# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author 'Maw-Cherng Suen' _publ_contact_author_email sun@nanya.edu.tw _publ_contact_author_name 'Maw-Cherng Suen' _publ_author_name 'Maw-Cherng Suen' data_L1 _database_code_depnum_ccdc_archive 'CCDC 612141' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N4' _chemical_formula_weight 236.28 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.8273(6) _cell_length_b 12.2630(11) _cell_length_c 7.4173(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.954(2) _cell_angle_gamma 90.00 _cell_volume 615.03(10) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.9579 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3488 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0113 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.03 _reflns_number_total 1269 _reflns_number_gt 1147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.1425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.041(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1269 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 N1 N 0.8840(3) 0.2500 1.4152(2) 0.0431(4) Uani 1 2 d S . . N2 N 0.2306(2) 0.2500 0.7093(2) 0.0390(4) Uani 1 2 d S . . H2A H 0.1041 0.2500 0.6812 0.047 Uiso 1 2 calc SR . . N3 N 0.7136(2) -0.03262(13) 0.8224(3) 0.0732(5) Uani 1 1 d . . . C1 C 0.6894(3) 0.2500 1.3580(3) 0.0435(5) Uani 1 2 d S . . H1A H 0.6039 0.2500 1.4454 0.052 Uiso 1 2 calc SR . . C2 C 0.6079(3) 0.2500 1.1769(3) 0.0398(5) Uani 1 2 d S . . H2B H 0.4713 0.2500 1.1446 0.048 Uiso 1 2 calc SR . . C3 C 0.7310(2) 0.2500 1.0444(2) 0.0307(4) Uani 1 2 d S . . C4 C 0.9316(3) 0.2500 1.1016(3) 0.0524(6) Uani 1 2 d S . . H4A H 1.0204 0.2500 1.0172 0.063 Uiso 1 2 calc SR . . C5 C 0.9993(3) 0.2500 1.2865(3) 0.0577(7) Uani 1 2 d S . . H5A H 1.1354 0.2500 1.3224 0.069 Uiso 1 2 calc SR . . C6 C 0.6487(2) 0.2500 0.8423(2) 0.0310(4) Uani 1 2 d S . . H6A H 0.7604 0.2500 0.7724 0.037 Uiso 1 2 calc SR . . C7 C 0.52462(19) 0.14921(10) 0.79009(16) 0.0336(4) Uani 1 1 d . . . C8 C 0.32803(19) 0.15172(11) 0.73091(16) 0.0356(4) Uani 1 1 d . . . C9 C 0.6251(2) 0.04741(12) 0.8073(2) 0.0451(4) Uani 1 1 d . . . C10 C 0.2039(2) 0.05296(13) 0.6835(2) 0.0533(5) Uani 1 1 d . . . H10A H 0.2845 -0.0112 0.7042 0.080 Uiso 1 1 calc R . . H10B H 0.1476 0.0562 0.5576 0.080 Uiso 1 1 calc R . . H10C H 0.0998 0.0503 0.7581 0.080 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 N1 0.0427(9) 0.0515(10) 0.0312(8) 0.000 -0.0082(7) 0.000 N2 0.0274(7) 0.0462(10) 0.0399(9) 0.000 -0.0083(6) 0.000 N3 0.0614(9) 0.0482(9) 0.1076(14) -0.0012(8) 0.0030(9) 0.0131(7) C1 0.0403(10) 0.0610(13) 0.0287(9) 0.000 0.0034(7) 0.000 C2 0.0286(8) 0.0568(12) 0.0323(9) 0.000 -0.0012(7) 0.000 C3 0.0306(8) 0.0321(9) 0.0271(8) 0.000 -0.0034(6) 0.000 C4 0.0293(10) 0.0913(18) 0.0354(10) 0.000 0.0004(8) 0.000 C5 0.0305(10) 0.0987(19) 0.0399(11) 0.000 -0.0093(8) 0.000 C6 0.0279(8) 0.0390(9) 0.0251(8) 0.000 -0.0002(6) 0.000 C7 0.0351(7) 0.0374(7) 0.0268(6) -0.0018(5) -0.0010(5) 0.0010(5) C8 0.0359(7) 0.0425(8) 0.0264(6) -0.0013(5) -0.0027(5) -0.0030(5) C9 0.0406(7) 0.0422(8) 0.0505(8) -0.0038(6) -0.0011(6) 0.0013(6) C10 0.0477(8) 0.0482(9) 0.0590(9) -0.0029(7) -0.0110(7) -0.0110(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 N1 C5 1.319(3) . ? N1 C1 1.337(3) . ? N2 C8 1.3752(15) . ? N2 C8 1.3752(15) 4_565 ? N3 C9 1.150(2) . ? C1 C2 1.381(3) . ? C2 C3 1.379(3) . ? C3 C4 1.376(3) . ? C3 C6 1.526(2) . ? C4 C5 1.386(3) . ? C6 C7 1.5182(15) . ? C6 C7 1.5182(15) 4_565 ? C7 C8 1.3535(19) . ? C7 C9 1.4218(18) . ? C8 C10 1.4920(19) . ? 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 C5 N1 C1 115.91(16) . . ? C8 N2 C8 122.42(15) . 4_565 ? N1 C1 C2 123.87(18) . . ? C3 C2 C1 119.34(17) . . ? C4 C3 C2 117.33(16) . . ? C4 C3 C6 121.20(16) . . ? C2 C3 C6 121.47(15) . . ? C3 C4 C5 119.13(19) . . ? N1 C5 C4 124.42(18) . . ? C7 C6 C7 109.00(14) . 4_565 ? C7 C6 C3 111.55(9) . . ? C7 C6 C3 111.55(9) 4_565 . ? C8 C7 C9 119.59(12) . . ? C8 C7 C6 123.89(11) . . ? C9 C7 C6 116.52(11) . . ? C7 C8 N2 119.98(12) . . ? C7 C8 C10 124.29(12) . . ? N2 C8 C10 115.73(12) . . ? N3 C9 C7 177.20(15) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.275 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.041 data_3 _database_code_depnum_ccdc_archive 'CCDC 612142' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 Ag N5 O5' _chemical_formula_sum 'C14 H15 Ag N5 O4.50' _chemical_formula_weight 433.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.1806(19) _cell_length_b 16.9307(9) _cell_length_c 11.4029(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.485(14) _cell_angle_gamma 90.00 _cell_volume 1637.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 12.00 _cell_measurement_theta_max 12.50 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 0.8429 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker P4 diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3052 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2864 _reflns_number_gt 2240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.1064P] 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 2864 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.60253(4) 0.18648(2) 0.69333(4) 0.05286(15) Uani 1 1 d . . . O1 O 0.5302(9) 0.1375(4) 0.8863(7) 0.137(2) Uani 1 1 d . . . O2 O 0.6499(10) 0.0586(4) 1.0328(7) 0.160(3) Uani 1 1 d . . . O3 O 0.7548(6) 0.1007(4) 0.9045(5) 0.119(2) Uani 1 1 d . . . O4 O 0.2109(5) 0.0950(3) 0.8404(4) 0.1007(15) Uani 1 1 d . . . H4B H 0.2871 0.1225 0.8334 0.121 Uiso 1 1 d R . . H4C H 0.1829 0.1214 0.8925 0.121 Uiso 1 1 d R . . O5 O 0.9143(12) -0.0373(7) 1.0087(9) 0.114(4) Uani 0.50 1 d P . . N1 N 0.6866(4) -0.2357(2) 0.7600(4) 0.0448(8) Uani 1 1 d . . . N2 N 0.0467(4) -0.0983(2) 0.4013(4) 0.0450(8) Uani 1 1 d . . . H2A H -0.0108 -0.1087 0.3234 0.054 Uiso 1 1 calc R . . N3 N 0.4687(4) 0.0815(2) 0.6014(4) 0.0482(9) Uani 1 1 d . . . N4 N 0.0653(5) -0.2049(3) 0.7923(5) 0.0696(13) Uani 1 1 d . . . N5 N 0.6597(12) 0.0927(4) 0.9495(6) 0.107(2) Uani 1 1 d . . . C1 C 0.5520(5) -0.2531(3) 0.6629(5) 0.0542(12) Uani 1 1 d . . . H1A H 0.5479 -0.2990 0.6171 0.065 Uiso 1 1 calc R . . C2 C 0.4198(5) -0.2064(3) 0.6276(5) 0.0489(11) Uani 1 1 d . . . H2B H 0.3297 -0.2203 0.5583 0.059 Uiso 1 1 calc R . . C3 C 0.4209(4) -0.1387(2) 0.6953(4) 0.0333(8) Uani 1 1 d . . . C4 C 0.5584(5) -0.1204(2) 0.7959(4) 0.0445(10) Uani 1 1 d . . . H4A H 0.5642 -0.0755 0.8445 0.057(14) Uiso 1 1 calc R . . C5 C 0.6872(5) -0.1694(3) 0.8236(5) 0.0499(11) Uani 1 1 d . . . H5A H 0.7799 -0.1555 0.8905 0.060 Uiso 1 1 calc R . . C6 C 0.2760(4) -0.0848(2) 0.6583(4) 0.0334(8) Uani 1 1 d . . . H6A H 0.2843 -0.0522 0.7316 0.040 Uiso 1 1 calc R . . C7 C 0.2652(4) -0.0309(2) 0.5483(4) 0.0336(8) Uani 1 1 d . . . C8 C 0.1596(4) -0.0403(2) 0.4281(4) 0.0364(9) Uani 1 1 d . . . C9 C 0.0237(5) -0.1399(2) 0.4962(4) 0.0431(10) Uani 1 1 d . . . C10 C 0.1236(4) -0.1327(2) 0.6172(4) 0.0380(9) Uani 1 1 d . . . C11 C 0.3771(5) 0.0313(2) 0.5752(4) 0.0366(9) Uani 1 1 d . . . C12 C 0.1561(5) 0.0078(3) 0.3169(4) 0.0500(11) Uani 1 1 d . . . H12A H 0.2209 0.0538 0.3465 0.075 Uiso 1 1 calc R . . H12B H 0.0497 0.0236 0.2678 0.075 Uiso 1 1 calc R . . H12C H 0.1955 -0.0233 0.2650 0.075 Uiso 1 1 calc R . . C13 C -0.1171(5) -0.1931(3) 0.4515(6) 0.0632(14) Uani 1 1 d . . . H13A H -0.2045 -0.1661 0.3894 0.095 Uiso 1 1 calc R . . H13B H -0.1437 -0.2078 0.5222 0.095 Uiso 1 1 calc R . . H13C H -0.0934 -0.2398 0.4142 0.095 Uiso 1 1 calc R . . C14 C 0.0924(5) -0.1734(3) 0.7140(5) 0.0485(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0448(2) 0.0426(2) 0.0731(3) -0.01365(18) 0.02466(17) -0.01395(15) O1 0.189(7) 0.098(5) 0.161(6) -0.018(4) 0.107(6) -0.030(5) O2 0.275(9) 0.119(5) 0.142(5) 0.021(4) 0.143(6) -0.013(5) O3 0.104(4) 0.184(6) 0.087(3) 0.002(4) 0.056(3) -0.025(4) O4 0.086(3) 0.099(4) 0.088(3) -0.009(3) -0.001(2) 0.004(3) O5 0.107(8) 0.139(10) 0.081(6) -0.005(6) 0.018(6) -0.032(7) N1 0.0342(18) 0.041(2) 0.058(2) 0.0092(17) 0.0165(17) 0.0057(15) N2 0.0383(18) 0.043(2) 0.048(2) -0.0109(17) 0.0099(16) -0.0031(15) N3 0.050(2) 0.0318(18) 0.063(2) -0.0052(17) 0.0227(18) -0.0084(17) N4 0.048(2) 0.065(3) 0.098(3) 0.035(3) 0.030(2) -0.002(2) N5 0.203(8) 0.059(3) 0.077(4) -0.016(3) 0.075(5) -0.041(4) C1 0.044(2) 0.046(3) 0.070(3) -0.013(2) 0.019(2) 0.008(2) C2 0.034(2) 0.049(3) 0.055(3) -0.013(2) 0.0065(19) 0.0065(18) C3 0.0278(18) 0.031(2) 0.042(2) 0.0028(16) 0.0139(16) -0.0002(15) C4 0.043(2) 0.034(2) 0.048(2) -0.0051(19) 0.0087(19) 0.0019(18) C5 0.038(2) 0.046(3) 0.054(3) 0.001(2) 0.003(2) 0.0033(19) C6 0.0288(18) 0.0278(18) 0.044(2) -0.0042(16) 0.0149(16) 0.0004(15) C7 0.0297(18) 0.0250(18) 0.047(2) -0.0032(16) 0.0159(17) 0.0007(14) C8 0.035(2) 0.031(2) 0.046(2) -0.0028(16) 0.0176(18) 0.0036(15) C9 0.030(2) 0.032(2) 0.065(3) -0.0025(19) 0.016(2) 0.0005(16) C10 0.0284(19) 0.0283(19) 0.061(3) 0.0061(18) 0.0212(18) 0.0036(15) C11 0.036(2) 0.0304(19) 0.045(2) -0.0014(17) 0.0169(17) 0.0026(17) C12 0.053(3) 0.052(3) 0.047(3) 0.006(2) 0.020(2) 0.008(2) C13 0.034(2) 0.049(3) 0.096(4) -0.005(3) 0.013(2) -0.009(2) C14 0.031(2) 0.039(2) 0.073(3) 0.013(2) 0.017(2) 0.0046(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.188(4) . ? Ag1 N1 2.231(3) 2_656 ? Ag1 N4 2.444(4) 2_556 ? O1 N5 1.362(10) . ? O2 N5 1.144(7) . ? O3 N5 1.178(8) . ? O4 H4B 0.8700 . ? O4 H4C 0.8580 . ? N1 C5 1.335(6) . ? N1 C1 1.339(6) . ? N1 Ag1 2.231(3) 2_646 ? N2 C9 1.374(6) . ? N2 C8 1.374(5) . ? N2 H2A 0.8600 . ? N3 C11 1.151(5) . ? N4 C14 1.146(6) . ? N4 Ag1 2.445(4) 2_546 ? C1 C2 1.374(6) . ? C1 H1A 0.9300 . ? C2 C3 1.379(6) . ? C2 H2B 0.9300 . ? C3 C4 1.378(5) . ? C3 C6 1.534(5) . ? C4 C5 1.380(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.523(5) . ? C6 C10 1.528(5) . ? C6 H6A 0.9800 . ? C7 C8 1.352(6) . ? C7 C11 1.421(5) . ? C8 C12 1.497(6) . ? C9 C10 1.339(6) . ? C9 C13 1.496(6) . ? C10 C14 1.420(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 N1 150.59(14) . 2_656 ? N3 Ag1 N4 113.01(14) . 2_556 ? N1 Ag1 N4 92.95(14) 2_656 2_556 ? H4B O4 H4C 104.4 . . ? C5 N1 C1 116.4(4) . . ? C5 N1 Ag1 122.9(3) . 2_646 ? C1 N1 Ag1 120.7(3) . 2_646 ? C9 N2 C8 121.5(4) . . ? C9 N2 H2A 119.3 . . ? C8 N2 H2A 119.3 . . ? C11 N3 Ag1 160.8(4) . . ? C14 N4 Ag1 137.1(5) . 2_546 ? O2 N5 O3 136.6(11) . . ? O2 N5 O1 113.0(9) . . ? O3 N5 O1 110.3(6) . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 119.8(4) . . ? C1 C2 H2B 120.1 . . ? C3 C2 H2B 120.1 . . ? C4 C3 C2 117.5(4) . . ? C4 C3 C6 121.1(3) . . ? C2 C3 C6 121.4(3) . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 123.8(4) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? C7 C6 C10 107.6(3) . . ? C7 C6 C3 111.1(3) . . ? C10 C6 C3 111.3(3) . . ? C7 C6 H6A 108.9 . . ? C10 C6 H6A 108.9 . . ? C3 C6 H6A 108.9 . . ? C8 C7 C11 119.0(4) . . ? C8 C7 C6 124.1(3) . . ? C11 C7 C6 116.9(3) . . ? C7 C8 N2 119.8(4) . . ? C7 C8 C12 124.7(4) . . ? N2 C8 C12 115.5(4) . . ? C10 C9 N2 120.9(4) . . ? C10 C9 C13 124.6(4) . . ? N2 C9 C13 114.5(4) . . ? C9 C10 C14 119.7(4) . . ? C9 C10 C6 123.4(4) . . ? C14 C10 C6 116.9(4) . . ? N3 C11 C7 177.6(4) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 178.6(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.928 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.079 data_2 _database_code_depnum_ccdc_archive 'CCDC 612143' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 Ag Cl N4 O5' _chemical_formula_weight 474.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3461(13) _cell_length_b 16.2898(15) _cell_length_c 12.2215(15) _cell_angle_alpha 90.00 _cell_angle_beta 108.782(9) _cell_angle_gamma 90.00 _cell_volume 1761.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 1.331 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.86227 _exptl_absorpt_correction_T_max 0.91107 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3272 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3076 _reflns_number_gt 1832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^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 3076 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.10797(6) 0.27909(3) -0.31974(5) 0.0627(2) Uani 1 1 d . . . Cl1 Cl 0.2078(3) 0.39401(12) -0.00696(19) 0.0710(6) Uani 1 1 d . . . O1 O 0.146(2) 0.4060(9) -0.1289(12) 0.108(6) Uani 0.50 1 d P A 1 O2 O 0.1782(17) 0.3062(7) 0.0041(10) 0.082(4) Uani 0.50 1 d P A 1 O3 O 0.348(4) 0.4010(18) 0.005(3) 0.183(12) Uani 0.50 1 d P A 1 O4 O 0.136(3) 0.4405(15) 0.049(2) 0.193(10) Uani 0.50 1 d P A 1 O1A O 0.227(3) 0.353(2) -0.093(2) 0.208(13) Uani 0.50 1 d P A 2 O2A O 0.1102(17) 0.3535(11) 0.0433(11) 0.107(5) Uani 0.50 1 d P A 2 O3A O 0.357(2) 0.4057(16) 0.0808(12) 0.093(6) Uani 0.50 1 d P A 2 O4A O 0.160(2) 0.4766(11) -0.030(2) 0.162(9) Uani 0.50 1 d P A 2 O5 O -0.2963(13) 0.0891(5) 0.3523(6) 0.161(4) Uani 1 1 d . . . H5B H -0.3121 0.0973 0.2832 0.193 Uiso 1 1 calc R . . N1 N -0.0790(5) 0.2142(3) -0.2774(5) 0.0496(13) Uani 1 1 d . . . N2 N -0.3169(6) 0.0917(3) 0.1157(4) 0.0473(13) Uani 1 1 d . . . N3 N -0.6664(7) 0.2177(4) -0.2133(5) 0.0613(16) Uani 1 1 d . . . N4 N -0.1489(7) -0.1043(3) -0.1056(5) 0.0586(15) Uani 1 1 d . . . C1 C -0.1029(8) 0.2372(4) -0.1811(7) 0.0628(19) Uani 1 1 d . . . H1A H -0.0550 0.2842 -0.1436 0.075 Uiso 1 1 calc R . . C2 C -0.1955(8) 0.1945(4) -0.1341(6) 0.0561(18) Uani 1 1 d . . . H2B H -0.2095 0.2135 -0.0665 0.067 Uiso 1 1 calc R . . C3 C -0.2672(6) 0.1248(3) -0.1845(5) 0.0355(13) Uani 1 1 d . . . C4 C -0.2434(7) 0.1008(4) -0.2846(5) 0.0450(15) Uani 1 1 d . . . H4A H -0.2908 0.0543 -0.3238 0.054 Uiso 1 1 calc R . . C5 C -0.1483(7) 0.1464(4) -0.3268(6) 0.0518(17) Uani 1 1 d . . . H5A H -0.1318 0.1285 -0.3940 0.062 Uiso 1 1 calc R . . C6 C -0.3669(6) 0.0750(3) -0.1301(5) 0.0352(13) Uani 1 1 d . . . H6A H -0.4380 0.0419 -0.1905 0.042 Uiso 1 1 calc R . . C7 C -0.4554(6) 0.1306(3) -0.0760(5) 0.0354(13) Uani 1 1 d . . . C8 C -0.4260(7) 0.1386(3) 0.0384(5) 0.0416(15) Uani 1 1 d . . . C9 C -0.2456(7) 0.0288(3) 0.0763(5) 0.0421(15) Uani 1 1 d . . . C10 C -0.2713(6) 0.0183(3) -0.0373(5) 0.0365(14) Uani 1 1 d . . . C11 C -0.5736(7) 0.1793(4) -0.1516(6) 0.0437(15) Uani 1 1 d . . . C12 C -0.5029(8) 0.1989(4) 0.0937(6) 0.0543(18) Uani 1 1 d . . . H12A H -0.4339 0.2422 0.1290 0.065 Uiso 1 1 calc R . . H12B H -0.5346 0.1714 0.1515 0.065 Uiso 1 1 calc R . . H12C H -0.5895 0.2215 0.0359 0.065 Uiso 1 1 calc R . . C13 C -0.1427(8) -0.0236(4) 0.1693(6) 0.0589(19) Uani 1 1 d . . . H13A H -0.0582 0.0086 0.2144 0.071 Uiso 1 1 calc R . . H13B H -0.1070 -0.0688 0.1349 0.071 Uiso 1 1 calc R . . H13C H -0.1968 -0.0441 0.2183 0.071 Uiso 1 1 calc R . . C14 C -0.2003(7) -0.0494(4) -0.0746(6) 0.0462(15) Uani 1 1 d . . . C15 C -0.4405(16) 0.1002(7) 0.3798(10) 0.145(5) Uani 1 1 d . . . H15A H -0.4708 0.0485 0.4031 0.174 Uiso 1 1 calc R . . H15B H -0.5181 0.1199 0.3125 0.174 Uiso 1 1 calc R . . H15C H -0.4248 0.1392 0.4414 0.174 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 0.0527(3) 0.0564(3) 0.0839(4) 0.0230(3) 0.0287(3) -0.0037(3) Cl1 0.0854(16) 0.0569(12) 0.0728(15) 0.0006(11) 0.0284(12) 0.0017(11) O1 0.20(2) 0.066(9) 0.063(9) 0.024(8) 0.053(11) -0.010(10) O2 0.123(11) 0.069(8) 0.054(7) 0.004(6) 0.028(7) -0.006(7) O3 0.13(2) 0.118(16) 0.31(4) -0.01(3) 0.09(3) -0.035(15) O4 0.23(2) 0.143(19) 0.26(3) -0.115(19) 0.14(2) 0.003(18) O1A 0.17(2) 0.29(3) 0.20(3) -0.19(3) 0.101(19) -0.04(2) O2A 0.131(12) 0.132(14) 0.078(9) 0.008(9) 0.062(9) -0.049(11) O3A 0.062(9) 0.128(13) 0.068(9) 0.003(10) -0.008(8) -0.029(8) O4A 0.165(17) 0.108(14) 0.22(2) 0.094(16) 0.074(16) 0.070(12) O5 0.306(13) 0.119(6) 0.075(5) 0.033(4) 0.085(7) 0.066(8) N1 0.041(3) 0.050(3) 0.064(4) 0.011(3) 0.025(3) -0.006(3) N2 0.061(3) 0.042(3) 0.042(3) 0.001(2) 0.021(3) 0.008(3) N3 0.053(3) 0.077(4) 0.051(4) 0.011(3) 0.014(3) 0.018(4) N4 0.072(4) 0.041(3) 0.068(4) -0.008(3) 0.030(3) 0.005(3) C1 0.062(4) 0.058(4) 0.075(5) -0.007(4) 0.031(4) -0.023(4) C2 0.066(4) 0.058(4) 0.054(4) -0.017(3) 0.032(4) -0.022(4) C3 0.033(3) 0.034(3) 0.038(4) 0.001(3) 0.010(3) 0.001(3) C4 0.049(4) 0.048(4) 0.039(4) -0.009(3) 0.016(3) -0.013(3) C5 0.054(4) 0.058(4) 0.050(4) 0.003(4) 0.026(3) 0.001(4) C6 0.034(3) 0.037(3) 0.037(3) -0.006(3) 0.014(3) -0.007(3) C7 0.036(3) 0.038(3) 0.034(4) 0.002(3) 0.013(3) -0.004(3) C8 0.045(4) 0.033(3) 0.052(4) 0.005(3) 0.023(3) 0.001(3) C9 0.047(4) 0.033(3) 0.046(4) 0.006(3) 0.014(3) -0.005(3) C10 0.038(3) 0.025(3) 0.048(4) -0.001(3) 0.015(3) -0.002(3) C11 0.039(4) 0.047(4) 0.051(4) 0.002(3) 0.022(3) -0.002(3) C12 0.063(4) 0.050(4) 0.055(4) -0.005(3) 0.026(4) 0.003(3) C13 0.070(5) 0.045(4) 0.059(4) 0.009(3) 0.018(4) 0.010(4) C14 0.054(4) 0.041(4) 0.048(4) 0.001(3) 0.022(3) -0.004(3) C15 0.211(15) 0.114(9) 0.104(9) 0.009(7) 0.043(10) 0.053(10) _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 2.194(5) 2_554 ? Ag1 N1 2.241(5) . ? Ag1 N3 2.318(6) 1_655 ? Cl1 O3 1.28(3) . ? Cl1 O1A 1.307(15) . ? Cl1 O4 1.336(15) . ? Cl1 O4A 1.416(16) . ? Cl1 O2A 1.416(11) . ? Cl1 O1 1.428(14) . ? Cl1 O3A 1.470(19) . ? Cl1 O2 1.472(11) . ? O5 C15 1.501(13) . ? N1 C1 1.321(8) . ? N1 C5 1.323(8) . ? N2 C8 1.377(8) . ? N2 C9 1.389(7) . ? N3 C11 1.136(8) . ? N3 Ag1 2.318(6) 1_455 ? N4 C14 1.137(7) . ? N4 Ag1 2.194(5) 2_544 ? C1 C2 1.373(9) . ? C2 C3 1.360(8) . ? C3 C4 1.370(8) . ? C3 C6 1.538(7) . ? C4 C5 1.379(8) . ? C6 C10 1.511(8) . ? C6 C7 1.515(8) . ? C7 C8 1.342(8) . ? C7 C11 1.430(9) . ? C8 C12 1.499(8) . ? C9 C10 1.342(8) . ? C9 C13 1.497(9) . ? C10 C14 1.435(8) . ? 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 139.3(2) 2_554 . ? N4 Ag1 N3 111.0(2) 2_554 1_655 ? N1 Ag1 N3 107.7(2) . 1_655 ? O3 Cl1 O1A 74.9(16) . . ? O3 Cl1 O4 123.7(17) . . ? O1A Cl1 O4 157.2(17) . . ? O3 Cl1 O4A 100.6(16) . . ? O1A Cl1 O4A 115.9(18) . . ? O4 Cl1 O4A 52.1(12) . . ? O3 Cl1 O2A 140.5(16) . . ? O1A Cl1 O2A 112.9(15) . . ? O4 Cl1 O2A 62.8(12) . . ? O4A Cl1 O2A 108.9(11) . . ? O3 Cl1 O1 99.7(16) . . ? O1A Cl1 O1 48.7(12) . . ? O4 Cl1 O1 110.8(15) . . ? O4A Cl1 O1 70.6(11) . . ? O2A Cl1 O1 114.5(10) . . ? O3 Cl1 O3A 37.6(15) . . ? O1A Cl1 O3A 108.3(14) . . ? O4 Cl1 O3A 93.8(13) . . ? O4A Cl1 O3A 100.6(15) . . ? O2A Cl1 O3A 109.5(9) . . ? O1 Cl1 O3A 135.6(11) . . ? O3 Cl1 O2 107.1(15) . . ? O1A Cl1 O2 70.2(15) . . ? O4 Cl1 O2 111.3(13) . . ? O4A Cl1 O2 152.2(11) . . ? O2A Cl1 O2 48.8(8) . . ? O1 Cl1 O2 101.7(7) . . ? O3A Cl1 O2 102.8(11) . . ? C1 N1 C5 116.4(5) . . ? C1 N1 Ag1 116.1(4) . . ? C5 N1 Ag1 126.3(4) . . ? C8 N2 C9 120.3(5) . . ? C11 N3 Ag1 166.4(5) . 1_455 ? C14 N4 Ag1 165.8(6) . 2_544 ? N1 C1 C2 122.7(7) . . ? C3 C2 C1 121.2(6) . . ? C2 C3 C4 116.3(5) . . ? C2 C3 C6 121.6(5) . . ? C4 C3 C6 122.1(5) . . ? C3 C4 C5 119.4(6) . . ? N1 C5 C4 123.9(6) . . ? C10 C6 C7 108.2(5) . . ? C10 C6 C3 110.6(4) . . ? C7 C6 C3 111.4(4) . . ? C8 C7 C11 118.4(5) . . ? C8 C7 C6 123.7(5) . . ? C11 C7 C6 117.8(5) . . ? C7 C8 N2 121.2(5) . . ? C7 C8 C12 124.5(6) . . ? N2 C8 C12 114.3(6) . . ? C10 C9 N2 120.4(5) . . ? C10 C9 C13 124.8(6) . . ? N2 C9 C13 114.8(5) . . ? C9 C10 C14 118.7(5) . . ? C9 C10 C6 124.4(5) . . ? C14 C10 C6 116.9(5) . . ? N3 C11 C7 178.7(7) . . ? N4 C14 C10 177.6(7) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.444 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.087 data_1 _database_code_depnum_ccdc_archive 'CCDC 612144' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C15 H16 Ag B F4 N4 O' _chemical_formula_sum 'C15 H16 Ag B F4 N4 O' _chemical_melting_point ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _diffrn_ambient_temperature 298(2) _chemical_formula_weight 463.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 9.3243(8) _cell_length_b 16.2532(8) _cell_length_c 12.1352(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.483(5) _cell_angle_gamma 90.00 _cell_volume 1733.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.50 _cell_measurement_theta_max 25.00 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.7759 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3230 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3033 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+2.1491P] 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 3033 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.39744(4) 0.78500(2) -0.18086(3) 0.06216(15) Uani 1 1 d . . . O1 O 1.1803(11) 0.4101(3) -0.1509(4) 0.180(3) Uani 1 1 d . . . H1O H 1.2532 0.4241 -0.0944 0.217 Uiso 1 1 calc R . . N1 N 0.5782(4) 0.7177(2) -0.2261(3) 0.0504(8) Uani 1 1 d . . . N2 N 0.8230(4) 0.5927(2) -0.6162(3) 0.0493(8) Uani 1 1 d . . . H2A H 0.8000 0.6019 -0.6899 0.059 Uiso 1 1 calc R . . N3 N 1.1711(5) 0.7198(3) -0.2827(4) 0.0632(10) Uani 1 1 d . . . N4 N 0.6444(4) 0.3991(2) -0.3981(3) 0.0600(10) Uani 1 1 d . . . C1 C 0.6015(5) 0.7399(3) -0.3243(4) 0.0620(12) Uani 1 1 d . . . H1A H 0.5525 0.7868 -0.3627 0.074 Uiso 1 1 calc R . . C2 C 0.6942(5) 0.6974(3) -0.3723(4) 0.0554(11) Uani 1 1 d . . . H2B H 0.7065 0.7156 -0.4412 0.066 Uiso 1 1 calc R . . C3 C 0.7686(4) 0.6275(2) -0.3173(3) 0.0365(8) Uani 1 1 d . . . C4 C 0.7455(5) 0.6046(2) -0.2157(3) 0.0463(9) Uani 1 1 d . . . H4A H 0.7940 0.5583 -0.1753 0.056 Uiso 1 1 calc R . . C5 C 0.6500(5) 0.6506(3) -0.1733(4) 0.0525(10) Uani 1 1 d . . . H5A H 0.6355 0.6336 -0.1046 0.063 Uiso 1 1 calc R . . C6 C 0.8691(4) 0.5771(2) -0.3697(3) 0.0377(8) Uani 1 1 d . . . H6A H 0.9397 0.5439 -0.3078 0.045 Uiso 1 1 calc R . . C7 C 0.7723(4) 0.5201(2) -0.4648(3) 0.0396(8) Uani 1 1 d . . . C8 C 0.7486(4) 0.5306(2) -0.5805(3) 0.0443(9) Uani 1 1 d . . . C9 C 0.9321(4) 0.6404(2) -0.5395(3) 0.0427(9) Uani 1 1 d . . . C10 C 0.9603(4) 0.6320(2) -0.4232(3) 0.0385(8) Uani 1 1 d . . . C11 C 0.6999(5) 0.4531(2) -0.4293(4) 0.0460(9) Uani 1 1 d . . . C12 C 0.6454(5) 0.4787(3) -0.6757(4) 0.0618(12) Uani 1 1 d . . . H12A H 0.6050 0.4348 -0.6420 0.093 Uiso 1 1 calc R . . H12B H 0.7015 0.4561 -0.7221 0.093 Uiso 1 1 calc R . . H12C H 0.5634 0.5119 -0.7242 0.093 Uiso 1 1 calc R . . C13 C 1.0105(6) 0.7001(3) -0.5941(4) 0.0579(11) Uani 1 1 d . . . H13A H 1.0909 0.7271 -0.5340 0.087 Uiso 1 1 calc R . . H13B H 0.9386 0.7403 -0.6379 0.087 Uiso 1 1 calc R . . H13C H 1.0522 0.6712 -0.6453 0.087 Uiso 1 1 calc R . . C14 C 1.0778(5) 0.6810(3) -0.3455(4) 0.0465(9) Uani 1 1 d . . . B1 B 1.2931(11) 0.6011(5) 0.0064(7) 0.088(2) Uani 1 1 d . . . F1A F 1.1522(14) 0.5929(8) -0.0765(7) 0.097(3) Uani 0.50 1 d P A 1 F2A F 1.3965(9) 0.6386(6) -0.0417(6) 0.091(2) Uani 0.50 1 d P A 1 F3A F 1.2923(19) 0.6347(12) 0.0970(13) 0.181(7) Uani 0.50 1 d P A 1 F4A F 1.3403(15) 0.5196(7) 0.0210(15) 0.146(6) Uani 0.50 1 d P A 1 F1B F 1.145(3) 0.5941(15) -0.001(3) 0.36(2) Uani 0.50 1 d P A 2 F2B F 1.3158(14) 0.6805(7) -0.0040(11) 0.144(4) Uani 0.50 1 d P A 2 F3B F 1.362(2) 0.5890(10) 0.1250(12) 0.177(8) Uani 0.50 1 d P A 2 F4B F 1.336(4) 0.5493(16) -0.035(3) 0.358(19) Uani 0.50 1 d P A 2 C15 C 1.0454(12) 0.4031(6) -0.1161(7) 0.165(4) Uani 1 1 d . . . H15A H 0.9574 0.4199 -0.1797 0.247 Uiso 1 1 calc R . . H15B H 1.0567 0.4378 -0.0497 0.247 Uiso 1 1 calc R . . H15C H 1.0334 0.3470 -0.0959 0.247 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 0.0525(2) 0.0577(2) 0.0821(3) -0.01961(18) 0.03014(18) 0.00482(16) O1 0.366(11) 0.115(4) 0.083(3) -0.033(3) 0.104(5) -0.073(6) N1 0.0427(18) 0.052(2) 0.061(2) -0.0092(17) 0.0242(16) 0.0015(16) N2 0.064(2) 0.0451(19) 0.0397(17) 0.0038(14) 0.0180(16) -0.0016(16) N3 0.051(2) 0.075(3) 0.063(2) -0.011(2) 0.0202(19) -0.011(2) N4 0.064(2) 0.047(2) 0.074(3) 0.0112(18) 0.030(2) -0.0085(18) C1 0.062(3) 0.057(3) 0.074(3) 0.013(2) 0.031(2) 0.027(2) C2 0.061(3) 0.060(3) 0.053(2) 0.017(2) 0.028(2) 0.022(2) C3 0.0332(17) 0.0364(19) 0.0399(19) -0.0020(15) 0.0121(15) 0.0007(15) C4 0.052(2) 0.044(2) 0.048(2) 0.0081(17) 0.0244(19) 0.0071(18) C5 0.057(2) 0.059(3) 0.050(2) -0.001(2) 0.029(2) 0.004(2) C6 0.0365(19) 0.0366(18) 0.044(2) 0.0069(15) 0.0178(16) 0.0065(15) C7 0.043(2) 0.0310(18) 0.049(2) 0.0005(16) 0.0215(17) 0.0026(15) C8 0.045(2) 0.036(2) 0.053(2) -0.0032(17) 0.0163(18) 0.0041(17) C9 0.046(2) 0.0347(19) 0.055(2) 0.0010(17) 0.0268(18) 0.0062(17) C10 0.0360(19) 0.0375(19) 0.046(2) -0.0009(16) 0.0197(16) 0.0021(15) C11 0.049(2) 0.035(2) 0.057(2) -0.0009(18) 0.0219(19) 0.0026(18) C12 0.066(3) 0.055(3) 0.059(3) -0.015(2) 0.014(2) -0.006(2) C13 0.067(3) 0.054(3) 0.065(3) 0.010(2) 0.038(2) 0.000(2) C14 0.043(2) 0.047(2) 0.054(2) -0.0002(19) 0.023(2) 0.0020(18) B1 0.120(7) 0.064(4) 0.078(5) -0.004(4) 0.033(5) -0.005(4) F1A 0.075(6) 0.103(6) 0.093(5) 0.013(4) 0.002(4) -0.021(5) F2A 0.100(5) 0.102(6) 0.082(5) 0.014(4) 0.049(4) -0.015(5) F3A 0.195(14) 0.244(18) 0.154(12) -0.138(13) 0.126(12) -0.108(13) F4A 0.130(8) 0.069(6) 0.202(14) 0.043(8) 0.006(7) 0.012(5) F1B 0.128(14) 0.165(16) 0.75(6) 0.04(3) 0.09(3) -0.007(12) F2B 0.134(9) 0.116(8) 0.133(9) 0.034(6) -0.020(7) -0.019(7) F3B 0.251(19) 0.144(12) 0.108(8) 0.066(9) 0.024(9) -0.024(10) F4B 0.52(5) 0.23(3) 0.32(3) -0.14(2) 0.13(3) 0.09(3) C15 0.220(12) 0.173(9) 0.095(6) -0.015(6) 0.044(7) -0.094(9) _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 2.182(3) 2_654 ? Ag1 N1 2.226(3) . ? Ag1 N3 2.317(4) 1_455 ? O1 C15 1.459(11) . ? N1 C1 1.331(6) . ? N1 C5 1.328(5) . ? N2 C9 1.369(5) . ? N2 C8 1.374(5) . ? N3 C14 1.137(5) . ? N3 Ag1 2.316(4) 1_655 ? N4 C11 1.145(5) . ? N4 Ag1 2.182(3) 2_644 ? C1 C2 1.378(6) . ? C2 C3 1.382(5) . ? C3 C4 1.371(5) . ? C3 C6 1.534(5) . ? C4 C5 1.387(5) . ? C6 C7 1.520(5) . ? C6 C10 1.520(5) . ? C7 C8 1.357(5) . ? C7 C11 1.423(5) . ? C8 C12 1.493(6) . ? C9 C10 1.353(5) . ? C9 C13 1.495(5) . ? C10 C14 1.426(6) . ? B1 F3A 1.230(12) . ? B1 F4B 1.12(2) . ? B1 F1B 1.36(2) . ? B1 F2B 1.321(12) . ? B1 F1A 1.369(14) . ? B1 F2A 1.420(11) . ? B1 F4A 1.387(15) . ? B1 F3B 1.380(15) . ? 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 141.91(13) 2_654 . ? N4 Ag1 N3 111.02(14) 2_654 1_455 ? N1 Ag1 N3 105.89(13) . 1_455 ? C1 N1 C5 116.7(3) . . ? C1 N1 Ag1 116.8(3) . . ? C5 N1 Ag1 125.8(3) . . ? C9 N2 C8 122.8(3) . . ? C14 N3 Ag1 165.6(4) . 1_655 ? C11 N4 Ag1 164.4(4) . 2_644 ? N1 C1 C2 123.7(4) . . ? C1 C2 C3 119.5(4) . . ? C4 C3 C2 117.0(3) . . ? C4 C3 C6 121.9(3) . . ? C2 C3 C6 121.1(3) . . ? C3 C4 C5 120.0(4) . . ? N1 C5 C4 123.1(4) . . ? C7 C6 C10 108.0(3) . . ? C7 C6 C3 110.5(3) . . ? C10 C6 C3 111.7(3) . . ? C8 C7 C11 118.6(4) . . ? C8 C7 C6 124.1(3) . . ? C11 C7 C6 117.3(3) . . ? C7 C8 N2 119.5(3) . . ? C7 C8 C12 124.8(4) . . ? N2 C8 C12 115.7(4) . . ? C10 C9 N2 119.6(3) . . ? C10 C9 C13 125.0(4) . . ? N2 C9 C13 115.4(4) . . ? C9 C10 C14 118.2(3) . . ? C9 C10 C6 124.3(3) . . ? C14 C10 C6 117.4(3) . . ? N4 C11 C7 178.3(5) . . ? N3 C14 C10 179.4(5) . . ? F3A B1 F4B 147(2) . . ? F3A B1 F1B 77.6(17) . . ? F4B B1 F1B 115(2) . . ? F3A B1 F2B 72.6(11) . . ? F4B B1 F2B 127(2) . . ? F1B B1 F2B 105.5(13) . . ? F3A B1 F1A 114.2(13) . . ? F4B B1 F1A 89.9(19) . . ? F1B B1 F1A 40.5(16) . . ? F2B B1 F1A 99.8(9) . . ? F3A B1 F2A 112.6(9) . . ? F4B B1 F2A 75.3(19) . . ? F1B B1 F2A 145.5(15) . . ? F2B B1 F2A 52.3(7) . . ? F1A B1 F2A 110.9(7) . . ? F3A B1 F4A 114.0(14) . . ? F4B B1 F4A 36(2) . . ? F1B B1 F4A 101.6(13) . . ? F2B B1 F4A 152.9(12) . . ? F1A B1 F4A 100.8(10) . . ? F2A B1 F4A 103.4(10) . . ? F3A B1 F3B 43.2(11) . . ? F4B B1 F3B 104.2(19) . . ? F1B B1 F3B 99.5(18) . . ? F2B B1 F3B 101.8(10) . . ? F1A B1 F3B 138.7(12) . . ? F2A B1 F3B 110.2(11) . . ? F4A B1 F3B 73.3(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.403 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.066 data_L2 _database_code_depnum_ccdc_archive 'CCDC 788610' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N4' _chemical_formula_weight 236.28 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 5.8153(6) _cell_length_b 12.6387(12) _cell_length_c 16.3614(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.692(2) _cell_angle_gamma 90.00 _cell_volume 1201.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.589 _cell_measurement_theta_max 1.000 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.9734 _exptl_absorpt_correction_T_max 0.9870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6702 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2360 _reflns_number_gt 1747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.1530P] 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 2360 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _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 N1 N -0.1953(3) 0.76052(12) 1.16960(9) 0.0435(4) Uani 1 1 d . . . N2 N 0.0125(2) 0.73678(11) 0.81333(8) 0.0359(4) Uani 1 1 d . . . H2A H 0.1310 0.7469 0.7848 0.043 Uiso 1 1 calc R . . N3 N -0.2688(3) 0.44493(13) 0.96357(10) 0.0497(4) Uani 1 1 d . . . N4 N -0.6117(3) 0.95615(15) 0.88773(12) 0.0618(5) Uani 1 1 d . . . C1 C 0.0029(3) 0.81286(15) 1.17120(11) 0.0425(5) Uani 1 1 d . . . H1B H 0.0706 0.8312 1.2219 0.051 Uiso 1 1 calc R . . C2 C 0.1139(3) 0.84145(16) 1.10196(12) 0.0448(5) Uani 1 1 d . . . H2B H 0.2523 0.8784 1.1059 0.054 Uiso 1 1 calc R . . C3 C 0.0154(3) 0.81413(15) 1.02677(11) 0.0413(5) Uani 1 1 d . . . H3A H 0.0861 0.8331 0.9791 0.050 Uiso 1 1 calc R . . C4 C -0.1896(3) 0.75829(12) 1.02256(9) 0.0299(4) Uani 1 1 d . . . C5 C -0.2872(3) 0.73409(13) 1.09556(10) 0.0365(4) Uani 1 1 d . . . H5A H -0.4256 0.6971 1.0933 0.044 Uiso 1 1 calc R . . C6 C -0.3045(3) 0.72311(12) 0.94111(9) 0.0307(4) Uani 1 1 d . . . H6A H -0.4640 0.7028 0.9500 0.037 Uiso 1 1 calc R . . C7 C -0.1786(3) 0.62874(12) 0.90627(10) 0.0314(4) Uani 1 1 d . . . C8 C -0.0159(3) 0.64028(13) 0.85047(10) 0.0323(4) Uani 1 1 d . . . C9 C -0.1437(3) 0.81725(13) 0.82075(10) 0.0328(4) Uani 1 1 d . . . C10 C -0.3039(3) 0.81124(13) 0.87750(10) 0.0321(4) Uani 1 1 d . . . C11 C -0.2242(3) 0.52651(13) 0.93882(10) 0.0351(4) Uani 1 1 d . . . C12 C 0.1423(3) 0.55485(15) 0.82462(11) 0.0428(5) Uani 1 1 d . . . H12A H 0.0955 0.4885 0.8471 0.064 Uiso 1 1 calc R . . H12B H 0.2967 0.5708 0.8442 0.064 Uiso 1 1 calc R . . H12C H 0.1366 0.5503 0.7660 0.064 Uiso 1 1 calc R . . C13 C -0.1229(4) 0.90652(15) 0.76175(12) 0.0460(5) Uani 1 1 d . . . H13A H -0.2348 0.9599 0.7727 0.069 Uiso 1 1 calc R . . H13B H -0.1493 0.8807 0.7069 0.069 Uiso 1 1 calc R . . H13C H 0.0288 0.9363 0.7676 0.069 Uiso 1 1 calc R . . C14 C -0.4728(3) 0.89213(14) 0.88283(11) 0.0395(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 N1 0.0553(10) 0.0478(9) 0.0279(8) -0.0006(6) 0.0076(7) -0.0066(7) N2 0.0400(9) 0.0385(8) 0.0304(8) 0.0030(6) 0.0135(6) 0.0003(6) N3 0.0534(10) 0.0387(9) 0.0571(11) 0.0046(8) 0.0041(8) -0.0078(7) N4 0.0590(12) 0.0598(11) 0.0680(13) 0.0103(9) 0.0166(9) 0.0207(9) C1 0.0500(11) 0.0466(11) 0.0304(9) -0.0071(8) -0.0021(8) 0.0020(9) C2 0.0406(10) 0.0527(11) 0.0415(10) -0.0090(9) 0.0043(8) -0.0099(8) C3 0.0424(10) 0.0514(11) 0.0311(9) -0.0041(8) 0.0115(8) -0.0100(8) C4 0.0352(9) 0.0293(8) 0.0257(8) -0.0010(6) 0.0073(6) 0.0011(7) C5 0.0420(10) 0.0382(9) 0.0299(9) -0.0006(7) 0.0091(7) -0.0063(7) C6 0.0326(9) 0.0339(9) 0.0263(8) 0.0005(6) 0.0071(6) -0.0027(7) C7 0.0383(9) 0.0295(8) 0.0266(8) -0.0012(6) 0.0026(7) -0.0018(7) C8 0.0386(9) 0.0327(9) 0.0256(8) -0.0026(6) 0.0012(7) -0.0011(7) C9 0.0385(9) 0.0329(9) 0.0271(8) 0.0009(7) 0.0030(7) -0.0009(7) C10 0.0364(9) 0.0338(9) 0.0264(8) 0.0001(7) 0.0042(7) -0.0004(7) C11 0.0383(10) 0.0341(10) 0.0329(9) -0.0019(7) 0.0028(7) -0.0042(7) C12 0.0468(11) 0.0422(10) 0.0399(10) -0.0042(8) 0.0084(8) 0.0050(8) C13 0.0546(12) 0.0463(11) 0.0381(10) 0.0121(8) 0.0127(8) 0.0017(9) C14 0.0425(10) 0.0416(10) 0.0350(10) 0.0049(7) 0.0074(7) 0.0019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.328(2) . ? N1 C5 1.343(2) . ? N2 C9 1.373(2) . ? N2 C8 1.376(2) . ? N3 C11 1.142(2) . ? N4 C14 1.149(2) . ? C1 C2 1.378(3) . ? C2 C3 1.377(3) . ? C3 C4 1.384(2) . ? C4 C5 1.381(2) . ? C4 C6 1.529(2) . ? C6 C7 1.524(2) . ? C6 C10 1.525(2) . ? C7 C8 1.353(2) . ? C7 C11 1.427(2) . ? C8 C12 1.493(2) . ? C9 C10 1.348(2) . ? C9 C13 1.494(2) . ? C10 C14 1.423(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 C1 N1 C5 116.75(15) . . ? C9 N2 C8 121.60(13) . . ? N1 C1 C2 123.64(17) . . ? C3 C2 C1 118.51(18) . . ? C2 C3 C4 119.60(16) . . ? C5 C4 C3 117.26(15) . . ? C5 C4 C6 120.60(15) . . ? C3 C4 C6 122.14(14) . . ? N1 C5 C4 124.23(17) . . ? C7 C6 C10 107.45(12) . . ? C7 C6 C4 110.83(13) . . ? C10 C6 C4 111.58(13) . . ? C8 C7 C11 119.84(15) . . ? C8 C7 C6 122.10(14) . . ? C11 C7 C6 117.90(13) . . ? C7 C8 N2 119.72(15) . . ? C7 C8 C12 124.97(15) . . ? N2 C8 C12 115.31(14) . . ? C10 C9 N2 120.05(14) . . ? C10 C9 C13 124.56(16) . . ? N2 C9 C13 115.38(14) . . ? C9 C10 C14 120.21(15) . . ? C9 C10 C6 122.35(15) . . ? C14 C10 C6 117.34(13) . . ? N3 C11 C7 177.5(2) . . ? N4 C14 C10 178.79(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.205 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.046 data_5 _database_code_depnum_ccdc_archive 'CCDC 788611' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Ag2 N10 O6' _chemical_formula_sum 'C28 H24 Ag2 N10 O6' _chemical_formula_weight 812.31 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 8.4131(6) _cell_length_b 12.2429(10) _cell_length_c 15.7364(12) _cell_angle_alpha 90.0550(10) _cell_angle_beta 98.513(2) _cell_angle_gamma 107.133(2) _cell_volume 1530.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7755 _exptl_absorpt_correction_T_max 0.8666 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8804 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.03 _reflns_number_total 5971 _reflns_number_gt 4269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; isor N9' O1' O2' O3' O4' O5' O6' flat N9' O1' O2' O3' eadp N9 N9' eadp O3 O3' SAME N9' O1' O2' O3' SAME O4' O5' O6' ; _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^)+(0.0484P)^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 5971 _refine_ls_number_parameters 470 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.027 _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 0.61760(4) 0.57757(3) 0.29327(2) 0.05009(12) Uani 1 1 d . . . Ag2 Ag 1.17471(4) 1.00654(3) 0.80209(2) 0.05292(12) Uani 1 1 d . . . N1 N 0.8133(4) 0.6200(3) 0.4091(2) 0.0376(7) Uani 1 1 d . . . N2 N 1.3179(4) 1.0110(3) 0.3859(2) 0.0450(8) Uani 1 1 d . . . H2A H 1.3296 1.0666 0.3517 0.054 Uiso 1 1 calc R . . N3 N 1.3974(5) 0.6416(3) 0.3686(3) 0.0622(11) Uani 1 1 d . . . N4 N 1.1608(5) 0.9626(4) 0.6638(3) 0.0664(12) Uani 1 1 d . B . N5 N 1.3428(4) 1.0757(3) 0.9294(2) 0.0458(9) Uani 1 1 d . B . N6 N 1.8668(4) 1.5215(3) 1.1034(2) 0.0464(9) Uani 1 1 d . B . H6A H 1.8944 1.5830 1.1357 0.056 Uiso 1 1 calc R . . N7 N 1.5320(5) 1.4148(4) 0.8297(2) 0.0617(11) Uani 1 1 d . . . N8 N 1.9779(5) 1.1654(4) 1.1381(3) 0.0700(12) Uani 1 1 d . . . N10 N 1.0058(6) 1.1936(4) 0.8140(3) 0.0594(11) Uani 1 1 d . . . C1 C 0.7724(5) 0.5665(4) 0.4795(3) 0.0464(10) Uani 1 1 d . . . H1A H 0.6669 0.5130 0.4765 0.056 Uiso 1 1 calc R C . C2 C 0.8781(6) 0.5865(4) 0.5558(3) 0.0555(12) Uani 1 1 d . . . H2B H 0.8450 0.5474 0.6040 0.067 Uiso 1 1 calc R . . C3 C 1.0357(5) 0.6657(4) 0.5609(3) 0.0483(11) Uani 1 1 d . . . H3A H 1.1106 0.6794 0.6122 0.058 Uiso 1 1 calc R C . C4 C 1.0800(4) 0.7237(3) 0.4896(2) 0.0324(8) Uani 1 1 d . . . C5 C 0.9656(4) 0.6984(3) 0.4147(2) 0.0337(8) Uani 1 1 d . . . H5A H 0.9949 0.7372 0.3658 0.040 Uiso 1 1 calc R C . C6 C 1.2509(5) 0.8161(3) 0.4944(2) 0.0352(9) Uani 1 1 d . . . H6B H 1.3304 0.7979 0.5401 0.042 Uiso 1 1 calc R C . C7 C 1.3229(4) 0.8222(3) 0.4105(2) 0.0346(9) Uani 1 1 d . . . C8 C 1.3511(5) 0.9132(3) 0.3614(3) 0.0389(9) Uani 1 1 d . . . C9 C 1.2662(5) 1.0222(3) 0.4638(3) 0.0422(10) Uani 1 1 d . . . C10 C 1.2378(5) 0.9346(3) 0.5155(3) 0.0393(9) Uani 1 1 d . B . C11 C 1.3642(5) 0.7227(4) 0.3858(3) 0.0409(9) Uani 1 1 d . . . C12 C 1.4175(6) 0.9171(4) 0.2780(3) 0.0536(12) Uani 1 1 d . . . H12A H 1.4796 0.8628 0.2773 0.080 Uiso 1 1 calc R . . H12B H 1.4903 0.9926 0.2720 0.080 Uiso 1 1 calc R . . H12C H 1.3252 0.8986 0.2313 0.080 Uiso 1 1 calc R . . C13 C 1.2500(6) 1.1380(4) 0.4824(3) 0.0583(13) Uani 1 1 d . . . H13A H 1.2277 1.1427 0.5402 0.087 Uiso 1 1 calc R . . H13B H 1.1590 1.1501 0.4428 0.087 Uiso 1 1 calc R . . H13C H 1.3529 1.1956 0.4761 0.087 Uiso 1 1 calc R . . C14 C 1.1950(5) 0.9519(4) 0.5973(3) 0.0468(11) Uani 1 1 d . . . C15 C 1.2779(5) 1.0588(4) 1.0025(3) 0.0466(10) Uani 1 1 d . . . H15A H 1.1726 1.0056 1.0013 0.056 Uiso 1 1 calc R B . C16 C 1.3579(5) 1.1156(4) 1.0789(3) 0.0474(10) Uani 1 1 d . B . H16A H 1.3085 1.0997 1.1283 0.057 Uiso 1 1 calc R . . C17 C 1.5141(5) 1.1973(3) 1.0821(2) 0.0407(9) Uani 1 1 d . . . H17A H 1.5696 1.2381 1.1332 0.049 Uiso 1 1 calc R B . C18 C 1.5852(5) 1.2166(3) 1.0072(2) 0.0336(8) Uani 1 1 d . B . C19 C 1.4951(5) 1.1534(3) 0.9342(3) 0.0420(10) Uani 1 1 d . . . H19A H 1.5433 1.1653 0.8841 0.050 Uiso 1 1 calc R B . C20 C 1.7491(5) 1.3082(3) 1.0017(2) 0.0363(9) Uani 1 1 d . . . H20A H 1.8034 1.2827 0.9578 0.044 Uiso 1 1 calc R B . C21 C 1.7180(5) 1.4210(3) 0.9750(2) 0.0391(9) Uani 1 1 d . B . C22 C 1.7723(5) 1.5184(4) 1.0249(3) 0.0415(9) Uani 1 1 d . . . C23 C 1.9197(5) 1.4312(3) 1.1333(3) 0.0411(9) Uani 1 1 d . . . C24 C 1.8712(5) 1.3319(3) 1.0858(3) 0.0395(9) Uani 1 1 d . B . C25 C 1.6193(5) 1.4201(4) 0.8942(3) 0.0449(10) Uani 1 1 d . . . C26 C 1.7374(6) 1.6283(4) 1.0002(3) 0.0563(12) Uani 1 1 d . B . H26A H 1.6674 1.6173 0.9450 0.084 Uiso 1 1 calc R . . H26B H 1.8417 1.6864 0.9975 0.084 Uiso 1 1 calc R . . H26C H 1.6808 1.6516 1.0424 0.084 Uiso 1 1 calc R . . C27 C 2.0286(6) 1.4520(4) 1.2182(3) 0.0600(13) Uani 1 1 d . B . H27A H 2.0720 1.3885 1.2302 0.090 Uiso 1 1 calc R . . H27B H 1.9640 1.4605 1.2619 0.090 Uiso 1 1 calc R . . H27C H 2.1204 1.5206 1.2177 0.090 Uiso 1 1 calc R . . C28 C 1.9310(5) 1.2401(4) 1.1167(3) 0.0489(11) Uani 1 1 d . . . N9 N 0.5320(6) 0.3075(5) 0.3058(4) 0.0491(17) Uani 0.80 1 d PD A 1 O1 O 0.6325(8) 0.3701(6) 0.2676(4) 0.0811(19) Uani 0.80 1 d PD A 1 O2 O 0.5047(10) 0.2036(6) 0.3012(5) 0.077(2) Uani 0.80 1 d PD A 1 O3 O 0.471(4) 0.3523(13) 0.3526(11) 0.150(3) Uani 0.80 1 d PD A 1 O4 O 0.9502(8) 1.0954(5) 0.8350(6) 0.100(2) Uani 0.80 1 d PD B 1 O5 O 0.9267(8) 1.2639(6) 0.8229(5) 0.085(2) Uani 0.80 1 d PD B 1 O6 O 1.1369(7) 1.2210(6) 0.7865(4) 0.0933(17) Uani 0.80 1 d PD B 1 N9' N 0.468(4) 0.305(2) 0.2989(18) 0.0491(17) Uani 0.20 1 d PDU C 2 O1' O 0.522(5) 0.372(2) 0.2460(15) 0.143(17) Uani 0.20 1 d PDU C 2 O2' O 0.422(4) 0.203(2) 0.281(2) 0.088(12) Uani 0.20 1 d PDU C 2 O3' O 0.462(15) 0.344(5) 0.366(4) 0.150(3) Uani 0.20 1 d PDU C 2 O4' O 1.021(4) 1.132(2) 0.7572(12) 0.104(9) Uani 0.20 1 d PDU B 2 O5' O 0.976(4) 1.159(3) 0.8799(16) 0.122(12) Uani 0.20 1 d PDU B 2 O6' O 1.010(4) 1.290(2) 0.7898(15) 0.090(9) Uani 0.20 1 d PDU B 2 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) 0.0536(2) 0.0393(2) -0.00175(15) -0.01296(15) 0.01397(16) Ag2 0.0599(2) 0.0546(2) 0.0397(2) -0.01028(15) 0.00219(16) 0.01292(17) N1 0.0315(17) 0.0429(18) 0.0322(17) -0.0005(14) -0.0048(14) 0.0063(14) N2 0.047(2) 0.0419(19) 0.045(2) 0.0034(16) 0.0063(17) 0.0125(16) N3 0.062(3) 0.048(2) 0.081(3) -0.006(2) 0.025(2) 0.0172(19) N4 0.059(3) 0.081(3) 0.051(2) -0.025(2) 0.009(2) 0.007(2) N5 0.046(2) 0.044(2) 0.042(2) -0.0076(16) 0.0033(17) 0.0084(16) N6 0.052(2) 0.042(2) 0.0383(19) -0.0052(15) -0.0063(17) 0.0109(16) N7 0.059(3) 0.074(3) 0.043(2) 0.011(2) -0.008(2) 0.015(2) N8 0.059(3) 0.055(3) 0.090(3) 0.023(2) -0.005(2) 0.013(2) N10 0.064(3) 0.046(3) 0.060(3) -0.009(2) -0.013(2) 0.015(2) C1 0.039(2) 0.043(2) 0.048(3) 0.004(2) 0.004(2) 0.0000(18) C2 0.058(3) 0.059(3) 0.032(2) 0.013(2) 0.002(2) -0.006(2) C3 0.050(3) 0.054(3) 0.031(2) 0.0042(19) -0.0049(19) 0.005(2) C4 0.033(2) 0.036(2) 0.0283(19) -0.0004(15) 0.0034(16) 0.0115(16) C5 0.034(2) 0.033(2) 0.032(2) 0.0034(16) 0.0034(16) 0.0077(16) C6 0.030(2) 0.042(2) 0.030(2) -0.0029(16) 0.0016(16) 0.0073(16) C7 0.0271(19) 0.040(2) 0.033(2) -0.0072(17) 0.0018(16) 0.0056(16) C8 0.028(2) 0.043(2) 0.040(2) -0.0061(18) 0.0016(17) 0.0043(17) C9 0.026(2) 0.042(2) 0.053(3) -0.011(2) -0.0044(19) 0.0064(17) C10 0.028(2) 0.045(2) 0.039(2) -0.0136(18) 0.0021(17) 0.0029(17) C11 0.035(2) 0.043(2) 0.042(2) -0.0014(19) 0.0108(18) 0.0052(18) C12 0.051(3) 0.063(3) 0.039(2) -0.003(2) 0.010(2) 0.004(2) C13 0.048(3) 0.044(3) 0.083(4) -0.013(2) 0.002(3) 0.019(2) C14 0.037(2) 0.053(3) 0.043(3) -0.020(2) 0.0038(19) 0.0047(19) C15 0.040(2) 0.044(2) 0.050(3) 0.001(2) 0.007(2) 0.0035(18) C16 0.051(3) 0.052(3) 0.040(2) 0.008(2) 0.013(2) 0.014(2) C17 0.040(2) 0.046(2) 0.031(2) -0.0007(17) -0.0011(18) 0.0094(18) C18 0.036(2) 0.037(2) 0.029(2) 0.0012(16) 0.0038(16) 0.0135(16) C19 0.045(2) 0.046(2) 0.034(2) -0.0020(18) 0.0050(19) 0.0128(19) C20 0.039(2) 0.041(2) 0.0276(19) 0.0013(16) 0.0027(17) 0.0120(17) C21 0.030(2) 0.049(2) 0.034(2) 0.0063(18) -0.0010(17) 0.0077(17) C22 0.034(2) 0.048(2) 0.044(2) 0.0108(19) 0.0102(18) 0.0112(18) C23 0.034(2) 0.046(2) 0.037(2) 0.0061(18) 0.0009(18) 0.0041(18) C24 0.032(2) 0.043(2) 0.039(2) 0.0043(18) -0.0014(17) 0.0071(17) C25 0.039(2) 0.053(3) 0.038(2) 0.0126(19) 0.005(2) 0.0067(19) C26 0.056(3) 0.052(3) 0.065(3) 0.017(2) 0.010(2) 0.022(2) C27 0.056(3) 0.066(3) 0.043(3) -0.001(2) -0.014(2) 0.006(2) C28 0.039(2) 0.044(3) 0.056(3) 0.008(2) -0.002(2) 0.006(2) N9 0.057(5) 0.040(2) 0.047(3) 0.001(2) 0.005(3) 0.012(3) O1 0.098(4) 0.053(3) 0.083(5) 0.005(3) 0.025(4) 0.004(3) O2 0.110(6) 0.043(3) 0.074(6) 0.010(3) 0.012(4) 0.017(3) O3 0.197(7) 0.084(4) 0.177(8) -0.021(5) 0.121(6) 0.011(4) O4 0.065(4) 0.063(4) 0.172(9) 0.038(4) 0.017(4) 0.021(3) O5 0.069(4) 0.063(4) 0.123(7) -0.035(4) -0.010(3) 0.030(3) O6 0.083(4) 0.104(5) 0.095(4) 0.047(4) 0.023(3) 0.027(3) N9' 0.057(5) 0.040(2) 0.047(3) 0.001(2) 0.005(3) 0.012(3) O1' 0.33(5) 0.039(12) 0.037(11) 0.006(9) -0.02(2) 0.04(2) O2' 0.14(3) 0.048(13) 0.050(13) 0.005(9) -0.022(18) 0.012(16) O3' 0.197(7) 0.084(4) 0.177(8) -0.021(5) 0.121(6) 0.011(4) O4' 0.17(3) 0.113(18) 0.044(11) -0.023(12) -0.038(14) 0.102(19) O5' 0.12(2) 0.13(3) 0.076(18) 0.046(18) -0.021(16) -0.01(2) O6' 0.17(3) 0.052(15) 0.055(14) -0.015(10) -0.021(15) 0.057(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 N7 2.165(4) 2_776 ? Ag1 N1 2.215(3) . ? Ag1 O1' 2.48(2) . ? Ag1 N3 2.638(4) 1_455 ? Ag2 N4 2.220(4) . ? Ag2 N5 2.277(3) . ? Ag2 O4' 2.328(18) . ? Ag2 N8 2.395(4) 2_877 ? Ag2 O4 2.553(7) . ? N1 C1 1.325(5) . ? N1 C5 1.346(5) . ? N2 C8 1.374(5) . ? N2 C9 1.380(5) . ? N2 H2A 0.8600 . ? N3 C11 1.149(5) . ? N3 Ag1 2.637(4) 1_655 ? N4 C14 1.142(5) . ? N5 C15 1.336(5) . ? N5 C19 1.343(5) . ? N6 C22 1.361(5) . ? N6 C23 1.367(5) . ? N6 H6A 0.8600 . ? N7 C25 1.151(5) . ? N7 Ag1 2.165(4) 2_776 ? N8 C28 1.131(6) . ? N8 Ag2 2.395(4) 2_877 ? N10 O5' 1.15(2) . ? N10 O6 1.200(6) . ? N10 O4' 1.216(18) . ? N10 O4 1.220(7) . ? N10 O6' 1.23(2) . ? N10 O5 1.252(7) . ? C1 C2 1.360(6) . ? C1 H1A 0.9300 . ? C2 C3 1.384(6) . ? C2 H2B 0.9300 . ? C3 C4 1.368(5) . ? C3 H3A 0.9300 . ? C4 C5 1.378(5) . ? C4 C6 1.536(5) . ? C5 H5A 0.9300 . ? C6 C7 1.526(5) . ? C6 C10 1.527(5) . ? C6 H6B 0.9800 . ? C7 C8 1.338(5) . ? C7 C11 1.430(6) . ? C8 C12 1.496(6) . ? C9 C10 1.333(6) . ? C9 C13 1.497(6) . ? C10 C14 1.419(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C16 1.365(6) . ? C15 H15A 0.9300 . ? C16 C17 1.392(6) . ? C16 H16A 0.9300 . ? C17 C18 1.388(5) . ? C17 H17A 0.9300 . ? C18 C19 1.375(5) . ? C18 C20 1.514(5) . ? C19 H19A 0.9300 . ? C20 C24 1.520(5) . ? C20 C21 1.528(6) . ? C20 H20A 0.9800 . ? C21 C22 1.348(6) . ? C21 C25 1.409(5) . ? C22 C26 1.498(6) . ? C23 C24 1.349(5) . ? C23 C27 1.480(6) . ? C24 C28 1.419(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N9 O3 1.176(13) . ? N9 O1 1.198(7) . ? N9 O2 1.224(6) . ? N9' O3' 1.17(2) . ? N9' O1' 1.208(17) . ? N9' O2' 1.213(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ag1 N1 163.20(14) 2_776 . ? N7 Ag1 O1' 80.0(6) 2_776 . ? N1 Ag1 O1' 114.1(7) . . ? N7 Ag1 N3 88.55(15) 2_776 1_455 ? N1 Ag1 N3 93.63(13) . 1_455 ? O1' Ag1 N3 113.5(10) . 1_455 ? N4 Ag2 N5 146.93(14) . . ? N4 Ag2 O4' 86.8(5) . . ? N5 Ag2 O4' 109.1(5) . . ? N4 Ag2 N8 105.75(16) . 2_877 ? N5 Ag2 N8 93.47(14) . 2_877 ? O4' Ag2 N8 115.6(10) . 2_877 ? N4 Ag2 O4 114.5(2) . . ? N5 Ag2 O4 92.4(2) . . ? O4' Ag2 O4 34.3(8) . . ? N8 Ag2 O4 87.90(18) 2_877 . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ag1 116.4(2) . . ? C5 N1 Ag1 125.7(3) . . ? C8 N2 C9 121.7(4) . . ? C8 N2 H2A 119.2 . . ? C9 N2 H2A 119.2 . . ? C11 N3 Ag1 140.7(3) . 1_655 ? C14 N4 Ag2 163.3(4) . . ? C15 N5 C19 116.2(3) . . ? C15 N5 Ag2 119.5(3) . . ? C19 N5 Ag2 122.7(3) . . ? C22 N6 C23 122.9(3) . . ? C22 N6 H6A 118.5 . . ? C23 N6 H6A 118.5 . . ? C25 N7 Ag1 174.3(4) . 2_776 ? C28 N8 Ag2 127.4(4) . 2_877 ? O5' N10 O6 129.9(17) . . ? O5' N10 O4' 122(2) . . ? O6 N10 O4' 63.0(17) . . ? O5' N10 O4 50.2(15) . . ? O6 N10 O4 119.0(6) . . ? O4' N10 O4 73.3(15) . . ? O5' N10 O6' 126(2) . . ? O6 N10 O6' 79.1(16) . . ? O4' N10 O6' 112.4(17) . . ? O4 N10 O6' 160.3(17) . . ? O5' N10 O5 88(2) . . ? O6 N10 O5 121.6(6) . . ? O4' N10 O5 138.1(10) . . ? O4 N10 O5 119.5(7) . . ? O6' N10 O5 43.4(14) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C1 C2 C3 119.1(4) . . ? C1 C2 H2B 120.5 . . ? C3 C2 H2B 120.5 . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 118.0(3) . . ? C3 C4 C6 120.4(3) . . ? C5 C4 C6 121.6(3) . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? C7 C6 C10 107.5(3) . . ? C7 C6 C4 112.5(3) . . ? C10 C6 C4 111.6(3) . . ? C7 C6 H6B 108.4 . . ? C10 C6 H6B 108.4 . . ? C4 C6 H6B 108.4 . . ? C8 C7 C11 119.8(4) . . ? C8 C7 C6 124.6(3) . . ? C11 C7 C6 115.6(3) . . ? C7 C8 N2 120.5(4) . . ? C7 C8 C12 124.1(4) . . ? N2 C8 C12 115.3(4) . . ? C10 C9 N2 120.1(4) . . ? C10 C9 C13 125.8(4) . . ? N2 C9 C13 114.1(4) . . ? C9 C10 C14 118.4(4) . . ? C9 C10 C6 125.0(4) . . ? C14 C10 C6 116.6(4) . . ? N3 C11 C7 177.9(5) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 178.0(5) . . ? N5 C15 C16 123.5(4) . . ? N5 C15 H15A 118.3 . . ? C16 C15 H15A 118.3 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 118.5(4) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C19 C18 C17 117.3(3) . . ? C19 C18 C20 119.5(3) . . ? C17 C18 C20 123.1(3) . . ? N5 C19 C18 125.1(4) . . ? N5 C19 H19A 117.5 . . ? C18 C19 H19A 117.5 . . ? C18 C20 C24 113.4(3) . . ? C18 C20 C21 111.1(3) . . ? C24 C20 C21 107.7(3) . . ? C18 C20 H20A 108.2 . . ? C24 C20 H20A 108.2 . . ? C21 C20 H20A 108.2 . . ? C22 C21 C25 118.7(4) . . ? C22 C21 C20 124.3(4) . . ? C25 C21 C20 116.9(4) . . ? C21 C22 N6 119.9(4) . . ? C21 C22 C26 124.6(4) . . ? N6 C22 C26 115.4(4) . . ? C24 C23 N6 119.8(4) . . ? C24 C23 C27 124.8(4) . . ? N6 C23 C27 115.4(4) . . ? C23 C24 C28 119.0(4) . . ? C23 C24 C20 124.5(4) . . ? C28 C24 C20 116.4(4) . . ? N7 C25 C21 176.4(5) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C24 177.4(5) . . ? O3 N9 O1 115.8(8) . . ? O3 N9 O2 122.3(8) . . ? O1 N9 O2 121.7(7) . . ? N10 O4 Ag2 101.9(5) . . ? O3' N9' O1' 117(3) . . ? O3' N9' O2' 123(3) . . ? O1' N9' O2' 120(2) . . ? N9' O1' Ag1 116(2) . . ? N10 O4' Ag2 115.1(11) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.579 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.084 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 788612' #TrackingRef '- Suen(4,3-ddph)-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24.50 Ag N8 O2 S0.50' _chemical_formula_weight 628.96 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' 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 8.9090(11) _cell_length_b 11.0665(14) _cell_length_c 14.3207(17) _cell_angle_alpha 99.183(2) _cell_angle_beta 101.952(2) _cell_angle_gamma 91.228(2) _cell_volume 1361.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 639 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7244 _exptl_absorpt_correction_T_max 0.8089 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7734 _diffrn_reflns_av_R_equivalents 0.2121 _diffrn_reflns_av_sigmaI/netI 0.1132 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.12 _reflns_number_total 5273 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXS-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1744P)^2^+7.9686P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.007(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5273 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0977 _refine_ls_wR_factor_ref 0.3360 _refine_ls_wR_factor_gt 0.2666 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.27324(7) 0.66408(7) 0.34288(6) 0.0551(4) Uani 1 1 d . . . S S -0.5000 0.0000 0.0000 0.0714(13) Uani 1 2 d S . . O1 O -0.6587(15) -0.0674(13) -0.0781(11) 0.058(4) Uani 0.50 1 d P . . H1A H -0.7096 -0.0149 -0.1022 0.070 Uiso 0.50 1 calc PR . . O2 O -0.5214(18) -0.0624(16) 0.0827(9) 0.060(4) Uani 0.50 1 d P . . O3 O -0.3834(19) -0.053(3) -0.0378(12) 0.091(7) Uani 0.50 1 d P . . O4 O -0.532(2) 0.1146(18) 0.0157(18) 0.093(7) Uani 0.50 1 d P . . N1 N 0.0426(8) 0.7174(8) 0.2658(7) 0.056(2) Uani 1 1 d . . . N2 N -0.3252(9) 0.3189(8) 0.0786(6) 0.052(2) Uani 1 1 d . . . H2B H -0.3218 0.2416 0.0801 0.063 Uiso 1 1 calc R . . N3 N -0.1450(11) 0.5788(10) -0.1135(8) 0.068(3) Uani 1 1 d . . . N4 N -0.5400(10) 0.6414(10) 0.2568(7) 0.062(3) Uani 1 1 d . . . N5 N 0.2774(10) 0.5215(9) 0.4406(8) 0.070(3) Uani 1 1 d . . . N6 N 0.3306(10) 0.0591(9) 0.2228(7) 0.060(2) Uani 1 1 d . . . H6A H 0.3522 0.0164 0.1721 0.071 Uiso 1 1 calc R . . N7 N -0.1128(14) 0.2553(16) 0.2924(12) 0.116(6) Uani 1 1 d . . . N8 N 0.6087(11) 0.1569(9) 0.5465(7) 0.064(3) Uani 1 1 d . . . C1 C 0.0223(10) 0.8340(10) 0.2696(9) 0.059(3) Uani 1 1 d . . . H1B H 0.0950 0.8894 0.3120 0.071 Uiso 1 1 calc R . . C2 C -0.1024(11) 0.8794(9) 0.2136(10) 0.061(3) Uani 1 1 d . . . H2C H -0.1127 0.9635 0.2177 0.073 Uiso 1 1 calc R . . C3 C -0.2105(11) 0.7976(9) 0.1517(9) 0.056(3) Uani 1 1 d . . . H3A H -0.2947 0.8256 0.1125 0.068 Uiso 1 1 calc R . . C4 C -0.1932(8) 0.6747(8) 0.1484(7) 0.040(2) Uani 1 1 d . . . C5 C -0.0640(8) 0.6375(8) 0.2057(6) 0.042(2) Uani 1 1 d . . . H5A H -0.0502 0.5540 0.2027 0.050 Uiso 1 1 calc R . . C6 C -0.3151(8) 0.5814(8) 0.0848(7) 0.044(2) Uani 1 1 d . . . H6B H -0.3923 0.6260 0.0467 0.053 Uiso 1 1 calc R . . C7 C -0.2525(8) 0.4876(9) 0.0146(6) 0.043(2) Uani 1 1 d . . . C8 C -0.2598(9) 0.3678(9) 0.0139(7) 0.047(2) Uani 1 1 d . . . C9 C -0.3966(9) 0.3916(9) 0.1413(7) 0.048(2) Uani 1 1 d . . . C10 C -0.3955(8) 0.5117(9) 0.1454(7) 0.047(2) Uani 1 1 d . . . C11 C -0.1908(10) 0.5371(9) -0.0568(8) 0.053(3) Uani 1 1 d . . . C12 C -0.1976(12) 0.2756(10) -0.0547(8) 0.054(2) Uani 1 1 d . . . H12A H -0.2594 0.2002 -0.0680 0.081 Uiso 1 1 calc R . . H12B H -0.0936 0.2612 -0.0261 0.081 Uiso 1 1 calc R . . H12C H -0.1998 0.3063 -0.1140 0.081 Uiso 1 1 calc R . . C13 C -0.4739(12) 0.3224(11) 0.2019(9) 0.063(3) Uani 1 1 d . . . H13A H -0.5439 0.3739 0.2300 0.094 Uiso 1 1 calc R . . H13B H -0.3978 0.2983 0.2525 0.094 Uiso 1 1 calc R . . H13C H -0.5294 0.2507 0.1620 0.094 Uiso 1 1 calc R . . C14 C -0.4753(9) 0.5833(9) 0.2076(8) 0.049(2) Uani 1 1 d . . . C15 C 0.2469(13) 0.5483(10) 0.5279(7) 0.057(3) Uani 1 1 d . . . H15A H 0.2431 0.6302 0.5544 0.068 Uiso 1 1 calc R . . C16 C 0.2209(16) 0.4610(12) 0.5801(9) 0.074(4) Uani 1 1 d . . . H16A H 0.2029 0.4837 0.6421 0.089 Uiso 1 1 calc R . . C17 C 0.2211(14) 0.3369(12) 0.5409(9) 0.068(3) Uani 1 1 d . . . H17A H 0.2005 0.2758 0.5749 0.081 Uiso 1 1 calc R . . C18 C 0.2529(10) 0.3084(9) 0.4503(7) 0.048(2) Uani 1 1 d . . . C19 C 0.2788(11) 0.4036(9) 0.4030(8) 0.053(2) Uani 1 1 d . . . H19A H 0.2983 0.3842 0.3411 0.063 Uiso 1 1 calc R . . C20 C 0.2462(10) 0.1756(9) 0.3985(7) 0.048(2) Uani 1 1 d . . . H20A H 0.1992 0.1227 0.4346 0.058 Uiso 1 1 calc R . . C21 C 0.1472(10) 0.1636(10) 0.2961(8) 0.054(3) Uani 1 1 d . . . C22 C 0.1907(11) 0.1107(10) 0.2158(8) 0.055(3) Uani 1 1 d . . . C23 C 0.4355(11) 0.0736(9) 0.3076(8) 0.052(2) Uani 1 1 d . . . C24 C 0.4032(10) 0.1309(8) 0.3899(7) 0.044(2) Uani 1 1 d . . . C25 C 0.0016(13) 0.2141(12) 0.2905(10) 0.072(4) Uani 1 1 d . . . C26 C 0.0971(17) 0.1017(14) 0.1156(9) 0.080(4) Uani 1 1 d . . . H26A H 0.0050 0.1448 0.1174 0.120 Uiso 1 1 calc R . . H26B H 0.0704 0.0171 0.0882 0.120 Uiso 1 1 calc R . . H26C H 0.1555 0.1375 0.0766 0.120 Uiso 1 1 calc R . . C27 C 0.5857(14) 0.0170(12) 0.3013(10) 0.070(3) Uani 1 1 d . . . H27A H 0.6624 0.0510 0.3576 0.105 Uiso 1 1 calc R . . H27B H 0.6170 0.0340 0.2443 0.105 Uiso 1 1 calc R . . H27C H 0.5735 -0.0701 0.2981 0.105 Uiso 1 1 calc R . . C28 C 0.5176(11) 0.1441(9) 0.4766(8) 0.052(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 Ag 0.0383(5) 0.0606(6) 0.0580(6) -0.0090(4) 0.0054(3) 0.0034(3) S 0.082(3) 0.088(3) 0.051(2) 0.009(2) 0.0271(19) 0.048(2) O1 0.043(7) 0.049(8) 0.067(9) -0.018(7) -0.005(6) -0.001(5) O2 0.068(9) 0.087(11) 0.036(6) 0.037(7) 0.012(6) 0.034(8) O3 0.046(9) 0.18(2) 0.045(8) -0.008(11) 0.017(7) 0.009(11) O4 0.073(12) 0.067(12) 0.111(16) -0.012(11) -0.020(12) -0.013(9) N1 0.026(3) 0.061(5) 0.065(5) -0.025(4) 0.005(3) -0.001(3) N2 0.042(4) 0.046(4) 0.065(5) -0.012(4) 0.020(4) 0.002(3) N3 0.060(5) 0.072(6) 0.083(7) 0.008(5) 0.042(5) 0.001(4) N4 0.049(4) 0.077(6) 0.059(5) -0.012(5) 0.025(4) 0.005(4) N5 0.050(5) 0.064(6) 0.079(6) -0.036(5) 0.015(4) 0.000(4) N6 0.057(5) 0.061(5) 0.056(5) -0.017(4) 0.024(4) -0.003(4) N7 0.059(7) 0.130(12) 0.124(12) -0.044(10) -0.011(7) 0.030(7) N8 0.067(5) 0.050(5) 0.060(5) -0.011(4) -0.007(5) -0.004(4) C1 0.036(4) 0.049(5) 0.080(7) -0.025(5) 0.011(4) -0.009(4) C2 0.047(5) 0.031(4) 0.098(8) 0.000(5) 0.009(5) 0.003(4) C3 0.038(4) 0.045(5) 0.080(7) -0.004(5) 0.008(4) 0.006(4) C4 0.022(3) 0.045(5) 0.050(5) -0.011(4) 0.012(3) 0.000(3) C5 0.027(4) 0.041(4) 0.050(5) -0.014(4) 0.011(3) -0.003(3) C6 0.022(3) 0.047(5) 0.052(5) -0.013(4) -0.001(3) 0.006(3) C7 0.024(3) 0.053(5) 0.043(4) -0.013(4) 0.005(3) 0.000(3) C8 0.027(4) 0.055(5) 0.050(5) -0.018(4) 0.009(3) 0.000(3) C9 0.026(4) 0.058(6) 0.053(5) -0.011(4) 0.009(3) -0.004(3) C10 0.023(3) 0.057(5) 0.052(5) -0.018(4) 0.010(3) -0.003(3) C11 0.030(4) 0.053(5) 0.067(6) -0.018(5) 0.011(4) 0.001(4) C12 0.058(5) 0.050(5) 0.055(5) -0.005(4) 0.025(4) 0.008(4) C13 0.047(5) 0.065(7) 0.074(7) -0.005(6) 0.021(5) -0.003(4) C14 0.031(4) 0.053(5) 0.059(5) -0.008(4) 0.013(4) -0.006(3) C15 0.077(7) 0.044(5) 0.045(5) -0.007(4) 0.011(5) 0.011(5) C16 0.098(9) 0.070(8) 0.047(6) -0.017(6) 0.019(6) 0.017(6) C17 0.074(7) 0.067(7) 0.053(6) -0.014(5) 0.012(5) 0.006(5) C18 0.035(4) 0.054(5) 0.047(5) -0.013(4) 0.004(4) 0.006(4) C19 0.056(5) 0.050(5) 0.050(5) -0.012(4) 0.023(4) 0.000(4) C20 0.041(4) 0.048(5) 0.052(5) -0.010(4) 0.015(4) 0.003(4) C21 0.037(4) 0.050(5) 0.062(6) -0.017(5) 0.002(4) -0.003(4) C22 0.047(5) 0.049(5) 0.060(6) -0.010(5) 0.003(4) -0.010(4) C23 0.045(5) 0.049(5) 0.059(6) -0.010(4) 0.019(4) -0.003(4) C24 0.038(4) 0.038(4) 0.050(5) -0.008(4) 0.006(4) 0.003(3) C25 0.053(6) 0.070(7) 0.074(8) -0.020(6) -0.008(5) 0.006(5) C26 0.091(9) 0.082(9) 0.049(6) -0.006(6) -0.008(6) -0.020(7) C27 0.063(6) 0.066(7) 0.081(8) -0.005(6) 0.029(6) 0.017(5) C28 0.048(5) 0.038(5) 0.064(6) -0.011(4) 0.014(5) -0.001(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 Ag N1 2.261(8) . ? Ag N4 2.263(8) 1_655 ? Ag N5 2.266(14) . ? Ag N8 2.400(8) 2_666 ? S O4 1.30(2) 2_455 ? S O4 1.30(2) . ? S O3 1.369(17) . ? S O3 1.369(17) 2_455 ? S O2 1.504(14) . ? S O2 1.504(14) 2_455 ? S O1 1.685(12) . ? S O1 1.685(12) 2_455 ? O1 H1A 0.8200 . ? O2 O4 1.61(3) 2_455 ? O2 O3 1.69(3) 2_455 ? O3 O4 1.13(3) 2_455 ? O3 O2 1.69(3) 2_455 ? O4 O3 1.13(3) 2_455 ? O4 O2 1.61(3) 2_455 ? N1 C1 1.300(15) . ? N1 C5 1.344(10) . ? N2 C8 1.365(15) . ? N2 C9 1.373(11) . ? N2 H2B 0.8600 . ? N3 C11 1.133(16) . ? N4 C14 1.131(12) . ? N4 Ag 2.263(8) 1_455 ? N5 C15 1.323(15) . ? N5 C19 1.331(13) . ? N6 C23 1.354(14) . ? N6 C22 1.374(14) . ? N6 H6A 0.8600 . ? N7 C25 1.129(16) . ? N8 C28 1.138(14) . ? N8 Ag 2.400(8) 2_666 ? C1 C2 1.384(17) . ? C1 H1B 0.9300 . ? C2 C3 1.373(14) . ? C2 H2C 0.9300 . ? C3 C4 1.367(14) . ? C3 H3A 0.9300 . ? C4 C5 1.380(13) . ? C4 C6 1.522(10) . ? C5 H5A 0.9300 . ? C6 C10 1.519(15) . ? C6 C7 1.524(10) . ? C6 H6B 0.9800 . ? C7 C8 1.324(15) . ? C7 C11 1.431(16) . ? C8 C12 1.497(11) . ? C9 C10 1.321(15) . ? C9 C13 1.500(17) . ? C10 C14 1.410(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C16 1.356(19) . ? C15 H15A 0.9300 . ? C16 C17 1.399(17) . ? C16 H16A 0.9300 . ? C17 C18 1.373(15) . ? C17 H17A 0.9300 . ? C18 C19 1.380(17) . ? C18 C20 1.531(12) . ? C19 H19A 0.9300 . ? C20 C24 1.516(12) . ? C20 C21 1.531(14) . ? C20 H20A 0.9800 . ? C21 C22 1.339(15) . ? C21 C25 1.416(15) . ? C22 C26 1.490(16) . ? C23 C24 1.335(13) . ? C23 C27 1.503(14) . ? C24 C28 1.419(14) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? 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 Ag N4 116.8(4) . 1_655 ? N1 Ag N5 118.3(3) . . ? N4 Ag N5 112.2(4) 1_655 . ? N1 Ag N8 106.6(3) . 2_666 ? N4 Ag N8 96.2(4) 1_655 2_666 ? N5 Ag N8 102.7(3) . 2_666 ? O4 S O4 179.999(2) 2_455 . ? O4 S O3 49.9(15) 2_455 . ? O4 S O3 130.1(15) . . ? O4 S O3 130.1(15) 2_455 2_455 ? O4 S O3 49.9(15) . 2_455 ? O3 S O3 179.999(2) . 2_455 ? O4 S O2 69.4(14) 2_455 . ? O4 S O2 110.6(14) . . ? O3 S O2 108.3(12) . . ? O3 S O2 71.7(12) 2_455 . ? O4 S O2 110.6(14) 2_455 2_455 ? O4 S O2 69.4(14) . 2_455 ? O3 S O2 71.7(12) . 2_455 ? O3 S O2 108.3(12) 2_455 2_455 ? O2 S O2 180.0(5) . 2_455 ? O4 S O1 76.8(9) 2_455 . ? O4 S O1 103.2(9) . . ? O3 S O1 102.9(9) . . ? O3 S O1 77.1(9) 2_455 . ? O2 S O1 95.5(9) . . ? O2 S O1 84.5(9) 2_455 . ? O4 S O1 103.2(9) 2_455 2_455 ? O4 S O1 76.8(9) . 2_455 ? O3 S O1 77.1(9) . 2_455 ? O3 S O1 102.9(9) 2_455 2_455 ? O2 S O1 84.5(9) . 2_455 ? O2 S O1 95.5(9) 2_455 2_455 ? O1 S O1 180.0(6) . 2_455 ? S O1 H1A 109.5 . . ? S O2 O4 49.3(9) . 2_455 ? S O2 O3 50.4(7) . 2_455 ? O4 O2 O3 94.6(12) 2_455 2_455 ? O4 O3 S 62.0(13) 2_455 . ? O4 O3 O2 108.7(18) 2_455 2_455 ? S O3 O2 57.9(10) . 2_455 ? O3 O4 S 68.2(17) 2_455 . ? O3 O4 O2 115.8(18) 2_455 2_455 ? S O4 O2 61.3(11) . 2_455 ? C1 N1 C5 118.3(9) . . ? C1 N1 Ag 117.0(6) . . ? C5 N1 Ag 123.9(7) . . ? C8 N2 C9 120.8(9) . . ? C8 N2 H2B 119.6 . . ? C9 N2 H2B 119.6 . . ? C14 N4 Ag 151.5(9) . 1_455 ? C15 N5 C19 117.7(12) . . ? C15 N5 Ag 121.8(8) . . ? C19 N5 Ag 119.0(8) . . ? C23 N6 C22 121.7(8) . . ? C23 N6 H6A 119.2 . . ? C22 N6 H6A 119.2 . . ? C28 N8 Ag 132.5(9) . 2_666 ? N1 C1 C2 123.1(8) . . ? N1 C1 H1B 118.5 . . ? C2 C1 H1B 118.5 . . ? C3 C2 C1 118.5(9) . . ? C3 C2 H2C 120.8 . . ? C1 C2 H2C 120.8 . . ? C4 C3 C2 119.3(10) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 118.3(8) . . ? C3 C4 C6 120.8(8) . . ? C5 C4 C6 120.9(8) . . ? N1 C5 C4 122.5(9) . . ? N1 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C10 C6 C4 111.4(8) . . ? C10 C6 C7 107.8(8) . . ? C4 C6 C7 113.7(6) . . ? C10 C6 H6B 107.9 . . ? C4 C6 H6B 107.9 . . ? C7 C6 H6B 107.9 . . ? C8 C7 C11 120.5(8) . . ? C8 C7 C6 124.3(9) . . ? C11 C7 C6 115.0(9) . . ? C7 C8 N2 121.1(7) . . ? C7 C8 C12 124.4(10) . . ? N2 C8 C12 114.5(9) . . ? C10 C9 N2 121.3(10) . . ? C10 C9 C13 124.5(8) . . ? N2 C9 C13 114.2(9) . . ? C9 C10 C14 120.0(10) . . ? C9 C10 C6 124.3(7) . . ? C14 C10 C6 115.7(9) . . ? N3 C11 C7 178.0(11) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C10 179.3(14) . . ? N5 C15 C16 122.6(10) . . ? N5 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C15 C16 C17 120.0(11) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 117.7(13) . . ? C18 C17 H17A 121.2 . . ? C16 C17 H17A 121.2 . . ? C17 C18 C19 118.1(9) . . ? C17 C18 C20 121.6(11) . . ? C19 C18 C20 120.0(9) . . ? N5 C19 C18 123.8(10) . . ? N5 C19 H19A 118.1 . . ? C18 C19 H19A 118.1 . . ? C24 C20 C21 107.7(7) . . ? C24 C20 C18 112.9(7) . . ? C21 C20 C18 109.8(9) . . ? C24 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? C18 C20 H20A 108.7 . . ? C22 C21 C25 120.6(10) . . ? C22 C21 C20 124.5(9) . . ? C25 C21 C20 114.9(9) . . ? C21 C22 N6 119.8(10) . . ? C21 C22 C26 124.9(11) . . ? N6 C22 C26 115.3(10) . . ? C24 C23 N6 121.4(9) . . ? C24 C23 C27 123.7(10) . . ? N6 C23 C27 114.8(9) . . ? C23 C24 C28 119.1(8) . . ? C23 C24 C20 123.8(8) . . ? C28 C24 C20 116.9(8) . . ? N7 C25 C21 175.6(16) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C24 178.8(10) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.868 _refine_diff_density_min -3.512 _refine_diff_density_rms 0.206