16) 151.3 . yes O7 H7O O4B 0.97 2.00 2.84(2) 142.7 . yes O7 H7O S2 0.97 2.32 2.859(13) 114.3 . yes O7 H7P O6 0.87 1.75 2.452(12) 135.7 . yes _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.794 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.103 #===END======================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 855061' #TrackingRef 'Koskinen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Ag2 N12, C H4 O, 2(Cl O3)' _chemical_formula_sum 'C25 H36 Ag2 Cl2 N12 O7' _chemical_formula_weight 903.30 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' 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_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6179(4) _cell_length_b 13.4765(3) _cell_length_c 20.5256(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.897(3) _cell_angle_gamma 90.00 _cell_volume 3321.38(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23292 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6297 _exptl_absorpt_correction_T_max 0.7211 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The OH hydrogen atom was located from the difference Fourier map but constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.66 \%A from atom N2 and the deepest hole is located 0.16 \%A from atom H15A. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69325 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 32.01 _reflns_number_total 11489 _reflns_number_gt 8998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0209P)^2^+2.6132P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11489 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.016 _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 0.188309(12) 0.763081(9) 0.015816(7) 0.01878(4) Uani 1 1 d . . . Ag2 Ag 0.425082(11) 0.687120(10) 0.034672(6) 0.01662(3) Uani 1 1 d . . . Cl1 Cl 0.40449(4) 0.28647(3) 0.09391(2) 0.01611(8) Uani 1 1 d . . . Cl2 Cl -0.07271(4) 0.32493(3) -0.26753(2) 0.02200(9) Uani 1 1 d . . . O1 O 0.46619(13) 0.31900(12) 0.16306(7) 0.0320(3) Uani 1 1 d . . . O2 O 0.28835(13) 0.31845(12) 0.07928(9) 0.0385(4) Uani 1 1 d . . . O3 O 0.40120(13) 0.17647(10) 0.09441(8) 0.0276(3) Uani 1 1 d . . . O4 O -0.10505(14) 0.29180(11) -0.20835(8) 0.0335(4) Uani 1 1 d . . . O5 O -0.11624(12) 0.42714(11) -0.28335(7) 0.0280(3) Uani 1 1 d . . . O6 O 0.04922(13) 0.33018(14) -0.24697(9) 0.0397(4) Uani 1 1 d . . . O7 O 0.37392(17) 0.42219(13) -0.29319(9) 0.0470(5) Uani 1 1 d . . . H7O H 0.3658 0.3757 -0.3261 0.070 Uiso 1 1 d R . . N1 N 0.09565(13) 0.87749(11) 0.06567(8) 0.0164(3) Uani 1 1 d . . . N2 N 0.08349(12) 1.03563(10) 0.09053(7) 0.0139(3) Uani 1 1 d . . . N3 N 0.27140(12) 0.91554(10) 0.01407(7) 0.0139(3) Uani 1 1 d . . . N4 N 0.35166(12) 0.78010(10) -0.06931(7) 0.0141(3) Uani 1 1 d . . . N5 N 0.36965(12) 0.57599(11) -0.05224(7) 0.0133(3) Uani 1 1 d . . . N6 N 0.27376(12) 0.54974(11) -0.16052(7) 0.0159(3) Uani 1 1 d . . . N7 N 0.09545(12) 0.64026(10) -0.05588(7) 0.0137(3) Uani 1 1 d . . . N8 N 0.06591(12) 0.47922(10) -0.07136(7) 0.0140(3) Uani 1 1 d . . . N9 N 0.22763(12) 0.61140(11) 0.07873(7) 0.0146(3) Uani 1 1 d . . . N10 N 0.43799(12) 0.71518(11) 0.14548(7) 0.0149(3) Uani 1 1 d . . . N11 N 0.60664(12) 0.77009(11) 0.08800(7) 0.0142(3) Uani 1 1 d . . . N12 N 0.70886(12) 0.82943(11) 0.18810(7) 0.0159(3) Uani 1 1 d . . . C1 C 0.01274(16) 0.88900(13) 0.09417(9) 0.0185(4) Uani 1 1 d . . . H1 H -0.0326 0.8370 0.1021 0.022 Uiso 1 1 calc R . . C2 C 0.00406(15) 0.98652(13) 0.10988(9) 0.0172(3) Uani 1 1 d . . . H2 H -0.0473 1.0144 0.1303 0.021 Uiso 1 1 calc R . . C3 C 0.10466(16) 1.14209(12) 0.09837(10) 0.0203(4) Uani 1 1 d . . . H3A H 0.1753 1.1574 0.0900 0.030 Uiso 1 1 calc R . . H3B H 0.1088 1.1622 0.1450 0.030 Uiso 1 1 calc R . . H3C H 0.0441 1.1781 0.0654 0.030 Uiso 1 1 calc R . . C4 C 0.13743(14) 0.96750(12) 0.06404(8) 0.0130(3) Uani 1 1 d . . . C5 C 0.22991(14) 0.98687(12) 0.03868(8) 0.0134(3) Uani 1 1 d . . . H5 H 0.2595 1.0520 0.0403 0.016 Uiso 1 1 calc R . . C6 C 0.36782(14) 0.93632(12) -0.00855(9) 0.0158(3) Uani 1 1 d . . . H6A H 0.4360 0.9113 0.0259 0.019 Uiso 1 1 calc R . . H6B H 0.3757 1.0089 -0.0128 0.019 Uiso 1 1 calc R . . C7 C 0.35530(15) 0.88731(12) -0.07689(9) 0.0163(3) Uani 1 1 d . . . H7A H 0.2859 0.9105 -0.1112 0.020 Uiso 1 1 calc R . . H7B H 0.4189 0.9056 -0.0931 0.020 Uiso 1 1 calc R . . C8 C 0.31711(14) 0.72528(13) -0.12177(9) 0.0144(3) Uani 1 1 d . . . H8 H 0.2901 0.7534 -0.1663 0.017 Uiso 1 1 calc R . . C9 C 0.31992(14) 0.61865(12) -0.11214(8) 0.0130(3) Uani 1 1 d . . . C10 C 0.35450(15) 0.47634(12) -0.06290(9) 0.0162(3) Uani 1 1 d . . . H10 H 0.3811 0.4266 -0.0290 0.019 Uiso 1 1 calc R . . C11 C 0.29524(16) 0.45917(13) -0.12971(9) 0.0190(4) Uani 1 1 d . . . H11 H 0.2733 0.3964 -0.1506 0.023 Uiso 1 1 calc R . . C12 C 0.20721(17) 0.56519(16) -0.23192(9) 0.0252(4) Uani 1 1 d . . . H12A H 0.1283 0.5545 -0.2368 0.038 Uiso 1 1 calc R . . H12B H 0.2308 0.5182 -0.2612 0.038 Uiso 1 1 calc R . . H12C H 0.2179 0.6332 -0.2456 0.038 Uiso 1 1 calc R . . C13 C 0.02836(14) 0.62387(13) -0.12115(9) 0.0160(3) Uani 1 1 d . . . H13 H -0.0009 0.6740 -0.1543 0.019 Uiso 1 1 calc R . . C14 C 0.00975(15) 0.52436(13) -0.13145(9) 0.0176(3) Uani 1 1 d . . . H14 H -0.0337 0.4929 -0.1724 0.021 Uiso 1 1 calc R . . C15 C 0.07344(16) 0.37209(12) -0.06049(10) 0.0195(4) Uani 1 1 d . . . H15A H 0.0133 0.3393 -0.0959 0.029 Uiso 1 1 calc R . . H15B H 0.0666 0.3567 -0.0153 0.029 Uiso 1 1 calc R . . H15C H 0.1455 0.3483 -0.0630 0.029 Uiso 1 1 calc R . . C16 C 0.11689(14) 0.55160(12) -0.02711(8) 0.0124(3) Uani 1 1 d . . . C17 C 0.18528(14) 0.53601(12) 0.04324(9) 0.0143(3) Uani 1 1 d . . . H17 H 0.1980 0.4711 0.0622 0.017 Uiso 1 1 calc R . . C18 C 0.29360(16) 0.59667(13) 0.15014(9) 0.0185(4) Uani 1 1 d . . . H18A H 0.3481 0.5426 0.1534 0.022 Uiso 1 1 calc R . . H18B H 0.2442 0.5773 0.1773 0.022 Uiso 1 1 calc R . . C19 C 0.35406(15) 0.69127(14) 0.17849(9) 0.0186(4) Uani 1 1 d . . . H19A H 0.2998 0.7464 0.1713 0.022 Uiso 1 1 calc R . . H19B H 0.3903 0.6839 0.2284 0.022 Uiso 1 1 calc R . . C20 C 0.52755(15) 0.75455(12) 0.18278(9) 0.0152(3) Uani 1 1 d . . . H20 H 0.5385 0.7648 0.2302 0.018 Uiso 1 1 calc R . . C21 C 0.61266(14) 0.78374(12) 0.15312(8) 0.0134(3) Uani 1 1 d . . . C22 C 0.70301(15) 0.80786(13) 0.08199(9) 0.0171(3) Uani 1 1 d . . . H22 H 0.7231 0.8083 0.0410 0.021 Uiso 1 1 calc R . . C23 C 0.76666(16) 0.84513(14) 0.14330(9) 0.0199(4) Uani 1 1 d . . . H23 H 0.8375 0.8760 0.1527 0.024 Uiso 1 1 calc R . . C24 C 0.74825(16) 0.85438(16) 0.26062(9) 0.0249(4) Uani 1 1 d . . . H24A H 0.7939 0.7999 0.2861 0.037 Uiso 1 1 calc R . . H24B H 0.6843 0.8650 0.2774 0.037 Uiso 1 1 calc R . . H24C H 0.7930 0.9151 0.2671 0.037 Uiso 1 1 calc R . . C25 C 0.4424(2) 0.5056(2) -0.28994(15) 0.0529(8) Uani 1 1 d . . . H25A H 0.5144 0.4842 -0.2940 0.079 Uiso 1 1 calc R . . H25B H 0.4542 0.5395 -0.2460 0.079 Uiso 1 1 calc R . . H25C H 0.4065 0.5511 -0.3275 0.079 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 Ag1 0.01882(7) 0.00855(5) 0.02981(8) -0.00477(5) 0.00870(5) -0.00226(5) Ag2 0.01729(6) 0.02100(6) 0.00997(5) -0.00377(5) 0.00185(4) 0.00071(5) Cl1 0.0194(2) 0.01616(18) 0.01311(17) 0.00176(14) 0.00548(15) -0.00044(15) Cl2 0.0263(2) 0.0219(2) 0.01724(19) -0.00579(17) 0.00593(17) -0.00273(18) O1 0.0350(8) 0.0447(9) 0.0164(6) -0.0090(6) 0.0083(6) -0.0161(7) O2 0.0245(8) 0.0383(9) 0.0486(10) 0.0114(8) 0.0051(7) 0.0145(7) O3 0.0349(8) 0.0162(6) 0.0358(8) -0.0005(6) 0.0168(7) 0.0009(6) O4 0.0437(9) 0.0288(8) 0.0310(8) 0.0056(6) 0.0158(7) -0.0094(7) O5 0.0321(8) 0.0269(7) 0.0235(7) 0.0044(6) 0.0065(6) 0.0025(6) O6 0.0252(8) 0.0501(10) 0.0455(10) -0.0018(8) 0.0133(7) 0.0057(7) O7 0.0708(13) 0.0317(9) 0.0400(10) -0.0125(8) 0.0194(9) 0.0023(9) N1 0.0194(7) 0.0120(6) 0.0207(7) -0.0010(6) 0.0105(6) -0.0012(6) N2 0.0162(7) 0.0095(6) 0.0170(7) -0.0018(5) 0.0066(6) 0.0007(5) N3 0.0127(7) 0.0116(6) 0.0180(7) -0.0009(5) 0.0055(5) -0.0004(5) N4 0.0132(7) 0.0128(6) 0.0168(7) 0.0001(5) 0.0055(6) 0.0013(5) N5 0.0129(7) 0.0150(6) 0.0119(6) -0.0005(5) 0.0035(5) 0.0021(5) N6 0.0175(7) 0.0159(7) 0.0118(6) -0.0023(5) 0.0009(6) 0.0032(6) N7 0.0129(7) 0.0107(6) 0.0167(7) -0.0011(5) 0.0031(5) 0.0004(5) N8 0.0136(7) 0.0095(6) 0.0167(7) -0.0028(5) 0.0016(5) 0.0000(5) N9 0.0138(7) 0.0148(6) 0.0147(7) -0.0017(5) 0.0038(5) -0.0025(5) N10 0.0152(7) 0.0173(7) 0.0125(6) -0.0020(5) 0.0047(5) -0.0014(6) N11 0.0161(7) 0.0136(6) 0.0124(6) 0.0000(5) 0.0038(5) 0.0001(6) N12 0.0121(7) 0.0204(7) 0.0147(7) -0.0043(6) 0.0032(5) -0.0021(6) C1 0.0216(9) 0.0139(8) 0.0243(9) -0.0009(7) 0.0137(7) -0.0018(7) C2 0.0187(9) 0.0163(8) 0.0195(8) -0.0015(7) 0.0104(7) 0.0016(7) C3 0.0235(9) 0.0099(7) 0.0290(10) -0.0048(7) 0.0103(8) -0.0001(7) C4 0.0156(8) 0.0103(7) 0.0131(7) -0.0012(6) 0.0043(6) 0.0005(6) C5 0.0149(8) 0.0097(7) 0.0152(8) -0.0002(6) 0.0040(6) -0.0006(6) C6 0.0140(8) 0.0117(7) 0.0232(9) -0.0025(6) 0.0081(7) -0.0010(6) C7 0.0171(8) 0.0133(7) 0.0198(8) 0.0018(6) 0.0078(7) 0.0013(6) C8 0.0142(8) 0.0155(8) 0.0133(7) 0.0014(6) 0.0037(6) 0.0031(6) C9 0.0130(8) 0.0146(7) 0.0112(7) -0.0006(6) 0.0036(6) 0.0023(6) C10 0.0187(9) 0.0121(7) 0.0179(8) 0.0009(6) 0.0057(7) 0.0023(6) C11 0.0212(9) 0.0142(8) 0.0204(9) -0.0042(7) 0.0048(7) 0.0019(7) C12 0.0304(11) 0.0277(10) 0.0118(8) -0.0027(7) -0.0018(7) 0.0051(8) C13 0.0152(8) 0.0143(7) 0.0168(8) 0.0007(6) 0.0022(6) 0.0017(6) C14 0.0157(8) 0.0165(8) 0.0170(8) -0.0030(7) -0.0004(7) 0.0014(7) C15 0.0208(9) 0.0086(7) 0.0245(9) -0.0030(7) 0.0005(7) 0.0007(6) C16 0.0112(7) 0.0099(7) 0.0160(8) -0.0018(6) 0.0041(6) 0.0000(6) C17 0.0138(8) 0.0114(7) 0.0172(8) 0.0002(6) 0.0044(6) 0.0007(6) C18 0.0203(9) 0.0201(8) 0.0139(8) 0.0003(7) 0.0033(7) -0.0058(7) C19 0.0185(9) 0.0246(9) 0.0139(8) -0.0056(7) 0.0066(7) -0.0084(7) C20 0.0169(8) 0.0155(8) 0.0122(7) -0.0015(6) 0.0033(6) -0.0007(6) C21 0.0122(8) 0.0133(7) 0.0132(7) -0.0022(6) 0.0017(6) 0.0012(6) C22 0.0193(8) 0.0179(8) 0.0158(8) 0.0007(7) 0.0080(7) 0.0009(7) C23 0.0164(9) 0.0234(9) 0.0212(9) -0.0015(7) 0.0080(7) -0.0028(7) C24 0.0193(9) 0.0385(11) 0.0151(8) -0.0089(8) 0.0027(7) -0.0085(8) C25 0.0512(17) 0.0395(14) 0.0521(16) -0.0224(13) -0.0075(13) -0.0002(13) _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 N7 2.2844(14) . yes Ag1 N3 2.3119(14) . yes Ag1 N1 2.3509(15) . yes Ag1 N9 2.3871(14) . yes Ag1 Ag2 3.0680(2) . yes Ag2 N10 2.2617(14) . yes Ag2 N5 2.2688(14) . yes Ag2 N4 2.4017(14) . yes Ag2 N11 2.4809(15) . yes Cl1 O1 1.4606(14) . ? Cl1 O2 1.4673(16) . ? Cl1 O3 1.4832(14) . ? Cl2 O4 1.4649(15) . ? Cl2 O6 1.4666(16) . ? Cl2 O5 1.4815(15) . ? O7 C25 1.407(3) . ? O7 H7O 0.9030 . ? N1 C4 1.327(2) . ? N1 C1 1.355(2) . ? N2 C4 1.352(2) . ? N2 C2 1.358(2) . ? N2 C3 1.459(2) . ? N3 C5 1.271(2) . ? N3 C6 1.457(2) . ? N4 C8 1.268(2) . ? N4 C7 1.455(2) . ? N5 C9 1.327(2) . ? N5 C10 1.365(2) . ? N6 C9 1.354(2) . ? N6 C11 1.363(2) . ? N6 C12 1.463(2) . ? N7 C16 1.323(2) . ? N7 C13 1.365(2) . ? N8 C16 1.353(2) . ? N8 C14 1.362(2) . ? N8 C15 1.460(2) . ? N9 C17 1.268(2) . ? N9 C18 1.460(2) . ? N10 C20 1.270(2) . ? N10 C19 1.458(2) . ? N11 C21 1.328(2) . ? N11 C22 1.358(2) . ? N12 C21 1.354(2) . ? N12 C23 1.354(2) . ? N12 C24 1.456(2) . ? C1 C2 1.366(2) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.440(2) . ? C5 H5 0.9500 . ? C6 C7 1.514(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.449(2) . ? C8 H8 0.9500 . ? C10 C11 1.365(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.367(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.452(2) . ? C17 H17 0.9500 . ? C18 C19 1.508(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.442(2) . ? C20 H20 0.9500 . ? C22 C23 1.364(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 N7 Ag1 N3 141.19(5) . . ? N7 Ag1 N1 122.03(5) . . ? N3 Ag1 N1 73.29(5) . . yes N7 Ag1 N9 73.03(5) . . yes N3 Ag1 N9 138.55(5) . . ? N1 Ag1 N9 112.00(5) . . ? N7 Ag1 Ag2 97.26(4) . . ? N3 Ag1 Ag2 82.52(4) . . ? N1 Ag1 Ag2 139.39(4) . . yes N9 Ag1 Ag2 67.27(4) . . ? N10 Ag2 N5 144.15(5) . . ? N10 Ag2 N4 134.06(5) . . ? N5 Ag2 N4 72.79(5) . . yes N10 Ag2 N11 73.12(5) . . yes N5 Ag2 N11 131.62(5) . . ? N4 Ag2 N11 102.05(5) . . ? N10 Ag2 Ag1 80.65(4) . . ? N5 Ag2 Ag1 93.91(4) . . ? N4 Ag2 Ag1 67.61(3) . . ? N11 Ag2 Ag1 129.54(3) . . yes O1 Cl1 O2 108.14(10) . . ? O1 Cl1 O3 107.51(9) . . ? O2 Cl1 O3 105.47(9) . . ? O4 Cl2 O6 108.12(10) . . ? O4 Cl2 O5 106.63(9) . . ? O6 Cl2 O5 107.68(10) . . ? C25 O7 H7O 121.1 . . ? C4 N1 C1 105.76(14) . . ? C4 N1 Ag1 109.50(11) . . ? C1 N1 Ag1 144.70(12) . . ? C4 N2 C2 107.12(14) . . ? C4 N2 C3 127.90(15) . . ? C2 N2 C3 124.98(15) . . ? C5 N3 C6 117.89(14) . . ? C5 N3 Ag1 114.95(12) . . ? C6 N3 Ag1 127.08(10) . . ? C8 N4 C7 120.11(15) . . ? C8 N4 Ag2 112.88(11) . . ? C7 N4 Ag2 126.64(11) . . ? C9 N5 C10 105.94(14) . . ? C9 N5 Ag2 112.72(11) . . ? C10 N5 Ag2 140.34(11) . . ? C9 N6 C11 107.13(14) . . ? C9 N6 C12 128.49(15) . . ? C11 N6 C12 124.29(15) . . ? C16 N7 C13 105.79(14) . . ? C16 N7 Ag1 111.88(11) . . ? C13 N7 Ag1 142.20(12) . . ? C16 N8 C14 107.06(14) . . ? C16 N8 C15 127.97(14) . . ? C14 N8 C15 124.85(14) . . ? C17 N9 C18 118.50(15) . . ? C17 N9 Ag1 113.23(11) . . ? C18 N9 Ag1 128.26(11) . . ? C20 N10 C19 116.82(14) . . ? C20 N10 Ag2 116.85(12) . . ? C19 N10 Ag2 126.32(11) . . ? C21 N11 C22 105.28(14) . . ? C21 N11 Ag2 105.43(11) . . ? C22 N11 Ag2 149.29(12) . . ? C21 N12 C23 107.04(14) . . ? C21 N12 C24 128.02(15) . . ? C23 N12 C24 124.90(15) . . ? N1 C1 C2 109.92(16) . . ? N1 C1 H1 125.0 . . ? C2 C1 H1 125.0 . . ? N2 C2 C1 106.25(15) . . ? N2 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 110.95(15) . . ? N1 C4 C5 123.17(15) . . ? N2 C4 C5 125.86(15) . . ? N3 C5 C4 119.01(15) . . ? N3 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N3 C6 C7 110.61(14) . . ? N3 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N4 C7 C6 109.37(14) . . ? N4 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N4 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 118.31(15) . . ? N4 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? N5 C9 N6 110.90(15) . . ? N5 C9 C8 122.72(15) . . ? N6 C9 C8 126.38(15) . . ? N5 C10 C11 109.54(15) . . ? N5 C10 H10 125.2 . . ? C11 C10 H10 125.2 . . ? N6 C11 C10 106.48(15) . . ? N6 C11 H11 126.8 . . ? C10 C11 H11 126.8 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 C14 109.62(15) . . ? N7 C13 H13 125.2 . . ? C14 C13 H13 125.2 . . ? N8 C14 C13 106.34(15) . . ? N8 C14 H14 126.8 . . ? C13 C14 H14 126.8 . . ? N8 C15 H15A 109.5 . . ? N8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 111.19(14) . . ? N7 C16 C17 123.51(15) . . ? N8 C16 C17 125.30(15) . . ? N9 C17 C16 118.15(15) . . ? N9 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? N9 C18 C19 109.71(14) . . ? N9 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? N9 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N10 C19 C18 111.18(15) . . ? N10 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? N10 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N10 C20 C21 119.98(16) . . ? N10 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? N11 C21 N12 111.20(15) . . ? N11 C21 C20 124.56(15) . . ? N12 C21 C20 124.25(15) . . ? N11 C22 C23 110.11(16) . . ? N11 C22 H22 124.9 . . ? C23 C22 H22 124.9 . . ? N12 C23 C22 106.37(16) . . ? N12 C23 H23 126.8 . . ? C22 C23 H23 126.8 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O7 H7O O3 0.90 1.95 2.774(2) 150.7 4_565 yes _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.653 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.099 #===END======================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 855062' #TrackingRef 'Koskinen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H64 Ag6 F6 N24 O6 S2, 4(C F3 O3 S)' _chemical_formula_sum 'C54 H64 Ag6 F18 N24 O18 S6' _chemical_formula_weight 2518.87 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3742(2) _cell_length_b 13.8840(2) _cell_length_c 14.1976(2) _cell_angle_alpha 110.8790(10) _cell_angle_beta 101.3660(10) _cell_angle_gamma 102.3070(10) _cell_volume 2124.72(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 73803 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4865 _exptl_absorpt_correction_T_max 0.8051 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; Hydrogen atoms were positioned geometrically and were constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 1.77 \%A from atom C9 and the deepest hole is located 0.59 \%A from atom S2. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74427 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.06 _reflns_number_total 12415 _reflns_number_gt 10698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0233P)^2^+2.2515P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 12415 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.009992(12) 0.180831(12) 0.453767(11) 0.01699(4) Uani 1 1 d . . . Ag2 Ag 0.060497(12) 0.320033(12) 0.356638(11) 0.01573(4) Uani 1 1 d . . . Ag3 Ag 0.022430(14) 0.304419(12) 0.127844(13) 0.02102(4) Uani 1 1 d . . . S1 S -0.08911(4) 0.07462(4) 0.64844(4) 0.01992(10) Uani 1 1 d . . . S2 S 0.63723(4) 0.36608(4) 0.47261(4) 0.02042(10) Uani 1 1 d . . . S3 S 0.53124(4) 0.26997(4) 0.03063(4) 0.01744(9) Uani 1 1 d . . . F1 F -0.28968(15) -0.07553(16) 0.56028(18) 0.0657(6) Uani 1 1 d . . . F2 F -0.25500(15) 0.02006(15) 0.72601(16) 0.0499(4) Uani 1 1 d . . . F3 F -0.30094(15) 0.08685(18) 0.61554(18) 0.0627(6) Uani 1 1 d . . . F4 F 0.6934(2) 0.19762(18) 0.48007(17) 0.0738(7) Uani 1 1 d . . . F5 F 0.69704(15) 0.31248(15) 0.62959(12) 0.0489(4) Uani 1 1 d . . . F6 F 0.53560(17) 0.20950(15) 0.51643(16) 0.0602(5) Uani 1 1 d . . . F7 F 0.36950(12) 0.24996(11) -0.13145(11) 0.0339(3) Uani 1 1 d . . . F8 F 0.43016(13) 0.40751(11) -0.00273(11) 0.0323(3) Uani 1 1 d . . . F9 F 0.53622(13) 0.35996(12) -0.10358(11) 0.0346(3) Uani 1 1 d . . . O1 O -0.08896(16) 0.07764(16) 0.54858(14) 0.0374(4) Uani 1 1 d . . . O2 O -0.04386(14) -0.00554(12) 0.66939(12) 0.0253(3) Uani 1 1 d . . . O3 O -0.04962(15) 0.17937(13) 0.73738(14) 0.0318(4) Uani 1 1 d . . . O4 O 0.58186(14) 0.43371(13) 0.53498(13) 0.0286(3) Uani 1 1 d . . . O5 O 0.57019(15) 0.30238(14) 0.36374(13) 0.0315(4) Uani 1 1 d . . . O6 O 0.75752(14) 0.41791(15) 0.48862(14) 0.0331(4) Uani 1 1 d . . . O7 O 0.44218(13) 0.24451(13) 0.07781(13) 0.0256(3) Uani 1 1 d . . . O8 O 0.55290(14) 0.17784(12) -0.04161(12) 0.0266(3) Uani 1 1 d . . . O9 O 0.63386(13) 0.35738(12) 0.10253(12) 0.0253(3) Uani 1 1 d . . . N1 N 0.16485(14) 0.28993(13) 0.57953(13) 0.0165(3) Uani 1 1 d . . . N2 N 0.33745(14) 0.40566(13) 0.68024(13) 0.0165(3) Uani 1 1 d . . . N3 N 0.23859(14) 0.32661(13) 0.39912(12) 0.0150(3) Uani 1 1 d . . . N4 N 0.12669(13) 0.18965(13) 0.17406(12) 0.0138(3) Uani 1 1 d . . . N5 N -0.10667(14) 0.13922(13) 0.06760(13) 0.0156(3) Uani 1 1 d . . . N6 N -0.14686(14) -0.02566(12) 0.06446(12) 0.0146(3) Uani 1 1 d . . . N7 N -0.15443(14) 0.12036(13) 0.33070(13) 0.0164(3) Uani 1 1 d . . . N8 N -0.33321(14) 0.08590(13) 0.23402(13) 0.0169(3) Uani 1 1 d . . . N9 N -0.10644(14) 0.34043(13) 0.31806(13) 0.0152(3) Uani 1 1 d . . . N10 N 0.03706(14) 0.48194(13) 0.23629(13) 0.0153(3) Uani 1 1 d . . . N11 N 0.09554(15) 0.40972(13) 0.04768(13) 0.0187(3) Uani 1 1 d . . . N12 N 0.16570(15) 0.57817(13) 0.06578(14) 0.0182(3) Uani 1 1 d . . . C1 C 0.17257(17) 0.31187(16) 0.68294(15) 0.0180(4) Uani 1 1 d . . . H1 H 0.1135 0.2815 0.7072 0.022 Uiso 1 1 calc R . . C2 C 0.27851(17) 0.38437(16) 0.74581(15) 0.0182(4) Uani 1 1 d . . . H2 H 0.3059 0.4142 0.8208 0.022 Uiso 1 1 calc R . . C3 C 0.45449(17) 0.48285(18) 0.71553(16) 0.0229(4) Uani 1 1 d . . . H3A H 0.4985 0.4531 0.6683 0.034 Uiso 1 1 calc R . . H3B H 0.4942 0.4952 0.7877 0.034 Uiso 1 1 calc R . . H3C H 0.4487 0.5517 0.7141 0.034 Uiso 1 1 calc R . . C4 C 0.26581(16) 0.34804(15) 0.57959(15) 0.0156(4) Uani 1 1 d . . . C5 C 0.30524(17) 0.34912(15) 0.48985(15) 0.0165(4) Uani 1 1 d . . . H5 H 0.3864 0.3679 0.4996 0.020 Uiso 1 1 calc R . . C6 C 0.29512(16) 0.32678(15) 0.31682(14) 0.0157(4) Uani 1 1 d . . . H6A H 0.3800 0.3462 0.3470 0.019 Uiso 1 1 calc R . . H6B H 0.2793 0.3819 0.2918 0.019 Uiso 1 1 calc R . . C7 C 0.25051(16) 0.21612(15) 0.22450(15) 0.0152(3) Uani 1 1 d . . . H7A H 0.2933 0.2159 0.1724 0.018 Uiso 1 1 calc R . . H7B H 0.2640 0.1606 0.2498 0.018 Uiso 1 1 calc R . . C8 C 0.05951(16) 0.09478(15) 0.14759(14) 0.0139(3) Uani 1 1 d . . . H8 H 0.0884 0.0419 0.1624 0.017 Uiso 1 1 calc R . . C9 C -0.06281(16) 0.06958(15) 0.09403(14) 0.0140(3) Uani 1 1 d . . . C10 C -0.22250(17) 0.08672(16) 0.01956(16) 0.0186(4) Uani 1 1 d . . . H10 H -0.2767 0.1164 -0.0080 0.022 Uiso 1 1 calc R . . C11 C -0.24858(17) -0.01519(16) 0.01710(15) 0.0180(4) Uani 1 1 d . . . H11 H -0.3228 -0.0683 -0.0118 0.022 Uiso 1 1 calc R . . C12 C -0.13315(18) -0.12151(15) 0.08005(16) 0.0186(4) Uani 1 1 d . . . H12A H -0.0717 -0.1431 0.0517 0.028 Uiso 1 1 calc R . . H12B H -0.2062 -0.1810 0.0432 0.028 Uiso 1 1 calc R . . H12C H -0.1123 -0.1046 0.1557 0.028 Uiso 1 1 calc R . . C13 C -0.21876(18) 0.01760(16) 0.30970(16) 0.0193(4) Uani 1 1 d . . . H13 H -0.1908 -0.0311 0.3332 0.023 Uiso 1 1 calc R . . C14 C -0.32933(18) -0.00416(16) 0.24987(16) 0.0193(4) Uani 1 1 d . . . H14 H -0.3913 -0.0695 0.2244 0.023 Uiso 1 1 calc R . . C15 C -0.43580(18) 0.09504(17) 0.16946(17) 0.0230(4) Uani 1 1 d . . . H15A H -0.5014 0.0297 0.1466 0.034 Uiso 1 1 calc R . . H15B H -0.4194 0.1029 0.1073 0.034 Uiso 1 1 calc R . . H15C H -0.4549 0.1586 0.2114 0.034 Uiso 1 1 calc R . . C16 C -0.22616(16) 0.16077(15) 0.28362(15) 0.0156(4) Uani 1 1 d . . . C17 C -0.20522(17) 0.26869(15) 0.28560(15) 0.0161(4) Uani 1 1 d . . . H17 H -0.2710 0.2875 0.2604 0.019 Uiso 1 1 calc R . . C18 C -0.11057(17) 0.44883(16) 0.32464(16) 0.0176(4) Uani 1 1 d . . . H18A H -0.1350 0.4850 0.3870 0.021 Uiso 1 1 calc R . . H18B H -0.1696 0.4392 0.2610 0.021 Uiso 1 1 calc R . . C19 C 0.00460(17) 0.52120(15) 0.33321(15) 0.0165(4) Uani 1 1 d . . . H19A H 0.0000 0.5954 0.3491 0.020 Uiso 1 1 calc R . . H19B H 0.0654 0.5250 0.3925 0.020 Uiso 1 1 calc R . . C20 C 0.07839(16) 0.55115(15) 0.20273(16) 0.0165(4) Uani 1 1 d . . . H20 H 0.0865 0.6257 0.2394 0.020 Uiso 1 1 calc R . . C21 C 0.11287(16) 0.51365(15) 0.10698(15) 0.0163(4) Uani 1 1 d . . . C22 C 0.13820(18) 0.40791(17) -0.03456(16) 0.0203(4) Uani 1 1 d . . . H22 H 0.1374 0.3443 -0.0904 0.024 Uiso 1 1 calc R . . C23 C 0.18230(18) 0.51164(17) -0.02431(17) 0.0208(4) Uani 1 1 d . . . H23 H 0.2174 0.5331 -0.0705 0.025 Uiso 1 1 calc R . . C24 C 0.2010(2) 0.69674(17) 0.10863(19) 0.0261(5) Uani 1 1 d . . . H24A H 0.1330 0.7213 0.1145 0.039 Uiso 1 1 calc R . . H24B H 0.2358 0.7210 0.0614 0.039 Uiso 1 1 calc R . . H24C H 0.2579 0.7273 0.1787 0.039 Uiso 1 1 calc R . . C25 C -0.2424(2) 0.0236(2) 0.6355(2) 0.0359(6) Uani 1 1 d . . . C26 C 0.46415(19) 0.32480(16) -0.05634(17) 0.0228(4) Uani 1 1 d . . . C27 C 0.6409(2) 0.2654(2) 0.52643(19) 0.0328(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01475(7) 0.01795(7) 0.01601(7) 0.00812(6) 0.00156(5) 0.00160(5) Ag2 0.01264(7) 0.01949(7) 0.01818(7) 0.01009(6) 0.00520(5) 0.00651(5) Ag3 0.02778(8) 0.01162(7) 0.02492(8) 0.00888(6) 0.00982(6) 0.00454(6) S1 0.0193(2) 0.0199(2) 0.0214(2) 0.01066(19) 0.00609(19) 0.00428(19) S2 0.0172(2) 0.0213(2) 0.0208(2) 0.00654(19) 0.00555(19) 0.00613(19) S3 0.0141(2) 0.0148(2) 0.0196(2) 0.00687(18) 0.00137(18) 0.00093(17) F1 0.0323(9) 0.0506(11) 0.0822(14) 0.0168(10) -0.0023(9) -0.0125(8) F2 0.0429(9) 0.0640(11) 0.0803(13) 0.0551(10) 0.0396(9) 0.0260(8) F3 0.0314(9) 0.0873(14) 0.1109(17) 0.0783(14) 0.0240(10) 0.0318(9) F4 0.140(2) 0.0779(14) 0.0683(13) 0.0537(12) 0.0661(14) 0.0873(15) F5 0.0534(10) 0.0629(11) 0.0299(8) 0.0266(8) 0.0043(7) 0.0117(9) F6 0.0535(11) 0.0474(10) 0.0704(13) 0.0361(10) 0.0056(10) -0.0107(9) F7 0.0319(7) 0.0235(7) 0.0333(7) 0.0089(6) -0.0095(6) 0.0065(6) F8 0.0402(8) 0.0218(6) 0.0372(8) 0.0115(6) 0.0112(6) 0.0156(6) F9 0.0434(8) 0.0372(8) 0.0347(8) 0.0238(7) 0.0169(7) 0.0143(7) O1 0.0399(10) 0.0458(11) 0.0303(9) 0.0251(8) 0.0108(8) 0.0043(8) O2 0.0276(8) 0.0249(8) 0.0253(8) 0.0095(6) 0.0071(6) 0.0138(7) O3 0.0335(9) 0.0192(8) 0.0382(9) 0.0063(7) 0.0152(8) 0.0051(7) O4 0.0246(8) 0.0245(8) 0.0322(9) 0.0044(7) 0.0131(7) 0.0072(7) O5 0.0350(9) 0.0326(9) 0.0219(8) 0.0068(7) 0.0031(7) 0.0134(8) O6 0.0187(8) 0.0478(11) 0.0357(9) 0.0204(8) 0.0109(7) 0.0084(7) O7 0.0186(7) 0.0258(8) 0.0336(8) 0.0172(7) 0.0076(6) 0.0009(6) O8 0.0280(8) 0.0206(7) 0.0265(8) 0.0061(6) 0.0012(6) 0.0110(6) O9 0.0192(7) 0.0240(8) 0.0224(7) 0.0080(6) 0.0013(6) -0.0057(6) N1 0.0155(8) 0.0177(8) 0.0169(8) 0.0081(6) 0.0045(6) 0.0047(6) N2 0.0142(7) 0.0182(8) 0.0140(7) 0.0054(6) 0.0026(6) 0.0030(6) N3 0.0137(7) 0.0146(7) 0.0149(7) 0.0048(6) 0.0045(6) 0.0034(6) N4 0.0136(7) 0.0135(7) 0.0115(7) 0.0038(6) 0.0029(6) 0.0022(6) N5 0.0146(7) 0.0140(7) 0.0164(7) 0.0057(6) 0.0031(6) 0.0037(6) N6 0.0155(7) 0.0108(7) 0.0136(7) 0.0032(6) 0.0031(6) 0.0012(6) N7 0.0146(7) 0.0160(8) 0.0165(7) 0.0057(6) 0.0028(6) 0.0047(6) N8 0.0155(8) 0.0157(8) 0.0167(8) 0.0054(6) 0.0017(6) 0.0045(6) N9 0.0156(7) 0.0169(8) 0.0159(7) 0.0078(6) 0.0064(6) 0.0073(6) N10 0.0145(7) 0.0135(7) 0.0173(7) 0.0061(6) 0.0039(6) 0.0043(6) N11 0.0197(8) 0.0162(8) 0.0198(8) 0.0073(7) 0.0071(7) 0.0039(7) N12 0.0173(8) 0.0153(8) 0.0245(8) 0.0102(7) 0.0084(7) 0.0046(6) C1 0.0182(9) 0.0199(9) 0.0174(9) 0.0087(8) 0.0066(7) 0.0059(8) C2 0.0197(9) 0.0203(9) 0.0158(9) 0.0083(8) 0.0055(7) 0.0070(8) C3 0.0151(9) 0.0260(11) 0.0178(9) 0.0049(8) 0.0012(8) -0.0016(8) C4 0.0145(8) 0.0161(9) 0.0148(8) 0.0054(7) 0.0033(7) 0.0046(7) C5 0.0142(8) 0.0161(9) 0.0164(9) 0.0046(7) 0.0043(7) 0.0031(7) C6 0.0135(8) 0.0164(9) 0.0140(8) 0.0046(7) 0.0041(7) 0.0014(7) C7 0.0124(8) 0.0159(9) 0.0157(8) 0.0050(7) 0.0046(7) 0.0038(7) C8 0.0170(9) 0.0133(8) 0.0110(8) 0.0042(7) 0.0049(7) 0.0050(7) C9 0.0144(8) 0.0113(8) 0.0137(8) 0.0037(7) 0.0041(7) 0.0021(7) C10 0.0154(9) 0.0162(9) 0.0201(9) 0.0054(8) 0.0015(7) 0.0042(7) C11 0.0138(9) 0.0161(9) 0.0174(9) 0.0031(7) 0.0016(7) 0.0015(7) C12 0.0217(10) 0.0127(8) 0.0210(9) 0.0080(7) 0.0059(8) 0.0031(7) C13 0.0206(10) 0.0145(9) 0.0197(9) 0.0065(7) 0.0017(8) 0.0045(8) C14 0.0200(9) 0.0127(9) 0.0194(9) 0.0036(7) 0.0026(8) 0.0019(7) C15 0.0176(9) 0.0192(10) 0.0239(10) 0.0059(8) -0.0028(8) 0.0035(8) C16 0.0143(8) 0.0159(9) 0.0139(8) 0.0036(7) 0.0038(7) 0.0043(7) C17 0.0156(9) 0.0168(9) 0.0150(8) 0.0056(7) 0.0037(7) 0.0062(7) C18 0.0190(9) 0.0161(9) 0.0225(9) 0.0095(8) 0.0096(8) 0.0092(7) C19 0.0191(9) 0.0128(8) 0.0172(9) 0.0051(7) 0.0058(7) 0.0059(7) C20 0.0139(8) 0.0126(8) 0.0212(9) 0.0061(7) 0.0041(7) 0.0032(7) C21 0.0140(8) 0.0154(9) 0.0193(9) 0.0080(7) 0.0043(7) 0.0034(7) C22 0.0219(10) 0.0204(10) 0.0200(9) 0.0091(8) 0.0081(8) 0.0068(8) C23 0.0200(10) 0.0227(10) 0.0256(10) 0.0134(8) 0.0114(8) 0.0080(8) C24 0.0289(11) 0.0150(9) 0.0359(12) 0.0119(9) 0.0146(10) 0.0033(8) C25 0.0231(11) 0.0367(14) 0.0558(16) 0.0311(13) 0.0078(11) 0.0072(10) C26 0.0266(11) 0.0147(9) 0.0235(10) 0.0071(8) 0.0030(8) 0.0052(8) C27 0.0389(14) 0.0350(13) 0.0262(11) 0.0132(10) 0.0114(10) 0.0125(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.1542(16) . yes Ag1 N7 2.1731(16) . yes Ag1 O1 2.5770(17) . yes Ag1 Ag2 2.7842(2) . yes Ag2 N9 2.1357(16) . yes Ag2 N3 2.1401(16) . yes Ag2 Ag3 3.1100(2) . yes Ag3 N5 2.2462(16) . yes Ag3 N11 2.2977(17) . yes Ag3 N10 2.3394(16) . yes Ag3 N4 2.4335(16) . yes S1 O1 1.4336(17) . ? S1 O2 1.4410(16) . ? S1 O3 1.4468(17) . ? S1 C25 1.826(3) . ? S2 O4 1.4338(16) . ? S2 O5 1.4377(17) . ? S2 O6 1.4417(17) . ? S2 C27 1.821(3) . ? S3 O9 1.4410(15) . ? S3 O8 1.4419(16) . ? S3 O7 1.4429(15) . ? S3 C26 1.824(2) . ? F1 C25 1.319(3) . ? F2 C25 1.340(3) . ? F3 C25 1.321(3) . ? F4 C27 1.315(3) . ? F5 C27 1.333(3) . ? F6 C27 1.318(3) . ? F7 C26 1.337(2) . ? F8 C26 1.336(2) . ? F9 C26 1.329(3) . ? N1 C4 1.335(2) . ? N1 C1 1.368(2) . ? N2 C4 1.361(2) . ? N2 C2 1.363(3) . ? N2 C3 1.472(3) . ? N3 C5 1.273(2) . ? N3 C6 1.476(2) . ? N4 C8 1.275(2) . ? N4 C7 1.461(2) . ? N5 C9 1.331(2) . ? N5 C10 1.366(2) . ? N6 C9 1.361(2) . ? N6 C11 1.368(2) . ? N6 C12 1.463(2) . ? N7 C16 1.340(2) . ? N7 C13 1.370(3) . ? N8 C14 1.356(3) . ? N8 C16 1.362(2) . ? N8 C15 1.470(3) . ? N9 C17 1.277(3) . ? N9 C18 1.487(2) . ? N10 C20 1.275(2) . ? N10 C19 1.459(2) . ? N11 C21 1.330(3) . ? N11 C22 1.367(3) . ? N12 C21 1.359(2) . ? N12 C23 1.369(3) . ? N12 C24 1.465(3) . ? C1 C2 1.365(3) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.455(3) . ? C5 H5 0.9500 . ? C6 C7 1.517(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.457(3) . ? C8 H8 0.9500 . ? C10 C11 1.369(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.367(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.454(3) . ? C17 H17 0.9500 . ? C18 C19 1.513(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.456(3) . ? C20 H20 0.9500 . ? C22 C23 1.370(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 N1 Ag1 N7 161.41(6) . . yes N1 Ag1 O1 100.64(6) . . ? N7 Ag1 O1 88.67(6) . . ? N1 Ag1 Ag2 85.34(4) . . ? N7 Ag1 Ag2 81.27(4) . . ? O1 Ag1 Ag2 162.04(4) . . yes N9 Ag2 N3 170.61(6) . . yes N9 Ag2 Ag1 98.19(4) . . ? N3 Ag2 Ag1 89.58(4) . . ? N9 Ag2 Ag3 76.63(4) . . ? N3 Ag2 Ag3 101.15(4) . . ? Ag1 Ag2 Ag3 137.578(7) . . yes N5 Ag3 N11 133.85(6) . . ? N5 Ag3 N10 136.41(6) . . ? N11 Ag3 N10 74.39(6) . . yes N5 Ag3 N4 73.03(5) . . yes N11 Ag3 N4 120.29(6) . . ? N10 Ag3 N4 126.88(5) . . ? N5 Ag3 Ag2 89.18(4) . . ? N11 Ag3 Ag2 136.94(4) . . ? N10 Ag3 Ag2 72.94(4) . . ? N4 Ag3 Ag2 63.29(4) . . ? O1 S1 O2 115.28(11) . . ? O1 S1 O3 115.14(11) . . ? O2 S1 O3 114.01(10) . . ? O1 S1 C25 104.19(12) . . ? O2 S1 C25 102.29(10) . . ? O3 S1 C25 103.66(12) . . ? O4 S2 O5 114.70(10) . . ? O4 S2 O6 114.82(10) . . ? O5 S2 O6 114.39(11) . . ? O4 S2 C27 103.27(11) . . ? O5 S2 C27 103.51(11) . . ? O6 S2 C27 104.06(11) . . ? O9 S3 O8 114.77(10) . . ? O9 S3 O7 114.76(9) . . ? O8 S3 O7 115.40(10) . . ? O9 S3 C26 104.29(10) . . ? O8 S3 C26 102.89(10) . . ? O7 S3 C26 102.30(10) . . ? S1 O1 Ag1 145.54(11) . . ? C4 N1 C1 106.39(16) . . ? C4 N1 Ag1 132.19(13) . . ? C1 N1 Ag1 121.43(13) . . ? C4 N2 C2 107.43(16) . . ? C4 N2 C3 127.66(17) . . ? C2 N2 C3 124.81(17) . . ? C5 N3 C6 116.32(16) . . ? C5 N3 Ag2 128.42(13) . . ? C6 N3 Ag2 113.99(12) . . ? C8 N4 C7 119.44(16) . . ? C8 N4 Ag3 111.91(12) . . ? C7 N4 Ag3 128.65(12) . . ? C9 N5 C10 105.92(16) . . ? C9 N5 Ag3 113.39(12) . . ? C10 N5 Ag3 140.28(13) . . ? C9 N6 C11 106.85(16) . . ? C9 N6 C12 127.34(16) . . ? C11 N6 C12 125.81(16) . . ? C16 N7 C13 106.02(16) . . ? C16 N7 Ag1 137.98(13) . . ? C13 N7 Ag1 113.89(13) . . ? C14 N8 C16 107.99(16) . . ? C14 N8 C15 124.16(17) . . ? C16 N8 C15 127.78(17) . . ? C17 N9 C18 114.92(16) . . ? C17 N9 Ag2 127.58(13) . . ? C18 N9 Ag2 117.44(12) . . ? C20 N10 C19 117.87(16) . . ? C20 N10 Ag3 113.20(13) . . ? C19 N10 Ag3 128.92(12) . . ? C21 N11 C22 105.88(17) . . ? C21 N11 Ag3 110.00(13) . . ? C22 N11 Ag3 143.77(14) . . ? C21 N12 C23 107.16(16) . . ? C21 N12 C24 127.53(17) . . ? C23 N12 C24 125.30(17) . . ? C2 C1 N1 109.30(17) . . ? C2 C1 H1 125.4 . . ? N1 C1 H1 125.4 . . ? N2 C2 C1 106.73(17) . . ? N2 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 110.14(16) . . ? N1 C4 C5 128.65(17) . . ? N2 C4 C5 121.06(17) . . ? N3 C5 C4 124.56(18) . . ? N3 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? N3 C6 C7 110.56(15) . . ? N3 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N4 C7 C6 110.23(15) . . ? N4 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N4 C8 C9 118.20(17) . . ? N4 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N5 C9 N6 110.99(16) . . ? N5 C9 C8 123.20(17) . . ? N6 C9 C8 125.81(17) . . ? N5 C10 C11 109.66(17) . . ? N5 C10 H10 125.2 . . ? C11 C10 H10 125.2 . . ? N6 C11 C10 106.58(17) . . ? N6 C11 H11 126.7 . . ? C10 C11 H11 126.7 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N7 109.61(17) . . ? C14 C13 H13 125.2 . . ? N7 C13 H13 125.2 . . ? N8 C14 C13 106.50(17) . . ? N8 C14 H14 126.8 . . ? C13 C14 H14 126.8 . . ? N8 C15 H15A 109.5 . . ? N8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N8 109.88(17) . . ? N7 C16 C17 129.32(17) . . ? N8 C16 C17 120.68(17) . . ? N9 C17 C16 125.96(18) . . ? N9 C17 H17 117.0 . . ? C16 C17 H17 117.0 . . ? N9 C18 C19 113.05(15) . . ? N9 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N9 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N10 C19 C18 112.09(16) . . ? N10 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? N10 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N10 C20 C21 118.63(17) . . ? N10 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? N11 C21 N12 110.96(17) . . ? N11 C21 C20 123.55(17) . . ? N12 C21 C20 125.49(17) . . ? N11 C22 C23 109.77(18) . . ? N11 C22 H22 125.1 . . ? C23 C22 H22 125.1 . . ? N12 C23 C22 106.22(18) . . ? N12 C23 H23 126.9 . . ? C22 C23 H23 126.9 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F1 C25 F3 109.3(2) . . ? F1 C25 F2 107.8(2) . . ? F3 C25 F2 106.6(2) . . ? F1 C25 S1 110.8(2) . . ? F3 C25 S1 111.97(17) . . ? F2 C25 S1 110.24(18) . . ? F9 C26 F8 107.94(17) . . ? F9 C26 F7 107.93(18) . . ? F8 C26 F7 106.70(18) . . ? F9 C26 S3 111.91(15) . . ? F8 C26 S3 111.07(15) . . ? F7 C26 S3 111.07(14) . . ? F4 C27 F6 108.8(2) . . ? F4 C27 F5 107.7(2) . . ? F6 C27 F5 106.2(2) . . ? F4 C27 S2 111.58(17) . . ? F6 C27 S2 111.38(18) . . ? F5 C27 S2 111.02(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.918 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.090 #===END======================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 855063' #TrackingRef 'Koskinen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H18 Ag N6, C F3 O3 S' _chemical_formula_sum 'C14 H18 Ag F3 N6 O3 S' _chemical_formula_weight 515.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 20.1692(7) _cell_length_b 6.8605(2) _cell_length_c 28.4044(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.456(2) _cell_angle_gamma 90.00 _cell_volume 3682.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11845 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description colourless _exptl_crystal_colour needle _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7584 _exptl_absorpt_correction_T_max 0.9290 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The hydrogen atoms were positioned geometrically and were also constrained to ride on their parent atoms, with C---H = 0.95-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). The highest peak is located 0.96 \%A from atom Ag1 and the deepest hole is located 0.88 \%A from atom Ag1B. ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55255 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8431 _reflns_number_gt 5935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1e (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0247P)^2^+6.2108P] 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 8431 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.485948(14) 0.29479(4) 0.263893(9) 0.02766(8) Uani 1 1 d . . . S3 S 0.33771(5) 0.70028(14) 0.40638(3) 0.0282(2) Uani 1 1 d . . . F1 F 0.30539(12) 0.8121(4) 0.48363(9) 0.0481(6) Uani 1 1 d . . . F2 F 0.31621(11) 0.5012(3) 0.47857(8) 0.0419(6) Uani 1 1 d . . . F3 F 0.22374(11) 0.6476(4) 0.42934(8) 0.0449(6) Uani 1 1 d . . . O1 O 0.41137(13) 0.7081(4) 0.43837(10) 0.0345(6) Uani 1 1 d . . . O2 O 0.31776(14) 0.5308(4) 0.37463(9) 0.0390(7) Uani 1 1 d . . . O3 O 0.30844(14) 0.8808(4) 0.38227(10) 0.0387(7) Uani 1 1 d . . . N1 N 0.50168(14) 0.3274(4) 0.34445(10) 0.0211(6) Uani 1 1 d . . . N2 N 0.46971(15) 0.2812(4) 0.41029(10) 0.0231(6) Uani 1 1 d . . . N3 N 0.37707(15) 0.1513(4) 0.28103(10) 0.0232(6) Uani 1 1 d . . . N4 N 0.55017(14) 0.2662(4) 0.21262(10) 0.0202(6) Uani 1 1 d . . . N5 N 0.40887(15) 0.3860(4) 0.18085(10) 0.0235(6) Uani 1 1 d . . . N6 N 0.40087(14) 0.3866(4) 0.10107(10) 0.0216(6) Uani 1 1 d . . . C1 C 0.55544(18) 0.3857(5) 0.38650(13) 0.0251(8) Uani 1 1 d . . . H1 H 0.5994 0.4374 0.3870 0.030 Uiso 1 1 calc R . . C2 C 0.53660(19) 0.3584(5) 0.42803(13) 0.0271(8) Uani 1 1 d . . . H2 H 0.5641 0.3871 0.4620 0.033 Uiso 1 1 calc R . . C3 C 0.4302(2) 0.2199(5) 0.44240(13) 0.0290(8) Uani 1 1 d . . . H3A H 0.3798 0.2483 0.4255 0.043 Uiso 1 1 calc R . . H3B H 0.4478 0.2908 0.4743 0.043 Uiso 1 1 calc R . . H3C H 0.4366 0.0796 0.4489 0.043 Uiso 1 1 calc R . . C4 C 0.45023(17) 0.2649(5) 0.35982(11) 0.0196(7) Uani 1 1 d . . . C5 C 0.38428(17) 0.1825(5) 0.32674(12) 0.0210(7) Uani 1 1 d . . . H5 H 0.3472 0.1525 0.3389 0.025 Uiso 1 1 calc R . . C6 C 0.68718(18) 0.5517(5) 0.25065(13) 0.0254(8) Uani 1 1 d . . . H6A H 0.7135 0.6369 0.2792 0.030 Uiso 1 1 calc R . . H6B H 0.7180 0.5250 0.2309 0.030 Uiso 1 1 calc R . . C7 C 0.66875(18) 0.3604(5) 0.27060(12) 0.0228(7) Uani 1 1 d . . . H7A H 0.6413 0.3902 0.2926 0.027 Uiso 1 1 calc R . . H7B H 0.7132 0.2961 0.2915 0.027 Uiso 1 1 calc R . . C8 C 0.62627(17) 0.2176(5) 0.22997(12) 0.0225(7) Uani 1 1 d . . . H8A H 0.6432 0.2231 0.2012 0.027 Uiso 1 1 calc R . . H8B H 0.6335 0.0833 0.2436 0.027 Uiso 1 1 calc R . . C9 C 0.51735(17) 0.2976(5) 0.16614(12) 0.0207(7) Uani 1 1 d . . . H9 H 0.5410 0.2842 0.1427 0.025 Uiso 1 1 calc R . . C10 C 0.44351(17) 0.3538(5) 0.14933(12) 0.0213(7) Uani 1 1 d . . . C11 C 0.34199(18) 0.4398(5) 0.15130(13) 0.0277(8) Uani 1 1 d . . . H11 H 0.3050 0.4717 0.1634 0.033 Uiso 1 1 calc R . . C12 C 0.33611(18) 0.4409(5) 0.10200(13) 0.0255(8) Uani 1 1 d . . . H12 H 0.2953 0.4729 0.0740 0.031 Uiso 1 1 calc R . . C13 C 0.41814(19) 0.3634(5) 0.05568(12) 0.0261(8) Uani 1 1 d . . . H13A H 0.4657 0.3079 0.0644 0.039 Uiso 1 1 calc R . . H13B H 0.4167 0.4908 0.0397 0.039 Uiso 1 1 calc R . . H13C H 0.3837 0.2760 0.0323 0.039 Uiso 1 1 calc R . . C14 C 0.29320(19) 0.6636(6) 0.45131(14) 0.0299(8) Uani 1 1 d . . . Ag1B Ag 0.016602(14) 0.22436(4) 0.244706(10) 0.02936(8) Uani 1 1 d . . . S1B S 0.15884(5) -0.25541(13) 0.07269(3) 0.0263(2) Uani 1 1 d . . . F1B F 0.19823(12) 0.0789(3) 0.04642(9) 0.0453(6) Uani 1 1 d . . . F2B F 0.28092(11) -0.0784(3) 0.10226(9) 0.0436(6) Uani 1 1 d . . . F3B F 0.20121(12) 0.0682(3) 0.12296(9) 0.0449(6) Uani 1 1 d . . . O1B O 0.17765(14) -0.3457(4) 0.03327(9) 0.0380(7) Uani 1 1 d . . . O2B O 0.18226(14) -0.3578(4) 0.11976(9) 0.0360(6) Uani 1 1 d . . . O3B O 0.08755(13) -0.1827(4) 0.05706(10) 0.0382(7) Uani 1 1 d . . . N1B N 0.08848(14) 0.1596(4) 0.32557(10) 0.0259(7) Uani 1 1 d . . . N2B N 0.09822(15) 0.1636(4) 0.40545(10) 0.0250(6) Uani 1 1 d . . . N3B N -0.05341(14) 0.2646(4) 0.29416(10) 0.0217(6) Uani 1 1 d . . . N4B N 0.12294(15) 0.3705(4) 0.21982(10) 0.0234(6) Uani 1 1 d . . . N5B N -0.00801(15) 0.2050(4) 0.16414(10) 0.0233(6) Uani 1 1 d . . . N6B N 0.01145(16) 0.2451(4) 0.09349(10) 0.0274(7) Uani 1 1 d . . . C1B C 0.15666(19) 0.1161(6) 0.35436(14) 0.0324(9) Uani 1 1 d . . . H1B H 0.1936 0.0883 0.3418 0.039 Uiso 1 1 calc R . . C2B C 0.16365(19) 0.1186(6) 0.40384(14) 0.0329(9) Uani 1 1 d . . . H2B H 0.2056 0.0939 0.4317 0.039 Uiso 1 1 calc R . . C3B C 0.0813(2) 0.1875(5) 0.45116(13) 0.0312(9) Uani 1 1 d . . . H3B1 H 0.1022 0.3092 0.4679 0.047 Uiso 1 1 calc R . . H3B2 H 0.1007 0.0774 0.4738 0.047 Uiso 1 1 calc R . . H3B3 H 0.0299 0.1919 0.4424 0.047 Uiso 1 1 calc R . . C4B C 0.05413(17) 0.1888(5) 0.35716(12) 0.0218(7) Uani 1 1 d . . . C5B C -0.02056(18) 0.2385(5) 0.34069(12) 0.0217(7) Uani 1 1 d . . . H5B H -0.0442 0.2511 0.3642 0.026 Uiso 1 1 calc R . . C6B C -0.12942(17) 0.3096(5) 0.27609(13) 0.0244(8) Uani 1 1 d . . . H6B1 H -0.1369 0.4450 0.2632 0.029 Uiso 1 1 calc R . . H6B2 H -0.1471 0.3003 0.3044 0.029 Uiso 1 1 calc R . . C7B C 0.17096(18) 0.6705(5) 0.26539(13) 0.0257(8) Uani 1 1 d . . . H7B1 H 0.1435 0.6473 0.2877 0.031 Uiso 1 1 calc R . . H7B2 H 0.2159 0.7345 0.2857 0.031 Uiso 1 1 calc R . . C8B C 0.18836(17) 0.4730(5) 0.24729(13) 0.0265(8) Uani 1 1 d . . . H8B1 H 0.2164 0.4931 0.2252 0.032 Uiso 1 1 calc R . . H8B2 H 0.2170 0.3940 0.2765 0.032 Uiso 1 1 calc R . . C9B C 0.10863(18) 0.3377(5) 0.17325(13) 0.0230(8) Uani 1 1 d . . . H9B H 0.1423 0.3651 0.1576 0.028 Uiso 1 1 calc R . . C10B C 0.03976(18) 0.2576(5) 0.14446(12) 0.0219(7) Uani 1 1 d . . . C11B C -0.06840(19) 0.1574(5) 0.12488(13) 0.0286(8) Uani 1 1 d . . . H11B H -0.1114 0.1131 0.1279 0.034 Uiso 1 1 calc R . . C12B C -0.0568(2) 0.1839(5) 0.08135(14) 0.0321(9) Uani 1 1 d . . . H12B H -0.0900 0.1636 0.0485 0.039 Uiso 1 1 calc R . . C13B C 0.0458(2) 0.2870(6) 0.05701(13) 0.0352(9) Uani 1 1 d . . . H13D H 0.0885 0.3646 0.0731 0.053 Uiso 1 1 calc R . . H13E H 0.0132 0.3600 0.0287 0.053 Uiso 1 1 calc R . . H13F H 0.0587 0.1643 0.0448 0.053 Uiso 1 1 calc R . . C14B C 0.21226(19) -0.0360(5) 0.08654(14) 0.0298(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02967(16) 0.03536(17) 0.02148(14) 0.00006(12) 0.01335(12) 0.00091(13) S3 0.0255(5) 0.0304(5) 0.0294(5) 0.0052(4) 0.0104(4) 0.0010(4) F1 0.0475(14) 0.0558(16) 0.0408(14) -0.0152(12) 0.0153(11) 0.0070(12) F2 0.0386(13) 0.0485(15) 0.0416(13) 0.0181(11) 0.0177(11) 0.0057(11) F3 0.0218(12) 0.0637(16) 0.0467(14) 0.0083(12) 0.0090(10) 0.0003(11) O1 0.0216(13) 0.0383(16) 0.0442(16) 0.0035(13) 0.0122(12) -0.0014(12) O2 0.0462(17) 0.0410(17) 0.0272(14) -0.0039(12) 0.0094(13) 0.0073(14) O3 0.0361(16) 0.0307(15) 0.0477(17) 0.0130(13) 0.0127(13) 0.0014(13) N1 0.0225(15) 0.0190(15) 0.0219(15) 0.0026(12) 0.0078(12) 0.0009(12) N2 0.0292(16) 0.0222(15) 0.0178(14) 0.0001(12) 0.0083(12) 0.0015(13) N3 0.0281(16) 0.0202(15) 0.0203(15) 0.0007(12) 0.0070(13) -0.0002(13) N4 0.0188(14) 0.0210(15) 0.0203(14) -0.0008(12) 0.0061(12) -0.0021(12) N5 0.0248(16) 0.0243(16) 0.0232(15) -0.0007(12) 0.0105(13) 0.0007(13) N6 0.0233(15) 0.0218(16) 0.0192(14) 0.0004(12) 0.0067(12) 0.0008(12) C1 0.0222(18) 0.0215(19) 0.029(2) 0.0001(15) 0.0063(15) 0.0006(15) C2 0.032(2) 0.0218(19) 0.0235(18) -0.0003(15) 0.0038(16) 0.0001(16) C3 0.040(2) 0.029(2) 0.0218(17) 0.0003(16) 0.0160(16) -0.0014(18) C4 0.0244(18) 0.0176(17) 0.0165(16) 0.0005(13) 0.0068(14) 0.0030(14) C5 0.0221(18) 0.0176(18) 0.0248(18) 0.0015(14) 0.0101(14) 0.0024(14) C6 0.0237(19) 0.027(2) 0.0232(18) 0.0005(15) 0.0059(15) 0.0016(16) C7 0.0220(18) 0.0242(19) 0.0205(17) 0.0047(14) 0.0051(14) 0.0029(15) C8 0.0236(18) 0.0242(18) 0.0206(16) 0.0016(14) 0.0088(14) 0.0031(15) C9 0.0236(18) 0.0189(17) 0.0215(17) -0.0018(14) 0.0104(14) -0.0001(15) C10 0.0246(19) 0.0193(18) 0.0202(17) 0.0007(14) 0.0081(15) -0.0026(15) C11 0.026(2) 0.030(2) 0.028(2) -0.0014(16) 0.0107(16) 0.0052(16) C12 0.0212(18) 0.026(2) 0.0259(19) -0.0018(15) 0.0037(15) -0.0002(15) C13 0.030(2) 0.0266(19) 0.0227(18) -0.0005(15) 0.0101(16) 0.0006(16) C14 0.024(2) 0.031(2) 0.031(2) 0.0035(17) 0.0055(16) 0.0054(17) Ag1B 0.03082(16) 0.03861(18) 0.02116(14) -0.00036(12) 0.01223(12) -0.00144(13) S1B 0.0234(5) 0.0308(5) 0.0241(4) 0.0009(4) 0.0075(4) -0.0014(4) F1B 0.0407(13) 0.0434(14) 0.0466(14) 0.0198(12) 0.0086(11) -0.0037(11) F2B 0.0219(12) 0.0466(15) 0.0555(15) 0.0053(12) 0.0050(11) -0.0013(11) F3B 0.0467(14) 0.0394(14) 0.0432(14) -0.0126(11) 0.0089(11) 0.0014(12) O1B 0.0410(16) 0.0433(17) 0.0288(14) -0.0093(12) 0.0111(12) 0.0006(13) O2B 0.0408(16) 0.0361(16) 0.0302(14) 0.0098(12) 0.0112(12) -0.0023(13) O3B 0.0229(14) 0.0402(17) 0.0490(17) -0.0016(13) 0.0095(12) -0.0010(12) N1B 0.0184(15) 0.0347(18) 0.0237(15) 0.0035(13) 0.0061(12) 0.0031(13) N2B 0.0273(16) 0.0251(16) 0.0204(15) 0.0017(12) 0.0056(12) -0.0012(13) N3B 0.0179(14) 0.0235(16) 0.0207(14) 0.0035(12) 0.0029(11) -0.0020(12) N4B 0.0250(16) 0.0206(15) 0.0249(16) 0.0002(12) 0.0089(13) -0.0006(13) N5B 0.0280(16) 0.0225(15) 0.0178(14) 0.0020(12) 0.0060(12) 0.0011(13) N6B 0.0401(19) 0.0236(17) 0.0188(14) 0.0017(12) 0.0106(13) 0.0014(14) C1B 0.022(2) 0.040(2) 0.034(2) 0.0026(18) 0.0099(17) 0.0013(17) C2B 0.023(2) 0.037(2) 0.031(2) 0.0044(17) 0.0013(16) 0.0001(17) C3B 0.040(2) 0.029(2) 0.0211(18) -0.0003(16) 0.0066(16) -0.0013(18) C4B 0.0238(18) 0.0200(18) 0.0208(17) 0.0004(14) 0.0068(14) -0.0033(15) C5B 0.0249(18) 0.0202(18) 0.0232(17) -0.0004(14) 0.0124(15) -0.0004(15) C6B 0.0206(18) 0.026(2) 0.0267(18) -0.0003(15) 0.0081(15) 0.0018(15) C7B 0.0216(18) 0.029(2) 0.0243(18) -0.0006(15) 0.0049(15) -0.0020(15) C8B 0.0194(18) 0.030(2) 0.0272(19) 0.0001(16) 0.0043(15) -0.0010(16) C9B 0.0282(19) 0.0186(18) 0.0271(19) 0.0011(14) 0.0156(16) 0.0038(15) C10B 0.0287(19) 0.0186(18) 0.0185(16) 0.0010(13) 0.0085(14) 0.0039(15) C11B 0.0243(19) 0.027(2) 0.030(2) 0.0023(16) 0.0031(16) -0.0014(16) C12B 0.040(2) 0.023(2) 0.0244(19) -0.0007(16) 0.0006(16) -0.0022(17) C13B 0.052(3) 0.035(2) 0.0216(18) 0.0002(17) 0.0170(18) 0.002(2) C14B 0.024(2) 0.032(2) 0.030(2) 0.0055(17) 0.0067(16) 0.0018(17) _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 N1 2.209(3) . yes Ag1 N4 2.271(3) . yes Ag1 N5 2.410(3) . yes Ag1 N3 2.603(3) . yes Ag1 Ag1 3.6088(4) 2_645 yes Ag1 Ag1 3.6088(4) 2_655 yes S3 O3 1.438(3) . ? S3 O2 1.440(3) . ? S3 O1 1.446(3) . ? S3 C14 1.816(4) . ? F1 C14 1.336(4) . ? F2 C14 1.343(4) . ? F3 C14 1.324(4) . ? N1 C4 1.330(4) . ? N1 C1 1.363(4) . ? N2 C4 1.352(4) . ? N2 C2 1.371(4) . ? N2 C3 1.467(4) . ? N3 C5 1.273(4) . ? N3 C6 1.463(4) 2_645 ? N4 C9 1.271(4) . ? N4 C8 1.477(4) . ? N5 C10 1.333(4) . ? N5 C11 1.367(4) . ? N6 C10 1.358(4) . ? N6 C12 1.367(4) . ? N6 C13 1.457(4) . ? C1 C2 1.373(5) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.448(5) . ? C5 H5 0.9500 . ? C6 N3 1.463(4) 2_655 ? C6 C7 1.526(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.528(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.449(5) . ? C9 H9 0.9500 . ? C11 C12 1.363(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Ag1B N5B 2.169(3) . yes Ag1B N1B 2.291(3) . yes Ag1B N3B 2.330(3) . yes Ag1B N4B 2.677(3) . yes Ag1B Ag1B 3.5279(4) 2_545 yes Ag1B Ag1B 3.5279(4) 2 yes S1B O2B 1.436(3) . ? S1B O3B 1.438(3) . ? S1B O1B 1.442(3) . ? S1B C14B 1.813(4) . ? F1B C14B 1.332(4) . ? F2B C14B 1.330(4) . ? F3B C14B 1.338(4) . ? N1B C4B 1.326(4) . ? N1B C1B 1.365(4) . ? N2B C4B 1.360(4) . ? N2B C2B 1.372(4) . ? N2B C3B 1.462(4) . ? N3B C5B 1.267(4) . ? N3B C6B 1.469(4) . ? N4B C9B 1.271(4) . ? N4B C8B 1.458(4) . ? N5B C10B 1.322(4) . ? N5B C11B 1.373(4) . ? N6B C10B 1.361(4) . ? N6B C12B 1.364(5) . ? N6B C13B 1.462(4) . ? C1B C2B 1.363(5) . ? C1B H1B 0.9500 . ? C2B H2B 0.9500 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4B C5B 1.453(5) . ? C5B H5B 0.9500 . ? C6B C7B 1.520(5) 2_545 ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B C6B 1.520(5) 2 ? C7B C8B 1.533(5) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9B C10B 1.451(5) . ? C9B H9B 0.9500 . ? C11B C12B 1.348(5) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? 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 N1 Ag1 N4 139.96(10) . . ? N1 Ag1 N5 142.89(9) . . ? N4 Ag1 N5 73.27(9) . . yes N1 Ag1 N3 70.72(9) . . yes N4 Ag1 N3 142.65(9) . . ? N5 Ag1 N3 89.05(9) . . ? N1 Ag1 Ag1 110.25(7) . 2_645 ? N4 Ag1 Ag1 67.00(7) . 2_645 ? N5 Ag1 Ag1 97.45(7) . 2_645 ? N3 Ag1 Ag1 83.61(6) . 2_645 ? N1 Ag1 Ag1 98.83(7) . 2_655 ? N4 Ag1 Ag1 76.90(7) . 2_655 ? N5 Ag1 Ag1 68.66(7) . 2_655 ? N3 Ag1 Ag1 127.42(6) . 2_655 ? Ag1 Ag1 Ag1 143.802(15) 2_645 2_655 yes O3 S3 O2 114.75(16) . . ? O3 S3 O1 115.33(16) . . ? O2 S3 O1 115.10(16) . . ? O3 S3 C14 103.45(16) . . ? O2 S3 C14 103.27(17) . . ? O1 S3 C14 102.43(16) . . ? C4 N1 C1 106.3(3) . . ? C4 N1 Ag1 117.5(2) . . ? C1 N1 Ag1 136.0(2) . . ? C4 N2 C2 107.8(3) . . ? C4 N2 C3 128.0(3) . . ? C2 N2 C3 124.1(3) . . ? C5 N3 C6 117.8(3) . 2_645 ? C5 N3 Ag1 108.9(2) . . ? C6 N3 Ag1 133.3(2) 2_645 . ? C9 N4 C8 119.2(3) . . ? C9 N4 Ag1 116.4(2) . . ? C8 N4 Ag1 124.38(19) . . ? C10 N5 C11 105.6(3) . . ? C10 N5 Ag1 107.7(2) . . ? C11 N5 Ag1 146.3(2) . . ? C10 N6 C12 107.3(3) . . ? C10 N6 C13 127.7(3) . . ? C12 N6 C13 124.9(3) . . ? N1 C1 C2 109.8(3) . . ? N1 C1 H1 125.1 . . ? C2 C1 H1 125.1 . . ? N2 C2 C1 105.6(3) . . ? N2 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 110.5(3) . . ? N1 C4 C5 123.9(3) . . ? N2 C4 C5 125.5(3) . . ? N3 C5 C4 118.6(3) . . ? N3 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N3 C6 C7 110.6(3) 2_655 . ? N3 C6 H6A 109.5 2_655 . ? C7 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 2_655 . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 114.6(3) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? N4 C8 C7 110.5(3) . . ? N4 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N4 C9 C10 119.3(3) . . ? N4 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N5 C10 N6 110.8(3) . . ? N5 C10 C9 122.9(3) . . ? N6 C10 C9 126.3(3) . . ? C12 C11 N5 110.2(3) . . ? C12 C11 H11 124.9 . . ? N5 C11 H11 124.9 . . ? C11 C12 N6 106.1(3) . . ? C11 C12 H12 126.9 . . ? N6 C12 H12 126.9 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? F3 C14 F1 107.3(3) . . ? F3 C14 F2 107.4(3) . . ? F1 C14 F2 107.0(3) . . ? F3 C14 S3 112.4(2) . . ? F1 C14 S3 111.1(3) . . ? F2 C14 S3 111.3(2) . . ? N5B Ag1B N1B 151.30(10) . . ? N5B Ag1B N3B 132.82(10) . . ? N1B Ag1B N3B 73.91(9) . . yes N5B Ag1B N4B 69.72(10) . . yes N1B Ag1B N4B 93.03(9) . . ? N3B Ag1B N4B 145.61(9) . . ? N5B Ag1B Ag1B 92.87(8) . 2_545 ? N1B Ag1B Ag1B 78.37(8) . 2_545 ? N3B Ag1B Ag1B 83.72(7) . 2_545 ? N4B Ag1B Ag1B 125.46(6) . 2_545 ? N5B Ag1B Ag1B 99.74(7) . 2 ? N1B Ag1B Ag1B 100.11(8) . 2 ? N3B Ag1B Ag1B 70.15(7) . 2 ? N4B Ag1B Ag1B 81.48(6) . 2 ? Ag1B Ag1B Ag1B 152.971(16) 2_545 2 yes O2B S1B O3B 115.17(16) . . ? O2B S1B O1B 114.99(17) . . ? O3B S1B O1B 114.55(16) . . ? O2B S1B C14B 103.12(16) . . ? O3B S1B C14B 103.49(16) . . ? O1B S1B C14B 103.16(17) . . ? C4B N1B C1B 106.4(3) . . ? C4B N1B Ag1B 110.6(2) . . ? C1B N1B Ag1B 142.7(2) . . ? C4B N2B C2B 107.0(3) . . ? C4B N2B C3B 127.5(3) . . ? C2B N2B C3B 125.5(3) . . ? C5B N3B C6B 119.7(3) . . ? C5B N3B Ag1B 113.9(2) . . ? C6B N3B Ag1B 126.3(2) . . ? C9B N4B C8B 118.4(3) . . ? C9B N4B Ag1B 107.3(2) . . ? C8B N4B Ag1B 134.3(2) . . ? C10B N5B C11B 107.0(3) . . ? C10B N5B Ag1B 119.8(2) . . ? C11B N5B Ag1B 133.0(2) . . ? C10B N6B C12B 107.4(3) . . ? C10B N6B C13B 128.0(3) . . ? C12B N6B C13B 124.6(3) . . ? C2B C1B N1B 109.5(3) . . ? C2B C1B H1B 125.2 . . ? N1B C1B H1B 125.2 . . ? C1B C2B N2B 106.5(3) . . ? C1B C2B H2B 126.8 . . ? N2B C2B H2B 126.8 . . ? N2B C3B H3B1 109.5 . . ? N2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N1B C4B N2B 110.6(3) . . ? N1B C4B C5B 123.0(3) . . ? N2B C4B C5B 126.4(3) . . ? N3B C5B C4B 118.3(3) . . ? N3B C5B H5B 120.8 . . ? C4B C5B H5B 120.8 . . ? N3B C6B C7B 111.3(3) . 2_545 ? N3B C6B H6B1 109.4 . . ? C7B C6B H6B1 109.4 2_545 . ? N3B C6B H6B2 109.4 . . ? C7B C6B H6B2 109.4 2_545 . ? H6B1 C6B H6B2 108.0 . . ? C6B C7B C8B 115.1(3) 2 . ? C6B C7B H7B1 108.5 2 . ? C8B C7B H7B1 108.5 . . ? C6B C7B H7B2 108.5 2 . ? C8B C7B H7B2 108.5 . . ? H7B1 C7B H7B2 107.5 . . ? N4B C8B C7B 109.6(3) . . ? N4B C8B H8B1 109.7 . . ? C7B C8B H8B1 109.7 . . ? N4B C8B H8B2 109.7 . . ? C7B C8B H8B2 109.7 . . ? H8B1 C8B H8B2 108.2 . . ? N4B C9B C10B 118.5(3) . . ? N4B C9B H9B 120.7 . . ? C10B C9B H9B 120.7 . . ? N5B C10B N6B 109.6(3) . . ? N5B C10B C9B 124.1(3) . . ? N6B C10B C9B 125.9(3) . . ? C12B C11B N5B 108.9(3) . . ? C12B C11B H11B 125.5 . . ? N5B C11B H11B 125.5 . . ? C11B C12B N6B 107.0(3) . . ? C11B C12B H12B 126.5 . . ? N6B C12B H12B 126.5 . . ? N6B C13B H13D 109.5 . . ? N6B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? N6B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? F2B C14B F1B 107.5(3) . . ? F2B C14B F3B 107.0(3) . . ? F1B C14B F3B 107.6(3) . . ? F2B C14B S1B 111.2(3) . . ? F1B C14B S1B 111.9(3) . . ? F3B C14B S1B 111.4(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.350 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.098