Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email ICDD@MAHENDRA.IACS.RES.IN _publ_section_title ; Effect of the size of discrete anions on the nuclearity of a complex cation ; loop_ _publ_author_name 'Dipankar Datta' 'Senjuti De' 'Israel Goldberg' 'Goutam Kumar Patra' data_1 _database_code_depnum_ccdc_archive 'CCDC 646201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 Ag N2 O, C H4 O, Cl O4' _chemical_formula_sum 'C22 H22 Ag Cl N2 O6' _chemical_formula_weight 553.74 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 8.7001(2) _cell_length_b 10.0485(2) _cell_length_c 14.2342(3) _cell_angle_alpha 105.9560(12) _cell_angle_beta 94.3267(12) _cell_angle_gamma 107.7168(12) _cell_volume 1122.38(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3963 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.25 _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8162 _exptl_absorpt_correction_T_max 0.9016 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10938 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5258 _reflns_number_gt 3990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.5811P] 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 5258 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.005 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 0.0000 0.0000 0.0000 0.01934(9) Uani 1 2 d S . . Ag2 Ag 0.0000 0.0000 0.5000 0.02043(9) Uani 1 2 d S . . N3 N -0.0283(3) 0.0193(2) 0.35113(15) 0.0145(5) Uani 1 1 d . . . N4 N -0.0128(3) -0.0104(2) 0.15146(15) 0.0136(4) Uani 1 1 d . . . C5 C -0.1565(3) -0.0777(3) 0.17912(19) 0.0159(5) Uani 1 1 d . . . C6 C -0.2985(3) -0.1629(3) 0.1063(2) 0.0200(6) Uani 1 1 d . . . H6 H -0.2933 -0.1778 0.0380 0.024 Uiso 1 1 calc R . . C7 C -0.4429(3) -0.2233(3) 0.1350(2) 0.0231(6) Uani 1 1 d . . . H7 H -0.5381 -0.2795 0.0861 0.028 Uiso 1 1 calc R . . C8 C -0.4531(3) -0.2038(3) 0.2361(2) 0.0219(6) Uani 1 1 d . . . H8 H -0.5548 -0.2462 0.2546 0.026 Uiso 1 1 calc R . . C9 C -0.3160(3) -0.1233(3) 0.3079(2) 0.0197(6) Uani 1 1 d . . . H9 H -0.3228 -0.1107 0.3759 0.024 Uiso 1 1 calc R . . C10 C -0.1660(3) -0.0601(3) 0.28029(19) 0.0144(5) Uani 1 1 d . . . C11 C 0.1090(3) 0.0828(3) 0.32344(19) 0.0137(5) Uani 1 1 d . . . C12 C 0.2556(3) 0.1679(3) 0.40257(19) 0.0164(5) Uani 1 1 d . . . C13 C 0.3930(3) 0.1257(3) 0.4044(2) 0.0225(6) Uani 1 1 d . . . H13 H 0.3957 0.0423 0.3539 0.027 Uiso 1 1 calc R . . C14 C 0.5267(4) 0.2058(4) 0.4802(2) 0.0278(7) Uani 1 1 d . . . H14 H 0.6199 0.1754 0.4826 0.033 Uiso 1 1 calc R . . C15 C 0.5248(4) 0.3292(4) 0.5520(2) 0.0289(7) Uani 1 1 d . . . H15 H 0.6182 0.3854 0.6023 0.035 Uiso 1 1 calc R . . C16 C 0.3880(4) 0.3716(4) 0.5513(2) 0.0304(7) Uani 1 1 d . . . H16 H 0.3868 0.4560 0.6015 0.037 Uiso 1 1 calc R . . C17 C 0.2518(4) 0.2902(3) 0.4767(2) 0.0233(6) Uani 1 1 d . . . H17 H 0.1567 0.3179 0.4765 0.028 Uiso 1 1 calc R . . C18 C 0.1166(3) 0.0701(3) 0.22146(19) 0.0136(5) Uani 1 1 d . . . C19 C 0.2695(3) 0.1488(3) 0.19103(18) 0.0147(5) Uani 1 1 d . . . C20 C 0.3615(3) 0.0709(3) 0.1403(2) 0.0194(6) Uani 1 1 d . . . H20 H 0.3255 -0.0333 0.1229 0.023 Uiso 1 1 calc R . . C21 C 0.5068(3) 0.1467(3) 0.1151(2) 0.0230(6) Uani 1 1 d . . . H21 H 0.5710 0.0940 0.0815 0.028 Uiso 1 1 calc R . . C22 C 0.5580(3) 0.2976(3) 0.1388(2) 0.0224(6) Uani 1 1 d . . . H22 H 0.6573 0.3486 0.1214 0.027 Uiso 1 1 calc R . . C23 C 0.4651(3) 0.3753(3) 0.1880(2) 0.0233(6) Uani 1 1 d . . . H23 H 0.4996 0.4793 0.2032 0.028 Uiso 1 1 calc R . . C24 C 0.3217(3) 0.3010(3) 0.2147(2) 0.0207(6) Uani 1 1 d . . . H24 H 0.2589 0.3543 0.2494 0.025 Uiso 1 1 calc R . . Cl25 Cl -.06610(8) 0.31414(8) 0.70606(6) 0.02335(16) Uani 1 1 d . . . O26 O -.1401(3) 0.4283(2) 0.72156(17) 0.0319(5) Uani 1 1 d . . . O27 O -.1368(3) 0.2177(3) 0.76074(17) 0.0349(6) Uani 1 1 d . . . O28 O -.1008(3) 0.2325(3) 0.60126(18) 0.0412(6) Uani 1 1 d . . . O29 O 0.1065(3) 0.3795(3) 0.7390(2) 0.0478(7) Uani 1 1 d . . . O30 O 0.9336(3) 0.2969(3) 0.27239(17) 0.0312(5) Uani 1 1 d . . . H30 H 0.9988 0.3962 0.2844 0.067(14) Uiso 1 1 d R . . C31 C 0.8200(4) 0.2992(4) 0.3398(3) 0.0342(8) Uani 1 1 d . . . H31A H 0.8729 0.3060 0.4050 0.051 Uiso 1 1 calc R . . H31B H 0.7245 0.2088 0.3148 0.051 Uiso 1 1 calc R . . H31C H 0.7846 0.3845 0.3457 0.051 Uiso 1 1 calc R . . O32 O -.1109(3) 0.2173(2) 0.06261(17) 0.0325(5) Uani 1 1 d . . . H32 H -.0980 0.2451 0.1273 0.056(13) Uiso 1 1 d R . . C33 C -.0305(5) 0.3444(4) 0.0351(3) 0.0432(9) Uani 1 1 d . . . H33A H -.0802 0.4199 0.0593 0.065 Uiso 1 1 calc R . . H33B H -.0423 0.3174 -0.0374 0.065 Uiso 1 1 calc R . . H33C H 0.0861 0.3830 0.0643 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02088(16) 0.02625(18) 0.00844(14) 0.00712(12) 0.00271(11) 0.00304(13) Ag2 0.02156(16) 0.03047(19) 0.01008(15) 0.01052(13) 0.00348(12) 0.00606(13) N3 0.0201(11) 0.0153(12) 0.0081(10) 0.0051(9) 0.0022(9) 0.0048(9) N4 0.0180(11) 0.0162(12) 0.0076(10) 0.0054(9) 0.0037(9) 0.0054(9) C5 0.0180(13) 0.0166(14) 0.0148(13) 0.0068(11) 0.0031(11) 0.0063(11) C6 0.0216(14) 0.0244(16) 0.0120(13) 0.0064(12) 0.0002(11) 0.0049(12) C7 0.0174(13) 0.0276(17) 0.0208(15) 0.0095(13) -0.0013(12) 0.0020(12) C8 0.0168(13) 0.0229(16) 0.0273(16) 0.0105(13) 0.0064(12) 0.0058(12) C9 0.0204(14) 0.0251(16) 0.0157(14) 0.0092(12) 0.0072(11) 0.0073(12) C10 0.0180(13) 0.0151(14) 0.0112(12) 0.0051(10) 0.0020(10) 0.0062(11) C11 0.0176(13) 0.0129(14) 0.0109(12) 0.0049(10) 0.0032(10) 0.0045(11) C12 0.0176(13) 0.0197(15) 0.0102(12) 0.0076(11) 0.0023(10) 0.0014(11) C13 0.0215(14) 0.0328(18) 0.0136(13) 0.0092(12) 0.0032(11) 0.0081(13) C14 0.0169(14) 0.045(2) 0.0218(15) 0.0169(15) 0.0026(12) 0.0052(14) C15 0.0245(15) 0.0339(19) 0.0201(15) 0.0146(14) -0.0054(12) -0.0049(13) C16 0.0388(18) 0.0221(17) 0.0199(15) 0.0015(13) -0.0054(14) 0.0027(14) C17 0.0273(15) 0.0207(16) 0.0188(14) 0.0044(12) -0.0012(12) 0.0068(13) C18 0.0181(13) 0.0144(14) 0.0105(12) 0.0057(10) 0.0030(10) 0.0065(11) C19 0.0174(13) 0.0195(15) 0.0054(11) 0.0046(10) 0.0004(10) 0.0038(11) C20 0.0225(14) 0.0173(15) 0.0151(13) 0.0029(11) 0.0026(11) 0.0041(12) C21 0.0200(14) 0.0297(17) 0.0176(14) 0.0045(12) 0.0066(11) 0.0082(13) C22 0.0157(13) 0.0301(17) 0.0172(14) 0.0079(12) 0.0026(11) 0.0016(12) C23 0.0253(15) 0.0210(16) 0.0221(15) 0.0098(12) 0.0027(12) 0.0034(12) C24 0.0214(14) 0.0198(15) 0.0217(14) 0.0077(12) 0.0072(12) 0.0064(12) Cl25 0.0206(3) 0.0207(4) 0.0301(4) 0.0079(3) 0.0035(3) 0.0092(3) O26 0.0269(11) 0.0257(13) 0.0459(14) 0.0100(11) 0.0050(10) 0.0144(10) O27 0.0434(14) 0.0323(14) 0.0382(13) 0.0189(11) 0.0148(11) 0.0168(11) O28 0.0565(16) 0.0467(16) 0.0299(13) 0.0092(11) 0.0081(12) 0.0332(14) O29 0.0188(11) 0.0358(15) 0.084(2) 0.0163(14) -0.0025(12) 0.0084(11) O30 0.0357(12) 0.0283(13) 0.0357(13) 0.0112(10) 0.0173(10) 0.0158(11) C31 0.0367(18) 0.039(2) 0.0374(19) 0.0169(16) 0.0152(15) 0.0205(16) O32 0.0415(13) 0.0306(13) 0.0300(13) 0.0115(10) 0.0119(10) 0.0155(11) C33 0.053(2) 0.038(2) 0.040(2) 0.0156(17) 0.0132(18) 0.0135(18) _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 N4 2.196(2) 2 ? Ag1 N4 2.196(2) . ? Ag2 N3 2.183(2) . ? Ag2 N3 2.183(2) 2_556 ? N3 C11 1.317(3) . ? N3 C10 1.372(3) . ? N4 C18 1.322(3) . ? N4 C5 1.372(3) . ? C5 C10 1.414(4) . ? C5 C6 1.417(4) . ? C6 C7 1.364(4) . ? C6 H6 0.9500 . ? C7 C8 1.411(4) . ? C7 H7 0.9500 . ? C8 C9 1.377(4) . ? C8 H8 0.9500 . ? C9 C10 1.403(4) . ? C9 H9 0.9500 . ? C11 C18 1.430(3) . ? C11 C12 1.489(4) . ? C12 C13 1.386(4) . ? C12 C17 1.393(4) . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.379(5) . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C15 H15 0.9500 . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.490(4) . ? C19 C24 1.390(4) . ? C19 C20 1.390(4) . ? C20 C21 1.392(4) . ? C20 H20 0.9500 . ? C21 C22 1.377(4) . ? C21 H21 0.9500 . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cl25 O29 1.425(2) . ? Cl25 O27 1.431(2) . ? Cl25 O26 1.452(2) . ? Cl25 O28 1.448(2) . ? O30 C31 1.429(4) . ? O30 H30 0.9451 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O32 C33 1.431(4) . ? O32 H32 0.8731 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N4 180.0 2 . ? N3 Ag2 N3 180.0 . 2_556 ? C11 N3 C10 118.9(2) . . ? C11 N3 Ag2 115.07(16) . . ? C10 N3 Ag2 123.84(17) . . ? C18 N4 C5 118.5(2) . . ? C18 N4 Ag1 118.30(17) . . ? C5 N4 Ag1 122.42(16) . . ? N4 C5 C10 120.6(2) . . ? N4 C5 C6 120.1(2) . . ? C10 C5 C6 119.3(2) . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 120.2(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N3 C10 C9 120.3(2) . . ? N3 C10 C5 119.7(2) . . ? C9 C10 C5 120.0(2) . . ? N3 C11 C18 121.2(2) . . ? N3 C11 C12 117.3(2) . . ? C18 C11 C12 121.5(2) . . ? C13 C12 C17 120.0(3) . . ? C13 C12 C11 121.1(3) . . ? C17 C12 C11 118.9(2) . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 119.8(3) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? N4 C18 C11 120.9(2) . . ? N4 C18 C19 118.0(2) . . ? C11 C18 C19 121.1(2) . . ? C24 C19 C20 119.9(3) . . ? C24 C19 C18 119.8(2) . . ? C20 C19 C18 120.3(2) . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.2(3) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? O29 Cl25 O27 110.43(15) . . ? O29 Cl25 O26 109.63(14) . . ? O27 Cl25 O26 108.45(14) . . ? O29 Cl25 O28 109.86(17) . . ? O27 Cl25 O28 109.61(16) . . ? O26 Cl25 O28 108.83(14) . . ? C31 O30 H30 105.9 . . ? O30 C31 H31A 109.5 . . ? O30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 O32 H32 107.1 . . ? O32 C33 H33A 109.5 . . ? O32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.072 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.099 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 646202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H28 Ag N4, C F3 O3 S' _chemical_formula_sum 'C41 H28 Ag F3 N4 O3 S' _chemical_formula_weight 821.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2181(2) _cell_length_b 11.6140(1) _cell_length_c 13.7958(2) _cell_angle_alpha 77.7882(5) _cell_angle_beta 81.4908(5) _cell_angle_gamma 76.7651(5) _cell_volume 1700.71(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6030 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.24 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8133 _exptl_absorpt_correction_T_max 0.8998 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16693 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.24 _reflns_number_total 7965 _reflns_number_gt 7012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+1.0692P] 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 7965 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.006 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 0.134901(13) -0.022734(11) 0.175704(10) 0.01645(5) Uani 1 1 d . . . N2 N 0.24235(14) -0.21026(13) 0.19865(11) 0.0139(3) Uani 1 1 d . . . N3 N -0.00655(14) 0.14123(13) 0.13175(11) 0.0150(3) Uani 1 1 d . . . N4 N 0.42460(15) -0.42135(14) 0.23367(12) 0.0174(3) Uani 1 1 d . . . N5 N -0.19408(15) 0.34177(14) 0.08055(12) 0.0178(3) Uani 1 1 d . . . C6 C 0.42383(17) -0.34707(16) 0.14247(14) 0.0165(4) Uani 1 1 d . . . C7 C 0.51412(19) -0.37892(17) 0.06420(15) 0.0215(4) Uani 1 1 d . . . H7 H 0.5753 -0.4505 0.0756 0.026 Uiso 1 1 calc R . . C8 C 0.5129(2) -0.30625(17) -0.02795(15) 0.0236(4) Uani 1 1 d . . . H8 H 0.5728 -0.3286 -0.0807 0.028 Uiso 1 1 calc R . . C9 C 0.42412(19) -0.19866(17) -0.04562(15) 0.0220(4) Uani 1 1 d . . . H9 H 0.4250 -0.1488 -0.1098 0.026 Uiso 1 1 calc R . . C10 C 0.33623(18) -0.16552(16) 0.02956(14) 0.0181(4) Uani 1 1 d . . . H10 H 0.2768 -0.0927 0.0173 0.022 Uiso 1 1 calc R . . C11 C 0.33417(17) -0.23934(15) 0.12469(14) 0.0149(4) Uani 1 1 d . . . C12 C 0.33493(17) -0.39262(15) 0.30348(14) 0.0152(4) Uani 1 1 d . . . C13 C 0.34016(16) -0.47377(16) 0.40273(14) 0.0150(4) Uani 1 1 d . . . C14 C 0.36822(17) -0.59854(16) 0.40723(15) 0.0172(4) Uani 1 1 d . . . H14 H 0.3792 -0.6301 0.3476 0.021 Uiso 1 1 calc R . . C15 C 0.38009(18) -0.67606(16) 0.49809(15) 0.0196(4) Uani 1 1 d . . . H15 H 0.3973 -0.7606 0.5006 0.024 Uiso 1 1 calc R . . C16 C 0.36693(18) -0.63109(18) 0.58563(15) 0.0219(4) Uani 1 1 d . . . H16 H 0.3759 -0.6845 0.6478 0.026 Uiso 1 1 calc R . . C17 C 0.34034(18) -0.50664(18) 0.58154(15) 0.0209(4) Uani 1 1 d . . . H17 H 0.3321 -0.4752 0.6410 0.025 Uiso 1 1 calc R . . C18 C 0.32603(17) -0.42918(17) 0.49081(14) 0.0182(4) Uani 1 1 d . . . H18 H 0.3063 -0.3447 0.4886 0.022 Uiso 1 1 calc R . . C19 C 0.23819(17) -0.28691(15) 0.28447(14) 0.0145(3) Uani 1 1 d . . . C20 C 0.12645(16) -0.26801(16) 0.35749(13) 0.0148(4) Uani 1 1 d . . . C21 C 0.05105(18) -0.35217(17) 0.37498(15) 0.0202(4) Uani 1 1 d . . . H21 H 0.0721 -0.4183 0.3410 0.024 Uiso 1 1 calc R . . C22 C -0.05449(19) -0.33972(18) 0.44172(16) 0.0233(4) Uani 1 1 d . . . H22 H -0.1064 -0.3964 0.4524 0.028 Uiso 1 1 calc R . . C23 C -0.08420(18) -0.24443(17) 0.49290(15) 0.0199(4) Uani 1 1 d . . . H23 H -0.1561 -0.2361 0.5390 0.024 Uiso 1 1 calc R . . C24 C -0.00887(18) -0.16165(17) 0.47661(15) 0.0207(4) Uani 1 1 d . . . H24 H -0.0287 -0.0973 0.5126 0.025 Uiso 1 1 calc R . . C25 C 0.09556(18) -0.17166(16) 0.40814(15) 0.0190(4) Uani 1 1 d . . . H25 H 0.1455 -0.1132 0.3960 0.023 Uiso 1 1 calc R . . C26 C -0.10872(17) 0.16722(16) 0.19797(14) 0.0174(4) Uani 1 1 d . . . C27 C -0.1187(2) 0.09495(18) 0.29319(15) 0.0240(4) Uani 1 1 d . . . H27 H -0.0531 0.0301 0.3130 0.029 Uiso 1 1 calc R . . C28 C -0.2231(2) 0.11822(19) 0.35733(16) 0.0276(5) Uani 1 1 d . . . H28 H -0.2294 0.0698 0.4219 0.033 Uiso 1 1 calc R . . C29 C -0.3211(2) 0.21356(19) 0.32800(16) 0.0259(4) Uani 1 1 d . . . H29 H -0.3938 0.2276 0.3726 0.031 Uiso 1 1 calc R . . C30 C -0.31335(18) 0.28616(18) 0.23646(16) 0.0228(4) Uani 1 1 d . . . H30 H -0.3799 0.3505 0.2178 0.027 Uiso 1 1 calc R . . C31 C -0.20529(17) 0.26507(16) 0.16919(14) 0.0171(4) Uani 1 1 d . . . C32 C 0.00188(17) 0.21394(15) 0.04387(13) 0.0141(3) Uani 1 1 d . . . C33 C 0.10982(17) 0.17875(15) -0.02734(13) 0.0145(3) Uani 1 1 d . . . C34 C 0.22840(18) 0.16231(16) 0.00016(15) 0.0188(4) Uani 1 1 d . . . H34 H 0.2398 0.1721 0.0646 0.023 Uiso 1 1 calc R . . C35 C 0.3296(2) 0.13146(18) -0.06760(17) 0.0274(5) Uani 1 1 d . . . H35 H 0.4105 0.1194 -0.0491 0.033 Uiso 1 1 calc R . . C36 C 0.3133(2) 0.11828(19) -0.16166(18) 0.0325(5) Uani 1 1 d . . . H36 H 0.3830 0.0974 -0.2076 0.039 Uiso 1 1 calc R . . C37 C 0.1959(2) 0.13535(19) -0.18939(17) 0.0318(5) Uani 1 1 d . . . H37 H 0.1853 0.1264 -0.2543 0.038 Uiso 1 1 calc R . . C38 C 0.0937(2) 0.16558(17) -0.12245(15) 0.0218(4) Uani 1 1 d . . . H38 H 0.0131 0.1772 -0.1414 0.026 Uiso 1 1 calc R . . C39 C -0.09207(17) 0.32058(16) 0.02005(14) 0.0157(4) Uani 1 1 d . . . C40 C -0.07938(18) 0.41432(16) -0.07090(14) 0.0167(4) Uani 1 1 d . . . C41 C 0.03394(19) 0.44135(17) -0.11473(15) 0.0196(4) Uani 1 1 d . . . H41 H 0.1077 0.3960 -0.0884 0.024 Uiso 1 1 calc R . . C42 C 0.0396(2) 0.53415(18) -0.19670(15) 0.0249(4) Uani 1 1 d . . . H42 H 0.1171 0.5506 -0.2269 0.030 Uiso 1 1 calc R . . C43 C -0.0676(2) 0.60260(18) -0.23440(15) 0.0276(5) Uani 1 1 d . . . H43 H -0.0636 0.6665 -0.2899 0.033 Uiso 1 1 calc R . . C44 C -0.1807(2) 0.57744(19) -0.19082(16) 0.0282(5) Uani 1 1 d . . . H44 H -0.2543 0.6246 -0.2163 0.034 Uiso 1 1 calc R . . C45 C -0.1867(2) 0.48375(17) -0.11024(15) 0.0218(4) Uani 1 1 d . . . H45 H -0.2644 0.4665 -0.0815 0.026 Uiso 1 1 calc R . . S46 S 0.33893(4) 0.07469(4) 0.27178(3) 0.01662(10) Uani 1 1 d . . . O47 O 0.38375(14) 0.18339(12) 0.26061(12) 0.0276(3) Uani 1 1 d . . . O48 O 0.20897(13) 0.08272(13) 0.30452(12) 0.0273(3) Uani 1 1 d . . . O49 O 0.38214(15) 0.00653(14) 0.19301(11) 0.0296(3) Uani 1 1 d . . . F50 F 0.37587(13) 0.02957(13) 0.45930(9) 0.0347(3) Uani 1 1 d . . . F51 F 0.38396(13) -0.12874(11) 0.39913(10) 0.0342(3) Uani 1 1 d . . . F52 F 0.53487(11) -0.03544(11) 0.36228(9) 0.0273(3) Uani 1 1 d . . . C53 C 0.41178(18) -0.02044(17) 0.37828(14) 0.0183(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01658(8) 0.01209(8) 0.01718(8) -0.00039(5) -0.00090(5) 0.00147(5) N2 0.0138(7) 0.0102(7) 0.0165(8) -0.0015(5) -0.0008(6) -0.0017(5) N3 0.0140(7) 0.0135(7) 0.0155(8) -0.0016(6) -0.0007(6) -0.0004(6) N4 0.0167(8) 0.0145(7) 0.0185(8) -0.0018(6) 0.0010(6) -0.0012(6) N5 0.0164(8) 0.0171(8) 0.0188(8) -0.0035(6) -0.0035(6) -0.0002(6) C6 0.0159(9) 0.0129(8) 0.0199(9) -0.0028(7) -0.0001(7) -0.0023(7) C7 0.0216(10) 0.0157(9) 0.0231(10) -0.0042(7) 0.0055(8) 0.0001(7) C8 0.0272(11) 0.0200(10) 0.0208(10) -0.0062(8) 0.0081(8) -0.0033(8) C9 0.0282(11) 0.0189(9) 0.0168(9) -0.0012(7) 0.0026(8) -0.0055(8) C10 0.0199(10) 0.0131(9) 0.0191(9) -0.0017(7) -0.0004(8) -0.0013(7) C11 0.0149(9) 0.0121(8) 0.0173(9) -0.0029(6) 0.0004(7) -0.0028(7) C12 0.0151(9) 0.0119(8) 0.0178(9) -0.0021(7) -0.0011(7) -0.0024(7) C13 0.0095(8) 0.0137(8) 0.0187(9) 0.0011(7) 0.0000(7) -0.0010(6) C14 0.0131(9) 0.0149(9) 0.0220(10) -0.0021(7) -0.0022(7) -0.0006(7) C15 0.0162(9) 0.0121(9) 0.0278(11) 0.0017(7) -0.0038(8) -0.0016(7) C16 0.0171(10) 0.0221(10) 0.0216(10) 0.0064(7) -0.0035(8) -0.0028(7) C17 0.0201(10) 0.0233(10) 0.0174(9) -0.0013(7) -0.0008(8) -0.0035(8) C18 0.0161(9) 0.0157(9) 0.0214(10) -0.0028(7) -0.0014(7) -0.0015(7) C19 0.0140(9) 0.0119(8) 0.0169(9) -0.0025(6) -0.0009(7) -0.0019(6) C20 0.0118(9) 0.0143(8) 0.0153(9) 0.0003(6) -0.0007(7) 0.0002(6) C21 0.0173(9) 0.0180(9) 0.0259(10) -0.0065(7) 0.0001(8) -0.0037(7) C22 0.0173(10) 0.0210(10) 0.0306(11) -0.0035(8) 0.0027(8) -0.0065(8) C23 0.0143(9) 0.0217(10) 0.0188(10) 0.0006(7) 0.0019(7) -0.0002(7) C24 0.0215(10) 0.0182(9) 0.0208(10) -0.0057(7) 0.0025(8) -0.0021(7) C25 0.0206(10) 0.0124(9) 0.0225(10) -0.0018(7) 0.0011(8) -0.0040(7) C26 0.0168(9) 0.0150(9) 0.0191(9) -0.0044(7) 0.0007(7) -0.0014(7) C27 0.0228(10) 0.0201(10) 0.0221(10) 0.0008(8) 0.0029(8) 0.0021(8) C28 0.0271(11) 0.0271(11) 0.0230(11) -0.0002(8) 0.0057(9) -0.0035(9) C29 0.0209(10) 0.0272(11) 0.0262(11) -0.0062(8) 0.0074(8) -0.0029(8) C30 0.0148(9) 0.0246(10) 0.0265(11) -0.0061(8) 0.0013(8) 0.0004(7) C31 0.0162(9) 0.0152(9) 0.0198(9) -0.0047(7) -0.0011(7) -0.0022(7) C32 0.0143(9) 0.0128(8) 0.0160(9) -0.0030(6) -0.0035(7) -0.0029(7) C33 0.0157(9) 0.0099(8) 0.0159(9) -0.0003(6) -0.0010(7) -0.0010(6) C34 0.0180(9) 0.0149(9) 0.0198(10) 0.0022(7) -0.0024(7) -0.0006(7) C35 0.0168(10) 0.0202(10) 0.0374(13) 0.0037(8) 0.0034(9) -0.0004(8) C36 0.0328(13) 0.0232(11) 0.0325(12) -0.0033(9) 0.0159(10) -0.0014(9) C37 0.0469(15) 0.0258(11) 0.0204(11) -0.0079(8) 0.0068(10) -0.0063(10) C38 0.0257(11) 0.0213(10) 0.0200(10) -0.0067(7) -0.0035(8) -0.0045(8) C39 0.0153(9) 0.0147(9) 0.0176(9) -0.0035(7) -0.0040(7) -0.0018(7) C40 0.0212(10) 0.0131(8) 0.0159(9) -0.0038(7) -0.0041(7) -0.0009(7) C41 0.0238(10) 0.0155(9) 0.0202(10) -0.0022(7) -0.0043(8) -0.0049(7) C42 0.0371(12) 0.0200(10) 0.0194(10) -0.0032(7) -0.0021(9) -0.0107(9) C43 0.0493(14) 0.0153(9) 0.0168(10) -0.0004(7) -0.0069(9) -0.0035(9) C44 0.0376(13) 0.0223(10) 0.0208(10) -0.0044(8) -0.0115(9) 0.0078(9) C45 0.0238(10) 0.0203(10) 0.0197(10) -0.0062(7) -0.0059(8) 0.0035(8) S46 0.0182(2) 0.0136(2) 0.0172(2) 0.00111(16) -0.00545(18) -0.00289(17) O47 0.0305(8) 0.0151(7) 0.0357(9) 0.0017(6) -0.0053(7) -0.0064(6) O48 0.0167(7) 0.0242(7) 0.0385(9) -0.0004(6) -0.0060(6) -0.0021(6) O49 0.0401(9) 0.0340(8) 0.0165(7) -0.0078(6) -0.0068(7) -0.0062(7) F50 0.0347(8) 0.0568(9) 0.0142(6) -0.0109(6) 0.0023(5) -0.0120(6) F51 0.0361(8) 0.0215(6) 0.0408(8) 0.0130(5) -0.0131(6) -0.0083(5) F52 0.0155(6) 0.0378(7) 0.0258(6) -0.0010(5) -0.0058(5) -0.0016(5) C53 0.0188(10) 0.0223(10) 0.0121(9) 0.0009(7) -0.0014(7) -0.0045(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.2171(14) . ? Ag1 N3 2.2191(15) . ? N2 C19 1.324(2) . ? N2 C11 1.375(2) . ? N3 C32 1.327(2) . ? N3 C26 1.374(2) . ? N4 C12 1.322(2) . ? N4 C6 1.367(2) . ? N5 C39 1.320(2) . ? N5 C31 1.360(2) . ? C6 C7 1.415(3) . ? C6 C11 1.416(2) . ? C7 C8 1.369(3) . ? C8 C9 1.409(3) . ? C9 C10 1.374(3) . ? C10 C11 1.408(3) . ? C12 C19 1.446(2) . ? C12 C13 1.490(2) . ? C13 C18 1.393(3) . ? C13 C14 1.401(3) . ? C14 C15 1.384(3) . ? C15 C16 1.390(3) . ? C16 C17 1.398(3) . ? C17 C18 1.385(3) . ? C19 C20 1.493(2) . ? C20 C25 1.394(3) . ? C20 C21 1.395(3) . ? C21 C22 1.388(3) . ? C22 C23 1.388(3) . ? C23 C24 1.383(3) . ? C24 C25 1.391(3) . ? C26 C27 1.406(3) . ? C26 C31 1.413(3) . ? C27 C28 1.371(3) . ? C28 C29 1.408(3) . ? C29 C30 1.365(3) . ? C30 C31 1.421(3) . ? C32 C39 1.444(2) . ? C32 C33 1.480(2) . ? C33 C38 1.395(3) . ? C33 C34 1.397(3) . ? C34 C35 1.390(3) . ? C35 C36 1.381(3) . ? C36 C37 1.385(4) . ? C37 C38 1.390(3) . ? C39 C40 1.490(3) . ? C40 C45 1.399(3) . ? C40 C41 1.398(3) . ? C41 C42 1.392(3) . ? C42 C43 1.385(3) . ? C43 C44 1.388(3) . ? C44 C45 1.387(3) . ? S46 O47 1.4337(15) . ? S46 O49 1.4405(15) . ? S46 O48 1.4487(15) . ? S46 C53 1.8173(19) . ? F50 C53 1.335(2) . ? F51 C53 1.327(2) . ? F52 C53 1.342(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 163.23(6) . . ? C19 N2 C11 118.42(15) . . ? C19 N2 Ag1 123.94(12) . . ? C11 N2 Ag1 116.51(11) . . ? C32 N3 C26 118.57(15) . . ? C32 N3 Ag1 123.07(12) . . ? C26 N3 Ag1 118.35(12) . . ? C12 N4 C6 117.77(16) . . ? C39 N5 C31 118.46(16) . . ? N4 C6 C7 119.28(17) . . ? N4 C6 C11 121.31(16) . . ? C7 C6 C11 119.42(17) . . ? C8 C7 C6 119.78(18) . . ? C7 C8 C9 120.85(18) . . ? C10 C9 C8 120.31(18) . . ? C9 C10 C11 120.07(17) . . ? N2 C11 C10 120.37(16) . . ? N2 C11 C6 120.00(16) . . ? C10 C11 C6 119.56(16) . . ? N4 C12 C19 121.51(16) . . ? N4 C12 C13 116.42(16) . . ? C19 C12 C13 122.06(16) . . ? C18 C13 C14 118.97(17) . . ? C18 C13 C12 121.81(16) . . ? C14 C13 C12 119.08(17) . . ? C15 C14 C13 120.32(18) . . ? C14 C15 C16 120.45(18) . . ? C15 C16 C17 119.51(18) . . ? C18 C17 C16 119.97(19) . . ? C17 C18 C13 120.75(18) . . ? N2 C19 C12 120.65(16) . . ? N2 C19 C20 118.65(15) . . ? C12 C19 C20 120.48(15) . . ? C25 C20 C21 119.52(17) . . ? C25 C20 C19 123.07(16) . . ? C21 C20 C19 117.41(16) . . ? C22 C21 C20 120.36(18) . . ? C23 C22 C21 119.96(18) . . ? C24 C23 C22 119.82(18) . . ? C23 C24 C25 120.70(18) . . ? C20 C25 C24 119.62(17) . . ? N3 C26 C27 120.19(17) . . ? N3 C26 C31 119.78(17) . . ? C27 C26 C31 120.01(17) . . ? C28 C27 C26 119.91(19) . . ? C27 C28 C29 120.32(19) . . ? C30 C29 C28 121.03(19) . . ? C29 C30 C31 119.72(19) . . ? N5 C31 C26 121.13(17) . . ? N5 C31 C30 119.84(17) . . ? C26 C31 C30 118.97(17) . . ? N3 C32 C39 120.61(16) . . ? N3 C32 C33 116.76(15) . . ? C39 C32 C33 122.62(16) . . ? C38 C33 C34 120.05(17) . . ? C38 C33 C32 120.36(17) . . ? C34 C33 C32 119.56(17) . . ? C35 C34 C33 119.42(19) . . ? C36 C35 C34 120.4(2) . . ? C37 C36 C35 120.3(2) . . ? C36 C37 C38 120.1(2) . . ? C37 C38 C33 119.7(2) . . ? N5 C39 C32 120.93(16) . . ? N5 C39 C40 116.02(16) . . ? C32 C39 C40 123.03(16) . . ? C45 C40 C41 118.52(18) . . ? C45 C40 C39 118.26(18) . . ? C41 C40 C39 123.08(17) . . ? C42 C41 C40 120.53(19) . . ? C43 C42 C41 120.3(2) . . ? C42 C43 C44 119.71(19) . . ? C45 C44 C43 120.3(2) . . ? C44 C45 C40 120.7(2) . . ? O47 S46 O49 115.69(10) . . ? O47 S46 O48 116.02(9) . . ? O49 S46 O48 113.35(10) . . ? O47 S46 C53 102.92(9) . . ? O49 S46 C53 103.58(9) . . ? O48 S46 C53 102.81(9) . . ? F51 C53 F50 107.73(15) . . ? F51 C53 F52 107.76(16) . . ? F50 C53 F52 107.24(16) . . ? F51 C53 S46 112.15(14) . . ? F50 C53 S46 110.47(14) . . ? F52 C53 S46 111.29(12) . . ? 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 N3 Ag1 N2 C19 -102.2(2) . . . . ? N3 Ag1 N2 C11 90.2(2) . . . . ? N2 Ag1 N3 C32 -88.6(2) . . . . ? N2 Ag1 N3 C26 90.1(2) . . . . ? C12 N4 C6 C7 -176.19(18) . . . . ? C12 N4 C6 C11 3.5(3) . . . . ? N4 C6 C7 C8 178.87(19) . . . . ? C11 C6 C7 C8 -0.8(3) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C8 C9 C10 C11 -0.3(3) . . . . ? C19 N2 C11 C10 174.72(17) . . . . ? Ag1 N2 C11 C10 -17.0(2) . . . . ? C19 N2 C11 C6 -2.2(3) . . . . ? Ag1 N2 C11 C6 166.15(13) . . . . ? C9 C10 C11 N2 -176.29(18) . . . . ? C9 C10 C11 C6 0.6(3) . . . . ? N4 C6 C11 N2 -2.8(3) . . . . ? C7 C6 C11 N2 176.84(18) . . . . ? N4 C6 C11 C10 -179.73(18) . . . . ? C7 C6 C11 C10 -0.1(3) . . . . ? C6 N4 C12 C19 0.6(3) . . . . ? C6 N4 C12 C13 -178.55(16) . . . . ? N4 C12 C13 C18 131.43(19) . . . . ? C19 C12 C13 C18 -47.7(3) . . . . ? N4 C12 C13 C14 -44.2(2) . . . . ? C19 C12 C13 C14 136.68(19) . . . . ? C18 C13 C14 C15 0.8(3) . . . . ? C12 C13 C14 C15 176.59(17) . . . . ? C13 C14 C15 C16 -1.4(3) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C15 C16 C17 C18 0.7(3) . . . . ? C16 C17 C18 C13 -1.2(3) . . . . ? C14 C13 C18 C17 0.5(3) . . . . ? C12 C13 C18 C17 -175.16(18) . . . . ? C11 N2 C19 C12 6.2(3) . . . . ? Ag1 N2 C19 C12 -161.23(13) . . . . ? C11 N2 C19 C20 -168.47(16) . . . . ? Ag1 N2 C19 C20 24.1(2) . . . . ? N4 C12 C19 N2 -5.6(3) . . . . ? C13 C12 C19 N2 173.45(17) . . . . ? N4 C12 C19 C20 168.94(17) . . . . ? C13 C12 C19 C20 -12.0(3) . . . . ? N2 C19 C20 C25 -68.7(2) . . . . ? C12 C19 C20 C25 116.7(2) . . . . ? N2 C19 C20 C21 111.6(2) . . . . ? C12 C19 C20 C21 -63.0(2) . . . . ? C25 C20 C21 C22 0.5(3) . . . . ? C19 C20 C21 C22 -179.78(18) . . . . ? C20 C21 C22 C23 -1.2(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C22 C23 C24 C25 1.1(3) . . . . ? C21 C20 C25 C24 1.0(3) . . . . ? C19 C20 C25 C24 -178.69(18) . . . . ? C23 C24 C25 C20 -1.8(3) . . . . ? C32 N3 C26 C27 -177.54(18) . . . . ? Ag1 N3 C26 C27 3.7(2) . . . . ? C32 N3 C26 C31 4.1(3) . . . . ? Ag1 N3 C26 C31 -174.69(13) . . . . ? N3 C26 C27 C28 -177.20(19) . . . . ? C31 C26 C27 C28 1.2(3) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C28 C29 C30 C31 0.4(3) . . . . ? C39 N5 C31 C26 2.2(3) . . . . ? C39 N5 C31 C30 179.29(18) . . . . ? N3 C26 C31 N5 -6.6(3) . . . . ? C27 C26 C31 N5 174.96(18) . . . . ? N3 C26 C31 C30 176.25(18) . . . . ? C27 C26 C31 C30 -2.2(3) . . . . ? C29 C30 C31 N5 -175.82(19) . . . . ? C29 C30 C31 C26 1.3(3) . . . . ? C26 N3 C32 C39 2.4(3) . . . . ? Ag1 N3 C32 C39 -178.93(12) . . . . ? C26 N3 C32 C33 -176.56(16) . . . . ? Ag1 N3 C32 C33 2.1(2) . . . . ? N3 C32 C33 C38 124.29(19) . . . . ? C39 C32 C33 C38 -54.6(2) . . . . ? N3 C32 C33 C34 -57.6(2) . . . . ? C39 C32 C33 C34 123.43(19) . . . . ? C38 C33 C34 C35 -0.7(3) . . . . ? C32 C33 C34 C35 -178.80(17) . . . . ? C33 C34 C35 C36 0.6(3) . . . . ? C34 C35 C36 C37 -0.2(3) . . . . ? C35 C36 C37 C38 -0.2(3) . . . . ? C36 C37 C38 C33 0.1(3) . . . . ? C34 C33 C38 C37 0.4(3) . . . . ? C32 C33 C38 C37 178.44(18) . . . . ? C31 N5 C39 C32 4.4(3) . . . . ? C31 N5 C39 C40 -173.83(16) . . . . ? N3 C32 C39 N5 -6.9(3) . . . . ? C33 C32 C39 N5 171.96(17) . . . . ? N3 C32 C39 C40 171.14(17) . . . . ? C33 C32 C39 C40 -10.0(3) . . . . ? N5 C39 C40 C45 -28.5(3) . . . . ? C32 C39 C40 C45 153.34(18) . . . . ? N5 C39 C40 C41 147.17(18) . . . . ? C32 C39 C40 C41 -31.0(3) . . . . ? C45 C40 C41 C42 -1.0(3) . . . . ? C39 C40 C41 C42 -176.67(17) . . . . ? C40 C41 C42 C43 1.4(3) . . . . ? C41 C42 C43 C44 -0.7(3) . . . . ? C42 C43 C44 C45 -0.4(3) . . . . ? C43 C44 C45 C40 0.8(3) . . . . ? C41 C40 C45 C44 -0.1(3) . . . . ? C39 C40 C45 C44 175.76(18) . . . . ? O47 S46 C53 F51 -178.17(13) . . . . ? O49 S46 C53 F51 -57.31(16) . . . . ? O48 S46 C53 F51 60.92(16) . . . . ? O47 S46 C53 F50 61.65(15) . . . . ? O49 S46 C53 F50 -177.49(13) . . . . ? O48 S46 C53 F50 -59.26(15) . . . . ? O47 S46 C53 F52 -57.37(15) . . . . ? O49 S46 C53 F52 63.50(15) . . . . ? O48 S46 C53 F52 -178.27(13) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.511 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.071 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 646203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H16 Ag N2 O), 2(B F4), C2 O' _chemical_formula_sum 'C42 H32 Ag2 B2 F8 N4 O3' _chemical_formula_weight 1030.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' 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 13.7290(2) _cell_length_b 17.3654(2) _cell_length_c 8.5825(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2046.15(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2559 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.85 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7812 _exptl_absorpt_correction_T_max 0.8598 _exptl_absorpt_process_details 'Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KappaCCD' _diffrn_measurement_method '1 deg. Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12132 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.85 _reflns_number_total 4769 _reflns_number_gt 4534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains molecules of ethanol as crystallization solvent, located on and disordered about the twofold axes. ; _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^)+(0.0446P)^2^+1.0606P] 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 -0.03(2) _refine_ls_number_reflns 4769 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.155454(15) 0.702722(13) 0.06934(3) 0.02234(7) Uani 1 1 d . . . N2 N 0.00672(17) 0.74294(14) 0.0101(3) 0.0172(5) Uani 1 1 d . . . N3 N -0.18710(16) 0.78411(13) -0.0478(3) 0.0163(5) Uani 1 1 d . . . C4 C -0.0402(2) 0.71478(16) -0.1195(3) 0.0168(5) Uani 1 1 d . . . C5 C 0.0081(2) 0.66482(18) -0.2229(4) 0.0209(6) Uani 1 1 d . . . H5 H 0.0734 0.6498 -0.2032 0.025 Uiso 1 1 calc R . . C6 C -0.0396(2) 0.63784(17) -0.3523(4) 0.0226(6) Uani 1 1 d . . . H6 H -0.0071 0.6038 -0.4216 0.027 Uiso 1 1 calc R . . C7 C -0.1367(2) 0.66023(17) -0.3836(3) 0.0210(6) Uani 1 1 d . . . H7 H -0.1688 0.6416 -0.4741 0.025 Uiso 1 1 calc R . . C8 C -0.1845(2) 0.70865(18) -0.2835(3) 0.0201(5) Uani 1 1 d . . . H8 H -0.2499 0.7231 -0.3045 0.024 Uiso 1 1 calc R . . C9 C -0.13763(19) 0.73693(16) -0.1507(3) 0.0165(6) Uani 1 1 d . . . C10 C -0.14060(19) 0.81019(14) 0.0766(3) 0.0164(5) Uani 1 1 d . . . C11 C -0.1969(2) 0.86012(16) 0.1852(4) 0.0173(6) Uani 1 1 d . . . C12 C -0.2433(2) 0.92536(17) 0.1278(4) 0.0213(6) Uani 1 1 d . . . H12 H -0.2390 0.9376 0.0202 0.026 Uiso 1 1 calc R . . C13 C -0.2966(2) 0.97320(17) 0.2280(4) 0.0238(6) Uani 1 1 d . . . H13 H -0.3271 1.0184 0.1893 0.029 Uiso 1 1 calc R . . C14 C -0.3041(2) 0.95368(18) 0.3848(4) 0.0243(6) Uani 1 1 d . . . H14 H -0.3408 0.9854 0.4534 0.029 Uiso 1 1 calc R . . C15 C -0.2584(2) 0.88829(17) 0.4416(4) 0.0225(6) Uani 1 1 d . . . H15 H -0.2643 0.8752 0.5486 0.027 Uiso 1 1 calc R . . C16 C -0.2038(2) 0.84161(17) 0.3428(4) 0.0205(6) Uani 1 1 d . . . H16 H -0.1714 0.7974 0.3826 0.025 Uiso 1 1 calc R . . C17 C -0.0408(2) 0.78926(16) 0.1061(3) 0.0165(5) Uani 1 1 d . . . C18 C 0.0139(2) 0.81974(16) 0.2422(3) 0.0171(6) Uani 1 1 d . . . C19 C 0.0429(2) 0.77121(17) 0.3624(4) 0.0214(6) Uani 1 1 d . . . H19 H 0.0280 0.7178 0.3577 0.026 Uiso 1 1 calc R . . C20 C 0.0937(2) 0.8006(2) 0.4894(4) 0.0258(6) Uani 1 1 d . . . H20 H 0.1122 0.7677 0.5727 0.031 Uiso 1 1 calc R . . C21 C 0.1175(2) 0.8793(2) 0.4938(4) 0.0271(7) Uani 1 1 d . . . H21 H 0.1530 0.8996 0.5795 0.033 Uiso 1 1 calc R . . C22 C 0.0892(2) 0.92700(19) 0.3734(4) 0.0276(7) Uani 1 1 d . . . H22 H 0.1060 0.9800 0.3765 0.033 Uiso 1 1 calc R . . C23 C 0.0367(2) 0.89881(18) 0.2482(4) 0.0236(6) Uani 1 1 d . . . H23 H 0.0162 0.9324 0.1672 0.028 Uiso 1 1 calc R . . B24 B -0.6899(3) 0.9065(2) 0.8400(4) 0.0286(8) Uani 1 1 d . . . F25 F -0.70959(19) 0.96737(12) 0.7402(3) 0.0446(6) Uani 1 1 d . . . F26 F -0.60533(16) 0.92484(13) 0.9245(3) 0.0409(5) Uani 1 1 d . . . F27 F -0.6733(2) 0.84004(12) 0.7563(3) 0.0498(7) Uani 1 1 d . . . F28 F -0.76639(19) 0.89668(15) 0.9407(3) 0.0552(6) Uani 1 1 d . . . O29 O 0.08224(19) 0.59452(13) 0.2139(3) 0.0334(5) Uani 1 1 d . . . H29A H 0.0187 0.5797 0.1611 0.042(12) Uiso 1 1 d R . . H29B H 0.1167 0.5522 0.2090 0.050(14) Uiso 1 1 d R . . C30 C -0.0314(5) 0.9655(5) 0.7800(6) 0.107(4) Uani 1 1 d . . . O31 O -0.0736(5) 0.9767(5) 0.9239(9) 0.075(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01148(11) 0.02943(11) 0.02610(12) -0.00590(10) -0.00013(8) 0.00019(9) N2 0.0128(11) 0.0188(11) 0.0201(12) -0.0020(9) -0.0006(9) 0.0012(9) N3 0.0117(10) 0.0177(11) 0.0195(12) -0.0009(9) 0.0000(9) 0.0002(8) C4 0.0137(13) 0.0196(13) 0.0171(13) 0.0003(10) -0.0003(10) -0.0025(11) C5 0.0128(13) 0.0254(14) 0.0245(15) -0.0028(12) 0.0034(11) 0.0010(11) C6 0.0215(14) 0.0228(14) 0.0237(15) -0.0041(12) 0.0025(12) 0.0002(12) C7 0.0215(16) 0.0232(14) 0.0184(14) 0.0007(11) -0.0001(10) -0.0017(11) C8 0.0151(12) 0.0251(14) 0.0200(14) -0.0017(13) -0.0017(10) -0.0002(11) C9 0.0101(13) 0.0192(12) 0.0201(14) 0.0004(11) 0.0015(10) -0.0003(10) C10 0.0135(13) 0.0177(12) 0.0180(13) 0.0023(11) 0.0022(11) 0.0004(9) C11 0.0129(13) 0.0183(13) 0.0208(15) -0.0052(11) -0.0001(11) -0.0006(10) C12 0.0206(15) 0.0211(14) 0.0224(15) -0.0022(11) -0.0021(11) 0.0003(11) C13 0.0233(15) 0.0186(13) 0.0294(17) -0.0034(12) -0.0021(12) 0.0063(11) C14 0.0195(14) 0.0244(14) 0.0289(17) -0.0091(12) 0.0011(12) 0.0001(12) C15 0.0187(14) 0.0277(14) 0.0211(15) -0.0025(13) 0.0019(12) -0.0031(11) C16 0.0164(14) 0.0229(14) 0.0221(15) -0.0013(12) 0.0022(11) 0.0012(11) C17 0.0150(13) 0.0146(12) 0.0198(13) 0.0008(10) 0.0007(10) -0.0017(11) C18 0.0112(13) 0.0221(14) 0.0179(14) 0.0001(10) 0.0004(10) -0.0018(10) C19 0.0198(15) 0.0235(14) 0.0209(14) -0.0005(11) 0.0033(11) 0.0010(11) C20 0.0204(15) 0.0356(16) 0.0213(14) 0.0017(14) -0.0008(11) 0.0032(14) C21 0.0173(14) 0.0377(18) 0.0263(16) -0.0134(14) 0.0011(12) -0.0004(13) C22 0.0216(15) 0.0262(16) 0.0351(18) -0.0105(13) -0.0021(13) -0.0027(13) C23 0.0209(14) 0.0205(13) 0.0293(16) -0.0021(12) -0.0015(11) -0.0056(12) B24 0.038(2) 0.0249(17) 0.0231(19) 0.0035(14) -0.0030(15) 0.0051(15) F25 0.0585(15) 0.0284(10) 0.0468(14) 0.0103(10) -0.0250(11) -0.0020(10) F26 0.0398(12) 0.0486(12) 0.0343(11) 0.0006(11) -0.0130(10) 0.0104(10) F27 0.091(2) 0.0289(11) 0.0299(11) -0.0052(9) 0.0004(12) 0.0091(12) F28 0.0511(14) 0.0570(15) 0.0576(16) -0.0024(14) 0.0173(13) -0.0099(12) O29 0.0333(13) 0.0226(11) 0.0444(15) 0.0015(11) 0.0037(12) 0.0000(10) C30 0.117(7) 0.167(9) 0.038(3) 0.018(3) 0.022(3) 0.095(6) O31 0.056(4) 0.112(6) 0.056(4) 0.025(5) 0.015(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.182(2) 3_565 ? Ag1 N2 2.217(2) . ? Ag1 O29 2.466(2) . ? N2 C17 1.323(4) . ? N2 C4 1.375(4) . ? N3 C10 1.324(4) . ? N3 C9 1.383(4) . ? N3 Ag1 2.182(2) 3_465 ? C4 C5 1.407(4) . ? C4 C9 1.418(4) . ? C5 C6 1.372(4) . ? C5 H5 0.9500 . ? C6 C7 1.414(4) . ? C6 H6 0.9500 . ? C7 C8 1.369(4) . ? C7 H7 0.9500 . ? C8 C9 1.398(4) . ? C8 H8 0.9500 . ? C10 C17 1.440(4) . ? C10 C11 1.489(4) . ? C11 C12 1.390(4) . ? C11 C16 1.394(4) . ? C12 C13 1.401(4) . ? C12 H12 0.9500 . ? C13 C14 1.392(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.486(4) . ? C18 C19 1.390(4) . ? C18 C23 1.409(4) . ? C19 C20 1.392(4) . ? C19 H19 0.9500 . ? C20 C21 1.404(5) . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 C23 1.383(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? B24 F28 1.370(5) . ? B24 F27 1.379(4) . ? B24 F25 1.387(4) . ? B24 F26 1.405(5) . ? O29 H29A 1.0161 . ? O29 H29B 0.8757 . ? C30 O31 1.378(9) . ? C30 C30 1.478(18) 2_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N2 149.32(10) 3_565 . ? N3 Ag1 O29 121.77(9) 3_565 . ? N2 Ag1 O29 88.86(9) . . ? C17 N2 C4 119.3(2) . . ? C17 N2 Ag1 120.17(19) . . ? C4 N2 Ag1 120.32(19) . . ? C10 N3 C9 118.7(2) . . ? C10 N3 Ag1 120.69(18) . 3_465 ? C9 N3 Ag1 119.64(18) . 3_465 ? N2 C4 C5 120.6(3) . . ? N2 C4 C9 119.9(3) . . ? C5 C4 C9 119.5(3) . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.5(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N3 C9 C8 120.2(3) . . ? N3 C9 C4 120.2(3) . . ? C8 C9 C4 119.5(3) . . ? N3 C10 C17 120.9(2) . . ? N3 C10 C11 117.0(2) . . ? C17 C10 C11 122.1(3) . . ? C12 C11 C16 120.0(3) . . ? C12 C11 C10 119.4(3) . . ? C16 C11 C10 120.6(3) . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.2(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 119.5(3) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? N2 C17 C10 120.9(3) . . ? N2 C17 C18 117.2(2) . . ? C10 C17 C18 121.9(2) . . ? C19 C18 C23 120.0(3) . . ? C19 C18 C17 120.8(3) . . ? C23 C18 C17 119.2(3) . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.6(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 119.9(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.0(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 119.3(3) . . ? C22 C23 H23 120.4 . . ? C18 C23 H23 120.4 . . ? F28 B24 F27 110.6(3) . . ? F28 B24 F25 109.6(3) . . ? F27 B24 F25 110.4(3) . . ? F28 B24 F26 109.6(3) . . ? F27 B24 F26 108.7(3) . . ? F25 B24 F26 107.9(3) . . ? Ag1 O29 H29A 108.6 . . ? Ag1 O29 H29B 113.3 . . ? H29A O29 H29B 103.3 . . ? O31 C30 C30 97.5(6) . 2_575 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.788 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.083 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 646204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H28 Ag F3 N4 O2' _chemical_formula_sum 'C42 H28 Ag F3 N4 O2' _chemical_formula_weight 785.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.1133(3) _cell_length_b 12.2933(2) _cell_length_c 13.1444(3) _cell_angle_alpha 74.5910(14) _cell_angle_beta 83.1028(11) _cell_angle_gamma 74.0146(12) _cell_volume 1662.15(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5418 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8506 _exptl_absorpt_correction_T_max 0.8778 _exptl_absorpt_process_details 'Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scan' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13543 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7127 _reflns_number_gt 6413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius V.B.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.6944P] 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 7127 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.859977(15) 0.537033(13) 0.314748(13) 0.01850(6) Uani 1 1 d . . . N2 N 1.00890(16) 0.37130(15) 0.36267(14) 0.0170(4) Uani 1 1 d . . . N3 N 0.76420(16) 0.72626(14) 0.30365(14) 0.0158(4) Uani 1 1 d . . . N4 N 1.18926(17) 0.15800(15) 0.41526(14) 0.0177(4) Uani 1 1 d . . . N5 N 0.57702(17) 0.93780(15) 0.26643(14) 0.0176(4) Uani 1 1 d . . . C6 C 1.2011(2) 0.23799(18) 0.32272(17) 0.0172(4) Uani 1 1 d . . . C7 C 1.3049(2) 0.21206(19) 0.25122(18) 0.0205(4) Uani 1 1 d . . . H7 H 1.3680 0.1411 0.2693 0.025 Uiso 1 1 calc R . . C8 C 1.3136(2) 0.2898(2) 0.15607(18) 0.0230(5) Uani 1 1 d . . . H8 H 1.3825 0.2716 0.1079 0.028 Uiso 1 1 calc R . . C9 C 1.2219(2) 0.3963(2) 0.12842(19) 0.0249(5) Uani 1 1 d . . . H9 H 1.2296 0.4492 0.0621 0.030 Uiso 1 1 calc R . . C10 C 1.1219(2) 0.4238(2) 0.19673(18) 0.0240(5) Uani 1 1 d . . . H10 H 1.0608 0.4961 0.1783 0.029 Uiso 1 1 calc R . . C11 C 1.1098(2) 0.34449(18) 0.29463(17) 0.0174(4) Uani 1 1 d . . . C12 C 1.08822(19) 0.18239(18) 0.47784(17) 0.0166(4) Uani 1 1 d . . . C13 C 1.0732(2) 0.08616(18) 0.57127(16) 0.0173(4) Uani 1 1 d . . . C14 C 1.1810(2) 0.00491(19) 0.61442(18) 0.0222(5) Uani 1 1 d . . . H14 H 1.2612 0.0161 0.5881 0.027 Uiso 1 1 calc R . . C15 C 1.1718(2) -0.0919(2) 0.69524(19) 0.0279(5) Uani 1 1 d . . . H15 H 1.2458 -0.1465 0.7237 0.034 Uiso 1 1 calc R . . C16 C 1.0554(2) -0.1095(2) 0.73486(18) 0.0277(5) Uani 1 1 d . . . H16 H 1.0492 -0.1763 0.7897 0.033 Uiso 1 1 calc R . . C17 C 0.9483(2) -0.0286(2) 0.69350(18) 0.0241(5) Uani 1 1 d . . . H17 H 0.8683 -0.0392 0.7213 0.029 Uiso 1 1 calc R . . C18 C 0.9566(2) 0.06808(19) 0.61187(18) 0.0207(4) Uani 1 1 d . . . H18 H 0.8823 0.1222 0.5836 0.025 Uiso 1 1 calc R . . C19 C 0.99680(19) 0.29368(18) 0.45216(16) 0.0156(4) Uani 1 1 d . . . C20 C 0.88409(19) 0.32769(17) 0.52126(16) 0.0155(4) Uani 1 1 d . . . C21 C 0.8935(2) 0.33653(19) 0.62320(17) 0.0215(5) Uani 1 1 d . . . H21 H 0.9736 0.3221 0.6500 0.026 Uiso 1 1 calc R . . C22 C 0.7858(2) 0.3665(2) 0.68575(19) 0.0276(5) Uani 1 1 d . . . H22 H 0.7921 0.3732 0.7552 0.033 Uiso 1 1 calc R . . C23 C 0.6687(2) 0.38672(19) 0.6470(2) 0.0279(5) Uani 1 1 d . . . H23 H 0.5951 0.4064 0.6902 0.033 Uiso 1 1 calc R . . C24 C 0.6590(2) 0.37832(19) 0.5458(2) 0.0259(5) Uani 1 1 d . . . H24 H 0.5787 0.3927 0.5194 0.031 Uiso 1 1 calc R . . C25 C 0.7662(2) 0.34896(18) 0.48258(18) 0.0199(4) Uani 1 1 d . . . H25 H 0.7593 0.3434 0.4129 0.024 Uiso 1 1 calc R . . C26 C 0.67298(19) 0.75054(18) 0.38085(16) 0.0155(4) Uani 1 1 d . . . C27 C 0.6743(2) 0.67019(18) 0.47991(17) 0.0191(4) Uani 1 1 d . . . H27 H 0.7353 0.5973 0.4923 0.023 Uiso 1 1 calc R . . C28 C 0.5874(2) 0.69771(19) 0.55811(18) 0.0221(5) Uani 1 1 d . . . H28 H 0.5890 0.6442 0.6253 0.026 Uiso 1 1 calc R . . C29 C 0.4955(2) 0.80495(19) 0.53974(18) 0.0237(5) Uani 1 1 d . . . H29 H 0.4355 0.8225 0.5948 0.028 Uiso 1 1 calc R . . C30 C 0.4912(2) 0.88411(19) 0.44397(17) 0.0211(5) Uani 1 1 d . . . H30 H 0.4281 0.9556 0.4324 0.025 Uiso 1 1 calc R . . C31 C 0.5816(2) 0.85857(18) 0.36219(17) 0.0168(4) Uani 1 1 d . . . C32 C 0.76408(19) 0.80678(17) 0.21358(16) 0.0154(4) Uani 1 1 d . . . C33 C 0.87513(19) 0.78732(18) 0.13868(16) 0.0170(4) Uani 1 1 d . . . C34 C 0.9007(2) 0.70019(18) 0.08421(17) 0.0207(4) Uani 1 1 d . . . H34 H 0.8453 0.6514 0.0926 0.025 Uiso 1 1 calc R . . C35 C 1.0076(2) 0.6847(2) 0.01735(18) 0.0252(5) Uani 1 1 d . . . H35 H 1.0245 0.6261 -0.0209 0.030 Uiso 1 1 calc R . . C36 C 1.0895(2) 0.7544(2) 0.00632(18) 0.0265(5) Uani 1 1 d . . . H36 H 1.1634 0.7422 -0.0382 0.032 Uiso 1 1 calc R . . C37 C 1.0643(2) 0.8418(2) 0.05999(19) 0.0279(5) Uani 1 1 d . . . H37 H 1.1205 0.8896 0.0521 0.033 Uiso 1 1 calc R . . C38 C 0.9564(2) 0.85915(19) 0.12531(18) 0.0217(5) Uani 1 1 d . . . H38 H 0.9379 0.9201 0.1610 0.026 Uiso 1 1 calc R . . C39 C 0.66472(19) 0.91247(18) 0.19317(16) 0.0161(4) Uani 1 1 d . . . C40 C 0.65291(19) 0.99562(18) 0.08719(16) 0.0162(4) Uani 1 1 d . . . C41 C 0.66841(19) 0.95598(19) -0.00495(17) 0.0190(4) Uani 1 1 d . . . H41 H 0.6941 0.8746 -0.0008 0.023 Uiso 1 1 calc R . . C42 C 0.6466(2) 1.0347(2) -0.10245(18) 0.0224(5) Uani 1 1 d . . . H42 H 0.6556 1.0070 -0.1646 0.027 Uiso 1 1 calc R . . C43 C 0.6116(2) 1.1536(2) -0.10950(18) 0.0238(5) Uani 1 1 d . . . H43 H 0.5968 1.2074 -0.1763 0.029 Uiso 1 1 calc R . . C44 C 0.5982(2) 1.19373(19) -0.01857(18) 0.0221(5) Uani 1 1 d . . . H44 H 0.5757 1.2752 -0.0234 0.027 Uiso 1 1 calc R . . C45 C 0.6176(2) 1.11537(18) 0.07938(18) 0.0195(4) Uani 1 1 d . . . H45 H 0.6068 1.1435 0.1414 0.023 Uiso 1 1 calc R . . O46 O 0.64385(18) 0.53817(17) 0.26704(15) 0.0385(4) Uani 1 1 d . . . O47 O 0.79691(17) 0.45035(18) 0.16849(17) 0.0414(5) Uani 1 1 d . . . C48 C 0.6871(2) 0.48192(19) 0.20025(18) 0.0226(5) Uani 1 1 d . . . C49 C 0.5916(2) 0.44031(19) 0.15426(17) 0.0193(4) Uani 1 1 d . . . F50 F 0.47514(13) 0.50788(13) 0.15513(12) 0.0314(3) Uani 1 1 d . . . F51 F 0.62195(14) 0.43175(15) 0.05487(11) 0.0388(4) Uani 1 1 d . . . F52 F 0.58506(15) 0.33335(12) 0.21102(12) 0.0361(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01710(9) 0.01474(9) 0.02105(9) -0.00513(6) -0.00066(6) 0.00080(6) N2 0.0152(9) 0.0155(8) 0.0185(9) -0.0050(7) -0.0001(7) -0.0008(7) N3 0.0146(9) 0.0128(8) 0.0196(9) -0.0051(7) -0.0003(7) -0.0019(7) N4 0.0172(9) 0.0160(9) 0.0198(9) -0.0058(7) -0.0014(7) -0.0027(7) N5 0.0181(9) 0.0161(9) 0.0188(9) -0.0065(7) 0.0003(7) -0.0030(7) C6 0.0156(10) 0.0174(10) 0.0200(11) -0.0069(8) -0.0007(8) -0.0042(8) C7 0.0157(11) 0.0186(10) 0.0267(12) -0.0087(9) 0.0008(9) -0.0013(8) C8 0.0190(11) 0.0243(11) 0.0240(12) -0.0075(9) 0.0053(9) -0.0038(9) C9 0.0239(12) 0.0240(11) 0.0227(12) -0.0016(9) 0.0025(9) -0.0050(9) C10 0.0227(12) 0.0192(11) 0.0242(12) -0.0017(9) 0.0033(9) -0.0012(9) C11 0.0151(10) 0.0164(10) 0.0199(11) -0.0053(8) 0.0001(8) -0.0022(8) C12 0.0145(10) 0.0162(10) 0.0197(11) -0.0063(8) -0.0018(8) -0.0024(8) C13 0.0206(11) 0.0149(10) 0.0179(10) -0.0064(8) -0.0007(8) -0.0047(8) C14 0.0224(12) 0.0222(11) 0.0200(11) -0.0047(9) -0.0020(9) -0.0023(9) C15 0.0304(13) 0.0257(12) 0.0228(12) -0.0018(9) -0.0076(10) -0.0006(10) C16 0.0417(15) 0.0214(11) 0.0202(12) -0.0018(9) -0.0015(10) -0.0114(10) C17 0.0283(13) 0.0248(12) 0.0231(12) -0.0078(9) 0.0032(9) -0.0129(10) C18 0.0213(11) 0.0177(10) 0.0241(11) -0.0067(9) -0.0003(9) -0.0054(9) C19 0.0141(10) 0.0170(10) 0.0168(10) -0.0060(8) -0.0014(8) -0.0035(8) C20 0.0167(10) 0.0123(9) 0.0157(10) -0.0020(8) 0.0011(8) -0.0031(8) C21 0.0235(12) 0.0205(11) 0.0211(11) -0.0063(9) -0.0021(9) -0.0051(9) C22 0.0398(15) 0.0225(12) 0.0202(12) -0.0089(9) 0.0077(10) -0.0076(10) C23 0.0261(13) 0.0175(11) 0.0367(14) -0.0084(10) 0.0142(10) -0.0051(9) C24 0.0186(12) 0.0188(11) 0.0374(14) -0.0044(10) 0.0015(10) -0.0036(9) C25 0.0194(11) 0.0168(10) 0.0220(11) -0.0042(8) -0.0013(9) -0.0023(8) C26 0.0158(10) 0.0150(10) 0.0170(10) -0.0055(8) -0.0010(8) -0.0046(8) C27 0.0217(11) 0.0133(10) 0.0216(11) -0.0038(8) -0.0002(9) -0.0039(8) C28 0.0271(12) 0.0195(11) 0.0186(11) -0.0038(9) 0.0015(9) -0.0061(9) C29 0.0257(12) 0.0216(11) 0.0220(11) -0.0080(9) 0.0077(9) -0.0045(9) C30 0.0210(11) 0.0190(10) 0.0219(11) -0.0072(9) 0.0024(9) -0.0020(9) C31 0.0166(10) 0.0151(10) 0.0187(10) -0.0051(8) -0.0008(8) -0.0033(8) C32 0.0158(10) 0.0143(10) 0.0173(10) -0.0049(8) -0.0016(8) -0.0042(8) C33 0.0133(10) 0.0169(10) 0.0160(10) -0.0009(8) -0.0010(8) 0.0012(8) C34 0.0224(11) 0.0164(10) 0.0199(11) -0.0020(8) -0.0007(9) -0.0019(9) C35 0.0267(13) 0.0235(12) 0.0183(11) -0.0053(9) 0.0006(9) 0.0048(9) C36 0.0178(11) 0.0316(13) 0.0204(12) 0.0007(10) 0.0035(9) 0.0011(9) C37 0.0195(12) 0.0323(13) 0.0280(13) -0.0009(10) 0.0014(10) -0.0073(10) C38 0.0183(11) 0.0210(11) 0.0248(12) -0.0064(9) -0.0008(9) -0.0030(9) C39 0.0150(10) 0.0141(10) 0.0199(11) -0.0061(8) -0.0012(8) -0.0030(8) C40 0.0117(10) 0.0160(10) 0.0190(10) -0.0028(8) 0.0009(8) -0.0026(8) C41 0.0148(11) 0.0194(10) 0.0210(11) -0.0065(9) -0.0001(8) -0.0003(8) C42 0.0173(11) 0.0293(12) 0.0190(11) -0.0054(9) 0.0005(9) -0.0043(9) C43 0.0194(11) 0.0255(12) 0.0207(11) 0.0041(9) -0.0005(9) -0.0057(9) C44 0.0197(11) 0.0160(10) 0.0275(12) -0.0013(9) -0.0004(9) -0.0038(8) C45 0.0163(11) 0.0182(10) 0.0228(11) -0.0053(9) 0.0009(8) -0.0026(8) O46 0.0384(11) 0.0481(12) 0.0379(11) -0.0242(9) -0.0058(8) -0.0104(9) O47 0.0193(9) 0.0531(12) 0.0555(13) -0.0187(10) 0.0004(8) -0.0114(8) C48 0.0253(12) 0.0203(11) 0.0210(11) 0.0019(9) -0.0063(9) -0.0084(9) C49 0.0196(11) 0.0194(10) 0.0174(11) -0.0042(8) 0.0003(8) -0.0032(8) F50 0.0196(7) 0.0358(8) 0.0375(8) -0.0144(6) -0.0074(6) 0.0026(6) F51 0.0354(9) 0.0654(11) 0.0232(8) -0.0222(7) 0.0037(6) -0.0162(8) F52 0.0418(9) 0.0222(7) 0.0443(9) 0.0009(6) -0.0099(7) -0.0137(6) _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 N2 2.2356(17) . ? Ag1 N3 2.2491(17) . ? Ag1 O46 2.5496(19) . ? N2 C19 1.322(3) . ? N2 C11 1.370(3) . ? N3 C32 1.326(3) . ? N3 C26 1.376(3) . ? N4 C12 1.323(3) . ? N4 C6 1.364(3) . ? N5 C39 1.320(3) . ? N5 C31 1.368(3) . ? C6 C11 1.408(3) . ? C6 C7 1.418(3) . ? C7 C8 1.369(3) . ? C7 H7 0.9500 . ? C8 C9 1.409(3) . ? C8 H8 0.9500 . ? C9 C10 1.367(3) . ? C9 H9 0.9500 . ? C10 C11 1.410(3) . ? C10 H10 0.9500 . ? C12 C19 1.445(3) . ? C12 C13 1.491(3) . ? C13 C18 1.394(3) . ? C13 C14 1.399(3) . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.486(3) . ? C20 C21 1.391(3) . ? C20 C25 1.394(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C24 C25 1.388(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.409(3) . ? C26 C31 1.414(3) . ? C27 C28 1.368(3) . ? C27 H27 0.9500 . ? C28 C29 1.410(3) . ? C28 H28 0.9500 . ? C29 C30 1.368(3) . ? C29 H29 0.9500 . ? C30 C31 1.418(3) . ? C30 H30 0.9500 . ? C32 C39 1.440(3) . ? C32 C33 1.490(3) . ? C33 C34 1.390(3) . ? C33 C38 1.394(3) . ? C34 C35 1.391(3) . ? C34 H34 0.9500 . ? C35 C36 1.384(4) . ? C35 H35 0.9500 . ? C36 C37 1.385(4) . ? C36 H36 0.9500 . ? C37 C38 1.389(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.489(3) . ? C40 C45 1.394(3) . ? C40 C41 1.397(3) . ? C41 C42 1.387(3) . ? C41 H41 0.9500 . ? C42 C43 1.385(3) . ? C42 H42 0.9500 . ? C43 C44 1.387(3) . ? C43 H43 0.9500 . ? C44 C45 1.388(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? O46 C48 1.232(3) . ? O47 C48 1.232(3) . ? C48 C49 1.539(3) . ? C49 F50 1.332(3) . ? C49 F51 1.334(3) . ? C49 F52 1.345(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 155.53(6) . . ? N2 Ag1 O46 121.86(6) . . ? N3 Ag1 O46 81.25(6) . . ? C19 N2 C11 118.85(18) . . ? C19 N2 Ag1 121.17(14) . . ? C11 N2 Ag1 119.76(13) . . ? C32 N3 C26 118.26(17) . . ? C32 N3 Ag1 121.69(13) . . ? C26 N3 Ag1 116.73(13) . . ? C12 N4 C6 118.15(18) . . ? C39 N5 C31 117.67(18) . . ? N4 C6 C11 121.33(19) . . ? N4 C6 C7 119.62(19) . . ? C11 C6 C7 119.00(19) . . ? C8 C7 C6 119.7(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.3(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N2 C11 C10 119.89(19) . . ? N2 C11 C6 119.92(19) . . ? C10 C11 C6 120.2(2) . . ? N4 C12 C19 120.95(19) . . ? N4 C12 C13 115.59(18) . . ? C19 C12 C13 123.38(18) . . ? C18 C13 C14 118.5(2) . . ? C18 C13 C12 122.78(19) . . ? C14 C13 C12 118.48(19) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.1(2) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.8(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 120.4(2) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? N2 C19 C12 120.66(18) . . ? N2 C19 C20 115.96(18) . . ? C12 C19 C20 123.37(18) . . ? C21 C20 C25 119.7(2) . . ? C21 C20 C19 121.83(19) . . ? C25 C20 C19 118.47(18) . . ? C22 C21 C20 119.9(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.2(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 120.0(2) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? N3 C26 C27 119.97(19) . . ? N3 C26 C31 119.82(18) . . ? C27 C26 C31 120.15(19) . . ? C28 C27 C26 119.6(2) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.5(2) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 121.1(2) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119.5(2) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N5 C31 C26 121.49(19) . . ? N5 C31 C30 119.37(19) . . ? C26 C31 C30 119.13(19) . . ? N3 C32 C39 120.92(18) . . ? N3 C32 C33 117.25(18) . . ? C39 C32 C33 121.67(18) . . ? C34 C33 C38 119.8(2) . . ? C34 C33 C32 122.57(19) . . ? C38 C33 C32 117.65(19) . . ? C33 C34 C35 119.7(2) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 120.3(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 119.7(2) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C33 120.2(2) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? N5 C39 C32 121.49(19) . . ? N5 C39 C40 116.83(18) . . ? C32 C39 C40 121.62(18) . . ? C45 C40 C41 119.0(2) . . ? C45 C40 C39 119.77(19) . . ? C41 C40 C39 121.10(18) . . ? C42 C41 C40 120.4(2) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.2(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.7(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.3(2) . . ? C44 C45 H45 119.8 . . ? C40 C45 H45 119.8 . . ? C48 O46 Ag1 93.21(15) . . ? O47 C48 O46 128.8(2) . . ? O47 C48 C49 115.6(2) . . ? O46 C48 C49 115.5(2) . . ? F50 C49 F51 106.64(18) . . ? F50 C49 F52 105.94(18) . . ? F51 C49 F52 106.30(18) . . ? F50 C49 C48 114.13(18) . . ? F51 C49 C48 113.13(18) . . ? F52 C49 C48 110.16(18) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.869 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.072 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 646205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Ag2 N4 O6' _chemical_formula_sum 'C20 H14 Ag2 N4 O6' _chemical_formula_weight 622.09 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.3039(2) _cell_length_b 7.00040(10) _cell_length_c 21.1996(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.5097(7) _cell_angle_gamma 90.00 _cell_volume 1961.65(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4358 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6288 _exptl_absorpt_correction_T_max 0.7489 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15380 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.22 _reflns_number_total 4721 _reflns_number_gt 3890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4721 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.144308(19) 0.13979(3) 0.106191(11) 0.02643(9) Uani 1 1 d . . . Ag2 Ag 0.087896(18) 0.09287(3) 0.446437(10) 0.02528(9) Uani 1 1 d . . . N3 N 0.1193(2) 0.0895(3) 0.21013(11) 0.0193(5) Uani 1 1 d . . . N4 N 0.10069(19) 0.0902(3) 0.33991(11) 0.0176(5) Uani 1 1 d . . . C5 C 0.0165(2) 0.0801(4) 0.29659(14) 0.0180(6) Uani 1 1 d . . . C6 C -0.0810(2) 0.0672(4) 0.31725(15) 0.0228(6) Uani 1 1 d . . . H6 H -0.0881 0.0579 0.3612 0.027 Uiso 1 1 calc R . . C7 C -0.1649(2) 0.0684(4) 0.27336(16) 0.0253(7) Uani 1 1 d . . . H7 H -0.2302 0.0587 0.2872 0.030 Uiso 1 1 calc R . . C8 C -0.1556(3) 0.0839(4) 0.20825(16) 0.0261(7) Uani 1 1 d . . . H8 H -0.2148 0.0913 0.1788 0.031 Uiso 1 1 calc R . . C9 C -0.0620(2) 0.0886(4) 0.18652(15) 0.0229(6) Uani 1 1 d . . . H9 H -0.0564 0.0937 0.1423 0.027 Uiso 1 1 calc R . . C10 C 0.0253(2) 0.0856(4) 0.23092(14) 0.0195(6) Uani 1 1 d . . . C11 C 0.2010(2) 0.0922(4) 0.25238(14) 0.0182(6) Uani 1 1 d . . . C12 C 0.2988(2) 0.0913(4) 0.22469(14) 0.0198(6) Uani 1 1 d . . . C13 C 0.3104(2) -0.0381(4) 0.17531(14) 0.0225(6) Uani 1 1 d . . . H13 H 0.2581 -0.1271 0.1626 0.027 Uiso 1 1 calc R . . C14 C 0.3973(2) -0.0369(4) 0.14510(15) 0.0262(7) Uani 1 1 d . . . H14 H 0.4047 -0.1254 0.1120 0.031 Uiso 1 1 calc R . . C15 C 0.4736(3) 0.0934(4) 0.16317(16) 0.0272(7) Uani 1 1 d . . . H15 H 0.5332 0.0949 0.1424 0.033 Uiso 1 1 calc R . . C16 C 0.4626(2) 0.2221(4) 0.21190(14) 0.0250(6) Uani 1 1 d . . . H16 H 0.5148 0.3117 0.2241 0.030 Uiso 1 1 calc R . . C17 C 0.3761(2) 0.2211(4) 0.24287(14) 0.0226(6) Uani 1 1 d . . . H17 H 0.3697 0.3086 0.2764 0.027 Uiso 1 1 calc R . . C18 C 0.1909(2) 0.0997(4) 0.31934(14) 0.0176(6) Uani 1 1 d . . . C19 C 0.2796(2) 0.1290(4) 0.36778(14) 0.0210(6) Uani 1 1 d . . . C20 C 0.2765(2) 0.2783(4) 0.41108(14) 0.0231(6) Uani 1 1 d . . . H20 H 0.2175 0.3549 0.4105 0.028 Uiso 1 1 calc R . . C21 C 0.3598(3) 0.3149(5) 0.45513(15) 0.0296(7) Uani 1 1 d . . . H21 H 0.3574 0.4161 0.4848 0.036 Uiso 1 1 calc R . . C22 C 0.4456(3) 0.2051(5) 0.45595(16) 0.0339(8) Uani 1 1 d . . . H22 H 0.5030 0.2327 0.4855 0.041 Uiso 1 1 calc R . . C23 C 0.4489(2) 0.0538(5) 0.41378(16) 0.0303(7) Uani 1 1 d . . . H23 H 0.5082 -0.0222 0.4146 0.036 Uiso 1 1 calc R . . C24 C 0.3657(2) 0.0142(5) 0.37065(14) 0.0251(7) Uani 1 1 d . . . H24 H 0.3671 -0.0919 0.3428 0.030 Uiso 1 1 calc R . . N25 N 0.25378(19) 0.0001(4) 0.55935(12) 0.0240(6) Uani 1 1 d . . . O26 O 0.17259(18) 0.1033(3) 0.54554(10) 0.0273(5) Uani 1 1 d . . . O27 O 0.27573(19) -0.1178(3) 0.52087(12) 0.0336(6) Uani 1 1 d . . . O28 O 0.30326(19) 0.0278(4) 0.61135(12) 0.0396(6) Uani 1 1 d . . . N29 N 0.08137(19) -0.1513(3) 0.00417(12) 0.0207(5) Uani 1 1 d . . . O30 O 0.06554(19) -0.1813(4) 0.06094(10) 0.0335(5) Uani 1 1 d . . . O31 O 0.0378(2) -0.2534(3) -0.03880(11) 0.0397(6) Uani 1 1 d . . . O32 O 0.13759(19) -0.0194(4) -0.00706(13) 0.0421(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 Ag1 0.03277(16) 0.03184(15) 0.01451(14) 0.00233(8) 0.00196(10) -0.00345(10) Ag2 0.02958(15) 0.03225(15) 0.01422(14) 0.00114(8) 0.00341(10) 0.00210(9) N3 0.0258(13) 0.0181(11) 0.0142(12) 0.0005(9) 0.0027(10) -0.0009(10) N4 0.0199(13) 0.0168(11) 0.0161(12) 0.0003(9) 0.0029(10) 0.0031(9) C5 0.0225(15) 0.0122(12) 0.0191(15) -0.0005(10) 0.0020(12) -0.0006(11) C6 0.0253(16) 0.0217(14) 0.0222(16) -0.0035(11) 0.0057(12) -0.0009(12) C7 0.0242(16) 0.0232(15) 0.0294(17) -0.0045(12) 0.0069(13) -0.0007(13) C8 0.0261(16) 0.0237(15) 0.0274(17) -0.0053(12) -0.0021(14) 0.0030(13) C9 0.0271(17) 0.0232(15) 0.0179(15) -0.0008(11) 0.0007(13) 0.0007(12) C10 0.0220(15) 0.0173(13) 0.0194(15) 0.0002(10) 0.0028(12) -0.0003(11) C11 0.0228(15) 0.0173(13) 0.0152(14) -0.0002(10) 0.0046(12) -0.0003(11) C12 0.0235(15) 0.0215(14) 0.0145(14) 0.0024(10) 0.0025(12) 0.0024(11) C13 0.0277(16) 0.0239(14) 0.0161(15) 0.0008(11) 0.0035(12) -0.0011(13) C14 0.0322(17) 0.0278(15) 0.0203(16) -0.0005(12) 0.0093(13) 0.0056(14) C15 0.0282(17) 0.0295(16) 0.0254(17) 0.0036(12) 0.0103(14) 0.0028(13) C16 0.0265(16) 0.0286(16) 0.0200(15) 0.0037(12) 0.0033(12) -0.0051(13) C17 0.0257(15) 0.0250(15) 0.0172(14) 0.0017(11) 0.0032(12) 0.0010(13) C18 0.0217(15) 0.0162(12) 0.0152(14) -0.0004(10) 0.0030(11) 0.0011(11) C19 0.0247(16) 0.0264(15) 0.0121(14) 0.0037(10) 0.0025(12) 0.0005(12) C20 0.0268(16) 0.0267(15) 0.0163(14) 0.0010(11) 0.0049(12) 0.0012(13) C21 0.0369(18) 0.0343(16) 0.0171(15) 0.0005(13) 0.0001(13) -0.0076(15) C22 0.0307(17) 0.050(2) 0.0204(16) 0.0115(15) -0.0003(13) -0.0118(16) C23 0.0246(16) 0.0459(19) 0.0213(16) 0.0132(14) 0.0061(13) 0.0050(15) C24 0.0277(16) 0.0323(16) 0.0166(15) 0.0061(12) 0.0081(12) 0.0046(13) N25 0.0248(13) 0.0301(14) 0.0176(13) 0.0012(10) 0.0044(11) -0.0017(11) O26 0.0313(13) 0.0318(11) 0.0178(11) -0.0035(8) -0.0011(10) 0.0093(9) O27 0.0368(14) 0.0320(12) 0.0333(14) -0.0074(10) 0.0095(11) 0.0042(10) O28 0.0311(13) 0.0639(17) 0.0221(13) -0.0041(11) -0.0047(10) 0.0049(12) N29 0.0204(13) 0.0211(12) 0.0202(13) 0.0020(9) 0.0012(10) 0.0018(10) O30 0.0390(14) 0.0457(13) 0.0165(11) 0.0069(10) 0.0058(10) 0.0035(11) O31 0.0490(15) 0.0317(12) 0.0332(14) -0.0134(10) -0.0180(12) 0.0119(12) O32 0.0342(14) 0.0344(13) 0.0586(18) 0.0218(12) 0.0099(13) -0.0037(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O26 2.267(2) 4_565 ? Ag1 N3 2.293(2) . ? Ag2 O26 2.270(2) . ? Ag2 N4 2.284(2) . ? Ag2 O31 2.497(2) 4_556 ? Ag2 O30 2.573(3) 2 ? N3 C11 1.328(4) . ? N3 C10 1.372(4) . ? N4 C18 1.325(4) . ? N4 C5 1.368(4) . ? C5 C10 1.411(4) . ? C5 C6 1.418(4) . ? C6 C7 1.370(5) . ? C6 H6 0.9500 . ? C7 C8 1.404(5) . ? C7 H7 0.9500 . ? C8 C9 1.375(5) . ? C8 H8 0.9500 . ? C9 C10 1.410(4) . ? C9 H9 0.9500 . ? C11 C18 1.442(4) . ? C11 C12 1.487(4) . ? C12 C17 1.394(4) . ? C12 C13 1.406(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(5) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.488(4) . ? C19 C20 1.395(4) . ? C19 C24 1.395(4) . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C22 1.375(5) . ? C21 H21 0.9500 . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C23 C24 1.382(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? N25 O27 1.219(3) . ? N25 O28 1.234(3) . ? N25 O26 1.305(3) . ? O26 Ag1 2.267(2) 4_566 ? N29 O32 1.228(3) . ? N29 O31 1.248(3) . ? N29 O30 1.263(3) . ? O30 Ag2 2.573(3) 2_545 ? O31 Ag2 2.497(2) 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 O26 Ag1 N3 135.93(8) 4_565 . ? O26 Ag2 N4 146.17(9) . . ? O26 Ag2 O31 91.49(7) . 4_556 ? N4 Ag2 O31 99.61(8) . 4_556 ? O26 Ag2 O30 110.10(7) . 2 ? N4 Ag2 O30 95.31(8) . 2 ? O31 Ag2 O30 111.80(8) 4_556 2 ? C11 N3 C10 119.3(3) . . ? C11 N3 Ag1 116.7(2) . . ? C10 N3 Ag1 123.3(2) . . ? C18 N4 C5 119.1(3) . . ? C18 N4 Ag2 119.8(2) . . ? C5 N4 Ag2 121.14(19) . . ? N4 C5 C10 120.5(3) . . ? N4 C5 C6 120.3(3) . . ? C10 C5 C6 119.2(3) . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N3 C10 C9 119.8(3) . . ? N3 C10 C5 119.9(3) . . ? C9 C10 C5 120.3(3) . . ? N3 C11 C18 120.3(3) . . ? N3 C11 C12 114.8(3) . . ? C18 C11 C12 124.9(3) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 C11 122.7(3) . . ? C13 C12 C11 118.1(3) . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C12 119.9(3) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? N4 C18 C11 120.7(3) . . ? N4 C18 C19 117.2(3) . . ? C11 C18 C19 122.0(3) . . ? C20 C19 C24 119.3(3) . . ? C20 C19 C18 118.5(3) . . ? C24 C19 C18 122.2(3) . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.4(3) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? O27 N25 O28 124.1(3) . . ? O27 N25 O26 118.7(3) . . ? O28 N25 O26 117.2(3) . . ? N25 O26 Ag1 119.90(17) . 4_566 ? N25 O26 Ag2 120.08(17) . . ? Ag1 O26 Ag2 116.98(9) 4_566 . ? O32 N29 O31 122.1(3) . . ? O32 N29 O30 118.7(3) . . ? O31 N29 O30 119.1(3) . . ? N29 O30 Ag2 105.14(18) . 2_545 ? N29 O31 Ag2 121.92(18) . 4 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.210 _refine_diff_density_min -1.189 _refine_diff_density_rms 0.137 #=====END===========================