# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Maw-Cherng Sun' _publ_contact_author_email SUN@NANYA.EDU.TW _publ_section_title ; Self-Assembly of Two-dimensional Coordination Polymers from AgX(X = BF4-, ClO4-, NO3- and PF6-) and 2,6-dimethyl-3,5-dicyano-4-(6-methyl-2-pyridyl)-1,4-dihydropyridine ; loop_ _publ_author_name 'Maw-Cherng Sun' 'Yuh-Wen Ho' 'Ju-Chun Wang' 'Chun-Wei Yeh' data_1 _database_code_depnum_ccdc_archive 'CCDC 612145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 N4' _chemical_formula_weight 250.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.3722(19) _cell_length_b 15.558(4) _cell_length_c 15.257(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.475(10) _cell_angle_gamma 90.00 _cell_volume 2691.2(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.23 _cell_measurement_theta_max 12.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8524 _exptl_absorpt_correction_T_max 0.8950 _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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 497 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.65 _diffrn_reflns_number 4481 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1162 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4481 _reflns_number_gt 1993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4481 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1714 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 C1 C -0.5314(5) 0.2399(3) 1.1735(4) 0.0572(13) Uani 1 1 d . . . H1C H -0.467(4) 0.198(3) 1.182(3) 0.065(14) Uiso 1 1 d . . . H1B H -0.579(5) 0.238(4) 1.231(4) 0.15(3) Uiso 1 1 d . . . H1A H -0.572(4) 0.223(3) 1.129(3) 0.072(17) Uiso 1 1 d . . . C2 C -0.6338(5) 0.5389(4) 1.1452(4) 0.0588(13) Uani 1 1 d . . . H2C H -0.697(4) 0.525(3) 1.102(3) 0.075(15) Uiso 1 1 d . . . H2B H -0.605(4) 0.594(3) 1.138(3) 0.088(18) Uiso 1 1 d . . . H2A H -0.672(4) 0.535(3) 1.202(3) 0.087(17) Uiso 1 1 d . . . C3 C -0.2968(4) 0.2722(3) 1.1227(3) 0.0483(11) Uani 1 1 d . . . C4 C -0.4048(4) 0.5788(3) 1.0816(3) 0.0527(11) Uani 1 1 d . . . C5 C 0.1379(4) 0.2315(4) 0.8783(4) 0.0566(13) Uani 1 1 d . . . H5C H 0.183(4) 0.222(3) 0.825(3) 0.094(18) Uiso 1 1 d . . . H5B H 0.113(4) 0.293(4) 0.878(3) 0.102(19) Uiso 1 1 d . . . H5A H 0.201(5) 0.220(3) 0.923(4) 0.11(2) Uiso 1 1 d . . . C6 C 0.0303(5) -0.0673(3) 0.8512(4) 0.0573(13) Uani 1 1 d . . . H6C H 0.086(5) -0.068(4) 0.799(4) 0.15(3) Uiso 1 1 d . . . H6B H -0.033(5) -0.111(4) 0.835(4) 0.12(2) Uiso 1 1 d . . . H6A H 0.078(4) -0.091(3) 0.896(3) 0.10(2) Uiso 1 1 d . . . C7 C -0.0981(3) 0.2771(3) 0.9241(3) 0.0459(10) Uani 1 1 d . . . C8 C -0.2059(4) -0.0326(3) 0.8956(3) 0.0485(11) Uani 1 1 d . . . C12 C -0.4821(3) 0.3274(2) 1.1579(2) 0.0410(10) Uani 1 1 d . . . C13 C -0.3730(3) 0.3419(2) 1.1334(2) 0.0392(10) Uani 1 1 d . . . C14 C -0.3267(3) 0.4305(3) 1.1118(3) 0.0397(10) Uani 1 1 d . . . H14 H -0.298(2) 0.4304(19) 1.0561(19) 0.018(8) Uiso 1 1 d . . . C15 C -0.4275(3) 0.4950(2) 1.1134(2) 0.0378(9) Uani 1 1 d . . . C16 C -0.5336(3) 0.4766(3) 1.1416(2) 0.0406(10) Uani 1 1 d . . . C21 C -0.0294(4) 0.5151(3) 1.2723(4) 0.0620(14) Uani 1 1 d . . . H21 H 0.029(4) 0.533(3) 1.312(3) 0.062(13) Uiso 1 1 d . . . C22 C -0.0242(4) 0.5156(3) 1.1839(4) 0.0670(15) Uani 1 1 d . . . H22 H 0.047(4) 0.537(3) 1.156(3) 0.078(15) Uiso 1 1 d . . . C23 C -0.1198(4) 0.4861(3) 1.1305(4) 0.0572(13) Uani 1 1 d . . . H23 H -0.120(4) 0.487(3) 1.065(3) 0.095(18) Uiso 1 1 d . . . C24 C -0.2182(3) 0.4588(2) 1.1694(3) 0.0412(10) Uani 1 1 d . . . C26 C -0.1301(4) 0.4864(3) 1.3079(3) 0.0542(12) Uani 1 1 d . . . C27 C -0.1411(6) 0.4870(6) 1.4039(4) 0.090(2) Uani 1 1 d . . . H27C H -0.076(7) 0.495(5) 1.448(6) 0.20(3) Uiso 1 1 d . . . H27B H -0.192(9) 0.531(8) 1.416(8) 0.32(7) Uiso 1 1 d . . . H27A H -0.149(5) 0.426(4) 1.428(4) 0.11(2) Uiso 1 1 d . . . C32 C 0.0371(3) 0.1699(3) 0.8805(3) 0.0436(10) Uani 1 1 d . . . C33 C -0.0711(3) 0.1904(2) 0.9031(3) 0.0402(10) Uani 1 1 d . . . C34 C -0.1723(3) 0.1264(2) 0.9067(3) 0.0386(9) Uani 1 1 d . . . H34 H -0.190(3) 0.131(2) 0.968(2) 0.030(9) Uiso 1 1 d . . . C35 C -0.1266(3) 0.0380(2) 0.8880(2) 0.0378(9) Uani 1 1 d . . . C36 C -0.0162(3) 0.0211(3) 0.8666(2) 0.0410(10) Uani 1 1 d . . . C41 C -0.4658(4) 0.2062(3) 0.7392(5) 0.0671(15) Uani 1 1 d . . . H41 H -0.534(4) 0.223(3) 0.699(3) 0.089(16) Uiso 1 1 d . . . C42 C -0.4751(4) 0.2083(3) 0.8272(5) 0.0713(16) Uani 1 1 d . . . H42 H -0.552(4) 0.229(3) 0.853(3) 0.094(17) Uiso 1 1 d . . . C43 C -0.3798(4) 0.1828(3) 0.8827(4) 0.0563(12) Uani 1 1 d . . . H43 H -0.383(3) 0.174(2) 0.947(2) 0.036(10) Uiso 1 1 d . . . C44 C -0.2798(3) 0.1531(2) 0.8468(3) 0.0427(10) Uani 1 1 d . . . C46 C -0.3640(4) 0.1763(3) 0.7061(3) 0.0575(13) Uani 1 1 d . . . C47 C -0.3541(7) 0.1743(7) 0.6099(4) 0.099(3) Uani 1 1 d . . . H47C H -0.421(5) 0.165(4) 0.573(4) 0.13(2) Uiso 1 1 d . . . H47B H -0.295(5) 0.203(4) 0.591(4) 0.10(2) Uiso 1 1 d . . . H47A H -0.316(6) 0.119(5) 0.595(4) 0.15(4) Uiso 1 1 d . . . N1 N -0.2334(3) 0.2156(3) 1.1135(3) 0.0726(12) Uani 1 1 d . . . N2 N -0.3813(3) 0.6443(3) 1.0537(3) 0.0713(12) Uani 1 1 d . . . N3 N -0.1237(3) 0.3456(3) 0.9416(3) 0.0638(11) Uani 1 1 d . . . N4 N -0.2700(3) -0.0881(3) 0.9024(3) 0.0797(13) Uani 1 1 d . . . N11 N -0.5588(3) 0.3950(2) 1.1668(2) 0.0464(9) Uani 1 1 d . . . H11N H -0.623(3) 0.382(2) 1.188(2) 0.038(12) Uiso 1 1 d . . . N25 N -0.2251(3) 0.4583(2) 1.2567(2) 0.0465(9) Uani 1 1 d . . . N31 N 0.0645(3) 0.0859(2) 0.8614(2) 0.0466(9) Uani 1 1 d . . . H31N H 0.136(4) 0.072(3) 0.835(3) 0.103(19) Uiso 1 1 d . . . N45 N -0.2716(3) 0.1495(2) 0.7597(2) 0.0463(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(3) 0.042(3) 0.076(4) -0.005(3) -0.001(3) -0.009(2) C2 0.059(3) 0.061(4) 0.056(3) 0.003(3) -0.004(3) 0.015(3) C3 0.048(3) 0.045(3) 0.052(3) -0.011(2) 0.002(2) -0.004(2) C4 0.057(3) 0.052(3) 0.048(3) -0.002(2) -0.001(2) 0.006(2) C5 0.040(3) 0.064(4) 0.066(3) 0.000(3) 0.001(3) -0.012(2) C6 0.055(3) 0.052(3) 0.064(3) 0.002(3) -0.002(3) 0.017(3) C7 0.044(3) 0.042(3) 0.052(3) -0.004(2) 0.0028(19) -0.004(2) C8 0.044(3) 0.042(3) 0.058(3) 0.000(2) -0.003(2) -0.002(2) C12 0.045(3) 0.037(2) 0.040(2) -0.0019(19) -0.0025(18) 0.001(2) C13 0.045(3) 0.036(2) 0.037(2) -0.0043(18) 0.0000(18) 0.0023(19) C14 0.041(2) 0.045(3) 0.034(2) -0.0022(19) 0.0062(18) 0.0008(19) C15 0.045(2) 0.035(2) 0.033(2) 0.0033(18) -0.0049(17) 0.0000(18) C16 0.046(3) 0.039(2) 0.035(2) -0.0032(19) -0.0024(18) 0.009(2) C21 0.036(3) 0.045(3) 0.102(4) -0.016(3) -0.015(3) -0.002(2) C22 0.044(3) 0.045(3) 0.113(5) 0.005(3) 0.015(3) -0.011(2) C23 0.048(3) 0.049(3) 0.075(4) 0.011(3) 0.011(3) -0.002(2) C24 0.038(2) 0.032(2) 0.054(3) 0.0029(19) 0.0040(19) 0.0035(18) C26 0.039(3) 0.057(3) 0.064(3) -0.018(2) -0.008(2) 0.003(2) C27 0.072(4) 0.126(7) 0.069(4) -0.031(4) -0.013(3) -0.002(4) C32 0.040(2) 0.047(3) 0.042(2) -0.008(2) -0.0074(18) -0.003(2) C33 0.039(2) 0.039(2) 0.043(2) -0.0037(19) -0.0007(18) -0.0023(19) C34 0.039(2) 0.039(2) 0.038(2) -0.005(2) 0.0041(18) 0.0013(18) C35 0.038(2) 0.036(2) 0.039(2) -0.0004(18) -0.0020(17) -0.0005(18) C36 0.047(3) 0.040(2) 0.034(2) -0.0038(19) -0.0064(18) 0.007(2) C41 0.041(3) 0.042(3) 0.114(5) 0.014(3) -0.022(3) 0.001(2) C42 0.041(3) 0.052(3) 0.120(5) -0.014(3) 0.002(3) 0.006(2) C43 0.040(3) 0.058(3) 0.071(4) -0.015(3) 0.006(2) 0.006(2) C44 0.038(2) 0.033(2) 0.058(3) -0.004(2) 0.0039(19) 0.0004(18) C46 0.041(3) 0.055(3) 0.074(3) 0.023(2) -0.010(2) -0.004(2) C47 0.061(4) 0.164(8) 0.069(4) 0.039(5) -0.018(3) -0.015(5) N1 0.069(3) 0.059(3) 0.090(3) -0.008(2) 0.007(2) 0.019(2) N2 0.082(3) 0.047(3) 0.085(3) 0.012(2) 0.011(2) -0.002(2) N3 0.067(3) 0.046(2) 0.078(3) -0.006(2) 0.008(2) -0.001(2) N4 0.068(3) 0.058(3) 0.113(4) -0.004(3) 0.005(2) -0.015(2) N11 0.039(2) 0.048(2) 0.052(2) 0.0018(18) 0.0035(18) 0.0016(19) N25 0.041(2) 0.048(2) 0.050(2) -0.0110(17) 0.0011(16) -0.0033(16) N31 0.036(2) 0.049(2) 0.055(2) -0.0040(18) 0.0036(17) 0.0039(18) N45 0.0299(18) 0.058(2) 0.050(2) 0.0094(18) -0.0023(15) -0.0003(15) _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 C1 C12 1.498(6) . ? C1 H1C 0.98(4) . ? C1 H1B 1.06(6) . ? C1 H1A 0.83(5) . ? C2 C16 1.501(6) . ? C2 H2C 0.96(5) . ? C2 H2B 0.93(5) . ? C2 H2A 1.00(5) . ? C3 N1 1.154(5) . ? C3 C13 1.406(6) . ? C4 N2 1.144(5) . ? C4 C15 1.422(6) . ? C5 C32 1.497(6) . ? C5 H5C 1.01(5) . ? C5 H5B 1.00(5) . ? C5 H5A 0.97(6) . ? C6 C36 1.500(6) . ? C6 H6C 1.06(6) . ? C6 H6B 1.00(6) . ? C6 H6A 0.91(5) . ? C7 N3 1.142(5) . ? C7 C33 1.425(6) . ? C8 N4 1.140(5) . ? C8 C35 1.432(6) . ? C12 C13 1.342(5) . ? C12 N11 1.380(5) . ? C13 C14 1.521(5) . ? C14 C24 1.523(5) . ? C14 C15 1.525(5) . ? C14 H14 0.93(3) . ? C15 C16 1.343(5) . ? C16 N11 1.363(5) . ? C21 C22 1.355(7) . ? C21 C26 1.379(6) . ? C21 H21 0.91(4) . ? C22 C23 1.384(7) . ? C22 H22 1.00(4) . ? C23 C24 1.375(5) . ? C23 H23 1.00(5) . ? C24 N25 1.339(5) . ? C26 N25 1.355(5) . ? C26 C27 1.480(7) . ? C27 H27C 0.96(8) . ? C27 H27B 0.92(11) . ? C27 H27A 1.02(6) . ? C32 C33 1.342(5) . ? C32 N31 1.379(5) . ? C33 C34 1.526(5) . ? C34 C35 1.505(5) . ? C34 C44 1.525(5) . ? C34 H34 0.97(3) . ? C35 C36 1.348(5) . ? C36 N31 1.370(5) . ? C41 C42 1.356(7) . ? C41 C46 1.378(6) . ? C41 H41 0.99(5) . ? C42 C43 1.381(7) . ? C42 H42 1.04(5) . ? C43 C44 1.379(5) . ? C43 H43 0.99(3) . ? C44 N45 1.341(5) . ? C46 N45 1.346(5) . ? C46 C47 1.481(8) . ? C47 H47C 0.92(6) . ? C47 H47B 0.87(5) . ? C47 H47A 1.00(7) . ? N11 H11N 0.85(3) . ? N31 H31N 0.96(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 C1 H1C 110(2) . . ? C12 C1 H1B 112(4) . . ? H1C C1 H1B 107(4) . . ? C12 C1 H1A 110(3) . . ? H1C C1 H1A 105(4) . . ? H1B C1 H1A 112(5) . . ? C16 C2 H2C 111(3) . . ? C16 C2 H2B 109(3) . . ? H2C C2 H2B 113(4) . . ? C16 C2 H2A 112(3) . . ? H2C C2 H2A 103(4) . . ? H2B C2 H2A 109(4) . . ? N1 C3 C13 179.2(5) . . ? N2 C4 C15 176.1(5) . . ? C32 C5 H5C 112(3) . . ? C32 C5 H5B 113(3) . . ? H5C C5 H5B 107(4) . . ? C32 C5 H5A 113(3) . . ? H5C C5 H5A 98(4) . . ? H5B C5 H5A 113(4) . . ? C36 C6 H6C 111(4) . . ? C36 C6 H6B 114(3) . . ? H6C C6 H6B 106(5) . . ? C36 C6 H6A 116(3) . . ? H6C C6 H6A 102(4) . . ? H6B C6 H6A 107(4) . . ? N3 C7 C33 177.5(5) . . ? N4 C8 C35 179.0(5) . . ? C13 C12 N11 120.3(4) . . ? C13 C12 C1 124.2(4) . . ? N11 C12 C1 115.5(4) . . ? C12 C13 C3 119.6(4) . . ? C12 C13 C14 123.7(4) . . ? C3 C13 C14 116.6(4) . . ? C13 C14 C24 114.6(3) . . ? C13 C14 C15 108.6(3) . . ? C24 C14 C15 112.2(3) . . ? C13 C14 H14 110.2(19) . . ? C24 C14 H14 101.9(18) . . ? C15 C14 H14 109.2(18) . . ? C16 C15 C4 119.8(4) . . ? C16 C15 C14 124.1(4) . . ? C4 C15 C14 116.2(4) . . ? C15 C16 N11 120.2(4) . . ? C15 C16 C2 125.3(4) . . ? N11 C16 C2 114.5(4) . . ? C22 C21 C26 119.7(4) . . ? C22 C21 H21 125(3) . . ? C26 C21 H21 115(3) . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22 122(3) . . ? C23 C22 H22 119(3) . . ? C24 C23 C22 118.4(5) . . ? C24 C23 H23 120(3) . . ? C22 C23 H23 122(3) . . ? N25 C24 C23 123.0(4) . . ? N25 C24 C14 117.7(3) . . ? C23 C24 C14 119.3(4) . . ? N25 C26 C21 121.8(5) . . ? N25 C26 C27 116.6(5) . . ? C21 C26 C27 121.6(5) . . ? C26 C27 H27C 125(5) . . ? C26 C27 H27B 107(8) . . ? H27C C27 H27B 103(8) . . ? C26 C27 H27A 111(3) . . ? H27C C27 H27A 88(5) . . ? H27B C27 H27A 124(8) . . ? C33 C32 N31 120.4(4) . . ? C33 C32 C5 124.9(4) . . ? N31 C32 C5 114.5(4) . . ? C32 C33 C7 120.0(4) . . ? C32 C33 C34 124.3(4) . . ? C7 C33 C34 115.7(3) . . ? C35 C34 C44 114.0(3) . . ? C35 C34 C33 108.4(3) . . ? C44 C34 C33 111.9(3) . . ? C35 C34 H34 110(2) . . ? C44 C34 H34 109.6(18) . . ? C33 C34 H34 101.8(18) . . ? C36 C35 C8 118.3(4) . . ? C36 C35 C34 124.5(3) . . ? C8 C35 C34 117.2(3) . . ? C35 C36 N31 120.8(4) . . ? C35 C36 C6 124.3(4) . . ? N31 C36 C6 114.8(4) . . ? C42 C41 C46 120.3(5) . . ? C42 C41 H41 120(3) . . ? C46 C41 H41 120(3) . . ? C41 C42 C43 118.8(5) . . ? C41 C42 H42 121(3) . . ? C43 C42 H42 120(3) . . ? C44 C43 C42 119.0(5) . . ? C44 C43 H43 116(2) . . ? C42 C43 H43 124(2) . . ? N45 C44 C43 122.0(4) . . ? N45 C44 C34 118.0(3) . . ? C43 C44 C34 120.0(4) . . ? N45 C46 C41 121.3(5) . . ? N45 C46 C47 118.6(5) . . ? C41 C46 C47 120.1(5) . . ? C46 C47 H47C 119(4) . . ? C46 C47 H47B 115(4) . . ? H47C C47 H47B 120(5) . . ? C46 C47 H47A 108(4) . . ? H47C C47 H47A 95(6) . . ? H47B C47 H47A 91(5) . . ? C16 N11 C12 122.3(4) . . ? C16 N11 H11N 122(3) . . ? C12 N11 H11N 115(3) . . ? C24 N25 C26 117.7(4) . . ? C36 N31 C32 121.4(4) . . ? C36 N31 H31N 117(3) . . ? C32 N31 H31N 121(3) . . ? C44 N45 C46 118.6(4) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.169 _refine_diff_density_min -0.149 _refine_diff_density_rms 0.039 data_2 _database_code_depnum_ccdc_archive 'CCDC 612146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag N5 O3' _chemical_formula_weight 420.18 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.598(3) _cell_length_b 11.630(3) _cell_length_c 13.641(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.949(4) _cell_angle_gamma 90.00 _cell_volume 1631.6(7) _cell_formula_units_Z 4 _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 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8926 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3194 _reflns_number_gt 2795 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3194 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ag Ag 0.38975(2) 0.146324(18) 0.052545(16) 0.04714(13) Uani 1 1 d . . . N1 N 0.53546(19) 0.28236(15) 0.03362(13) 0.0304(4) Uani 1 1 d . . . C1 C 0.3908(4) 0.3125(4) -0.1326(2) 0.0598(8) Uani 1 1 d . . . H1C H 0.319(4) 0.319(3) -0.097(3) 0.058(9) Uiso 1 1 d . . . H1B H 0.370(5) 0.366(4) -0.168(4) 0.082(15) Uiso 1 1 d . . . H1A H 0.349(5) 0.239(5) -0.139(3) 0.098(14) Uiso 1 1 d . . . O1 O 0.2128(7) 0.1867(6) 0.1332(6) 0.0777(17) Uani 0.60 1 d P . . O1' O 0.2371(18) 0.253(3) 0.1487(10) 0.230(14) Uani 0.40 1 d P . . N2 N 0.9186(2) 0.2217(2) 0.34258(16) 0.0459(5) Uani 1 1 d . . . H2A H 0.9961 0.2200 0.3807 0.055 Uiso 1 1 calc R . . C2 C 0.5142(3) 0.3378(2) -0.0565(2) 0.0384(5) Uani 1 1 d . . . O2 O 0.1563(9) 0.2846(9) 0.0008(7) 0.087(4) Uani 0.60 1 d P . . O2' O 0.1670(17) 0.2500(19) 0.0001(14) 0.132(8) Uani 0.40 1 d P . . N3 N 0.5726(3) 0.4853(2) 0.32275(18) 0.0525(6) Uani 1 1 d . . . C3 C 0.6059(3) 0.4138(2) -0.0777(2) 0.0442(6) Uani 1 1 d . . . H3A H 0.5888 0.4527 -0.1390 0.053 Uiso 1 1 calc R . . O3 O 0.0457(6) 0.2927(6) 0.1153(6) 0.103(2) Uani 0.60 1 d P . . O3' O 0.0686(13) 0.3490(9) 0.0686(13) 0.127(5) Uani 0.40 1 d P . . N4 N 0.6906(3) -0.0172(2) 0.07450(18) 0.0529(6) Uani 1 1 d . . . C4 C 0.7206(3) 0.4308(3) -0.0083(2) 0.0522(7) Uani 1 1 d . . . H4A H 0.7831 0.4801 -0.0223 0.063 Uiso 1 1 calc R . . N5 N 0.1451(3) 0.2675(3) 0.0823(3) 0.0740(9) Uani 1 1 d . . . C5 C 0.7428(3) 0.3734(3) 0.0837(2) 0.0459(6) Uani 1 1 d . . . H5A H 0.8207 0.3828 0.1319 0.055 Uiso 1 1 calc R . . C6 C 0.6466(2) 0.30191(18) 0.10217(17) 0.0304(5) Uani 1 1 d . . . C7 C 0.6663(2) 0.23884(18) 0.20277(15) 0.0305(5) Uani 1 1 d . . . H7A H 0.5827 0.2074 0.2088 0.037 Uiso 1 1 calc R . . C8 C 0.7190(2) 0.3191(2) 0.29233(16) 0.0331(5) Uani 1 1 d . . . C9 C 0.8380(2) 0.3097(2) 0.35460(17) 0.0360(5) Uani 1 1 d . . . C10 C 0.8810(3) 0.1361(2) 0.2723(2) 0.0393(6) Uani 1 1 d . . . C11 C 0.7627(3) 0.14015(17) 0.20815(18) 0.0336(5) Uani 1 1 d . . . C12 C 0.6373(3) 0.4109(2) 0.30875(17) 0.0372(5) Uani 1 1 d . . . C13 C 0.8919(3) 0.3898(3) 0.4398(2) 0.0505(7) Uani 1 1 d . . . H13C H 0.977(4) 0.414(3) 0.436(3) 0.066(10) Uiso 1 1 d . . . H13B H 0.900(5) 0.350(3) 0.504(4) 0.077(13) Uiso 1 1 d . . . H13A H 0.857(4) 0.470(4) 0.427(3) 0.077(12) Uiso 1 1 d . . . C14 C 0.9806(4) 0.0452(3) 0.2737(3) 0.0611(9) Uani 1 1 d . . . H14C H 0.942(5) -0.004(4) 0.232(3) 0.077(12) Uiso 1 1 d . . . H14B H 1.040(7) 0.067(5) 0.245(4) 0.11(2) Uiso 1 1 d . . . H14A H 0.996(4) 0.013(3) 0.342(3) 0.085(13) Uiso 1 1 d . . . C15 C 0.7243(3) 0.0508(2) 0.13548(19) 0.0389(5) 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 0.04606(19) 0.04355(18) 0.04949(18) -0.00443(7) 0.00701(12) -0.01545(8) N1 0.0305(10) 0.0285(9) 0.0296(9) -0.0014(7) 0.0021(7) -0.0022(7) C1 0.056(2) 0.073(2) 0.0397(15) 0.0138(15) -0.0091(14) -0.0106(18) O1 0.061(3) 0.102(3) 0.070(5) 0.016(3) 0.014(3) 0.030(3) O1' 0.126(12) 0.50(4) 0.042(5) 0.023(16) -0.028(6) 0.08(2) N2 0.0349(12) 0.0530(12) 0.0409(11) -0.0147(10) -0.0079(9) 0.0072(10) C2 0.0446(15) 0.0352(12) 0.0327(12) 0.0000(9) 0.0042(11) 0.0028(10) O2 0.060(5) 0.111(6) 0.077(6) 0.054(5) -0.011(4) -0.014(4) O2' 0.047(6) 0.22(2) 0.129(13) -0.081(12) 0.027(7) -0.004(9) N3 0.0606(16) 0.0470(13) 0.0492(13) -0.0044(10) 0.0120(11) 0.0148(12) C3 0.0568(18) 0.0392(14) 0.0370(12) 0.0101(11) 0.0122(11) -0.0014(11) O3 0.062(3) 0.106(5) 0.149(6) -0.037(4) 0.038(3) 0.022(4) O3' 0.083(8) 0.082(8) 0.206(17) -0.016(7) 0.013(9) 0.010(6) N4 0.0669(18) 0.0451(13) 0.0455(12) -0.0145(11) 0.0112(12) -0.0115(12) C4 0.0577(18) 0.0515(15) 0.0487(15) 0.0066(12) 0.0154(14) -0.0200(14) N5 0.0478(17) 0.093(2) 0.071(2) -0.028(2) -0.0056(14) 0.0182(17) C5 0.0419(16) 0.0493(14) 0.0421(14) 0.0012(11) 0.0016(12) -0.0165(12) C6 0.0317(12) 0.0275(11) 0.0303(10) -0.0018(9) 0.0038(9) -0.0041(9) C7 0.0323(12) 0.0298(10) 0.0276(10) -0.0016(8) 0.0035(8) -0.0033(9) C8 0.0382(13) 0.0313(11) 0.0283(10) -0.0043(9) 0.0055(9) 0.0009(10) C9 0.0396(14) 0.0356(12) 0.0302(11) -0.0067(10) 0.0030(10) -0.0021(10) C10 0.0409(15) 0.0381(13) 0.0364(13) -0.0032(9) 0.0041(11) 0.0067(10) C11 0.0414(14) 0.0296(12) 0.0284(11) -0.0032(8) 0.0059(10) -0.0002(9) C12 0.0418(14) 0.0386(13) 0.0288(11) -0.0011(9) 0.0036(10) 0.0005(11) C13 0.0491(18) 0.0531(16) 0.0421(15) -0.0178(14) -0.0032(13) -0.0027(14) C14 0.063(2) 0.0557(19) 0.060(2) -0.0113(16) 0.0048(17) 0.0235(17) C15 0.0449(14) 0.0346(12) 0.0371(12) -0.0033(10) 0.0096(10) -0.0019(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 Ag N1 2.2685(19) . ? Ag N4 2.296(2) 3_655 ? Ag O1 2.437(7) . ? Ag N3 2.497(2) 2_645 ? Ag O2' 2.593(18) . ? N1 C6 1.335(3) . ? N1 C2 1.358(3) . ? C1 C2 1.490(4) . ? C1 H1C 1.01(4) . ? C1 H1B 0.78(4) . ? C1 H1A 0.96(5) . ? O1 O1' 0.82(3) . ? O1 N5 1.281(7) . ? O1' N5 1.172(14) . ? N2 C9 1.368(3) . ? N2 C10 1.373(3) . ? N2 H2A 0.8600 . ? C2 C3 1.394(4) . ? O2 N5 1.163(9) . ? O2 O3' 1.641(19) . ? O2' N5 1.216(17) . ? N3 C12 1.148(3) . ? N3 Ag 2.497(2) 2_655 ? C3 C4 1.363(4) . ? C3 H3A 0.9300 . ? O3 O3' 0.985(14) . ? O3 N5 1.276(6) . ? O3' N5 1.232(11) . ? N4 C15 1.141(3) . ? N4 Ag 2.296(2) 3_655 ? C4 C5 1.390(4) . ? C4 H4A 0.9300 . ? C5 C6 1.385(4) . ? C5 H5A 0.9300 . ? C6 C7 1.525(3) . ? C7 C11 1.527(3) . ? C7 C8 1.532(3) . ? C7 H7A 0.9800 . ? C8 C9 1.344(4) . ? C8 C12 1.426(4) . ? C9 C13 1.492(3) . ? C10 C11 1.346(4) . ? C10 C14 1.490(4) . ? C11 C15 1.426(3) . ? C13 H13C 0.97(4) . ? C13 H13B 0.98(5) . ? C13 H13A 1.00(5) . ? C14 H14C 0.83(5) . ? C14 H14B 0.86(6) . ? C14 H14A 0.98(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N4 120.59(8) . 3_655 ? N1 Ag O1 122.40(18) . . ? N4 Ag O1 106.3(2) 3_655 . ? N1 Ag N3 126.82(8) . 2_645 ? N4 Ag N3 89.60(9) 3_655 2_645 ? O1 Ag N3 81.43(17) . 2_645 ? N1 Ag O2' 104.1(5) . . ? N4 Ag O2' 87.0(5) 3_655 . ? O1 Ag O2' 44.5(4) . . ? N3 Ag O2' 121.5(4) 2_645 . ? C6 N1 C2 118.6(2) . . ? C6 N1 Ag 123.29(15) . . ? C2 N1 Ag 117.72(17) . . ? C2 C1 H1C 107(2) . . ? C2 C1 H1B 110(4) . . ? H1C C1 H1B 96(4) . . ? C2 C1 H1A 123(3) . . ? H1C C1 H1A 74(3) . . ? H1B C1 H1A 127(5) . . ? O1' O1 N5 63.4(13) . . ? O1' O1 Ag 94.0(17) . . ? N5 O1 Ag 106.7(4) . . ? O1 O1' N5 77.7(16) . . ? C9 N2 C10 122.8(2) . . ? C9 N2 H2A 118.6 . . ? C10 N2 H2A 118.6 . . ? N1 C2 C3 121.1(3) . . ? N1 C2 C1 117.6(3) . . ? C3 C2 C1 121.3(3) . . ? N5 O2 O3' 48.5(7) . . ? N5 O2' Ag 100.7(11) . . ? C12 N3 Ag 132.5(2) . 2_655 ? C4 C3 C2 119.8(2) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? O3' O3 N5 64.5(9) . . ? O3 O3' N5 69.2(9) . . ? O3 O3' O2 108.8(10) . . ? N5 O3' O2 45.0(6) . . ? C15 N4 Ag 176.0(3) . 3_655 ? C3 C4 C5 119.0(3) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? O2 N5 O1' 120.5(11) . . ? O2 N5 O2' 20.1(12) . . ? O1' N5 O2' 112.4(13) . . ? O2 N5 O3' 86.5(10) . . ? O1' N5 O3' 128.5(16) . . ? O2' N5 O3' 104.7(12) . . ? O2 N5 O3 125.5(7) . . ? O1' N5 O3 111.3(10) . . ? O2' N5 O3 136.2(9) . . ? O3' N5 O3 46.2(7) . . ? O2 N5 O1 118.1(7) . . ? O1' N5 O1 38.9(15) . . ? O2' N5 O1 99.8(10) . . ? O3' N5 O1 155.4(10) . . ? O3 N5 O1 112.3(6) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? N1 C6 C5 122.6(2) . . ? N1 C6 C7 117.02(19) . . ? C5 C6 C7 120.4(2) . . ? C6 C7 C11 110.45(18) . . ? C6 C7 C8 111.64(18) . . ? C11 C7 C8 107.96(19) . . ? C6 C7 H7A 108.9 . . ? C11 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C9 C8 C12 118.3(2) . . ? C9 C8 C7 124.1(2) . . ? C12 C8 C7 117.5(2) . . ? C8 C9 N2 120.2(2) . . ? C8 C9 C13 124.5(2) . . ? N2 C9 C13 115.3(2) . . ? C11 C10 N2 119.8(2) . . ? C11 C10 C14 125.3(3) . . ? N2 C10 C14 114.8(3) . . ? C10 C11 C15 119.5(2) . . ? C10 C11 C7 124.4(2) . . ? C15 C11 C7 116.0(2) . . ? N3 C12 C8 179.2(3) . . ? C9 C13 H13C 109(2) . . ? C9 C13 H13B 110(2) . . ? H13C C13 H13B 108(4) . . ? C9 C13 H13A 113(2) . . ? H13C C13 H13A 92(3) . . ? H13B C13 H13A 123(3) . . ? C10 C14 H14C 104(3) . . ? C10 C14 H14B 112(4) . . ? H14C C14 H14B 101(4) . . ? C10 C14 H14A 104(2) . . ? H14C C14 H14A 109(4) . . ? H14B C14 H14A 125(5) . . ? N4 C15 C11 177.0(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.485 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.083 data_3 _database_code_depnum_ccdc_archive 'CCDC 612147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag Cl N4 O4' _chemical_formula_weight 457.62 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 10.682(3) _cell_length_b 11.957(4) _cell_length_c 13.368(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.245(7) _cell_angle_gamma 90.00 _cell_volume 1668.5(9) _cell_formula_units_Z 4 _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 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9294 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3264 _reflns_number_gt 1997 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3264 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.91581(4) 0.87348(4) 0.05496(3) 0.04240(16) Uani 1 1 d . . . C1 C 0.8877(8) 0.6929(7) -0.1247(6) 0.0553(19) Uani 1 1 d . . . H1C H 0.863(6) 0.770(6) -0.137(5) 0.07(2) Uiso 1 1 d . . . H1B H 0.878(7) 0.657(6) -0.181(6) 0.08(3) Uiso 1 1 d . . . H1A H 0.825(7) 0.689(6) -0.100(6) 0.08(3) Uiso 1 1 d . . . C2 C 1.0104(5) 0.6678(4) -0.0522(4) 0.0294(12) Uani 1 1 d . . . C3 C 1.0955(5) 0.5890(4) -0.0753(4) 0.0387(14) Uani 1 1 d . . . H3 H 1.0753 0.5485 -0.1360 0.046 Uiso 1 1 calc R . . C4 C 1.2092(6) 0.5715(5) -0.0079(4) 0.0458(15) Uani 1 1 d . . . H4 H 1.2683 0.5210 -0.0239 0.055 Uiso 1 1 calc R . . C5 C 1.2365(5) 0.6287(4) 0.0837(4) 0.0396(13) Uani 1 1 d . . . H5 H 1.3137 0.6177 0.1301 0.048 Uiso 1 1 calc R . . C6 C 1.1463(5) 0.7025(4) 0.1047(4) 0.0257(11) Uani 1 1 d . . . C7 C 1.1709(5) 0.7642(4) 0.2078(3) 0.0254(11) Uani 1 1 d . . . H7A H 1.0891 0.7942 0.2179 0.030 Uiso 1 1 calc R . . C8 C 1.2630(5) 0.8611(4) 0.2105(3) 0.0257(11) Uani 1 1 d . . . C9 C 1.3787(5) 0.8668(4) 0.2745(4) 0.0321(12) Uani 1 1 d . . . C10 C 1.3380(5) 0.6954(4) 0.3574(4) 0.0292(12) Uani 1 1 d . . . C11 C 1.2220(5) 0.6854(4) 0.2947(3) 0.0268(11) Uani 1 1 d . . . C12 C 1.2221(5) 0.9480(4) 0.1379(4) 0.0328(12) Uani 1 1 d . . . C13 C 1.4741(7) 0.9572(5) 0.2757(6) 0.0428(15) Uani 1 1 d . . . H13C H 1.532(5) 0.927(5) 0.251(4) 0.042(19) Uiso 1 1 d . . . H13B H 1.440(6) 1.007(6) 0.223(5) 0.07(2) Uiso 1 1 d . . . H13A H 1.516(7) 0.990(6) 0.344(5) 0.09(2) Uiso 1 1 d . . . C14 C 1.3947(7) 0.6159(6) 0.4428(5) 0.0457(16) Uani 1 1 d . . . H14C H 1.404(5) 0.653(4) 0.506(4) 0.034(15) Uiso 1 1 d . . . H14B H 1.489(7) 0.598(6) 0.442(5) 0.08(2) Uiso 1 1 d . . . H14A H 1.351(7) 0.556(6) 0.433(5) 0.07(2) Uiso 1 1 d . . . C15 C 1.1450(5) 0.5920(4) 0.3114(4) 0.0313(12) Uani 1 1 d . . . N1 N 1.0368(4) 0.7251(3) 0.0377(3) 0.0250(9) Uani 1 1 d . . . N2 N 1.4163(4) 0.7845(4) 0.3462(3) 0.0353(10) Uani 1 1 d . . . H2A H 1.4911 0.7886 0.3855 0.042 Uiso 1 1 calc R . . N3 N 1.1851(5) 1.0142(4) 0.0776(4) 0.0428(12) Uani 1 1 d . . . N4 N 1.0841(5) 0.5176(4) 0.3254(3) 0.0472(12) Uani 1 1 d . . . Cl Cl 0.66429(14) 0.71523(12) 0.11501(11) 0.0430(4) Uani 1 1 d . . . O1 O 0.704(2) 0.8256(12) 0.1114(17) 0.074(5) Uani 0.60 1 d P . . O1' O 0.698(3) 0.822(3) 0.073(3) 0.118(14) Uani 0.40 1 d P . . O2 O 0.779(2) 0.659(2) 0.1546(17) 0.057(4) Uani 0.60 1 d P . . O2' O 0.750(4) 0.638(3) 0.178(3) 0.052(6) Uani 0.40 1 d P . . O3 O 0.629(2) 0.6728(18) 0.0084(12) 0.106(8) Uani 0.60 1 d P . . O3' O 0.587(3) 0.653(2) 0.0414(16) 0.067(6) Uani 0.40 1 d P . . O4 O 0.5510(15) 0.7221(15) 0.1541(13) 0.090(6) Uani 0.60 1 d P . . O4' O 0.604(2) 0.727(3) 0.1986(17) 0.080(8) Uani 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0423(3) 0.0333(2) 0.0498(3) 0.0007(2) 0.00578(19) 0.0136(2) C1 0.050(5) 0.064(5) 0.041(4) -0.015(4) -0.014(4) 0.013(4) C2 0.036(3) 0.025(3) 0.026(3) 0.001(2) 0.004(2) -0.001(2) C3 0.049(4) 0.029(3) 0.037(3) -0.002(2) 0.008(3) 0.004(3) C4 0.056(4) 0.039(3) 0.046(4) 0.001(3) 0.017(3) 0.020(3) C5 0.044(3) 0.042(3) 0.031(3) 0.000(3) 0.004(2) 0.017(3) C6 0.027(3) 0.019(2) 0.029(3) 0.003(2) 0.002(2) -0.002(2) C7 0.024(3) 0.028(3) 0.023(2) 0.000(2) 0.002(2) 0.005(2) C8 0.035(3) 0.018(2) 0.023(2) 0.001(2) 0.004(2) 0.001(2) C9 0.040(3) 0.027(3) 0.029(3) -0.001(2) 0.009(2) -0.003(3) C10 0.029(3) 0.028(3) 0.028(3) 0.001(2) -0.002(2) 0.001(2) C11 0.035(3) 0.024(3) 0.021(3) 0.001(2) 0.005(2) -0.003(2) C12 0.037(3) 0.023(3) 0.040(3) -0.001(2) 0.012(3) -0.002(2) C13 0.046(4) 0.034(3) 0.048(4) 0.001(3) 0.010(4) -0.010(3) C14 0.052(5) 0.038(4) 0.042(4) 0.014(3) -0.003(3) 0.002(4) C15 0.029(3) 0.037(3) 0.025(3) 0.006(2) 0.000(2) 0.000(2) N1 0.029(2) 0.020(2) 0.025(2) -0.0013(17) 0.0030(18) 0.0019(18) N2 0.026(2) 0.039(2) 0.035(3) 0.009(2) -0.007(2) -0.007(2) N3 0.050(3) 0.031(3) 0.046(3) 0.009(2) 0.006(2) 0.007(2) N4 0.052(3) 0.042(3) 0.045(3) 0.008(2) 0.003(2) -0.014(3) Cl 0.0387(9) 0.0392(8) 0.0496(9) -0.0053(7) 0.0060(7) 0.0026(7) O1 0.097(10) 0.030(5) 0.108(11) 0.000(6) 0.053(7) -0.020(6) O1' 0.049(13) 0.123(19) 0.20(4) 0.10(2) 0.071(17) 0.028(12) O2 0.059(10) 0.063(12) 0.044(11) 0.001(7) -0.001(6) 0.010(8) O2' 0.067(18) 0.042(9) 0.040(13) 0.018(8) -0.001(9) 0.006(10) O3 0.116(15) 0.137(16) 0.045(9) -0.038(9) -0.027(7) 0.078(12) O3' 0.080(15) 0.071(10) 0.034(12) -0.025(9) -0.023(8) 0.010(9) O4 0.069(11) 0.065(8) 0.158(17) 0.022(11) 0.072(10) 0.010(8) O4' 0.086(19) 0.097(12) 0.071(13) -0.036(11) 0.047(11) -0.014(14) _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 2.236(4) . ? Ag N3 2.301(5) 3_775 ? Ag N4 2.351(5) 2_755 ? Ag O1' 2.47(3) . ? Ag O1 2.600(19) . ? C1 C2 1.487(8) . ? C2 N1 1.360(6) . ? C2 C3 1.389(7) . ? C3 C4 1.366(7) . ? C4 C5 1.379(7) . ? C5 C6 1.379(7) . ? C6 N1 1.341(6) . ? C6 C7 1.536(6) . ? C7 C11 1.506(6) . ? C7 C8 1.515(6) . ? C8 C9 1.347(7) . ? C8 C12 1.426(7) . ? C9 N2 1.373(6) . ? C9 C13 1.483(7) . ? C10 C11 1.345(7) . ? C10 N2 1.382(6) . ? C10 C14 1.510(7) . ? C11 C15 1.433(7) . ? C12 N3 1.139(6) . ? C15 N4 1.140(6) . ? N3 Ag 2.301(5) 3_775 ? N4 Ag 2.351(5) 2_745 ? Cl O3' 1.36(2) . ? Cl O2 1.40(3) . ? Cl O1 1.389(14) . ? Cl O4' 1.41(3) . ? Cl O4 1.419(17) . ? Cl O2' 1.44(4) . ? Cl O1' 1.47(3) . ? Cl O3 1.484(16) . ? O1 O1' 0.50(5) . ? O2 O2' 0.54(3) . ? O3 O3' 0.73(3) . ? O4 O4' 0.73(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N3 124.77(15) . 3_775 ? N1 Ag N4 137.32(16) . 2_755 ? N3 Ag N4 91.64(16) 3_775 2_755 ? N1 Ag O1' 113.1(7) . . ? N3 Ag O1' 85.6(8) 3_775 . ? N4 Ag O1' 88.8(8) 2_755 . ? N1 Ag O1 114.5(4) . . ? N3 Ag O1 93.3(5) 3_775 . ? N4 Ag O1 80.7(4) 2_755 . ? O1' Ag O1 11.0(13) . . ? N1 C2 C3 121.0(5) . . ? N1 C2 C1 117.6(5) . . ? C3 C2 C1 121.4(5) . . ? C4 C3 C2 119.3(5) . . ? C3 C4 C5 120.0(5) . . ? C4 C5 C6 118.3(5) . . ? N1 C6 C5 122.7(4) . . ? N1 C6 C7 117.5(4) . . ? C5 C6 C7 119.8(4) . . ? C11 C7 C8 109.4(4) . . ? C11 C7 C6 110.9(4) . . ? C8 C7 C6 112.1(4) . . ? C9 C8 C12 120.1(4) . . ? C9 C8 C7 123.9(4) . . ? C12 C8 C7 115.9(4) . . ? C8 C9 N2 120.0(4) . . ? C8 C9 C13 125.4(5) . . ? N2 C9 C13 114.6(5) . . ? C11 C10 N2 120.0(4) . . ? C11 C10 C14 125.7(5) . . ? N2 C10 C14 114.4(5) . . ? C10 C11 C15 117.1(4) . . ? C10 C11 C7 124.0(4) . . ? C15 C11 C7 118.8(4) . . ? N3 C12 C8 176.9(6) . . ? N4 C15 C11 179.5(6) . . ? C6 N1 C2 118.5(4) . . ? C6 N1 Ag 122.1(3) . . ? C2 N1 Ag 118.3(3) . . ? C9 N2 C10 122.3(4) . . ? C12 N3 Ag 170.4(4) . 3_775 ? C15 N4 Ag 140.0(4) . 2_745 ? O3' Cl O2 110.9(16) . . ? O3' Cl O1 129.5(14) . . ? O2 Cl O1 102.8(13) . . ? O3' Cl O4' 108.7(13) . . ? O2 Cl O4' 104.8(13) . . ? O1 Cl O4' 97.2(15) . . ? O3' Cl O4 82.4(11) . . ? O2 Cl O4 129.4(9) . . ? O1 Cl O4 104.2(11) . . ? O4' Cl O4 30.0(10) . . ? O3' Cl O2' 107(2) . . ? O2 Cl O2' 22.0(12) . . ? O1 Cl O2' 117.8(18) . . ? O4' Cl O2' 86.5(16) . . ? O4 Cl O2' 108.1(12) . . ? O3' Cl O1' 111.2(18) . . ? O2 Cl O1' 107.2(13) . . ? O1 Cl O1' 20(2) . . ? O4' Cl O1' 113.9(18) . . ? O4 Cl O1' 112.7(13) . . ? O2' Cl O1' 126.9(17) . . ? O3' Cl O3 29.2(12) . . ? O2 Cl O3 103.1(13) . . ? O1 Cl O3 108.0(12) . . ? O4' Cl O3 136.8(12) . . ? O4 Cl O3 108.0(10) . . ? O2' Cl O3 110.3(18) . . ? O1' Cl O3 88.1(16) . . ? O1' O1 Cl 89(5) . . ? O1' O1 Ag 69(5) . . ? Cl O1 Ag 120.5(10) . . ? O1 O1' Cl 71(5) . . ? O1 O1' Ag 100(6) . . ? Cl O1' Ag 124.4(16) . . ? O2' O2 Cl 84(7) . . ? O2 O2' Cl 74(6) . . ? O3' O3 Cl 66(3) . . ? O3 O3' Cl 85(4) . . ? O4' O4 Cl 74(3) . . ? O4 O4' Cl 76(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.462 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.108 data_4 _database_code_depnum_ccdc_archive 'CCDC 612148' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag B F4 N4' _chemical_formula_weight 444.98 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6811(8) _cell_length_b 11.9175(9) _cell_length_c 13.2109(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.1170(10) _cell_angle_gamma 90.00 _cell_volume 1644.2(2) _cell_formula_units_Z 4 _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 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9112 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.04 _reflns_number_total 3234 _reflns_number_gt 2704 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.4886P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3234 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 1.41995(2) 0.626080(18) 0.056140(16) 0.04202(10) Uani 1 1 d . . . B B 1.1632(4) 0.7835(3) 0.1132(3) 0.0500(8) Uani 1 1 d . . . F1 F 1.2815(13) 0.8317(13) 0.1500(12) 0.078(3) Uani 0.50 1 d P . . F1' F 1.2462(12) 0.8558(13) 0.1690(11) 0.069(3) Uani 0.50 1 d P . . F2 F 1.1944(14) 0.6816(13) 0.0800(15) 0.135(6) Uani 0.50 1 d P . . F2' F 1.2002(15) 0.6750(10) 0.1119(12) 0.088(3) Uani 0.50 1 d P . . F3 F 1.0921(9) 0.8460(9) 0.0357(8) 0.082(3) Uani 0.50 1 d P . . F3' F 1.1362(9) 0.8168(10) 0.0090(7) 0.094(4) Uani 0.50 1 d P . . F4 F 1.0969(10) 0.7679(10) 0.1846(9) 0.114(4) Uani 0.50 1 d P . . F4' F 1.0495(9) 0.7829(8) 0.1506(9) 0.095(3) Uani 0.50 1 d P . . N1 N 1.53870(19) 0.77491(16) 0.03704(14) 0.0276(4) Uani 1 1 d . . . N2 N 1.9195(2) 0.71452(19) 0.34746(17) 0.0381(5) Uani 1 1 d . . . H2A H 1.9944 0.7099 0.3870 0.046 Uiso 1 1 calc R . . N3 N 1.5902(3) 0.9833(2) 0.32715(19) 0.0480(6) Uani 1 1 d . . . N4 N 1.6855(3) 0.4844(2) 0.07781(18) 0.0468(6) Uani 1 1 d . . . C1 C 1.3859(4) 0.8068(4) -0.1249(3) 0.0550(9) Uani 1 1 d . . . H1C H 1.316(4) 0.801(3) -0.088(3) 0.074(12) Uiso 1 1 d . . . H1B H 1.382(4) 0.734(4) -0.148(3) 0.088(14) Uiso 1 1 d . . . H1A H 1.365(5) 0.860(4) -0.167(4) 0.100(17) Uiso 1 1 d . . . C2 C 1.5107(3) 0.8328(2) -0.05343(19) 0.0331(6) Uani 1 1 d . . . C3 C 1.5938(3) 0.9122(3) -0.0772(2) 0.0406(6) Uani 1 1 d . . . H3A H 1.5719 0.9531 -0.1384 0.049 Uiso 1 1 calc R . . C4 C 1.7091(3) 0.9310(3) -0.0104(2) 0.0469(7) Uani 1 1 d . . . H4A H 1.7673 0.9823 -0.0270 0.056 Uiso 1 1 calc R . . C5 C 1.7370(3) 0.8723(2) 0.0815(2) 0.0405(7) Uani 1 1 d . . . H5A H 1.8145 0.8834 0.1278 0.049 Uiso 1 1 calc R . . C6 C 1.6492(2) 0.79736(19) 0.10394(17) 0.0268(5) Uani 1 1 d . . . C7 C 1.6729(2) 0.73606(19) 0.20802(17) 0.0264(5) Uani 1 1 d . . . H7A H 1.5910 0.7066 0.2187 0.032 Uiso 1 1 calc R . . C8 C 1.7270(2) 0.8150(2) 0.29715(18) 0.0289(5) Uani 1 1 d . . . C9 C 1.8434(2) 0.8036(2) 0.35906(18) 0.0312(5) Uani 1 1 d . . . C10 C 1.8811(3) 0.6320(2) 0.27516(19) 0.0329(5) Uani 1 1 d . . . C11 C 1.7652(3) 0.63845(19) 0.21087(18) 0.0298(5) Uani 1 1 d . . . C12 C 1.6502(3) 0.9083(2) 0.31290(18) 0.0338(6) Uani 1 1 d . . . C13 C 1.8996(3) 0.8821(3) 0.4449(2) 0.0439(7) Uani 1 1 d . . . H13C H 1.901(4) 0.845(3) 0.512(3) 0.070(11) Uiso 1 1 d . . . H13B H 1.987(4) 0.906(3) 0.442(3) 0.064(10) Uiso 1 1 d . . . H13A H 1.862(4) 0.954(4) 0.439(3) 0.076(12) Uiso 1 1 d . . . C14 C 1.9748(4) 0.5401(3) 0.2754(3) 0.0488(8) Uani 1 1 d . . . H14C H 1.931(4) 0.483(4) 0.233(3) 0.092(14) Uiso 1 1 d . . . H14B H 2.011(4) 0.522(3) 0.337(3) 0.074(13) Uiso 1 1 d . . . H14A H 2.043(4) 0.564(3) 0.258(3) 0.065(12) Uiso 1 1 d . . . C15 C 1.7238(3) 0.5507(2) 0.13859(19) 0.0332(5) 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 0.04281(15) 0.03448(14) 0.04669(15) 0.00024(9) 0.00467(10) -0.01345(8) B 0.049(2) 0.051(2) 0.0479(19) 0.0061(17) 0.0057(16) -0.0037(16) F1 0.058(6) 0.092(8) 0.074(7) 0.016(5) -0.011(4) -0.021(5) F1' 0.070(8) 0.073(5) 0.055(4) -0.005(3) -0.009(4) -0.016(4) F2 0.067(6) 0.108(9) 0.242(18) -0.085(9) 0.065(8) -0.012(5) F2' 0.100(7) 0.048(4) 0.119(6) 0.014(5) 0.033(4) 0.028(4) F3 0.081(6) 0.077(4) 0.070(6) 0.016(4) -0.023(4) -0.015(4) F3' 0.071(6) 0.145(10) 0.050(4) 0.036(5) -0.020(3) -0.050(5) F4 0.116(9) 0.119(6) 0.133(7) 0.043(5) 0.085(7) 0.015(6) F4' 0.071(5) 0.067(4) 0.164(9) -0.031(5) 0.061(5) 0.004(3) N1 0.0320(11) 0.0249(10) 0.0249(9) 0.0000(8) 0.0035(8) -0.0025(8) N2 0.0308(12) 0.0427(13) 0.0356(11) -0.0104(10) -0.0050(9) 0.0046(9) N3 0.0526(15) 0.0424(14) 0.0457(13) -0.0114(11) 0.0031(11) 0.0143(12) N4 0.0568(16) 0.0407(13) 0.0406(13) -0.0118(11) 0.0051(11) -0.0084(12) C1 0.054(2) 0.061(2) 0.0400(17) 0.0141(17) -0.0140(15) -0.0064(17) C2 0.0401(15) 0.0292(13) 0.0278(12) 0.0009(10) 0.0019(11) 0.0032(11) C3 0.0592(18) 0.0341(14) 0.0299(13) 0.0052(11) 0.0127(12) 0.0004(12) C4 0.0602(19) 0.0405(16) 0.0431(16) 0.0024(13) 0.0176(14) -0.0175(14) C5 0.0405(16) 0.0427(16) 0.0360(14) 0.0012(12) 0.0027(12) -0.0148(12) C6 0.0320(13) 0.0241(11) 0.0233(11) -0.0021(9) 0.0034(9) -0.0034(9) C7 0.0310(12) 0.0246(11) 0.0225(11) -0.0010(9) 0.0032(9) -0.0034(9) C8 0.0361(13) 0.0258(12) 0.0238(11) -0.0037(9) 0.0042(10) 0.0000(10) C9 0.0361(14) 0.0318(13) 0.0246(11) -0.0037(10) 0.0044(10) -0.0017(10) C10 0.0375(14) 0.0324(14) 0.0286(12) -0.0002(10) 0.0064(10) 0.0020(10) C11 0.0410(14) 0.0244(12) 0.0238(11) -0.0024(9) 0.0062(10) -0.0020(10) C12 0.0410(15) 0.0325(13) 0.0253(12) -0.0044(10) 0.0009(10) 0.0000(11) C13 0.0458(18) 0.0445(17) 0.0356(15) -0.0143(13) -0.0045(13) -0.0007(13) C14 0.0463(19) 0.0441(18) 0.053(2) -0.0056(15) 0.0045(16) 0.0122(15) C15 0.0385(14) 0.0287(13) 0.0322(13) -0.0003(11) 0.0072(11) -0.0007(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 Ag N1 2.2256(19) . ? Ag N4 2.302(2) 3_865 ? Ag N3 2.314(2) 2_845 ? B F4 1.305(11) . ? B F1' 1.341(16) . ? B F2' 1.352(12) . ? B F2 1.356(16) . ? B F3 1.362(11) . ? B F1 1.380(16) . ? B F3' 1.404(10) . ? B F4' 1.404(11) . ? F1 F1' 0.572(15) . ? F3 F3' 0.733(12) . ? F4 F4' 0.628(17) . ? N1 C6 1.345(3) . ? N1 C2 1.358(3) . ? N2 C9 1.365(3) . ? N2 C10 1.373(3) . ? N2 H2A 0.8600 . ? N3 C12 1.138(3) . ? N3 Ag 2.314(2) 2_855 ? N4 C15 1.139(3) . ? N4 Ag 2.302(2) 3_865 ? C1 C2 1.496(4) . ? C1 H1C 0.98(4) . ? C1 H1B 0.92(5) . ? C1 H1A 0.84(5) . ? C2 C3 1.378(4) . ? C3 C4 1.375(4) . ? C3 H3A 0.9300 . ? C4 C5 1.379(4) . ? C4 H4A 0.9300 . ? C5 C6 1.371(4) . ? C5 H5A 0.9300 . ? C6 C7 1.530(3) . ? C7 C11 1.520(3) . ? C7 C8 1.523(3) . ? C7 H7A 0.9800 . ? C8 C9 1.344(3) . ? C8 C12 1.423(4) . ? C9 C13 1.495(4) . ? C10 C11 1.349(4) . ? C10 C14 1.482(4) . ? C11 C15 1.423(3) . ? C13 H13C 0.99(4) . ? C13 H13B 0.98(4) . ? C13 H13A 0.95(4) . ? C14 H14C 0.94(5) . ? C14 H14B 0.86(4) . ? C14 H14A 0.85(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N4 124.57(8) . 3_865 ? N1 Ag N3 140.28(8) . 2_845 ? N4 Ag N3 90.44(9) 3_865 2_845 ? F4 B F1' 95.2(9) . . ? F4 B F2' 94.5(8) . . ? F1' B F2' 117.4(10) . . ? F4 B F2 108.3(9) . . ? F1' B F2 125.0(9) . . ? F2' B F2 17.8(13) . . ? F4 B F3 108.6(6) . . ? F1' B F3 105.2(9) . . ? F2' B F3 129.2(9) . . ? F2 B F3 112.5(9) . . ? F4 B F1 113.5(8) . . ? F1' B F1 24.2(6) . . ? F2' B F1 98.9(10) . . ? F2 B F1 102.6(8) . . ? F3 B F1 111.2(9) . . ? F4 B F3' 135.9(7) . . ? F1' B F3' 109.4(9) . . ? F2' B F3' 105.0(9) . . ? F2 B F3' 87.1(9) . . ? F3 B F3' 30.7(5) . . ? F1 B F3' 102.2(8) . . ? F4 B F4' 26.5(7) . . ? F1' B F4' 109.3(7) . . ? F2' B F4' 106.1(8) . . ? F2 B F4' 113.5(8) . . ? F3 B F4' 83.1(6) . . ? F1 B F4' 132.4(7) . . ? F3' B F4' 109.4(6) . . ? F1' F1 B 74(3) . . ? F1 F1' B 82(3) . . ? F3' F3 B 77.8(15) . . ? F3 F3' B 71.5(14) . . ? F4' F4 B 86(2) . . ? F4 F4' B 67.9(17) . . ? C6 N1 C2 118.6(2) . . ? C6 N1 Ag 121.77(15) . . ? C2 N1 Ag 118.64(16) . . ? C9 N2 C10 122.5(2) . . ? C9 N2 H2A 118.7 . . ? C10 N2 H2A 118.7 . . ? C12 N3 Ag 142.6(2) . 2_855 ? C15 N4 Ag 169.7(2) . 3_865 ? C2 C1 H1C 112(2) . . ? C2 C1 H1B 112(3) . . ? H1C C1 H1B 96(3) . . ? C2 C1 H1A 110(3) . . ? H1C C1 H1A 105(4) . . ? H1B C1 H1A 121(4) . . ? N1 C2 C3 121.1(2) . . ? N1 C2 C1 116.9(3) . . ? C3 C2 C1 122.0(3) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? N1 C6 C5 122.2(2) . . ? N1 C6 C7 116.9(2) . . ? C5 C6 C7 120.9(2) . . ? C11 C7 C8 108.33(19) . . ? C11 C7 C6 111.80(19) . . ? C8 C7 C6 111.35(19) . . ? C11 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C9 C8 C12 118.6(2) . . ? C9 C8 C7 124.1(2) . . ? C12 C8 C7 117.3(2) . . ? C8 C9 N2 120.4(2) . . ? C8 C9 C13 124.8(2) . . ? N2 C9 C13 114.7(2) . . ? C11 C10 N2 119.9(2) . . ? C11 C10 C14 125.0(3) . . ? N2 C10 C14 115.1(3) . . ? C10 C11 C15 119.7(2) . . ? C10 C11 C7 124.4(2) . . ? C15 C11 C7 115.9(2) . . ? N3 C12 C8 178.8(3) . . ? C9 C13 H13C 109(2) . . ? C9 C13 H13B 113(2) . . ? H13C C13 H13B 109(3) . . ? C9 C13 H13A 114(2) . . ? H13C C13 H13A 114(3) . . ? H13B C13 H13A 97(3) . . ? C10 C14 H14C 107(3) . . ? C10 C14 H14B 111(3) . . ? H14C C14 H14B 117(4) . . ? C10 C14 H14A 112(3) . . ? H14C C14 H14A 114(4) . . ? H14B C14 H14A 96(4) . . ? N4 C15 C11 176.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.507 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.086 data_5 _database_code_depnum_ccdc_archive 'CCDC 612149' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag F6 N4 P' _chemical_formula_weight 503.14 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 6.6550(8) _cell_length_b 20.7600(18) _cell_length_c 13.537(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.726(12) _cell_angle_gamma 90.00 _cell_volume 1824.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 12.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7635 _exptl_absorpt_correction_T_max 0.9689 _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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.26 _diffrn_reflns_number 3489 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3199 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+2.9047P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3199 _refine_ls_number_parameters 335 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.040 _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 Ag Ag -0.14951(4) 0.233112(13) 0.367982(19) 0.04426(12) Uani 1 1 d . . . P P 0.37025(15) 0.03944(5) 0.22945(8) 0.0536(3) Uani 1 1 d D . . N1 N 0.1066(4) 0.18874(12) 0.48267(18) 0.0348(5) Uani 1 1 d . . . C1 C -0.0503(9) 0.0870(2) 0.4216(4) 0.0722(13) Uani 1 1 d . . . H1C H -0.015(8) 0.045(3) 0.419(4) 0.091(17) Uiso 1 1 d . . . H1B H -0.168(9) 0.100(3) 0.438(4) 0.10(2) Uiso 1 1 d . . . H1A H -0.046(9) 0.094(3) 0.336(5) 0.12(2) Uiso 1 1 d . . . F1 F 0.435(3) 0.1141(7) 0.2338(15) 0.146(8) Uani 0.50 1 d P A 1 F1' F 0.338(3) 0.1087(5) 0.2552(12) 0.108(5) Uani 0.50 1 d P A 2 N2 N -0.0226(4) 0.39553(13) 0.4207(2) 0.0418(6) Uani 1 1 d . . . H2A H -0.0863 0.4293 0.3933 0.050 Uiso 1 1 calc R . . C2 C 0.1254(6) 0.12392(16) 0.4836(3) 0.0446(8) Uani 1 1 d . . . F2 F 0.433(3) 0.0261(8) 0.3471(14) 0.099(4) Uani 0.50 1 d P A 1 F2' F 0.361(4) 0.0255(12) 0.3381(15) 0.169(11) Uani 0.50 1 d P A 2 N3 N -0.0707(5) 0.27363(17) 0.7110(2) 0.0566(8) Uani 1 1 d . . . C3 C 0.3004(6) 0.09410(18) 0.5385(3) 0.0538(9) Uani 1 1 d . . . H3A H 0.3116 0.0495 0.5381 0.065 Uiso 1 1 calc R . . F3 F 0.1411(12) 0.0621(9) 0.2288(12) 0.175(8) Uani 0.50 1 d PD A 1 F3' F 0.1265(6) 0.0292(4) 0.1961(10) 0.093(3) Uani 0.50 1 d PD A 2 N4 N 0.5432(5) 0.27236(16) 0.3613(2) 0.0503(7) Uani 1 1 d . . . C4 C 0.4559(6) 0.13036(19) 0.5931(3) 0.0548(9) Uani 1 1 d . . . H4A H 0.5751 0.1107 0.6293 0.066 Uiso 1 1 calc R . . F4 F 0.330(2) -0.0330(6) 0.2183(12) 0.173(8) Uani 0.50 1 d P A 1 F4' F 0.3791(16) -0.0368(4) 0.2022(9) 0.072(3) Uani 0.50 1 d P A 2 C5 C 0.4363(5) 0.19656(18) 0.5947(2) 0.0462(8) Uani 1 1 d . . . H5A H 0.5401 0.2220 0.6328 0.055 Uiso 1 1 calc R . . F5 F 0.6061(9) 0.0201(7) 0.2440(15) 0.152(7) Uani 0.50 1 d PD A 1 F5' F 0.6132(6) 0.0414(5) 0.2390(7) 0.074(2) Uani 0.50 1 d PD A 2 C6 C 0.2586(4) 0.22425(15) 0.5381(2) 0.0329(6) Uani 1 1 d . . . F6 F 0.318(2) 0.0498(6) 0.1100(8) 0.097(4) Uani 0.50 1 d P A 1 F6' F 0.368(2) 0.0541(7) 0.1170(9) 0.098(5) Uani 0.50 1 d P A 2 C7 C 0.2353(4) 0.29685(15) 0.5321(2) 0.0330(6) Uani 1 1 d . . . H7A H 0.3505 0.3158 0.5812 0.040 Uiso 1 1 calc R . . C8 C 0.0362(4) 0.32171(15) 0.5558(2) 0.0341(6) Uani 1 1 d . . . C9 C -0.0731(5) 0.37070(15) 0.5062(2) 0.0373(7) Uani 1 1 d . . . C10 C 0.1249(5) 0.36870(15) 0.3774(2) 0.0371(7) Uani 1 1 d . . . C11 C 0.2460(4) 0.32130(14) 0.4267(2) 0.0336(6) Uani 1 1 d . . . C12 C -0.0218(5) 0.29595(17) 0.6427(2) 0.0424(7) Uani 1 1 d . . . C13 C -0.2503(6) 0.4032(2) 0.5369(4) 0.0530(9) Uani 1 1 d . . . H13C H -0.366(8) 0.408(2) 0.480(4) 0.079(15) Uiso 1 1 d . . . H13B H -0.221(10) 0.440(3) 0.565(5) 0.12(2) Uiso 1 1 d . . . H13A H -0.305(9) 0.383(3) 0.585(4) 0.097(18) Uiso 1 1 d . . . C14 C 0.1377(8) 0.3941(2) 0.2760(3) 0.0564(10) Uani 1 1 d . . . H14A H 0.222(8) 0.381(3) 0.257(4) 0.077(17) Uiso 1 1 d . . . H14B H 0.159(8) 0.439(3) 0.281(4) 0.100(18) Uiso 1 1 d . . . H14A H 0.002(12) 0.385(3) 0.230(5) 0.14(3) Uiso 1 1 d . . . C15 C 0.4069(5) 0.29493(16) 0.3861(2) 0.0381(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.03558(16) 0.05199(18) 0.04249(17) -0.00303(11) 0.00268(10) 0.00903(11) P 0.0515(6) 0.0522(6) 0.0537(6) 0.0086(4) 0.0043(4) 0.0051(4) N1 0.0360(13) 0.0369(13) 0.0309(12) 0.0017(10) 0.0060(10) 0.0018(11) C1 0.077(3) 0.042(2) 0.089(4) -0.010(2) 0.001(3) -0.010(2) F1 0.26(2) 0.060(5) 0.105(9) 0.023(5) 0.007(10) -0.015(9) F1' 0.174(13) 0.037(5) 0.099(8) -0.014(5) 0.002(7) 0.028(6) N2 0.0404(15) 0.0394(14) 0.0492(16) 0.0068(12) 0.0175(12) 0.0112(12) C2 0.052(2) 0.0392(17) 0.0420(17) 0.0024(14) 0.0098(15) 0.0027(15) F2 0.134(9) 0.111(7) 0.045(4) 0.019(4) 0.004(5) 0.062(7) F2' 0.23(2) 0.226(15) 0.068(9) 0.068(8) 0.068(11) 0.170(15) N3 0.0571(19) 0.077(2) 0.0432(17) 0.0046(15) 0.0263(15) -0.0021(16) C3 0.068(2) 0.0389(18) 0.056(2) 0.0091(16) 0.0161(19) 0.0124(17) F3 0.107(8) 0.28(2) 0.156(12) 0.118(13) 0.073(7) 0.110(10) F3' 0.042(3) 0.083(5) 0.157(9) 0.016(5) 0.026(4) 0.005(3) N4 0.0406(16) 0.068(2) 0.0457(16) 0.0054(14) 0.0181(13) 0.0169(14) C4 0.049(2) 0.062(2) 0.051(2) 0.0162(18) 0.0062(17) 0.0205(18) F4 0.191(13) 0.112(10) 0.159(12) 0.058(8) -0.089(9) -0.112(9) F4' 0.081(5) 0.051(4) 0.075(4) -0.013(3) -0.005(4) 0.024(4) C5 0.0371(17) 0.059(2) 0.0390(17) 0.0065(15) 0.0007(14) 0.0049(15) F5 0.075(6) 0.101(10) 0.273(15) 0.052(8) 0.020(7) 0.010(5) F5' 0.045(4) 0.082(6) 0.087(4) 0.000(4) -0.007(3) -0.015(3) C6 0.0323(15) 0.0414(16) 0.0263(14) 0.0014(12) 0.0094(12) 0.0034(12) F6 0.130(9) 0.089(6) 0.050(5) -0.013(4) -0.028(5) 0.038(5) F6' 0.083(6) 0.134(8) 0.087(8) 0.051(6) 0.043(6) -0.011(5) C7 0.0297(14) 0.0396(16) 0.0295(14) -0.0038(12) 0.0063(11) -0.0018(12) C8 0.0330(15) 0.0398(16) 0.0322(15) -0.0078(12) 0.0132(12) -0.0042(13) C9 0.0327(15) 0.0402(16) 0.0424(17) -0.0082(13) 0.0154(13) -0.0014(13) C10 0.0348(16) 0.0384(16) 0.0416(17) 0.0007(13) 0.0157(13) -0.0006(13) C11 0.0302(14) 0.0375(16) 0.0361(15) -0.0006(12) 0.0137(12) 0.0001(12) C12 0.0382(17) 0.0512(19) 0.0397(17) -0.0083(15) 0.0124(14) -0.0003(15) C13 0.045(2) 0.057(2) 0.063(3) -0.008(2) 0.0258(19) 0.0091(18) C14 0.064(3) 0.058(3) 0.056(2) 0.0192(19) 0.031(2) 0.014(2) C15 0.0357(16) 0.0439(17) 0.0365(16) 0.0046(13) 0.0118(13) 0.0038(14) _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 N4 2.185(3) 1_455 ? Ag N1 2.235(2) . ? Ag N3 2.303(3) 4_565 ? P F1' 1.505(11) . ? P F2' 1.51(2) . ? P F4 1.529(12) . ? P F6' 1.549(11) . ? P F2 1.579(18) . ? P F5 1.590(4) . ? P F6 1.591(11) . ? P F5' 1.594(4) . ? P F3 1.594(4) . ? P F3' 1.600(4) . ? P F1 1.606(16) . ? P F4' 1.630(8) . ? N1 C6 1.340(4) . ? N1 C2 1.351(4) . ? C1 C2 1.492(6) . ? C1 H1C 0.91(6) . ? C1 H1B 0.90(6) . ? C1 H1A 1.18(6) . ? N2 C10 1.368(4) . ? N2 C9 1.375(4) . ? N2 H2A 0.8600 . ? C2 C3 1.382(5) . ? N3 C12 1.144(4) . ? N3 Ag 2.303(3) 4_566 ? C3 C4 1.359(6) . ? C3 H3A 0.9300 . ? N4 C15 1.135(4) . ? N4 Ag 2.185(3) 1_655 ? C4 C5 1.381(5) . ? C4 H4A 0.9300 . ? C5 C6 1.384(4) . ? C5 H5A 0.9300 . ? C6 C7 1.516(4) . ? C7 C8 1.521(4) . ? C7 C11 1.530(4) . ? C7 H7A 0.9800 . ? C8 C9 1.341(5) . ? C8 C12 1.420(4) . ? C9 C13 1.495(4) . ? C10 C11 1.352(4) . ? C10 C14 1.490(5) . ? C11 C15 1.417(4) . ? C13 H13C 0.97(5) . ? C13 H13B 0.85(7) . ? C13 H13A 0.91(6) . ? C14 H14A 0.73(5) . ? C14 H14B 0.94(6) . ? C14 H14A 1.00(7) . ? 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 Ag N1 138.24(10) 1_455 . ? N4 Ag N3 112.70(12) 1_455 4_565 ? N1 Ag N3 108.78(11) . 4_565 ? F1' P F2' 85.4(11) . . ? F1' P F4 158.6(9) . . ? F2' P F4 82.1(12) . . ? F1' P F6' 93.9(8) . . ? F2' P F6' 177.0(10) . . ? F4 P F6' 97.6(8) . . ? F1' P F2 87.4(9) . . ? F2' P F2 17.2(15) . . ? F4 P F2 85.9(9) . . ? F6' P F2 165.8(9) . . ? F1' P F5 113.5(8) . . ? F2' P F5 94.8(10) . . ? F4 P F5 85.0(8) . . ? F6' P F5 88.2(9) . . ? F2 P F5 78.3(10) . . ? F1' P F6 95.5(7) . . ? F2' P F6 165.1(11) . . ? F4 P F6 92.2(7) . . ? F6' P F6 12.0(9) . . ? F2 P F6 176.4(8) . . ? F5 P F6 98.5(9) . . ? F1' P F5' 98.6(8) . . ? F2' P F5' 100.7(9) . . ? F4 P F5' 100.8(7) . . ? F6' P F5' 82.3(6) . . ? F2 P F5' 83.5(8) . . ? F5 P F5' 16.3(8) . . ? F6 P F5' 93.9(6) . . ? F1' P F3 62.3(9) . . ? F2' P F3 79.4(9) . . ? F4 P F3 98.1(9) . . ? F6' P F3 97.6(7) . . ? F2 P F3 95.5(9) . . ? F5 P F3 172.9(9) . . ? F6 P F3 87.8(7) . . ? F5' P F3 160.9(8) . . ? F1' P F3' 90.3(7) . . ? F2' P F3' 89.5(10) . . ? F4 P F3' 72.3(7) . . ? F6' P F3' 87.6(7) . . ? F2 P F3' 106.6(9) . . ? F5 P F3' 156.0(6) . . ? F6 P F3' 75.6(7) . . ? F5' P F3' 166.9(5) . . ? F3 P F3' 29.3(7) . . ? F1' P F1 28.4(9) . . ? F2' P F1 102.6(12) . . ? F4 P F1 173.0(10) . . ? F6' P F1 78.0(8) . . ? F2 P F1 97.1(10) . . ? F5 P F1 89.4(9) . . ? F6 P F1 84.4(8) . . ? F5' P F1 73.3(8) . . ? F3 P F1 87.9(9) . . ? F3' P F1 112.7(8) . . ? F1' P F4' 173.8(7) . . ? F2' P F4' 92.6(10) . . ? F4 P F4' 15.6(9) . . ? F6' P F4' 87.8(7) . . ? F2 P F4' 92.5(7) . . ? F5 P F4' 72.5(6) . . ? F6 P F4' 85.0(6) . . ? F5' P F4' 87.5(5) . . ? F3 P F4' 111.6(8) . . ? F3' P F4' 83.8(5) . . ? F1 P F4' 157.4(7) . . ? C6 N1 C2 119.0(3) . . ? C6 N1 Ag 121.9(2) . . ? C2 N1 Ag 118.1(2) . . ? C2 C1 H1C 110(3) . . ? C2 C1 H1B 109(4) . . ? H1C C1 H1B 123(5) . . ? C2 C1 H1A 108(3) . . ? H1C C1 H1A 91(4) . . ? H1B C1 H1A 114(5) . . ? C10 N2 C9 122.6(3) . . ? C10 N2 H2A 118.7 . . ? C9 N2 H2A 118.7 . . ? N1 C2 C3 121.1(3) . . ? N1 C2 C1 116.5(3) . . ? C3 C2 C1 122.4(4) . . ? C12 N3 Ag 159.1(3) . 4_566 ? C4 C3 C2 119.7(3) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C15 N4 Ag 160.6(3) . 1_655 ? C3 C4 C5 119.7(3) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 118.5(3) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? N1 C6 C5 121.9(3) . . ? N1 C6 C7 117.5(2) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C8 114.2(2) . . ? C6 C7 C11 110.8(2) . . ? C8 C7 C11 107.8(2) . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? C11 C7 H7A 108.0 . . ? C9 C8 C12 119.0(3) . . ? C9 C8 C7 123.5(3) . . ? C12 C8 C7 117.1(3) . . ? C8 C9 N2 120.0(3) . . ? C8 C9 C13 125.2(3) . . ? N2 C9 C13 114.8(3) . . ? C11 C10 N2 119.4(3) . . ? C11 C10 C14 124.3(3) . . ? N2 C10 C14 116.2(3) . . ? C10 C11 C15 120.6(3) . . ? C10 C11 C7 123.8(3) . . ? C15 C11 C7 115.3(3) . . ? N3 C12 C8 178.0(4) . . ? C9 C13 H13C 112(3) . . ? C9 C13 H13B 114(4) . . ? H13C C13 H13B 109(5) . . ? C9 C13 H13A 117(4) . . ? H13C C13 H13A 104(4) . . ? H13B C13 H13A 100(5) . . ? C10 C14 H14A 114(4) . . ? C10 C14 H14B 109(3) . . ? H14A C14 H14B 107(5) . . ? C10 C14 H14A 106(4) . . ? H14A C14 H14A 112(6) . . ? H14B C14 H14A 109(5) . . ? N4 C15 C11 174.5(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.552 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.067