# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Braga, Dario' _publ_contact_author_address ; ; _publ_contact_author_email dario.braga@unibo.it loop_ _publ_author_name D.Braga F.Grepioni data_e_23_red2d _database_code_depnum_ccdc_archive 'CCDC 801410' #TrackingRef 'Form I.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Ag N7 O5' _chemical_formula_weight 696.47 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' 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9972(7) _cell_length_b 9.1664(5) _cell_length_c 21.5610(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.587(5) _cell_angle_gamma 90.00 _cell_volume 2903.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3914 _cell_measurement_theta_min 2.6188 _cell_measurement_theta_max 28.9697 _exptl_crystal_description prism _exptl_crystal_colour brown-yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.077 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61256 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_device '92mm CCD camera (sapphire) on \k-goniostat' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12854 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 29.04 _reflns_number_total 6146 _reflns_number_gt 2575 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -7.00 36.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 77.0000 150.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega -39.00 6.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -18.5330 77.0000 -90.0000 45 #__ type_ start__ end____ width___ exp.time_ 3 omega -19.00 50.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -18.5330 77.0000 150.0000 69 #__ type_ start__ end____ width___ exp.time_ 4 omega -48.00 51.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -18.5330 77.0000 30.0000 99 ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6146 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.09675(2) 0.10548(4) 0.054873(18) 0.06727(17) Uani 1 1 d . . . O1 O 0.4593(2) -0.4410(3) 0.27658(14) 0.0659(9) Uani 1 1 d . . . N1 N 0.2043(2) -0.0442(4) 0.05365(19) 0.0518(9) Uani 1 1 d . . . N2 N 0.4187(3) -0.3900(5) 0.1716(2) 0.0553(11) Uani 1 1 d . . . H2N H 0.436(2) -0.393(4) 0.1426(15) 0.011(11) Uiso 1 1 d . . . N3 N 0.5376(3) -0.5408(4) 0.2072(2) 0.0556(11) Uani 1 1 d . . . H3N H 0.538(2) -0.543(4) 0.1680(18) 0.042(13) Uiso 1 1 d . . . C1 C 0.6836(4) -0.7188(6) 0.3447(3) 0.0894(18) Uani 1 1 d . . . H1 H 0.6903 -0.7256 0.3885 0.107 Uiso 1 1 calc R . . C2 C 0.7400(4) -0.7953(6) 0.3157(3) 0.0869(18) Uani 1 1 d . . . H2 H 0.7869 -0.8503 0.3395 0.104 Uiso 1 1 calc R . . C3 C 0.7283(3) -0.7920(6) 0.2517(3) 0.0807(16) Uani 1 1 d . . . H3 H 0.7652 -0.8480 0.2311 0.097 Uiso 1 1 calc R . . C4 C 0.6612(3) -0.7047(5) 0.2174(2) 0.0682(14) Uani 1 1 d . . . H4 H 0.6545 -0.6999 0.1736 0.082 Uiso 1 1 calc R . . C5 C 0.6042(3) -0.6249(5) 0.2465(2) 0.0499(11) Uani 1 1 d . . . C6 C 0.6159(3) -0.6302(6) 0.3114(2) 0.0761(15) Uani 1 1 d . . . H6 H 0.5790 -0.5754 0.3325 0.091 Uiso 1 1 calc R . . C7 C 0.4709(3) -0.4573(5) 0.2232(2) 0.0458(11) Uani 1 1 d . . . C8 C 0.3472(3) -0.2902(4) 0.1699(2) 0.0453(11) Uani 1 1 d . . . C9 C 0.3073(3) -0.2643(5) 0.2204(2) 0.0526(12) Uani 1 1 d . . . H9 H 0.3284 -0.3132 0.2583 0.063 Uiso 1 1 calc R . . C10 C 0.2351(3) -0.1653(5) 0.2161(2) 0.0529(12) Uani 1 1 d . . . H10 H 0.2096 -0.1485 0.2514 0.064 Uiso 1 1 calc R . . C11 C 0.2019(3) -0.0935(5) 0.1614(2) 0.0548(12) Uani 1 1 d . . . H11 H 0.1534 -0.0293 0.1592 0.066 Uiso 1 1 calc R . . C12 C 0.2402(3) -0.1156(5) 0.1085(2) 0.0434(10) Uani 1 1 d . . . C13 C 0.3135(3) -0.2159(4) 0.11135(19) 0.0398(10) Uani 1 1 d . . . C14 C 0.3497(3) -0.2320(4) 0.0564(2) 0.0482(11) Uani 1 1 d . . . H14 H 0.3993 -0.2933 0.0569 0.058 Uiso 1 1 calc R . . C15 C 0.3127(3) -0.1582(5) 0.0027(2) 0.0554(12) Uani 1 1 d . . . H15 H 0.3357 -0.1696 -0.0340 0.066 Uiso 1 1 calc R . . C16 C 0.2403(3) -0.0663(5) 0.0037(2) 0.0593(13) Uani 1 1 d . . . H16 H 0.2153 -0.0166 -0.0333 0.071 Uiso 1 1 calc R . . O2 O -0.2422(2) 0.7343(3) -0.13299(15) 0.0599(9) Uani 1 1 d . . . N4 N -0.0159(2) 0.2435(4) 0.05455(19) 0.0571(10) Uani 1 1 d . . . N5 N -0.2446(3) 0.5829(4) -0.05003(19) 0.0539(11) Uani 1 1 d . . . H5N H -0.273(2) 0.555(4) -0.0228(17) 0.036(13) Uiso 1 1 d . . . N6 N -0.3631(3) 0.7371(4) -0.0851(2) 0.0580(12) Uani 1 1 d . . . H6N H -0.379(2) 0.708(3) -0.0566(14) 0.044(10) Uiso 1 1 d . . . C17 C -0.5387(4) 1.0517(6) -0.1829(3) 0.0756(15) Uani 1 1 d . . . H17 H -0.5785 1.1210 -0.2045 0.091 Uiso 1 1 calc R . . C18 C -0.5450(3) 1.0114(5) -0.1226(3) 0.0755(15) Uani 1 1 d . . . H18 H -0.5886 1.0534 -0.1030 0.091 Uiso 1 1 calc R . . C19 C -0.4856(3) 0.9073(5) -0.0913(2) 0.0632(13) Uani 1 1 d . . . H19 H -0.4901 0.8789 -0.0506 0.076 Uiso 1 1 calc R . . C20 C -0.4743(4) 0.9905(5) -0.2109(2) 0.0727(15) Uani 1 1 d . . . H20 H -0.4701 1.0190 -0.2517 0.087 Uiso 1 1 calc R . . C21 C -0.4148(3) 0.8863(5) -0.1798(2) 0.0599(12) Uani 1 1 d . . . H21 H -0.3716 0.8444 -0.1998 0.072 Uiso 1 1 calc R . . C22 C -0.4199(3) 0.8450(5) -0.1193(2) 0.0519(12) Uani 1 1 d . . . C23 C -0.2812(3) 0.6890(5) -0.0932(2) 0.0498(11) Uani 1 1 d . . . C24 C -0.1698(3) 0.4939(4) -0.0527(2) 0.0444(11) Uani 1 1 d . . . C25 C -0.1294(3) 0.4191(4) 0.0039(2) 0.0430(11) Uani 1 1 d . . . C26 C -0.1365(3) 0.4734(5) -0.1066(2) 0.0531(12) Uani 1 1 d . . . H26 H -0.1621 0.5235 -0.1434 0.064 Uiso 1 1 calc R . . C27 C -0.0645(3) 0.3781(5) -0.1067(2) 0.0549(12) Uani 1 1 d . . . H27 H -0.0425 0.3658 -0.1437 0.066 Uiso 1 1 calc R . . C28 C -0.0256(3) 0.3026(5) -0.0541(2) 0.0543(12) Uani 1 1 d . . . H28 H 0.0218 0.2381 -0.0556 0.065 Uiso 1 1 calc R . . C29 C -0.0564(3) 0.3218(5) 0.0020(2) 0.0449(11) Uani 1 1 d . . . C30 C -0.1552(3) 0.4370(5) 0.0624(2) 0.0526(12) Uani 1 1 d . . . H30 H -0.2014 0.5023 0.0658 0.063 Uiso 1 1 calc R . . C31 C -0.1139(3) 0.3607(5) 0.1139(2) 0.0658(14) Uani 1 1 d . . . H31 H -0.1311 0.3729 0.1527 0.079 Uiso 1 1 calc R . . C32 C -0.0447(3) 0.2628(5) 0.1073(2) 0.0679(14) Uani 1 1 d . . . H32 H -0.0177 0.2083 0.1425 0.082 Uiso 1 1 calc R . . N7 N 0.5815(3) 0.5523(7) 0.0544(2) 0.0783(14) Uani 1 1 d . . . O3 O 0.5879(5) 0.6780(6) 0.0411(2) 0.185(3) Uani 1 1 d . . . O4 O 0.5183(3) 0.5090(6) 0.07539(16) 0.1240(17) Uani 1 1 d . . . O5 O 0.6397(3) 0.4772(6) 0.0465(2) 0.145(2) 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 0.0501(2) 0.0659(3) 0.0829(3) 0.0131(2) 0.00633(18) 0.0152(2) O1 0.071(2) 0.092(3) 0.0341(19) -0.0030(18) 0.0078(16) 0.0147(18) N1 0.051(2) 0.052(2) 0.052(3) 0.002(2) 0.009(2) -0.0011(18) N2 0.062(3) 0.069(3) 0.038(3) 0.010(2) 0.017(2) 0.019(2) N3 0.063(3) 0.068(3) 0.034(3) 0.007(2) 0.007(2) 0.023(2) C1 0.107(5) 0.092(4) 0.060(4) 0.020(3) -0.004(3) 0.025(4) C2 0.068(4) 0.086(4) 0.094(5) 0.022(4) -0.013(3) 0.022(3) C3 0.068(4) 0.086(4) 0.085(4) 0.008(4) 0.010(3) 0.033(3) C4 0.062(3) 0.077(4) 0.063(3) 0.002(3) 0.005(3) 0.015(3) C5 0.047(3) 0.046(3) 0.054(3) 0.005(3) 0.004(2) 0.004(2) C6 0.084(4) 0.086(4) 0.054(4) 0.012(3) 0.003(3) 0.024(3) C7 0.044(3) 0.045(3) 0.045(3) 0.000(2) 0.002(2) 0.005(2) C8 0.047(3) 0.047(3) 0.043(3) -0.001(2) 0.012(2) 0.003(2) C9 0.061(3) 0.059(3) 0.040(3) 0.006(2) 0.015(2) 0.010(2) C10 0.054(3) 0.056(3) 0.054(3) -0.009(2) 0.024(2) -0.001(2) C11 0.052(3) 0.056(3) 0.056(3) 0.002(3) 0.010(2) 0.011(2) C12 0.038(2) 0.049(3) 0.042(3) 0.002(2) 0.008(2) 0.001(2) C13 0.042(2) 0.044(3) 0.033(3) -0.004(2) 0.006(2) 0.002(2) C14 0.050(3) 0.049(3) 0.046(3) 0.003(2) 0.008(2) 0.001(2) C15 0.055(3) 0.068(3) 0.045(3) 0.002(3) 0.014(2) 0.004(3) C16 0.056(3) 0.072(4) 0.046(3) 0.015(3) 0.001(2) 0.005(3) O2 0.059(2) 0.063(2) 0.060(2) 0.0147(17) 0.0176(17) 0.0069(16) N4 0.047(2) 0.067(3) 0.055(3) 0.009(2) 0.004(2) 0.0061(19) N5 0.051(2) 0.064(3) 0.049(3) 0.019(2) 0.014(2) 0.012(2) N6 0.054(3) 0.064(3) 0.059(3) 0.021(2) 0.019(2) 0.015(2) C17 0.062(3) 0.063(4) 0.094(5) 0.011(3) -0.002(3) 0.015(3) C18 0.047(3) 0.064(4) 0.113(5) 0.005(3) 0.009(3) 0.017(3) C19 0.055(3) 0.056(3) 0.078(3) 0.005(3) 0.013(3) 0.013(3) C20 0.073(4) 0.066(4) 0.069(4) 0.015(3) -0.009(3) 0.009(3) C21 0.063(3) 0.057(3) 0.058(3) -0.001(3) 0.008(2) 0.009(3) C22 0.046(3) 0.044(3) 0.062(3) 0.003(2) 0.002(2) 0.000(2) C23 0.045(3) 0.050(3) 0.051(3) -0.003(3) 0.000(2) 0.006(2) C24 0.038(2) 0.049(3) 0.045(3) 0.004(2) 0.006(2) 0.004(2) C25 0.034(2) 0.050(3) 0.045(3) -0.005(2) 0.007(2) -0.002(2) C26 0.056(3) 0.059(3) 0.042(3) 0.008(2) 0.005(2) 0.002(2) C27 0.052(3) 0.063(3) 0.052(3) -0.003(3) 0.016(2) -0.004(3) C28 0.049(3) 0.054(3) 0.060(3) -0.002(3) 0.011(3) 0.006(2) C29 0.037(2) 0.048(3) 0.048(3) 0.004(2) 0.003(2) -0.006(2) C30 0.042(3) 0.064(3) 0.053(3) 0.000(2) 0.010(2) 0.006(2) C31 0.058(3) 0.092(4) 0.048(3) 0.014(3) 0.010(2) 0.011(3) C32 0.055(3) 0.083(4) 0.058(4) 0.023(3) -0.006(3) 0.011(3) N7 0.054(3) 0.121(4) 0.064(3) -0.017(3) 0.022(3) -0.009(3) O3 0.328(9) 0.099(4) 0.111(4) -0.011(3) 0.002(4) -0.064(5) O4 0.088(3) 0.230(5) 0.059(3) 0.028(3) 0.027(2) 0.035(3) O5 0.065(3) 0.207(6) 0.159(4) -0.062(4) 0.009(3) 0.035(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 Ag1 N4 2.109(4) . ? Ag1 N1 2.122(3) . ? O1 C7 1.208(5) . ? N1 C16 1.313(5) . ? N1 C12 1.364(5) . ? N2 C7 1.371(5) . ? N2 C8 1.404(5) . ? N3 C7 1.359(5) . ? N3 C5 1.405(5) . ? C1 C2 1.346(7) . ? C1 C6 1.383(6) . ? C2 C3 1.357(7) . ? C3 C4 1.379(6) . ? C4 C5 1.369(6) . ? C5 C6 1.376(6) . ? C8 C9 1.365(5) . ? C8 C13 1.434(5) . ? C9 C10 1.401(5) . ? C10 C11 1.356(5) . ? C11 C12 1.391(5) . ? C12 C13 1.424(5) . ? C13 C14 1.406(5) . ? C14 C15 1.360(5) . ? C15 C16 1.378(6) . ? O2 C23 1.206(5) . ? N4 C32 1.307(5) . ? N4 C29 1.375(5) . ? N5 C23 1.381(5) . ? N5 C24 1.397(5) . ? N6 C23 1.348(5) . ? N6 C22 1.413(5) . ? C17 C20 1.360(6) . ? C17 C18 1.373(7) . ? C18 C19 1.385(6) . ? C19 C22 1.378(6) . ? C20 C21 1.384(6) . ? C21 C22 1.376(6) . ? C24 C26 1.367(5) . ? C24 C25 1.425(5) . ? C25 C30 1.401(5) . ? C25 C29 1.420(5) . ? C26 C27 1.388(6) . ? C27 C28 1.355(6) . ? C28 C29 1.390(5) . ? C30 C31 1.353(5) . ? C31 C32 1.402(6) . ? N7 O5 1.150(5) . ? N7 O3 1.196(6) . ? N7 O4 1.197(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 N4 Ag1 N1 176.44(13) . . ? C16 N1 C12 118.7(4) . . ? C16 N1 Ag1 123.3(3) . . ? C12 N1 Ag1 117.9(3) . . ? C7 N2 C8 128.6(4) . . ? C7 N3 C5 128.8(4) . . ? C2 C1 C6 122.0(5) . . ? C1 C2 C3 119.7(5) . . ? C2 C3 C4 119.3(5) . . ? C5 C4 C3 121.3(5) . . ? C4 C5 C6 119.0(4) . . ? C4 C5 N3 116.7(4) . . ? C6 C5 N3 124.3(4) . . ? C5 C6 C1 118.6(5) . . ? O1 C7 N3 124.5(4) . . ? O1 C7 N2 123.3(4) . . ? N3 C7 N2 112.2(4) . . ? C9 C8 N2 123.1(4) . . ? C9 C8 C13 119.1(4) . . ? N2 C8 C13 117.7(4) . . ? C8 C9 C10 121.1(4) . . ? C11 C10 C9 121.1(4) . . ? C10 C11 C12 120.2(4) . . ? N1 C12 C11 119.0(4) . . ? N1 C12 C13 121.0(4) . . ? C11 C12 C13 120.0(4) . . ? C14 C13 C12 117.1(4) . . ? C14 C13 C8 124.3(4) . . ? C12 C13 C8 118.5(4) . . ? C15 C14 C13 120.3(4) . . ? C14 C15 C16 118.5(4) . . ? N1 C16 C15 124.3(4) . . ? C32 N4 C29 118.6(4) . . ? C32 N4 Ag1 118.8(3) . . ? C29 N4 Ag1 122.4(3) . . ? C23 N5 C24 126.7(4) . . ? C23 N6 C22 129.1(4) . . ? C20 C17 C18 120.0(5) . . ? C17 C18 C19 119.2(5) . . ? C22 C19 C18 121.2(5) . . ? C17 C20 C21 121.0(5) . . ? C22 C21 C20 119.7(5) . . ? C21 C22 C19 118.9(4) . . ? C21 C22 N6 123.0(4) . . ? C19 C22 N6 118.1(4) . . ? O2 C23 N6 124.4(4) . . ? O2 C23 N5 122.5(4) . . ? N6 C23 N5 113.1(4) . . ? C26 C24 N5 123.3(4) . . ? C26 C24 C25 119.8(4) . . ? N5 C24 C25 116.9(4) . . ? C30 C25 C29 117.0(4) . . ? C30 C25 C24 124.6(4) . . ? C29 C25 C24 118.3(4) . . ? C24 C26 C27 120.3(4) . . ? C28 C27 C26 121.7(4) . . ? C27 C28 C29 120.0(4) . . ? N4 C29 C28 118.9(4) . . ? N4 C29 C25 121.3(4) . . ? C28 C29 C25 119.8(4) . . ? C31 C30 C25 121.0(4) . . ? C30 C31 C32 118.3(4) . . ? N4 C32 C31 123.8(4) . . ? O5 N7 O3 116.2(6) . . ? O5 N7 O4 122.7(7) . . ? O3 N7 O4 121.1(7) . . ? _diffrn_measured_fraction_theta_max 0.792 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.607 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.064 # Attachment 'Form II.cif' data_crist_gel _database_code_depnum_ccdc_archive 'CCDC 801411' #TrackingRef 'Form II.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Ag0.50 N3.50 O2.50' _chemical_formula_weight 348.23 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' 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 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 13.8418(12) _cell_length_b 8.3439(7) _cell_length_c 25.2079(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.141(7) _cell_angle_gamma 90.00 _cell_volume 2882.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2152 _cell_measurement_theta_min 2.8444 _cell_measurement_theta_max 28.8421 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63076 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_device '92mm CCD camera (sapphire) on \k-goniostat' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6327 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.87 _reflns_number_total 3262 _reflns_number_gt 1921 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 61.00 88.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 179.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega -45.00 91.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 0.0000 -30.0000 136 #__ type_ start__ end____ width___ exp.time_ 3 omega -95.00 -58.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -18.5330 179.0000 0.0000 37 #__ type_ start__ end____ width___ exp.time_ 4 omega -93.00 -60.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -18.5330 179.0000 -180.0000 33 ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3262 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _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 0.0000 0.0000 0.5000 0.06589(17) Uani 1 2 d S . . N1 N -0.00783(18) 0.1976(3) 0.55301(11) 0.0494(6) Uani 1 1 d . . . N2 N 0.10471(19) 0.7239(3) 0.61625(12) 0.0495(7) Uani 1 1 d . . . H2N H 0.0851(17) 0.705(3) 0.6446(11) 0.029(8) Uiso 1 1 d . . . N3 N 0.1408(2) 0.9634(3) 0.65668(12) 0.0529(7) Uani 1 1 d . . . H3N H 0.1105(18) 0.929(3) 0.6773(11) 0.028(8) Uiso 1 1 d . . . N4 N 0.0000 0.2261(5) 0.2500 0.0619(11) Uani 1 2 d S . . O1 O 0.17290(15) 0.9216(3) 0.57195(9) 0.0550(6) Uani 1 1 d . . . O2 O -0.0446(2) 0.2997(4) 0.27968(12) 0.1159(12) Uani 1 1 d . . . O3 O 0.0000 0.0829(5) 0.2500 0.1254(19) Uani 1 2 d S . . C1 C 0.2528(4) 1.4190(5) 0.69330(19) 0.0915(15) Uani 1 1 d . . . H1 H 0.2783 1.5201 0.7022 0.110 Uiso 1 1 calc R . . C2 C 0.1799(3) 1.3593(5) 0.71772(16) 0.0831(12) Uani 1 1 d . . . H2 H 0.1551 1.4200 0.7436 0.100 Uiso 1 1 calc R . . C3 C 0.2885(3) 1.3288(5) 0.65530(19) 0.0828(12) Uani 1 1 d . . . H3 H 0.3387 1.3699 0.6384 0.099 Uiso 1 1 calc R . . C4 C 0.1419(3) 1.2095(4) 0.70477(14) 0.0645(10) Uani 1 1 d . . . H4 H 0.0917 1.1696 0.7220 0.077 Uiso 1 1 calc R . . C5 C 0.2524(2) 1.1791(4) 0.64134(14) 0.0606(9) Uani 1 1 d . . . H5 H 0.2779 1.1194 0.6154 0.073 Uiso 1 1 calc R . . C6 C 0.1780(2) 1.1186(3) 0.66633(12) 0.0500(8) Uani 1 1 d . . . C7 C 0.1419(2) 0.8739(3) 0.61195(13) 0.0416(7) Uani 1 1 d . . . C8 C 0.10836(19) 0.5963(3) 0.58016(11) 0.0387(7) Uani 1 1 d . . . C9 C 0.1695(2) 0.5943(4) 0.54247(12) 0.0455(7) Uani 1 1 d . . . H9 H 0.2090 0.6826 0.5387 0.055 Uiso 1 1 calc R . . C10 C 0.1738(2) 0.4606(4) 0.50934(13) 0.0492(8) Uani 1 1 d . . . H10 H 0.2171 0.4611 0.4843 0.059 Uiso 1 1 calc R . . C11 C 0.1166(2) 0.3311(4) 0.51286(12) 0.0499(8) Uani 1 1 d . . . H11 H 0.1207 0.2435 0.4905 0.060 Uiso 1 1 calc R . . C12 C 0.05131(19) 0.3291(3) 0.55033(12) 0.0409(7) Uani 1 1 d . . . C13 C 0.0462(2) 0.4622(3) 0.58467(11) 0.0387(7) Uani 1 1 d . . . C14 C -0.0224(2) 0.4550(4) 0.62105(13) 0.0490(8) Uani 1 1 d . . . H14 H -0.0281 0.5400 0.6442 0.059 Uiso 1 1 calc R . . C15 C -0.0800(2) 0.3232(4) 0.62214(14) 0.0577(9) Uani 1 1 d . . . H15 H -0.1257 0.3176 0.6458 0.069 Uiso 1 1 calc R . . C16 C -0.0697(2) 0.1979(4) 0.58760(15) 0.0587(9) Uani 1 1 d . . . H16 H -0.1092 0.1084 0.5890 0.070 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 0.0897(3) 0.04084(19) 0.0622(3) -0.0097(2) -0.00631(19) -0.0111(2) N1 0.0480(15) 0.0386(13) 0.0590(18) -0.0016(13) -0.0019(13) -0.0071(13) N2 0.0675(18) 0.0427(14) 0.0438(17) -0.0064(13) 0.0268(14) -0.0163(13) N3 0.0769(19) 0.0395(16) 0.0455(17) -0.0026(12) 0.0203(15) -0.0143(14) N4 0.070(3) 0.063(3) 0.056(3) 0.000 0.018(2) 0.000 O1 0.0735(14) 0.0448(12) 0.0492(14) 0.0036(11) 0.0176(11) -0.0146(12) O2 0.143(3) 0.135(3) 0.085(2) -0.036(2) 0.067(2) -0.001(2) O3 0.088(3) 0.058(3) 0.228(6) 0.000 0.012(3) 0.000 C1 0.131(4) 0.041(2) 0.087(3) 0.001(2) -0.039(3) -0.017(3) C2 0.127(4) 0.048(2) 0.066(3) -0.015(2) -0.015(2) 0.003(2) C3 0.091(3) 0.061(2) 0.089(3) 0.013(2) -0.012(2) -0.026(2) C4 0.086(3) 0.050(2) 0.055(2) -0.0067(17) -0.0018(18) 0.0038(19) C5 0.065(2) 0.0478(18) 0.066(2) 0.0015(17) -0.0005(18) -0.0116(18) C6 0.064(2) 0.0357(15) 0.0462(19) 0.0027(15) -0.0073(16) -0.0037(16) C7 0.0412(16) 0.0362(15) 0.0476(19) 0.0026(14) 0.0066(14) -0.0021(14) C8 0.0407(15) 0.0384(15) 0.0370(17) -0.0006(13) 0.0055(13) -0.0025(14) C9 0.0446(16) 0.0459(17) 0.0470(19) 0.0006(15) 0.0101(14) -0.0085(15) C10 0.0490(17) 0.056(2) 0.0459(19) -0.0004(15) 0.0177(14) 0.0001(16) C11 0.0578(19) 0.0482(18) 0.0438(18) -0.0097(15) 0.0082(15) 0.0024(17) C12 0.0408(16) 0.0352(14) 0.0436(18) -0.0016(13) -0.0047(13) -0.0004(14) C13 0.0368(15) 0.0374(16) 0.0410(16) 0.0027(12) 0.0028(12) -0.0007(12) C14 0.0535(18) 0.0445(17) 0.052(2) -0.0005(14) 0.0169(15) -0.0088(15) C15 0.054(2) 0.056(2) 0.068(2) 0.0028(18) 0.0248(17) -0.0109(17) C16 0.0500(19) 0.0458(18) 0.078(3) 0.0045(18) 0.0007(18) -0.0142(16) _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 2.135(3) 5_556 ? Ag1 N1 2.135(3) . ? N1 C16 1.306(4) . ? N1 C12 1.376(4) . ? N2 C7 1.363(4) . ? N2 C8 1.406(4) . ? N3 C7 1.354(4) . ? N3 C6 1.402(4) . ? N4 O3 1.194(5) . ? N4 O2 1.204(3) 2 ? N4 O2 1.204(3) . ? O1 C7 1.218(3) . ? C1 C2 1.349(6) . ? C1 C3 1.365(6) . ? C2 C4 1.377(5) . ? C3 C5 1.373(5) . ? C4 C6 1.379(4) . ? C5 C6 1.377(4) . ? C8 C9 1.359(4) . ? C8 C13 1.426(4) . ? C9 C10 1.399(4) . ? C10 C11 1.350(4) . ? C11 C12 1.397(4) . ? C12 C13 1.416(4) . ? C13 C14 1.411(4) . ? C14 C15 1.361(4) . ? C15 C16 1.380(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 N1 Ag1 N1 180.00(11) 5_556 . ? C16 N1 C12 118.8(3) . . ? C16 N1 Ag1 121.0(2) . . ? C12 N1 Ag1 120.1(2) . . ? C7 N2 C8 126.5(3) . . ? C7 N3 C6 127.4(3) . . ? O3 N4 O2 120.7(2) . 2 ? O3 N4 O2 120.7(2) . . ? O2 N4 O2 118.6(5) 2 . ? C2 C1 C3 119.0(4) . . ? C1 C2 C4 120.8(4) . . ? C5 C3 C1 121.8(4) . . ? C2 C4 C6 120.0(4) . . ? C3 C5 C6 119.0(4) . . ? C5 C6 C4 119.3(3) . . ? C5 C6 N3 122.6(3) . . ? C4 C6 N3 118.0(3) . . ? O1 C7 N3 123.7(3) . . ? O1 C7 N2 123.2(3) . . ? N3 C7 N2 113.1(3) . . ? C9 C8 N2 123.0(3) . . ? C9 C8 C13 119.2(3) . . ? N2 C8 C13 117.7(2) . . ? C8 C9 C10 120.7(3) . . ? C11 C10 C9 121.6(3) . . ? C10 C11 C12 119.7(3) . . ? N1 C12 C11 119.3(3) . . ? N1 C12 C13 120.9(3) . . ? C11 C12 C13 119.8(3) . . ? C12 C13 C14 117.4(3) . . ? C12 C13 C8 118.9(3) . . ? C14 C13 C8 123.7(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 119.0(3) . . ? N1 C16 C15 124.0(3) . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.055 # Attachment 'Form III.cif' data_f _database_code_depnum_ccdc_archive 'CCDC 801412' #TrackingRef 'Form III.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Ag0.50 N3.50 O2.50' _chemical_formula_weight 348.23 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.265 _cell_length_b 7.879 _cell_length_c 15.022 _cell_angle_alpha 95.16 _cell_angle_beta 91.58 _cell_angle_gamma 94.16 _cell_volume 736.1 _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1987 _cell_measurement_theta_min 2.5977 _cell_measurement_theta_max 29.0623 _exptl_crystal_description prism _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.061 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 354 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78871 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_device '92mm CCD camera (sapphire) on \k-goniostat' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5778 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 29.13 _reflns_number_total 3315 _reflns_number_gt 1588 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -8.00 83.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 77.0000 60.0000 91 #__ type_ start__ end____ width___ exp.time_ 2 omega -6.00 45.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 77.0000 -180.0000 51 #__ type_ start__ end____ width___ exp.time_ 3 omega 18.00 56.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 38.0000 30.0000 38 #__ type_ start__ end____ width___ exp.time_ 4 omega -51.00 47.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 -77.0000 -150.0000 98 #__ type_ start__ end____ width___ exp.time_ 5 omega -49.00 47.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 -77.0000 -60.0000 96 ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'sir 2008 (Giacovazzo 2008)' _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^)+(0.1197P)^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 3315 _refine_ls_number_parameters 191 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.967 _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 0.0000 0.0000 0.5000 0.0735(4) Uani 1 2 d S . . O1 O 0.9652(7) 0.7469(6) 0.6490(3) 0.0536(12) Uani 1 1 d . . . N1 N 0.1597(8) 0.1677(7) 0.6050(4) 0.0498(14) Uani 1 1 d . . . N2 N 0.7445(7) 0.5687(6) 0.7249(3) 0.0427(12) Uani 1 1 d . . . H2N H 0.7092 0.5384 0.7862 0.050 Uiso 1 1 d . . . N3 N 1.0002(8) 0.7499(7) 0.8002(3) 0.0494(13) Uani 1 1 d . . . H3N H 0.9178 0.6905 0.8444 0.050 Uiso 1 1 d . . . C1 C 1.5419(6) 1.0911(5) 0.8580(4) 0.075(2) Uani 1 1 d G . . H1 H 1.6626 1.1655 0.8722 0.090 Uiso 1 1 calc R . . C2 C 1.3747(8) 1.0841(5) 0.9168(3) 0.080(3) Uani 1 1 d G . . H2 H 1.3834 1.1539 0.9703 0.095 Uiso 1 1 calc R . . C3 C 1.1943(6) 0.9729(6) 0.8956(2) 0.0625(19) Uani 1 1 d G . . H3 H 1.0824 0.9682 0.9350 0.075 Uiso 1 1 calc R . . C4 C 1.1812(5) 0.8687(5) 0.8156(2) 0.0442(15) Uani 1 1 d G . . C5 C 1.3484(6) 0.8757(5) 0.7569(2) 0.0512(16) Uani 1 1 d G . . H5 H 1.3396 0.8059 0.7033 0.061 Uiso 1 1 calc R . . C6 C 1.5288(5) 0.9869(6) 0.7780(3) 0.066(2) Uani 1 1 d G . . H6 H 1.6407 0.9916 0.7387 0.079 Uiso 1 1 calc R . . C7 C 0.9116(9) 0.6929(8) 0.7185(4) 0.0405(14) Uani 1 1 d . . . C8 C 0.6517(9) 0.4605(7) 0.6518(4) 0.0371(13) Uani 1 1 d . . . C9 C 0.7509(9) 0.4286(8) 0.5737(4) 0.0448(15) Uani 1 1 d . . . H9 H 0.8838 0.4845 0.5655 0.054 Uiso 1 1 calc R . . C10 C 0.6566(10) 0.3132(8) 0.5053(4) 0.0485(16) Uani 1 1 d . . . H10 H 0.7278 0.2946 0.4522 0.058 Uiso 1 1 calc R . . C11 C 0.4631(10) 0.2274(8) 0.5145(4) 0.0472(16) Uani 1 1 d . . . H11 H 0.4032 0.1506 0.4683 0.057 Uiso 1 1 calc R . . C12 C 0.3547(9) 0.2560(7) 0.5945(4) 0.0413(15) Uani 1 1 d . . . C13 C 0.4455(8) 0.3762(7) 0.6646(4) 0.0370(13) Uani 1 1 d . . . C14 C 0.3298(9) 0.4015(8) 0.7435(4) 0.0439(15) Uani 1 1 d . . . H14 H 0.3834 0.4803 0.7900 0.053 Uiso 1 1 calc R . . C15 C 0.1384(10) 0.3093(8) 0.7511(4) 0.0503(16) Uani 1 1 d . . . H15 H 0.0598 0.3243 0.8025 0.060 Uiso 1 1 calc R . . C16 C 0.0644(10) 0.1926(9) 0.6798(5) 0.0572(18) Uani 1 1 d . . . H16 H -0.0631 0.1276 0.6865 0.069 Uiso 1 1 calc R . . N4 N 0.7882(14) 0.5112(14) 0.9695(6) 0.061(3) Uiso 0.50 1 d PD . . O2 O 0.6772(9) 0.5494(8) 0.9186(4) 0.0282(15) Uiso 0.50 1 d PD . . O4 O 0.7422(16) 0.4568(14) 1.0392(6) 0.087(3) Uiso 0.50 1 d PD . . O3 O 0.9741(13) 0.5535(17) 0.9627(7) 0.107(4) Uiso 0.50 1 d PD . . 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 0.0582(5) 0.0661(6) 0.0883(7) -0.0117(4) -0.0174(4) -0.0193(4) O1 0.060(3) 0.058(3) 0.040(2) 0.010(2) 0.001(2) -0.021(2) N1 0.043(3) 0.046(3) 0.059(3) 0.007(3) -0.002(3) -0.010(2) N2 0.040(3) 0.049(3) 0.036(2) -0.002(2) 0.002(2) -0.012(2) N3 0.047(3) 0.057(3) 0.039(3) 0.000(2) 0.006(2) -0.021(3) C1 0.059(4) 0.058(5) 0.104(6) 0.013(4) -0.026(4) -0.018(4) C2 0.111(7) 0.049(5) 0.072(5) -0.009(4) -0.037(5) -0.004(5) C3 0.074(5) 0.068(5) 0.042(4) -0.005(3) 0.001(3) -0.010(4) C4 0.043(3) 0.044(4) 0.044(3) 0.002(3) -0.001(3) -0.004(3) C5 0.043(3) 0.055(4) 0.054(4) 0.004(3) 0.007(3) -0.007(3) C6 0.043(4) 0.063(5) 0.092(5) 0.014(4) 0.006(4) -0.004(4) C7 0.037(3) 0.041(3) 0.042(3) 0.001(3) 0.005(3) -0.004(3) C8 0.037(3) 0.037(3) 0.037(3) 0.006(2) -0.002(3) 0.001(3) C9 0.039(3) 0.053(4) 0.042(3) 0.005(3) 0.008(3) -0.002(3) C10 0.055(4) 0.051(4) 0.039(3) 0.001(3) 0.002(3) 0.006(3) C11 0.058(4) 0.045(4) 0.037(3) 0.000(3) -0.004(3) -0.001(3) C12 0.041(3) 0.037(3) 0.046(3) 0.007(3) -0.009(3) 0.001(3) C13 0.033(3) 0.034(3) 0.044(3) 0.006(3) -0.003(3) 0.000(3) C14 0.038(3) 0.048(4) 0.045(3) 0.005(3) -0.002(3) -0.001(3) C15 0.041(3) 0.055(4) 0.055(4) 0.012(3) 0.007(3) -0.002(3) C16 0.042(3) 0.054(4) 0.077(5) 0.021(4) 0.001(4) -0.013(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 Ag1 N1 2.140(5) . ? Ag1 N1 2.140(5) 2_556 ? O1 C7 1.209(6) . ? N1 C16 1.293(8) . ? N1 C12 1.381(7) . ? N2 C7 1.392(7) . ? N2 C8 1.412(7) . ? N3 C7 1.359(7) . ? N3 C4 1.417(5) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C8 C9 1.354(8) . ? C8 C13 1.435(8) . ? C9 C10 1.398(8) . ? C10 C11 1.362(9) . ? C11 C12 1.405(8) . ? C12 C13 1.428(8) . ? C13 C14 1.413(8) . ? C14 C15 1.369(8) . ? C15 C16 1.393(9) . ? N4 O2 1.096(7) . ? N4 O3 1.197(8) . ? N4 O4 1.201(8) . ? O4 O3 1.786(14) 2_767 ? O3 O3 1.50(2) 2_767 ? O3 O4 1.786(14) 2_767 ? 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 180.0 . 2_556 ? C16 N1 C12 119.0(5) . . ? C16 N1 Ag1 118.3(4) . . ? C12 N1 Ag1 122.7(4) . . ? C7 N2 C8 124.4(5) . . ? C7 N3 C4 125.0(4) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 N3 122.3(3) . . ? C3 C4 N3 117.5(3) . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? O1 C7 N3 124.6(5) . . ? O1 C7 N2 123.9(5) . . ? N3 C7 N2 111.4(5) . . ? C9 C8 N2 123.5(5) . . ? C9 C8 C13 119.8(5) . . ? N2 C8 C13 116.7(5) . . ? C8 C9 C10 121.1(6) . . ? C11 C10 C9 121.6(6) . . ? C10 C11 C12 119.3(5) . . ? N1 C12 C11 119.8(5) . . ? N1 C12 C13 120.1(5) . . ? C11 C12 C13 120.1(5) . . ? C14 C13 C12 118.1(5) . . ? C14 C13 C8 123.8(5) . . ? C12 C13 C8 118.1(5) . . ? C15 C14 C13 119.6(5) . . ? C14 C15 C16 118.3(6) . . ? N1 C16 C15 124.9(5) . . ? O2 N4 O3 116.8(8) . . ? O2 N4 O4 126.8(9) . . ? O3 N4 O4 115.2(8) . . ? N4 O4 O3 76.5(8) . 2_767 ? N4 O3 O3 89.0(9) . 2_767 ? N4 O3 O4 160.5(12) . 2_767 ? O3 O3 O4 75.5(7) 2_767 2_767 ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.534 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.102 # Attachment 'Form IV.cif' data_meoh_giallr1 _database_code_depnum_ccdc_archive 'CCDC 801413' #TrackingRef 'Form IV.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Ag N7 O5' _chemical_formula_weight 696.47 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' 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 7.6870(3) _cell_length_b 10.5157(4) _cell_length_c 18.9647(8) _cell_angle_alpha 100.092(3) _cell_angle_beta 101.640(3) _cell_angle_gamma 99.170(3) _cell_volume 1447.79(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4006 _cell_measurement_theta_min 2.6671 _cell_measurement_theta_max 28.9284 _exptl_crystal_description prism _exptl_crystal_colour 'bright yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.065 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98637 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10982 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.99 _reflns_number_total 6475 _reflns_number_gt 3237 _reflns_threshold_expression >2\s(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 44.00 71.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 179.0000 90.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega -12.00 80.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 77.0000 -30.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -46.00 25.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 -77.0000 90.0000 71 #__ type_ start__ end____ width___ exp.time_ 4 omega 53.00 91.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 -152.0000 157.0000 38 #__ type_ start__ end____ width___ exp.time_ 5 omega 16.00 59.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 38.0000 -180.0000 43 #__ type_ start__ end____ width___ exp.time_ 6 omega -52.00 46.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 18.0642 -77.0000 -150.0000 98 ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0086P)^2^+0.0828P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6475 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _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 0.25821(3) 0.08556(2) 0.450941(14) 0.05692(9) Uani 1 1 d . . . N1 N 0.0270(2) -0.0572(2) 0.37521(13) 0.0425(6) Uani 1 1 d . . . N2 N -0.3142(3) -0.5126(2) 0.30271(15) 0.0457(7) Uani 1 1 d . . . N3 N -0.3643(3) -0.7014(2) 0.21533(13) 0.0457(7) Uani 1 1 d . . . O1 O -0.1183(2) -0.53852(16) 0.22699(9) 0.0475(5) Uani 1 1 d . . . C1 C -0.1667(4) -0.8199(3) 0.15395(17) 0.0592(9) Uani 1 1 d . . . H1 H -0.0659 -0.7532 0.1767 0.071 Uiso 1 1 calc R . . C2 C -0.1497(4) -0.9314(3) 0.10786(19) 0.0738(10) Uani 1 1 d . . . H2 H -0.0366 -0.9382 0.0989 0.089 Uiso 1 1 calc R . . C3 C -0.2954(5) -1.0332(3) 0.07461(16) 0.0677(10) Uani 1 1 d . . . H3 H -0.2815 -1.1082 0.0438 0.081 Uiso 1 1 calc R . . C4 C -0.4621(4) -1.0214(3) 0.08797(16) 0.0608(9) Uani 1 1 d . . . H4 H -0.5619 -1.0896 0.0665 0.073 Uiso 1 1 calc R . . C5 C -0.4820(3) -0.9101(3) 0.13254(15) 0.0472(8) Uani 1 1 d . . . H5 H -0.5958 -0.9027 0.1405 0.057 Uiso 1 1 calc R . . C6 C -0.3347(3) -0.8083(3) 0.16592(15) 0.0397(7) Uani 1 1 d . . . C7 C -0.2548(3) -0.5820(3) 0.24646(16) 0.0383(7) Uani 1 1 d . . . C8 C -0.1998(3) -0.4039(3) 0.35655(17) 0.0398(7) Uani 1 1 d . . . C9 C -0.1464(3) -0.4161(3) 0.42772(16) 0.0466(8) Uani 1 1 d . . . H9 H -0.1825 -0.4961 0.4403 0.056 Uiso 1 1 calc R . . C10 C -0.0377(3) -0.3097(3) 0.48228(15) 0.0468(8) Uani 1 1 d . . . H10 H -0.0062 -0.3186 0.5309 0.056 Uiso 1 1 calc R . . C11 C 0.0219(3) -0.1932(3) 0.46420(15) 0.0442(8) Uani 1 1 d . . . H11 H 0.0987 -0.1244 0.5001 0.053 Uiso 1 1 calc R . . C12 C -0.0321(3) -0.1768(3) 0.39166(15) 0.0332(7) Uani 1 1 d . . . C13 C -0.1507(3) -0.2817(3) 0.33731(15) 0.0341(7) Uani 1 1 d . . . C14 C -0.2171(3) -0.2562(3) 0.26700(15) 0.0432(8) Uani 1 1 d . . . H14 H -0.2972 -0.3221 0.2304 0.052 Uiso 1 1 calc R . . C15 C -0.1638(3) -0.1355(3) 0.25305(16) 0.0484(8) Uani 1 1 d . . . H15 H -0.2098 -0.1167 0.2077 0.058 Uiso 1 1 calc R . . C16 C -0.0378(3) -0.0399(3) 0.30869(17) 0.0495(8) Uani 1 1 d . . . H16 H 0.0025 0.0410 0.2978 0.059 Uiso 1 1 calc R . . H2N H -0.376(3) -0.557(2) 0.3259(14) 0.060(10) Uiso 1 1 d . . . H3N H -0.450(2) -0.711(2) 0.2295(12) 0.016(7) Uiso 1 1 d . . . N4 N 0.4760(2) 0.2094(2) 0.54102(12) 0.0406(6) Uani 1 1 d . . . N5 N 0.8585(3) 0.3144(3) 0.78984(13) 0.0430(7) Uani 1 1 d . . . N6 N 1.0690(3) 0.4006(3) 0.89809(14) 0.0456(7) Uani 1 1 d . . . O2 O 0.8849(2) 0.20016(19) 0.88251(10) 0.0578(6) Uani 1 1 d . . . C17 C 1.3596(4) 0.4882(3) 1.11817(17) 0.0632(10) Uani 1 1 d . . . H17 H 1.4256 0.5087 1.1669 0.076 Uiso 1 1 calc R . . C18 C 1.2394(4) 0.3705(3) 1.09002(18) 0.0597(9) Uani 1 1 d . . . H18 H 1.2236 0.3112 1.1204 0.072 Uiso 1 1 calc R . . C19 C 1.1410(3) 0.3377(3) 1.01754(16) 0.0486(8) Uani 1 1 d . . . H19 H 1.0600 0.2572 0.9997 0.058 Uiso 1 1 calc R . . C20 C 1.1629(3) 0.4242(3) 0.97197(16) 0.0393(7) Uani 1 1 d . . . C21 C 1.2847(3) 0.5449(3) 1.00053(16) 0.0513(8) Uani 1 1 d . . . H21 H 1.3007 0.6048 0.9705 0.062 Uiso 1 1 calc R . . C22 C 1.3809(3) 0.5753(3) 1.07295(17) 0.0587(9) Uani 1 1 d . . . H22 H 1.4613 0.6559 1.0915 0.070 Uiso 1 1 calc R . . C23 C 0.9336(3) 0.2962(3) 0.85949(15) 0.0404(7) Uani 1 1 d . . . C24 C 0.7222(3) 0.2262(3) 0.73402(15) 0.0370(7) Uani 1 1 d . . . C25 C 0.6473(3) 0.1033(3) 0.74203(15) 0.0471(8) Uani 1 1 d . . . H25 H 0.6821 0.0773 0.7863 0.057 Uiso 1 1 calc R . . C26 C 0.5181(3) 0.0174(3) 0.68286(17) 0.0530(9) Uani 1 1 d . . . H26 H 0.4667 -0.0649 0.6890 0.064 Uiso 1 1 calc R . . C27 C 0.4657(3) 0.0510(3) 0.61677(16) 0.0465(8) Uani 1 1 d . . . H27 H 0.3839 -0.0096 0.5779 0.056 Uiso 1 1 calc R . . C28 C 0.6651(3) 0.2672(3) 0.66653(15) 0.0326(7) Uani 1 1 d . . . C29 C 0.5347(3) 0.1763(3) 0.60732(16) 0.0355(7) Uani 1 1 d . . . C30 C 0.7282(3) 0.3925(2) 0.65400(15) 0.0381(7) Uani 1 1 d . . . H30 H 0.8102 0.4554 0.6916 0.046 Uiso 1 1 calc R . . C31 C 0.6704(3) 0.4222(3) 0.58757(16) 0.0433(8) Uani 1 1 d . . . H31 H 0.7149 0.5041 0.5788 0.052 Uiso 1 1 calc R . . C32 C 0.5425(3) 0.3274(3) 0.53229(15) 0.0457(8) Uani 1 1 d . . . H32 H 0.5026 0.3491 0.4871 0.055 Uiso 1 1 calc R . . H5N H 0.899(3) 0.380(2) 0.7810(13) 0.036(9) Uiso 1 1 d . . . H6N H 1.090(3) 0.454(2) 0.8745(13) 0.035(9) Uiso 1 1 d . . . N7 N 0.3113(4) 0.2703(2) 0.32678(17) 0.0578(8) Uani 1 1 d . . . O3 O 0.1906(3) 0.2510(2) 0.36054(12) 0.0811(7) Uani 1 1 d . . . O4 O 0.4734(3) 0.2991(2) 0.36153(11) 0.0693(6) Uani 1 1 d . . . O5 O 0.2764(3) 0.2660(3) 0.25991(13) 0.0956(9) 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 0.04333(13) 0.04914(15) 0.05991(18) -0.00329(12) -0.00536(10) -0.00505(10) N1 0.0367(13) 0.0360(15) 0.0486(18) 0.0024(12) 0.0052(11) 0.0024(11) N2 0.0479(15) 0.0366(15) 0.046(2) -0.0007(14) 0.0163(13) -0.0077(13) N3 0.0354(15) 0.0399(17) 0.056(2) -0.0020(14) 0.0178(13) -0.0034(14) O1 0.0401(10) 0.0401(12) 0.0576(14) 0.0032(10) 0.0171(9) -0.0048(10) C1 0.056(2) 0.047(2) 0.070(3) -0.0020(19) 0.0202(17) 0.0075(17) C2 0.070(2) 0.069(3) 0.091(3) 0.008(2) 0.038(2) 0.025(2) C3 0.107(3) 0.046(2) 0.050(3) 0.0016(18) 0.018(2) 0.024(2) C4 0.078(2) 0.043(2) 0.046(2) -0.0011(17) -0.0035(17) 0.0041(19) C5 0.0487(17) 0.0337(17) 0.053(2) 0.0035(16) 0.0082(14) 0.0004(15) C6 0.0455(17) 0.0346(17) 0.038(2) 0.0060(15) 0.0086(14) 0.0078(15) C7 0.0355(16) 0.0323(18) 0.041(2) 0.0061(16) 0.0007(14) 0.0030(15) C8 0.0312(14) 0.0374(18) 0.049(2) 0.0027(16) 0.0129(14) 0.0035(14) C9 0.0509(18) 0.0430(19) 0.048(2) 0.0143(17) 0.0123(15) 0.0089(15) C10 0.0483(17) 0.057(2) 0.037(2) 0.0129(17) 0.0100(14) 0.0139(16) C11 0.0326(15) 0.050(2) 0.041(2) -0.0069(16) 0.0045(13) 0.0079(15) C12 0.0239(14) 0.0338(17) 0.039(2) 0.0007(15) 0.0071(12) 0.0069(13) C13 0.0264(14) 0.0355(17) 0.037(2) 0.0021(15) 0.0082(12) 0.0026(13) C14 0.0317(15) 0.0450(19) 0.044(2) 0.0032(16) 0.0012(13) -0.0011(14) C15 0.0464(17) 0.047(2) 0.045(2) 0.0102(16) -0.0001(14) 0.0034(15) C16 0.0455(17) 0.049(2) 0.052(2) 0.0094(18) 0.0091(15) 0.0070(15) N4 0.0368(12) 0.0356(15) 0.0408(17) -0.0019(12) 0.0024(11) 0.0023(11) N5 0.0426(14) 0.0435(17) 0.0380(19) 0.0111(14) 0.0048(12) -0.0020(14) N6 0.0447(15) 0.0479(17) 0.0400(19) 0.0139(15) 0.0057(12) -0.0022(13) O2 0.0662(13) 0.0488(13) 0.0513(15) 0.0196(12) 0.0020(10) -0.0040(11) C17 0.0520(19) 0.077(3) 0.048(2) 0.001(2) -0.0111(16) 0.0207(19) C18 0.061(2) 0.072(2) 0.051(3) 0.021(2) 0.0076(17) 0.0247(18) C19 0.0485(17) 0.049(2) 0.043(2) 0.0072(17) -0.0015(15) 0.0125(15) C20 0.0312(15) 0.053(2) 0.033(2) 0.0037(16) 0.0043(13) 0.0158(15) C21 0.0409(16) 0.057(2) 0.054(2) 0.0104(18) 0.0089(15) 0.0068(15) C22 0.0450(17) 0.061(2) 0.056(3) -0.002(2) -0.0034(16) 0.0053(16) C23 0.0381(16) 0.049(2) 0.031(2) 0.0019(17) 0.0071(14) 0.0095(16) C24 0.0299(14) 0.0372(18) 0.041(2) 0.0010(15) 0.0095(13) 0.0044(14) C25 0.0470(17) 0.045(2) 0.048(2) 0.0134(17) 0.0109(14) -0.0006(15) C26 0.0467(17) 0.0339(18) 0.071(3) 0.0082(18) 0.0114(17) -0.0057(15) C27 0.0326(15) 0.0392(19) 0.058(2) -0.0001(16) 0.0022(14) 0.0012(14) C28 0.0253(13) 0.0327(17) 0.036(2) -0.0027(14) 0.0069(12) 0.0064(13) C29 0.0256(14) 0.0379(18) 0.040(2) -0.0006(15) 0.0078(13) 0.0071(13) C30 0.0322(14) 0.0348(17) 0.041(2) -0.0017(14) 0.0039(13) 0.0062(13) C31 0.0410(16) 0.0351(17) 0.049(2) 0.0069(16) 0.0050(14) 0.0031(14) C32 0.0431(16) 0.047(2) 0.043(2) 0.0079(16) 0.0015(14) 0.0083(15) N7 0.0623(19) 0.0369(16) 0.069(2) 0.0050(16) 0.0230(17) -0.0065(15) O3 0.0842(15) 0.0583(15) 0.097(2) 0.0004(13) 0.0555(14) -0.0224(13) O4 0.0700(14) 0.0729(15) 0.0595(17) 0.0121(13) 0.0120(12) 0.0046(13) O5 0.0650(14) 0.163(3) 0.0505(18) 0.0181(18) 0.0089(12) 0.0100(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.1883(19) . ? Ag1 N1 2.1997(19) . ? N1 C16 1.315(3) . ? N1 C12 1.378(3) . ? N2 C7 1.382(3) . ? N2 C8 1.425(3) . ? N3 C7 1.355(3) . ? N3 C6 1.412(3) . ? O1 C7 1.228(3) . ? C1 C6 1.376(3) . ? C1 C2 1.375(4) . ? C2 C3 1.376(4) . ? C3 C4 1.376(4) . ? C4 C5 1.368(4) . ? C5 C6 1.384(3) . ? C8 C9 1.364(3) . ? C8 C13 1.412(3) . ? C9 C10 1.403(3) . ? C10 C11 1.363(3) . ? C11 C12 1.404(3) . ? C12 C13 1.418(3) . ? C13 C14 1.416(3) . ? C14 C15 1.358(3) . ? C15 C16 1.403(3) . ? N4 C32 1.317(3) . ? N4 C29 1.371(3) . ? N5 C23 1.390(3) . ? N5 C24 1.406(3) . ? N6 C23 1.368(3) . ? N6 C20 1.399(3) . ? O2 C23 1.205(3) . ? C17 C18 1.369(4) . ? C17 C22 1.373(4) . ? C18 C19 1.383(3) . ? C19 C20 1.374(3) . ? C20 C21 1.398(3) . ? C21 C22 1.377(3) . ? C24 C25 1.375(3) . ? C24 C28 1.430(3) . ? C25 C26 1.404(3) . ? C26 C27 1.362(3) . ? C27 C29 1.396(3) . ? C28 C30 1.406(3) . ? C28 C29 1.430(3) . ? C30 C31 1.356(3) . ? C31 C32 1.401(3) . ? N7 O5 1.233(3) . ? N7 O3 1.240(3) . ? N7 O4 1.248(3) . ? 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 N1 169.95(9) . . ? C16 N1 C12 118.2(2) . . ? C16 N1 Ag1 120.64(17) . . ? C12 N1 Ag1 120.28(17) . . ? C7 N2 C8 122.7(2) . . ? C7 N3 C6 129.4(3) . . ? C6 C1 C2 119.2(3) . . ? C3 C2 C1 121.8(3) . . ? C4 C3 C2 118.4(3) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 120.7(3) . . ? C1 C6 C5 119.3(3) . . ? C1 C6 N3 123.4(3) . . ? C5 C6 N3 117.1(3) . . ? O1 C7 N3 124.4(3) . . ? O1 C7 N2 123.1(2) . . ? N3 C7 N2 112.6(2) . . ? C9 C8 C13 120.0(3) . . ? C9 C8 N2 119.8(3) . . ? C13 C8 N2 120.1(3) . . ? C8 C9 C10 121.0(3) . . ? C11 C10 C9 120.1(3) . . ? C10 C11 C12 120.3(2) . . ? N1 C12 C11 119.1(2) . . ? N1 C12 C13 121.2(2) . . ? C11 C12 C13 119.6(2) . . ? C8 C13 C14 123.7(2) . . ? C8 C13 C12 118.6(3) . . ? C14 C13 C12 117.7(2) . . ? C15 C14 C13 120.0(2) . . ? C14 C15 C16 118.5(3) . . ? N1 C16 C15 124.2(3) . . ? C32 N4 C29 118.7(2) . . ? C32 N4 Ag1 116.79(18) . . ? C29 N4 Ag1 124.21(16) . . ? C23 N5 C24 127.5(3) . . ? C23 N6 C20 128.1(3) . . ? C18 C17 C22 118.7(3) . . ? C17 C18 C19 121.6(3) . . ? C20 C19 C18 119.9(3) . . ? C19 C20 C21 118.8(3) . . ? C19 C20 N6 124.2(3) . . ? C21 C20 N6 117.0(3) . . ? C22 C21 C20 120.2(3) . . ? C17 C22 C21 120.9(3) . . ? O2 C23 N6 124.6(3) . . ? O2 C23 N5 123.9(3) . . ? N6 C23 N5 111.5(2) . . ? C25 C24 N5 122.3(3) . . ? C25 C24 C28 120.1(2) . . ? N5 C24 C28 117.5(2) . . ? C24 C25 C26 119.5(3) . . ? C27 C26 C25 122.1(2) . . ? C26 C27 C29 120.0(2) . . ? C30 C28 C29 117.0(2) . . ? C30 C28 C24 124.4(2) . . ? C29 C28 C24 118.6(2) . . ? N4 C29 C27 119.0(2) . . ? N4 C29 C28 121.4(2) . . ? C27 C29 C28 119.6(3) . . ? C31 C30 C28 120.6(2) . . ? C30 C31 C32 118.9(3) . . ? N4 C32 C31 123.4(3) . . ? O5 N7 O3 122.1(3) . . ? O5 N7 O4 118.5(3) . . ? O3 N7 O4 119.4(3) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.295 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.056