# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C18 H24 Ag F3 N8 O3 S)2' _chemical_formula_sum 'C36 H48 Ag2 F6 N16 O6 S2' _chemical_formula_weight 1194.76 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4378(19) _cell_length_b 13.969(3) _cell_length_c 17.639(4) _cell_angle_alpha 91.920(4) _cell_angle_beta 103.279(3) _cell_angle_gamma 99.284(3) _cell_volume 2227.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6636 _exptl_absorpt_correction_T_max 0.8399 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10998 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.35 _reflns_number_total 10998 _reflns_number_gt 8247 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10998 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.01888(2) 0.388534(14) 1.003579(11) 0.01839(6) Uani 1 1 d . . . Ag2 Ag 0.99161(2) 0.115104(13) 0.512035(10) 0.01798(6) Uani 1 1 d . . . N1 N 0.0391(2) 0.39649(14) 0.86809(11) 0.0146(4) Uani 1 1 d . . . N2 N 0.1448(2) 0.46869(14) 0.85246(11) 0.0130(4) Uani 1 1 d . . . N3 N 0.2163(2) 0.50993(14) 0.98486(11) 0.0136(4) Uani 1 1 d . . . N4 N 0.3625(2) 0.57827(14) 0.90095(11) 0.0134(4) Uani 1 1 d . . . N5 N 0.4496(2) 0.60761(14) 1.04064(11) 0.0134(4) Uani 1 1 d . . . N6 N 0.1919(2) 0.45403(14) 1.12263(11) 0.0134(4) Uani 1 1 d . . . N7 N 0.3069(2) 0.52640(14) 1.11820(11) 0.0126(4) Uani 1 1 d . . . N8 N 0.5742(2) 0.68868(14) 0.95673(11) 0.0136(4) Uani 1 1 d . . . N9 N 0.9765(2) 0.07716(14) 0.64289(11) 0.0137(4) Uani 1 1 d . . . N10 N 0.8683(2) 0.00188(14) 0.65076(11) 0.0129(4) Uani 1 1 d . . . N11 N 0.7887(2) -0.01028(14) 0.51649(11) 0.0137(4) Uani 1 1 d . . . N12 N 0.6426(2) -0.09623(14) 0.59407(11) 0.0132(4) Uani 1 1 d . . . N13 N 0.5491(2) -0.09629(14) 0.45477(11) 0.0131(4) Uani 1 1 d . . . N14 N 0.8098(2) 0.07674(14) 0.38935(11) 0.0140(4) Uani 1 1 d . . . N15 N 0.6911(2) 0.00222(14) 0.38600(11) 0.0125(4) Uani 1 1 d . . . N16 N 0.4255(2) -0.19582(14) 0.52936(11) 0.0141(4) Uani 1 1 d . . . C1 C 0.1356(3) 0.46951(18) 0.77280(13) 0.0147(5) Uani 1 1 d . . . C2 C 0.0211(3) 0.39684(18) 0.73850(14) 0.0186(5) Uani 1 1 d . . . H2 H -0.0138 0.3786 0.6842 0.022 Uiso 1 1 calc R . . C3 C -0.0352(3) 0.35419(18) 0.79931(14) 0.0159(5) Uani 1 1 d . . . C4 C 0.2318(3) 0.53841(19) 0.73533(14) 0.0197(5) Uani 1 1 d . . . H4A H 0.1966 0.5284 0.6784 0.030 Uiso 1 1 calc R . . H4B H 0.3338 0.5267 0.7508 0.030 Uiso 1 1 calc R . . H4C H 0.2284 0.6054 0.7522 0.030 Uiso 1 1 calc R . . C5 C -0.1592(3) 0.27109(18) 0.79388(15) 0.0208(5) Uani 1 1 d . . . H5A H -0.1330 0.2119 0.7736 0.031 Uiso 1 1 calc R . . H5B H -0.2487 0.2853 0.7586 0.031 Uiso 1 1 calc R . . H5C H -0.1773 0.2615 0.8459 0.031 Uiso 1 1 calc R . . C7 C 0.3269(2) 0.55066(17) 1.04427(13) 0.0119(5) Uani 1 1 d . . . C8 C 0.4588(2) 0.62501(17) 0.96606(14) 0.0138(5) Uani 1 1 d . . . C9 C 0.2077(3) 0.44170(17) 1.19814(14) 0.0142(5) Uani 1 1 d . . . C10 C 0.3328(3) 0.50602(17) 1.24264(13) 0.0155(5) Uani 1 1 d . . . H10 H 0.3672 0.5110 1.2979 0.019 Uiso 1 1 calc R . . C11 C 0.3948(3) 0.55934(17) 1.19164(13) 0.0141(5) Uani 1 1 d . . . C12 C 0.1048(3) 0.36626(18) 1.22555(14) 0.0191(5) Uani 1 1 d . . . H12A H 0.0156 0.3453 1.1836 0.029 Uiso 1 1 calc R . . H12B H 0.0775 0.3933 1.2711 0.029 Uiso 1 1 calc R . . H12C H 0.1533 0.3103 1.2400 0.029 Uiso 1 1 calc R . . C13 C 0.5243(3) 0.63933(18) 1.20744(14) 0.0184(5) Uani 1 1 d . . . H13A H 0.5642 0.6516 1.2640 0.028 Uiso 1 1 calc R . . H13B H 0.4937 0.6984 1.1856 0.028 Uiso 1 1 calc R . . H13C H 0.6005 0.6208 1.1832 0.028 Uiso 1 1 calc R . . C14 C 0.5908(3) 0.71002(18) 0.87813(14) 0.0164(5) Uani 1 1 d . . . H14A H 0.5586 0.6493 0.8436 0.020 Uiso 1 1 calc R . . H14B H 0.6966 0.7333 0.8804 0.020 Uiso 1 1 calc R . . C15 C 0.5019(3) 0.78604(19) 0.84332(14) 0.0209(6) Uani 1 1 d . . . H15A H 0.3982 0.7659 0.8447 0.031 Uiso 1 1 calc R . . H15B H 0.5088 0.7928 0.7891 0.031 Uiso 1 1 calc R . . H15C H 0.5414 0.8486 0.8737 0.031 Uiso 1 1 calc R . . C16 C 0.6745(3) 0.74767(18) 1.02432(14) 0.0188(5) Uani 1 1 d . . . H16A H 0.7667 0.7763 1.0097 0.023 Uiso 1 1 calc R . . H16B H 0.7010 0.7051 1.0673 0.023 Uiso 1 1 calc R . . C17 C 0.6061(3) 0.82892(18) 1.05309(15) 0.0230(6) Uani 1 1 d . . . H17A H 0.5772 0.8702 1.0104 0.034 Uiso 1 1 calc R . . H17B H 0.6783 0.8681 1.0964 0.034 Uiso 1 1 calc R . . H17C H 0.5186 0.8008 1.0711 0.034 Uiso 1 1 calc R . . C18 C -0.1868(3) 0.07768(19) 0.97228(16) 0.0232(6) Uani 1 1 d . . . C20 C 0.8847(3) -0.01989(18) 0.72836(13) 0.0153(5) Uani 1 1 d . . . C21 C 1.0069(3) 0.04239(18) 0.76879(14) 0.0167(5) Uani 1 1 d . . . H21 H 1.0486 0.0455 0.8234 0.020 Uiso 1 1 calc R . . C22 C 1.0603(3) 0.10160(17) 0.71427(14) 0.0143(5) Uani 1 1 d . . . C23 C 0.7862(3) -0.09658(18) 0.75740(14) 0.0200(5) Uani 1 1 d . . . H23A H 0.8323 -0.1072 0.8115 0.030 Uiso 1 1 calc R . . H23B H 0.7704 -0.1572 0.7246 0.030 Uiso 1 1 calc R . . H23C H 0.6911 -0.0759 0.7552 0.030 Uiso 1 1 calc R . . C24 C 1.1882(3) 0.18275(18) 0.72884(15) 0.0202(5) Uani 1 1 d . . . H24A H 1.2106 0.2004 0.6790 0.030 Uiso 1 1 calc R . . H24B H 1.2744 0.1623 0.7625 0.030 Uiso 1 1 calc R . . H24C H 1.1639 0.2391 0.7546 0.030 Uiso 1 1 calc R . . C25 C 0.7594(2) -0.03863(17) 0.58426(13) 0.0119(5) Uani 1 1 d . . . C26 C 0.6734(2) -0.03820(16) 0.45575(13) 0.0116(5) Uani 1 1 d . . . C27 C 0.5418(2) -0.12946(17) 0.52565(13) 0.0125(5) Uani 1 1 d . . . C28 C 0.6056(3) -0.01795(18) 0.31064(13) 0.0153(5) Uani 1 1 d . . . C29 C 0.6728(3) 0.04535(17) 0.26617(13) 0.0154(5) Uani 1 1 d . . . H29 H 0.6413 0.0499 0.2114 0.018 Uiso 1 1 calc R . . C30 C 0.7973(3) 0.10218(17) 0.31728(13) 0.0144(5) Uani 1 1 d . . . C31 C 0.4717(3) -0.09411(19) 0.28644(14) 0.0192(5) Uani 1 1 d . . . H31A H 0.4371 -0.0990 0.2294 0.029 Uiso 1 1 calc R . . H31B H 0.3939 -0.0769 0.3100 0.029 Uiso 1 1 calc R . . H31C H 0.4955 -0.1567 0.3039 0.029 Uiso 1 1 calc R . . C32 C 0.9028(3) 0.18451(18) 0.29954(14) 0.0183(5) Uani 1 1 d . . . H32A H 0.8584 0.2435 0.2965 0.028 Uiso 1 1 calc R . . H32B H 0.9253 0.1691 0.2495 0.028 Uiso 1 1 calc R . . H32C H 0.9941 0.1952 0.3409 0.028 Uiso 1 1 calc R . . C33 C 0.3150(3) -0.23735(18) 0.45774(14) 0.0176(5) Uani 1 1 d . . . H33A H 0.2951 -0.1848 0.4226 0.021 Uiso 1 1 calc R . . H33B H 0.2214 -0.2644 0.4716 0.021 Uiso 1 1 calc R . . C34 C 0.3642(3) -0.31638(18) 0.41490(15) 0.0233(6) Uani 1 1 d . . . H34A H 0.4505 -0.2885 0.3958 0.035 Uiso 1 1 calc R . . H34B H 0.2837 -0.3454 0.3706 0.035 Uiso 1 1 calc R . . H34C H 0.3905 -0.3666 0.4505 0.035 Uiso 1 1 calc R . . C35 C 0.4139(3) -0.23688(18) 0.60387(14) 0.0176(5) Uani 1 1 d . . . H35A H 0.3088 -0.2629 0.6012 0.021 Uiso 1 1 calc R . . H35B H 0.4477 -0.1841 0.6462 0.021 Uiso 1 1 calc R . . C36 C 0.5035(3) -0.31717(19) 0.62408(15) 0.0223(6) Uani 1 1 d . . . H36A H 0.4616 -0.3736 0.5865 0.033 Uiso 1 1 calc R . . H36B H 0.5007 -0.3360 0.6768 0.033 Uiso 1 1 calc R . . H36C H 0.6061 -0.2939 0.6220 0.033 Uiso 1 1 calc R . . C37 C 1.1664(3) 0.4223(2) 0.47212(15) 0.0238(6) Uani 1 1 d . . . S1 S -0.13171(7) 0.18044(5) 1.04463(4) 0.01763(13) Uani 1 1 d . . . O1 O -0.1810(2) 0.26022(13) 1.00080(11) 0.0261(4) Uani 1 1 d . . . O2 O 0.02678(19) 0.18960(14) 1.06755(12) 0.0331(5) Uani 1 1 d . . . O3 O -0.2096(2) 0.15135(15) 1.10256(11) 0.0370(5) Uani 1 1 d . . . F1 F -0.15474(18) -0.00393(11) 1.00351(10) 0.0335(4) Uani 1 1 d . . . F2 F -0.1181(2) 0.09050(13) 0.91488(10) 0.0469(5) Uani 1 1 d . . . F3 F -0.33193(19) 0.06204(13) 0.94078(11) 0.0507(5) Uani 1 1 d . . . S2 S 1.17683(7) 0.32560(5) 0.53888(4) 0.01725(13) Uani 1 1 d . . . C6 C 0.2474(2) 0.52293(17) 0.91516(13) 0.0128(5) Uani 1 1 d . . . O4 O 1.1879(2) 0.24195(13) 0.49112(11) 0.0280(4) Uani 1 1 d . . . O5 O 1.03767(19) 0.31579(14) 0.56126(11) 0.0282(4) Uani 1 1 d . . . O6 O 1.3055(2) 0.36241(15) 0.59949(11) 0.0313(5) Uani 1 1 d . . . F4 F 1.0449(2) 0.40169(13) 0.41409(9) 0.0398(4) Uani 1 1 d . . . F5 F 1.2819(2) 0.43538(12) 0.44015(11) 0.0449(5) Uani 1 1 d . . . F6 F 1.16310(18) 0.50634(11) 0.50909(10) 0.0309(4) 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 0.01477(10) 0.01932(11) 0.01902(10) 0.00228(8) 0.00408(7) -0.00334(7) Ag2 0.01516(10) 0.01901(11) 0.01743(10) 0.00204(8) 0.00409(7) -0.00430(7) N1 0.0117(10) 0.0128(10) 0.0179(10) 0.0017(8) 0.0021(8) -0.0003(8) N2 0.0126(10) 0.0142(11) 0.0111(10) 0.0016(8) 0.0013(7) 0.0008(8) N3 0.0116(10) 0.0159(11) 0.0117(10) 0.0001(8) 0.0020(7) -0.0010(8) N4 0.0121(10) 0.0140(10) 0.0139(10) 0.0019(8) 0.0032(8) 0.0011(8) N5 0.0131(10) 0.0123(10) 0.0132(10) 0.0021(8) 0.0015(8) 0.0002(8) N6 0.0130(10) 0.0115(10) 0.0160(10) 0.0016(8) 0.0050(8) 0.0001(8) N7 0.0125(10) 0.0127(10) 0.0108(9) -0.0001(8) 0.0020(7) -0.0019(8) N8 0.0103(10) 0.0155(11) 0.0144(10) 0.0042(8) 0.0029(8) 0.0000(8) N9 0.0120(10) 0.0109(10) 0.0168(10) 0.0022(8) 0.0024(8) -0.0010(8) N10 0.0121(10) 0.0142(10) 0.0111(10) 0.0027(8) 0.0023(7) -0.0014(8) N11 0.0137(10) 0.0154(11) 0.0107(10) 0.0016(8) 0.0029(8) -0.0010(8) N12 0.0122(10) 0.0134(10) 0.0145(10) 0.0016(8) 0.0047(8) 0.0014(8) N13 0.0112(10) 0.0138(10) 0.0139(10) 0.0022(8) 0.0029(8) 0.0008(8) N14 0.0144(10) 0.0120(10) 0.0153(10) 0.0018(8) 0.0057(8) -0.0012(8) N15 0.0117(10) 0.0152(11) 0.0092(9) 0.0019(8) 0.0015(7) -0.0009(8) N16 0.0125(10) 0.0151(11) 0.0139(10) 0.0000(8) 0.0035(8) -0.0006(8) C1 0.0147(12) 0.0192(13) 0.0111(11) 0.0001(10) 0.0025(9) 0.0067(10) C2 0.0188(13) 0.0210(14) 0.0153(12) -0.0004(10) 0.0007(10) 0.0063(10) C3 0.0142(12) 0.0159(13) 0.0171(12) -0.0002(10) 0.0010(9) 0.0051(10) C4 0.0190(13) 0.0255(15) 0.0143(12) 0.0045(10) 0.0037(10) 0.0030(11) C5 0.0177(13) 0.0177(14) 0.0239(14) -0.0017(11) 0.0018(10) -0.0004(10) C7 0.0116(11) 0.0111(12) 0.0140(11) 0.0020(9) 0.0029(9) 0.0047(9) C8 0.0113(12) 0.0144(12) 0.0163(12) 0.0025(9) 0.0037(9) 0.0035(9) C9 0.0143(12) 0.0145(12) 0.0162(12) 0.0022(10) 0.0065(9) 0.0049(9) C10 0.0203(13) 0.0165(13) 0.0101(11) 0.0009(9) 0.0024(9) 0.0060(10) C11 0.0138(12) 0.0146(13) 0.0131(11) -0.0006(9) 0.0016(9) 0.0027(9) C12 0.0218(13) 0.0158(13) 0.0202(13) 0.0042(10) 0.0092(10) -0.0015(10) C13 0.0189(13) 0.0201(14) 0.0135(12) 0.0003(10) 0.0015(9) -0.0013(10) C14 0.0154(12) 0.0181(13) 0.0174(12) 0.0029(10) 0.0087(10) 0.0009(10) C15 0.0241(14) 0.0249(15) 0.0169(13) 0.0085(11) 0.0082(10) 0.0073(11) C16 0.0131(12) 0.0230(14) 0.0183(13) 0.0051(11) 0.0022(9) -0.0010(10) C17 0.0305(15) 0.0178(14) 0.0184(13) 0.0007(11) 0.0051(11) -0.0012(11) C18 0.0221(14) 0.0208(15) 0.0262(14) 0.0001(11) 0.0034(11) 0.0056(11) C20 0.0166(12) 0.0187(13) 0.0119(11) 0.0021(10) 0.0039(9) 0.0053(10) C21 0.0173(13) 0.0206(14) 0.0116(11) -0.0012(10) 0.0022(9) 0.0036(10) C22 0.0124(12) 0.0122(12) 0.0173(12) -0.0018(9) 0.0017(9) 0.0024(9) C23 0.0195(13) 0.0237(14) 0.0150(12) 0.0044(10) 0.0031(10) -0.0001(10) C24 0.0141(12) 0.0181(14) 0.0243(14) -0.0014(11) 0.0003(10) -0.0029(10) C25 0.0124(11) 0.0120(12) 0.0116(11) 0.0027(9) 0.0017(9) 0.0040(9) C26 0.0129(12) 0.0109(12) 0.0115(11) 0.0007(9) 0.0034(9) 0.0030(9) C27 0.0115(11) 0.0137(12) 0.0130(11) 0.0016(9) 0.0035(9) 0.0030(9) C28 0.0148(12) 0.0172(13) 0.0130(12) -0.0008(10) 0.0001(9) 0.0053(10) C29 0.0183(13) 0.0171(13) 0.0111(11) 0.0018(9) 0.0018(9) 0.0064(10) C30 0.0176(12) 0.0134(12) 0.0155(12) 0.0039(9) 0.0074(9) 0.0063(9) C31 0.0183(13) 0.0220(14) 0.0148(12) 0.0003(10) 0.0010(10) 0.0001(10) C32 0.0206(13) 0.0162(13) 0.0201(13) 0.0041(10) 0.0093(10) 0.0017(10) C33 0.0115(12) 0.0194(13) 0.0186(12) 0.0013(10) 0.0005(9) -0.0022(10) C34 0.0284(15) 0.0173(14) 0.0193(13) -0.0017(11) 0.0008(11) -0.0028(11) C35 0.0170(13) 0.0183(13) 0.0178(12) 0.0029(10) 0.0079(10) -0.0018(10) C36 0.0264(15) 0.0224(14) 0.0201(13) 0.0054(11) 0.0077(11) 0.0061(11) C37 0.0320(16) 0.0223(15) 0.0226(14) 0.0035(11) 0.0163(12) 0.0062(12) S1 0.0161(3) 0.0184(3) 0.0181(3) -0.0012(2) 0.0060(2) 0.0001(2) O1 0.0212(10) 0.0177(10) 0.0379(11) 0.0047(8) 0.0052(8) 0.0011(8) O2 0.0138(10) 0.0350(12) 0.0438(12) -0.0064(10) -0.0023(8) 0.0004(8) O3 0.0464(13) 0.0430(13) 0.0297(11) 0.0064(10) 0.0251(10) 0.0076(10) F1 0.0322(10) 0.0168(9) 0.0536(11) 0.0065(8) 0.0124(8) 0.0065(7) F2 0.0815(15) 0.0423(12) 0.0274(10) 0.0029(8) 0.0275(10) 0.0202(10) F3 0.0309(10) 0.0389(11) 0.0662(14) -0.0228(10) -0.0184(9) 0.0080(8) S2 0.0146(3) 0.0181(3) 0.0175(3) 0.0030(2) 0.0036(2) -0.0014(2) C6 0.0133(12) 0.0123(12) 0.0128(11) 0.0021(9) 0.0019(9) 0.0033(9) O4 0.0334(11) 0.0174(10) 0.0335(11) 0.0008(8) 0.0104(9) 0.0024(8) O5 0.0188(10) 0.0388(12) 0.0270(10) 0.0058(9) 0.0104(8) -0.0027(8) O6 0.0194(10) 0.0379(12) 0.0289(11) -0.0005(9) -0.0067(8) 0.0013(9) F4 0.0580(12) 0.0421(11) 0.0178(8) 0.0031(8) -0.0012(8) 0.0185(9) F5 0.0632(13) 0.0284(10) 0.0645(13) 0.0159(9) 0.0534(11) 0.0125(9) F6 0.0397(10) 0.0155(8) 0.0423(10) -0.0016(7) 0.0182(8) 0.0078(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.3738(18) . ? Ag1 N6 2.393(2) . ? Ag1 N3 2.3995(19) . ? Ag1 N1 2.445(2) . ? Ag1 Ag1 3.1943(7) 2_567 ? Ag2 N11 2.3953(19) . ? Ag2 N14 2.416(2) . ? Ag2 N9 2.416(2) . ? Ag2 O4 2.4511(19) . ? Ag2 Ag2 3.2634(8) 2_756 ? N1 C3 1.319(3) . ? N1 N2 1.382(3) . ? N2 C1 1.388(3) . ? N2 C6 1.396(3) . ? N3 C7 1.333(3) . ? N3 C6 1.339(3) . ? N4 C6 1.307(3) . ? N4 C8 1.360(3) . ? N5 C7 1.311(3) . ? N5 C8 1.365(3) . ? N6 C9 1.326(3) . ? N6 N7 1.377(2) . ? N7 C11 1.386(3) . ? N7 C7 1.404(3) . ? N8 C8 1.335(3) . ? N8 C14 1.466(3) . ? N8 C16 1.470(3) . ? N9 C22 1.324(3) . ? N9 N10 1.377(2) . ? N10 C20 1.391(3) . ? N10 C25 1.402(3) . ? N11 C26 1.335(3) . ? N11 C25 1.345(3) . ? N12 C25 1.305(3) . ? N12 C27 1.367(3) . ? N13 C26 1.310(3) . ? N13 C27 1.360(3) . ? N14 C30 1.316(3) . ? N14 N15 1.389(2) . ? N15 C28 1.381(3) . ? N15 C26 1.404(3) . ? N16 C27 1.333(3) . ? N16 C35 1.471(3) . ? N16 C33 1.473(3) . ? C1 C2 1.367(3) . ? C1 C4 1.491(3) . ? C2 C3 1.411(3) . ? C3 C5 1.493(3) . ? C9 C10 1.415(3) . ? C9 C12 1.486(3) . ? C10 C11 1.361(3) . ? C11 C13 1.484(3) . ? C14 C15 1.517(3) . ? C16 C17 1.521(3) . ? C18 F2 1.324(3) . ? C18 F1 1.331(3) . ? C18 F3 1.334(3) . ? C18 S1 1.814(3) . ? C20 C21 1.361(3) . ? C20 C23 1.486(3) . ? C21 C22 1.416(3) . ? C22 C24 1.485(3) . ? C28 C29 1.376(3) . ? C28 C31 1.483(3) . ? C29 C30 1.410(3) . ? C30 C32 1.486(3) . ? C33 C34 1.509(3) . ? C35 C36 1.515(3) . ? C37 F5 1.328(3) . ? C37 F6 1.332(3) . ? C37 F4 1.334(3) . ? C37 S2 1.822(3) . ? S1 O3 1.4234(19) . ? S1 O2 1.4402(19) . ? S1 O1 1.4547(19) . ? S2 O6 1.4306(18) . ? S2 O5 1.4434(18) . ? S2 O4 1.449(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 N6 122.08(7) . . ? O1 Ag1 N3 170.82(6) . . ? N6 Ag1 N3 66.45(6) . . ? O1 Ag1 N1 105.27(7) . . ? N6 Ag1 N1 130.41(6) . . ? N3 Ag1 N1 65.63(6) . . ? O1 Ag1 Ag1 122.91(5) . 2_567 ? N6 Ag1 Ag1 80.68(5) . 2_567 ? N3 Ag1 Ag1 59.52(5) . 2_567 ? N1 Ag1 Ag1 85.96(5) . 2_567 ? N11 Ag2 N14 65.94(6) . . ? N11 Ag2 N9 66.23(6) . . ? N14 Ag2 N9 130.41(6) . . ? N11 Ag2 O4 173.39(6) . . ? N14 Ag2 O4 107.53(6) . . ? N9 Ag2 O4 120.36(6) . . ? N11 Ag2 Ag2 58.02(5) . 2_756 ? N14 Ag2 Ag2 81.51(5) . 2_756 ? N9 Ag2 Ag2 84.29(5) . 2_756 ? O4 Ag2 Ag2 121.27(5) . 2_756 ? C3 N1 N2 105.35(19) . . ? C3 N1 Ag1 136.93(16) . . ? N2 N1 Ag1 117.38(13) . . ? N1 N2 C1 111.05(19) . . ? N1 N2 C6 118.59(18) . . ? C1 N2 C6 130.2(2) . . ? C7 N3 C6 112.93(19) . . ? C7 N3 Ag1 121.76(15) . . ? C6 N3 Ag1 122.91(15) . . ? C6 N4 C8 113.82(19) . . ? C7 N5 C8 113.3(2) . . ? C9 N6 N7 105.41(18) . . ? C9 N6 Ag1 136.62(16) . . ? N7 N6 Ag1 117.93(13) . . ? N6 N7 C11 111.44(18) . . ? N6 N7 C7 118.81(18) . . ? C11 N7 C7 129.5(2) . . ? C8 N8 C14 120.2(2) . . ? C8 N8 C16 120.42(19) . . ? C14 N8 C16 118.87(18) . . ? C22 N9 N10 105.53(18) . . ? C22 N9 Ag2 136.12(16) . . ? N10 N9 Ag2 117.60(13) . . ? N9 N10 C20 111.21(18) . . ? N9 N10 C25 118.89(18) . . ? C20 N10 C25 129.87(19) . . ? C26 N11 C25 112.27(19) . . ? C26 N11 Ag2 122.98(15) . . ? C25 N11 Ag2 122.21(15) . . ? C25 N12 C27 113.44(19) . . ? C26 N13 C27 113.43(19) . . ? C30 N14 N15 105.59(18) . . ? C30 N14 Ag2 136.18(16) . . ? N15 N14 Ag2 117.82(13) . . ? C28 N15 N14 111.06(18) . . ? C28 N15 C26 130.5(2) . . ? N14 N15 C26 118.42(18) . . ? C27 N16 C35 120.47(19) . . ? C27 N16 C33 120.62(19) . . ? C35 N16 C33 118.55(18) . . ? C2 C1 N2 105.6(2) . . ? C2 C1 C4 129.0(2) . . ? N2 C1 C4 125.4(2) . . ? C1 C2 C3 106.8(2) . . ? N1 C3 C2 111.2(2) . . ? N1 C3 C5 120.1(2) . . ? C2 C3 C5 128.6(2) . . ? N5 C7 N3 127.5(2) . . ? N5 C7 N7 118.2(2) . . ? N3 C7 N7 114.3(2) . . ? N8 C8 N4 118.0(2) . . ? N8 C8 N5 117.6(2) . . ? N4 C8 N5 124.3(2) . . ? N6 C9 C10 110.4(2) . . ? N6 C9 C12 120.8(2) . . ? C10 C9 C12 128.7(2) . . ? C11 C10 C9 107.3(2) . . ? C10 C11 N7 105.4(2) . . ? C10 C11 C13 129.5(2) . . ? N7 C11 C13 125.0(2) . . ? N8 C14 C15 112.76(19) . . ? N8 C16 C17 112.3(2) . . ? F2 C18 F1 106.8(2) . . ? F2 C18 F3 107.9(2) . . ? F1 C18 F3 107.0(2) . . ? F2 C18 S1 111.78(19) . . ? F1 C18 S1 111.45(19) . . ? F3 C18 S1 111.71(18) . . ? C21 C20 N10 105.5(2) . . ? C21 C20 C23 129.3(2) . . ? N10 C20 C23 125.2(2) . . ? C20 C21 C22 107.2(2) . . ? N9 C22 C21 110.6(2) . . ? N9 C22 C24 120.8(2) . . ? C21 C22 C24 128.6(2) . . ? N12 C25 N11 127.6(2) . . ? N12 C25 N10 118.3(2) . . ? N11 C25 N10 114.12(19) . . ? N13 C26 N11 127.8(2) . . ? N13 C26 N15 118.2(2) . . ? N11 C26 N15 114.02(19) . . ? N16 C27 N13 118.0(2) . . ? N16 C27 N12 117.6(2) . . ? N13 C27 N12 124.4(2) . . ? C29 C28 N15 105.4(2) . . ? C29 C28 C31 129.5(2) . . ? N15 C28 C31 125.0(2) . . ? C28 C29 C30 106.9(2) . . ? N14 C30 C29 111.0(2) . . ? N14 C30 C32 120.4(2) . . ? C29 C30 C32 128.6(2) . . ? N16 C33 C34 112.8(2) . . ? N16 C35 C36 113.48(19) . . ? F5 C37 F6 107.8(2) . . ? F5 C37 F4 107.5(2) . . ? F6 C37 F4 107.8(2) . . ? F5 C37 S2 111.41(19) . . ? F6 C37 S2 111.01(17) . . ? F4 C37 S2 111.14(18) . . ? O3 S1 O2 116.25(13) . . ? O3 S1 O1 114.82(12) . . ? O2 S1 O1 113.29(12) . . ? O3 S1 C18 103.55(13) . . ? O2 S1 C18 103.46(12) . . ? O1 S1 C18 103.23(12) . . ? S1 O1 Ag1 111.43(10) . . ? O6 S2 O5 115.74(12) . . ? O6 S2 O4 115.37(12) . . ? O5 S2 O4 112.71(12) . . ? O6 S2 C37 103.67(13) . . ? O5 S2 C37 103.32(12) . . ? O4 S2 C37 103.96(12) . . ? N4 C6 N3 127.1(2) . . ? N4 C6 N2 118.3(2) . . ? N3 C6 N2 114.6(2) . . ? S2 O4 Ag2 103.72(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.787 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 948731' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 Ag2 F6 N14 O8 S2' _chemical_formula_sum 'C30 H34 Ag2 F6 N14 O8 S2' _chemical_formula_weight 1112.59 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9492(6) _cell_length_b 13.8345(9) _cell_length_c 16.1715(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.7840(10) _cell_angle_gamma 90.00 _cell_volume 1960.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6712 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15235 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4488 _reflns_number_gt 3353 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.5078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4488 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.59930(3) 0.093176(16) 0.022587(14) 0.02821(9) Uani 1 1 d . . . S2 S 0.38687(8) 0.29007(5) -0.03336(4) 0.02338(17) Uani 1 1 d . . . O1 O 0.4469(3) 0.22340(14) 0.03468(12) 0.0335(5) Uani 1 1 d . . . O2 O 0.4970(2) 0.32497(16) -0.07958(13) 0.0350(5) Uani 1 1 d . . . O3 O 0.2411(3) 0.26290(17) -0.08315(12) 0.0404(6) Uani 1 1 d . . . N1 N 0.7802(3) 0.09205(16) 0.16286(14) 0.0225(5) Uani 1 1 d . . . N4 N 1.0142(3) -0.10262(16) 0.11891(14) 0.0214(5) Uani 1 1 d . . . N7 N 0.6164(3) 0.01578(16) -0.10682(13) 0.0221(5) Uani 1 1 d . . . N5 N 0.9301(3) -0.14110(17) -0.02755(13) 0.0211(5) Uani 1 1 d . . . N6 N 0.7207(3) -0.05837(16) -0.10380(13) 0.0202(5) Uani 1 1 d . . . N2 N 0.8811(3) 0.01487(16) 0.17707(13) 0.0210(5) Uani 1 1 d . . . N3 N 0.7944(3) -0.02765(16) 0.03819(13) 0.0194(5) Uani 1 1 d . . . O4 O 1.1302(2) -0.21752(14) 0.05868(12) 0.0269(5) Uani 1 1 d . . . C9 C 0.7124(3) -0.09852(19) -0.18337(17) 0.0227(6) Uani 1 1 d . . . C8 C 0.8198(3) -0.07779(18) -0.02753(16) 0.0189(6) Uani 1 1 d . . . C13 C 0.4266(3) 0.0969(2) -0.21476(18) 0.0284(7) Uani 1 1 d . . . H13A H 0.3950 0.1233 -0.1662 0.043 Uiso 1 1 calc R . . H13B H 0.3405 0.0680 -0.2517 0.043 Uiso 1 1 calc R . . H13C H 0.4674 0.1475 -0.2442 0.043 Uiso 1 1 calc R . . C6 C 0.8984(3) -0.04214(19) 0.10834(16) 0.0194(6) Uani 1 1 d . . . C3 C 0.9500(3) 0.0082(2) 0.26172(16) 0.0231(6) Uani 1 1 d . . . C11 C 0.5461(3) 0.0221(2) -0.18719(16) 0.0234(6) Uani 1 1 d . . . C7 C 1.0192(3) -0.1526(2) 0.04836(17) 0.0221(6) Uani 1 1 d . . . C10 C 0.6029(3) -0.0471(2) -0.23597(17) 0.0250(6) Uani 1 1 d . . . H10 H 0.5714 -0.0562 -0.2939 0.030 Uiso 1 1 calc R . . C1 C 0.7881(3) 0.1326(2) 0.23731(17) 0.0239(6) Uani 1 1 d . . . C2 C 0.8927(4) 0.0823(2) 0.30050(17) 0.0278(7) Uani 1 1 d . . . H2 H 0.9174 0.0974 0.3577 0.033 Uiso 1 1 calc R . . C12 C 0.8027(3) -0.1827(2) -0.20208(17) 0.0282(7) Uani 1 1 d . . . H12A H 0.7757 -0.1974 -0.2613 0.042 Uiso 1 1 calc R . . H12B H 0.7812 -0.2376 -0.1700 0.042 Uiso 1 1 calc R . . H12C H 0.9095 -0.1677 -0.1870 0.042 Uiso 1 1 calc R . . C4 C 0.6940(4) 0.2183(2) 0.24702(18) 0.0302(7) Uani 1 1 d . . . H4A H 0.6337 0.2360 0.1930 0.045 Uiso 1 1 calc R . . H4B H 0.7595 0.2712 0.2692 0.045 Uiso 1 1 calc R . . H4C H 0.6280 0.2034 0.2852 0.045 Uiso 1 1 calc R . . C5 C 1.0589(4) -0.0691(2) 0.29870(17) 0.0299(7) Uani 1 1 d . . . H5A H 1.0827 -0.0627 0.3591 0.045 Uiso 1 1 calc R . . H5B H 1.1508 -0.0634 0.2771 0.045 Uiso 1 1 calc R . . H5C H 1.0135 -0.1312 0.2838 0.045 Uiso 1 1 calc R . . C14 C 0.3432(4) 0.3959(2) 0.0248(2) 0.0308(7) Uani 1 1 d . . . F1 F 0.2376(2) 0.37528(14) 0.06996(12) 0.0454(5) Uani 1 1 d . . . F2 F 0.4655(3) 0.42757(14) 0.07778(13) 0.0518(6) Uani 1 1 d . . . F3 F 0.2889(3) 0.46697(14) -0.02764(14) 0.0582(6) Uani 1 1 d . . . C15 C 1.1376(4) -0.2799(2) -0.01296(18) 0.0296(7) Uani 1 1 d . . . H15A H 1.0437 -0.3150 -0.0288 0.044 Uiso 1 1 calc R . . H15B H 1.2208 -0.3245 0.0024 0.044 Uiso 1 1 calc R . . H15C H 1.1532 -0.2411 -0.0597 0.044 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 0.02693(14) 0.02809(14) 0.02917(14) -0.00282(10) 0.00466(10) 0.00385(10) S2 0.0279(4) 0.0230(4) 0.0192(3) 0.0023(3) 0.0050(3) -0.0017(3) O1 0.0486(14) 0.0260(11) 0.0275(11) 0.0095(9) 0.0112(10) 0.0123(10) O2 0.0321(13) 0.0452(14) 0.0298(11) 0.0052(10) 0.0118(10) 0.0015(10) O3 0.0416(14) 0.0503(14) 0.0260(11) 0.0015(10) -0.0006(10) -0.0181(11) N1 0.0234(13) 0.0237(12) 0.0199(11) -0.0014(10) 0.0034(10) -0.0006(10) N4 0.0201(13) 0.0257(13) 0.0179(11) -0.0014(9) 0.0025(9) -0.0007(10) N7 0.0196(13) 0.0264(13) 0.0189(11) 0.0003(10) 0.0008(9) 0.0004(10) N5 0.0222(13) 0.0231(12) 0.0185(11) 0.0007(9) 0.0054(10) -0.0011(10) N6 0.0223(13) 0.0220(11) 0.0161(11) -0.0019(9) 0.0036(9) -0.0014(10) N2 0.0239(13) 0.0213(12) 0.0174(11) 0.0004(9) 0.0036(9) -0.0016(10) N3 0.0203(12) 0.0235(12) 0.0139(11) -0.0005(9) 0.0023(9) -0.0010(10) O4 0.0263(12) 0.0301(11) 0.0225(10) -0.0041(9) 0.0009(9) 0.0063(9) C9 0.0278(16) 0.0262(15) 0.0153(12) -0.0018(11) 0.0072(11) -0.0086(12) C8 0.0211(15) 0.0195(14) 0.0160(13) 0.0022(10) 0.0032(11) -0.0060(11) C13 0.0252(17) 0.0338(17) 0.0233(14) 0.0049(13) -0.0016(12) -0.0001(13) C6 0.0189(15) 0.0208(14) 0.0184(13) 0.0000(11) 0.0035(11) -0.0048(11) C3 0.0253(16) 0.0249(15) 0.0184(13) 0.0025(11) 0.0031(12) -0.0042(12) C11 0.0219(15) 0.0268(15) 0.0208(14) 0.0018(12) 0.0029(11) -0.0065(12) C7 0.0224(15) 0.0233(14) 0.0216(14) -0.0008(12) 0.0067(11) -0.0055(12) C10 0.0267(17) 0.0313(16) 0.0162(13) 0.0001(12) 0.0025(12) -0.0075(13) C1 0.0244(16) 0.0269(14) 0.0208(14) -0.0014(12) 0.0056(12) -0.0044(13) C2 0.0319(18) 0.0350(17) 0.0160(13) -0.0032(12) 0.0037(12) -0.0040(14) C12 0.0349(18) 0.0306(16) 0.0186(14) -0.0053(12) 0.0042(13) -0.0033(14) C4 0.0342(18) 0.0299(16) 0.0281(15) -0.0054(13) 0.0102(13) 0.0000(14) C5 0.0363(19) 0.0338(16) 0.0179(14) 0.0022(12) 0.0016(13) 0.0020(14) C14 0.0322(18) 0.0269(16) 0.0349(17) 0.0071(13) 0.0107(14) 0.0005(13) F1 0.0471(13) 0.0484(12) 0.0481(12) 0.0000(10) 0.0270(10) 0.0019(10) F2 0.0573(15) 0.0490(12) 0.0477(12) -0.0184(10) 0.0074(11) -0.0220(11) F3 0.0795(17) 0.0330(11) 0.0661(14) 0.0224(10) 0.0244(12) 0.0216(11) C15 0.0302(18) 0.0309(17) 0.0290(16) -0.0050(13) 0.0087(13) 0.0038(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 O1 2.292(2) . ? Ag1 N7 2.383(2) . ? Ag1 N3 2.393(2) . ? Ag1 N1 2.503(2) . ? Ag1 Ag1 3.1319(5) 3_655 ? S2 O3 1.436(2) . ? S2 O2 1.437(2) . ? S2 O1 1.452(2) . ? S2 C14 1.826(3) . ? N1 C1 1.317(3) . ? N1 N2 1.387(3) . ? N4 C6 1.316(3) . ? N4 C7 1.343(3) . ? N7 C11 1.326(3) . ? N7 N6 1.381(3) . ? N5 C8 1.319(4) . ? N5 C7 1.330(3) . ? N6 C9 1.390(3) . ? N6 C8 1.391(3) . ? N2 C3 1.385(3) . ? N2 C6 1.397(3) . ? N3 C8 1.327(3) . ? N3 C6 1.327(3) . ? O4 C7 1.324(3) . ? O4 C15 1.457(3) . ? C9 C10 1.360(4) . ? C9 C12 1.483(4) . ? C13 C11 1.489(4) . ? C3 C2 1.356(4) . ? C3 C5 1.488(4) . ? C11 C10 1.400(4) . ? C1 C2 1.419(4) . ? C1 C4 1.481(4) . ? C14 F2 1.319(4) . ? C14 F3 1.325(3) . ? C14 F1 1.337(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 N7 125.03(7) . . ? O1 Ag1 N3 166.95(7) . . ? N7 Ag1 N3 66.58(7) . . ? O1 Ag1 N1 102.33(7) . . ? N7 Ag1 N1 130.34(8) . . ? N3 Ag1 N1 64.99(7) . . ? O1 Ag1 Ag1 110.34(6) . 3_655 ? N7 Ag1 Ag1 63.92(6) . 3_655 ? N3 Ag1 Ag1 79.44(5) . 3_655 ? N1 Ag1 Ag1 115.94(5) . 3_655 ? O3 S2 O2 115.93(13) . . ? O3 S2 O1 114.30(13) . . ? O2 S2 O1 114.90(13) . . ? O3 S2 C14 103.50(15) . . ? O2 S2 C14 103.92(13) . . ? O1 S2 C14 101.75(13) . . ? S2 O1 Ag1 124.67(12) . . ? C1 N1 N2 105.4(2) . . ? C1 N1 Ag1 136.9(2) . . ? N2 N1 Ag1 115.69(15) . . ? C6 N4 C7 112.3(2) . . ? C11 N7 N6 105.4(2) . . ? C11 N7 Ag1 136.77(19) . . ? N6 N7 Ag1 117.82(15) . . ? C8 N5 C7 112.8(2) . . ? N7 N6 C9 110.9(2) . . ? N7 N6 C8 118.6(2) . . ? C9 N6 C8 130.4(2) . . ? C3 N2 N1 111.0(2) . . ? C3 N2 C6 130.5(2) . . ? N1 N2 C6 118.5(2) . . ? C8 N3 C6 113.6(2) . . ? C8 N3 Ag1 121.42(17) . . ? C6 N3 Ag1 124.37(18) . . ? C7 O4 C15 117.1(2) . . ? C10 C9 N6 105.4(3) . . ? C10 C9 C12 129.5(2) . . ? N6 C9 C12 125.1(2) . . ? N5 C8 N3 126.7(2) . . ? N5 C8 N6 118.0(2) . . ? N3 C8 N6 115.3(2) . . ? N4 C6 N3 127.1(2) . . ? N4 C6 N2 117.9(2) . . ? N3 C6 N2 115.0(2) . . ? C2 C3 N2 105.8(2) . . ? C2 C3 C5 129.5(3) . . ? N2 C3 C5 124.6(3) . . ? N7 C11 C10 110.7(2) . . ? N7 C11 C13 120.5(3) . . ? C10 C11 C13 128.8(2) . . ? O4 C7 N5 119.4(2) . . ? O4 C7 N4 113.4(2) . . ? N5 C7 N4 127.2(3) . . ? C9 C10 C11 107.6(2) . . ? N1 C1 C2 110.7(3) . . ? N1 C1 C4 120.8(3) . . ? C2 C1 C4 128.4(3) . . ? C3 C2 C1 107.1(2) . . ? F2 C14 F3 108.4(3) . . ? F2 C14 F1 107.6(3) . . ? F3 C14 F1 107.5(3) . . ? F2 C14 S2 111.4(2) . . ? F3 C14 S2 110.7(2) . . ? F1 C14 S2 111.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.415 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 948732'