# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Steed, Jonathan' _publ_contact_author_email jon.steed@durham.ac.uk _publ_section_title ; Metal-Induced Gelation in Dipyridyl Ureas ; loop_ _publ_author_name P.Byrne G.Lloyd L.Applegarth K.Anderson N.Clarke J.Steed # Attachment '- 1.cif' data_z:\xraydata\peter\07srv5~3\work\xm _database_code_depnum_ccdc_archive 'CCDC 773253' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H28 Cu N8 O14' _chemical_formula_weight 595.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4582(11) _cell_length_b 9.4917(14) _cell_length_c 9.6997(14) _cell_angle_alpha 113.399(4) _cell_angle_beta 106.638(4) _cell_angle_gamma 98.603(4) _cell_volume 576.10(15) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 808 _cell_measurement_theta_min 2.450 _cell_measurement_theta_max 24.701 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 309 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6125 _exptl_absorpt_correction_T_max 0.9035 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 sMART-6k _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8766 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.02 _reflns_number_total 3371 _reflns_number_gt 2609 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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. DFIX restraints used on water hydrogen atoms to fix them in a chemically sensible geometry. ; _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^)+(0.0639P)^2^+0.0054P] 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 3371 _refine_ls_number_parameters 193 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _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 Cu1 Cu 0.0000 0.0000 0.0000 0.01579(12) Uani 1 2 d S . . O1 O -0.0763(3) 0.3074(2) -0.32957(19) 0.0206(3) Uani 1 1 d . . . O2 O -0.2765(3) -0.0754(2) 0.0803(2) 0.0305(4) Uani 1 1 d . . . O3 O -0.5433(3) -0.1267(2) 0.1196(2) 0.0247(4) Uani 1 1 d . . . O4 O -0.5323(3) -0.2703(2) -0.1144(2) 0.0252(4) Uani 1 1 d . . . O5 O 0.0677(2) -0.2030(2) -0.06735(19) 0.0188(3) Uani 1 1 d D . . O6 O -0.2024(3) -0.4584(2) -0.1444(2) 0.0256(4) Uani 1 1 d D . . O7 O 0.3022(3) 0.4304(3) -0.1104(2) 0.0313(4) Uani 1 1 d D . . N1 N -0.1677(3) -0.0746(2) -0.2342(2) 0.0159(4) Uani 1 1 d . . . N2 N -0.2246(3) 0.0597(2) -0.5504(2) 0.0184(4) Uani 1 1 d . . . H1N H -0.2647 0.0070 -0.6569 0.022 Uiso 1 1 calc R . . N3 N -0.1489(3) 0.2851(2) -0.5824(2) 0.0219(4) Uani 1 1 d . . . H2N H -0.1769 0.2209 -0.6855 0.026 Uiso 1 1 calc R . . N4 N -0.4509(3) -0.1589(2) 0.0262(2) 0.0181(4) Uani 1 1 d . . . C1 C -0.3017(3) -0.2195(3) -0.3213(3) 0.0168(4) Uani 1 1 d . . . H1 H -0.3215 -0.2839 -0.2698 0.020 Uiso 1 1 calc R . . C2 C -0.4125(3) -0.2782(3) -0.4851(3) 0.0191(4) Uani 1 1 d . . . H2 H -0.5059 -0.3821 -0.5451 0.023 Uiso 1 1 calc R . . C3 C -0.3858(3) -0.1842(3) -0.5602(3) 0.0184(4) Uani 1 1 d . . . H3 H -0.4598 -0.2233 -0.6725 0.022 Uiso 1 1 calc R . . C4 C -0.2492(3) -0.0316(3) -0.4695(3) 0.0149(4) Uani 1 1 d . . . C5 C -0.1402(3) 0.0187(3) -0.3056(3) 0.0169(4) Uani 1 1 d . . . H5 H -0.0442 0.1213 -0.2429 0.020 Uiso 1 1 calc R . . C6 C -0.1443(3) 0.2225(3) -0.4792(3) 0.0174(4) Uani 1 1 d . . . C7 C -0.1078(4) 0.4591(3) -0.5245(3) 0.0217(5) Uani 1 1 d . . . H7A H -0.1456 0.5061 -0.4300 0.026 Uiso 1 1 calc R . . H7B H -0.1880 0.4792 -0.6115 0.026 Uiso 1 1 calc R . . H5AW H 0.1930(17) -0.187(4) -0.007(3) 0.042(10) Uiso 1 1 d D . . H6AW H -0.153(5) -0.538(3) -0.190(4) 0.060(12) Uiso 1 1 d D . . H7AW H 0.183(3) 0.393(5) -0.191(4) 0.076(15) Uiso 1 1 d D . . H5BW H -0.019(4) -0.291(2) -0.084(4) 0.030(8) Uiso 1 1 d D . . H6BW H -0.248(5) -0.447(5) -0.065(3) 0.057(12) Uiso 1 1 d D . . H7BW H 0.374(6) 0.525(3) -0.094(5) 0.076(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0181(2) 0.0158(2) 0.01329(19) 0.00855(15) 0.00307(15) 0.00506(16) O1 0.0262(9) 0.0164(8) 0.0153(7) 0.0074(6) 0.0039(7) 0.0036(7) O2 0.0191(9) 0.0406(11) 0.0251(9) 0.0164(8) 0.0037(7) -0.0031(8) O3 0.0199(8) 0.0355(10) 0.0168(8) 0.0097(7) 0.0063(7) 0.0111(8) O4 0.0257(9) 0.0267(9) 0.0174(8) 0.0068(7) 0.0071(7) 0.0043(8) O5 0.0173(8) 0.0170(8) 0.0183(8) 0.0080(7) 0.0023(6) 0.0052(7) O6 0.0299(10) 0.0204(9) 0.0277(9) 0.0118(8) 0.0118(8) 0.0075(8) O7 0.0267(10) 0.0352(11) 0.0266(10) 0.0157(9) 0.0047(8) 0.0023(9) N1 0.0175(9) 0.0168(9) 0.0159(8) 0.0095(7) 0.0064(7) 0.0066(8) N2 0.0250(10) 0.0160(9) 0.0121(8) 0.0084(7) 0.0031(7) 0.0025(8) N3 0.0294(11) 0.0179(10) 0.0161(9) 0.0099(8) 0.0051(8) 0.0024(9) N4 0.0187(9) 0.0216(10) 0.0167(9) 0.0123(8) 0.0049(7) 0.0066(8) C1 0.0175(10) 0.0173(11) 0.0172(10) 0.0099(9) 0.0059(8) 0.0054(9) C2 0.0178(11) 0.0150(10) 0.0206(11) 0.0089(9) 0.0030(9) 0.0013(9) C3 0.0200(11) 0.0182(11) 0.0143(10) 0.0080(8) 0.0025(8) 0.0045(9) C4 0.0171(10) 0.0152(10) 0.0153(10) 0.0091(8) 0.0064(8) 0.0061(9) C5 0.0184(11) 0.0160(10) 0.0161(10) 0.0086(9) 0.0053(8) 0.0040(9) C6 0.0186(10) 0.0180(11) 0.0170(10) 0.0103(9) 0.0055(8) 0.0059(9) C7 0.0227(12) 0.0229(12) 0.0227(11) 0.0151(10) 0.0059(9) 0.0078(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 Cu1 O5 1.9680(17) 2 ? Cu1 O5 1.9681(17) . ? Cu1 N1 2.0141(19) 2 ? Cu1 N1 2.0142(19) . ? Cu1 O2 2.508(2) . ? O1 C6 1.241(3) . ? O2 N4 1.251(3) . ? O3 N4 1.261(2) . ? O4 N4 1.239(3) . ? O5 H5AW 0.900 . ? O5 H5BW 0.900 . ? O6 H6AW 0.900 . ? O6 H6BW 0.900 . ? O7 H7AW 0.900 . ? O7 H7BW 0.900 . ? N1 C1 1.337(3) . ? N1 C5 1.349(3) . ? N2 C6 1.364(3) . ? N2 C4 1.406(3) . ? N2 H1N 0.8800 . ? N3 C6 1.347(3) . ? N3 C7 1.466(3) . ? N3 H2N 0.8800 . ? C1 C2 1.387(3) . ? C1 H1 0.9500 . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.399(3) . ? C5 H5 0.9500 . ? C7 C7 1.519(5) 2_564 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu1 O5 180.0 2 . ? O5 Cu1 N1 88.82(7) 2 2 ? O5 Cu1 N1 91.18(7) . 2 ? O5 Cu1 N1 91.18(7) 2 . ? O5 Cu1 N1 88.82(7) . . ? N1 Cu1 N1 180.0 2 . ? Cu1 O5 H5AW 111(2) . . ? Cu1 O5 H5BW 118(2) . . ? H5AW O5 H5BW 115(3) . . ? H6AW O6 H6BW 125(4) . . ? H7AW O7 H7BW 112(4) . . ? C1 N1 C5 119.67(19) . . ? C1 N1 Cu1 120.08(15) . . ? C5 N1 Cu1 120.20(15) . . ? C6 N2 C4 126.06(18) . . ? C6 N2 H1N 117.0 . . ? C4 N2 H1N 117.0 . . ? C6 N3 C7 120.67(19) . . ? C6 N3 H2N 119.7 . . ? C7 N3 H2N 119.7 . . ? O4 N4 O2 121.82(19) . . ? O4 N4 O3 120.2(2) . . ? O2 N4 O3 117.95(19) . . ? N1 C1 C2 121.7(2) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.1(2) . . ? C3 C4 N2 117.73(19) . . ? C5 C4 N2 124.1(2) . . ? N1 C5 C4 121.7(2) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? O1 C6 N3 122.3(2) . . ? O1 C6 N2 122.2(2) . . ? N3 C6 N2 115.46(19) . . ? N3 C7 C7 111.8(3) . 2_564 ? N3 C7 H7A 109.3 . . ? C7 C7 H7A 109.3 2_564 . ? N3 C7 H7B 109.3 . . ? C7 C7 H7B 109.3 2_564 . ? H7A C7 H7B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cu1 N1 C1 -128.56(17) 2 . . . ? O5 Cu1 N1 C1 51.44(17) . . . . ? N1 Cu1 N1 C1 88(7) 2 . . . ? O5 Cu1 N1 C5 54.08(17) 2 . . . ? O5 Cu1 N1 C5 -125.92(17) . . . . ? N1 Cu1 N1 C5 -89(7) 2 . . . ? C5 N1 C1 C2 0.8(3) . . . . ? Cu1 N1 C1 C2 -176.53(17) . . . . ? N1 C1 C2 C3 -0.7(4) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C2 C3 C4 N2 179.3(2) . . . . ? C6 N2 C4 C3 160.2(2) . . . . ? C6 N2 C4 C5 -22.3(4) . . . . ? C1 N1 C5 C4 0.3(3) . . . . ? Cu1 N1 C5 C4 177.70(16) . . . . ? C3 C4 C5 N1 -1.6(3) . . . . ? N2 C4 C5 N1 -179.1(2) . . . . ? C7 N3 C6 O1 -11.6(4) . . . . ? C7 N3 C6 N2 166.6(2) . . . . ? C4 N2 C6 O1 2.8(4) . . . . ? C4 N2 C6 N3 -175.4(2) . . . . ? C6 N3 C7 C7 92.4(3) . . . 2_564 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.731 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.095 # Attachment '- 2.cif' data_z:\xraydata\peter\08srv0~2\work\xm _database_code_depnum_ccdc_archive 'CCDC 773254' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 Ag2 Cl6 N16 O10' _chemical_formula_weight 1261.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5449(16) _cell_length_b 13.819(4) _cell_length_c 15.927(5) _cell_angle_alpha 85.794(8) _cell_angle_beta 84.557(8) _cell_angle_gamma 87.260(7) _cell_volume 1210.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.576 _cell_measurement_theta_max 31.830 _exptl_crystal_description 'flat needles' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5371 _exptl_absorpt_correction_T_max 0.8027 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart-6K _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21797 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 32.56 _reflns_number_total 8123 _reflns_number_gt 5974 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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^)+(0.0648P)^2^+0.7129P] 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 8123 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.67364(4) 0.672919(16) 0.245253(16) 0.02791(8) Uani 1 1 d . . . Cl1 Cl 0.57718(17) 0.38791(6) 0.05353(6) 0.03588(19) Uani 1 1 d . . . Cl2 Cl 0.66724(15) 0.19019(6) 0.00332(6) 0.03336(17) Uani 1 1 d . . . Cl3 Cl 0.18823(19) 0.25443(10) 0.06420(11) 0.0767(5) Uani 1 1 d . . . O1 O 0.4392(5) 0.34009(18) 0.40580(16) 0.0382(6) Uani 1 1 d . . . O2 O 0.5702(4) 0.21689(14) 0.63841(14) 0.0243(4) Uani 1 1 d . . . O3 O -0.1690(4) 0.10583(16) 0.32351(15) 0.0319(5) Uani 1 1 d . . . O4 O -0.4495(4) 0.11674(16) 0.23594(16) 0.0350(5) Uani 1 1 d . . . O5 O -0.2082(6) 0.2332(2) 0.23680(19) 0.0534(9) Uani 1 1 d . . . N1 N 0.4005(4) 0.56934(16) 0.22276(16) 0.0209(5) Uani 1 1 d . . . N2 N 0.1644(5) 0.33167(17) 0.30730(17) 0.0263(5) Uani 1 1 d . . . H2N H 0.0526 0.2951 0.2922 0.032 Uiso 1 1 calc R . . N3 N 0.2252(6) 0.20318(18) 0.40239(18) 0.0304(6) Uani 1 1 d . . . H3N H 0.1033 0.1777 0.3815 0.037 Uiso 1 1 calc R . . N4 N 0.3449(4) 0.08933(16) 0.61607(16) 0.0224(5) Uani 1 1 d . . . H4N H 0.3132 0.0280 0.6294 0.027 Uiso 1 1 calc R . . N5 N 0.6270(4) 0.06993(16) 0.71318(17) 0.0229(5) Uani 1 1 d . . . H5N H 0.5778 0.0100 0.7200 0.028 Uiso 1 1 calc R . . N6 N 1.1111(4) 0.19707(17) 0.79861(16) 0.0218(5) Uani 1 1 d . . . N7 N 0.8864(5) 0.60813(18) 0.36490(18) 0.0293(6) Uani 1 1 d . . . N8 N -0.2749(5) 0.15147(18) 0.26561(17) 0.0279(5) Uani 1 1 d . . . C1 C 0.2414(5) 0.59401(19) 0.16569(19) 0.0224(5) Uani 1 1 d . . . H1 H 0.2562 0.6542 0.1331 0.027 Uiso 1 1 calc R . . C2 C 0.0560(5) 0.5345(2) 0.15271(19) 0.0231(6) Uani 1 1 d . . . H2 H -0.0523 0.5531 0.1111 0.028 Uiso 1 1 calc R . . C3 C 0.0304(5) 0.44786(19) 0.20096(19) 0.0216(5) Uani 1 1 d . . . H3 H -0.0977 0.4069 0.1937 0.026 Uiso 1 1 calc R . . C4 C 0.1950(5) 0.42093(18) 0.26075(18) 0.0196(5) Uani 1 1 d . . . C5 C 0.3814(5) 0.48358(19) 0.26926(18) 0.0202(5) Uani 1 1 d . . . H5 H 0.4969 0.4654 0.3086 0.024 Uiso 1 1 calc R . . C6 C 0.2901(6) 0.2945(2) 0.3743(2) 0.0250(6) Uani 1 1 d . . . C7 C 0.3533(6) 0.1472(2) 0.4662(2) 0.0298(7) Uani 1 1 d . . . H7A H 0.5123 0.1757 0.4694 0.036 Uiso 1 1 calc R . . H7B H 0.3837 0.0799 0.4492 0.036 Uiso 1 1 calc R . . C8 C 0.2123(5) 0.1449(2) 0.55309(19) 0.0237(6) Uani 1 1 d . . . H8A H 0.1805 0.2121 0.5701 0.028 Uiso 1 1 calc R . . H8B H 0.0541 0.1156 0.5502 0.028 Uiso 1 1 calc R . . C9 C 0.5168(5) 0.13114(18) 0.65432(18) 0.0195(5) Uani 1 1 d . . . C10 C 0.8079(5) 0.09257(18) 0.76317(18) 0.0193(5) Uani 1 1 d . . . C11 C 0.8773(6) 0.0231(2) 0.8254(2) 0.0251(6) Uani 1 1 d . . . H11 H 0.7974 -0.0366 0.8349 0.030 Uiso 1 1 calc R . . C12 C 1.0635(6) 0.0419(2) 0.8731(2) 0.0270(6) Uani 1 1 d . . . H12 H 1.1129 -0.0046 0.9156 0.032 Uiso 1 1 calc R . . C13 C 1.1775(5) 0.1299(2) 0.8580(2) 0.0250(6) Uani 1 1 d . . . H13 H 1.3058 0.1426 0.8906 0.030 Uiso 1 1 calc R . . C14 C 0.9283(5) 0.18002(19) 0.75278(18) 0.0198(5) Uani 1 1 d . . . H14 H 0.8791 0.2288 0.7120 0.024 Uiso 1 1 calc R . . C15 C 1.0341(6) 0.6011(2) 0.4101(2) 0.0255(6) Uani 1 1 d . . . C16 C 1.2251(7) 0.5920(3) 0.4678(2) 0.0361(8) Uani 1 1 d . . . H16A H 1.2938 0.5252 0.4700 0.054 Uiso 1 1 calc R . . H16B H 1.1569 0.6076 0.5244 0.054 Uiso 1 1 calc R . . H16C H 1.3528 0.6369 0.4476 0.054 Uiso 1 1 calc R . . C17 C 0.4955(6) 0.2661(2) 0.0739(2) 0.0301(6) Uani 1 1 d . . . H17 H 0.5295 0.2441 0.1330 0.036 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 0.02787(12) 0.01700(10) 0.03990(15) -0.00338(8) -0.00327(9) -0.00907(8) Cl1 0.0463(5) 0.0228(3) 0.0378(5) -0.0021(3) 0.0009(4) -0.0034(3) Cl2 0.0330(4) 0.0238(3) 0.0436(5) -0.0029(3) -0.0068(3) 0.0030(3) Cl3 0.0281(5) 0.0731(8) 0.1347(13) -0.0598(9) 0.0061(6) -0.0101(5) O1 0.0471(15) 0.0292(12) 0.0419(15) 0.0082(10) -0.0248(12) -0.0136(10) O2 0.0297(10) 0.0116(8) 0.0319(11) 0.0031(8) -0.0056(9) -0.0052(7) O3 0.0418(13) 0.0217(10) 0.0332(12) 0.0032(9) -0.0069(10) -0.0111(9) O4 0.0397(13) 0.0216(10) 0.0458(14) 0.0031(10) -0.0104(11) -0.0176(9) O5 0.080(2) 0.0353(14) 0.0501(17) 0.0199(12) -0.0314(15) -0.0432(14) N1 0.0226(11) 0.0129(9) 0.0275(13) -0.0014(9) -0.0013(9) -0.0049(8) N2 0.0343(13) 0.0149(10) 0.0315(14) 0.0041(9) -0.0125(11) -0.0108(9) N3 0.0459(16) 0.0167(11) 0.0299(14) 0.0049(10) -0.0116(12) -0.0073(10) N4 0.0282(12) 0.0133(10) 0.0263(13) 0.0012(9) -0.0047(10) -0.0060(8) N5 0.0287(12) 0.0111(9) 0.0296(13) 0.0039(9) -0.0070(10) -0.0069(8) N6 0.0239(11) 0.0148(10) 0.0273(13) -0.0027(9) -0.0022(9) -0.0050(8) N7 0.0335(14) 0.0190(11) 0.0348(15) -0.0020(10) -0.0015(12) 0.0023(10) N8 0.0388(14) 0.0173(11) 0.0281(13) -0.0011(10) -0.0010(11) -0.0123(10) C1 0.0281(14) 0.0134(11) 0.0261(15) -0.0004(10) -0.0030(11) -0.0033(10) C2 0.0249(13) 0.0187(12) 0.0259(15) -0.0002(10) -0.0060(11) 0.0014(10) C3 0.0217(13) 0.0163(11) 0.0276(15) -0.0034(10) -0.0035(11) -0.0041(9) C4 0.0248(13) 0.0120(10) 0.0224(13) -0.0017(9) -0.0020(10) -0.0049(9) C5 0.0235(13) 0.0132(11) 0.0245(14) -0.0001(10) -0.0046(10) -0.0025(9) C6 0.0340(15) 0.0160(12) 0.0253(15) 0.0003(10) -0.0051(12) -0.0027(11) C7 0.0410(17) 0.0194(13) 0.0277(16) 0.0025(11) -0.0017(13) 0.0050(12) C8 0.0253(13) 0.0200(12) 0.0258(15) 0.0003(11) -0.0044(11) -0.0015(10) C9 0.0224(12) 0.0130(11) 0.0229(14) -0.0013(9) 0.0003(10) -0.0031(9) C10 0.0214(12) 0.0132(11) 0.0232(14) -0.0011(9) 0.0006(10) -0.0044(9) C11 0.0302(14) 0.0141(11) 0.0308(16) 0.0031(11) -0.0029(12) -0.0051(10) C12 0.0319(15) 0.0194(13) 0.0300(16) 0.0039(11) -0.0081(12) -0.0023(11) C13 0.0252(14) 0.0210(13) 0.0297(16) -0.0015(11) -0.0061(11) -0.0021(10) C14 0.0210(12) 0.0129(10) 0.0253(14) 0.0002(10) -0.0002(10) -0.0037(9) C15 0.0319(15) 0.0138(11) 0.0297(16) 0.0013(10) 0.0010(12) -0.0022(10) C16 0.0393(18) 0.0310(16) 0.0394(19) 0.0074(14) -0.0135(15) -0.0119(14) C17 0.0318(16) 0.0274(15) 0.0320(17) -0.0040(12) -0.0033(13) -0.0072(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.204(2) . ? Ag1 N6 2.237(2) 2_766 ? Ag1 N7 2.429(3) . ? Cl1 C17 1.763(3) . ? Cl2 C17 1.773(3) . ? Cl3 C17 1.741(3) . ? O1 C6 1.227(4) . ? O2 C9 1.238(3) . ? O3 N8 1.255(4) . ? O4 N8 1.247(3) . ? O5 N8 1.247(3) . ? N1 C1 1.341(4) . ? N1 C5 1.354(3) . ? N2 C6 1.384(4) . ? N2 C4 1.401(3) . ? N2 H2N 0.8800 . ? N3 C6 1.361(4) . ? N3 C7 1.450(4) . ? N3 H3N 0.8800 . ? N4 C9 1.352(4) . ? N4 C8 1.452(4) . ? N4 H4N 0.8800 . ? N5 C9 1.382(4) . ? N5 C10 1.399(4) . ? N5 H5N 0.8800 . ? N6 C13 1.341(4) . ? N6 C14 1.343(4) . ? N6 Ag1 2.237(2) 2_766 ? N7 C15 1.137(4) . ? C1 C2 1.387(4) . ? C1 H1 0.9500 . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C4 1.399(4) . ? C3 H3 0.9500 . ? C4 C5 1.402(4) . ? C5 H5 0.9500 . ? C7 C8 1.523(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.396(4) . ? C10 C14 1.400(3) . ? C11 C12 1.384(4) . ? C11 H11 0.9500 . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.461(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 149.68(10) . 2_766 ? N1 Ag1 N7 108.45(9) . . ? N6 Ag1 N7 101.11(9) 2_766 . ? C1 N1 C5 119.4(2) . . ? C1 N1 Ag1 119.53(18) . . ? C5 N1 Ag1 120.97(19) . . ? C6 N2 C4 127.4(2) . . ? C6 N2 H2N 116.3 . . ? C4 N2 H2N 116.3 . . ? C6 N3 C7 121.2(3) . . ? C6 N3 H3N 119.4 . . ? C7 N3 H3N 119.4 . . ? C9 N4 C8 120.5(2) . . ? C9 N4 H4N 119.8 . . ? C8 N4 H4N 119.8 . . ? C9 N5 C10 127.3(2) . . ? C9 N5 H5N 116.4 . . ? C10 N5 H5N 116.4 . . ? C13 N6 C14 119.5(2) . . ? C13 N6 Ag1 123.52(19) . 2_766 ? C14 N6 Ag1 116.14(18) . 2_766 ? C15 N7 Ag1 157.6(2) . . ? O5 N8 O4 118.5(3) . . ? O5 N8 O3 120.5(3) . . ? O4 N8 O3 121.1(2) . . ? N1 C1 C2 122.1(2) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 N2 117.4(2) . . ? C3 C4 C5 118.3(2) . . ? N2 C4 C5 124.3(3) . . ? N1 C5 C4 121.5(3) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? O1 C6 N3 124.1(3) . . ? O1 C6 N2 123.5(3) . . ? N3 C6 N2 112.4(3) . . ? N3 C7 C8 112.4(3) . . ? N3 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? N4 C8 C7 111.4(2) . . ? N4 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N4 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O2 C9 N4 123.0(3) . . ? O2 C9 N5 122.8(3) . . ? N4 C9 N5 114.2(2) . . ? C11 C10 N5 118.2(2) . . ? C11 C10 C14 118.1(3) . . ? N5 C10 C14 123.6(3) . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 119.2(3) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? N6 C13 C12 121.7(3) . . ? N6 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? N6 C14 C10 122.1(3) . . ? N6 C14 H14 119.0 . . ? C10 C14 H14 119.0 . . ? N7 C15 C16 179.6(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl3 C17 Cl1 111.0(2) . . ? Cl3 C17 Cl2 109.09(18) . . ? Cl1 C17 Cl2 110.76(18) . . ? Cl3 C17 H17 108.6 . . ? Cl1 C17 H17 108.6 . . ? Cl2 C17 H17 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C1 -20.7(3) 2_766 . . . ? N7 Ag1 N1 C1 172.7(2) . . . . ? N6 Ag1 N1 C5 163.3(2) 2_766 . . . ? N7 Ag1 N1 C5 -3.3(2) . . . . ? N1 Ag1 N7 C15 165.9(6) . . . . ? N6 Ag1 N7 C15 -7.3(7) 2_766 . . . ? C5 N1 C1 C2 0.2(4) . . . . ? Ag1 N1 C1 C2 -175.8(2) . . . . ? N1 C1 C2 C3 1.3(4) . . . . ? C1 C2 C3 C4 -1.3(4) . . . . ? C2 C3 C4 N2 -179.0(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C6 N2 C4 C3 -173.7(3) . . . . ? C6 N2 C4 C5 7.5(5) . . . . ? C1 N1 C5 C4 -1.7(4) . . . . ? Ag1 N1 C5 C4 174.3(2) . . . . ? C3 C4 C5 N1 1.6(4) . . . . ? N2 C4 C5 N1 -179.6(3) . . . . ? C7 N3 C6 O1 -8.2(5) . . . . ? C7 N3 C6 N2 173.4(3) . . . . ? C4 N2 C6 O1 5.1(5) . . . . ? C4 N2 C6 N3 -176.5(3) . . . . ? C6 N3 C7 C8 103.1(4) . . . . ? C9 N4 C8 C7 83.5(3) . . . . ? N3 C7 C8 N4 -179.4(2) . . . . ? C8 N4 C9 O2 0.0(4) . . . . ? C8 N4 C9 N5 179.6(2) . . . . ? C10 N5 C9 O2 0.4(5) . . . . ? C10 N5 C9 N4 -179.2(3) . . . . ? C9 N5 C10 C11 173.3(3) . . . . ? C9 N5 C10 C14 -8.5(5) . . . . ? N5 C10 C11 C12 177.1(3) . . . . ? C14 C10 C11 C12 -1.2(4) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C14 N6 C13 C12 0.7(4) . . . . ? Ag1 N6 C13 C12 -168.5(2) 2_766 . . . ? C11 C12 C13 N6 0.3(5) . . . . ? C13 N6 C14 C10 -1.9(4) . . . . ? Ag1 N6 C14 C10 168.0(2) 2_766 . . . ? C11 C10 C14 N6 2.2(4) . . . . ? N5 C10 C14 N6 -176.0(3) . . . . ? Ag1 N7 C15 C16 -61(45) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.447 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.129 # Attachment '- 4.CIF' data_z:\xraydata\peter\08srv351\work\platon _database_code_depnum_ccdc_archive 'CCDC 773255' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H27 Ag N6 O8' _chemical_formula_weight 539.31 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8864(5) _cell_length_b 12.0430(10) _cell_length_c 13.2699(10) _cell_angle_alpha 78.535(3) _cell_angle_beta 77.905(3) _cell_angle_gamma 78.335(3) _cell_volume 1039.71(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4613 _cell_measurement_theta_min 2.165 _cell_measurement_theta_max 32.017 _exptl_crystal_description 'flat needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7671 _exptl_absorpt_correction_T_max 0.9043 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart-6K _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15692 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 32.50 _reflns_number_total 7102 _reflns_number_gt 5317 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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. DFIX restraints used on water hydrogen atoms to fix them in a chemically sensible geometry. ; _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^)+(0.0355P)^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 7102 _refine_ls_number_parameters 312 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 0.20836(3) 0.540062(17) 0.908928(14) 0.01983(6) Uani 1 1 d . . . O1 O 0.3563(3) 0.27095(15) 0.44887(13) 0.0204(4) Uani 1 1 d . . . O2 O 1.1321(2) -0.19269(15) 0.35864(13) 0.0187(3) Uani 1 1 d . . . O3 O 0.6073(3) -0.14681(15) 0.15072(14) 0.0240(4) Uani 1 1 d . . . O4 O 0.5108(3) 0.01135(15) 0.22149(14) 0.0214(4) Uani 1 1 d . . . O5 O 0.2052(3) 0.16927(16) 0.30778(14) 0.0231(4) Uani 1 1 d D . . O6 O 0.0513(3) 0.25596(16) 0.12500(14) 0.0218(4) Uani 1 1 d D . . O7 O 0.3935(3) 0.29230(16) -0.02270(14) 0.0226(4) Uani 1 1 d D . . O8 O 0.6658(3) 0.21235(18) 0.11548(16) 0.0314(5) Uani 1 1 d D . . N1 N 0.2393(3) 0.51480(16) 0.74852(14) 0.0139(4) Uani 1 1 d . . . N2 N 0.4744(3) 0.28866(16) 0.59387(14) 0.0141(4) Uani 1 1 d . . . H2N H 0.5523 0.2514 0.6387 0.017 Uiso 1 1 calc R . . N3 N 0.6379(3) 0.15205(17) 0.49452(15) 0.0168(4) Uani 1 1 d . . . H3N H 0.7225 0.1318 0.5389 0.020 Uiso 1 1 calc R . . N4 N 0.8425(3) -0.07235(17) 0.32890(15) 0.0158(4) Uani 1 1 d . . . H4N H 0.7473 -0.0523 0.2905 0.019 Uiso 1 1 calc R . . N5 N 0.9651(3) -0.21645(16) 0.23271(14) 0.0142(4) Uani 1 1 d . . . H5N H 0.8673 -0.1843 0.1976 0.017 Uiso 1 1 calc R . . N6 N 1.1929(3) -0.43503(16) 0.06834(14) 0.0145(4) Uani 1 1 d . . . C1 C 0.3365(3) 0.41551(19) 0.71778(17) 0.0131(4) Uani 1 1 d . . . H1 H 0.3963 0.3578 0.7674 0.016 Uiso 1 1 calc R . . C2 C 0.3546(3) 0.39221(19) 0.61677(17) 0.0124(4) Uani 1 1 d . . . C3 C 0.2591(3) 0.4752(2) 0.54589(17) 0.0155(4) Uani 1 1 d . . . H3 H 0.2632 0.4618 0.4772 0.019 Uiso 1 1 calc R . . C4 C 0.1577(4) 0.5779(2) 0.57729(18) 0.0168(5) Uani 1 1 d . . . H4 H 0.0918 0.6358 0.5300 0.020 Uiso 1 1 calc R . . C5 C 0.1529(4) 0.5958(2) 0.67776(18) 0.0167(5) Uani 1 1 d . . . H5 H 0.0867 0.6675 0.6975 0.020 Uiso 1 1 calc R . . C6 C 0.4815(3) 0.2397(2) 0.50751(17) 0.0149(4) Uani 1 1 d . . . C7 C 0.6647(4) 0.0916(2) 0.40630(18) 0.0175(5) Uani 1 1 d . . . H7B H 0.6907 0.1456 0.3401 0.021 Uiso 1 1 calc R . . H7A H 0.5399 0.0620 0.4077 0.021 Uiso 1 1 calc R . . C8 C 0.8389(3) -0.00722(19) 0.41093(17) 0.0153(4) Uani 1 1 d . . . H8B H 0.9671 0.0223 0.4001 0.018 Uiso 1 1 calc R . . H8A H 0.8216 -0.0570 0.4801 0.018 Uiso 1 1 calc R . . C9 C 0.9883(3) -0.16254(19) 0.31079(17) 0.0137(4) Uani 1 1 d . . . C10 C 1.0944(3) -0.3374(2) 0.10290(17) 0.0140(4) Uani 1 1 d . . . H10 H 1.0288 -0.2789 0.0560 0.017 Uiso 1 1 calc R . . C11 C 1.0839(3) -0.31792(19) 0.20468(16) 0.0122(4) Uani 1 1 d . . . C12 C 1.1825(3) -0.4038(2) 0.27221(17) 0.0153(4) Uani 1 1 d . . . H12 H 1.1799 -0.3938 0.3417 0.018 Uiso 1 1 calc R . . C13 C 1.2844(3) -0.5039(2) 0.23665(18) 0.0156(4) Uani 1 1 d . . . H13 H 1.3517 -0.5636 0.2819 0.019 Uiso 1 1 calc R . . C14 C 1.2879(3) -0.5169(2) 0.13486(18) 0.0154(4) Uani 1 1 d . . . H14 H 1.3595 -0.5858 0.1112 0.018 Uiso 1 1 calc R . . C15 C 0.4846(3) -0.0568(2) 0.16661(17) 0.0159(4) Uani 1 1 d . . . C16 C 0.3003(4) -0.0266(2) 0.11522(19) 0.0201(5) Uani 1 1 d . . . H16F H 0.2197 0.0454 0.1345 0.030 Uiso 0.50 1 calc PR . . H16B H 0.2195 -0.0883 0.1387 0.030 Uiso 0.50 1 calc PR . . H16D H 0.3422 -0.0175 0.0392 0.030 Uiso 0.50 1 calc PR . . H16C H 0.3012 -0.0857 0.0737 0.030 Uiso 0.50 1 calc PR . . H16E H 0.3014 0.0480 0.0695 0.030 Uiso 0.50 1 calc PR . . H16A H 0.1787 -0.0227 0.1691 0.030 Uiso 0.50 1 calc PR . . H5AW H 0.261(5) 0.206(3) 0.350(2) 0.053(11) Uiso 1 1 d D . . H6AW H 0.101(5) 0.228(3) 0.1892(13) 0.047(10) Uiso 1 1 d D . . H7AW H 0.511(3) 0.265(2) 0.009(2) 0.034(9) Uiso 1 1 d D . . H8AW H 0.635(5) 0.1399(14) 0.154(2) 0.048(10) Uiso 1 1 d D . . H5BW H 0.311(4) 0.111(2) 0.284(3) 0.079(14) Uiso 1 1 d D . . H6BW H 0.173(3) 0.261(3) 0.075(2) 0.061(12) Uiso 1 1 d D . . H7BW H 0.416(5) 0.238(2) -0.069(2) 0.053(11) Uiso 1 1 d D . . H8BW H 0.8053(16) 0.209(4) 0.117(3) 0.087(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02420(10) 0.02298(10) 0.01438(8) -0.00986(7) -0.00258(7) -0.00288(7) O1 0.0239(9) 0.0198(9) 0.0204(8) -0.0100(7) -0.0110(7) 0.0037(7) O2 0.0188(8) 0.0202(9) 0.0199(8) -0.0102(7) -0.0085(7) 0.0024(7) O3 0.0261(9) 0.0202(9) 0.0299(10) -0.0114(8) -0.0163(8) 0.0053(7) O4 0.0222(9) 0.0190(9) 0.0265(9) -0.0087(7) -0.0121(7) 0.0016(7) O5 0.0218(9) 0.0254(10) 0.0239(9) -0.0098(8) -0.0095(8) 0.0032(8) O6 0.0206(9) 0.0248(10) 0.0209(9) -0.0072(7) -0.0070(7) 0.0012(7) O7 0.0240(9) 0.0220(9) 0.0241(9) -0.0102(7) -0.0081(8) 0.0011(8) O8 0.0322(11) 0.0337(12) 0.0307(11) 0.0083(9) -0.0147(9) -0.0150(9) N1 0.0151(9) 0.0140(9) 0.0132(9) -0.0045(7) -0.0023(7) -0.0016(7) N2 0.0173(9) 0.0134(9) 0.0124(8) -0.0059(7) -0.0055(7) 0.0025(7) N3 0.0195(10) 0.0162(10) 0.0163(9) -0.0097(8) -0.0089(8) 0.0062(8) N4 0.0165(9) 0.0171(10) 0.0164(9) -0.0093(8) -0.0085(8) 0.0038(8) N5 0.0149(9) 0.0154(9) 0.0141(9) -0.0072(7) -0.0063(7) 0.0022(7) N6 0.0150(9) 0.0157(10) 0.0137(9) -0.0060(7) -0.0019(7) -0.0019(7) C1 0.0141(10) 0.0131(10) 0.0135(10) -0.0041(8) -0.0034(8) -0.0022(8) C2 0.0130(10) 0.0127(10) 0.0126(10) -0.0039(8) -0.0030(8) -0.0024(8) C3 0.0188(11) 0.0155(11) 0.0128(10) -0.0043(8) -0.0033(9) -0.0016(9) C4 0.0190(11) 0.0142(11) 0.0162(11) -0.0016(9) -0.0058(9) 0.0016(9) C5 0.0187(11) 0.0136(11) 0.0177(11) -0.0052(9) -0.0025(9) -0.0005(9) C6 0.0165(11) 0.0145(11) 0.0147(10) -0.0059(8) -0.0025(9) -0.0014(9) C7 0.0220(12) 0.0158(11) 0.0157(10) -0.0078(9) -0.0081(9) 0.0047(9) C8 0.0168(11) 0.0159(11) 0.0149(10) -0.0084(9) -0.0046(9) 0.0012(9) C9 0.0155(10) 0.0136(11) 0.0127(10) -0.0045(8) -0.0023(8) -0.0017(8) C10 0.0153(11) 0.0147(11) 0.0125(10) -0.0042(8) -0.0030(8) -0.0013(8) C11 0.0123(10) 0.0135(10) 0.0118(10) -0.0059(8) -0.0016(8) -0.0016(8) C12 0.0167(11) 0.0179(11) 0.0126(10) -0.0028(9) -0.0045(9) -0.0033(9) C13 0.0152(11) 0.0158(11) 0.0164(10) -0.0036(9) -0.0044(9) -0.0013(9) C14 0.0140(11) 0.0143(11) 0.0189(11) -0.0074(9) -0.0019(9) -0.0013(8) C15 0.0191(11) 0.0154(11) 0.0132(10) -0.0009(8) -0.0057(9) -0.0012(9) C16 0.0191(12) 0.0191(12) 0.0240(12) -0.0047(10) -0.0096(10) -0.0003(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 N1 2.1703(18) . ? Ag1 N6 2.1729(18) 1_466 ? O1 C6 1.234(3) . ? O2 C9 1.241(3) . ? O3 C15 1.257(3) . ? O4 C15 1.260(3) . ? O5 H5AW 0.96(3) . ? O5 H5BW 0.96(3) . ? O6 H6AW 0.96(2) . ? O6 H6BW 0.96(2) . ? O7 H7AW 0.96(2) . ? O7 H7BW 0.96(2) . ? O8 H8AW 0.96(2) . ? O8 H8BW 0.96(2) . ? N1 C1 1.342(3) . ? N1 C5 1.350(3) . ? N2 C6 1.377(3) . ? N2 C2 1.399(3) . ? N2 H2N 0.8800 . ? N3 C6 1.356(3) . ? N3 C7 1.459(3) . ? N3 H3N 0.8800 . ? N4 C9 1.345(3) . ? N4 C8 1.456(3) . ? N4 H4N 0.8800 . ? N5 C9 1.378(3) . ? N5 C11 1.396(3) . ? N5 H5N 0.8800 . ? N6 C10 1.347(3) . ? N6 C14 1.347(3) . ? N6 Ag1 2.1729(18) 1_644 ? C1 C2 1.399(3) . ? C1 H1 0.9500 . ? C2 C3 1.391(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.511(3) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C10 C11 1.401(3) . ? C10 H10 0.9500 . ? C11 C12 1.391(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.512(3) . ? C16 H16F 0.9800 . ? C16 H16B 0.9800 . ? C16 H16D 0.9800 . ? C16 H16C 0.9800 . ? C16 H16E 0.9800 . ? C16 H16A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 177.26(7) . 1_466 ? H5AW O5 H5BW 105(3) . . ? H6AW O6 H6BW 103(3) . . ? H7AW O7 H7BW 99(3) . . ? H8AW O8 H8BW 104(3) . . ? C1 N1 C5 117.74(19) . . ? C1 N1 Ag1 120.91(15) . . ? C5 N1 Ag1 121.27(15) . . ? C6 N2 C2 125.97(19) . . ? C6 N2 H2N 117.0 . . ? C2 N2 H2N 117.0 . . ? C6 N3 C7 119.39(18) . . ? C6 N3 H3N 120.3 . . ? C7 N3 H3N 120.3 . . ? C9 N4 C8 121.23(19) . . ? C9 N4 H4N 119.4 . . ? C8 N4 H4N 119.4 . . ? C9 N5 C11 125.39(19) . . ? C9 N5 H5N 117.3 . . ? C11 N5 H5N 117.3 . . ? C10 N6 C14 118.08(19) . . ? C10 N6 Ag1 121.73(15) . 1_644 ? C14 N6 Ag1 120.16(14) . 1_644 ? N1 C1 C2 123.7(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 117.8(2) . . ? C3 C2 N2 125.1(2) . . ? C1 C2 N2 117.10(19) . . ? C4 C3 C2 118.8(2) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 122.2(2) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? O1 C6 N3 123.3(2) . . ? O1 C6 N2 123.5(2) . . ? N3 C6 N2 113.14(19) . . ? N3 C7 C8 110.47(18) . . ? N3 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? N3 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? H7B C7 H7A 108.1 . . ? N4 C8 C7 107.83(18) . . ? N4 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? N4 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? H8B C8 H8A 108.5 . . ? O2 C9 N4 123.0(2) . . ? O2 C9 N5 123.4(2) . . ? N4 C9 N5 113.58(19) . . ? N6 C10 C11 123.2(2) . . ? N6 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C12 C11 N5 124.71(19) . . ? C12 C11 C10 117.8(2) . . ? N5 C11 C10 117.4(2) . . ? C13 C12 C11 119.1(2) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 119.8(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N6 C14 C13 122.1(2) . . ? N6 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? O3 C15 O4 122.9(2) . . ? O3 C15 C16 118.8(2) . . ? O4 C15 C16 118.3(2) . . ? C15 C16 H16F 109.5 . . ? C15 C16 H16B 109.5 . . ? H16F C16 H16B 109.5 . . ? C15 C16 H16D 109.5 . . ? H16F C16 H16D 109.5 . . ? H16B C16 H16D 109.5 . . ? C15 C16 H16C 109.5 . . ? H16F C16 H16C 141.1 . . ? H16B C16 H16C 56.3 . . ? H16D C16 H16C 56.3 . . ? C15 C16 H16E 109.5 . . ? H16F C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16D C16 H16E 56.3 . . ? H16C C16 H16E 109.5 . . ? C15 C16 H16A 109.5 . . ? H16F C16 H16A 56.3 . . ? H16B C16 H16A 56.3 . . ? H16D C16 H16A 141.1 . . ? H16C C16 H16A 109.5 . . ? H16E C16 H16A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C1 66.3(16) 1_466 . . . ? N6 Ag1 N1 C5 -117.1(15) 1_466 . . . ? C5 N1 C1 C2 0.7(3) . . . . ? Ag1 N1 C1 C2 177.36(16) . . . . ? N1 C1 C2 C3 -2.7(3) . . . . ? N1 C1 C2 N2 174.9(2) . . . . ? C6 N2 C2 C3 -15.7(4) . . . . ? C6 N2 C2 C1 166.9(2) . . . . ? C1 C2 C3 C4 2.4(3) . . . . ? N2 C2 C3 C4 -175.0(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C1 N1 C5 C4 1.7(3) . . . . ? Ag1 N1 C5 C4 -174.95(17) . . . . ? C3 C4 C5 N1 -2.0(4) . . . . ? C7 N3 C6 O1 1.1(4) . . . . ? C7 N3 C6 N2 179.9(2) . . . . ? C2 N2 C6 O1 -13.5(4) . . . . ? C2 N2 C6 N3 167.7(2) . . . . ? C6 N3 C7 C8 -176.3(2) . . . . ? C9 N4 C8 C7 176.7(2) . . . . ? N3 C7 C8 N4 173.11(19) . . . . ? C8 N4 C9 O2 -3.3(4) . . . . ? C8 N4 C9 N5 178.1(2) . . . . ? C11 N5 C9 O2 7.5(4) . . . . ? C11 N5 C9 N4 -173.9(2) . . . . ? C14 N6 C10 C11 -0.9(3) . . . . ? Ag1 N6 C10 C11 -179.08(16) 1_644 . . . ? C9 N5 C11 C12 28.1(3) . . . . ? C9 N5 C11 C10 -155.9(2) . . . . ? N6 C10 C11 C12 0.7(3) . . . . ? N6 C10 C11 N5 -175.6(2) . . . . ? N5 C11 C12 C13 175.6(2) . . . . ? C10 C11 C12 C13 -0.4(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C10 N6 C14 C13 0.8(3) . . . . ? Ag1 N6 C14 C13 179.06(17) 1_644 . . . ? C12 C13 C14 N6 -0.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.132 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.117 # Attachment '- 5.CIF' data_Z:\mss\Current\Metallogel\srv354m\SRV354M.CIF _database_code_depnum_ccdc_archive 'CCDC 773256' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common srv354m _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H23 Ag F3 N7 O3 Si0.50' _chemical_formula_weight 552.34 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' Si Si 0.0817 0.0704 '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 P21/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 9.0260(8) _cell_length_b 16.3903(17) _cell_length_c 14.0277(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.969(3) _cell_angle_gamma 90.00 _cell_volume 2055.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8556 _exptl_absorpt_correction_T_max 0.9096 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 SMART6000 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15292 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4722 _reflns_number_gt 2915 _reflns_threshold_expression >2sigma(I) _computing_data_collection Saint _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4722 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _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 0.52068(3) 0.241131(19) 0.70719(2) 0.02392(9) Uani 1 1 d . . . Si1 Si 0.0000 0.5000 0.5000 0.0214(3) Uani 1 2 d S . . F1 F 0.0747(2) 0.41354(14) 0.54888(17) 0.0305(6) Uani 1 1 d . . . F2 F -0.0611(2) 0.44916(14) 0.39636(16) 0.0317(6) Uani 1 1 d . . . F3 F -0.1638(2) 0.47989(14) 0.54139(17) 0.0317(6) Uani 1 1 d . . . O1 O -0.2580(3) 0.17766(17) 0.5113(2) 0.0276(7) Uani 1 1 d . . . O2 O -0.6718(2) 0.25124(17) 0.32877(16) 0.0204(5) Uani 1 1 d . . . O3 O 0.4422(3) 0.39522(17) 0.6840(2) 0.0307(7) Uani 1 1 d . . . N1 N 0.3210(3) 0.18194(19) 0.6301(2) 0.0207(7) Uani 1 1 d . . . N2 N -0.0478(3) 0.2584(2) 0.5366(2) 0.0201(7) Uani 1 1 d . . . H2A H -0.0167 0.3090 0.5324 0.024 Uiso 1 1 calc R . . N3 N -0.2777(3) 0.3159(2) 0.4988(2) 0.0209(8) Uani 1 1 d . . . H3A H -0.2284 0.3618 0.4946 0.025 Uiso 1 1 calc R . . N4 N -0.6678(3) 0.37720(19) 0.3965(2) 0.0218(7) Uani 1 1 d . . . H4 H -0.7198 0.4188 0.4135 0.026 Uiso 1 1 calc R . . N5 N -0.8926(3) 0.31409(19) 0.3464(2) 0.0210(7) Uani 1 1 d . . . H5A H -0.9321 0.3590 0.3665 0.025 Uiso 1 1 calc R . . N6 N -1.2497(3) 0.22132(18) 0.2508(2) 0.0174(7) Uani 1 1 d . . . N7 N 0.3721(4) 0.4598(2) 0.8154(2) 0.0248(8) Uani 1 1 d . . . C1 C 0.2978(4) 0.1013(2) 0.6323(3) 0.0236(9) Uani 1 1 d . . . H1 H 0.3782 0.0668 0.6578 0.028 Uiso 1 1 calc R . . C2 C 0.1612(4) 0.0668(3) 0.5989(3) 0.0272(10) Uani 1 1 d . . . H2 H 0.1492 0.0092 0.5998 0.033 Uiso 1 1 calc R . . C3 C 0.0414(4) 0.1163(3) 0.5641(3) 0.0244(9) Uani 1 1 d . . . H3 H -0.0532 0.0932 0.5407 0.029 Uiso 1 1 calc R . . C4 C 0.0620(4) 0.1997(2) 0.5641(2) 0.0187(8) Uani 1 1 d . . . C5 C 0.2054(4) 0.2306(2) 0.5958(3) 0.0203(9) Uani 1 1 d . . . H5 H 0.2216 0.2878 0.5930 0.024 Uiso 1 1 calc R . . C6 C -0.2002(4) 0.2453(3) 0.5152(2) 0.0210(8) Uani 1 1 d . . . C7 C -0.4408(4) 0.3177(2) 0.4879(3) 0.0221(9) Uani 1 1 d . . . H7A H -0.4734 0.3321 0.5503 0.027 Uiso 1 1 calc R . . H7B H -0.4805 0.2628 0.4693 0.027 Uiso 1 1 calc R . . C8 C -0.5045(4) 0.3795(2) 0.4116(3) 0.0217(9) Uani 1 1 d . . . H8A H -0.4704 0.4350 0.4322 0.026 Uiso 1 1 calc R . . H8B H -0.4666 0.3673 0.3502 0.026 Uiso 1 1 calc R . . C9 C -0.7384(4) 0.3099(2) 0.3559(3) 0.0189(8) Uani 1 1 d . . . C10 C -1.1433(4) 0.2739(2) 0.2868(2) 0.0183(9) Uani 1 1 d . . . H10 H -1.1717 0.3284 0.2988 0.022 Uiso 1 1 calc R . . C11 C -0.9918(3) 0.2528(2) 0.3076(2) 0.0173(8) Uani 1 1 d . . . C12 C -0.9530(4) 0.1733(2) 0.2892(3) 0.0223(9) Uani 1 1 d . . . H12 H -0.8519 0.1560 0.3031 0.027 Uiso 1 1 calc R . . C13 C -1.0622(4) 0.1193(2) 0.2508(3) 0.0244(9) Uani 1 1 d . . . H13 H -1.0366 0.0648 0.2367 0.029 Uiso 1 1 calc R . . C14 C -1.2088(4) 0.1449(2) 0.2329(3) 0.0211(9) Uani 1 1 d . . . H14 H -1.2834 0.1071 0.2070 0.025 Uiso 1 1 calc R . . C15 C 0.3627(4) 0.4433(2) 0.7209(3) 0.0247(9) Uani 1 1 d . . . H15 H 0.2879 0.4713 0.6789 0.030 Uiso 1 1 calc R . . C16 C 0.2695(5) 0.5163(3) 0.8514(3) 0.0360(11) Uani 1 1 d . . . H16A H 0.2936 0.5206 0.9215 0.054 Uiso 0.50 1 calc PR . . H16B H 0.1668 0.4963 0.8348 0.054 Uiso 0.50 1 calc PR . . H16C H 0.2788 0.5700 0.8222 0.054 Uiso 0.50 1 calc PR . . H16D H 0.1992 0.5373 0.7975 0.054 Uiso 0.50 1 calc PR . . H16E H 0.3260 0.5617 0.8842 0.054 Uiso 0.50 1 calc PR . . H16F H 0.2140 0.4880 0.8968 0.054 Uiso 0.50 1 calc PR . . C17 C 0.4784(4) 0.4168(2) 0.8865(3) 0.0288(10) Uani 1 1 d . . . H17A H 0.4691 0.4371 0.9511 0.043 Uiso 0.50 1 calc PR . . H17B H 0.5805 0.4263 0.8726 0.043 Uiso 0.50 1 calc PR . . H17C H 0.4568 0.3582 0.8833 0.043 Uiso 0.50 1 calc PR . . H17D H 0.5352 0.3773 0.8536 0.043 Uiso 0.50 1 calc PR . . H17E H 0.4238 0.3881 0.9321 0.043 Uiso 0.50 1 calc PR . . H17F H 0.5474 0.4563 0.9213 0.043 Uiso 0.50 1 calc PR . . 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 0.01517(13) 0.02602(18) 0.02907(15) 0.00445(16) -0.00219(10) -0.00133(15) Si1 0.0199(8) 0.0133(9) 0.0299(9) -0.0006(6) 0.0004(7) 0.0020(6) F1 0.0300(13) 0.0205(14) 0.0395(15) -0.0010(11) 0.0002(12) 0.0015(10) F2 0.0301(13) 0.0258(15) 0.0374(14) -0.0050(11) -0.0015(11) 0.0040(10) F3 0.0252(13) 0.0266(15) 0.0447(15) -0.0034(11) 0.0097(11) -0.0006(10) O1 0.0178(15) 0.0227(18) 0.0405(18) 0.0051(13) -0.0022(14) -0.0053(12) O2 0.0140(11) 0.0232(16) 0.0241(12) -0.0065(13) 0.0035(10) 0.0020(12) O3 0.0321(17) 0.0286(19) 0.0313(17) -0.0017(13) 0.0041(14) 0.0077(13) N1 0.0211(17) 0.018(2) 0.0226(17) -0.0005(13) 0.0018(15) 0.0005(13) N2 0.0169(16) 0.0155(19) 0.0272(16) 0.0017(15) 0.0004(13) -0.0052(14) N3 0.0126(16) 0.023(2) 0.0261(19) 0.0029(14) -0.0010(15) -0.0041(13) N4 0.0144(16) 0.020(2) 0.0308(19) -0.0045(14) 0.0019(15) 0.0025(13) N5 0.0109(16) 0.0184(19) 0.0330(19) -0.0067(14) 0.0005(15) 0.0011(13) N6 0.0163(16) 0.0178(19) 0.0183(16) 0.0003(12) 0.0024(13) 0.0003(12) N7 0.0261(19) 0.019(2) 0.0285(19) 0.0001(14) 0.0015(16) 0.0020(14) C1 0.023(2) 0.020(2) 0.028(2) -0.0005(17) 0.0046(18) 0.0047(16) C2 0.031(2) 0.017(2) 0.032(2) 0.0013(17) 0.000(2) -0.0007(17) C3 0.017(2) 0.026(3) 0.029(2) -0.0032(18) -0.0019(18) -0.0067(16) C4 0.018(2) 0.024(2) 0.0140(19) -0.0013(15) 0.0008(16) -0.0013(16) C5 0.0167(18) 0.020(2) 0.024(2) -0.0017(16) -0.0006(16) -0.0030(16) C6 0.0215(18) 0.023(2) 0.0179(17) 0.0023(18) -0.0003(15) -0.0043(18) C7 0.016(2) 0.028(3) 0.022(2) 0.0026(17) -0.0003(17) -0.0022(16) C8 0.0148(19) 0.018(2) 0.031(2) -0.0011(17) -0.0002(17) -0.0028(15) C9 0.0151(19) 0.019(2) 0.023(2) 0.0039(16) 0.0031(17) -0.0011(15) C10 0.0179(19) 0.016(2) 0.0202(19) -0.0029(15) 0.0006(16) 0.0006(15) C11 0.0145(17) 0.018(2) 0.0201(18) 0.0020(17) 0.0033(14) -0.0008(15) C12 0.0147(19) 0.023(2) 0.028(2) 0.0015(17) -0.0004(17) 0.0012(16) C13 0.027(2) 0.017(2) 0.029(2) -0.0032(17) 0.0055(19) 0.0046(17) C14 0.020(2) 0.023(2) 0.020(2) 0.0021(16) 0.0010(17) -0.0033(16) C15 0.021(2) 0.022(2) 0.030(2) 0.0011(18) -0.0010(19) -0.0032(17) C16 0.044(3) 0.024(3) 0.041(3) -0.005(2) 0.010(2) 0.009(2) C17 0.032(2) 0.022(3) 0.030(2) 0.0007(18) -0.004(2) -0.0027(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 N6 2.167(3) 4_766 ? Ag1 N1 2.195(3) . ? Si1 F1 1.675(2) . ? Si1 F1 1.675(2) 3_566 ? Si1 F3 1.694(2) 3_566 ? Si1 F3 1.694(2) . ? Si1 F2 1.700(2) 3_566 ? Si1 F2 1.700(2) . ? O1 C6 1.223(5) . ? O2 C9 1.222(4) . ? O3 C15 1.227(5) . ? N1 C1 1.339(5) . ? N1 C5 1.348(5) . ? N2 C6 1.384(4) . ? N2 C4 1.396(5) . ? N2 H2A 0.8800 . ? N3 C6 1.355(5) . ? N3 C7 1.460(4) . ? N3 H3A 0.8800 . ? N4 C9 1.358(5) . ? N4 C8 1.460(4) . ? N4 H4 0.8800 . ? N5 C9 1.382(4) . ? N5 C11 1.404(4) . ? N5 H5A 0.8800 . ? N6 C10 1.337(4) . ? N6 C14 1.339(5) . ? N6 Ag1 2.167(3) 4_365 ? N7 C15 1.345(5) . ? N7 C16 1.448(5) . ? N7 C17 1.465(5) . ? C1 C2 1.379(5) . ? C1 H1 0.9500 . ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.380(5) . ? C3 H3 0.9500 . ? C4 C5 1.404(5) . ? C5 H5 0.9500 . ? C7 C8 1.527(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.401(5) . ? C10 H10 0.9500 . ? C11 C12 1.383(5) . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16E 0.9800 . ? C16 H16F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N1 162.23(11) 4_766 . ? F1 Si1 F1 180.00(15) . 3_566 ? F1 Si1 F3 89.07(11) . 3_566 ? F1 Si1 F3 90.93(11) 3_566 3_566 ? F1 Si1 F3 90.93(11) . . ? F1 Si1 F3 89.07(11) 3_566 . ? F3 Si1 F3 180.000(1) 3_566 . ? F1 Si1 F2 90.01(11) . 3_566 ? F1 Si1 F2 89.99(11) 3_566 3_566 ? F3 Si1 F2 90.16(11) 3_566 3_566 ? F3 Si1 F2 89.84(11) . 3_566 ? F1 Si1 F2 89.99(11) . . ? F1 Si1 F2 90.01(11) 3_566 . ? F3 Si1 F2 89.84(11) 3_566 . ? F3 Si1 F2 90.16(11) . . ? F2 Si1 F2 180.000(1) 3_566 . ? C1 N1 C5 118.5(3) . . ? C1 N1 Ag1 123.0(2) . . ? C5 N1 Ag1 117.1(3) . . ? C6 N2 C4 126.8(4) . . ? C6 N2 H2A 116.6 . . ? C4 N2 H2A 116.6 . . ? C6 N3 C7 121.6(3) . . ? C6 N3 H3A 119.2 . . ? C7 N3 H3A 119.2 . . ? C9 N4 C8 119.1(3) . . ? C9 N4 H4 120.4 . . ? C8 N4 H4 120.4 . . ? C9 N5 C11 125.6(3) . . ? C9 N5 H5A 117.2 . . ? C11 N5 H5A 117.2 . . ? C10 N6 C14 118.1(3) . . ? C10 N6 Ag1 122.2(2) . 4_365 ? C14 N6 Ag1 119.4(2) . 4_365 ? C15 N7 C16 121.1(3) . . ? C15 N7 C17 121.3(3) . . ? C16 N7 C17 117.4(3) . . ? N1 C1 C2 122.2(4) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 119.8(4) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 N2 126.3(3) . . ? C3 C4 C5 118.4(4) . . ? N2 C4 C5 115.3(3) . . ? N1 C5 C4 122.2(4) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? O1 C6 N3 124.0(3) . . ? O1 C6 N2 123.7(4) . . ? N3 C6 N2 112.2(4) . . ? N3 C7 C8 111.3(3) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C7 111.0(3) . . ? N4 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N4 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? O2 C9 N4 123.2(3) . . ? O2 C9 N5 122.8(3) . . ? N4 C9 N5 114.1(3) . . ? N6 C10 C11 123.3(3) . . ? N6 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C12 C11 C10 117.3(3) . . ? C12 C11 N5 125.6(3) . . ? C10 C11 N5 117.1(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 119.5(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? N6 C14 C13 122.3(3) . . ? N6 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? O3 C15 N7 125.7(4) . . ? O3 C15 H15 117.1 . . ? N7 C15 H15 117.1 . . ? N7 C16 H16A 109.5 . . ? N7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N7 C16 H16D 109.5 . . ? H16A C16 H16D 141.1 . . ? H16B C16 H16D 56.3 . . ? H16C C16 H16D 56.3 . . ? N7 C16 H16E 109.5 . . ? H16A C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16C C16 H16E 56.3 . . ? H16D C16 H16E 109.5 . . ? N7 C16 H16F 109.5 . . ? H16A C16 H16F 56.3 . . ? H16B C16 H16F 56.3 . . ? H16C C16 H16F 141.1 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? N7 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? N7 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? N7 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C1 67.3(5) 4_766 . . . ? N6 Ag1 N1 C5 -126.3(4) 4_766 . . . ? C5 N1 C1 C2 1.4(6) . . . . ? Ag1 N1 C1 C2 167.7(3) . . . . ? N1 C1 C2 C3 -1.9(6) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C2 C3 C4 N2 -176.4(4) . . . . ? C2 C3 C4 C5 2.6(6) . . . . ? C6 N2 C4 C3 8.3(6) . . . . ? C6 N2 C4 C5 -170.7(3) . . . . ? C1 N1 C5 C4 1.1(6) . . . . ? Ag1 N1 C5 C4 -166.0(3) . . . . ? C3 C4 C5 N1 -3.1(6) . . . . ? N2 C4 C5 N1 176.0(3) . . . . ? C7 N3 C6 O1 8.7(5) . . . . ? C7 N3 C6 N2 -171.5(3) . . . . ? C4 N2 C6 O1 -5.4(6) . . . . ? C4 N2 C6 N3 174.8(3) . . . . ? C6 N3 C7 C8 -142.6(3) . . . . ? C9 N4 C8 C7 -67.6(4) . . . . ? N3 C7 C8 N4 176.3(3) . . . . ? C8 N4 C9 O2 -1.8(6) . . . . ? C8 N4 C9 N5 179.1(3) . . . . ? C11 N5 C9 O2 1.4(6) . . . . ? C11 N5 C9 N4 -179.5(3) . . . . ? C14 N6 C10 C11 -0.7(5) . . . . ? Ag1 N6 C10 C11 -174.2(3) 4_365 . . . ? N6 C10 C11 C12 0.1(5) . . . . ? N6 C10 C11 N5 -179.1(3) . . . . ? C9 N5 C11 C12 12.9(6) . . . . ? C9 N5 C11 C10 -167.9(3) . . . . ? C10 C11 C12 C13 0.9(5) . . . . ? N5 C11 C12 C13 -180.0(3) . . . . ? C11 C12 C13 C14 -1.3(6) . . . . ? C10 N6 C14 C13 0.3(5) . . . . ? Ag1 N6 C14 C13 174.0(3) 4_365 . . . ? C12 C13 C14 N6 0.7(6) . . . . ? C16 N7 C15 O3 -178.3(4) . . . . ? C17 N7 C15 O3 -3.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A F1 0.88 1.90 2.769(4) 167.9 . N3 H3A F3 0.88 2.10 2.910(4) 152.6 . N3 H3A F2 0.88 2.61 3.382(4) 147.1 . N4 H4 F3 0.88 2.11 2.987(4) 177.5 3_466 N5 H5A F2 0.88 1.96 2.828(4) 167.4 1_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.774 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.107 # Attachment '- 6.CIF' data_z:\xraydata\peter\08srv353\work\platon _database_code_depnum_ccdc_archive 'CCDC 773257' #TrackingRef '- 6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Ag B F4 N6 O3' _chemical_formula_weight 527.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1412(13) _cell_length_b 9.2472(12) _cell_length_c 11.3257(15) _cell_angle_alpha 84.346(4) _cell_angle_beta 84.501(4) _cell_angle_gamma 87.385(4) _cell_volume 947.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5694 _cell_measurement_theta_min 2.215 _cell_measurement_theta_max 30.958 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7346 _exptl_absorpt_correction_T_max 0.8854 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'smart - 6K' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18399 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 32.96 _reflns_number_total 6538 _reflns_number_gt 5073 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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^)+(0.0251P)^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 6538 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 0.256754(17) 0.019736(17) 0.497460(14) 0.02118(5) Uani 1 1 d . . . F1 F 0.77620(14) 0.26661(13) 0.34747(13) 0.0359(3) Uani 1 1 d . . . F2 F 0.55164(13) 0.37687(13) 0.32669(13) 0.0357(3) Uani 1 1 d . . . F3 F 0.75685(14) 0.49674(14) 0.25600(12) 0.0360(3) Uani 1 1 d . . . F4 F 0.70200(19) 0.45487(15) 0.45424(13) 0.0489(4) Uani 1 1 d . . . O1 O 0.13035(14) 0.20858(14) 0.06642(12) 0.0213(3) Uani 1 1 d . . . O2 O 0.37077(13) -0.20822(14) 0.92321(12) 0.0192(3) Uani 1 1 d . . . O3 O 0.26257(17) 0.28573(17) 0.35957(16) 0.0359(4) Uani 1 1 d . . . H3M H 0.3488 0.3153 0.3518 0.043 Uiso 1 1 calc R . . N1 N 0.11160(17) -0.05786(17) 0.38113(14) 0.0183(3) Uani 1 1 d . . . N2 N -0.08537(16) 0.09494(16) 0.12594(13) 0.0165(3) Uani 1 1 d . . . H2N H -0.1743 0.0847 0.1050 0.020 Uiso 1 1 calc R . . N3 N -0.08624(17) 0.31760(16) 0.01717(14) 0.0184(3) Uani 1 1 d . . . H3N H -0.1822 0.3107 0.0195 0.022 Uiso 1 1 calc R . . N4 N 0.58151(17) -0.31634(16) 0.98601(14) 0.0172(3) Uani 1 1 d . . . H4N H 0.6767 -0.3090 0.9892 0.021 Uiso 1 1 calc R . . N5 N 0.58920(16) -0.09612(16) 0.87402(14) 0.0167(3) Uani 1 1 d . . . H5N H 0.6792 -0.0916 0.8946 0.020 Uiso 1 1 calc R . . N6 N 0.40177(17) 0.08013(17) 0.62127(14) 0.0179(3) Uani 1 1 d . . . C1 C 0.0654(2) 0.0343(2) 0.29210(16) 0.0168(4) Uani 1 1 d . . . H1 H 0.1007 0.1302 0.2812 0.020 Uiso 1 1 calc R . . C2 C -0.03299(19) -0.00621(19) 0.21466(16) 0.0158(4) Uani 1 1 d . . . C3 C -0.0840(2) -0.1459(2) 0.23176(17) 0.0192(4) Uani 1 1 d . . . H3 H -0.1504 -0.1767 0.1805 0.023 Uiso 1 1 calc R . . C4 C -0.0374(2) -0.2406(2) 0.32456(18) 0.0216(4) Uani 1 1 d . . . H4 H -0.0727 -0.3364 0.3384 0.026 Uiso 1 1 calc R . . C5 C 0.0614(2) -0.1937(2) 0.39698(18) 0.0211(4) Uani 1 1 d . . . H5 H 0.0946 -0.2593 0.4596 0.025 Uiso 1 1 calc R . . C6 C -0.00616(19) 0.2083(2) 0.07039(16) 0.0159(4) Uani 1 1 d . . . C7 C -0.0178(2) 0.4465(2) -0.04391(17) 0.0188(4) Uani 1 1 d . . . H7A H -0.0848 0.4956 -0.1002 0.023 Uiso 1 1 calc R . . H7B H 0.0741 0.4172 -0.0906 0.023 Uiso 1 1 calc R . . C8 C 0.5098(2) -0.44451(19) 1.04418(16) 0.0168(4) Uani 1 1 d . . . H8A H 0.4122 -0.4155 1.0823 0.020 Uiso 1 1 calc R . . H8B H 0.5692 -0.4899 1.1075 0.020 Uiso 1 1 calc R . . C9 C 0.50584(19) -0.20792(19) 0.92701(16) 0.0150(3) Uani 1 1 d . . . C10 C 0.4452(2) -0.02026(19) 0.70669(16) 0.0161(4) Uani 1 1 d . . . H10 H 0.4098 -0.1158 0.7111 0.019 Uiso 1 1 calc R . . C11 C 0.54073(19) 0.01199(19) 0.78884(16) 0.0146(3) Uani 1 1 d . . . C12 C 0.5929(2) 0.15125(19) 0.78122(17) 0.0177(4) Uani 1 1 d . . . H12 H 0.6583 0.1762 0.8357 0.021 Uiso 1 1 calc R . . C13 C 0.5481(2) 0.2535(2) 0.69294(18) 0.0222(4) Uani 1 1 d . . . H13 H 0.5833 0.3493 0.6858 0.027 Uiso 1 1 calc R . . C14 C 0.4517(2) 0.2153(2) 0.61537(18) 0.0214(4) Uani 1 1 d . . . H14 H 0.4199 0.2867 0.5562 0.026 Uiso 1 1 calc R . . C15 C 0.1634(3) 0.4041(3) 0.3456(2) 0.0438(6) Uani 1 1 d . . . H15C H 0.1478 0.4508 0.4200 0.066 Uiso 1 1 calc R . . H15A H 0.0695 0.3704 0.3256 0.066 Uiso 1 1 calc R . . H15B H 0.2032 0.4742 0.2813 0.066 Uiso 1 1 calc R . . B1 B 0.6977(3) 0.3999(2) 0.3465(2) 0.0221(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01885(7) 0.02843(8) 0.01648(7) -0.00099(5) -0.00443(5) 0.00015(5) F1 0.0342(8) 0.0280(7) 0.0479(8) -0.0083(6) -0.0163(6) 0.0077(5) F2 0.0224(7) 0.0310(7) 0.0511(9) 0.0073(6) -0.0008(6) -0.0033(5) F3 0.0305(7) 0.0415(8) 0.0340(7) 0.0099(6) -0.0001(6) -0.0137(6) F4 0.0841(12) 0.0351(8) 0.0291(8) -0.0078(6) -0.0125(8) 0.0059(7) O1 0.0119(6) 0.0259(7) 0.0246(7) 0.0069(6) -0.0031(5) -0.0018(5) O2 0.0104(6) 0.0230(7) 0.0231(7) 0.0054(5) -0.0030(5) -0.0016(5) O3 0.0269(9) 0.0341(9) 0.0464(10) 0.0060(7) -0.0087(8) -0.0084(7) N1 0.0156(8) 0.0225(8) 0.0162(8) 0.0004(6) -0.0023(6) 0.0018(6) N2 0.0116(7) 0.0194(8) 0.0181(8) 0.0035(6) -0.0037(6) -0.0015(6) N3 0.0121(7) 0.0188(8) 0.0234(8) 0.0046(6) -0.0028(6) -0.0020(6) N4 0.0121(7) 0.0163(7) 0.0226(8) 0.0032(6) -0.0041(6) -0.0008(6) N5 0.0117(7) 0.0173(8) 0.0204(8) 0.0042(6) -0.0038(6) -0.0015(6) N6 0.0169(8) 0.0198(8) 0.0162(8) 0.0001(6) -0.0006(6) 0.0009(6) C1 0.0151(9) 0.0161(9) 0.0182(9) 0.0009(7) -0.0006(7) 0.0006(7) C2 0.0131(8) 0.0186(9) 0.0149(9) 0.0006(7) -0.0004(7) 0.0009(7) C3 0.0179(9) 0.0176(9) 0.0220(10) -0.0021(7) -0.0011(8) -0.0013(7) C4 0.0238(10) 0.0159(9) 0.0248(10) 0.0015(7) -0.0035(8) -0.0020(7) C5 0.0222(10) 0.0198(9) 0.0199(10) 0.0039(7) -0.0023(8) 0.0020(7) C6 0.0137(8) 0.0194(9) 0.0142(9) -0.0005(7) -0.0008(7) 0.0000(7) C7 0.0164(9) 0.0197(9) 0.0192(9) 0.0052(7) -0.0028(7) -0.0010(7) C8 0.0169(9) 0.0164(9) 0.0164(9) 0.0027(7) -0.0022(7) -0.0010(7) C9 0.0142(8) 0.0170(9) 0.0138(8) -0.0008(7) -0.0020(7) -0.0004(7) C10 0.0159(9) 0.0154(8) 0.0165(9) 0.0001(7) -0.0012(7) -0.0003(7) C11 0.0119(8) 0.0163(8) 0.0145(9) -0.0001(7) 0.0015(7) 0.0014(6) C12 0.0179(9) 0.0181(9) 0.0175(9) -0.0032(7) -0.0019(7) -0.0010(7) C13 0.0300(11) 0.0146(9) 0.0218(10) 0.0002(7) -0.0020(8) -0.0032(8) C14 0.0276(11) 0.0168(9) 0.0186(9) 0.0014(7) -0.0012(8) 0.0023(8) C15 0.0519(17) 0.0360(14) 0.0460(16) -0.0018(11) -0.0174(13) -0.0060(12) B1 0.0242(11) 0.0205(11) 0.0211(11) 0.0007(8) -0.0020(9) -0.0015(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 N6 2.1479(16) . ? Ag1 N1 2.1493(16) . ? F1 B1 1.398(3) . ? F2 B1 1.404(3) . ? F3 B1 1.379(3) . ? F4 B1 1.372(3) . ? O1 C6 1.244(2) . ? O2 C9 1.240(2) . ? O3 C15 1.396(3) . ? O3 H3M 0.8400 . ? N1 C1 1.342(2) . ? N1 C5 1.346(2) . ? N2 C6 1.368(2) . ? N2 C2 1.407(2) . ? N2 H2N 0.8800 . ? N3 C6 1.348(2) . ? N3 C7 1.454(2) . ? N3 H3N 0.8800 . ? N4 C9 1.350(2) . ? N4 C8 1.450(2) . ? N4 H4N 0.8800 . ? N5 C9 1.368(2) . ? N5 C11 1.406(2) . ? N5 H5N 0.8800 . ? N6 C14 1.343(2) . ? N6 C10 1.348(2) . ? C1 C2 1.402(2) . ? C1 H1 0.9500 . ? C2 C3 1.383(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C7 1.535(4) 2_565 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C8 1.530(4) 2_647 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.397(2) . ? C10 H10 0.9500 . ? C11 C12 1.385(3) . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.382(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N1 175.39(6) . . ? C15 O3 H3M 109.5 . . ? C1 N1 C5 118.94(16) . . ? C1 N1 Ag1 118.63(12) . . ? C5 N1 Ag1 122.38(12) . . ? C6 N2 C2 123.83(15) . . ? C6 N2 H2N 118.1 . . ? C2 N2 H2N 118.1 . . ? C6 N3 C7 121.54(15) . . ? C6 N3 H3N 119.2 . . ? C7 N3 H3N 119.2 . . ? C9 N4 C8 121.59(15) . . ? C9 N4 H4N 119.2 . . ? C8 N4 H4N 119.2 . . ? C9 N5 C11 124.38(15) . . ? C9 N5 H5N 117.8 . . ? C11 N5 H5N 117.8 . . ? C14 N6 C10 118.89(16) . . ? C14 N6 Ag1 121.75(12) . . ? C10 N6 Ag1 119.35(12) . . ? N1 C1 C2 122.25(17) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.37(16) . . ? C3 C2 N2 120.57(16) . . ? C1 C2 N2 120.96(16) . . ? C2 C3 C4 119.34(17) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.19(18) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.90(17) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? O1 C6 N3 122.44(17) . . ? O1 C6 N2 122.36(16) . . ? N3 C6 N2 115.17(16) . . ? N3 C7 C7 111.76(19) . 2_565 ? N3 C7 H7A 109.3 . . ? C7 C7 H7A 109.3 2_565 . ? N3 C7 H7B 109.3 . . ? C7 C7 H7B 109.3 2_565 . ? H7A C7 H7B 107.9 . . ? N4 C8 C8 111.58(19) . 2_647 ? N4 C8 H8A 109.3 . . ? C8 C8 H8A 109.3 2_647 . ? N4 C8 H8B 109.3 . . ? C8 C8 H8B 109.3 2_647 . ? H8A C8 H8B 108.0 . . ? O2 C9 N4 122.58(16) . . ? O2 C9 N5 122.56(16) . . ? N4 C9 N5 114.85(16) . . ? N6 C10 C11 122.00(17) . . ? N6 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 118.67(16) . . ? C12 C11 N5 120.33(16) . . ? C10 C11 N5 120.92(16) . . ? C13 C12 C11 118.93(17) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 119.60(18) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N6 C14 C13 121.90(17) . . ? N6 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? O3 C15 H15C 109.5 . . ? O3 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? F4 B1 F3 109.92(18) . . ? F4 B1 F1 109.27(18) . . ? F3 B1 F1 110.42(18) . . ? F4 B1 F2 110.03(19) . . ? F3 B1 F2 108.77(17) . . ? F1 B1 F2 108.41(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C1 -180(25) . . . . ? N6 Ag1 N1 C5 2.5(8) . . . . ? N1 Ag1 N6 C14 -179(35) . . . . ? N1 Ag1 N6 C10 1.3(8) . . . . ? C5 N1 C1 C2 -0.2(3) . . . . ? Ag1 N1 C1 C2 -177.89(13) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? N1 C1 C2 N2 176.69(16) . . . . ? C6 N2 C2 C3 -152.64(18) . . . . ? C6 N2 C2 C1 31.0(3) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? N2 C2 C3 C4 -176.05(18) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C1 N1 C5 C4 -0.5(3) . . . . ? Ag1 N1 C5 C4 177.07(15) . . . . ? C3 C4 C5 N1 1.2(3) . . . . ? C7 N3 C6 O1 -2.9(3) . . . . ? C7 N3 C6 N2 179.04(16) . . . . ? C2 N2 C6 O1 21.8(3) . . . . ? C2 N2 C6 N3 -160.15(17) . . . . ? C6 N3 C7 C7 -79.3(3) . . . 2_565 ? C9 N4 C8 C8 81.8(2) . . . 2_647 ? C8 N4 C9 O2 3.1(3) . . . . ? C8 N4 C9 N5 -178.28(16) . . . . ? C11 N5 C9 O2 -15.0(3) . . . . ? C11 N5 C9 N4 166.37(16) . . . . ? C14 N6 C10 C11 -0.2(3) . . . . ? Ag1 N6 C10 C11 179.24(13) . . . . ? N6 C10 C11 C12 -0.5(3) . . . . ? N6 C10 C11 N5 -177.37(16) . . . . ? C9 N5 C11 C12 148.77(18) . . . . ? C9 N5 C11 C10 -34.4(3) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? N5 C11 C12 C13 177.15(17) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C10 N6 C14 C13 1.1(3) . . . . ? Ag1 N6 C14 C13 -178.28(15) . . . . ? C12 C13 C14 N6 -1.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.192 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.095 # Attachment '- 7.CIF' data_Z:\mss\Current\Metallogel\PLATON.CIF _database_code_depnum_ccdc_archive 'CCDC 773258' #TrackingRef '- 7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'thf macrocycle' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H92 Ag2 N14 O16' _chemical_formula_weight 1649.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z' 'x, -y, z+1/2' _cell_length_a 24.723(3) _cell_length_b 17.1669(19) _cell_length_c 17.388(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7379.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8880 _exptl_absorpt_correction_T_max 0.9702 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 SMART1000 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40550 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13276 _reflns_number_gt 9254 _reflns_threshold_expression >2sigma(I) _computing_data_collection SAINT _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material X-SEED _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. Refinement revealed a stranger disorder involving a second set of positions for the two independent half-macrocycles. This second position is a very minor component (ca. 0.1 occupancy) and has almost no effect on the light atom positions and hence was not modelled but the presence of the disordered Ag ions causes difficulties with the refinment of N1 and N10 and hence the minor Ag positions were included in the refinement with fixed occupancy of 0.1. The largest residual peaks apart from these 'ghost' Ag positions are associated with solvent molecules. ; _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^)+(0.1108P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(4) _refine_ls_number_reflns 13276 _refine_ls_number_parameters 972 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.19392(3) 0.15803(4) 0.41947(3) 0.02931(18) Uani 1 1 d . A 1 O1 O 0.2996(2) -0.0281(3) 0.2487(3) 0.0313(14) Uani 1 1 d . A 1 C1 C 0.1649(3) -0.0100(5) 0.4712(5) 0.032(2) Uani 1 1 d . A 1 H1 H 0.1417 0.0169 0.5058 0.038 Uiso 1 1 calc R A 1 Ag2 Ag 0.30588(3) 0.38459(4) 0.01425(4) 0.0327(2) Uani 1 1 d . B 1 O2 O 0.2999(3) 0.3470(4) 0.2476(4) 0.0302(16) Uani 1 1 d . A 1 N2 N 0.2638(3) -0.1287(4) 0.3190(4) 0.0292(17) Uani 1 1 d . A 1 H2N H 0.2653 -0.1795 0.3252 0.035 Uiso 1 1 calc R A 1 C2 C 0.1648(3) -0.0919(5) 0.4711(5) 0.029(2) Uani 1 1 d . A 1 H2 H 0.1422 -0.1200 0.5055 0.034 Uiso 1 1 calc R A 1 O3 O 0.2093(3) 0.5743(4) 0.1944(4) 0.0451(19) Uani 1 1 d . B 1 N3 N 0.3208(3) -0.1549(4) 0.2206(4) 0.0259(15) Uani 1 1 d . A 1 H3N H 0.3109 -0.2031 0.2306 0.031 Uiso 1 1 calc R A 1 C3 C 0.1975(3) -0.1300(5) 0.4211(6) 0.0286(17) Uani 1 1 d . A 1 H3 H 0.1983 -0.1853 0.4207 0.034 Uiso 1 1 calc R A 1 O4 O 0.1996(3) 0.1925(4) 0.1814(5) 0.053(2) Uani 1 1 d . B 1 N4 N 0.1832(3) 0.2837(4) 0.4081(4) 0.0273(16) Uani 1 1 d . A 1 C4 C 0.2292(3) -0.0889(5) 0.3715(5) 0.023(2) Uani 1 1 d . A 1 O5 O 0.2917(3) -0.4060(4) 0.3498(4) 0.053(2) Uani 1 1 d . . . N5 N 0.2470(3) 0.4449(4) 0.3012(4) 0.0293(16) Uani 1 1 d . A 1 H5N H 0.2383 0.4942 0.2947 0.035 Uiso 1 1 calc R A 1 C5 C 0.2280(3) -0.0051(5) 0.3748(5) 0.0257(19) Uani 1 1 d . A 1 H5 H 0.2500 0.0251 0.3412 0.031 Uiso 1 1 calc R A 1 O6 O 0.2593(3) -0.2875(4) 0.3585(4) 0.0524(17) Uani 1 1 d . . . N6 N 0.3232(3) 0.4757(4) 0.2329(4) 0.0302(16) Uani 1 1 d . A 1 H6N H 0.3164 0.5223 0.2518 0.036 Uiso 1 1 calc R A 1 C6 C 0.2953(3) -0.0996(6) 0.2599(6) 0.028(2) Uani 1 1 d . A 1 O7 O 0.3121(3) -0.3186(4) 0.2654(4) 0.0456(17) Uani 1 1 d . . . N7 N 0.3029(3) 0.5111(3) 0.0085(5) 0.0296(15) Uani 1 1 d . B 1 C7 C 0.3607(3) -0.1460(5) 0.1661(5) 0.029(2) Uani 1 1 d . A 1 O8 O 0.2111(4) 0.8257(4) 0.0690(4) 0.059(2) Uani 1 1 d . . . N8 N 0.2373(3) 0.6702(4) 0.1110(4) 0.0311(17) Uani 1 1 d . B 1 H8N H 0.2350 0.7205 0.1019 0.037 Uiso 1 1 calc R B 1 C8 C 0.3817(4) -0.0760(5) 0.1386(5) 0.033(2) Uani 1 1 d . A 1 H8 H 0.3657 -0.0286 0.1553 0.040 Uiso 1 1 calc R A 1 O9 O 0.1880(3) 0.8826(6) 0.1693(5) 0.070(3) Uani 1 1 d . . . N9 N 0.1762(3) 0.7007(4) 0.2054(4) 0.0341(17) Uani 1 1 d . B 1 H9N H 0.1816 0.7483 0.1883 0.041 Uiso 1 1 calc R B 1 C9 C 0.4236(3) -0.0725(5) 0.0896(5) 0.0285(18) Uani 1 1 d . A 1 H9 H 0.4357 -0.0229 0.0728 0.034 Uiso 1 1 calc R A 1 O10 O 0.2418(3) 0.9364(4) 0.0877(4) 0.0548(19) Uani 1 1 d . . . C10 C 0.4503(3) -0.1395(5) 0.0620(5) 0.0273(19) Uani 1 1 d . A 1 N11 N 0.2532(3) 0.0976(4) 0.1313(4) 0.0315(17) Uani 1 1 d . B 1 H11N H 0.2616 0.0480 0.1358 0.038 Uiso 1 1 calc R B 1 C11 C 0.4294(3) -0.2112(6) 0.0869(5) 0.036(2) Uani 1 1 d . A 1 H11 H 0.4447 -0.2585 0.0687 0.044 Uiso 1 1 calc R A 1 N12 N 0.1820(3) 0.0650(4) 0.2048(4) 0.0293(16) Uani 1 1 d . B 1 H12N H 0.1919 0.0176 0.1916 0.035 Uiso 1 1 calc R B 1 C12 C 0.3860(3) -0.2128(5) 0.1386(5) 0.028(2) Uani 1 1 d . A 1 H12 H 0.3733 -0.2620 0.1559 0.033 Uiso 1 1 calc R A 1 N13 N 0.2861(3) -0.3371(4) 0.3251(5) 0.0276(17) Uani 1 1 d . . . C13 C 0.5000 -0.1367(6) 0.0126(9) 0.032(3) Uani 1 2 d S . 1 H13A H 0.5000 -0.1814 -0.0234 0.038 Uiso 1 2 calc SR . 1 H13B H 0.5000 -0.0881 -0.0182 0.038 Uiso 1 2 calc SR . 1 N14 N 0.2119(3) 0.8808(4) 0.1077(5) 0.0303(19) Uani 1 1 d . . . C14 C 0.1520(3) 0.3246(6) 0.4542(5) 0.028(2) Uani 1 1 d . A 1 H14 H 0.1299 0.2975 0.4900 0.034 Uiso 1 1 calc R A 1 C15 C 0.1499(3) 0.4029(6) 0.4530(5) 0.0303(19) Uani 1 1 d . A 1 H15 H 0.1266 0.4303 0.4869 0.036 Uiso 1 1 calc R A 1 C16 C 0.1819(3) 0.4423(5) 0.4022(5) 0.032(2) Uani 1 1 d . A 1 H16 H 0.1817 0.4977 0.4016 0.038 Uiso 1 1 calc R A 1 C17 C 0.2146(3) 0.4021(5) 0.3516(5) 0.0236(18) Uani 1 1 d . A 1 C18 C 0.2140(3) 0.3205(5) 0.3575(5) 0.022(2) Uani 1 1 d . A 1 H18 H 0.2364 0.2908 0.3242 0.026 Uiso 1 1 calc R A 1 C19 C 0.2919(3) 0.4174(5) 0.2597(5) 0.0232(19) Uani 1 1 d . A 1 C20 C 0.3650(3) 0.4716(5) 0.1791(5) 0.0238(18) Uani 1 1 d . A 1 C21 C 0.3884(3) 0.5426(5) 0.1576(5) 0.0261(19) Uani 1 1 d . A 1 H21 H 0.3755 0.5897 0.1798 0.031 Uiso 1 1 calc R A 1 C22 C 0.4288(3) 0.5450(5) 0.1059(5) 0.0290(19) Uani 1 1 d . A 1 H22 H 0.4433 0.5938 0.0905 0.035 Uiso 1 1 calc R A 1 C23 C 0.4504(3) 0.4743(5) 0.0735(5) 0.0269(19) Uani 1 1 d . A 1 C24 C 0.4265(3) 0.4067(5) 0.0951(5) 0.0285(19) Uani 1 1 d . A 1 H24 H 0.4388 0.3594 0.0728 0.034 Uiso 1 1 calc R A 1 C25 C 0.3850(4) 0.4036(5) 0.1481(5) 0.031(2) Uani 1 1 d . A 1 H25 H 0.3703 0.3548 0.1631 0.038 Uiso 1 1 calc R A 1 C26 C 0.5000 0.4757(7) 0.0215(7) 0.034(3) Uani 1 2 d S . 1 H26A H 0.5000 0.4297 -0.0130 0.041 Uiso 1 2 calc SR . 1 H26B H 0.5000 0.5233 -0.0105 0.041 Uiso 1 2 calc SR . 1 C27 C 0.3334(3) 0.5491(5) -0.0405(5) 0.029(2) Uani 1 1 d . B 1 H27 H 0.3564 0.5215 -0.0747 0.035 Uiso 1 1 calc R B 1 C28 C 0.3321(3) 0.6287(6) -0.0421(5) 0.036(2) Uani 1 1 d . B 1 H28 H 0.3524 0.6558 -0.0800 0.043 Uiso 1 1 calc R B 1 C29 C 0.3016(3) 0.6705(4) 0.0104(6) 0.0291(18) Uani 1 1 d . B 1 H29 H 0.3023 0.7258 0.0113 0.035 Uiso 1 1 calc R B 1 C30 C 0.2695(3) 0.6276(5) 0.0628(5) 0.0271(19) Uani 1 1 d . B 1 C31 C 0.2710(3) 0.5470(5) 0.0591(5) 0.024(2) Uani 1 1 d . B 1 H31 H 0.2490 0.5171 0.0929 0.029 Uiso 1 1 calc R B 1 C32 C 0.2077(4) 0.6418(5) 0.1731(6) 0.032(2) Uani 1 1 d . B 1 C33 C 0.1350(3) 0.6905(5) 0.2651(5) 0.029(2) Uani 1 1 d . B 1 C34 C 0.1130(4) 0.7576(6) 0.2927(6) 0.039(2) Uani 1 1 d . B 1 H34 H 0.1266 0.8070 0.2773 0.047 Uiso 1 1 calc R B 1 C35 C 0.0701(4) 0.7520(5) 0.3440(5) 0.035(2) Uani 1 1 d . B 1 H35 H 0.0534 0.7981 0.3628 0.042 Uiso 1 1 calc R B 1 C36 C 0.0518(4) 0.6815(6) 0.3677(5) 0.035(2) Uani 1 1 d . B 1 C37 C 0.0749(4) 0.6166(5) 0.3417(5) 0.034(2) Uani 1 1 d . B 1 H37 H 0.0612 0.5680 0.3589 0.041 Uiso 1 1 calc R B 1 C38 C 0.1200(3) 0.6168(5) 0.2887(5) 0.029(2) Uani 1 1 d . B 1 H38 H 0.1375 0.5706 0.2717 0.035 Uiso 1 1 calc R B 1 C39 C 0.0000 0.6756(8) 0.4167(9) 0.041(3) Uani 1 2 d S . 1 H39A H 0.0000 0.6254 0.4446 0.049 Uiso 1 2 calc SR . 1 H39B H 0.0000 0.7180 0.4554 0.049 Uiso 1 2 calc SR . 1 C40 C 0.3483(4) 0.2204(5) -0.0222(5) 0.033(2) Uani 1 1 d . B 1 H40 H 0.3697 0.2485 -0.0580 0.039 Uiso 1 1 calc R B 1 C41 C 0.3506(4) 0.1383(6) -0.0210(6) 0.033(2) Uani 1 1 d . B 1 H41 H 0.3734 0.1105 -0.0554 0.040 Uiso 1 1 calc R B 1 C42 C 0.3183(3) 0.0993(5) 0.0321(5) 0.034(2) Uani 1 1 d . B 1 H42 H 0.3193 0.0440 0.0342 0.041 Uiso 1 1 calc R B 1 C43 C 0.2849(4) 0.1396(6) 0.0817(5) 0.024(2) Uani 1 1 d . B 1 C44 C 0.2865(4) 0.2216(5) 0.0772(5) 0.0276(19) Uani 1 1 d . B 1 H44 H 0.2649 0.2506 0.1122 0.033 Uiso 1 1 calc R B 1 C45 C 0.2101(4) 0.1220(6) 0.1751(6) 0.028(2) Uani 1 1 d . B 1 C46 C 0.1364(3) 0.0711(5) 0.2570(5) 0.029(2) Uani 1 1 d . B 1 C47 C 0.1181(3) 0.1431(5) 0.2861(5) 0.0278(19) Uani 1 1 d . B 1 H47 H 0.1341 0.1909 0.2706 0.033 Uiso 1 1 calc R B 1 C48 C 0.0748(4) 0.1409(5) 0.3394(5) 0.033(2) Uani 1 1 d . B 1 H48 H 0.0617 0.1882 0.3608 0.040 Uiso 1 1 calc R B 1 C49 C 0.0514(3) 0.0716(5) 0.3608(5) 0.0296(19) Uani 1 1 d . B 1 C50 C 0.0688(3) 0.0024(6) 0.3321(5) 0.034(2) Uani 1 1 d . B 1 H50 H 0.0520 -0.0450 0.3472 0.041 Uiso 1 1 calc R B 1 C51 C 0.1128(3) 0.0022(6) 0.2790(5) 0.032(2) Uani 1 1 d . B 1 H51 H 0.1258 -0.0457 0.2588 0.039 Uiso 1 1 calc R B 1 C52 C 0.0000 0.0709(8) 0.4129(8) 0.039(3) Uani 1 2 d S . 1 H52A H 0.0000 0.0238 0.4457 0.046 Uiso 1 2 calc SR . 1 H52B H 0.0000 0.1173 0.4468 0.046 Uiso 1 2 calc SR . 1 O1S O 0.2989(2) 0.1642(3) 0.3804(4) 0.0356(15) Uani 1 1 d . . . C1S C 0.3303(5) 0.1233(7) 0.4342(7) 0.065(4) Uani 1 1 d . . . H1S1 H 0.3065 0.0931 0.4690 0.078 Uiso 1 1 calc R . . H1S2 H 0.3517 0.1602 0.4655 0.078 Uiso 1 1 calc R . . O2S O 0.2029(3) 0.3868(4) 0.0647(4) 0.0455(18) Uani 1 1 d . . . C2S C 0.3657(5) 0.0716(7) 0.3935(6) 0.061(3) Uani 1 1 d . . . H2S1 H 0.3473 0.0227 0.3787 0.073 Uiso 1 1 calc R . . H2S2 H 0.3985 0.0593 0.4237 0.073 Uiso 1 1 calc R . . O3S O 0.5000 0.6060(18) -0.236(2) 0.243(15) Uani 1 2 d S . . C3S C 0.3795(5) 0.1255(8) 0.3190(9) 0.083(4) Uani 1 1 d . . . H3S1 H 0.4088 0.1631 0.3302 0.100 Uiso 1 1 calc R . . H3S2 H 0.3896 0.0935 0.2739 0.100 Uiso 1 1 calc R . . O4S O 0.5000 0.3513(16) -0.2291(10) 0.183(12) Uani 1 2 d S . . C4S C 0.3266(4) 0.1659(6) 0.3068(6) 0.047(3) Uani 1 1 d . . . H4S1 H 0.3325 0.2203 0.2899 0.056 Uiso 1 1 calc R . . H4S2 H 0.3050 0.1386 0.2672 0.056 Uiso 1 1 calc R . . O5S O 0.5000 0.0978(15) -0.2480(10) 0.161(9) Uani 1 2 d S . . C5S C 0.1748(5) 0.3808(5) 0.1381(6) 0.045(3) Uani 1 1 d . . . H5S1 H 0.1681 0.4333 0.1597 0.055 Uiso 1 1 calc R . . H5S2 H 0.1968 0.3507 0.1753 0.055 Uiso 1 1 calc R . . C6S C 0.1223(4) 0.3400(5) 0.1227(6) 0.042(2) Uani 1 1 d . . . H6S1 H 0.1155 0.2989 0.1615 0.050 Uiso 1 1 calc R . . H6S2 H 0.0917 0.3772 0.1230 0.050 Uiso 1 1 calc R . . C18S C -0.0285(3) -0.1165(6) 0.5308(5) 0.043(3) Uani 1 1 d . . . H18A H -0.0422 -0.0713 0.5012 0.052 Uiso 1 1 calc R . . H18B H -0.0422 -0.1646 0.5061 0.052 Uiso 1 1 calc R . . C7S C 0.1300(5) 0.3061(9) 0.0460(6) 0.077(4) Uani 1 1 d . . . H7S1 H 0.1458 0.2533 0.0501 0.093 Uiso 1 1 calc R . . H7S2 H 0.0950 0.3023 0.0187 0.093 Uiso 1 1 calc R . . O8S O 0.0000 0.2223(7) 0.5519(6) 0.085(4) Uani 1 2 d S . . C8S C 0.1656(4) 0.3562(7) 0.0059(7) 0.062(3) Uani 1 1 d . . . H8S1 H 0.1453 0.3992 -0.0188 0.074 Uiso 1 1 calc R . . H8S2 H 0.1857 0.3272 -0.0342 0.074 Uiso 1 1 calc R . . O9S O 0.0000 0.3502(10) 0.2529(7) 0.110(6) Uani 1 2 d S . . C9S C 0.4551(6) 0.6167(12) -0.1751(9) 0.126(8) Uani 1 1 d . . . H9S1 H 0.4229 0.6403 -0.1996 0.151 Uiso 1 1 calc R . . H9S2 H 0.4445 0.5651 -0.1545 0.151 Uiso 1 1 calc R . . O10S O 0.0000 0.5911(16) 0.1603(10) 0.180(11) Uani 1 2 d S . . C10S C 0.4743(5) 0.6683(8) -0.1099(7) 0.070(4) Uani 1 1 d . . . H10A H 0.4606 0.7219 -0.1170 0.084 Uiso 1 1 calc R . . H10B H 0.4606 0.6482 -0.0602 0.084 Uiso 1 1 calc R . . C11S C 0.4546(5) 0.3479(9) -0.1754(9) 0.092(5) Uani 1 1 d . . . H11A H 0.4425 0.4012 -0.1622 0.111 Uiso 1 1 calc R . . H11B H 0.4239 0.3198 -0.1991 0.111 Uiso 1 1 calc R . . C12S C 0.4726(4) 0.3070(7) -0.1060(5) 0.067(3) Uani 1 1 d . . . H12A H 0.4588 0.3338 -0.0595 0.080 Uiso 1 1 calc R . . H12B H 0.4588 0.2529 -0.1059 0.080 Uiso 1 1 calc R . . C13S C 0.5481(5) 0.0937(9) -0.1864(7) 0.077(4) Uani 1 1 d . . . H13C H 0.5763 0.0573 -0.2048 0.092 Uiso 1 1 calc R . . H13D H 0.5647 0.1458 -0.1807 0.092 Uiso 1 1 calc R . . C14S C 0.5284(5) 0.0682(8) -0.1142(5) 0.091(5) Uani 1 1 d . . . H14A H 0.5418 0.1032 -0.0732 0.110 Uiso 1 1 calc R . . H14B H 0.5418 0.0150 -0.1036 0.110 Uiso 1 1 calc R . . C15S C 0.5479(6) 0.1684(10) 0.1379(8) 0.092(5) Uani 1 1 d . . . H15A H 0.5652 0.2194 0.1479 0.111 Uiso 1 1 calc R . . H15B H 0.5756 0.1270 0.1432 0.111 Uiso 1 1 calc R . . C16S C 0.5245(6) 0.1669(14) 0.0622(8) 0.159(10) Uani 1 1 d . . . H16A H 0.5374 0.2129 0.0331 0.191 Uiso 1 1 calc R . . H16B H 0.5374 0.1197 0.0350 0.191 Uiso 1 1 calc R . . C17S C -0.0457(6) -0.1127(15) 0.6019(9) 0.173(11) Uani 1 1 d . . . H17A H -0.0669 -0.1600 0.6141 0.208 Uiso 1 1 calc R . . H17B H -0.0699 -0.0670 0.6077 0.208 Uiso 1 1 calc R . . O7S O 0.0000 -0.1058(13) 0.6565(6) 0.152(9) Uani 1 2 d S . . C19S C -0.0460(6) 0.1882(11) 0.5873(10) 0.114(6) Uani 1 1 d . . . H19A H -0.0710 0.1675 0.5478 0.136 Uiso 1 1 calc R . . H19B H -0.0655 0.2273 0.6186 0.136 Uiso 1 1 calc R . . C20S C -0.0262(9) 0.1255(11) 0.6358(15) 0.25(2) Uani 1 1 d . . . H20A H -0.0397 0.1325 0.6890 0.296 Uiso 1 1 calc R . . H20B H -0.0397 0.0749 0.6164 0.296 Uiso 1 1 calc R . . C21S C -0.0495(5) 0.3773(7) 0.3030(7) 0.062(3) Uani 1 1 d . . . H21A H -0.0701 0.4187 0.2764 0.074 Uiso 1 1 calc R . . H21B H -0.0741 0.3331 0.3137 0.074 Uiso 1 1 calc R . . C22S C -0.0264(4) 0.4060(9) 0.3721(7) 0.101(6) Uani 1 1 d . . . H22A H -0.0394 0.4598 0.3807 0.121 Uiso 1 1 calc R . . H22B H -0.0394 0.3737 0.4155 0.121 Uiso 1 1 calc R . . C23S C -0.0457(7) 0.5754(10) 0.1098(9) 0.115(6) Uani 1 1 d . . . H23A H -0.0776 0.5591 0.1403 0.138 Uiso 1 1 calc R . . H23B H -0.0554 0.6227 0.0803 0.138 Uiso 1 1 calc R . . C24S C -0.0305(6) 0.5173(7) 0.0612(6) 0.097(6) Uani 1 1 d . . . H24A H -0.0445 0.5271 0.0087 0.116 Uiso 1 1 calc R . . H24B H -0.0445 0.4665 0.0793 0.116 Uiso 1 1 calc R . . Ag2A Ag 0.3043(2) 0.2932(4) 0.0117(4) 0.0207(12) Uiso 0.10 1 d P C 2 N1 N 0.1954(2) 0.0298(4) 0.4259(5) 0.0255(15) Uiso 1 1 d . A 1 Ag1A Ag 0.1939(3) 0.0681(4) 0.4154(5) 0.0293(15) Uiso 0.10 1 d P D 2 N10 N 0.3157(3) 0.2598(5) 0.0278(4) 0.0278(17) Uiso 1 1 d . B 1 O6S O 0.5000 0.1542(17) 0.195(2) 0.259(17) Uani 1 2 d S . . 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 0.0313(3) 0.0225(3) 0.0341(3) 0.0022(3) 0.0048(4) 0.0011(3) O1 0.038(3) 0.016(3) 0.040(3) 0.006(3) 0.013(3) 0.005(2) C1 0.026(4) 0.034(5) 0.035(5) -0.003(4) 0.006(4) 0.006(4) Ag2 0.0357(4) 0.0219(4) 0.0405(4) 0.0011(3) 0.0065(4) 0.0026(3) O2 0.028(3) 0.023(4) 0.039(4) -0.003(3) 0.006(3) 0.004(3) N2 0.042(4) 0.019(4) 0.027(4) 0.006(3) 0.006(3) 0.001(3) C2 0.028(5) 0.016(5) 0.042(5) 0.007(4) 0.010(4) -0.004(4) O3 0.058(4) 0.020(4) 0.058(5) 0.016(3) 0.018(3) 0.007(3) N3 0.029(4) 0.016(4) 0.033(4) 0.008(3) 0.008(3) 0.000(3) C3 0.024(4) 0.027(4) 0.035(4) 0.002(4) -0.007(4) 0.003(3) O4 0.045(4) 0.019(4) 0.094(6) 0.011(4) 0.031(4) 0.007(3) N4 0.036(4) 0.012(3) 0.034(4) 0.006(3) 0.000(3) 0.007(3) C4 0.031(5) 0.017(5) 0.022(4) -0.007(4) -0.003(4) 0.005(4) O5 0.075(5) 0.040(4) 0.045(4) 0.010(3) 0.007(4) 0.016(4) N5 0.030(4) 0.017(4) 0.041(4) -0.004(3) 0.017(3) 0.001(3) C5 0.034(5) 0.017(4) 0.026(4) 0.010(3) -0.001(3) -0.003(3) O6 0.080(5) 0.028(4) 0.050(4) 0.004(3) 0.011(4) 0.014(3) N6 0.027(4) 0.020(4) 0.044(4) -0.002(3) 0.015(3) 0.006(3) C6 0.014(4) 0.037(6) 0.034(5) 0.011(5) -0.003(4) 0.003(4) O7 0.053(4) 0.039(4) 0.045(4) 0.007(3) 0.018(3) 0.008(3) N7 0.040(4) 0.010(3) 0.039(4) 0.007(3) -0.001(3) 0.002(3) C7 0.029(5) 0.027(5) 0.032(5) 0.006(4) 0.004(4) 0.001(4) O8 0.128(7) 0.026(4) 0.022(3) -0.001(3) -0.007(4) 0.006(4) N8 0.037(4) 0.020(4) 0.036(4) -0.001(3) 0.008(4) 0.009(3) C8 0.038(5) 0.025(5) 0.038(5) 0.004(4) 0.006(4) 0.005(4) O9 0.040(4) 0.128(9) 0.041(4) -0.002(5) 0.016(4) -0.006(4) N9 0.036(4) 0.022(4) 0.045(4) -0.001(4) 0.000(3) 0.005(3) C9 0.025(4) 0.028(5) 0.032(4) 0.000(4) 0.001(4) -0.001(4) O10 0.100(6) 0.028(3) 0.036(3) 0.007(3) 0.012(4) -0.023(4) C10 0.025(4) 0.031(5) 0.026(4) -0.005(4) -0.007(4) 0.000(4) N11 0.041(4) 0.013(3) 0.041(4) 0.005(3) -0.001(3) 0.009(3) C11 0.028(5) 0.040(6) 0.042(5) 0.001(4) -0.008(4) -0.005(4) N12 0.030(4) 0.021(4) 0.037(4) -0.003(3) 0.002(3) -0.003(3) C12 0.021(4) 0.032(5) 0.030(4) -0.002(4) 0.000(3) -0.001(4) N13 0.029(4) 0.022(4) 0.032(4) -0.003(3) 0.001(4) -0.005(3) C13 0.035(6) 0.021(6) 0.039(6) 0.002(6) 0.000 0.000 N14 0.046(5) 0.023(5) 0.022(4) 0.010(3) 0.003(4) 0.006(3) C14 0.018(4) 0.034(5) 0.032(5) 0.002(4) 0.008(4) 0.005(4) C15 0.025(4) 0.034(5) 0.031(4) -0.006(4) 0.013(4) 0.006(4) C16 0.033(5) 0.022(5) 0.039(6) 0.002(4) 0.006(4) 0.001(3) C17 0.015(4) 0.022(4) 0.034(5) -0.003(4) -0.003(4) 0.003(4) C18 0.016(4) 0.027(5) 0.023(4) -0.001(4) -0.007(4) 0.002(4) C19 0.031(5) 0.020(5) 0.019(4) -0.003(4) -0.007(3) 0.005(4) C20 0.020(4) 0.024(4) 0.027(4) -0.001(4) -0.006(3) 0.002(3) C21 0.020(4) 0.020(5) 0.038(5) -0.004(4) 0.002(4) 0.005(3) C22 0.026(4) 0.025(4) 0.036(5) 0.009(4) 0.001(4) -0.004(3) C23 0.022(4) 0.028(5) 0.031(4) 0.001(4) -0.002(4) 0.000(3) C24 0.028(5) 0.031(5) 0.027(4) -0.001(4) 0.003(4) 0.004(4) C25 0.039(5) 0.027(5) 0.029(5) 0.002(4) -0.003(4) -0.003(4) C26 0.037(6) 0.037(7) 0.028(6) 0.005(6) 0.000 0.000 C27 0.028(5) 0.030(5) 0.030(5) -0.006(4) 0.001(4) -0.003(4) C28 0.034(5) 0.038(6) 0.035(5) 0.006(4) 0.005(4) 0.001(4) C29 0.035(5) 0.020(4) 0.033(5) 0.001(4) 0.007(4) -0.005(3) C30 0.026(4) 0.020(5) 0.035(5) 0.009(4) -0.008(4) 0.002(4) C31 0.009(4) 0.023(5) 0.040(5) 0.001(4) 0.006(4) 0.003(3) C32 0.036(5) 0.022(5) 0.039(5) 0.005(4) 0.005(4) 0.010(4) C33 0.022(4) 0.026(5) 0.040(5) -0.006(4) -0.008(4) 0.005(4) C34 0.042(5) 0.025(5) 0.050(6) -0.007(4) 0.004(4) 0.000(4) C35 0.045(5) 0.024(5) 0.036(5) -0.011(4) 0.008(4) 0.007(4) C36 0.034(5) 0.043(6) 0.030(5) 0.002(4) -0.012(4) -0.011(4) C37 0.034(5) 0.026(5) 0.042(5) 0.003(4) -0.007(4) 0.002(4) C38 0.020(5) 0.028(5) 0.040(5) 0.001(4) 0.000(4) -0.003(4) C39 0.031(6) 0.059(9) 0.032(6) -0.020(8) 0.000 0.000 C40 0.038(5) 0.022(5) 0.038(5) 0.002(4) 0.006(4) -0.005(4) C41 0.036(5) 0.021(5) 0.043(6) 0.001(5) 0.005(5) 0.005(5) C42 0.025(4) 0.031(5) 0.045(6) -0.009(4) -0.012(4) 0.001(3) C43 0.028(5) 0.021(5) 0.024(5) -0.003(4) 0.006(4) -0.001(4) C44 0.038(5) 0.014(4) 0.030(4) -0.002(4) 0.007(4) 0.002(4) C45 0.021(4) 0.028(6) 0.035(5) 0.004(4) 0.006(4) 0.007(4) C46 0.028(5) 0.024(5) 0.036(5) 0.005(4) -0.013(4) 0.003(4) C47 0.019(4) 0.030(5) 0.034(5) 0.008(4) -0.006(4) 0.003(4) C48 0.037(5) 0.037(5) 0.026(4) 0.001(4) -0.009(4) 0.001(4) C49 0.032(5) 0.036(5) 0.021(4) 0.005(4) -0.010(3) 0.003(4) C50 0.024(4) 0.033(5) 0.045(5) 0.007(4) -0.014(4) 0.009(4) C51 0.026(4) 0.031(5) 0.040(5) 0.008(4) -0.013(4) -0.007(4) C52 0.052(7) 0.033(7) 0.031(7) -0.004(6) 0.000 0.000 O1S 0.025(3) 0.032(4) 0.050(4) 0.000(3) 0.000(3) 0.004(2) C1S 0.051(6) 0.085(9) 0.059(7) -0.020(6) -0.027(6) 0.038(6) O2S 0.046(4) 0.039(4) 0.051(4) -0.003(3) 0.004(3) -0.006(3) C2S 0.083(8) 0.050(7) 0.049(6) 0.000(5) -0.013(5) 0.018(6) O3S 0.15(2) 0.27(4) 0.31(4) -0.04(3) 0.000 0.000 C3S 0.036(7) 0.107(12) 0.107(12) 0.010(9) 0.011(7) -0.005(6) O4S 0.090(12) 0.40(4) 0.062(9) 0.046(14) 0.000 0.000 C4S 0.048(6) 0.047(7) 0.045(6) 0.005(5) 0.008(5) 0.004(5) O5S 0.093(12) 0.31(3) 0.077(11) -0.010(14) 0.000 0.000 C5S 0.067(7) 0.021(5) 0.048(6) -0.012(4) -0.008(5) 0.005(4) C6S 0.026(5) 0.053(7) 0.047(6) 0.006(5) 0.009(4) 0.005(4) C18S 0.025(4) 0.089(8) 0.015(4) -0.001(4) -0.008(3) 0.000(4) C7S 0.068(8) 0.124(12) 0.040(6) 0.005(7) -0.006(5) -0.049(8) O8S 0.148(12) 0.067(9) 0.041(6) 0.018(6) 0.000 0.000 C8S 0.032(6) 0.098(9) 0.056(7) 0.012(7) 0.007(5) 0.007(5) O9S 0.051(7) 0.237(19) 0.043(6) -0.012(8) 0.000 0.000 C9S 0.040(8) 0.28(2) 0.053(9) -0.052(11) -0.014(7) 0.018(10) O10S 0.096(13) 0.37(3) 0.073(10) -0.100(15) 0.000 0.000 C10S 0.057(7) 0.103(11) 0.050(7) -0.030(6) -0.006(5) 0.006(6) C11S 0.053(7) 0.130(14) 0.094(10) 0.056(9) -0.004(7) -0.024(8) C12S 0.082(7) 0.089(9) 0.029(5) 0.017(5) -0.010(4) -0.046(7) C13S 0.058(7) 0.121(12) 0.051(7) -0.003(7) -0.021(6) 0.009(7) C14S 0.143(12) 0.116(11) 0.016(4) 0.001(5) 0.001(5) 0.082(9) C15S 0.059(9) 0.149(16) 0.069(9) -0.005(9) 0.024(7) 0.011(8) C16S 0.079(11) 0.35(3) 0.048(9) 0.011(12) 0.013(7) 0.001(12) C17S 0.033(8) 0.44(4) 0.046(9) 0.000(13) -0.021(7) -0.022(12) O7S 0.028(6) 0.40(3) 0.026(5) -0.018(10) 0.000 0.000 C19S 0.093(11) 0.120(15) 0.128(14) 0.009(12) 0.048(11) 0.028(10) C20S 0.28(4) 0.136(17) 0.33(3) 0.14(2) 0.26(3) 0.110(18) C21S 0.055(7) 0.074(9) 0.056(7) -0.018(6) -0.009(6) -0.014(6) C22S 0.058(7) 0.175(15) 0.069(8) -0.088(9) 0.023(6) -0.063(8) C23S 0.114(12) 0.128(14) 0.103(12) -0.055(11) -0.054(10) 0.037(10) C24S 0.215(17) 0.051(7) 0.025(5) -0.006(5) 0.014(6) -0.064(8) O6S 0.110(19) 0.29(4) 0.38(5) 0.04(3) 0.000 0.000 _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(6) . ? Ag1 N1 2.205(8) . ? O1 C6 1.248(11) . ? C1 N1 1.287(11) . ? C1 C2 1.406(12) . ? C1 H1 0.9500 . ? Ag2 N10 2.169(8) . ? Ag2 N7 2.175(6) . ? O2 C19 1.242(11) . ? N2 C6 1.382(11) . ? N2 C4 1.425(11) . ? N2 H2N 0.8800 . ? C2 C3 1.355(13) . ? C2 H2 0.9500 . ? O3 C32 1.218(11) . ? N3 C6 1.329(12) . ? N3 C7 1.377(11) . ? N3 H3N 0.8800 . ? C3 C4 1.363(13) . ? C3 H3 0.9500 . ? O4 C45 1.242(12) . ? N4 C14 1.316(11) . ? N4 C18 1.324(11) . ? C4 C5 1.441(11) . ? O5 N13 1.266(9) . ? N5 C17 1.395(11) . ? N5 C19 1.407(11) . ? N5 H5N 0.8800 . ? C5 N1 1.341(11) . ? C5 H5 0.9500 . ? O6 N13 1.225(9) . ? N6 C19 1.349(11) . ? N6 C20 1.396(10) . ? N6 H6N 0.8800 . ? O7 N13 1.261(10) . ? N7 C27 1.312(11) . ? N7 C31 1.335(11) . ? C7 C8 1.394(12) . ? C7 C12 1.391(12) . ? O8 N14 1.161(9) . ? N8 C30 1.368(11) . ? N8 C32 1.391(12) . ? N8 H8N 0.8800 . ? C8 C9 1.342(12) . ? C8 H8 0.9500 . ? O9 N14 1.223(11) . ? N9 C32 1.394(11) . ? N9 C33 1.466(11) . ? N9 H9N 0.8800 . ? C9 C10 1.411(12) . ? C9 H9 0.9500 . ? O10 N14 1.256(9) . ? C10 C11 1.403(13) . ? C10 C13 1.500(12) . ? N11 C43 1.371(11) . ? N11 C45 1.376(12) . ? N11 H11N 0.8800 . ? C11 C12 1.400(12) . ? C11 H11 0.9500 . ? N12 C45 1.305(12) . ? N12 C46 1.451(11) . ? N12 H12N 0.8800 . ? C12 H12 0.9500 . ? C13 C10 1.500(12) 3_655 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.346(11) . ? C14 H14 0.9500 . ? C15 C16 1.365(12) . ? C15 H15 0.9500 . ? C16 C17 1.379(12) . ? C16 H16 0.9500 . ? C17 C18 1.405(11) . ? C18 H18 0.9500 . ? C20 C25 1.377(12) . ? C20 C21 1.400(11) . ? C21 C22 1.346(11) . ? C21 H21 0.9500 . ? C22 C23 1.440(11) . ? C22 H22 0.9500 . ? C23 C24 1.355(12) . ? C23 C26 1.525(11) . ? C24 C25 1.379(12) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C23 1.525(11) 3_655 ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.367(12) . ? C27 H27 0.9500 . ? C28 C29 1.384(13) . ? C28 H28 0.9500 . ? C29 C30 1.416(12) . ? C29 H29 0.9500 . ? C30 C31 1.386(11) . ? C31 H31 0.9500 . ? C33 C34 1.362(12) . ? C33 C38 1.381(13) . ? C34 C35 1.389(12) . ? C34 H34 0.9500 . ? C35 C36 1.356(12) . ? C35 H35 0.9500 . ? C36 C37 1.330(13) . ? C36 C39 1.542(13) . ? C37 C38 1.447(13) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C36 1.542(13) 3 ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N10 1.364(11) . ? C40 C41 1.411(12) . ? C40 H40 0.9500 . ? C41 C42 1.392(13) . ? C41 H41 0.9500 . ? C42 C43 1.380(13) . ? C42 H42 0.9500 . ? C43 C44 1.411(11) . ? C44 N10 1.300(11) . ? C44 H44 0.9500 . ? C46 C51 1.374(12) . ? C46 C47 1.411(12) . ? C47 C48 1.416(12) . ? C47 H47 0.9500 . ? C48 C49 1.374(12) . ? C48 H48 0.9500 . ? C49 C50 1.358(12) . ? C49 C52 1.562(11) . ? C50 C51 1.427(12) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C49 1.562(11) 3 ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? O1S C1S 1.404(12) . ? O1S C4S 1.451(12) . ? C1S C2S 1.433(14) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? O2S C5S 1.455(13) . ? O2S C8S 1.474(14) . ? C2S C3S 1.628(17) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? O3S C9S 1.54(3) 3_655 ? O3S C9S 1.54(3) . ? C3S C4S 1.495(16) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? O4S C11S 1.460(17) 3_655 ? O4S C11S 1.460(17) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? O5S C13S 1.602(15) . ? O5S C13S 1.602(15) 3_655 ? C5S C6S 1.500(14) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S C7S 1.467(15) . ? C6S H6S1 0.9900 . ? C6S H6S2 0.9900 . ? C18S C17S 1.309(18) . ? C18S C18S 1.411(17) 3 ? C18S H18A 0.9900 . ? C18S H18B 0.9900 . ? C7S C8S 1.413(15) . ? C7S H7S1 0.9900 . ? C7S H7S2 0.9900 . ? O8S C19S 1.420(16) . ? O8S C19S 1.420(16) 3 ? C8S H8S1 0.9900 . ? C8S H8S2 0.9900 . ? O9S C21S 1.572(14) 3 ? O9S C21S 1.572(14) . ? C9S C10S 1.515(17) . ? C9S H9S1 0.9900 . ? C9S H9S2 0.9900 . ? O10S C23S 1.457(16) . ? O10S C23S 1.457(16) 3 ? C10S C10S 1.27(2) 3_655 ? C10S H10A 0.9900 . ? C10S H10B 0.9900 . ? C11S C12S 1.466(16) . ? C11S H11A 0.9900 . ? C11S H11B 0.9900 . ? C12S C12S 1.35(2) 3_655 ? C12S H12A 0.9900 . ? C12S H12B 0.9900 . ? C13S C14S 1.415(16) . ? C13S H13C 0.9900 . ? C13S H13D 0.9900 . ? C14S C14S 1.40(2) 3_655 ? C14S H14A 0.9900 . ? C14S H14B 0.9900 . ? C15S C16S 1.44(2) . ? C15S O6S 1.57(3) . ? C15S H15A 0.9900 . ? C15S H15B 0.9900 . ? C16S C16S 1.21(3) 3_655 ? C16S H16A 0.9900 . ? C16S H16B 0.9900 . ? C17S O7S 1.481(14) . ? C17S H17A 0.9900 . ? C17S H17B 0.9900 . ? O7S C17S 1.481(14) 3 ? C19S C20S 1.45(2) . ? C19S H19A 0.9900 . ? C19S H19B 0.9900 . ? C20S C20S 1.30(5) 3 ? C20S H20A 0.9900 . ? C20S H20B 0.9900 . ? C21S C22S 1.417(14) . ? C21S H21A 0.9900 . ? C21S H21B 0.9900 . ? C22S C22S 1.31(2) 3 ? C22S H22A 0.9900 . ? C22S H22B 0.9900 . ? C23S C24S 1.360(18) . ? C23S H23A 0.9900 . ? C23S H23B 0.9900 . ? C24S C24S 1.51(3) 3 ? C24S H24A 0.9900 . ? C24S H24B 0.9900 . ? O6S C15S 1.57(3) 3_655 ? 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 173.6(2) . . ? N1 C1 C2 122.0(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? N10 Ag2 N7 174.2(3) . . ? C6 N2 C4 129.9(7) . . ? C6 N2 H2N 115.0 . . ? C4 N2 H2N 115.0 . . ? C3 C2 C1 118.9(8) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C6 N3 C7 128.0(8) . . ? C6 N3 H3N 116.0 . . ? C7 N3 H3N 116.0 . . ? C2 C3 C4 119.9(8) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C14 N4 C18 119.1(7) . . ? C14 N4 Ag1 122.9(6) . . ? C18 N4 Ag1 117.5(6) . . ? C3 C4 N2 120.2(8) . . ? C3 C4 C5 118.8(7) . . ? N2 C4 C5 121.0(7) . . ? C17 N5 C19 126.7(7) . . ? C17 N5 H5N 116.7 . . ? C19 N5 H5N 116.7 . . ? N1 C5 C4 118.9(7) . . ? N1 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C19 N6 C20 128.2(7) . . ? C19 N6 H6N 115.9 . . ? C20 N6 H6N 115.9 . . ? O1 C6 N3 125.5(8) . . ? O1 C6 N2 121.3(8) . . ? N3 C6 N2 113.1(8) . . ? C27 N7 C31 122.6(7) . . ? C27 N7 Ag2 120.5(6) . . ? C31 N7 Ag2 116.8(6) . . ? N3 C7 C8 126.8(9) . . ? N3 C7 C12 117.9(8) . . ? C8 C7 C12 115.2(9) . . ? C30 N8 C32 126.4(7) . . ? C30 N8 H8N 116.8 . . ? C32 N8 H8N 116.8 . . ? C9 C8 C7 122.9(9) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C32 N9 C33 125.9(8) . . ? C32 N9 H9N 117.0 . . ? C33 N9 H9N 117.0 . . ? C8 C9 C10 122.8(8) . . ? C8 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C11 C10 C9 115.9(9) . . ? C11 C10 C13 120.5(9) . . ? C9 C10 C13 123.5(9) . . ? C43 N11 C45 129.2(7) . . ? C43 N11 H11N 115.4 . . ? C45 N11 H11N 115.4 . . ? C12 C11 C10 119.9(9) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C45 N12 C46 127.3(8) . . ? C45 N12 H12N 116.4 . . ? C46 N12 H12N 116.4 . . ? C7 C12 C11 123.3(9) . . ? C7 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? O6 N13 O7 119.4(7) . . ? O6 N13 O5 123.1(8) . . ? O7 N13 O5 117.4(7) . . ? C10 C13 C10 110.0(11) 3_655 . ? C10 C13 H13A 109.7 3_655 . ? C10 C13 H13A 109.7 . . ? C10 C13 H13B 109.7 3_655 . ? C10 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O8 N14 O9 121.3(9) . . ? O8 N14 O10 117.9(9) . . ? O9 N14 O10 120.5(8) . . ? N4 C14 C15 123.1(8) . . ? N4 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C14 C15 C16 118.9(7) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C15 C16 C17 120.3(8) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 116.5(7) . . ? C16 C17 N5 118.2(8) . . ? C18 C17 N5 125.3(7) . . ? N4 C18 C17 122.1(8) . . ? N4 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? O2 C19 N6 125.0(8) . . ? O2 C19 N5 122.6(8) . . ? N6 C19 N5 112.4(7) . . ? C25 C20 N6 124.8(8) . . ? C25 C20 C21 119.1(8) . . ? N6 C20 C21 116.1(7) . . ? C22 C21 C20 120.7(8) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.8(8) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 116.9(8) . . ? C24 C23 C26 121.9(9) . . ? C22 C23 C26 121.1(8) . . ? C23 C24 C25 122.8(9) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C20 C25 C24 119.7(9) . . ? C20 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C23 C26 C23 107.2(10) 3_655 . ? C23 C26 H26A 110.3 3_655 . ? C23 C26 H26A 110.3 . . ? C23 C26 H26B 110.3 3_655 . ? C23 C26 H26B 110.3 . . ? H26A C26 H26B 108.5 . . ? N7 C27 C28 119.8(8) . . ? N7 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 121.2(8) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C30 117.4(8) . . ? C28 C29 H29 121.3 . . ? C30 C29 H29 121.3 . . ? N8 C30 C31 125.2(7) . . ? N8 C30 C29 116.3(8) . . ? C31 C30 C29 118.4(7) . . ? N7 C31 C30 120.5(7) . . ? N7 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? O3 C32 N8 123.6(8) . . ? O3 C32 N9 125.8(9) . . ? N8 C32 N9 110.6(8) . . ? C34 C33 C38 124.3(10) . . ? C34 C33 N9 115.2(8) . . ? C38 C33 N9 120.5(9) . . ? C33 C34 C35 118.1(9) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 120.8(9) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 120.1(10) . . ? C37 C36 C39 119.3(10) . . ? C35 C36 C39 120.2(10) . . ? C36 C37 C38 123.1(9) . . ? C36 C37 H37 118.5 . . ? C38 C37 H37 118.5 . . ? C33 C38 C37 113.4(9) . . ? C33 C38 H38 123.3 . . ? C37 C38 H38 123.3 . . ? C36 C39 C36 112.4(12) 3 . ? C36 C39 H39A 109.1 3 . ? C36 C39 H39A 109.1 . . ? C36 C39 H39B 109.1 3 . ? C36 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? N10 C40 C41 120.7(8) . . ? N10 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 117.8(8) . . ? C42 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? C43 C42 C41 121.1(9) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? N11 C43 C42 118.2(9) . . ? N11 C43 C44 125.1(8) . . ? C42 C43 C44 116.7(8) . . ? N10 C44 C43 123.7(7) . . ? N10 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? O4 C45 N12 125.8(9) . . ? O4 C45 N11 120.5(8) . . ? N12 C45 N11 113.7(8) . . ? C51 C46 C47 121.2(9) . . ? C51 C46 N12 116.3(8) . . ? C47 C46 N12 122.5(8) . . ? C46 C47 C48 117.0(9) . . ? C46 C47 H47 121.5 . . ? C48 C47 H47 121.5 . . ? C49 C48 C47 121.2(9) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C50 C49 C48 121.7(9) . . ? C50 C49 C52 117.7(9) . . ? C48 C49 C52 120.4(9) . . ? C49 C50 C51 118.8(9) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C46 C51 C50 120.2(10) . . ? C46 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C49 C52 C49 109.0(10) 3 . ? C49 C52 H52A 109.9 3 . ? C49 C52 H52A 109.9 . . ? C49 C52 H52B 109.9 3 . ? C49 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C1S O1S C4S 109.7(7) . . ? O1S C1S C2S 108.6(10) . . ? O1S C1S H1S1 110.0 . . ? C2S C1S H1S1 110.0 . . ? O1S C1S H1S2 110.0 . . ? C2S C1S H1S2 110.0 . . ? H1S1 C1S H1S2 108.3 . . ? C5S O2S C8S 106.6(7) . . ? C1S C2S C3S 99.7(10) . . ? C1S C2S H2S1 111.8 . . ? C3S C2S H2S1 111.8 . . ? C1S C2S H2S2 111.8 . . ? C3S C2S H2S2 111.8 . . ? H2S1 C2S H2S2 109.6 . . ? C9S O3S C9S 92(2) 3_655 . ? C4S C3S C2S 101.2(9) . . ? C4S C3S H3S1 111.5 . . ? C2S C3S H3S1 111.5 . . ? C4S C3S H3S2 111.5 . . ? C2S C3S H3S2 111.5 . . ? H3S1 C3S H3S2 109.4 . . ? C11S O4S C11S 100.4(15) 3_655 . ? O1S C4S C3S 106.2(9) . . ? O1S C4S H4S1 110.5 . . ? C3S C4S H4S1 110.5 . . ? O1S C4S H4S2 110.5 . . ? C3S C4S H4S2 110.5 . . ? H4S1 C4S H4S2 108.7 . . ? C13S O5S C13S 95.9(13) . 3_655 ? O2S C5S C6S 106.8(8) . . ? O2S C5S H5S1 110.4 . . ? C6S C5S H5S1 110.4 . . ? O2S C5S H5S2 110.4 . . ? C6S C5S H5S2 110.4 . . ? H5S1 C5S H5S2 108.6 . . ? C7S C6S C5S 103.6(8) . . ? C7S C6S H6S1 111.0 . . ? C5S C6S H6S1 111.0 . . ? C7S C6S H6S2 111.0 . . ? C5S C6S H6S2 111.0 . . ? H6S1 C6S H6S2 109.0 . . ? C17S C18S C18S 108.9(7) . 3 ? C17S C18S H18A 109.9 . . ? C18S C18S H18A 109.9 3 . ? C17S C18S H18B 109.9 . . ? C18S C18S H18B 109.9 3 . ? H18A C18S H18B 108.3 . . ? C8S C7S C6S 106.7(10) . . ? C8S C7S H7S1 110.4 . . ? C6S C7S H7S1 110.4 . . ? C8S C7S H7S2 110.4 . . ? C6S C7S H7S2 110.4 . . ? H7S1 C7S H7S2 108.6 . . ? C19S O8S C19S 106.4(16) . 3 ? C7S C8S O2S 105.3(10) . . ? C7S C8S H8S1 110.7 . . ? O2S C8S H8S1 110.7 . . ? C7S C8S H8S2 110.7 . . ? O2S C8S H8S2 110.7 . . ? H8S1 C8S H8S2 108.8 . . ? C21S O9S C21S 102.1(11) 3 . ? C10S C9S O3S 110.9(15) . . ? C10S C9S H9S1 109.5 . . ? O3S C9S H9S1 109.4 . . ? C10S C9S H9S2 109.5 . . ? O3S C9S H9S2 109.5 . . ? H9S1 C9S H9S2 108.0 . . ? C23S O10S C23S 101.7(16) . 3 ? C10S C10S C9S 108.2(7) 3_655 . ? C10S C10S H10A 110.1 3_655 . ? C9S C10S H10A 110.1 . . ? C10S C10S H10B 110.1 3_655 . ? C9S C10S H10B 110.1 . . ? H10A C10S H10B 108.4 . . ? C12S C11S O4S 108.2(12) . . ? C12S C11S H11A 110.1 . . ? O4S C11S H11A 110.1 . . ? C12S C11S H11B 110.1 . . ? O4S C11S H11B 110.1 . . ? H11A C11S H11B 108.4 . . ? C12S C12S C11S 107.7(6) 3_655 . ? C12S C12S H12A 110.2 3_655 . ? C11S C12S H12A 110.2 . . ? C12S C12S H12B 110.2 3_655 . ? C11S C12S H12B 110.2 . . ? H12A C12S H12B 108.5 . . ? C14S C13S O5S 110.5(11) . . ? C14S C13S H13C 109.5 . . ? O5S C13S H13C 109.5 . . ? C14S C13S H13D 109.5 . . ? O5S C13S H13D 109.5 . . ? H13C C13S H13D 108.1 . . ? C13S C14S C14S 110.1(7) . 3_655 ? C13S C14S H14A 109.6 . . ? C14S C14S H14A 109.6 3_655 . ? C13S C14S H14B 109.6 . . ? C14S C14S H14B 109.6 3_655 . ? H14A C14S H14B 108.1 . . ? C16S C15S O6S 106.1(16) . . ? C16S C15S H15A 110.5 . . ? O6S C15S H15A 110.5 . . ? C16S C15S H15B 110.5 . . ? O6S C15S H15B 110.5 . . ? H15A C15S H15B 108.7 . . ? C16S C16S C15S 113.7(8) 3_655 . ? C16S C16S H16A 108.8 3_655 . ? C15S C16S H16A 108.8 . . ? C16S C16S H16B 108.8 3_655 . ? C15S C16S H16B 108.8 . . ? H16A C16S H16B 107.7 . . ? C18S C17S O7S 111.2(11) . . ? C18S C17S H17A 109.4 . . ? O7S C17S H17A 109.4 . . ? C18S C17S H17B 109.4 . . ? O7S C17S H17B 109.4 . . ? H17A C17S H17B 108.0 . . ? C17S O7S C17S 99.5(14) 3 . ? O8S C19S C20S 106.8(13) . . ? O8S C19S H19A 110.4 . . ? C20S C19S H19A 110.4 . . ? O8S C19S H19B 110.4 . . ? C20S C19S H19B 110.4 . . ? H19A C19S H19B 108.6 . . ? C20S C20S C19S 109.7(11) 3 . ? C20S C20S H20A 109.7 3 . ? C19S C20S H20A 109.7 . . ? C20S C20S H20B 109.7 3 . ? C19S C20S H20B 109.7 . . ? H20A C20S H20B 108.2 . . ? C22S C21S O9S 105.0(9) . . ? C22S C21S H21A 110.7 . . ? O9S C21S H21A 110.7 . . ? C22S C21S H21B 110.7 . . ? O9S C21S H21B 110.7 . . ? H21A C21S H21B 108.8 . . ? C22S C22S C21S 113.7(7) 3 . ? C22S C22S H22A 108.8 3 . ? C21S C22S H22A 108.8 . . ? C22S C22S H22B 108.8 3 . ? C21S C22S H22B 108.8 . . ? H22A C22S H22B 107.7 . . ? C24S C23S O10S 107.2(14) . . ? C24S C23S H23A 110.3 . . ? O10S C23S H23A 110.3 . . ? C24S C23S H23B 110.3 . . ? O10S C23S H23B 110.3 . . ? H23A C23S H23B 108.5 . . ? C23S C24S C24S 106.1(9) . 3 ? C23S C24S H24A 110.5 . . ? C24S C24S H24A 110.5 3 . ? C23S C24S H24B 110.5 . . ? C24S C24S H24B 110.5 3 . ? H24A C24S H24B 108.7 . . ? C1 N1 C5 121.5(8) . . ? C1 N1 Ag1 123.4(6) . . ? C5 N1 Ag1 114.9(6) . . ? C44 N10 C40 120.0(8) . . ? C44 N10 Ag2 120.5(6) . . ? C40 N10 Ag2 119.1(6) . . ? C15S O6S C15S 98(2) 3_655 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O6 0.88 1.95 2.815(9) 167.6 . N3 H3N O7 0.88 2.07 2.924(10) 162.4 . N5 H5N O3 0.88 2.33 3.041(10) 137.5 . N5 H5N O5 0.88 2.36 2.913(10) 120.6 1_565 N6 H6N O5 0.88 2.19 2.977(10) 148.6 1_565 N8 H8N O8 0.88 1.98 2.842(10) 164.6 . N9 H9N O9 0.88 2.33 3.198(13) 167.4 . N9 H9N O8 0.88 2.57 3.312(10) 142.7 . N11 H11N O10 0.88 2.15 2.884(9) 140.8 1_545 N11 H11N O1 0.88 2.54 3.184(9) 130.9 . N12 H12N O9 0.88 2.35 3.196(13) 160.6 1_545 N12 H12N O10 0.88 2.59 3.347(10) 144.1 1_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.229 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.127 # Attachment '- 8.CIF' data_c:\docume~1\dch3gol\desktop\srv350\srv350m _database_code_depnum_ccdc_archive 'CCDC 773259' #TrackingRef '- 8.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H25 Ag N7 O6.50' _chemical_formula_weight 551.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.965(3) _cell_length_b 8.6312(9) _cell_length_c 21.090(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.509(3) _cell_angle_gamma 90.00 _cell_volume 4378.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.507 _cell_measurement_theta_max 30.259 _exptl_crystal_description colourless _exptl_crystal_colour Prism _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8216 _exptl_absorpt_correction_T_max 0.8442 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Smart-6K _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16078 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.99 _reflns_number_total 5275 _reflns_number_gt 3762 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xseed _computing_publication_material Xseed _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. DFIX restraints used on water hydrogen atoms to fix them in a chemically sensible geometry. ; _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^)+(0.0425P)^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 5275 _refine_ls_number_parameters 306 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 0.238557(9) 0.91884(3) 0.329371(12) 0.02817(8) Uani 1 1 d . . . O1 O 0.50313(9) 0.8895(3) 0.58384(11) 0.0371(6) Uani 1 1 d . . . O2 O 0.51646(9) 0.3743(3) 0.60789(11) 0.0320(5) Uani 1 1 d . . . O3 O 0.24335(9) 0.6830(3) 0.25769(11) 0.0326(5) Uani 1 1 d . . . O4 O 0.18399(9) 0.4995(3) 0.22005(11) 0.0334(5) Uani 1 1 d . . . O5 O 0.17101(10) 0.6560(3) 0.29481(12) 0.0369(6) Uani 1 1 d . . . O6 O 0.5000 0.8197(4) 0.7500 0.0557(11) Uani 1 2 d SD . . O7 O 0.56524(14) 0.9898(7) 0.69642(16) 0.1130(18) Uani 1 1 d D . . N1 N 0.30299(10) 0.8834(3) 0.42828(12) 0.0228(5) Uani 1 1 d . . . N2 N 0.45073(10) 0.8033(3) 0.48429(12) 0.0265(6) Uani 1 1 d . . . H2N H 0.4529 0.7655 0.4463 0.032 Uiso 1 1 calc R . . N3 N 0.54319(10) 0.7472(3) 0.51734(12) 0.0278(6) Uani 1 1 d . . . H3N H 0.5373 0.7085 0.4775 0.033 Uiso 1 1 calc R . . N4 N 0.56313(10) 0.5958(3) 0.64499(12) 0.0252(5) Uani 1 1 d . . . H4N H 0.5676 0.6704 0.6744 0.030 Uiso 1 1 calc R . . N5 N 0.48151(10) 0.5410(3) 0.67034(12) 0.0254(6) Uani 1 1 d . . . H5N H 0.4853 0.6326 0.6894 0.030 Uiso 1 1 calc R . . N6 N 0.34143(10) 0.4531(3) 0.68155(12) 0.0262(6) Uani 1 1 d . . . N7 N 0.19947(11) 0.6136(3) 0.25741(12) 0.0263(6) Uani 1 1 d . . . C1 C 0.35627(12) 0.8544(3) 0.43112(14) 0.0219(6) Uani 1 1 d . . . H1 H 0.3660 0.8418 0.3909 0.026 Uiso 1 1 calc R . . C2 C 0.39800(12) 0.8417(3) 0.48933(15) 0.0221(6) Uani 1 1 d . . . C3 C 0.38331(13) 0.8609(4) 0.54838(15) 0.0274(7) Uani 1 1 d . . . H3 H 0.4105 0.8541 0.5895 0.033 Uiso 1 1 calc R . . C4 C 0.32836(12) 0.8898(4) 0.54556(15) 0.0274(7) Uani 1 1 d . . . H4 H 0.3173 0.9023 0.5850 0.033 Uiso 1 1 calc R . . C5 C 0.28957(12) 0.9006(4) 0.48538(15) 0.0258(6) Uani 1 1 d . . . H5 H 0.2519 0.9211 0.4843 0.031 Uiso 1 1 calc R . . C6 C 0.50009(12) 0.8180(4) 0.53259(15) 0.0258(6) Uani 1 1 d . . . C7 C 0.59851(11) 0.7297(3) 0.56147(14) 0.0226(6) Uani 1 1 d . . . H7 H 0.6070 0.8227 0.5908 0.027 Uiso 1 1 calc R . . C8 C 0.60215(11) 0.5848(4) 0.60429(13) 0.0210(6) Uani 1 1 d . . . H8 H 0.5910 0.4939 0.5743 0.025 Uiso 1 1 calc R . . C9 C 0.66107(12) 0.5559(4) 0.64682(15) 0.0260(7) Uani 1 1 d . . . H9A H 0.6717 0.6395 0.6799 0.031 Uiso 1 1 calc R . . H9B H 0.6621 0.4565 0.6706 0.031 Uiso 1 1 calc R . . C10 C 0.70260(12) 0.5500(4) 0.60565(16) 0.0275(7) Uani 1 1 d . . . H10B H 0.7406 0.5378 0.6350 0.033 Uiso 1 1 calc R . . H10A H 0.6945 0.4591 0.5760 0.033 Uiso 1 1 calc R . . C11 C 0.69985(12) 0.6963(4) 0.56512(16) 0.0273(7) Uani 1 1 d . . . H11B H 0.7261 0.6880 0.5375 0.033 Uiso 1 1 calc R . . H11A H 0.7109 0.7864 0.5948 0.033 Uiso 1 1 calc R . . C12 C 0.64062(12) 0.7208(4) 0.52102(15) 0.0268(7) Uani 1 1 d . . . H12A H 0.6393 0.8180 0.4957 0.032 Uiso 1 1 calc R . . H12B H 0.6307 0.6342 0.4893 0.032 Uiso 1 1 calc R . . C13 C 0.52082(12) 0.4961(4) 0.63901(14) 0.0235(6) Uani 1 1 d . . . C14 C 0.38760(12) 0.5260(4) 0.67645(14) 0.0247(6) Uani 1 1 d . . . H14 H 0.3872 0.6360 0.6745 0.030 Uiso 1 1 calc R . . C15 C 0.43574(12) 0.4503(3) 0.67382(14) 0.0226(6) Uani 1 1 d . . . C16 C 0.43631(13) 0.2885(4) 0.67571(15) 0.0290(7) Uani 1 1 d . . . H16 H 0.4686 0.2321 0.6741 0.035 Uiso 1 1 calc R . . C17 C 0.38878(13) 0.2133(4) 0.67989(15) 0.0299(7) Uani 1 1 d . . . H17 H 0.3878 0.1033 0.6803 0.036 Uiso 1 1 calc R . . C18 C 0.34262(13) 0.2969(4) 0.68343(15) 0.0293(7) Uani 1 1 d . . . H18 H 0.3105 0.2426 0.6873 0.035 Uiso 1 1 calc R . . H6W H 0.4765(16) 0.892(4) 0.767(2) 0.079(16) Uiso 1 1 d D . . H7WA H 0.549(2) 0.959(6) 0.6504(9) 0.106(19) Uiso 1 1 d D . . H7WB H 0.6046(8) 1.019(8) 0.704(3) 0.15(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01863(11) 0.03414(14) 0.03089(13) 0.00164(12) 0.00518(9) 0.00014(11) O1 0.0254(12) 0.0476(15) 0.0347(13) -0.0167(11) 0.0020(10) 0.0059(10) O2 0.0286(12) 0.0362(13) 0.0359(12) -0.0141(11) 0.0167(10) -0.0088(10) O3 0.0247(11) 0.0347(13) 0.0382(13) 0.0041(11) 0.0078(10) 0.0006(10) O4 0.0310(12) 0.0329(13) 0.0385(13) -0.0085(11) 0.0131(11) 0.0008(10) O5 0.0431(14) 0.0342(13) 0.0421(14) -0.0020(11) 0.0267(12) 0.0044(11) O6 0.082(3) 0.025(2) 0.060(3) 0.000 0.019(2) 0.000 O7 0.0434(19) 0.259(5) 0.0394(17) -0.046(3) 0.0150(16) -0.059(3) N1 0.0207(12) 0.0226(13) 0.0258(13) -0.0009(10) 0.0077(10) -0.0003(10) N2 0.0186(12) 0.0359(15) 0.0236(13) -0.0057(12) 0.0031(10) 0.0046(11) N3 0.0207(12) 0.0376(15) 0.0236(13) -0.0032(12) 0.0032(10) 0.0052(12) N4 0.0216(12) 0.0310(14) 0.0258(13) -0.0063(12) 0.0112(10) -0.0044(11) N5 0.0214(12) 0.0258(14) 0.0329(14) -0.0020(11) 0.0143(11) 0.0000(10) N6 0.0231(13) 0.0322(15) 0.0232(13) 0.0025(11) 0.0058(10) 0.0005(11) N7 0.0303(14) 0.0244(14) 0.0254(13) 0.0039(11) 0.0095(11) 0.0057(11) C1 0.0233(14) 0.0199(14) 0.0235(15) -0.0023(12) 0.0077(12) -0.0002(12) C2 0.0193(13) 0.0189(14) 0.0284(15) 0.0005(12) 0.0069(12) 0.0016(11) C3 0.0269(16) 0.0308(16) 0.0238(15) 0.0010(13) 0.0056(13) 0.0026(13) C4 0.0260(15) 0.0331(18) 0.0261(15) 0.0013(13) 0.0121(13) 0.0017(13) C5 0.0188(14) 0.0279(17) 0.0323(16) 0.0021(14) 0.0094(12) 0.0010(12) C6 0.0203(14) 0.0281(16) 0.0278(16) -0.0015(14) 0.0046(12) 0.0008(12) C7 0.0182(13) 0.0246(15) 0.0254(15) -0.0008(13) 0.0063(11) 0.0013(12) C8 0.0173(13) 0.0256(14) 0.0219(13) -0.0013(13) 0.0081(11) -0.0028(12) C9 0.0236(15) 0.0286(18) 0.0261(15) 0.0038(13) 0.0069(12) 0.0016(12) C10 0.0189(14) 0.0281(17) 0.0353(17) 0.0043(14) 0.0071(13) 0.0022(12) C11 0.0191(14) 0.0260(16) 0.0389(18) 0.0065(14) 0.0112(13) -0.0008(12) C12 0.0252(15) 0.0285(17) 0.0283(16) 0.0061(13) 0.0099(13) 0.0011(13) C13 0.0204(14) 0.0279(17) 0.0229(15) 0.0006(13) 0.0071(12) 0.0018(12) C14 0.0221(15) 0.0273(15) 0.0260(16) 0.0021(13) 0.0088(13) -0.0013(12) C15 0.0229(14) 0.0255(16) 0.0209(14) 0.0001(12) 0.0082(12) -0.0017(12) C16 0.0277(16) 0.0278(17) 0.0340(17) 0.0040(14) 0.0127(14) 0.0054(13) C17 0.0328(17) 0.0246(17) 0.0344(17) 0.0037(14) 0.0125(14) -0.0003(13) C18 0.0243(15) 0.0315(17) 0.0330(17) 0.0024(14) 0.0091(13) -0.0061(13) _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 N6 2.240(2) 7_566 ? Ag1 N1 2.289(2) . ? Ag1 O4 2.527(2) 4 ? Ag1 O3 2.557(2) . ? O1 C6 1.229(4) . ? O2 C13 1.229(4) . ? O3 N7 1.248(3) . ? O4 N7 1.256(3) . ? O4 Ag1 2.527(2) 4_545 ? O5 N7 1.249(3) . ? O6 H6W 0.99(4) . ? O7 H7WA 0.99(2) . ? O7 H7WB 0.99(3) . ? N1 C1 1.339(4) . ? N1 C5 1.342(4) . ? N2 C6 1.379(4) . ? N2 C2 1.389(4) . ? N2 H2N 0.8800 . ? N3 C6 1.349(4) . ? N3 C7 1.452(3) . ? N3 H3N 0.8800 . ? N4 C13 1.342(4) . ? N4 C8 1.463(3) . ? N4 H4N 0.8800 . ? N5 C13 1.377(4) . ? N5 C15 1.403(4) . ? N5 H5N 0.8800 . ? N6 C14 1.342(4) . ? N6 C18 1.350(4) . ? N6 Ag1 2.240(2) 7_566 ? C1 C2 1.386(4) . ? C1 H1 0.9500 . ? C2 C3 1.399(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C12 1.523(4) . ? C7 C8 1.531(4) . ? C7 H7 1.0000 . ? C8 C9 1.525(4) . ? C8 H8 1.0000 . ? C9 C10 1.521(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.516(4) . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? C11 C12 1.536(4) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.396(4) . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? 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 N6 Ag1 N1 123.35(9) 7_566 . ? N6 Ag1 O4 125.53(8) 7_566 4 ? N1 Ag1 O4 89.08(8) . 4 ? N6 Ag1 O3 120.88(8) 7_566 . ? N1 Ag1 O3 107.45(8) . . ? O4 Ag1 O3 79.26(7) 4 . ? N7 O3 Ag1 101.86(17) . . ? N7 O4 Ag1 109.50(17) . 4_545 ? H7WA O7 H7WB 111(5) . . ? C1 N1 C5 117.6(3) . . ? C1 N1 Ag1 120.89(19) . . ? C5 N1 Ag1 121.32(19) . . ? C6 N2 C2 126.8(3) . . ? C6 N2 H2N 116.6 . . ? C2 N2 H2N 116.6 . . ? C6 N3 C7 125.2(3) . . ? C6 N3 H3N 117.4 . . ? C7 N3 H3N 117.4 . . ? C13 N4 C8 122.3(3) . . ? C13 N4 H4N 118.9 . . ? C8 N4 H4N 118.9 . . ? C13 N5 C15 124.2(3) . . ? C13 N5 H5N 117.9 . . ? C15 N5 H5N 117.9 . . ? C14 N6 C18 117.3(3) . . ? C14 N6 Ag1 121.4(2) . 7_566 ? C18 N6 Ag1 120.5(2) . 7_566 ? O3 N7 O5 120.2(3) . . ? O3 N7 O4 120.2(3) . . ? O5 N7 O4 119.6(3) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 N2 117.0(3) . . ? C1 C2 C3 117.7(3) . . ? N2 C2 C3 125.2(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O1 C6 N3 124.8(3) . . ? O1 C6 N2 121.9(3) . . ? N3 C6 N2 113.2(3) . . ? N3 C7 C12 109.1(2) . . ? N3 C7 C8 111.0(2) . . ? C12 C7 C8 110.4(2) . . ? N3 C7 H7 108.8 . . ? C12 C7 H7 108.8 . . ? C8 C7 H7 108.8 . . ? N4 C8 C9 110.8(2) . . ? N4 C8 C7 110.4(2) . . ? C9 C8 C7 112.1(2) . . ? N4 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C10 C9 C8 111.5(2) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.1(2) . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? H10B C10 H10A 108.0 . . ? C10 C11 C12 110.3(2) . . ? C10 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? H11B C11 H11A 108.1 . . ? C7 C12 C11 111.4(2) . . ? C7 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C7 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? O2 C13 N4 123.6(3) . . ? O2 C13 N5 121.6(3) . . ? N4 C13 N5 114.7(3) . . ? N6 C14 C15 123.8(3) . . ? N6 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C14 C15 C16 118.3(3) . . ? C14 C15 N5 117.8(3) . . ? C16 C15 N5 123.9(3) . . ? C17 C16 C15 118.1(3) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N6 C18 C17 122.2(3) . . ? N6 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 O3 N7 -41.8(2) 7_566 . . . ? N1 Ag1 O3 N7 107.49(17) . . . . ? O4 Ag1 O3 N7 -166.91(18) 4 . . . ? N6 Ag1 N1 C1 -157.5(2) 7_566 . . . ? O4 Ag1 N1 C1 -24.3(2) 4 . . . ? O3 Ag1 N1 C1 54.2(2) . . . . ? N6 Ag1 N1 C5 18.2(3) 7_566 . . . ? O4 Ag1 N1 C5 151.4(2) 4 . . . ? O3 Ag1 N1 C5 -130.1(2) . . . . ? Ag1 O3 N7 O5 -9.4(3) . . . . ? Ag1 O3 N7 O4 171.4(2) . . . . ? Ag1 O4 N7 O3 10.7(3) 4_545 . . . ? Ag1 O4 N7 O5 -168.6(2) 4_545 . . . ? C5 N1 C1 C2 -0.2(4) . . . . ? Ag1 N1 C1 C2 175.7(2) . . . . ? N1 C1 C2 N2 176.7(3) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? C6 N2 C2 C1 164.3(3) . . . . ? C6 N2 C2 C3 -19.1(5) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? N2 C2 C3 C4 -176.1(3) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C1 N1 C5 C4 0.1(4) . . . . ? Ag1 N1 C5 C4 -175.7(2) . . . . ? C3 C4 C5 N1 0.3(5) . . . . ? C7 N3 C6 O1 7.0(5) . . . . ? C7 N3 C6 N2 -173.2(3) . . . . ? C2 N2 C6 O1 -10.8(5) . . . . ? C2 N2 C6 N3 169.4(3) . . . . ? C6 N3 C7 C12 -152.1(3) . . . . ? C6 N3 C7 C8 86.0(4) . . . . ? C13 N4 C8 C9 -118.1(3) . . . . ? C13 N4 C8 C7 117.1(3) . . . . ? N3 C7 C8 N4 -61.0(3) . . . . ? C12 C7 C8 N4 177.9(2) . . . . ? N3 C7 C8 C9 175.0(2) . . . . ? C12 C7 C8 C9 53.9(3) . . . . ? N4 C8 C9 C10 -177.9(3) . . . . ? C7 C8 C9 C10 -54.0(3) . . . . ? C8 C9 C10 C11 55.5(3) . . . . ? C9 C10 C11 C12 -57.0(4) . . . . ? N3 C7 C12 C11 -177.9(2) . . . . ? C8 C7 C12 C11 -55.6(3) . . . . ? C10 C11 C12 C7 57.7(3) . . . . ? C8 N4 C13 O2 12.7(5) . . . . ? C8 N4 C13 N5 -166.8(3) . . . . ? C15 N5 C13 O2 4.5(5) . . . . ? C15 N5 C13 N4 -176.0(3) . . . . ? C18 N6 C14 C15 -0.8(4) . . . . ? Ag1 N6 C14 C15 -170.9(2) 7_566 . . . ? N6 C14 C15 C16 0.9(5) . . . . ? N6 C14 C15 N5 -178.2(3) . . . . ? C13 N5 C15 C14 -149.3(3) . . . . ? C13 N5 C15 C16 31.7(5) . . . . ? C14 C15 C16 C17 0.2(4) . . . . ? N5 C15 C16 C17 179.2(3) . . . . ? C15 C16 C17 C18 -1.3(5) . . . . ? C14 N6 C18 C17 -0.4(5) . . . . ? Ag1 N6 C18 C17 169.8(2) 7_566 . . . ? C16 C17 C18 N6 1.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.040 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.092