# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'R Puddephatt' _publ_contact_author_email PUDD@UWO.CA _publ_section_title ; Dynamic Ring-Opening Polymerization of Silver(I) Complexes with Bis(amidopyridine) Ligands ; loop_ _publ_author_name 'R Puddephatt' 'Michael C Jennings' 'Nancy Yue' # Attachment '10.cif' data_04082 _database_code_depnum_ccdc_archive 'CCDC 747042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Ag Cl2 F3 N4 O4' _chemical_formula_weight 708.30 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' F F 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7192(4) _cell_length_b 12.2831(7) _cell_length_c 13.4164(7) _cell_angle_alpha 67.884(2) _cell_angle_beta 77.113(3) _cell_angle_gamma 74.065(3) _cell_volume 1559.35(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5443 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7355 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16542 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5443 _reflns_number_gt 4329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 5443 _refine_ls_number_parameters 415 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Ag Ag 0.45388(2) 0.33454(2) -0.66143(2) 0.02762(11) Uani 1 1 d . . . N1 N 0.3844(3) 0.4998(2) -0.7894(2) 0.0272(7) Uani 1 1 d . . . C2 C 0.4645(3) 0.5555(3) -0.8741(3) 0.0351(9) Uani 1 1 d . . . H2A H 0.5557 0.5218 -0.8781 0.042 Uiso 1 1 calc R . . C3 C 0.4203(3) 0.6592(3) -0.9556(3) 0.0318(9) Uani 1 1 d . . . H3A H 0.4810 0.6964 -1.0132 0.038 Uiso 1 1 calc R . . C4 C 0.2878(3) 0.7094(3) -0.9539(3) 0.0241(8) Uani 1 1 d . . . C5 C 0.2046(3) 0.6511(3) -0.8661(3) 0.0320(9) Uani 1 1 d . . . H5A H 0.1128 0.6820 -0.8609 0.038 Uiso 1 1 calc R . . C6 C 0.2557(3) 0.5493(3) -0.7879(3) 0.0334(9) Uani 1 1 d . . . H6A H 0.1971 0.5112 -0.7288 0.040 Uiso 1 1 calc R . . C7 C 0.2330(3) 0.8211(3) -1.0420(3) 0.0240(8) Uani 1 1 d . . . H7A H 0.1696 0.8776 -1.0087 0.029 Uiso 1 1 calc R . . H7B H 0.3048 0.8614 -1.0873 0.029 Uiso 1 1 calc R . . N8 N 0.1677(2) 0.7917(2) -1.1104(2) 0.0240(6) Uani 1 1 d . . . H8A H 0.0816 0.8083 -1.1039 0.029 Uiso 1 1 calc R . . C9 C 0.2370(3) 0.7400(3) -1.1826(3) 0.0229(8) Uani 1 1 d . . . O10 O 0.3586(2) 0.7208(2) -1.19831(19) 0.0322(6) Uani 1 1 d . . . C11 C 0.1633(3) 0.7018(3) -1.2415(2) 0.0208(7) Uani 1 1 d . . . C12 C 0.0305(3) 0.7538(3) -1.2504(2) 0.0223(7) Uani 1 1 d . . . H12A H -0.0125 0.8170 -1.2223 0.027 Uiso 1 1 calc R . . C13 C -0.0374(3) 0.7123(3) -1.3005(2) 0.0212(7) Uani 1 1 d . . . C14 C 0.0270(3) 0.6232(3) -1.3448(2) 0.0231(7) Uani 1 1 d . . . H14A H -0.0200 0.5975 -1.3812 0.028 Uiso 1 1 calc R . . C15 C 0.1594(3) 0.5701(3) -1.3373(3) 0.0249(8) Uani 1 1 d . A . C16 C 0.2239(3) 0.6117(3) -1.2848(2) 0.0217(7) Uani 1 1 d . . . H16A H 0.3138 0.5768 -1.2782 0.026 Uiso 1 1 calc R . . C17 C -0.1817(3) 0.7603(3) -1.3049(3) 0.0223(8) Uani 1 1 d . . . O18 O -0.2383(2) 0.7422(2) -1.36609(18) 0.0280(6) Uani 1 1 d . . . N19 N -0.2453(2) 0.8231(2) -1.2389(2) 0.0237(6) Uani 1 1 d . . . H19A H -0.2017 0.8330 -1.1957 0.028 Uiso 1 1 calc R . . C20 C -0.3854(3) 0.8754(3) -1.2374(3) 0.0258(8) Uani 1 1 d . . . H20A H -0.4180 0.8999 -1.1722 0.031 Uiso 1 1 calc R . . H20B H -0.4318 0.8134 -1.2314 0.031 Uiso 1 1 calc R . . C21 C -0.4180(3) 0.9841(3) -1.3379(3) 0.0233(7) Uani 1 1 d . . . C22 C -0.3273(3) 1.0489(3) -1.4061(3) 0.0290(8) Uani 1 1 d . . . H22A H -0.2386 1.0249 -1.3931 0.035 Uiso 1 1 calc R . . C23 C -0.3657(3) 1.1484(3) -1.4931(3) 0.0292(8) Uani 1 1 d . . . H23A H -0.3015 1.1919 -1.5390 0.035 Uiso 1 1 calc R . . N24 N -0.4888(2) 1.1874(2) -1.5167(2) 0.0241(6) Uani 1 1 d . . . C25 C -0.5777(3) 1.1230(3) -1.4495(3) 0.0242(8) Uani 1 1 d . . . H25A H -0.6656 1.1478 -1.4648 0.029 Uiso 1 1 calc R . . C26 C -0.5467(3) 1.0243(3) -1.3612(3) 0.0232(7) Uani 1 1 d . . . H26A H -0.6126 0.9830 -1.3155 0.028 Uiso 1 1 calc R . . C27 C 0.2289(3) 0.4717(3) -1.3851(3) 0.0350(9) Uani 1 1 d . . . C28A C 0.2367(8) 0.5169(9) -1.5048(6) 0.066(2) Uani 0.60 1 d P A 1 H28A H 0.1540 0.5178 -1.5251 0.099 Uiso 0.60 1 calc PR A 1 H28B H 0.3084 0.4643 -1.5351 0.099 Uiso 0.60 1 calc PR A 1 H28C H 0.2528 0.5987 -1.5336 0.099 Uiso 0.60 1 calc PR A 1 C29A C 0.1452(6) 0.3683(7) -1.3391(8) 0.060(2) Uani 0.60 1 d P A 1 H29A H 0.0824 0.3791 -1.2764 0.090 Uiso 0.60 1 calc PR A 1 H29B H 0.2043 0.2893 -1.3170 0.090 Uiso 0.60 1 calc PR A 1 H29C H 0.0979 0.3736 -1.3959 0.090 Uiso 0.60 1 calc PR A 1 C30A C 0.3664(7) 0.4098(8) -1.3519(8) 0.050(2) Uani 0.60 1 d P A 1 H30A H 0.3588 0.3484 -1.2797 0.075 Uiso 0.60 1 calc PR A 1 H30B H 0.4095 0.4697 -1.3500 0.075 Uiso 0.60 1 calc PR A 1 H30C H 0.4185 0.3718 -1.4047 0.075 Uiso 0.60 1 calc PR A 1 C28B C 0.2878(17) 0.3653(12) -1.3014(12) 0.086(5) Uani 0.40 1 d P A 2 H28D H 0.2188 0.3335 -1.2449 0.129 Uiso 0.40 1 calc PR A 2 H28E H 0.3471 0.3869 -1.2693 0.129 Uiso 0.40 1 calc PR A 2 H28F H 0.3372 0.3040 -1.3338 0.129 Uiso 0.40 1 calc PR A 2 C29B C 0.3474(12) 0.5181(13) -1.4731(11) 0.076(4) Uani 0.40 1 d P A 2 H29D H 0.3659 0.5861 -1.4617 0.113 Uiso 0.40 1 calc PR A 2 H29E H 0.3235 0.5438 -1.5462 0.113 Uiso 0.40 1 calc PR A 2 H29F H 0.4254 0.4528 -1.4654 0.113 Uiso 0.40 1 calc PR A 2 C30B C 0.1494(11) 0.4442(11) -1.4471(10) 0.056(3) Uani 0.40 1 d P A 2 H30D H 0.2035 0.3832 -1.4783 0.084 Uiso 0.40 1 calc PR A 2 H30E H 0.1178 0.5175 -1.5056 0.084 Uiso 0.40 1 calc PR A 2 H30F H 0.0745 0.4137 -1.3983 0.084 Uiso 0.40 1 calc PR A 2 C51 C -0.0007(5) 0.9037(5) -0.7291(4) 0.0694(15) Uani 0.45 1 d PD B 1 H51A H -0.0180 0.9811 -0.7891 0.083 Uiso 0.45 1 calc PR B 1 H51B H -0.0401 0.8464 -0.7414 0.083 Uiso 0.45 1 calc PR B 1 Cl52 Cl 0.1692(5) 0.8488(5) -0.7349(4) 0.1122(16) Uani 0.45 1 d PD B 1 Cl53 Cl -0.0753(8) 0.9248(9) -0.6129(8) 0.143(4) Uani 0.45 1 d PD B 1 C54 C -0.0007(5) 0.9037(5) -0.7291(4) 0.0694(15) Uani 0.55 1 d PD C 2 H54A H -0.0494 0.8697 -0.7608 0.083 Uiso 0.55 1 calc PR C 2 H54B H 0.0343 0.9701 -0.7878 0.083 Uiso 0.55 1 calc PR C 2 Cl55 Cl 0.1267(3) 0.7927(3) -0.6666(4) 0.0971(11) Uani 0.55 1 d PD C 2 Cl56 Cl -0.1057(4) 0.9571(4) -0.6264(4) 0.0538(8) Uani 0.55 1 d PD C 2 O31 O 0.0899(3) 1.1473(3) -1.0837(2) 0.0641(9) Uani 1 1 d . . . O32 O 0.1202(2) 1.1452(3) -0.9255(2) 0.0499(8) Uani 1 1 d . . . C33 C 0.1563(3) 1.1356(3) -1.0155(3) 0.0323(9) Uani 1 1 d . . . C34 C 0.3061(3) 1.1020(4) -1.0432(3) 0.0351(9) Uani 1 1 d . . . F35 F 0.3471(2) 1.0890(3) -1.1395(2) 0.0625(7) Uani 1 1 d . . . F36 F 0.3632(2) 1.1853(2) -1.0408(2) 0.0636(7) Uani 1 1 d . . . F37 F 0.3562(2) 0.9996(2) -0.9710(2) 0.0622(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02608(15) 0.02751(17) 0.02434(15) -0.00251(11) -0.00806(10) -0.00301(10) N1 0.0277(15) 0.0274(17) 0.0227(15) -0.0038(13) -0.0048(12) -0.0053(12) C2 0.0188(17) 0.045(2) 0.033(2) -0.0036(18) -0.0070(15) -0.0035(15) C3 0.0268(18) 0.031(2) 0.0299(19) 0.0005(16) -0.0041(15) -0.0097(15) C4 0.0300(18) 0.0220(19) 0.0244(18) -0.0061(15) -0.0126(14) -0.0073(14) C5 0.0192(17) 0.039(2) 0.0298(19) -0.0081(17) -0.0036(14) 0.0013(15) C6 0.0243(18) 0.035(2) 0.0281(19) 0.0005(17) -0.0004(15) -0.0042(15) C7 0.0272(17) 0.0197(18) 0.0271(18) -0.0071(14) -0.0094(14) -0.0047(14) N8 0.0193(13) 0.0282(17) 0.0251(15) -0.0089(13) -0.0078(12) -0.0024(11) C9 0.0224(18) 0.0197(18) 0.0237(17) -0.0023(15) -0.0069(14) -0.0040(13) O10 0.0157(12) 0.0458(16) 0.0389(14) -0.0210(12) -0.0023(10) -0.0042(10) C11 0.0183(15) 0.0227(18) 0.0183(16) -0.0018(14) -0.0040(13) -0.0053(13) C12 0.0215(16) 0.0235(19) 0.0215(17) -0.0088(14) -0.0020(13) -0.0030(13) C13 0.0186(16) 0.0222(18) 0.0163(16) 0.0005(14) -0.0031(13) -0.0035(13) C14 0.0202(16) 0.0291(19) 0.0212(17) -0.0073(15) -0.0041(13) -0.0079(14) C15 0.0261(17) 0.0254(19) 0.0216(17) -0.0057(15) -0.0031(14) -0.0061(14) C16 0.0114(15) 0.0265(19) 0.0209(16) -0.0036(14) -0.0011(12) -0.0011(13) C17 0.0214(16) 0.0211(18) 0.0193(17) 0.0010(14) -0.0058(14) -0.0052(13) O18 0.0246(12) 0.0337(14) 0.0277(13) -0.0095(11) -0.0118(10) -0.0039(10) N19 0.0183(13) 0.0273(16) 0.0227(14) -0.0061(13) -0.0064(11) -0.0006(12) C20 0.0176(16) 0.029(2) 0.0251(17) -0.0054(15) -0.0069(13) 0.0010(14) C21 0.0207(16) 0.0257(19) 0.0239(17) -0.0105(15) -0.0048(13) -0.0013(14) C22 0.0186(16) 0.031(2) 0.033(2) -0.0033(17) -0.0094(14) -0.0044(14) C23 0.0213(17) 0.027(2) 0.034(2) -0.0031(16) -0.0033(15) -0.0070(14) N24 0.0243(14) 0.0223(16) 0.0245(15) -0.0061(12) -0.0092(12) -0.0006(12) C25 0.0196(16) 0.028(2) 0.0247(18) -0.0097(15) -0.0043(14) -0.0021(14) C26 0.0217(16) 0.0275(19) 0.0209(17) -0.0084(15) -0.0051(13) -0.0039(14) C27 0.0261(18) 0.039(2) 0.045(2) -0.0262(19) -0.0023(16) 0.0004(16) C28A 0.056(5) 0.093(7) 0.043(4) -0.039(5) -0.001(4) 0.010(5) C29A 0.036(4) 0.046(5) 0.116(8) -0.057(5) 0.006(4) -0.007(3) C30A 0.032(4) 0.060(6) 0.072(6) -0.048(5) -0.006(4) 0.006(4) C28B 0.127(14) 0.054(10) 0.083(11) -0.053(9) -0.056(10) 0.047(9) C29B 0.065(8) 0.090(11) 0.087(10) -0.068(9) 0.044(7) -0.029(7) C30B 0.057(7) 0.050(7) 0.066(8) -0.024(6) -0.011(6) -0.010(6) C51 0.086(4) 0.059(3) 0.069(3) -0.015(3) -0.021(3) -0.024(3) Cl52 0.123(4) 0.127(4) 0.121(4) -0.077(3) -0.010(3) -0.035(3) Cl53 0.136(7) 0.215(10) 0.095(5) -0.062(6) 0.012(4) -0.070(6) C54 0.086(4) 0.059(3) 0.069(3) -0.015(3) -0.021(3) -0.024(3) Cl55 0.084(2) 0.074(2) 0.151(4) -0.063(2) -0.048(2) 0.0150(16) Cl56 0.0460(14) 0.0519(14) 0.0534(17) -0.0034(12) 0.0074(12) -0.0259(12) O31 0.0414(16) 0.100(3) 0.0547(19) -0.0353(18) -0.0194(15) 0.0021(16) O32 0.0316(14) 0.083(2) 0.0461(18) -0.0398(16) 0.0014(13) -0.0097(14) C33 0.0263(18) 0.037(2) 0.034(2) -0.0142(18) -0.0063(17) -0.0016(16) C34 0.035(2) 0.041(2) 0.036(2) -0.0210(19) 0.0001(17) -0.0103(18) F35 0.0509(14) 0.093(2) 0.0555(16) -0.0472(15) 0.0166(12) -0.0208(14) F36 0.0473(14) 0.0727(19) 0.091(2) -0.0481(16) 0.0079(13) -0.0297(13) F37 0.0325(12) 0.0620(17) 0.0783(18) -0.0159(15) -0.0180(12) 0.0091(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 Ag N24 2.167(2) 1_646 ? Ag N1 2.177(3) . ? Ag O10 2.563(2) 2_663 ? N1 C2 1.341(4) . ? N1 C6 1.345(4) . ? C2 C3 1.376(5) . ? C3 C4 1.383(5) . ? C4 C5 1.394(4) . ? C4 C7 1.507(4) . ? C5 C6 1.362(5) . ? C7 N8 1.462(4) . ? N8 C9 1.332(4) . ? C9 O10 1.243(4) . ? C9 C11 1.494(4) . ? O10 Ag 2.563(2) 2_663 ? C11 C16 1.380(5) . ? C11 C12 1.402(4) . ? C12 C13 1.387(4) . ? C13 C14 1.385(5) . ? C13 C17 1.503(4) . ? C14 C15 1.399(4) . ? C15 C16 1.386(5) . ? C15 C27 1.517(5) . ? C17 O18 1.236(4) . ? C17 N19 1.340(4) . ? N19 C20 1.462(4) . ? C20 C21 1.524(4) . ? C21 C22 1.377(4) . ? C21 C26 1.394(4) . ? C22 C23 1.375(4) . ? C23 N24 1.341(4) . ? N24 C25 1.356(4) . ? N24 Ag 2.167(2) 1_464 ? C25 C26 1.363(4) . ? C27 C28B 1.458(13) . ? C27 C28A 1.480(8) . ? C27 C30B 1.490(12) . ? C27 C30A 1.540(8) . ? C27 C29B 1.598(11) . ? C27 C29A 1.608(7) . ? C51 Cl53 1.664(11) . ? C51 Cl52 1.756(7) . ? O31 C33 1.224(4) . ? O32 C33 1.223(4) . ? C33 C34 1.540(5) . ? C34 F35 1.323(4) . ? C34 F37 1.324(4) . ? C34 F36 1.341(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 N24 Ag N1 170.65(11) 1_646 . ? N24 Ag O10 99.40(9) 1_646 2_663 ? N1 Ag O10 88.38(9) . 2_663 ? C2 N1 C6 116.6(3) . . ? C2 N1 Ag 123.0(2) . . ? C6 N1 Ag 120.4(2) . . ? N1 C2 C3 123.0(3) . . ? C2 C3 C4 120.2(3) . . ? C3 C4 C5 116.8(3) . . ? C3 C4 C7 122.8(3) . . ? C5 C4 C7 120.4(3) . . ? C6 C5 C4 119.6(3) . . ? N1 C6 C5 123.8(3) . . ? N8 C7 C4 110.9(3) . . ? C9 N8 C7 120.8(3) . . ? O10 C9 N8 121.6(3) . . ? O10 C9 C11 120.9(3) . . ? N8 C9 C11 117.5(3) . . ? C9 O10 Ag 138.4(2) . 2_663 ? C16 C11 C12 119.0(3) . . ? C16 C11 C9 120.3(3) . . ? C12 C11 C9 120.6(3) . . ? C13 C12 C11 119.5(3) . . ? C14 C13 C12 120.0(3) . . ? C14 C13 C17 119.2(3) . . ? C12 C13 C17 120.8(3) . . ? C13 C14 C15 121.6(3) . . ? C16 C15 C14 116.9(3) . . ? C16 C15 C27 121.7(3) . . ? C14 C15 C27 121.3(3) . . ? C11 C16 C15 122.9(3) . . ? O18 C17 N19 122.1(3) . . ? O18 C17 C13 121.3(3) . . ? N19 C17 C13 116.6(3) . . ? C17 N19 C20 121.4(3) . . ? N19 C20 C21 113.2(2) . . ? C22 C21 C26 117.4(3) . . ? C22 C21 C20 123.3(3) . . ? C26 C21 C20 119.3(3) . . ? C23 C22 C21 119.6(3) . . ? N24 C23 C22 123.5(3) . . ? C23 N24 C25 116.6(3) . . ? C23 N24 Ag 123.5(2) . 1_464 ? C25 N24 Ag 119.63(19) . 1_464 ? N24 C25 C26 122.9(3) . . ? C25 C26 C21 119.9(3) . . ? C28B C27 C28A 137.5(7) . . ? C28B C27 C30B 113.0(8) . . ? C28A C27 C30B 55.1(6) . . ? C28B C27 C15 109.9(6) . . ? C28A C27 C15 111.6(4) . . ? C30B C27 C15 115.2(5) . . ? C28B C27 C30A 42.5(7) . . ? C28A C27 C30A 109.9(5) . . ? C30B C27 C30A 131.0(6) . . ? C15 C27 C30A 113.5(4) . . ? C28B C27 C29B 106.2(9) . . ? C28A C27 C29B 52.0(6) . . ? C30B C27 C29B 104.2(8) . . ? C15 C27 C29B 107.6(5) . . ? C30A C27 C29B 64.8(6) . . ? C28B C27 C29A 67.2(8) . . ? C28A C27 C29A 107.3(6) . . ? C30B C27 C29A 53.4(5) . . ? C15 C27 C29A 108.3(4) . . ? C30A C27 C29A 106.0(5) . . ? C29B C27 C29A 143.5(6) . . ? Cl53 C51 Cl52 114.9(4) . . ? O32 C33 O31 128.8(3) . . ? O32 C33 C34 113.9(3) . . ? O31 C33 C34 117.3(4) . . ? F35 C34 F37 106.5(3) . . ? F35 C34 F36 106.7(3) . . ? F37 C34 F36 106.1(3) . . ? F35 C34 C33 114.8(3) . . ? F37 C34 C33 111.1(3) . . ? F36 C34 C33 111.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8A O32 0.88 2.07 2.943(3) 173.4 2_573 N19 H19A O32 0.88 2.14 3.012(4) 171.9 2_573 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.463 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.079 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 1.000 111.1 36.5 _platon_squeeze_details ; ? ; # Attachment '5.CIF' data_05005 _database_code_depnum_ccdc_archive 'CCDC 747043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Ag B F4 N8 O4' _chemical_formula_weight 887.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 22.4396(14) _cell_length_b 15.2304(10) _cell_length_c 15.9332(12) _cell_angle_alpha 90.00 _cell_angle_beta 134.747(3) _cell_angle_gamma 90.00 _cell_volume 3867.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3442 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9032 _exptl_absorpt_correction_T_max 0.9568 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; There are no XH bonds ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15922 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3408 _reflns_number_gt 2626 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0321P)^2^+9.6324P] 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 3408 _refine_ls_number_parameters 276 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.088 _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 Ag Ag 0.0000 -0.03823(3) 0.2500 0.04425(17) Uani 1 2 d S . . N1 N -0.01760(19) -0.1100(2) 0.3595(3) 0.0408(8) Uani 1 1 d . . . C2 C 0.0195(2) -0.1850(2) 0.4179(3) 0.0379(9) Uani 1 1 d . . . H2A H 0.0573 -0.2116 0.4167 0.046 Uiso 1 1 calc R . . C3 C 0.0052(2) -0.2258(3) 0.4803(4) 0.0418(9) Uani 1 1 d . . . C4 C -0.0530(3) -0.1893(3) 0.4760(5) 0.0660(14) Uani 1 1 d . . . H4A H -0.0655 -0.2164 0.5158 0.079 Uiso 1 1 calc R . . C5 C -0.0925(3) -0.1132(4) 0.4137(5) 0.0789(17) Uani 1 1 d . . . H5A H -0.1337 -0.0876 0.4085 0.095 Uiso 1 1 calc R . . C6 C -0.0722(3) -0.0744(3) 0.3591(4) 0.0601(13) Uani 1 1 d . . . H6A H -0.0979 -0.0201 0.3193 0.072 Uiso 1 1 calc R . . N7 N 0.0471(2) -0.3055(2) 0.5431(3) 0.0450(8) Uani 1 1 d . . . C8 C -0.0042(3) -0.3823(3) 0.5125(4) 0.0607(12) Uani 1 1 d . . . H8A H -0.0623 -0.3639 0.4646 0.091 Uiso 1 1 calc R . . H8B H 0.0178 -0.4107 0.5849 0.091 Uiso 1 1 calc R . . H8C H -0.0024 -0.4239 0.4673 0.091 Uiso 1 1 calc R . . C9 C 0.1319(3) -0.3161(3) 0.6269(4) 0.0431(10) Uani 1 1 d . . . O10 O 0.16437(19) -0.38842(18) 0.6705(3) 0.0565(8) Uani 1 1 d . . . C11 C 0.1856(2) -0.2369(2) 0.6656(3) 0.0396(9) Uani 1 1 d . . . C12 C 0.2354(2) -0.2346(3) 0.6434(3) 0.0406(9) Uani 1 1 d . . . H12A H 0.2364 -0.2837 0.6076 0.049 Uiso 1 1 calc R . . C13 C 0.2839(2) -0.1608(3) 0.6734(3) 0.0397(9) Uani 1 1 d . . . C14 C 0.2850(2) -0.0913(3) 0.7321(3) 0.0417(9) Uani 1 1 d . . . H14A H 0.3176 -0.0406 0.7529 0.050 Uiso 1 1 calc R . . C15 C 0.2391(2) -0.0958(3) 0.7601(4) 0.0460(10) Uani 1 1 d . . . H15A H 0.2429 -0.0498 0.8040 0.055 Uiso 1 1 calc R . . C16 C 0.1872(3) -0.1674(3) 0.7241(4) 0.0430(10) Uani 1 1 d . . . H16A H 0.1531 -0.1689 0.7392 0.052 Uiso 1 1 calc R . . C17 C 0.3352(2) -0.1611(3) 0.6458(3) 0.0430(10) Uani 1 1 d . . . O18 O 0.37171(18) -0.22792(19) 0.6588(3) 0.0566(8) Uani 1 1 d . . . N19 N 0.34243(18) -0.0835(2) 0.6101(3) 0.0420(8) Uani 1 1 d . . . C20 C 0.4003(2) -0.0768(3) 0.5966(4) 0.0520(11) Uani 1 1 d . . . H20A H 0.4412 -0.1247 0.6400 0.078 Uiso 1 1 calc R . . H20B H 0.4297 -0.0204 0.6280 0.078 Uiso 1 1 calc R . . H20C H 0.3687 -0.0809 0.5126 0.078 Uiso 1 1 calc R . . C21 C 0.2786(2) -0.0172(2) 0.5504(3) 0.0382(9) Uani 1 1 d . . . C22 C 0.1966(2) -0.0389(3) 0.4514(3) 0.0377(8) Uani 1 1 d . . . H22A H 0.1839 -0.0981 0.4249 0.045 Uiso 1 1 calc R . . N23 N 0.13378(18) 0.0198(2) 0.3907(3) 0.0374(7) Uani 1 1 d . . . C24 C 0.1535(2) 0.1030(3) 0.4281(3) 0.0402(9) Uani 1 1 d . . . H24A H 0.1099 0.1456 0.3856 0.048 Uiso 1 1 calc R . . C25 C 0.2343(3) 0.1298(3) 0.5258(4) 0.0465(10) Uani 1 1 d . . . H25A H 0.2456 0.1896 0.5495 0.056 Uiso 1 1 calc R . . C26 C 0.2982(3) 0.0692(3) 0.5884(4) 0.0447(10) Uani 1 1 d . . . H26A H 0.3543 0.0861 0.6560 0.054 Uiso 1 1 calc R . . B31 B 0.0150(9) 0.3047(6) 0.2743(10) 0.046(4) Uani 0.50 1 d PD A -1 F32 F 0.0027(18) 0.3895(3) 0.270(2) 0.075(6) Uani 0.50 1 d PD A -1 F33 F -0.0432(2) 0.2643(2) 0.2642(3) 0.1068(12) Uani 1 1 d D A -1 F34 F 0.0864(3) 0.3067(3) 0.3937(4) 0.0556(12) Uani 0.50 1 d PD A -1 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 Ag 0.0340(2) 0.0566(3) 0.0378(3) 0.000 0.0236(2) 0.000 N1 0.0433(19) 0.0423(19) 0.039(2) 0.0068(16) 0.0296(17) 0.0076(15) C2 0.039(2) 0.038(2) 0.035(2) -0.0012(18) 0.025(2) 0.0018(17) C3 0.045(2) 0.039(2) 0.041(2) 0.0037(19) 0.030(2) 0.0034(18) C4 0.078(3) 0.073(3) 0.075(4) 0.026(3) 0.064(3) 0.021(3) C5 0.084(4) 0.099(4) 0.092(4) 0.046(3) 0.075(4) 0.049(3) C6 0.067(3) 0.067(3) 0.066(3) 0.026(3) 0.054(3) 0.030(2) N7 0.052(2) 0.0360(19) 0.045(2) 0.0016(16) 0.0330(19) -0.0025(15) C8 0.071(3) 0.044(3) 0.064(3) -0.005(2) 0.047(3) -0.014(2) C9 0.056(3) 0.034(2) 0.039(2) 0.0021(19) 0.033(2) 0.0029(19) O10 0.072(2) 0.0379(17) 0.053(2) 0.0092(14) 0.0413(18) 0.0091(15) C11 0.044(2) 0.032(2) 0.033(2) 0.0043(17) 0.024(2) 0.0048(17) C12 0.045(2) 0.035(2) 0.034(2) 0.0015(18) 0.024(2) 0.0096(18) C13 0.036(2) 0.039(2) 0.032(2) 0.0010(18) 0.0197(19) 0.0068(17) C14 0.039(2) 0.035(2) 0.034(2) -0.0020(17) 0.019(2) 0.0019(17) C15 0.050(2) 0.043(2) 0.039(2) -0.0045(19) 0.029(2) 0.0036(19) C16 0.049(2) 0.041(2) 0.039(2) 0.0015(19) 0.031(2) 0.0064(19) C17 0.033(2) 0.047(3) 0.034(2) -0.0020(19) 0.019(2) 0.0050(18) O18 0.0555(18) 0.0509(19) 0.061(2) 0.0081(16) 0.0404(18) 0.0201(15) N19 0.0304(17) 0.043(2) 0.045(2) -0.0020(16) 0.0237(17) 0.0019(14) C20 0.039(2) 0.059(3) 0.057(3) -0.013(2) 0.033(2) -0.006(2) C21 0.034(2) 0.039(2) 0.038(2) -0.0008(17) 0.0240(19) -0.0012(16) C22 0.0341(19) 0.034(2) 0.037(2) -0.0049(18) 0.0223(19) -0.0024(18) N23 0.0329(16) 0.0367(19) 0.0347(18) 0.0010(14) 0.0210(15) 0.0019(14) C24 0.047(2) 0.033(2) 0.041(2) 0.0034(18) 0.031(2) 0.0059(18) C25 0.056(3) 0.032(2) 0.049(3) -0.0017(19) 0.036(2) -0.0046(19) C26 0.041(2) 0.042(2) 0.042(3) -0.0047(19) 0.026(2) -0.0076(18) B31 0.063(13) 0.042(5) 0.036(14) 0.003(4) 0.036(12) -0.005(5) F32 0.048(4) 0.044(2) 0.102(15) -0.031(6) 0.042(10) -0.015(6) F33 0.133(3) 0.116(3) 0.100(3) -0.046(2) 0.092(3) -0.076(2) F34 0.052(3) 0.063(3) 0.048(3) 0.002(3) 0.034(3) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N23 2.312(3) . ? Ag N23 2.312(3) 6_556 ? Ag N1 2.316(3) . ? Ag N1 2.316(3) 6_556 ? N1 C2 1.332(5) . ? N1 C6 1.334(5) . ? C2 C3 1.389(5) . ? C3 C4 1.377(6) . ? C3 N7 1.426(5) . ? C4 C5 1.369(6) . ? C5 C6 1.370(6) . ? N7 C9 1.362(5) . ? N7 C8 1.463(5) . ? C9 O10 1.230(4) . ? C9 C11 1.497(5) . ? C11 C12 1.389(5) . ? C11 C16 1.393(5) . ? C12 C13 1.394(5) . ? C13 C14 1.401(5) . ? C13 C17 1.496(5) . ? C14 C15 1.383(5) . ? C15 C16 1.391(5) . ? C17 O18 1.229(4) . ? C17 N19 1.369(5) . ? N19 C21 1.434(5) . ? N19 C20 1.462(5) . ? C21 C22 1.377(5) . ? C21 C26 1.384(5) . ? C22 N23 1.343(5) . ? N23 C24 1.336(5) . ? C24 C25 1.379(6) . ? C25 C26 1.375(5) . ? B31 F32 1.314(11) . ? B31 F33 1.348(17) . ? B31 F34 1.377(12) . ? 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 N23 Ag N23 135.04(15) . 6_556 ? N23 Ag N1 104.09(11) . . ? N23 Ag N1 96.74(10) 6_556 . ? N23 Ag N1 96.74(10) . 6_556 ? N23 Ag N1 104.09(11) 6_556 6_556 ? N1 Ag N1 123.69(16) . 6_556 ? C2 N1 C6 118.2(3) . . ? C2 N1 Ag 125.2(2) . . ? C6 N1 Ag 116.5(3) . . ? N1 C2 C3 122.5(3) . . ? C4 C3 C2 118.3(4) . . ? C4 C3 N7 120.8(4) . . ? C2 C3 N7 120.9(3) . . ? C5 C4 C3 119.1(4) . . ? C4 C5 C6 119.3(4) . . ? N1 C6 C5 122.5(4) . . ? C9 N7 C3 124.4(3) . . ? C9 N7 C8 117.4(3) . . ? C3 N7 C8 118.2(3) . . ? O10 C9 N7 121.6(4) . . ? O10 C9 C11 120.3(4) . . ? N7 C9 C11 118.2(3) . . ? C12 C11 C16 120.3(4) . . ? C12 C11 C9 118.3(3) . . ? C16 C11 C9 121.5(4) . . ? C11 C12 C13 120.4(3) . . ? C12 C13 C14 118.7(3) . . ? C12 C13 C17 118.3(3) . . ? C14 C13 C17 122.9(4) . . ? C15 C14 C13 120.7(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 C11 119.5(4) . . ? O18 C17 N19 121.8(4) . . ? O18 C17 C13 120.8(4) . . ? N19 C17 C13 117.4(3) . . ? C17 N19 C21 121.9(3) . . ? C17 N19 C20 119.8(3) . . ? C21 N19 C20 115.4(3) . . ? C22 C21 C26 119.1(4) . . ? C22 C21 N19 119.7(3) . . ? C26 C21 N19 121.2(3) . . ? N23 C22 C21 123.0(4) . . ? C24 N23 C22 117.4(3) . . ? C24 N23 Ag 126.2(2) . . ? C22 N23 Ag 115.6(2) . . ? N23 C24 C25 122.9(4) . . ? C26 C25 C24 119.4(4) . . ? C25 C26 C21 118.2(4) . . ? F32 B31 F33 106.7(16) . . ? F32 B31 F34 92.5(13) . . ? F33 B31 F34 105.2(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N23 Ag N1 C2 -72.7(3) . . . . ? N23 Ag N1 C2 147.5(3) 6_556 . . . ? N1 Ag N1 C2 35.6(3) 6_556 . . . ? N23 Ag N1 C6 110.3(3) . . . . ? N23 Ag N1 C6 -29.5(3) 6_556 . . . ? N1 Ag N1 C6 -141.5(3) 6_556 . . . ? C6 N1 C2 C3 -1.8(6) . . . . ? Ag N1 C2 C3 -178.7(3) . . . . ? N1 C2 C3 C4 3.5(6) . . . . ? N1 C2 C3 N7 -179.1(3) . . . . ? C2 C3 C4 C5 -1.9(7) . . . . ? N7 C3 C4 C5 -179.3(5) . . . . ? C3 C4 C5 C6 -1.2(9) . . . . ? C2 N1 C6 C5 -1.6(7) . . . . ? Ag N1 C6 C5 175.7(4) . . . . ? C4 C5 C6 N1 3.1(9) . . . . ? C4 C3 N7 C9 -127.3(5) . . . . ? C2 C3 N7 C9 55.3(6) . . . . ? C4 C3 N7 C8 55.4(6) . . . . ? C2 C3 N7 C8 -121.9(4) . . . . ? C3 N7 C9 O10 -173.1(4) . . . . ? C8 N7 C9 O10 4.2(6) . . . . ? C3 N7 C9 C11 6.9(6) . . . . ? C8 N7 C9 C11 -175.8(4) . . . . ? O10 C9 C11 C12 63.7(5) . . . . ? N7 C9 C11 C12 -116.3(4) . . . . ? O10 C9 C11 C16 -115.2(4) . . . . ? N7 C9 C11 C16 64.8(5) . . . . ? C16 C11 C12 C13 -3.6(6) . . . . ? C9 C11 C12 C13 177.4(4) . . . . ? C11 C12 C13 C14 3.5(6) . . . . ? C11 C12 C13 C17 -178.9(3) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C17 C13 C14 C15 -177.3(4) . . . . ? C13 C14 C15 C16 -3.8(6) . . . . ? C14 C15 C16 C11 3.7(6) . . . . ? C12 C11 C16 C15 0.0(6) . . . . ? C9 C11 C16 C15 178.9(4) . . . . ? C12 C13 C17 O18 -39.1(5) . . . . ? C14 C13 C17 O18 138.3(4) . . . . ? C12 C13 C17 N19 143.4(4) . . . . ? C14 C13 C17 N19 -39.2(5) . . . . ? O18 C17 N19 C21 154.6(4) . . . . ? C13 C17 N19 C21 -27.9(5) . . . . ? O18 C17 N19 C20 -5.3(6) . . . . ? C13 C17 N19 C20 172.2(3) . . . . ? C17 N19 C21 C22 -52.7(5) . . . . ? C20 N19 C21 C22 108.1(4) . . . . ? C17 N19 C21 C26 129.2(4) . . . . ? C20 N19 C21 C26 -70.0(5) . . . . ? C26 C21 C22 N23 -1.4(6) . . . . ? N19 C21 C22 N23 -179.6(3) . . . . ? C21 C22 N23 C24 1.6(5) . . . . ? C21 C22 N23 Ag -169.2(3) . . . . ? N23 Ag N23 C24 14.2(3) 6_556 . . . ? N1 Ag N23 C24 -100.8(3) . . . . ? N1 Ag N23 C24 132.0(3) 6_556 . . . ? N23 Ag N23 C22 -175.9(3) 6_556 . . . ? N1 Ag N23 C22 69.1(3) . . . . ? N1 Ag N23 C22 -58.2(3) 6_556 . . . ? C22 N23 C24 C25 -0.9(5) . . . . ? Ag N23 C24 C25 168.8(3) . . . . ? N23 C24 C25 C26 0.1(6) . . . . ? C24 C25 C26 C21 0.0(6) . . . . ? C22 C21 C26 C25 0.6(6) . . . . ? N19 C21 C26 C25 178.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.346 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.070 # Attachment '6.cif' data_05009 _database_code_depnum_ccdc_archive 'CCDC 747044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H60 Ag2 B2 Cl8 F8 N8 O4' _chemical_formula_weight 1534.04 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' B B 0.0013 0.0007 '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' 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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.0345(13) _cell_length_b 10.4349(6) _cell_length_c 20.4898(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.409(3) _cell_angle_gamma 90.00 _cell_volume 3305.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5552 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7732 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27162 _diffrn_reflns_av_R_equivalents 0.141 _diffrn_reflns_av_sigmaI/netI 0.1436 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5670 _reflns_number_gt 2382 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1948P)^2^+3.2998P] 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 SHELXL _refine_ls_extinction_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5670 _refine_ls_number_parameters 449 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.2298 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.3674 _refine_ls_wR_factor_gt 0.2917 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.189 _refine_ls_shift/su_mean 0.007 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 Ag Ag 0.49999(8) 0.75177(8) 0.12701(5) 0.0859(7) Uani 1 1 d . . . N11 N 0.4274(8) 0.6254(9) 0.1742(5) 0.075(3) Uani 1 1 d . . . C12 C 0.4352(10) 0.4975(12) 0.1698(6) 0.076(4) Uani 1 1 d . . . H12A H 0.4719 0.4651 0.1441 0.092 Uiso 1 1 calc R . . C13 C 0.3929(10) 0.4106(12) 0.2007(6) 0.079(4) Uani 1 1 d . . . H13A H 0.3998 0.3209 0.1964 0.095 Uiso 1 1 calc R . . C14 C 0.3413(10) 0.4589(12) 0.2372(6) 0.084(4) Uani 1 1 d . . . C15 C 0.3334(11) 0.5934(12) 0.2428(6) 0.085(4) Uani 1 1 d . . . H15A H 0.2988 0.6289 0.2694 0.102 Uiso 1 1 calc R . . C16 C 0.3748(9) 0.6676(13) 0.2105(6) 0.081(4) Uani 1 1 d . . . H16A H 0.3670 0.7576 0.2131 0.097 Uiso 1 1 calc R . . N17 N 0.2933(8) 0.3748(10) 0.2700(5) 0.086(3) Uani 1 1 d . . . C18 C 0.2876(15) 0.4157(15) 0.3393(7) 0.138(8) Uani 1 1 d . . . H18A H 0.2543 0.3521 0.3571 0.208 Uiso 1 1 calc R . . H18B H 0.2589 0.4992 0.3361 0.208 Uiso 1 1 calc R . . H18C H 0.3460 0.4222 0.3698 0.208 Uiso 1 1 calc R . . C19 C 0.2597(14) 0.2595(14) 0.2468(8) 0.109(6) Uani 1 1 d . . . O20 O 0.2361(9) 0.1837(9) 0.2861(5) 0.122(4) Uani 1 1 d . . . C21 C 0.2440(10) 0.2252(11) 0.1754(6) 0.077(4) Uani 1 1 d . . . C22 C 0.2613(10) 0.0989(11) 0.1582(5) 0.078(4) Uani 1 1 d . . . H22A H 0.2818 0.0374 0.1930 0.094 Uiso 1 1 calc R . . C23 C 0.2486(8) 0.0640(10) 0.0916(6) 0.065(3) Uani 1 1 d . . . C24 C 0.2114(7) 0.1500(11) 0.0389(5) 0.057(3) Uani 1 1 d . . . H24A H 0.1996 0.1241 -0.0071 0.068 Uiso 1 1 calc R . . C25 C 0.1923(8) 0.2754(10) 0.0561(6) 0.054(3) Uani 1 1 d . . . C26 C 0.2102(8) 0.3131(10) 0.1231(6) 0.064(3) Uani 1 1 d . . . H26A H 0.1995 0.3990 0.1339 0.077 Uiso 1 1 calc R . . C27 C 0.1567(9) 0.3688(13) -0.0013(6) 0.071(4) Uani 1 1 d . . . C28 C 0.0757(15) 0.314(2) -0.0446(10) 0.160(8) Uani 1 1 d . . . H28A H 0.0882 0.2315 -0.0630 0.240 Uiso 1 1 calc R . . H28B H 0.0508 0.3729 -0.0819 0.240 Uiso 1 1 calc R . . H28C H 0.0344 0.3006 -0.0176 0.240 Uiso 1 1 calc R . . C29 C 0.1324(12) 0.4988(13) 0.0269(8) 0.112(6) Uani 1 1 d . . . H29A H 0.0861 0.4845 0.0491 0.168 Uiso 1 1 calc R . . H29B H 0.1125 0.5595 -0.0105 0.168 Uiso 1 1 calc R . . H29C H 0.1833 0.5339 0.0597 0.168 Uiso 1 1 calc R . . C30 C 0.2318(14) 0.4058(17) -0.0334(9) 0.139(7) Uani 1 1 d . . . H30A H 0.2512 0.3293 -0.0530 0.208 Uiso 1 1 calc R . . H30B H 0.2802 0.4415 0.0016 0.208 Uiso 1 1 calc R . . H30C H 0.2110 0.4699 -0.0690 0.208 Uiso 1 1 calc R . . C31 C 0.2569(10) -0.0783(12) 0.0777(7) 0.084(4) Uani 1 1 d . . . O32 O 0.2320(8) -0.1591(8) 0.1081(5) 0.104(4) Uani 1 1 d . . . N33 N 0.2975(8) -0.1116(10) 0.0286(6) 0.088(3) Uani 1 1 d . . . C34 C 0.2909(14) -0.2491(12) 0.0079(9) 0.119(7) Uani 1 1 d . . . H34A H 0.3197 -0.2619 -0.0282 0.178 Uiso 1 1 calc R . . H34B H 0.2299 -0.2731 -0.0086 0.178 Uiso 1 1 calc R . . H34C H 0.3189 -0.3025 0.0469 0.178 Uiso 1 1 calc R . . C35 C 0.3394(9) -0.0259(11) -0.0062(6) 0.069(4) Uani 1 1 d . . . C36 C 0.3323(12) -0.0346(14) -0.0749(8) 0.104(5) Uani 1 1 d . . . H36A H 0.2930 -0.0954 -0.1007 0.125 Uiso 1 1 calc R . . C37 C 0.3776(10) 0.0378(14) -0.1063(7) 0.085(4) Uani 1 1 d . . . H37A H 0.3724 0.0224 -0.1529 0.102 Uiso 1 1 calc R . . N38 N 0.4284(8) 0.1283(10) -0.0762(5) 0.080(3) Uani 1 1 d . . . C39 C 0.4369(9) 0.1421(11) -0.0109(7) 0.076(4) Uani 1 1 d . . . H39A H 0.4749 0.2069 0.0124 0.091 Uiso 1 1 calc R . . C40 C 0.3942(8) 0.0685(10) 0.0260(6) 0.062(3) Uani 1 1 d . . . H40A H 0.4027 0.0833 0.0730 0.075 Uiso 1 1 calc R . . B50 B 0.4941(15) 0.491(2) -0.0058(12) 0.096(11) Uani 0.50 1 d PD A -1 F51 F 0.4415(11) 0.4331(11) -0.0643(7) 0.083(5) Uani 0.50 1 d PD A -1 F52 F 0.4424(14) 0.5844(14) 0.0139(9) 0.113(7) Uani 0.50 1 d PD A -1 F53 F 0.5678(15) 0.5492(18) -0.0177(10) 0.112(7) Uani 0.50 1 d PD A -1 F54 F 0.5192(15) 0.4056(14) 0.0490(9) 0.101(5) Uani 0.50 1 d PD A -1 B60 B 0.5000 -0.0404(16) -0.2500 0.083(8) Uani 1 2 d SD . . F61 F 0.4392(14) 0.0239(18) -0.2989(9) 0.110(8) Uani 0.50 1 d PD . . F62 F 0.5478(17) -0.119(2) -0.2798(14) 0.117(10) Uani 0.50 1 d PD . . F63 F 0.501(2) -0.121(3) -0.1974(12) 0.148(15) Uani 0.50 1 d PD . . F64 F 0.5634(15) 0.0498(17) -0.2480(16) 0.132(8) Uani 0.50 1 d PD . . C70 C 0.073(6) -0.211(6) -0.138(4) 0.38(8) Uani 0.50 1 d PD B 1 H70A H 0.0608 -0.1572 -0.1797 0.460 Uiso 0.50 1 calc PR B 1 H70B H 0.1341 -0.2393 -0.1315 0.460 Uiso 0.50 1 calc PR B 1 Cl71 Cl 0.0175(8) -0.3417(11) -0.1638(6) 0.154(4) Uani 0.50 1 d PD B 1 Cl72 Cl 0.0810(18) -0.104(2) -0.0772(9) 0.269(11) Uani 0.50 1 d PD B 1 C73 C -0.0095(18) -0.058(6) -0.0912(17) 0.23(4) Uani 0.50 1 d PD C 2 H73A H -0.0418 -0.1358 -0.1114 0.282 Uiso 0.50 1 calc PR C 2 H73B H -0.0524 0.0089 -0.0891 0.282 Uiso 0.50 1 calc PR C 2 Cl74 Cl 0.0497(16) -0.093(3) -0.0112(11) 0.341(17) Uani 0.50 1 d PD C 2 Cl75 Cl 0.0498(9) -0.0084(14) -0.1408(8) 0.183(6) Uani 0.50 1 d PD C 2 C80 C 0.1048(16) 0.2450(19) -0.2963(9) 0.209(15) Uani 1 1 d D . . H80A H 0.1302 0.2328 -0.3349 0.251 Uiso 1 1 calc R . . H80B H 0.0462 0.2065 -0.3086 0.251 Uiso 1 1 calc R . . Cl81 Cl 0.1678(6) 0.1681(10) -0.2263(5) 0.235(4) Uani 1 1 d D . . Cl82 Cl 0.0970(5) 0.4008(12) -0.2820(4) 0.250(5) Uani 1 1 d 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 Ag 0.1255(13) 0.0801(8) 0.0598(8) 0.0046(5) 0.0381(7) 0.0151(6) N11 0.118(9) 0.062(6) 0.045(6) -0.003(5) 0.021(6) 0.015(6) C12 0.119(13) 0.071(8) 0.041(7) 0.002(6) 0.023(8) 0.017(7) C13 0.131(13) 0.072(8) 0.031(7) -0.004(6) 0.017(8) 0.016(8) C14 0.124(13) 0.075(9) 0.051(8) 0.015(7) 0.022(9) 0.008(8) C15 0.138(14) 0.078(9) 0.043(7) -0.012(6) 0.031(9) 0.006(8) C16 0.108(12) 0.083(9) 0.062(9) 0.008(7) 0.041(9) 0.027(8) N17 0.150(11) 0.083(7) 0.034(6) -0.006(5) 0.042(7) -0.003(7) C18 0.26(2) 0.123(12) 0.046(9) 0.003(8) 0.066(13) -0.061(13) C19 0.192(19) 0.088(10) 0.055(9) -0.002(8) 0.048(11) 0.039(10) O20 0.243(14) 0.092(6) 0.050(6) 0.010(5) 0.074(8) -0.017(7) C21 0.127(13) 0.075(8) 0.038(7) 0.006(6) 0.035(8) -0.002(7) C22 0.142(13) 0.071(7) 0.028(6) 0.005(5) 0.033(8) 0.001(7) C23 0.085(10) 0.066(7) 0.050(7) 0.010(6) 0.027(7) 0.002(6) C24 0.053(8) 0.078(8) 0.038(6) 0.016(6) 0.011(6) -0.012(6) C25 0.060(8) 0.057(7) 0.044(7) 0.014(5) 0.010(6) -0.001(5) C26 0.099(10) 0.053(6) 0.049(7) 0.008(5) 0.036(7) 0.006(6) C27 0.073(10) 0.100(9) 0.031(7) 0.014(6) -0.002(7) 0.002(7) C28 0.16(2) 0.146(16) 0.112(15) 0.041(13) -0.069(15) 0.001(15) C29 0.158(17) 0.072(9) 0.087(11) 0.026(8) -0.002(11) 0.009(9) C30 0.19(2) 0.140(14) 0.122(15) 0.022(12) 0.102(16) -0.006(13) C31 0.131(13) 0.069(8) 0.059(8) -0.009(7) 0.039(9) 0.004(8) O32 0.188(11) 0.071(6) 0.065(6) 0.021(5) 0.054(7) 0.011(6) N33 0.114(10) 0.076(7) 0.077(8) -0.027(6) 0.029(7) -0.013(6) C34 0.175(18) 0.092(11) 0.099(12) -0.050(9) 0.055(13) -0.058(10) C35 0.097(11) 0.058(7) 0.058(8) -0.011(6) 0.031(8) -0.003(7) C36 0.150(16) 0.098(10) 0.079(11) -0.030(9) 0.056(11) -0.026(10) C37 0.114(13) 0.092(10) 0.053(8) -0.022(8) 0.029(9) 0.014(9) N38 0.108(10) 0.080(7) 0.051(7) -0.015(6) 0.022(7) 0.011(7) C39 0.094(11) 0.056(7) 0.081(10) -0.020(7) 0.029(9) 0.013(6) C40 0.088(10) 0.058(7) 0.053(7) 0.001(6) 0.039(7) 0.009(7) B50 0.18(4) 0.060(17) 0.040(17) 0.008(13) 0.02(2) 0.01(2) F51 0.158(16) 0.050(7) 0.051(9) -0.014(6) 0.046(10) 0.006(8) F52 0.19(2) 0.074(10) 0.107(14) -0.025(9) 0.102(15) 0.001(11) F53 0.16(2) 0.097(13) 0.114(15) -0.001(10) 0.108(16) -0.004(13) F54 0.143(18) 0.082(10) 0.089(13) -0.025(9) 0.048(13) -0.003(10) B60 0.16(3) 0.044(12) 0.052(15) 0.000 0.036(19) 0.000 F61 0.16(2) 0.068(11) 0.089(14) -0.031(11) -0.001(14) 0.010(11) F62 0.15(3) 0.082(13) 0.11(2) -0.027(12) 0.013(18) -0.010(14) F63 0.19(3) 0.20(3) 0.065(15) 0.078(16) 0.06(2) 0.11(2) F64 0.16(2) 0.067(12) 0.17(2) -0.006(13) 0.04(2) -0.023(12) C70 0.7(2) 0.27(7) 0.28(9) -0.19(7) 0.34(12) -0.26(10) Cl71 0.183(11) 0.148(9) 0.150(9) 0.062(7) 0.079(9) 0.050(8) Cl72 0.36(3) 0.33(2) 0.107(11) -0.025(14) 0.042(15) -0.10(2) C73 0.05(2) 0.52(10) 0.13(4) 0.18(5) 0.02(2) -0.04(4) Cl74 0.32(3) 0.49(4) 0.193(19) -0.06(3) 0.03(2) -0.23(3) Cl75 0.192(13) 0.207(12) 0.175(13) -0.044(11) 0.090(12) -0.038(10) C80 0.20(3) 0.36(4) 0.066(13) -0.037(18) 0.023(15) 0.13(3) Cl81 0.246(9) 0.286(9) 0.206(8) 0.056(7) 0.115(8) -0.040(8) Cl82 0.164(7) 0.412(14) 0.180(8) -0.049(8) 0.053(6) 0.071(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 Ag N38 2.146(11) 3_665 ? Ag N11 2.151(10) . ? N11 C16 1.340(14) . ? N11 C12 1.346(15) . ? C12 C13 1.383(17) . ? C12 H12A 0.9500 . ? C13 C14 1.351(17) . ? C13 H13A 0.9500 . ? C14 C15 1.417(16) . ? C14 N17 1.446(15) . ? C15 C16 1.307(17) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N17 C19 1.351(18) . ? N17 C18 1.508(15) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O20 1.256(17) . ? C19 C21 1.463(18) . ? C21 C26 1.404(16) . ? C21 C22 1.411(15) . ? C22 C23 1.375(15) . ? C22 H22A 0.9500 . ? C23 C24 1.409(15) . ? C23 C31 1.524(15) . ? C24 C25 1.410(15) . ? C24 H24A 0.9500 . ? C25 C26 1.385(15) . ? C25 C27 1.517(15) . ? C26 H26A 0.9500 . ? C27 C28 1.48(2) . ? C27 C29 1.564(18) . ? C27 C30 1.565(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O32 1.179(13) . ? C31 N33 1.382(14) . ? N33 C35 1.419(15) . ? N33 C34 1.492(14) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.367(17) . ? C35 C36 1.383(17) . ? C36 C37 1.328(18) . ? C36 H36A 0.9500 . ? C37 N38 1.292(17) . ? C37 H37A 0.9500 . ? N38 C39 1.316(15) . ? N38 Ag 2.146(11) 3_665 ? C39 C40 1.380(15) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? B50 F52 1.41(2) . ? B50 F53 1.406(19) . ? B50 F51 1.406(19) . ? B50 F54 1.407(19) . ? B60 F63 1.365(17) 2_654 ? B60 F63 1.365(17) . ? B60 F62 1.369(17) . ? B60 F62 1.369(17) 2_654 ? B60 F61 1.374(16) 2_654 ? B60 F61 1.374(16) . ? B60 F64 1.378(16) . ? B60 F64 1.378(16) 2_654 ? F61 F64 1.01(2) 2_654 ? F62 F63 0.80(4) 2_654 ? F63 F62 0.80(4) 2_654 ? F64 F61 1.01(2) 2_654 ? C70 Cl71 1.643(19) . ? C70 Cl72 1.655(19) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C73 Cl75 1.649(17) . ? C73 Cl74 1.701(19) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C80 Cl82 1.662(16) . ? C80 Cl81 1.717(16) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? 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 N38 Ag N11 177.4(4) 3_665 . ? C16 N11 C12 116.5(11) . . ? C16 N11 Ag 123.0(8) . . ? C12 N11 Ag 120.4(8) . . ? N11 C12 C13 123.7(11) . . ? N11 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C14 C13 C12 117.1(11) . . ? C14 C13 H13A 121.4 . . ? C12 C13 H13A 121.4 . . ? C13 C14 C15 119.7(12) . . ? C13 C14 N17 120.7(12) . . ? C15 C14 N17 119.6(12) . . ? C16 C15 C14 118.5(12) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? C15 C16 N11 124.4(12) . . ? C15 C16 H16A 117.8 . . ? N11 C16 H16A 117.8 . . ? C19 N17 C14 126.1(10) . . ? C19 N17 C18 117.7(11) . . ? C14 N17 C18 116.0(11) . . ? N17 C18 H18A 109.5 . . ? N17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O20 C19 N17 119.7(12) . . ? O20 C19 C21 119.1(15) . . ? N17 C19 C21 121.1(13) . . ? C26 C21 C22 118.8(10) . . ? C26 C21 C19 122.1(11) . . ? C22 C21 C19 119.0(11) . . ? C23 C22 C21 120.5(11) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 120.9(10) . . ? C22 C23 C31 116.5(10) . . ? C24 C23 C31 121.2(11) . . ? C23 C24 C25 118.4(10) . . ? C23 C24 H24A 120.8 . . ? C25 C24 H24A 120.8 . . ? C26 C25 C24 120.7(10) . . ? C26 C25 C27 121.5(10) . . ? C24 C25 C27 117.7(10) . . ? C25 C26 C21 120.4(10) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C28 C27 C25 107.7(12) . . ? C28 C27 C29 107.0(14) . . ? C25 C27 C29 110.5(10) . . ? C28 C27 C30 119.6(15) . . ? C25 C27 C30 108.2(12) . . ? C29 C27 C30 103.7(12) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O32 C31 N33 119.8(11) . . ? O32 C31 C23 122.6(11) . . ? N33 C31 C23 117.5(11) . . ? C31 N33 C35 125.9(10) . . ? C31 N33 C34 115.9(11) . . ? C35 N33 C34 118.1(11) . . ? N33 C34 H34A 109.5 . . ? N33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 114.0(11) . . ? C40 C35 N33 122.7(11) . . ? C36 C35 N33 123.1(12) . . ? C37 C36 C35 123.2(14) . . ? C37 C36 H36A 118.4 . . ? C35 C36 H36A 118.4 . . ? N38 C37 C36 122.7(12) . . ? N38 C37 H37A 118.6 . . ? C36 C37 H37A 118.6 . . ? C37 N38 C39 116.6(11) . . ? C37 N38 Ag 123.0(9) . 3_665 ? C39 N38 Ag 120.3(10) . 3_665 ? N38 C39 C40 124.3(13) . . ? N38 C39 H39A 117.9 . . ? C40 C39 H39A 117.9 . . ? C35 C40 C39 119.0(11) . . ? C35 C40 H40A 120.5 . . ? C39 C40 H40A 120.5 . . ? F52 B50 F53 109.8(19) . . ? F52 B50 F51 106.2(16) . . ? F53 B50 F51 112(2) . . ? F52 B50 F54 106(2) . . ? F53 B50 F54 109.6(17) . . ? F51 B50 F54 112.8(19) . . ? F63 B60 F63 104(3) 2_654 . ? F63 B60 F62 34.0(16) 2_654 . ? F63 B60 F62 95.3(14) . . ? F63 B60 F62 95.3(14) 2_654 2_654 ? F63 B60 F62 34.0(16) . 2_654 ? F62 B60 F62 107(3) . 2_654 ? F63 B60 F61 137.4(17) 2_654 2_654 ? F63 B60 F61 82.4(18) . 2_654 ? F62 B60 F61 104.1(15) . 2_654 ? F62 B60 F61 109.8(15) 2_654 2_654 ? F63 B60 F61 82.4(18) 2_654 . ? F63 B60 F61 137.4(17) . . ? F62 B60 F61 109.8(15) . . ? F62 B60 F61 104.1(15) 2_654 . ? F61 B60 F61 121(2) 2_654 . ? F63 B60 F64 107.5(16) 2_654 . ? F63 B60 F64 123(2) . . ? F62 B60 F64 85.7(15) . . ? F62 B60 F64 152.9(18) 2_654 . ? F61 B60 F64 43.1(11) 2_654 . ? F61 B60 F64 93.6(15) . . ? F63 B60 F64 123(2) 2_654 2_654 ? F63 B60 F64 107.5(16) . 2_654 ? F62 B60 F64 152.9(18) . 2_654 ? F62 B60 F64 85.7(15) 2_654 2_654 ? F61 B60 F64 93.6(15) 2_654 2_654 ? F61 B60 F64 43.1(11) . 2_654 ? F64 B60 F64 94(2) . 2_654 ? F64 F61 B60 68.7(14) 2_654 . ? F63 F62 B60 73(2) 2_654 . ? F62 F63 B60 73.3(17) 2_654 . ? F61 F64 B60 68.2(13) 2_654 . ? Cl71 C70 Cl72 136(3) . . ? Cl71 C70 H70A 103.0 . . ? Cl72 C70 H70A 102.9 . . ? Cl71 C70 H70B 103.1 . . ? Cl72 C70 H70B 103.2 . . ? H70A C70 H70B 105.1 . . ? Cl75 C73 Cl74 113.3(19) . . ? Cl75 C73 H73A 109.0 . . ? Cl74 C73 H73A 109.0 . . ? Cl75 C73 H73B 108.9 . . ? Cl74 C73 H73B 108.9 . . ? H73A C73 H73B 107.7 . . ? Cl82 C80 Cl81 111.5(12) . . ? Cl82 C80 H80A 109.3 . . ? Cl81 C80 H80A 109.3 . . ? Cl82 C80 H80B 109.3 . . ? Cl81 C80 H80B 109.3 . . ? H80A C80 H80B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N38 Ag N11 C16 -145(9) 3_665 . . . ? N38 Ag N11 C12 37(10) 3_665 . . . ? C16 N11 C12 C13 0(2) . . . . ? Ag N11 C12 C13 177.7(10) . . . . ? N11 C12 C13 C14 0(2) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C12 C13 C14 N17 178.7(13) . . . . ? C13 C14 C15 C16 2(2) . . . . ? N17 C14 C15 C16 -177.3(13) . . . . ? C14 C15 C16 N11 -3(2) . . . . ? C12 N11 C16 C15 2(2) . . . . ? Ag N11 C16 C15 -176.2(12) . . . . ? C13 C14 N17 C19 -33(2) . . . . ? C15 C14 N17 C19 146.1(16) . . . . ? C13 C14 N17 C18 141.1(15) . . . . ? C15 C14 N17 C18 -40(2) . . . . ? C14 N17 C19 O20 164.5(15) . . . . ? C18 N17 C19 O20 -10(3) . . . . ? C14 N17 C19 C21 -20(3) . . . . ? C18 N17 C19 C21 165.6(16) . . . . ? O20 C19 C21 C26 134.5(16) . . . . ? N17 C19 C21 C26 -41(3) . . . . ? O20 C19 C21 C22 -44(2) . . . . ? N17 C19 C21 C22 141.1(16) . . . . ? C26 C21 C22 C23 3(2) . . . . ? C19 C21 C22 C23 -178.9(15) . . . . ? C21 C22 C23 C24 -5(2) . . . . ? C21 C22 C23 C31 -171.7(13) . . . . ? C22 C23 C24 C25 3.7(17) . . . . ? C31 C23 C24 C25 169.5(11) . . . . ? C23 C24 C25 C26 0.4(16) . . . . ? C23 C24 C25 C27 176.8(11) . . . . ? C24 C25 C26 C21 -3.0(18) . . . . ? C27 C25 C26 C21 -179.2(12) . . . . ? C22 C21 C26 C25 1.4(19) . . . . ? C19 C21 C26 C25 -176.9(15) . . . . ? C26 C25 C27 C28 -124.8(15) . . . . ? C24 C25 C27 C28 58.9(17) . . . . ? C26 C25 C27 C29 -8.2(17) . . . . ? C24 C25 C27 C29 175.4(11) . . . . ? C26 C25 C27 C30 104.6(14) . . . . ? C24 C25 C27 C30 -71.8(15) . . . . ? C22 C23 C31 O32 38(2) . . . . ? C24 C23 C31 O32 -128.5(15) . . . . ? C22 C23 C31 N33 -140.2(14) . . . . ? C24 C23 C31 N33 53.4(18) . . . . ? O32 C31 N33 C35 -172.2(14) . . . . ? C23 C31 N33 C35 6(2) . . . . ? O32 C31 N33 C34 12(2) . . . . ? C23 C31 N33 C34 -169.7(14) . . . . ? C31 N33 C35 C40 45(2) . . . . ? C34 N33 C35 C40 -139.5(15) . . . . ? C31 N33 C35 C36 -138.6(15) . . . . ? C34 N33 C35 C36 37(2) . . . . ? C40 C35 C36 C37 3(2) . . . . ? N33 C35 C36 C37 -173.6(14) . . . . ? C35 C36 C37 N38 -4(2) . . . . ? C36 C37 N38 C39 3(2) . . . . ? C36 C37 N38 Ag -178.8(12) . . . 3_665 ? C37 N38 C39 C40 -1.3(19) . . . . ? Ag N38 C39 C40 -179.3(9) 3_665 . . . ? C36 C35 C40 C39 -1.2(18) . . . . ? N33 C35 C40 C39 175.6(11) . . . . ? N38 C39 C40 C35 0.4(19) . . . . ? F63 B60 F61 F64 161(2) 2_654 . . 2_654 ? F63 B60 F61 F64 59(3) . . . 2_654 ? F62 B60 F61 F64 -178(2) . . . 2_654 ? F62 B60 F61 F64 68(2) 2_654 . . 2_654 ? F61 B60 F61 F64 -56.8(17) 2_654 . . 2_654 ? F64 B60 F61 F64 -92(3) . . . 2_654 ? F63 B60 F62 F63 107(5) . . . 2_654 ? F62 B60 F62 F63 74(4) 2_654 . . 2_654 ? F61 B60 F62 F63 -170(4) 2_654 . . 2_654 ? F61 B60 F62 F63 -38(4) . . . 2_654 ? F64 B60 F62 F63 -131(4) . . . 2_654 ? F64 B60 F62 F63 -41(6) 2_654 . . 2_654 ? F63 B60 F63 F62 -79(4) 2_654 . . 2_654 ? F62 B60 F63 F62 -112(4) . . . 2_654 ? F61 B60 F63 F62 144(4) 2_654 . . 2_654 ? F61 B60 F63 F62 15(5) . . . 2_654 ? F64 B60 F63 F62 159(3) . . . 2_654 ? F64 B60 F63 F62 53(4) 2_654 . . 2_654 ? F63 B60 F64 F61 -143(3) 2_654 . . 2_654 ? F63 B60 F64 F61 -22(3) . . . 2_654 ? F62 B60 F64 F61 -116(2) . . . 2_654 ? F62 B60 F64 F61 3(5) 2_654 . . 2_654 ? F61 B60 F64 F61 134(2) . . . 2_654 ? F64 B60 F64 F61 91(2) 2_654 . . 2_654 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.842 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.130 # Attachment '7.CIF' data_05003 _database_code_depnum_ccdc_archive 'CCDC 747045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Ag N5 O5' _chemical_formula_weight 572.37 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' 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.4077(6) _cell_length_b 9.8095(4) _cell_length_c 14.9862(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.438(2) _cell_angle_gamma 90.00 _cell_volume 2407.71(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2868 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7777 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12318 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4226 _reflns_number_gt 3752 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0348P)^2^+2.9515P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 4226 _refine_ls_number_parameters 317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.192 _refine_ls_shift/su_mean 0.002 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 Ag Ag 0.262114(17) 1.16285(4) 0.953970(18) 0.03211(10) Uani 1 1 d . . . N11 N 0.16634(18) 1.1667(6) 0.84561(18) 0.0278(7) Uani 1 1 d . . . C12 C 0.1777(3) 1.2315(5) 0.7683(3) 0.0279(10) Uani 1 1 d . . . H12A H 0.2272 1.2802 0.7625 0.033 Uiso 1 1 calc R . . C13 C 0.1209(3) 1.2299(5) 0.6976(3) 0.0265(10) Uani 1 1 d . . . H13A H 0.1315 1.2759 0.6438 0.032 Uiso 1 1 calc R . . C14 C 0.0474(2) 1.1610(8) 0.7048(2) 0.0221(7) Uani 1 1 d . . . C15 C 0.0344(3) 1.0968(5) 0.7855(3) 0.0256(10) Uani 1 1 d . . . H15A H -0.0154 1.0503 0.7938 0.031 Uiso 1 1 calc R . . C16 C 0.0949(3) 1.1019(5) 0.8529(3) 0.0286(10) Uani 1 1 d . . . H16A H 0.0857 1.0573 0.9076 0.034 Uiso 1 1 calc R . . N17 N -0.01385(16) 1.1656(6) 0.63333(17) 0.0227(6) Uani 1 1 d . . . C18 C -0.0422(3) 1.3033(6) 0.6038(4) 0.0320(14) Uani 1 1 d . . . H18A H -0.0838 1.2943 0.5545 0.048 Uiso 1 1 calc R . . H18B H 0.0042 1.3557 0.5836 0.048 Uiso 1 1 calc R . . H18C H -0.0655 1.3508 0.6539 0.048 Uiso 1 1 calc R . . C19 C -0.0585(3) 1.0544(6) 0.6047(3) 0.0208(12) Uani 1 1 d . . . O20 O -0.12125(18) 1.0708(3) 0.5568(2) 0.0327(7) Uani 1 1 d . . . C21 C -0.0264(2) 0.9171(4) 0.6283(2) 0.0211(9) Uani 1 1 d . . . C22 C -0.0814(2) 0.8248(5) 0.6620(3) 0.0235(9) Uani 1 1 d . . . H22A H -0.1367 0.8499 0.6681 0.028 Uiso 1 1 calc R . . C23 C -0.0537(2) 0.6954(4) 0.6866(2) 0.0218(12) Uani 1 1 d . . . C24 C 0.02595(19) 0.6572(8) 0.6708(2) 0.0211(8) Uani 1 1 d . . . H24A H 0.0438 0.5677 0.6863 0.025 Uiso 1 1 calc R . . C25 C 0.0805(2) 0.7474(4) 0.6327(3) 0.0214(9) Uani 1 1 d . . . C26 C 0.0526(2) 0.8774(4) 0.6143(3) 0.0207(9) Uani 1 1 d . . . H26A H 0.0890 0.9421 0.5912 0.025 Uiso 1 1 calc R . . C27 C 0.1660(2) 0.6965(4) 0.6149(3) 0.0218(11) Uani 1 1 d . . . C28 C 0.2173(3) 0.8093(5) 0.5756(3) 0.0314(11) Uani 1 1 d . . . H28A H 0.1907 0.8405 0.5189 0.047 Uiso 1 1 calc R . . H28B H 0.2717 0.7738 0.5650 0.047 Uiso 1 1 calc R . . H28C H 0.2223 0.8858 0.6176 0.047 Uiso 1 1 calc R . . C29 C 0.1603(3) 0.5780(5) 0.5484(3) 0.0314(11) Uani 1 1 d . . . H29A H 0.1335 0.6091 0.4919 0.047 Uiso 1 1 calc R . . H29B H 0.1285 0.5038 0.5729 0.047 Uiso 1 1 calc R . . H29C H 0.2154 0.5453 0.5379 0.047 Uiso 1 1 calc R . . C30 C 0.2087(2) 0.6476(8) 0.7030(3) 0.0353(13) Uani 1 1 d . . . H30A H 0.2638 0.6157 0.6919 0.053 Uiso 1 1 calc R . . H30B H 0.1774 0.5727 0.7274 0.053 Uiso 1 1 calc R . . H30C H 0.2123 0.7232 0.7458 0.053 Uiso 1 1 calc R . . C31 C -0.1118(3) 0.5992(5) 0.7269(3) 0.0246(10) Uani 1 1 d . . . O32 O -0.18133(17) 0.5840(3) 0.6953(2) 0.0321(7) Uani 1 1 d . . . N33 N -0.0825(2) 0.5206(4) 0.7988(2) 0.0252(8) Uani 1 1 d . . . C34 C -0.1345(3) 0.4057(6) 0.8259(4) 0.0301(12) Uani 1 1 d . . . H34A H -0.1809 0.3951 0.7821 0.045 Uiso 1 1 calc R . . H34B H -0.1547 0.4246 0.8849 0.045 Uiso 1 1 calc R . . H34C H -0.1023 0.3215 0.8286 0.045 Uiso 1 1 calc R . . C35 C -0.0116(3) 0.5530(5) 0.8524(3) 0.0238(9) Uani 1 1 d . . . C36 C 0.0078(3) 0.6875(5) 0.8758(3) 0.0258(12) Uani 1 1 d . . . H36A H -0.0275 0.7602 0.8570 0.031 Uiso 1 1 calc R . . C37 C 0.0794(3) 0.7131(5) 0.9270(3) 0.0289(11) Uani 1 1 d . . . H37A H 0.0924 0.8050 0.9418 0.035 Uiso 1 1 calc R . . N38 N 0.1313(2) 0.6153(4) 0.9569(2) 0.0280(9) Uani 1 1 d . . . C39 C 0.1108(3) 0.4876(5) 0.9344(3) 0.0283(10) Uani 1 1 d . . . H39A H 0.1470 0.4168 0.9545 0.034 Uiso 1 1 calc R . . C40 C 0.0414(3) 0.4507(5) 0.8842(3) 0.0297(11) Uani 1 1 d . . . H40A H 0.0299 0.3576 0.8715 0.036 Uiso 1 1 calc R . . N41 N 0.3384(3) 1.4780(4) 0.9128(3) 0.0358(10) Uani 1 1 d . . . O42 O 0.29994(19) 1.4270(3) 0.9754(2) 0.0350(8) Uani 1 1 d . . . O43 O 0.3531(3) 1.4082(5) 0.8459(3) 0.0580(14) Uani 1 1 d . . . O44 O 0.3599(3) 1.5994(4) 0.9192(3) 0.0668(12) 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 Ag 0.02943(16) 0.03281(18) 0.03271(16) -0.0005(2) -0.00971(11) 0.0021(2) N11 0.0293(17) 0.0242(18) 0.0287(16) 0.001(3) -0.0079(12) 0.010(3) C12 0.025(2) 0.029(3) 0.030(2) 0.0023(19) -0.0037(19) 0.0000(19) C13 0.027(2) 0.029(2) 0.024(2) 0.0054(18) 0.0029(18) 0.0009(19) C14 0.0248(18) 0.0198(19) 0.0213(16) -0.003(3) -0.0017(13) 0.003(3) C15 0.027(2) 0.023(2) 0.027(2) 0.0006(18) -0.0029(18) -0.0033(19) C16 0.035(3) 0.024(2) 0.026(2) 0.0001(18) -0.0042(19) -0.001(2) N17 0.0241(15) 0.0168(16) 0.0265(14) 0.000(3) -0.0036(12) 0.001(3) C18 0.032(3) 0.025(3) 0.039(3) 0.008(2) 0.002(2) 0.007(3) C19 0.021(3) 0.023(3) 0.018(2) -0.0036(19) -0.0015(19) 0.005(2) O20 0.0299(17) 0.0233(18) 0.0428(18) -0.0063(14) -0.0144(14) 0.0049(14) C21 0.021(2) 0.016(2) 0.026(2) -0.0020(18) -0.0057(17) 0.0056(18) C22 0.016(2) 0.031(3) 0.023(2) -0.0058(19) -0.0001(17) 0.0014(19) C23 0.025(2) 0.021(4) 0.0194(18) -0.0033(16) 0.0004(16) -0.0040(17) C24 0.0227(18) 0.020(2) 0.0197(16) -0.003(3) -0.0018(13) -0.002(3) C25 0.020(2) 0.024(3) 0.019(2) -0.0034(17) -0.0031(17) 0.0008(19) C26 0.020(2) 0.017(2) 0.025(2) -0.0017(17) -0.0014(17) -0.0034(17) C27 0.0159(19) 0.021(3) 0.028(2) -0.0002(17) 0.0039(15) -0.0001(16) C28 0.021(2) 0.026(3) 0.048(3) 0.007(2) 0.008(2) 0.002(2) C29 0.030(3) 0.024(3) 0.041(3) -0.008(2) 0.010(2) 0.005(2) C30 0.025(2) 0.040(4) 0.042(2) 0.010(3) 0.0025(17) 0.009(3) C31 0.023(2) 0.026(2) 0.025(2) -0.0026(19) -0.0006(18) -0.0004(19) O32 0.0206(16) 0.038(2) 0.0369(17) 0.0026(14) -0.0046(13) -0.0070(14) N33 0.0231(19) 0.026(2) 0.0260(18) 0.0017(16) -0.0005(15) -0.0057(16) C34 0.029(3) 0.023(3) 0.038(3) 0.001(2) -0.002(2) -0.007(2) C35 0.024(2) 0.026(3) 0.022(2) 0.0013(19) 0.0031(17) 0.000(2) C36 0.025(2) 0.025(4) 0.027(2) -0.007(2) -0.0023(16) -0.001(2) C37 0.033(3) 0.025(3) 0.028(2) -0.0066(18) -0.004(2) 0.000(2) N38 0.029(2) 0.029(2) 0.0257(19) -0.0029(15) -0.0034(16) 0.0044(16) C39 0.033(3) 0.022(3) 0.029(2) 0.000(2) -0.0037(19) 0.005(2) C40 0.035(3) 0.024(3) 0.030(2) -0.0049(19) -0.003(2) -0.002(2) N41 0.037(2) 0.035(3) 0.035(2) -0.004(2) -0.0057(19) 0.002(2) O42 0.0368(19) 0.031(2) 0.0371(18) 0.0066(16) 0.0042(15) 0.0005(16) O43 0.066(3) 0.068(3) 0.039(2) -0.018(2) 0.003(2) 0.021(3) O44 0.101(3) 0.047(3) 0.055(2) -0.0037(19) 0.018(2) -0.032(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N38 2.187(4) 4_557 ? Ag N11 2.191(3) . ? N11 C16 1.343(6) . ? N11 C12 1.344(6) . ? C12 C13 1.369(6) . ? C12 H12A 0.9500 . ? C13 C14 1.392(6) . ? C13 H13A 0.9500 . ? C14 C15 1.391(6) . ? C14 N17 1.425(4) . ? C15 C16 1.375(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N17 C19 1.369(7) . ? N17 C18 1.487(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O20 1.229(6) . ? C19 C21 1.482(7) . ? C21 C26 1.382(5) . ? C21 C22 1.394(6) . ? C22 C23 1.391(6) . ? C22 H22A 0.9500 . ? C23 C24 1.393(5) . ? C23 C31 1.494(6) . ? C24 C25 1.404(7) . ? C24 H24A 0.9500 . ? C25 C26 1.377(6) . ? C25 C27 1.528(5) . ? C26 H26A 0.9500 . ? C27 C28 1.529(6) . ? C27 C29 1.530(6) . ? C27 C30 1.533(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O32 1.219(5) . ? C31 N33 1.387(5) . ? N33 C35 1.410(5) . ? N33 C34 1.485(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.393(6) . ? C35 C36 1.397(7) . ? C36 C37 1.387(6) . ? C36 H36A 0.9500 . ? C37 N38 1.342(5) . ? C37 H37A 0.9500 . ? N38 C39 1.335(6) . ? N38 Ag 2.187(4) 4_547 ? C39 C40 1.375(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? N41 O44 1.244(5) . ? N41 O43 1.250(5) . ? N41 O42 1.263(5) . ? 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 N38 Ag N11 165.51(16) 4_557 . ? C16 N11 C12 117.4(3) . . ? C16 N11 Ag 121.5(3) . . ? C12 N11 Ag 121.1(3) . . ? N11 C12 C13 122.5(4) . . ? N11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 117.8(3) . . ? C15 C14 N17 122.0(4) . . ? C13 C14 N17 120.1(4) . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? N11 C16 C15 123.6(4) . . ? N11 C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? C19 N17 C14 123.4(5) . . ? C19 N17 C18 118.6(3) . . ? C14 N17 C18 116.5(5) . . ? N17 C18 H18A 109.5 . . ? N17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O20 C19 N17 119.6(5) . . ? O20 C19 C21 122.1(5) . . ? N17 C19 C21 118.2(4) . . ? C26 C21 C22 120.4(4) . . ? C26 C21 C19 122.9(4) . . ? C22 C21 C19 116.6(4) . . ? C23 C22 C21 118.7(4) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 C31 118.5(4) . . ? C24 C23 C31 121.7(4) . . ? C23 C24 C25 121.8(6) . . ? C23 C24 H24A 119.1 . . ? C25 C24 H24A 119.1 . . ? C26 C25 C24 116.9(4) . . ? C26 C25 C27 124.4(4) . . ? C24 C25 C27 118.6(4) . . ? C25 C26 C21 122.2(4) . . ? C25 C26 H26A 118.9 . . ? C21 C26 H26A 118.9 . . ? C25 C27 C28 111.3(3) . . ? C25 C27 C29 109.9(3) . . ? C28 C27 C29 108.1(3) . . ? C25 C27 C30 109.3(3) . . ? C28 C27 C30 108.9(4) . . ? C29 C27 C30 109.2(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O32 C31 N33 120.4(4) . . ? O32 C31 C23 121.7(4) . . ? N33 C31 C23 117.8(4) . . ? C31 N33 C35 123.5(4) . . ? C31 N33 C34 117.2(4) . . ? C35 N33 C34 118.9(4) . . ? N33 C34 H34A 109.5 . . ? N33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 117.8(4) . . ? C40 C35 N33 120.7(4) . . ? C36 C35 N33 121.6(4) . . ? C37 C36 C35 118.8(4) . . ? C37 C36 H36A 120.6 . . ? C35 C36 H36A 120.6 . . ? N38 C37 C36 123.7(4) . . ? N38 C37 H37A 118.2 . . ? C36 C37 H37A 118.2 . . ? C39 N38 C37 116.2(4) . . ? C39 N38 Ag 122.3(3) . 4_547 ? C37 N38 Ag 121.3(3) . 4_547 ? N38 C39 C40 124.9(4) . . ? N38 C39 H39A 117.6 . . ? C40 C39 H39A 117.6 . . ? C39 C40 C35 118.6(4) . . ? C39 C40 H40A 120.7 . . ? C35 C40 H40A 120.7 . . ? O44 N41 O43 121.2(4) . . ? O44 N41 O42 118.3(4) . . ? O43 N41 O42 120.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N38 Ag N11 C16 93.7(6) 4_557 . . . ? N38 Ag N11 C12 -84.7(9) 4_557 . . . ? C16 N11 C12 C13 -1.9(8) . . . . ? Ag N11 C12 C13 176.6(4) . . . . ? N11 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 0.8(8) . . . . ? C12 C13 C14 N17 176.4(5) . . . . ? C13 C14 C15 C16 -1.5(8) . . . . ? N17 C14 C15 C16 -177.0(5) . . . . ? C12 N11 C16 C15 1.2(8) . . . . ? Ag N11 C16 C15 -177.3(4) . . . . ? C14 C15 C16 N11 0.5(7) . . . . ? C15 C14 N17 C19 -46.6(7) . . . . ? C13 C14 N17 C19 138.0(5) . . . . ? C15 C14 N17 C18 119.3(6) . . . . ? C13 C14 N17 C18 -56.1(6) . . . . ? C14 N17 C19 O20 164.5(4) . . . . ? C18 N17 C19 O20 -1.1(5) . . . . ? C14 N17 C19 C21 -19.2(6) . . . . ? C18 N17 C19 C21 175.2(4) . . . . ? O20 C19 C21 C26 126.1(5) . . . . ? N17 C19 C21 C26 -50.1(6) . . . . ? O20 C19 C21 C22 -50.7(6) . . . . ? N17 C19 C21 C22 133.1(4) . . . . ? C26 C21 C22 C23 4.1(6) . . . . ? C19 C21 C22 C23 -178.9(4) . . . . ? C21 C22 C23 C24 -4.9(6) . . . . ? C21 C22 C23 C31 177.0(3) . . . . ? C22 C23 C24 C25 1.8(6) . . . . ? C31 C23 C24 C25 179.8(4) . . . . ? C23 C24 C25 C26 2.2(5) . . . . ? C23 C24 C25 C27 -178.2(3) . . . . ? C24 C25 C26 C21 -3.0(6) . . . . ? C27 C25 C26 C21 177.4(4) . . . . ? C22 C21 C26 C25 -0.1(6) . . . . ? C19 C21 C26 C25 -176.8(4) . . . . ? C26 C25 C27 C28 1.0(6) . . . . ? C24 C25 C27 C28 -178.6(4) . . . . ? C26 C25 C27 C29 -118.8(4) . . . . ? C24 C25 C27 C29 61.6(4) . . . . ? C26 C25 C27 C30 121.3(5) . . . . ? C24 C25 C27 C30 -58.3(5) . . . . ? C22 C23 C31 O32 45.4(6) . . . . ? C24 C23 C31 O32 -132.7(4) . . . . ? C22 C23 C31 N33 -138.6(4) . . . . ? C24 C23 C31 N33 43.3(5) . . . . ? O32 C31 N33 C35 -164.1(4) . . . . ? C23 C31 N33 C35 19.8(6) . . . . ? O32 C31 N33 C34 8.8(6) . . . . ? C23 C31 N33 C34 -167.3(4) . . . . ? C31 N33 C35 C40 -141.9(4) . . . . ? C34 N33 C35 C40 45.3(6) . . . . ? C31 N33 C35 C36 38.5(6) . . . . ? C34 N33 C35 C36 -134.3(5) . . . . ? C40 C35 C36 C37 1.8(6) . . . . ? N33 C35 C36 C37 -178.6(3) . . . . ? C35 C36 C37 N38 -1.0(7) . . . . ? C36 C37 N38 C39 0.2(6) . . . . ? C36 C37 N38 Ag -175.1(3) . . . 4_547 ? C37 N38 C39 C40 -0.4(6) . . . . ? Ag N38 C39 C40 174.9(3) 4_547 . . . ? N38 C39 C40 C35 1.3(7) . . . . ? C36 C35 C40 C39 -2.0(6) . . . . ? N33 C35 C40 C39 178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.348 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.070 # Attachment '8.cif' data_04073 _database_code_depnum_ccdc_archive 'CCDC 747046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 Ag F3 N4 O4' _chemical_formula_weight 567.27 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7454(3) _cell_length_b 11.3948(4) _cell_length_c 18.2357(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.076(2) _cell_angle_gamma 90.00 _cell_volume 2204.85(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3888 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.03 _exptl_crystal_description petal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4818 _exptl_absorpt_correction_T_max 0.8876 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23636 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3888 _reflns_number_gt 2900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.1570P] 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 3888 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _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 -0.5000 -1.0000 0.0000 0.0987(4) Uani 1 2 d S . . Ag2 Ag 0.0000 0.0000 0.0000 0.04445(18) Uani 1 2 d S . . N1 N -0.3691(4) -0.9627(4) -0.0716(3) 0.0504(12) Uani 1 1 d . . . C2 C -0.3337(4) -0.8523(4) -0.0814(3) 0.0355(11) Uani 1 1 d . . . H2A H -0.3662 -0.7919 -0.0539 0.043 Uiso 1 1 calc R . . C3 C -0.2522(4) -0.8218(4) -0.1294(3) 0.0301(10) Uani 1 1 d . . . C4 C -0.2038(5) -0.9106(5) -0.1674(3) 0.0475(14) Uani 1 1 d . . . H4A H -0.1468 -0.8928 -0.2008 0.057 Uiso 1 1 calc R . . C5 C -0.2377(7) -1.0254(5) -0.1572(4) 0.070(2) Uani 1 1 d . . . H5A H -0.2042 -1.0876 -0.1829 0.084 Uiso 1 1 calc R . . C6 C -0.3210(7) -1.0475(5) -0.1091(4) 0.068(2) Uani 1 1 d . . . H6A H -0.3454 -1.1264 -0.1023 0.082 Uiso 1 1 calc R . . C7 C -0.2162(5) -0.6953(4) -0.1376(3) 0.0341(11) Uani 1 1 d . . . H7A H -0.1438 -0.6914 -0.1650 0.041 Uiso 1 1 calc R . . H7B H -0.2877 -0.6533 -0.1673 0.041 Uiso 1 1 calc R . . N8 N -0.1830(3) -0.6369(3) -0.0667(2) 0.0317(9) Uani 1 1 d . . . H8A H -0.2282 -0.5775 -0.0548 0.038 Uiso 1 1 calc R . . C9 C -0.0825(4) -0.6742(4) -0.0192(3) 0.0301(10) Uani 1 1 d . . . O10 O -0.0204(3) -0.7593(3) -0.03519(19) 0.0382(8) Uani 1 1 d . . . C11 C -0.0491(4) -0.6135(4) 0.0538(3) 0.0273(10) Uani 1 1 d . . . C12 C -0.1189(4) -0.5210(4) 0.0753(3) 0.0314(11) Uani 1 1 d . . . H12A H -0.1906 -0.4936 0.0425 0.038 Uiso 1 1 calc R . . C13 C -0.0854(4) -0.4681(4) 0.1438(3) 0.0316(11) Uani 1 1 d . . . C14 C 0.0188(4) -0.5093(4) 0.1916(3) 0.0378(11) Uani 1 1 d . . . H14A H 0.0419 -0.4745 0.2392 0.045 Uiso 1 1 calc R . . C15 C 0.0892(5) -0.6009(4) 0.1701(3) 0.0432(13) Uani 1 1 d . . . H15A H 0.1608 -0.6284 0.2029 0.052 Uiso 1 1 calc R . . C16 C 0.0564(4) -0.6528(4) 0.1016(3) 0.0365(12) Uani 1 1 d . . . H16A H 0.1057 -0.7152 0.0870 0.044 Uiso 1 1 calc R . . C17 C -0.1557(5) -0.3658(4) 0.1685(3) 0.0381(12) Uani 1 1 d . . . O18 O -0.1169(4) -0.3141(3) 0.2266(2) 0.0595(11) Uani 1 1 d . . . N19 N -0.2630(4) -0.3332(3) 0.1252(2) 0.0338(9) Uani 1 1 d . . . H19A H -0.2896 -0.3717 0.0839 0.041 Uiso 1 1 calc R . . C20 C -0.3352(5) -0.2351(4) 0.1462(3) 0.0382(12) Uani 1 1 d . . . H20A H -0.3416 -0.2422 0.1996 0.046 Uiso 1 1 calc R . . H20B H -0.4216 -0.2397 0.1179 0.046 Uiso 1 1 calc R . . C21 C -0.2808(4) -0.1161(4) 0.1329(3) 0.0280(10) Uani 1 1 d . . . C22 C -0.1890(4) -0.1044(4) 0.0884(3) 0.0331(11) Uani 1 1 d . . . H22A H -0.1599 -0.1733 0.0671 0.040 Uiso 1 1 calc R . . N23 N -0.1384(3) -0.0005(3) 0.0735(2) 0.0341(9) Uani 1 1 d . . . C24 C -0.1809(5) 0.0956(4) 0.1032(3) 0.0391(12) Uani 1 1 d . . . H24A H -0.1461 0.1694 0.0933 0.047 Uiso 1 1 calc R . . C25 C -0.2732(5) 0.0921(4) 0.1476(3) 0.0394(12) Uani 1 1 d . . . H25A H -0.3021 0.1623 0.1674 0.047 Uiso 1 1 calc R . . C26 C -0.3230(4) -0.0146(4) 0.1629(3) 0.0324(11) Uani 1 1 d . . . H26A H -0.3862 -0.0188 0.1939 0.039 Uiso 1 1 calc R . . O31 O -0.6440(4) -0.5715(4) 0.0265(2) 0.0633(12) Uani 1 1 d . . . O32 O -0.5213(4) -0.7309(3) 0.0312(2) 0.0585(11) Uani 1 1 d . . . C33 C -0.5609(5) -0.6403(4) 0.0553(3) 0.0386(12) Uani 1 1 d . . . C34 C -0.4977(5) -0.6062(5) 0.1339(3) 0.0469(14) Uani 1 1 d . . . F35 F -0.5318(4) -0.6795(4) 0.1839(2) 0.0951(14) Uani 1 1 d . . . F36 F -0.5235(4) -0.4983(3) 0.1545(2) 0.0881(13) Uani 1 1 d . . . F37 F -0.3728(3) -0.6120(3) 0.1431(2) 0.0704(10) 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 0.0477(4) 0.1713(9) 0.0698(5) 0.0654(6) -0.0127(3) -0.0559(5) Ag2 0.0384(3) 0.0452(3) 0.0534(4) 0.0109(3) 0.0185(3) -0.0021(3) N1 0.047(3) 0.052(3) 0.048(3) 0.012(2) -0.008(2) -0.026(2) C2 0.031(2) 0.037(3) 0.037(3) 0.000(2) 0.002(2) -0.006(2) C3 0.032(2) 0.030(3) 0.029(3) -0.003(2) 0.006(2) -0.004(2) C4 0.060(3) 0.042(3) 0.042(3) -0.010(3) 0.016(3) -0.001(3) C5 0.114(6) 0.037(4) 0.055(4) -0.015(3) 0.004(4) 0.001(3) C6 0.097(5) 0.031(3) 0.064(5) 0.007(3) -0.025(4) -0.029(4) C7 0.045(3) 0.029(3) 0.030(3) -0.001(2) 0.010(2) -0.004(2) N8 0.037(2) 0.0220(19) 0.036(2) -0.0049(17) 0.0068(18) 0.0017(17) C9 0.030(2) 0.023(2) 0.040(3) 0.002(2) 0.014(2) -0.004(2) O10 0.0350(18) 0.0284(18) 0.053(2) -0.0074(16) 0.0136(16) 0.0032(15) C11 0.027(2) 0.019(2) 0.036(3) 0.0027(19) 0.007(2) -0.0022(18) C12 0.029(2) 0.030(3) 0.035(3) 0.001(2) 0.005(2) -0.0002(19) C13 0.038(3) 0.026(2) 0.033(3) 0.003(2) 0.011(2) -0.0048(19) C14 0.046(3) 0.032(3) 0.034(3) 0.008(2) 0.002(2) -0.011(2) C15 0.043(3) 0.036(3) 0.046(3) 0.012(3) -0.008(2) 0.001(2) C16 0.041(3) 0.018(2) 0.050(3) 0.008(2) 0.004(2) 0.003(2) C17 0.048(3) 0.034(3) 0.034(3) -0.002(2) 0.013(2) -0.006(2) O18 0.079(3) 0.053(2) 0.043(2) -0.018(2) -0.002(2) 0.007(2) N19 0.040(2) 0.023(2) 0.042(3) -0.0086(18) 0.018(2) -0.0027(17) C20 0.041(3) 0.031(3) 0.048(3) -0.006(2) 0.022(2) -0.003(2) C21 0.025(2) 0.028(2) 0.031(3) 0.001(2) 0.0061(19) 0.0031(19) C22 0.036(3) 0.024(2) 0.042(3) 0.000(2) 0.014(2) 0.003(2) N23 0.033(2) 0.028(2) 0.043(2) 0.008(2) 0.0095(18) 0.0043(19) C24 0.043(3) 0.025(3) 0.048(3) 0.005(2) 0.002(2) -0.003(2) C25 0.047(3) 0.029(3) 0.042(3) -0.003(2) 0.009(2) 0.007(2) C26 0.032(2) 0.034(3) 0.032(3) -0.002(2) 0.008(2) 0.003(2) O31 0.051(2) 0.067(3) 0.066(3) -0.012(2) -0.010(2) 0.023(2) O32 0.074(3) 0.040(2) 0.063(3) -0.012(2) 0.016(2) 0.011(2) C33 0.036(3) 0.035(3) 0.047(3) 0.000(2) 0.012(2) 0.000(2) C34 0.041(3) 0.040(3) 0.059(4) -0.007(3) 0.005(3) 0.003(2) F35 0.121(3) 0.116(4) 0.051(2) 0.016(2) 0.022(2) -0.039(3) F36 0.092(3) 0.069(2) 0.094(3) -0.041(2) -0.013(2) 0.026(2) F37 0.0442(19) 0.068(2) 0.092(3) -0.002(2) -0.0113(18) 0.0024(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 2.108(5) 3_435 ? Ag1 N1 2.108(5) . ? Ag2 N23 2.154(4) 3 ? Ag2 N23 2.154(4) . ? N1 C6 1.334(8) . ? N1 C2 1.334(6) . ? C2 C3 1.377(6) . ? C3 C4 1.374(7) . ? C3 C7 1.506(6) . ? C4 C5 1.378(8) . ? C5 C6 1.372(9) . ? C7 N8 1.448(6) . ? N8 C9 1.342(6) . ? C9 O10 1.237(5) . ? C9 C11 1.494(6) . ? C11 C12 1.385(6) . ? C11 C16 1.390(6) . ? C12 C13 1.384(6) . ? C13 C14 1.389(7) . ? C13 C17 1.496(6) . ? C14 C15 1.381(7) . ? C15 C16 1.377(7) . ? C17 O18 1.227(6) . ? C17 N19 1.343(6) . ? N19 C20 1.446(6) . ? C20 C21 1.511(6) . ? C21 C22 1.380(6) . ? C21 C26 1.385(6) . ? C22 N23 1.348(6) . ? N23 C24 1.333(6) . ? C24 C25 1.377(7) . ? C25 C26 1.374(7) . ? O31 C33 1.241(6) . ? O32 C33 1.224(6) . ? C33 C34 1.537(7) . ? C34 F37 1.327(6) . ? C34 F36 1.328(6) . ? C34 F35 1.330(6) . ? 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 N1 180.000(1) 3_435 . ? N23 Ag2 N23 180.00(16) 3 . ? C6 N1 C2 118.2(5) . . ? C6 N1 Ag1 121.5(4) . . ? C2 N1 Ag1 120.3(4) . . ? N1 C2 C3 123.1(5) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 C7 122.1(4) . . ? C2 C3 C7 120.3(4) . . ? C3 C4 C5 120.1(5) . . ? C6 C5 C4 118.3(6) . . ? N1 C6 C5 122.6(5) . . ? N8 C7 C3 112.5(4) . . ? C9 N8 C7 119.4(4) . . ? O10 C9 N8 120.4(4) . . ? O10 C9 C11 120.7(4) . . ? N8 C9 C11 119.0(4) . . ? C12 C11 C16 119.5(4) . . ? C12 C11 C9 122.7(4) . . ? C16 C11 C9 117.9(4) . . ? C13 C12 C11 120.8(4) . . ? C12 C13 C14 119.3(4) . . ? C12 C13 C17 122.6(4) . . ? C14 C13 C17 118.1(4) . . ? C15 C14 C13 120.0(5) . . ? C16 C15 C14 120.6(5) . . ? C15 C16 C11 119.8(4) . . ? O18 C17 N19 121.2(5) . . ? O18 C17 C13 121.0(5) . . ? N19 C17 C13 117.8(4) . . ? C17 N19 C20 120.4(4) . . ? N19 C20 C21 114.5(4) . . ? C22 C21 C26 117.5(4) . . ? C22 C21 C20 120.7(4) . . ? C26 C21 C20 121.8(4) . . ? N23 C22 C21 123.4(4) . . ? C24 N23 C22 117.7(4) . . ? C24 N23 Ag2 124.4(3) . . ? C22 N23 Ag2 117.8(3) . . ? N23 C24 C25 122.7(4) . . ? C26 C25 C24 119.0(4) . . ? C25 C26 C21 119.7(4) . . ? O32 C33 O31 130.5(5) . . ? O32 C33 C34 114.9(5) . . ? O31 C33 C34 114.7(5) . . ? F37 C34 F36 105.2(4) . . ? F37 C34 F35 105.3(5) . . ? F36 C34 F35 107.2(5) . . ? F37 C34 C33 113.2(4) . . ? F36 C34 C33 114.6(5) . . ? F35 C34 C33 110.6(4) . . ? 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 N8 H8A O31 0.88 2.29 3.173(5) 176.8 3_445 N19 H19A O31 0.88 2.13 2.993(6) 167.7 3_445 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.148 _refine_diff_density_min -2.256 _refine_diff_density_rms 0.093 # Attachment '9.cif' data_04108b _database_code_depnum_ccdc_archive 'CCDC 747047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 Ag N5 O5' _chemical_formula_weight 516.26 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.2247(5) _cell_length_b 9.6779(3) _cell_length_c 30.7686(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3938.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3495 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.11 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.069 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4635 _exptl_absorpt_correction_T_max 0.9241 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34193 _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.11 _reflns_number_total 3495 _reflns_number_gt 2250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.1714P] 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 3495 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Ag Ag 0.87893(3) 0.01992(4) 0.515465(12) 0.05135(19) Uani 1 1 d . . . N11 N 0.8536(3) 0.1816(4) 0.46838(12) 0.0391(9) Uani 1 1 d . . . C12 C 0.8621(3) 0.1596(5) 0.42544(14) 0.0351(10) Uani 1 1 d . . . H12A H 0.8722 0.0678 0.4154 0.042 Uiso 1 1 calc R . . C13 C 0.8567(3) 0.2647(4) 0.39520(14) 0.0280(10) Uani 1 1 d . . . C14 C 0.8433(3) 0.3983(4) 0.41028(14) 0.0362(11) Uani 1 1 d . . . H14A H 0.8401 0.4734 0.3904 0.043 Uiso 1 1 calc R . . C15 C 0.8345(4) 0.4213(5) 0.45439(16) 0.0435(12) Uani 1 1 d . . . H15A H 0.8260 0.5124 0.4652 0.052 Uiso 1 1 calc R . . C16 C 0.8384(3) 0.3119(5) 0.48217(15) 0.0390(11) Uani 1 1 d . . . H16A H 0.8300 0.3281 0.5124 0.047 Uiso 1 1 calc R . . C17 C 0.8644(3) 0.2321(4) 0.34751(14) 0.0309(10) Uani 1 1 d . . . H17A H 0.8849 0.3165 0.3316 0.037 Uiso 1 1 calc R . . H17B H 0.9176 0.1616 0.3431 0.037 Uiso 1 1 calc R . . N18 N 0.7693(2) 0.1812(3) 0.32957(10) 0.0295(8) Uani 1 1 d . . . H18A H 0.7632 0.0923 0.3242 0.035 Uiso 1 1 calc R . . C19 C 0.6910(3) 0.2648(4) 0.32101(13) 0.0266(10) Uani 1 1 d . . . O20 O 0.6958(2) 0.3916(3) 0.32605(9) 0.0355(7) Uani 1 1 d . . . C21 C 0.5967(3) 0.1985(4) 0.30458(13) 0.0252(10) Uani 1 1 d . . . C22 C 0.5038(3) 0.2587(4) 0.31400(12) 0.0243(9) Uani 1 1 d . . . H22A H 0.5012 0.3393 0.3316 0.029 Uiso 1 1 calc R . . C23 C 0.4150(3) 0.2021(4) 0.29800(12) 0.0247(9) Uani 1 1 d . . . C24 C 0.4193(3) 0.0848(4) 0.27175(13) 0.0288(10) Uani 1 1 d . . . H24A H 0.3588 0.0461 0.2604 0.035 Uiso 1 1 calc R . . C25 C 0.5118(3) 0.0249(4) 0.26224(13) 0.0300(10) Uani 1 1 d . . . H25A H 0.5147 -0.0551 0.2444 0.036 Uiso 1 1 calc R . . C26 C 0.5995(3) 0.0811(4) 0.27867(13) 0.0291(10) Uani 1 1 d . . . H26A H 0.6627 0.0391 0.2722 0.035 Uiso 1 1 calc R . . C27 C 0.3158(3) 0.2700(4) 0.30846(13) 0.0274(10) Uani 1 1 d . . . O28 O 0.3094(2) 0.3972(3) 0.31269(9) 0.0348(7) Uani 1 1 d . . . N29 N 0.2360(2) 0.1867(3) 0.31234(10) 0.0295(8) Uani 1 1 d . . . H29A H 0.2440 0.0977 0.3076 0.035 Uiso 1 1 calc R . . C30 C 0.1359(3) 0.2379(4) 0.32414(14) 0.0322(10) Uani 1 1 d . . . H30A H 0.0841 0.1700 0.3150 0.039 Uiso 1 1 calc R . . H30B H 0.1227 0.3256 0.3086 0.039 Uiso 1 1 calc R . . C31 C 0.1275(3) 0.2621(4) 0.37292(14) 0.0295(10) Uani 1 1 d . . . C32 C 0.1330(3) 0.1500(4) 0.40067(14) 0.0349(11) Uani 1 1 d . . . H32A H 0.1423 0.0609 0.3884 0.042 Uiso 1 1 calc R . . N33 N 0.1259(3) 0.1605(4) 0.44396(12) 0.0387(9) Uani 1 1 d . . . C34 C 0.1118(3) 0.2875(5) 0.46099(16) 0.0442(12) Uani 1 1 d . . . H34A H 0.1070 0.2972 0.4916 0.053 Uiso 1 1 calc R . . C35 C 0.1040(4) 0.4032(5) 0.43530(16) 0.0477(13) Uani 1 1 d . . . H35A H 0.0929 0.4913 0.4480 0.057 Uiso 1 1 calc R . . C36 C 0.1126(3) 0.3900(5) 0.39076(15) 0.0372(11) Uani 1 1 d . . . H36A H 0.1083 0.4692 0.3726 0.045 Uiso 1 1 calc R . . O41 O 1.0346(3) 0.1282(4) 0.55555(13) 0.0749(12) Uani 1 1 d . . . O42 O 0.9032(3) 0.2251(5) 0.58356(13) 0.0716(12) Uani 1 1 d . . . O43 O 1.0473(4) 0.3250(4) 0.58664(14) 0.0855(14) Uani 1 1 d . . . N44 N 0.9958(4) 0.2275(4) 0.57538(13) 0.0484(11) 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 Ag 0.0699(3) 0.0466(3) 0.0376(3) 0.00994(18) -0.00543(19) -0.0062(2) N11 0.043(2) 0.040(2) 0.034(2) -0.0012(19) -0.0030(18) -0.0065(18) C12 0.038(3) 0.032(2) 0.036(3) -0.005(2) -0.002(2) -0.001(2) C13 0.028(2) 0.028(2) 0.028(2) -0.0014(19) -0.0048(19) -0.0020(18) C14 0.045(3) 0.029(2) 0.035(3) 0.002(2) -0.009(2) 0.003(2) C15 0.050(3) 0.037(3) 0.044(3) -0.013(2) -0.007(2) 0.005(2) C16 0.045(3) 0.041(3) 0.031(3) -0.008(2) -0.002(2) 0.000(2) C17 0.026(2) 0.033(2) 0.034(3) 0.000(2) -0.0029(19) 0.0022(19) N18 0.032(2) 0.0270(18) 0.030(2) -0.0035(16) 0.0009(16) -0.0018(16) C19 0.032(2) 0.024(2) 0.024(2) 0.0023(18) 0.0046(19) 0.0000(19) O20 0.0384(17) 0.0222(17) 0.0459(19) 0.0000(14) -0.0043(14) -0.0036(13) C21 0.027(2) 0.022(2) 0.026(2) 0.0053(18) 0.0012(18) -0.0012(17) C22 0.031(2) 0.020(2) 0.022(2) 0.0019(17) -0.0015(18) 0.0010(18) C23 0.033(2) 0.022(2) 0.019(2) 0.0050(17) 0.0002(18) 0.0001(18) C24 0.033(2) 0.025(2) 0.028(2) -0.0005(19) -0.005(2) -0.001(2) C25 0.034(2) 0.026(2) 0.030(2) -0.0082(19) 0.002(2) -0.002(2) C26 0.035(2) 0.025(2) 0.027(2) 0.0010(19) 0.0038(19) 0.0014(19) C27 0.032(2) 0.026(2) 0.025(2) 0.0029(18) 0.0006(19) -0.001(2) O28 0.0386(17) 0.0211(17) 0.0448(19) -0.0002(14) 0.0027(14) 0.0005(14) N29 0.0297(19) 0.0236(18) 0.035(2) -0.0003(16) 0.0019(16) 0.0030(16) C30 0.027(2) 0.032(2) 0.038(3) 0.000(2) 0.0004(19) 0.0006(19) C31 0.023(2) 0.033(2) 0.032(3) 0.002(2) 0.0007(18) -0.0027(19) C32 0.037(3) 0.029(2) 0.038(3) -0.004(2) -0.002(2) -0.002(2) N33 0.049(2) 0.037(2) 0.031(2) -0.0008(18) -0.0004(18) -0.0077(19) C34 0.052(3) 0.043(3) 0.037(3) -0.004(2) -0.001(2) -0.005(2) C35 0.058(3) 0.041(3) 0.044(3) -0.011(2) -0.007(2) 0.002(2) C36 0.040(3) 0.032(3) 0.040(3) 0.001(2) -0.003(2) 0.002(2) O41 0.096(3) 0.056(2) 0.073(3) -0.025(2) -0.022(2) 0.026(2) O42 0.069(3) 0.094(3) 0.052(3) 0.002(2) 0.000(2) -0.003(2) O43 0.123(4) 0.046(2) 0.088(3) -0.005(2) -0.011(3) -0.033(3) N44 0.073(3) 0.041(3) 0.031(2) 0.007(2) -0.008(2) -0.003(3) _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 Ag N33 2.147(4) 5_656 ? Ag N11 2.158(4) . ? Ag Ag 3.3629(8) 5_756 ? N11 C12 1.343(5) . ? N11 C16 1.346(6) . ? C12 C13 1.380(6) . ? C13 C14 1.385(6) . ? C13 C17 1.504(6) . ? C14 C15 1.380(6) . ? C15 C16 1.362(6) . ? C17 N18 1.459(5) . ? N18 C19 1.340(5) . ? C19 O20 1.238(5) . ? C19 C21 1.491(5) . ? C21 C26 1.388(6) . ? C21 C22 1.390(5) . ? C22 C23 1.386(5) . ? C23 C24 1.394(5) . ? C23 C27 1.502(6) . ? C24 C25 1.385(5) . ? C25 C26 1.378(5) . ? C27 O28 1.240(5) . ? C27 N29 1.334(5) . ? N29 C30 1.459(5) . ? C30 C31 1.523(6) . ? C31 C36 1.368(6) . ? C31 C32 1.382(6) . ? C32 N33 1.339(5) . ? N33 C34 1.349(6) . ? N33 Ag 2.147(4) 5_656 ? C34 C35 1.375(7) . ? C35 C36 1.381(6) . ? O41 N44 1.249(5) . ? O42 N44 1.250(5) . ? O43 N44 1.213(5) . ? 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 N33 Ag N11 167.14(14) 5_656 . ? N33 Ag Ag 95.71(10) 5_656 5_756 ? N11 Ag Ag 92.36(10) . 5_756 ? C12 N11 C16 118.1(4) . . ? C12 N11 Ag 122.2(3) . . ? C16 N11 Ag 119.4(3) . . ? N11 C12 C13 122.9(4) . . ? C12 C13 C14 117.9(4) . . ? C12 C13 C17 120.0(4) . . ? C14 C13 C17 122.1(4) . . ? C15 C14 C13 119.4(4) . . ? C16 C15 C14 119.3(4) . . ? N11 C16 C15 122.4(4) . . ? N18 C17 C13 112.4(3) . . ? C19 N18 C17 122.4(3) . . ? O20 C19 N18 122.3(4) . . ? O20 C19 C21 120.8(4) . . ? N18 C19 C21 116.9(3) . . ? C26 C21 C22 119.1(4) . . ? C26 C21 C19 121.7(4) . . ? C22 C21 C19 119.2(4) . . ? C23 C22 C21 120.6(4) . . ? C22 C23 C24 119.5(4) . . ? C22 C23 C27 119.4(3) . . ? C24 C23 C27 121.1(4) . . ? C25 C24 C23 120.0(4) . . ? C26 C25 C24 120.0(4) . . ? C25 C26 C21 120.8(4) . . ? O28 C27 N29 122.4(4) . . ? O28 C27 C23 121.1(4) . . ? N29 C27 C23 116.5(3) . . ? C27 N29 C30 122.3(3) . . ? N29 C30 C31 111.4(3) . . ? C36 C31 C32 118.0(4) . . ? C36 C31 C30 123.0(4) . . ? C32 C31 C30 119.0(4) . . ? N33 C32 C31 123.5(4) . . ? C32 N33 C34 117.7(4) . . ? C32 N33 Ag 121.3(3) . 5_656 ? C34 N33 Ag 120.7(3) . 5_656 ? N33 C34 C35 122.0(5) . . ? C34 C35 C36 119.3(5) . . ? C31 C36 C35 119.6(4) . . ? O43 N44 O41 120.5(5) . . ? O43 N44 O42 120.4(5) . . ? O41 N44 O42 119.1(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 N18 H18A O20 0.88 2.02 2.842(4) 155.6 8_755 N29 H29A O28 0.88 2.07 2.866(4) 149.8 8_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.692 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.092