# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Fenton, Hazel' 'Tidmarsh, Ian' 'Ward, Mike' _publ_contact_author_name 'Ward, Mike' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Luminescent silver(I) coordination networks based on bis-(3,5-dimethylpyrazolyl)naphthalene ligands ; # Attachment '- Ward_silvernetworks.cif' #======================================================== data_imw1128p1n _database_code_depnum_ccdc_archive 'CCDC 797099' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N4' _chemical_formula_weight 344.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.546(4) _cell_length_b 11.661(6) _cell_length_c 10.097(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.355(8) _cell_angle_gamma 90.00 _cell_volume 955.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3710 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.46 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9772 _exptl_absorpt_correction_T_max 0.9786 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10009 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.36 _reflns_number_total 1942 _reflns_number_gt 1531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was carried out to a resolution of 0.8 angstroms. Hydrogen atoms were added in calculated positions. 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^)+(0.0680P)^2^+0.1389P] 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 1942 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 N11 N 0.12514(15) 0.41819(10) 0.12413(11) 0.0248(3) Uani 1 1 d . . . N12 N 0.05675(15) 0.31960(10) 0.05818(12) 0.0269(3) Uani 1 1 d . . . C13 C 0.17225(19) 0.27601(13) 0.00929(14) 0.0282(4) Uani 1 1 d . . . C14 C 0.31242(19) 0.34575(13) 0.04408(14) 0.0294(4) Uani 1 1 d . . . H14 H 0.4107 0.3330 0.0213 0.035 Uiso 1 1 calc R . . C15 C 0.27919(18) 0.43681(13) 0.11824(14) 0.0267(3) Uani 1 1 d . . . C16 C 0.1382(2) 0.16826(14) -0.07573(18) 0.0419(5) Uani 1 1 d . . . H16A H 0.1310 0.1035 -0.0161 0.063 Uiso 1 1 calc R . . H16B H 0.2277 0.1547 -0.1152 0.063 Uiso 1 1 calc R . . H16C H 0.0338 0.1761 -0.1515 0.063 Uiso 1 1 calc R . . C17 C 0.3777(2) 0.54005(15) 0.18090(17) 0.0407(4) Uani 1 1 d . . . H17A H 0.3246 0.6088 0.1308 0.061 Uiso 1 1 calc R . . H17B H 0.4891 0.5330 0.1738 0.061 Uiso 1 1 calc R . . H17C H 0.3843 0.5461 0.2793 0.061 Uiso 1 1 calc R . . C18 C 0.03345(19) 0.48567(13) 0.19565(14) 0.0286(4) Uani 1 1 d . . . H18A H -0.0859 0.4763 0.1464 0.034 Uiso 1 1 calc R . . H18B H 0.0609 0.5677 0.1904 0.034 Uiso 1 1 calc R . . C21 C 0.06829(18) 0.45290(12) 0.34821(13) 0.0232(3) Uani 1 1 d . . . C22 C 0.17937(18) 0.36937(12) 0.40992(14) 0.0258(3) Uani 1 1 d . . . H22 H 0.2345 0.3288 0.3561 0.031 Uiso 1 1 calc R . . C23 C 0.21360(18) 0.34237(12) 0.55290(14) 0.0269(3) Uani 1 1 d . . . H23 H 0.2921 0.2846 0.5944 0.032 Uiso 1 1 calc R . . C24 C -0.13399(18) 0.60075(12) 0.36837(14) 0.0250(3) Uani 1 1 d . . . H24 H -0.1576 0.6198 0.2726 0.030 Uiso 1 1 calc R . . C25 C -0.01701(17) 0.51400(11) 0.42769(13) 0.0215(3) 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 N11 0.0305(7) 0.0272(6) 0.0199(6) 0.0001(5) 0.0126(5) 0.0015(5) N12 0.0305(7) 0.0277(7) 0.0230(6) 0.0004(5) 0.0089(5) -0.0001(5) C13 0.0336(8) 0.0293(8) 0.0209(7) 0.0018(6) 0.0074(6) 0.0086(7) C14 0.0290(8) 0.0392(9) 0.0233(7) 0.0048(6) 0.0128(6) 0.0081(7) C15 0.0294(8) 0.0318(8) 0.0203(7) 0.0054(6) 0.0099(6) 0.0007(6) C16 0.0522(11) 0.0359(9) 0.0324(8) -0.0067(7) 0.0060(8) 0.0134(8) C17 0.0425(10) 0.0398(9) 0.0397(9) 0.0004(7) 0.0128(8) -0.0096(8) C18 0.0356(9) 0.0319(8) 0.0227(7) 0.0014(6) 0.0156(6) 0.0081(7) C21 0.0275(8) 0.0243(7) 0.0202(7) -0.0006(6) 0.0109(6) -0.0014(6) C22 0.0319(8) 0.0257(7) 0.0244(7) -0.0007(6) 0.0155(6) 0.0035(6) C23 0.0293(8) 0.0264(7) 0.0269(7) 0.0048(6) 0.0116(6) 0.0063(6) C24 0.0276(8) 0.0283(8) 0.0205(7) 0.0037(6) 0.0096(6) 0.0011(6) C25 0.0237(7) 0.0220(7) 0.0205(7) -0.0001(5) 0.0095(5) -0.0030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C15 1.354(2) . ? N11 N12 1.3644(17) . ? N11 C18 1.4529(17) . ? N12 C13 1.3353(19) . ? C13 C14 1.398(2) . ? C13 C16 1.498(2) . ? C14 C15 1.380(2) . ? C14 H14 0.9500 . ? C15 C17 1.491(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.523(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C22 1.366(2) . ? C21 C25 1.4323(19) . ? C22 C23 1.415(2) . ? C22 H22 0.9500 . ? C23 C24 1.3694(19) 3_566 ? C23 H23 0.9500 . ? C24 C23 1.3694(19) 3_566 ? C24 C25 1.416(2) . ? C24 H24 0.9500 . ? C25 C25 1.434(3) 3_566 ? 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 C15 N11 N12 112.75(11) . . ? C15 N11 C18 128.24(13) . . ? N12 N11 C18 118.93(12) . . ? C13 N12 N11 104.37(12) . . ? N12 C13 C14 111.12(13) . . ? N12 C13 C16 119.91(14) . . ? C14 C13 C16 128.92(14) . . ? C15 C14 C13 106.11(13) . . ? C15 C14 H14 126.9 . . ? C13 C14 H14 126.9 . . ? N11 C15 C14 105.64(13) . . ? N11 C15 C17 122.55(13) . . ? C14 C15 C17 131.80(14) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N11 C18 C21 113.75(12) . . ? N11 C18 H18A 108.8 . . ? C21 C18 H18A 108.8 . . ? N11 C18 H18B 108.8 . . ? C21 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C22 C21 C25 120.16(12) . . ? C22 C21 C18 121.79(12) . . ? C25 C21 C18 118.04(13) . . ? C21 C22 C23 120.97(12) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.24(13) 3_566 . ? C24 C23 H23 119.9 3_566 . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.94(12) 3_566 . ? C23 C24 H24 119.5 3_566 . ? C25 C24 H24 119.5 . . ? C24 C25 C21 122.31(12) . . ? C24 C25 C25 118.90(15) . 3_566 ? C21 C25 C25 118.78(16) . 3_566 ? 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 C15 N11 N12 C13 -0.28(15) . . . . ? C18 N11 N12 C13 -177.32(11) . . . . ? N11 N12 C13 C14 0.20(15) . . . . ? N11 N12 C13 C16 -177.45(12) . . . . ? N12 C13 C14 C15 -0.06(16) . . . . ? C16 C13 C14 C15 177.32(14) . . . . ? N12 N11 C15 C14 0.25(15) . . . . ? C18 N11 C15 C14 176.95(12) . . . . ? N12 N11 C15 C17 178.98(12) . . . . ? C18 N11 C15 C17 -4.3(2) . . . . ? C13 C14 C15 N11 -0.11(15) . . . . ? C13 C14 C15 C17 -178.67(15) . . . . ? C15 N11 C18 C21 -86.20(18) . . . . ? N12 N11 C18 C21 90.33(15) . . . . ? N11 C18 C21 C22 1.6(2) . . . . ? N11 C18 C21 C25 -179.59(12) . . . . ? C25 C21 C22 C23 -0.6(2) . . . . ? C18 C21 C22 C23 178.16(13) . . . . ? C21 C22 C23 C24 0.7(2) . . . 3_566 ? C23 C24 C25 C21 179.97(13) 3_566 . . . ? C23 C24 C25 C25 0.2(2) 3_566 . . 3_566 ? C22 C21 C25 C24 -179.59(14) . . . . ? C18 C21 C25 C24 1.6(2) . . . . ? C22 C21 C25 C25 0.2(2) . . . 3_566 ? C18 C21 C25 C25 -178.64(15) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.299 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.048 #===END data_imw1185p21c _database_code_depnum_ccdc_archive 'CCDC 797100' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N4' _chemical_formula_weight 344.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.3365(18) _cell_length_b 5.0427(7) _cell_length_c 12.6153(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.280(9) _cell_angle_gamma 90.00 _cell_volume 897.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2245 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 26.97 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9810 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6878 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 24.71 _reflns_number_total 1506 _reflns_number_gt 1068 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was carried out to a resolution of 0.85 angstroms. 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^)+(0.0431P)^2^+1.6415P] 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 1506 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _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 N11 N 0.23920(18) 0.3067(6) 0.23080(19) 0.0198(7) Uani 1 1 d . . . N12 N 0.22779(18) 0.4920(6) 0.15042(19) 0.0209(7) Uani 1 1 d . . . C13 C 0.1440(2) 0.6024(7) 0.1528(2) 0.0209(8) Uani 1 1 d . . . C14 C 0.1018(2) 0.4935(7) 0.2348(2) 0.0218(8) Uani 1 1 d . . . H14 H 0.0423 0.5395 0.2528 0.026 Uiso 1 1 calc R . . C15 C 0.1649(2) 0.3051(7) 0.2838(2) 0.0191(8) Uani 1 1 d . . . C16 C 0.1073(2) 0.8173(7) 0.0732(3) 0.0289(9) Uani 1 1 d . . . H16A H 0.1584 0.8772 0.0368 0.043 Uiso 1 1 calc R . . H16B H 0.0847 0.9669 0.1113 0.043 Uiso 1 1 calc R . . H16C H 0.0550 0.7475 0.0199 0.043 Uiso 1 1 calc R . . C17 C 0.1617(2) 0.1236(7) 0.3768(2) 0.0254(8) Uani 1 1 d . . . H17A H 0.1617 -0.0609 0.3524 0.038 Uiso 1 1 calc R . . H17B H 0.1039 0.1580 0.4060 0.038 Uiso 1 1 calc R . . H17C H 0.2173 0.1548 0.4329 0.038 Uiso 1 1 calc R . . C18 C 0.3255(2) 0.1528(7) 0.2529(2) 0.0235(8) Uani 1 1 d . . . H18A H 0.3528 0.1420 0.1863 0.028 Uiso 1 1 calc R . . H18B H 0.3095 -0.0298 0.2723 0.028 Uiso 1 1 calc R . . C21 C 0.3824(2) 0.4622(7) 0.4094(2) 0.0206(8) Uani 1 1 d . . . H21 H 0.3210 0.5391 0.3998 0.025 Uiso 1 1 calc R . . C22 C 0.4002(2) 0.2626(7) 0.3425(2) 0.0191(8) Uani 1 1 d . . . C23 C 0.4914(2) 0.1490(7) 0.3570(2) 0.0205(8) Uani 1 1 d . . . H23 H 0.5034 0.0090 0.3109 0.025 Uiso 1 1 calc R . . C24 C 0.5627(2) 0.2355(7) 0.4357(2) 0.0214(8) Uani 1 1 d . . . H24 H 0.6239 0.1575 0.4431 0.026 Uiso 1 1 calc R . . C25 C 0.4544(2) 0.5564(7) 0.4929(2) 0.0176(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N11 0.0243(15) 0.0208(16) 0.0144(13) -0.0007(13) 0.0031(11) 0.0009(13) N12 0.0287(16) 0.0217(15) 0.0123(13) 0.0018(13) 0.0032(11) -0.0013(14) C13 0.0279(18) 0.0196(18) 0.0144(16) -0.0036(15) 0.0017(13) -0.0023(16) C14 0.0223(17) 0.0234(19) 0.0196(16) -0.0060(16) 0.0038(13) 0.0004(16) C15 0.0279(18) 0.0161(17) 0.0131(15) -0.0040(15) 0.0032(13) -0.0048(15) C16 0.037(2) 0.026(2) 0.0222(18) 0.0003(17) 0.0026(15) 0.0055(18) C17 0.0353(19) 0.0240(19) 0.0165(16) 0.0006(16) 0.0035(14) -0.0043(16) C18 0.0271(18) 0.025(2) 0.0180(17) -0.0006(16) 0.0037(13) 0.0034(16) C21 0.0237(17) 0.0187(19) 0.0198(16) 0.0033(15) 0.0047(13) 0.0012(15) C22 0.0279(18) 0.0172(19) 0.0128(16) 0.0037(15) 0.0048(13) -0.0017(15) C23 0.0288(18) 0.0193(19) 0.0141(16) -0.0043(15) 0.0057(13) -0.0025(16) C24 0.0241(17) 0.0205(19) 0.0206(17) 0.0034(16) 0.0068(14) 0.0048(15) C25 0.0238(16) 0.0168(18) 0.0139(15) 0.0001(14) 0.0079(13) -0.0024(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C15 1.355(4) . ? N11 N12 1.367(4) . ? N11 C18 1.445(4) . ? N12 C13 1.330(4) . ? C13 C14 1.400(4) . ? C13 C16 1.507(5) . ? C14 C15 1.379(5) . ? C14 H14 0.9500 . ? C15 C17 1.495(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C22 1.516(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C22 1.366(5) . ? C21 C25 1.419(4) . ? C21 H21 0.9500 . ? C22 C23 1.409(4) . ? C23 C24 1.363(4) . ? C23 H23 0.9500 . ? C24 C25 1.432(5) 3_666 ? C24 H24 0.9500 . ? C25 C25 1.408(6) 3_666 ? C25 C24 1.432(5) 3_666 ? 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 C15 N11 N12 111.7(3) . . ? C15 N11 C18 128.5(3) . . ? N12 N11 C18 119.7(2) . . ? C13 N12 N11 105.0(2) . . ? N12 C13 C14 111.4(3) . . ? N12 C13 C16 119.7(3) . . ? C14 C13 C16 129.0(3) . . ? C15 C14 C13 105.4(3) . . ? C15 C14 H14 127.3 . . ? C13 C14 H14 127.3 . . ? N11 C15 C14 106.6(3) . . ? N11 C15 C17 121.9(3) . . ? C14 C15 C17 131.6(3) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N11 C18 C22 114.5(3) . . ? N11 C18 H18A 108.6 . . ? C22 C18 H18A 108.6 . . ? N11 C18 H18B 108.6 . . ? C22 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C22 C21 C25 121.0(3) . . ? C22 C21 H21 119.5 . . ? C25 C21 H21 119.5 . . ? C21 C22 C23 119.4(3) . . ? C21 C22 C18 123.0(3) . . ? C23 C22 C18 117.6(3) . . ? C24 C23 C22 121.5(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 120.1(3) . 3_666 ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 3_666 . ? C25 C25 C21 119.6(4) 3_666 . ? C25 C25 C24 118.4(4) 3_666 3_666 ? C21 C25 C24 121.9(3) . 3_666 ? 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 C15 N11 N12 C13 -1.2(3) . . . . ? C18 N11 N12 C13 -178.2(3) . . . . ? N11 N12 C13 C14 0.9(4) . . . . ? N11 N12 C13 C16 -179.5(3) . . . . ? N12 C13 C14 C15 -0.2(4) . . . . ? C16 C13 C14 C15 -179.9(3) . . . . ? N12 N11 C15 C14 1.1(4) . . . . ? C18 N11 C15 C14 177.7(3) . . . . ? N12 N11 C15 C17 -178.7(3) . . . . ? C18 N11 C15 C17 -2.1(5) . . . . ? C13 C14 C15 N11 -0.5(3) . . . . ? C13 C14 C15 C17 179.2(3) . . . . ? C15 N11 C18 C22 -81.1(4) . . . . ? N12 N11 C18 C22 95.3(3) . . . . ? C25 C21 C22 C23 0.0(5) . . . . ? C25 C21 C22 C18 179.3(3) . . . . ? N11 C18 C22 C21 10.8(4) . . . . ? N11 C18 C22 C23 -169.9(3) . . . . ? C21 C22 C23 C24 -0.6(5) . . . . ? C18 C22 C23 C24 -179.9(3) . . . . ? C22 C23 C24 C25 1.0(5) . . . 3_666 ? C22 C21 C25 C25 0.3(5) . . . 3_666 ? C22 C21 C25 C24 -179.7(3) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.291 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.061 #===END data_imw1372_0m _database_code_depnum_ccdc_archive 'CCDC 797101' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N4' _chemical_formula_weight 344.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 10.3591(4) _cell_length_b 12.9102(4) _cell_length_c 27.5492(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3684.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6786 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.70 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9925 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54346 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4224 _reflns_number_gt 2898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^)+(0.0479P)^2^+1.3856P] 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 4224 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 N11 N 1.07233(13) 0.39090(10) 0.04649(4) 0.0301(3) Uani 1 1 d . . . N12 N 1.03116(14) 0.30912(10) 0.01892(5) 0.0328(3) Uani 1 1 d . . . N21 N 0.74432(13) 0.29170(10) 0.27023(4) 0.0306(3) Uani 1 1 d . . . N22 N 0.83408(14) 0.32682(11) 0.30285(5) 0.0371(3) Uani 1 1 d . . . C13 C 1.13767(17) 0.25384(13) 0.01042(6) 0.0329(4) Uani 1 1 d . . . C14 C 1.24573(17) 0.30002(14) 0.03167(6) 0.0359(4) Uani 1 1 d . . . H14 H 1.3322 0.2757 0.0304 0.043 Uiso 1 1 calc R . . C15 C 1.20186(17) 0.38781(13) 0.05482(6) 0.0340(4) Uani 1 1 d . . . C16 C 1.1329(2) 0.15754(15) -0.01965(7) 0.0493(5) Uani 1 1 d . . . H16A H 1.0445 0.1304 -0.0200 0.074 Uiso 1 1 calc R . . H16B H 1.1911 0.1055 -0.0058 0.074 Uiso 1 1 calc R . . H16C H 1.1599 0.1735 -0.0529 0.074 Uiso 1 1 calc R . . C17 C 1.2712(2) 0.46729(16) 0.08426(7) 0.0501(5) Uani 1 1 d . . . H17B H 1.2354 0.5360 0.0773 0.075 Uiso 1 1 calc R . . H17A H 1.3632 0.4664 0.0760 0.075 Uiso 1 1 calc R . . H17C H 1.2605 0.4517 0.1188 0.075 Uiso 1 1 calc R . . C18 C 0.97788(17) 0.46755(13) 0.06145(6) 0.0346(4) Uani 1 1 d . . . H18B H 0.9139 0.4760 0.0351 0.042 Uiso 1 1 calc R . . H18A H 1.0223 0.5348 0.0657 0.042 Uiso 1 1 calc R . . C23 C 0.87079(17) 0.24199(15) 0.32705(6) 0.0380(4) Uani 1 1 d . . . C24 C 0.80589(18) 0.15435(14) 0.30982(6) 0.0387(4) Uani 1 1 d . . . H25 H 0.8156 0.0852 0.3210 0.046 Uiso 1 1 calc R . . C25 C 0.72543(16) 0.18788(13) 0.27350(6) 0.0327(4) Uani 1 1 d . . . C26 C 0.9705(2) 0.24904(17) 0.36647(6) 0.0507(5) Uani 1 1 d . . . H26A H 0.9980 0.3212 0.3702 0.076 Uiso 1 1 calc R . . H26C H 1.0451 0.2061 0.3579 0.076 Uiso 1 1 calc R . . H26B H 0.9334 0.2244 0.3971 0.076 Uiso 1 1 calc R . . C27 C 0.63320(18) 0.13136(14) 0.24165(7) 0.0418(4) Uani 1 1 d . . . H27A H 0.5462 0.1595 0.2462 0.063 Uiso 1 1 calc R . . H27C H 0.6336 0.0576 0.2501 0.063 Uiso 1 1 calc R . . H27B H 0.6591 0.1398 0.2077 0.063 Uiso 1 1 calc R . . C28 C 0.68363(16) 0.36480(12) 0.23751(5) 0.0310(4) Uani 1 1 d . . . H28A H 0.6672 0.4300 0.2554 0.037 Uiso 1 1 calc R . . H28B H 0.5990 0.3365 0.2274 0.037 Uiso 1 1 calc R . . C31 C 0.90618(16) 0.44171(12) 0.10822(5) 0.0270(3) Uani 1 1 d . . . C32 C 0.94919(16) 0.36852(12) 0.14031(6) 0.0306(4) Uani 1 1 d . . . H32 H 1.0284 0.3339 0.1341 0.037 Uiso 1 1 calc R . . C33 C 0.87808(16) 0.34339(12) 0.18260(5) 0.0295(4) Uani 1 1 d . . . H33 H 0.9115 0.2935 0.2046 0.035 Uiso 1 1 calc R . . C34 C 0.76218(15) 0.38965(11) 0.19224(5) 0.0263(3) Uani 1 1 d . . . C35 C 0.71333(15) 0.46620(11) 0.15945(5) 0.0256(3) Uani 1 1 d . . . C36 C 0.78753(15) 0.49429(11) 0.11771(5) 0.0259(3) Uani 1 1 d . . . C41 C 0.59253(16) 0.51638(12) 0.16694(6) 0.0314(4) Uani 1 1 d . . . H41 H 0.5409 0.4972 0.1940 0.038 Uiso 1 1 calc R . . C42 C 0.54928(17) 0.59149(13) 0.13606(6) 0.0362(4) Uani 1 1 d . . . H42 H 0.4684 0.6238 0.1418 0.043 Uiso 1 1 calc R . . C43 C 0.62371(17) 0.62116(13) 0.09586(6) 0.0364(4) Uani 1 1 d . . . H43 H 0.5939 0.6745 0.0749 0.044 Uiso 1 1 calc R . . C44 C 0.73878(17) 0.57355(12) 0.08682(5) 0.0315(4) Uani 1 1 d . . . H44 H 0.7876 0.5938 0.0592 0.038 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 N11 0.0330(8) 0.0314(7) 0.0258(6) 0.0008(6) 0.0051(6) -0.0005(6) N12 0.0345(8) 0.0334(7) 0.0306(7) 0.0003(6) 0.0003(6) -0.0022(6) N21 0.0362(8) 0.0332(7) 0.0224(6) 0.0034(5) 0.0034(6) -0.0021(6) N22 0.0430(9) 0.0438(8) 0.0245(7) 0.0035(6) -0.0002(6) -0.0055(7) C13 0.0362(9) 0.0364(9) 0.0261(8) 0.0012(7) 0.0016(7) 0.0035(8) C14 0.0318(9) 0.0459(10) 0.0301(8) -0.0011(8) 0.0012(7) 0.0055(8) C15 0.0344(9) 0.0413(10) 0.0262(8) 0.0023(7) 0.0010(7) -0.0032(8) C16 0.0569(13) 0.0457(11) 0.0453(11) -0.0122(9) -0.0083(10) 0.0083(10) C17 0.0535(13) 0.0521(12) 0.0446(11) -0.0085(9) -0.0037(9) -0.0083(10) C18 0.0415(10) 0.0313(9) 0.0310(8) 0.0048(7) 0.0089(8) 0.0053(8) C23 0.0411(10) 0.0470(11) 0.0260(8) 0.0076(8) 0.0054(8) 0.0017(9) C24 0.0429(10) 0.0382(10) 0.0348(9) 0.0112(8) 0.0074(8) 0.0032(8) C25 0.0350(9) 0.0321(9) 0.0310(8) 0.0022(7) 0.0116(7) -0.0001(7) C26 0.0535(12) 0.0669(14) 0.0317(9) 0.0084(9) -0.0029(9) 0.0059(11) C27 0.0417(11) 0.0359(10) 0.0476(11) -0.0031(8) 0.0059(9) 0.0000(8) C28 0.0349(9) 0.0308(8) 0.0272(8) 0.0024(7) 0.0044(7) 0.0011(7) C31 0.0333(9) 0.0247(8) 0.0231(7) -0.0008(6) 0.0027(7) -0.0010(7) C32 0.0324(9) 0.0291(8) 0.0302(8) 0.0010(7) 0.0047(7) 0.0055(7) C33 0.0357(9) 0.0271(8) 0.0259(8) 0.0050(6) 0.0008(7) 0.0034(7) C34 0.0318(9) 0.0235(7) 0.0235(7) -0.0003(6) 0.0022(7) -0.0015(7) C35 0.0296(8) 0.0225(7) 0.0247(7) -0.0022(6) -0.0003(6) -0.0010(6) C36 0.0321(9) 0.0222(8) 0.0233(7) -0.0028(6) -0.0012(6) -0.0013(6) C41 0.0308(9) 0.0288(8) 0.0346(9) -0.0015(7) 0.0042(7) -0.0010(7) C42 0.0337(9) 0.0303(9) 0.0446(10) -0.0026(8) -0.0026(8) 0.0064(7) C43 0.0441(10) 0.0288(9) 0.0362(9) 0.0029(7) -0.0086(8) 0.0064(8) C44 0.0417(10) 0.0269(8) 0.0258(8) 0.0021(6) 0.0004(7) 0.0012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C15 1.362(2) . ? N11 N12 1.3687(18) . ? N11 C18 1.451(2) . ? N12 C13 1.335(2) . ? N21 C25 1.358(2) . ? N21 N22 1.3703(19) . ? N21 C28 1.449(2) . ? N22 C23 1.337(2) . ? C13 C14 1.397(2) . ? C13 C16 1.495(2) . ? C14 C15 1.378(2) . ? C14 H14 0.9500 . ? C15 C17 1.492(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17C 0.9800 . ? C18 C31 1.524(2) . ? C18 H18B 0.9900 . ? C18 H18A 0.9900 . ? C23 C24 1.399(3) . ? C23 C26 1.501(3) . ? C24 C25 1.372(2) . ? C24 H25 0.9500 . ? C25 C27 1.488(2) . ? C26 H26A 0.9800 . ? C26 H26C 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C28 C34 1.523(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C31 C32 1.369(2) . ? C31 C36 1.428(2) . ? C32 C33 1.416(2) . ? C32 H32 0.9500 . ? C33 C34 1.367(2) . ? C33 H33 0.9500 . ? C34 C35 1.431(2) . ? C35 C41 1.424(2) . ? C35 C36 1.430(2) . ? C36 C44 1.423(2) . ? C41 C42 1.365(2) . ? C41 H41 0.9500 . ? C42 C43 1.403(2) . ? C42 H42 0.9500 . ? C43 C44 1.364(2) . ? C43 H43 0.9500 . ? C44 H44 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 C15 N11 N12 112.21(13) . . ? C15 N11 C18 129.52(14) . . ? N12 N11 C18 118.25(14) . . ? C13 N12 N11 104.60(13) . . ? C25 N21 N22 112.39(13) . . ? C25 N21 C28 128.46(14) . . ? N22 N21 C28 119.15(13) . . ? C23 N22 N21 104.42(14) . . ? N12 C13 C14 111.15(15) . . ? N12 C13 C16 120.96(16) . . ? C14 C13 C16 127.87(16) . . ? C15 C14 C13 106.31(15) . . ? C15 C14 H14 126.8 . . ? C13 C14 H14 126.8 . . ? N11 C15 C14 105.73(15) . . ? N11 C15 C17 123.08(16) . . ? C14 C15 C17 131.19(17) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C15 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? N11 C18 C31 114.79(13) . . ? N11 C18 H18B 108.6 . . ? C31 C18 H18B 108.6 . . ? N11 C18 H18A 108.6 . . ? C31 C18 H18A 108.6 . . ? H18B C18 H18A 107.5 . . ? N22 C23 C24 110.88(15) . . ? N22 C23 C26 120.44(17) . . ? C24 C23 C26 128.68(17) . . ? C25 C24 C23 106.51(15) . . ? C25 C24 H25 126.7 . . ? C23 C24 H25 126.7 . . ? N21 C25 C24 105.80(15) . . ? N21 C25 C27 122.52(15) . . ? C24 C25 C27 131.68(16) . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? N21 C28 C34 114.51(13) . . ? N21 C28 H28A 108.6 . . ? C34 C28 H28A 108.6 . . ? N21 C28 H28B 108.6 . . ? C34 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C32 C31 C36 119.35(14) . . ? C32 C31 C18 122.58(14) . . ? C36 C31 C18 118.04(13) . . ? C31 C32 C33 121.35(15) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 121.11(14) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 119.31(14) . . ? C33 C34 C28 122.42(14) . . ? C35 C34 C28 118.25(14) . . ? C41 C35 C36 118.27(14) . . ? C41 C35 C34 122.23(14) . . ? C36 C35 C34 119.51(14) . . ? C44 C36 C31 122.52(14) . . ? C44 C36 C35 118.18(14) . . ? C31 C36 C35 119.30(13) . . ? C42 C41 C35 121.40(15) . . ? C42 C41 H41 119.3 . . ? C35 C41 H41 119.3 . . ? C41 C42 C43 120.36(16) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 120.08(15) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C36 121.67(15) . . ? C43 C44 H44 119.2 . . ? C36 C44 H44 119.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.211 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.039 #===END data_imw1169c2c _database_code_depnum_ccdc_archive 'CCDC 797102' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Ag N5 O3' _chemical_formula_weight 514.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 23.0936(9) _cell_length_b 7.9450(3) _cell_length_c 15.8799(7) _cell_angle_alpha 90.00 _cell_angle_beta 132.487(3) _cell_angle_gamma 90.00 _cell_volume 2148.59(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9821 _cell_measurement_theta_min 2.3955 _cell_measurement_theta_max 33.471 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6970 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19168 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2464 _reflns_number_gt 2421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by Patterson methods. The data was processed to a resolution of 0.77 angstroms as it was only complete to this level. All hydrogens were added in geometrically calculated positions. The free nitrate solvent molecule (N1 O1 O2) sits in a special position causing only 2 of the 3 oxygens of the molecule to appear in the model. The occupancy of N1 and O2 have been set to 10.5 as a result of this. The silver atom Ag1 is also in a special position and so also has an occupancy of 10.5. 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^)+(0.0326P)^2^+4.3725P] 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 2464 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 1.0000 0.34831(3) 0.2500 0.02484(8) Uani 1 2 d S . . N11 N 0.95073(9) 0.1929(2) 0.03103(13) 0.0192(3) Uani 1 1 d . . . N12 N 1.01205(9) 0.2704(2) 0.13072(12) 0.0194(3) Uani 1 1 d . . . C13 C 1.06006(10) 0.3219(2) 0.11660(15) 0.0190(3) Uani 1 1 d . . . C14 C 1.02879(10) 0.2782(2) 0.00693(15) 0.0208(3) Uani 1 1 d . . . H14 H 1.0513 0.3000 -0.0245 0.025 Uiso 1 1 calc R . . C15 C 0.95859(10) 0.1972(2) -0.04583(15) 0.0202(3) Uani 1 1 d . . . C16 C 1.13555(11) 0.4065(3) 0.21290(16) 0.0248(4) Uani 1 1 d . . . H16A H 1.1312 0.4569 0.2648 0.037 Uiso 1 1 calc R . . H16B H 1.1469 0.4947 0.1826 0.037 Uiso 1 1 calc R . . H16C H 1.1781 0.3235 0.2545 0.037 Uiso 1 1 calc R . . C17 C 0.89793(12) 0.1260(3) -0.16335(16) 0.0262(4) Uani 1 1 d . . . H17A H 0.8970 0.0031 -0.1588 0.039 Uiso 1 1 calc R . . H17B H 0.9108 0.1563 -0.2090 0.039 Uiso 1 1 calc R . . H17C H 0.8463 0.1717 -0.1994 0.039 Uiso 1 1 calc R . . C18 C 0.88939(11) 0.1164(2) 0.02184(16) 0.0213(3) Uani 1 1 d . . . H18A H 0.9140 0.0532 0.0928 0.026 Uiso 1 1 calc R . . H18B H 0.8598 0.0350 -0.0422 0.026 Uiso 1 1 calc R . . C21 C 0.77777(9) 0.1908(2) 0.01124(14) 0.0165(3) Uani 1 1 d . . . C22 C 0.83257(10) 0.2443(2) 0.00227(14) 0.0175(3) Uani 1 1 d . . . C23 C 0.83199(10) 0.4082(2) -0.02519(15) 0.0207(3) Uani 1 1 d . . . H23 H 0.8692 0.4439 -0.0295 0.025 Uiso 1 1 calc R . . C24 C 0.77719(10) 0.5248(2) -0.04718(15) 0.0216(3) Uani 1 1 d . . . H24 H 0.7779 0.6377 -0.0662 0.026 Uiso 1 1 calc R . . C25 C 0.72306(10) 0.4774(2) -0.04142(15) 0.0192(3) Uani 1 1 d . . . H25 H 0.6859 0.5568 -0.0576 0.023 Uiso 1 1 calc R . . N1 N 1.0000 0.7296(3) 0.2500 0.0229(4) Uani 1 2 d S . . O1 O 1.06302(9) 0.6506(2) 0.32071(14) 0.0343(4) Uani 1 1 d . . . O2 O 1.0000 0.8861(3) 0.2500 0.0341(5) 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 0.02850(12) 0.03480(13) 0.02113(12) 0.000 0.02075(10) 0.000 N11 0.0171(7) 0.0262(7) 0.0185(7) -0.0008(6) 0.0137(6) -0.0002(6) N12 0.0190(7) 0.0258(8) 0.0168(7) 0.0002(6) 0.0134(6) 0.0007(6) C13 0.0178(8) 0.0242(8) 0.0173(8) 0.0032(6) 0.0128(7) 0.0031(6) C14 0.0212(8) 0.0286(9) 0.0180(8) 0.0023(7) 0.0154(7) 0.0016(7) C15 0.0203(8) 0.0260(8) 0.0178(8) 0.0020(7) 0.0143(7) 0.0039(7) C16 0.0201(8) 0.0350(10) 0.0184(8) 0.0003(7) 0.0126(7) -0.0029(7) C17 0.0257(9) 0.0325(10) 0.0188(9) -0.0028(7) 0.0145(8) -0.0010(8) C18 0.0198(8) 0.0254(9) 0.0255(9) 0.0000(7) 0.0180(8) -0.0004(7) C21 0.0148(7) 0.0217(8) 0.0120(7) -0.0012(6) 0.0087(6) -0.0019(6) C22 0.0148(7) 0.0244(8) 0.0136(7) -0.0001(6) 0.0097(6) -0.0006(6) C23 0.0182(8) 0.0265(9) 0.0193(8) 0.0013(7) 0.0134(7) -0.0024(7) C24 0.0203(8) 0.0213(8) 0.0216(8) 0.0037(7) 0.0135(7) -0.0008(7) C25 0.0178(8) 0.0214(8) 0.0174(8) 0.0013(6) 0.0114(7) 0.0007(6) N1 0.0261(11) 0.0309(12) 0.0165(10) 0.000 0.0163(9) 0.000 O1 0.0303(8) 0.0396(9) 0.0292(8) 0.0093(6) 0.0186(7) 0.0084(6) O2 0.0416(12) 0.0271(10) 0.0328(11) 0.000 0.0248(10) 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 N12 2.1819(14) 2_755 ? Ag1 N12 2.1819(14) . ? N11 C15 1.350(2) . ? N11 N12 1.364(2) . ? N11 C18 1.456(2) . ? N12 C13 1.335(2) . ? C13 C14 1.406(2) . ? C13 C16 1.493(3) . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C17 1.495(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C22 1.517(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C21 C25 1.424(2) 7_655 ? C21 C21 1.428(3) 7_655 ? C21 C22 1.430(2) . ? C22 C23 1.371(3) . ? C23 C24 1.408(3) . ? C23 H23 0.9500 . ? C24 C25 1.367(2) . ? C24 H24 0.9500 . ? C25 C21 1.424(2) 7_655 ? C25 H25 0.9500 . ? N1 O2 1.243(3) . ? N1 O1 1.2513(19) 2_755 ? N1 O1 1.2513(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Ag1 N12 147.02(8) 2_755 . ? C15 N11 N12 111.70(14) . . ? C15 N11 C18 129.47(16) . . ? N12 N11 C18 118.81(14) . . ? C13 N12 N11 105.79(14) . . ? C13 N12 Ag1 131.77(13) . . ? N11 N12 Ag1 119.62(11) . . ? N12 C13 C14 110.02(16) . . ? N12 C13 C16 119.58(16) . . ? C14 C13 C16 130.36(16) . . ? C15 C14 C13 106.07(16) . . ? C15 C14 H14 127.0 . . ? C13 C14 H14 127.0 . . ? N11 C15 C14 106.41(16) . . ? N11 C15 C17 122.31(17) . . ? C14 C15 C17 131.28(17) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N11 C18 C22 112.90(15) . . ? N11 C18 H18A 109.0 . . ? C22 C18 H18A 109.0 . . ? N11 C18 H18B 109.0 . . ? C22 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C25 C21 C21 119.22(19) 7_655 7_655 ? C25 C21 C22 121.75(16) 7_655 . ? C21 C21 C22 119.0(2) 7_655 . ? C23 C22 C21 119.65(16) . . ? C23 C22 C18 121.55(15) . . ? C21 C22 C18 118.80(16) . . ? C22 C23 C24 121.19(16) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 120.76(17) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C21 120.13(16) . 7_655 ? C24 C25 H25 119.9 . . ? C21 C25 H25 119.9 7_655 . ? O2 N1 O1 120.13(12) . 2_755 ? O2 N1 O1 120.13(12) . . ? O1 N1 O1 119.7(2) 2_755 . ? 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 C15 N11 N12 C13 -1.0(2) . . . . ? C18 N11 N12 C13 177.48(15) . . . . ? C15 N11 N12 Ag1 162.13(12) . . . . ? C18 N11 N12 Ag1 -19.4(2) . . . . ? N12 Ag1 N12 C13 -133.85(16) 2_755 . . . ? N12 Ag1 N12 N11 68.13(12) 2_755 . . . ? N11 N12 C13 C14 0.5(2) . . . . ? Ag1 N12 C13 C14 -159.75(13) . . . . ? N11 N12 C13 C16 -177.55(16) . . . . ? Ag1 N12 C13 C16 22.2(3) . . . . ? N12 C13 C14 C15 0.2(2) . . . . ? C16 C13 C14 C15 177.92(19) . . . . ? N12 N11 C15 C14 1.1(2) . . . . ? C18 N11 C15 C14 -177.17(17) . . . . ? N12 N11 C15 C17 -177.95(17) . . . . ? C18 N11 C15 C17 3.8(3) . . . . ? C13 C14 C15 N11 -0.8(2) . . . . ? C13 C14 C15 C17 178.19(19) . . . . ? C15 N11 C18 C22 -104.4(2) . . . . ? N12 N11 C18 C22 77.4(2) . . . . ? C25 C21 C22 C23 -178.91(16) 7_655 . . . ? C21 C21 C22 C23 1.4(3) 7_655 . . . ? C25 C21 C22 C18 2.0(2) 7_655 . . . ? C21 C21 C22 C18 -177.71(18) 7_655 . . . ? N11 C18 C22 C23 11.6(2) . . . . ? N11 C18 C22 C21 -169.33(15) . . . . ? C21 C22 C23 C24 -1.3(3) . . . . ? C18 C22 C23 C24 177.72(17) . . . . ? C22 C23 C24 C25 0.2(3) . . . . ? C23 C24 C25 C21 1.0(3) . . . 7_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.074 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.084 #===END data_imw1170p-1 _database_code_depnum_ccdc_archive 'CCDC 797103' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H81 Ag2 F6 N15 O6 S2' _chemical_formula_weight 1670.40 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8647(12) _cell_length_b 14.487(2) _cell_length_c 14.955(2) _cell_angle_alpha 92.109(9) _cell_angle_beta 104.197(8) _cell_angle_gamma 99.937(8) _cell_volume 1827.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4244 _cell_measurement_theta_min 2.4635 _cell_measurement_theta_max 24.0915 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9358 _exptl_absorpt_correction_T_max 0.9933 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19203 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7468 _reflns_number_gt 5570 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by Patterson methods. The data was processed to a resolution of 0.8 angstroms as it was only complete to this level. All hydrogens were added in geometrically calculated positions. The free acetonitrile solvent molecule (N1S C1S) sits on the inversion centre causing the molecule to appear as N1S-C1S-C-N. The occupancy of the nitrogen atom has been set to 10.5 as a result of this. These atoms have been left isotropic. As a result of this disorder the hydrogen atoms for this solvent molecule have been omitted 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^)+(0.0376P)^2^+1.6078P] 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 7468 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.90160(3) 0.750277(19) 0.738497(19) 0.02588(9) Uani 1 1 d . . . N111 N 0.7579(3) 0.94347(19) 0.70694(18) 0.0214(6) Uani 1 1 d . . . N112 N 0.7463(3) 0.85231(19) 0.67681(19) 0.0240(6) Uani 1 1 d . . . C113 C 0.6156(4) 0.8322(2) 0.6068(2) 0.0250(8) Uani 1 1 d . . . C114 C 0.5455(4) 0.9109(3) 0.5925(2) 0.0269(8) Uani 1 1 d . . . H114 H 0.4517 0.9152 0.5470 0.032 Uiso 1 1 calc R . . C115 C 0.6379(4) 0.9813(2) 0.6566(2) 0.0225(7) Uani 1 1 d . . . C116 C 0.5670(4) 0.7364(3) 0.5567(3) 0.0341(9) Uani 1 1 d . . . H11A H 0.6595 0.7060 0.5647 0.051 Uiso 1 1 calc R . . H11B H 0.5227 0.7417 0.4907 0.051 Uiso 1 1 calc R . . H11C H 0.4868 0.6985 0.5820 0.051 Uiso 1 1 calc R . . C117 C 0.6237(5) 1.0805(3) 0.6718(3) 0.0327(9) Uani 1 1 d . . . H11D H 0.5910 1.0892 0.7291 0.049 Uiso 1 1 calc R . . H11E H 0.5444 1.0967 0.6196 0.049 Uiso 1 1 calc R . . H11F H 0.7263 1.1213 0.6768 0.049 Uiso 1 1 calc R . . C118 C 0.8922(4) 0.9893(2) 0.7813(2) 0.0239(8) Uani 1 1 d . . . H11G H 0.9028 1.0582 0.7787 0.029 Uiso 1 1 calc R . . H11H H 0.9898 0.9716 0.7706 0.029 Uiso 1 1 calc R . . C121 C 0.8805(4) 0.9650(2) 0.8773(2) 0.0205(7) Uani 1 1 d . . . C122 C 0.7606(4) 0.8985(2) 0.8914(2) 0.0223(7) Uani 1 1 d . . . H122 H 0.6783 0.8688 0.8398 0.027 Uiso 1 1 calc R . . C123 C 1.0019(4) 1.0122(2) 0.9547(2) 0.0193(7) Uani 1 1 d . . . C131 C 1.2427(4) 1.1268(2) 1.0192(2) 0.0235(8) Uani 1 1 d . . . H131 H 1.3255 1.1743 1.0110 0.028 Uiso 1 1 calc R . . C132 C 1.1279(4) 1.0835(2) 0.9443(2) 0.0223(7) Uani 1 1 d . . . H132 H 1.1316 1.1010 0.8842 0.027 Uiso 1 1 calc R . . N211 N 1.1561(3) 0.78728(18) 0.93814(18) 0.0195(6) Uani 1 1 d . . . N212 N 1.1314(3) 0.8011(2) 0.84648(19) 0.0233(6) Uani 1 1 d . . . C213 C 1.2589(4) 0.8636(2) 0.8405(2) 0.0253(8) Uani 1 1 d . . . C214 C 1.3628(4) 0.8879(2) 0.9268(2) 0.0273(8) Uani 1 1 d . . . H214 H 1.4613 0.9306 0.9409 0.033 Uiso 1 1 calc R . . C215 C 1.2961(4) 0.8386(2) 0.9873(2) 0.0250(8) Uani 1 1 d . . . C216 C 1.2777(5) 0.8957(3) 0.7498(3) 0.0412(10) Uani 1 1 d . . . H21A H 1.3426 0.8578 0.7256 0.062 Uiso 1 1 calc R . . H21B H 1.3296 0.9620 0.7580 0.062 Uiso 1 1 calc R . . H21C H 1.1733 0.8884 0.7060 0.062 Uiso 1 1 calc R . . C217 C 1.3547(5) 0.8349(3) 1.0886(3) 0.0403(10) Uani 1 1 d . . . H21D H 1.2697 0.8409 1.1184 0.060 Uiso 1 1 calc R . . H21E H 1.4447 0.8865 1.1130 0.060 Uiso 1 1 calc R . . H21F H 1.3886 0.7747 1.1013 0.060 Uiso 1 1 calc R . . C218 C 1.0446(4) 0.7178(2) 0.9692(2) 0.0209(7) Uani 1 1 d . . . H21G H 0.9372 0.7150 0.9284 0.025 Uiso 1 1 calc R . . H21H H 1.0426 0.7386 1.0326 0.025 Uiso 1 1 calc R . . C221 C 1.0834(4) 0.6205(2) 0.9694(2) 0.0194(7) Uani 1 1 d . . . C222 C 0.9825(4) 0.5461(2) 1.0004(2) 0.0177(7) Uani 1 1 d . . . C223 C 1.2094(4) 0.6009(2) 0.9406(2) 0.0236(8) Uani 1 1 d . . . H223 H 1.2763 0.6499 0.9206 0.028 Uiso 1 1 calc R . . C231 C 0.7571(4) 0.4901(2) 1.0601(2) 0.0244(8) Uani 1 1 d . . . H231 H 0.6685 0.5018 1.0807 0.029 Uiso 1 1 calc R . . C232 C 0.8507(4) 0.5623(2) 1.0315(2) 0.0219(7) Uani 1 1 d . . . H232 H 0.8268 0.6237 1.0326 0.026 Uiso 1 1 calc R . . N311 N 0.8349(3) 0.52586(19) 0.74803(19) 0.0217(6) Uani 1 1 d . . . N312 N 0.7756(3) 0.60485(19) 0.75771(19) 0.0222(6) Uani 1 1 d . . . C313 C 0.6446(4) 0.5767(2) 0.7860(2) 0.0248(8) Uani 1 1 d . . . C314 C 0.6198(4) 0.4797(2) 0.7930(2) 0.0266(8) Uani 1 1 d . . . H314 H 0.5350 0.4427 0.8115 0.032 Uiso 1 1 calc R . . C315 C 0.7419(4) 0.4485(2) 0.7680(2) 0.0233(8) Uani 1 1 d . . . C316 C 0.5493(4) 0.6454(3) 0.8081(3) 0.0334(9) Uani 1 1 d . . . H31A H 0.5766 0.6607 0.8752 0.050 Uiso 1 1 calc R . . H31B H 0.4363 0.6178 0.7863 0.050 Uiso 1 1 calc R . . H31C H 0.5721 0.7028 0.7773 0.050 Uiso 1 1 calc R . . C317 C 0.7806(4) 0.3536(2) 0.7610(3) 0.0323(9) Uani 1 1 d . . . H31D H 0.7688 0.3337 0.6960 0.048 Uiso 1 1 calc R . . H31E H 0.7085 0.3091 0.7863 0.048 Uiso 1 1 calc R . . H31F H 0.8900 0.3552 0.7963 0.048 Uiso 1 1 calc R . . C318 C 0.9660(4) 0.5281(2) 0.7053(2) 0.0213(7) Uani 1 1 d . . . H31G H 1.0258 0.4786 0.7291 0.026 Uiso 1 1 calc R . . H31H H 1.0386 0.5896 0.7231 0.026 Uiso 1 1 calc R . . C321 C 0.9117(4) 0.5131(2) 0.6008(2) 0.0195(7) Uani 1 1 d . . . C322 C 1.0249(4) 0.5060(2) 0.5492(2) 0.0175(7) Uani 1 1 d . . . C323 C 0.7554(4) 0.5083(2) 0.5550(2) 0.0218(7) Uani 1 1 d . . . H323 H 0.6797 0.5124 0.5895 0.026 Uiso 1 1 calc R . . C331 C 1.2936(4) 0.5026(2) 0.5415(2) 0.0232(8) Uani 1 1 d . . . H331 H 1.4019 0.5051 0.5719 0.028 Uiso 1 1 calc R . . C332 C 1.1881(4) 0.5097(2) 0.5927(2) 0.0217(7) Uani 1 1 d . . . H332 H 1.2237 0.5173 0.6583 0.026 Uiso 1 1 calc R . . N411 N 0.9997(4) 0.7383(2) 0.5990(2) 0.0414(9) Uani 1 1 d . . . C412 C 1.0546(4) 0.7330(2) 0.5378(3) 0.0300(8) Uani 1 1 d . . . C413 C 1.1260(4) 0.7253(3) 0.4617(3) 0.0319(9) Uani 1 1 d . . . H41A H 1.1821 0.7874 0.4530 0.048 Uiso 1 1 calc R . . H41B H 1.0433 0.7011 0.4052 0.048 Uiso 1 1 calc R . . H41C H 1.2010 0.6822 0.4752 0.048 Uiso 1 1 calc R . . S1 S 0.19389(11) 0.27184(7) 0.77293(7) 0.0309(2) Uani 1 1 d . . . F1 F 0.1887(3) 0.1998(2) 0.60891(18) 0.0643(8) Uani 1 1 d . . . F2 F 0.4206(3) 0.25090(19) 0.69487(18) 0.0548(7) Uani 1 1 d . . . F3 F 0.2850(3) 0.12175(17) 0.7217(2) 0.0638(8) Uani 1 1 d . . . O1 O 0.0408(3) 0.2130(2) 0.7644(2) 0.0516(8) Uani 1 1 d . . . O2 O 0.1870(3) 0.35993(17) 0.73436(18) 0.0331(6) Uani 1 1 d . . . O3 O 0.3078(3) 0.2754(2) 0.86054(18) 0.0436(7) Uani 1 1 d . . . C1 C 0.2763(5) 0.2092(3) 0.6963(3) 0.0413(10) Uani 1 1 d . . . N1S N 0.8294(9) 0.0404(5) 0.5063(5) 0.0504(19) Uiso 0.50 1 d P . . C1S C 0.9284(6) 0.0141(4) 0.5068(4) 0.0663(15) Uiso 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 0.02639(15) 0.02082(15) 0.02671(15) 0.00344(11) 0.00118(11) 0.00217(10) N111 0.0281(15) 0.0159(14) 0.0191(14) 0.0012(12) 0.0040(12) 0.0036(12) N112 0.0295(16) 0.0183(15) 0.0217(15) 0.0013(12) 0.0020(12) 0.0043(12) C113 0.0255(18) 0.0244(19) 0.0218(17) 0.0004(15) 0.0019(14) 0.0017(15) C114 0.0247(18) 0.035(2) 0.0218(18) 0.0044(16) 0.0059(15) 0.0079(16) C115 0.0276(18) 0.0252(19) 0.0184(17) 0.0064(14) 0.0094(14) 0.0093(15) C116 0.033(2) 0.029(2) 0.032(2) -0.0041(17) -0.0043(17) 0.0020(17) C117 0.043(2) 0.030(2) 0.028(2) 0.0011(17) 0.0081(17) 0.0188(18) C118 0.0282(19) 0.0193(18) 0.0215(17) 0.0013(14) 0.0025(15) 0.0031(15) C121 0.0259(18) 0.0179(17) 0.0202(17) 0.0003(14) 0.0059(14) 0.0111(14) C122 0.0243(18) 0.0206(18) 0.0190(17) -0.0022(14) 0.0003(14) 0.0045(14) C123 0.0217(17) 0.0160(17) 0.0220(17) -0.0006(14) 0.0066(14) 0.0076(13) C131 0.0223(17) 0.0208(18) 0.0260(18) 0.0013(15) 0.0059(14) 0.0013(14) C132 0.0291(18) 0.0173(17) 0.0224(17) 0.0048(14) 0.0091(15) 0.0049(14) N211 0.0232(14) 0.0178(14) 0.0185(14) 0.0013(12) 0.0065(11) 0.0048(12) N212 0.0230(15) 0.0263(16) 0.0212(15) 0.0048(12) 0.0064(12) 0.0045(12) C213 0.0250(18) 0.0210(18) 0.0320(19) 0.0056(15) 0.0109(15) 0.0041(15) C214 0.0208(18) 0.0209(19) 0.037(2) -0.0005(16) 0.0042(16) 0.0003(14) C215 0.0283(19) 0.0181(18) 0.0249(18) -0.0031(15) 0.0018(15) 0.0024(15) C216 0.039(2) 0.049(3) 0.035(2) 0.011(2) 0.0131(18) -0.001(2) C217 0.042(2) 0.041(2) 0.028(2) -0.0013(18) -0.0010(18) -0.0037(19) C218 0.0232(17) 0.0174(17) 0.0225(17) 0.0021(14) 0.0067(14) 0.0038(14) C221 0.0231(17) 0.0202(17) 0.0158(16) 0.0000(13) 0.0057(13) 0.0056(14) C222 0.0204(16) 0.0207(17) 0.0124(15) -0.0024(13) 0.0049(13) 0.0049(13) C223 0.0262(18) 0.0223(19) 0.0236(18) 0.0024(15) 0.0104(15) 0.0018(15) C231 0.0243(18) 0.0248(19) 0.0283(19) 0.0010(15) 0.0134(15) 0.0067(15) C232 0.0241(17) 0.0205(18) 0.0221(17) 0.0000(14) 0.0066(14) 0.0062(14) N311 0.0219(15) 0.0197(15) 0.0241(15) 0.0015(12) 0.0074(12) 0.0029(12) N312 0.0219(14) 0.0186(15) 0.0262(15) -0.0002(12) 0.0065(12) 0.0037(12) C313 0.0231(18) 0.0258(19) 0.0241(18) -0.0049(15) 0.0080(14) -0.0010(15) C314 0.0273(19) 0.0230(19) 0.0279(19) -0.0019(15) 0.0110(15) -0.0047(15) C315 0.0264(18) 0.0216(18) 0.0213(17) 0.0009(14) 0.0076(14) 0.0008(15) C316 0.029(2) 0.028(2) 0.043(2) -0.0083(18) 0.0140(17) -0.0010(16) C317 0.037(2) 0.023(2) 0.040(2) 0.0040(17) 0.0162(18) 0.0052(16) C318 0.0169(16) 0.0219(18) 0.0258(18) 0.0047(15) 0.0068(14) 0.0031(14) C321 0.0187(16) 0.0155(17) 0.0247(17) 0.0040(14) 0.0070(14) 0.0017(13) C322 0.0181(16) 0.0125(16) 0.0215(16) 0.0035(13) 0.0063(13) -0.0001(12) C323 0.0182(16) 0.0221(18) 0.0278(18) 0.0030(15) 0.0102(14) 0.0045(14) C331 0.0122(16) 0.0259(19) 0.0303(19) 0.0039(15) 0.0047(14) 0.0011(14) C332 0.0202(17) 0.0195(18) 0.0232(17) 0.0027(14) 0.0029(14) 0.0014(14) N411 0.054(2) 0.032(2) 0.040(2) 0.0017(16) 0.0184(18) 0.0041(16) C412 0.038(2) 0.0199(19) 0.033(2) 0.0028(16) 0.0112(18) 0.0040(16) C413 0.039(2) 0.028(2) 0.034(2) 0.0074(17) 0.0165(17) 0.0090(17) S1 0.0314(5) 0.0255(5) 0.0388(5) 0.0118(4) 0.0109(4) 0.0089(4) F1 0.0609(17) 0.079(2) 0.0454(15) -0.0235(14) -0.0073(13) 0.0293(15) F2 0.0381(14) 0.0654(18) 0.0634(17) -0.0112(14) 0.0181(12) 0.0123(13) F3 0.0639(17) 0.0346(15) 0.094(2) -0.0024(14) 0.0115(16) 0.0260(13) O1 0.0343(16) 0.0417(18) 0.083(2) 0.0296(17) 0.0179(15) 0.0092(13) O2 0.0429(15) 0.0220(13) 0.0399(15) 0.0056(12) 0.0163(12) 0.0121(11) O3 0.0493(17) 0.0489(18) 0.0347(15) 0.0112(14) 0.0062(13) 0.0201(14) C1 0.038(2) 0.032(2) 0.046(3) -0.006(2) -0.0061(19) 0.0101(19) _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 N212 2.254(3) . ? Ag1 N112 2.261(3) . ? Ag1 N312 2.271(3) . ? Ag1 N411 2.461(4) . ? N111 C115 1.355(4) . ? N111 N112 1.358(4) . ? N111 C118 1.455(4) . ? N112 C113 1.338(4) . ? C113 C114 1.389(5) . ? C113 C116 1.494(5) . ? C114 C115 1.373(5) . ? C114 H114 0.9500 . ? C115 C117 1.478(5) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C118 C121 1.514(4) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.369(5) . ? C121 C123 1.430(4) . ? C122 C131 1.405(5) 2_777 ? C122 H122 0.9500 . ? C123 C123 1.419(6) 2_777 ? C123 C132 1.427(4) . ? C131 C132 1.362(4) . ? C131 C122 1.405(5) 2_777 ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? N211 C215 1.352(4) . ? N211 N212 1.362(4) . ? N211 C218 1.457(4) . ? N212 C213 1.344(4) . ? C213 C214 1.382(5) . ? C213 C216 1.488(5) . ? C214 C215 1.358(5) . ? C214 H214 0.9500 . ? C215 C217 1.482(5) . ? C216 H21A 0.9800 . ? C216 H21B 0.9800 . ? C216 H21C 0.9800 . ? C217 H21D 0.9800 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C218 C221 1.506(5) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C221 C223 1.361(5) . ? C221 C222 1.444(4) . ? C222 C232 1.411(4) . ? C222 C222 1.423(6) 2_767 ? C223 C231 1.400(5) 2_767 ? C223 H223 0.9500 . ? C231 C232 1.369(5) . ? C231 C223 1.400(5) 2_767 ? C231 H231 0.9500 . ? C232 H232 0.9500 . ? N311 N312 1.356(4) . ? N311 C315 1.360(4) . ? N311 C318 1.454(4) . ? N312 C313 1.336(4) . ? C313 C314 1.396(5) . ? C313 C316 1.489(5) . ? C314 C315 1.367(5) . ? C314 H314 0.9500 . ? C315 C317 1.479(5) . ? C316 H31A 0.9800 . ? C316 H31B 0.9800 . ? C316 H31C 0.9800 . ? C317 H31D 0.9800 . ? C317 H31E 0.9800 . ? C317 H31F 0.9800 . ? C318 C321 1.514(4) . ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? C321 C323 1.375(4) . ? C321 C322 1.422(4) . ? C322 C322 1.423(6) 2_766 ? C322 C332 1.424(4) . ? C323 C331 1.396(5) 2_766 ? C323 H323 0.9500 . ? C331 C332 1.359(5) . ? C331 C323 1.396(5) 2_766 ? C331 H331 0.9500 . ? C332 H332 0.9500 . ? N411 C412 1.143(5) . ? C412 C413 1.441(5) . ? C413 H41A 0.9800 . ? C413 H41B 0.9800 . ? C413 H41C 0.9800 . ? S1 O2 1.424(3) . ? S1 O3 1.438(3) . ? S1 O1 1.446(3) . ? S1 C1 1.798(4) . ? F1 C1 1.335(4) . ? F2 C1 1.323(5) . ? F3 C1 1.346(5) . ? N1S C1S 1.014(8) . ? C1S C1S 1.455(11) 2_756 ? 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 N212 Ag1 N112 120.76(10) . . ? N212 Ag1 N312 113.79(10) . . ? N112 Ag1 N312 116.61(10) . . ? N212 Ag1 N411 100.49(11) . . ? N112 Ag1 N411 91.99(11) . . ? N312 Ag1 N411 107.86(11) . . ? C115 N111 N112 111.4(3) . . ? C115 N111 C118 128.4(3) . . ? N112 N111 C118 120.1(3) . . ? C113 N112 N111 105.9(3) . . ? C113 N112 Ag1 126.2(2) . . ? N111 N112 Ag1 127.7(2) . . ? N112 C113 C114 109.8(3) . . ? N112 C113 C116 120.2(3) . . ? C114 C113 C116 130.1(3) . . ? C115 C114 C113 106.9(3) . . ? C115 C114 H114 126.6 . . ? C113 C114 H114 126.6 . . ? N111 C115 C114 106.0(3) . . ? N111 C115 C117 123.2(3) . . ? C114 C115 C117 130.7(3) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C115 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? N111 C118 C121 114.4(3) . . ? N111 C118 H11G 108.7 . . ? C121 C118 H11G 108.7 . . ? N111 C118 H11H 108.7 . . ? C121 C118 H11H 108.7 . . ? H11G C118 H11H 107.6 . . ? C122 C121 C123 119.8(3) . . ? C122 C121 C118 122.2(3) . . ? C123 C121 C118 118.0(3) . . ? C121 C122 C131 121.2(3) . 2_777 ? C121 C122 H122 119.4 . . ? C131 C122 H122 119.4 2_777 . ? C123 C123 C132 118.5(4) 2_777 . ? C123 C123 C121 119.3(4) 2_777 . ? C132 C123 C121 122.2(3) . . ? C132 C131 C122 120.2(3) . 2_777 ? C132 C131 H131 119.9 . . ? C122 C131 H131 119.9 2_777 . ? C131 C132 C123 121.0(3) . . ? C131 C132 H132 119.5 . . ? C123 C132 H132 119.5 . . ? C215 N211 N212 110.9(3) . . ? C215 N211 C218 129.0(3) . . ? N212 N211 C218 119.8(3) . . ? C213 N212 N211 105.0(3) . . ? C213 N212 Ag1 129.0(2) . . ? N211 N212 Ag1 124.94(19) . . ? N212 C213 C214 110.6(3) . . ? N212 C213 C216 121.3(3) . . ? C214 C213 C216 128.0(3) . . ? C215 C214 C213 106.3(3) . . ? C215 C214 H214 126.9 . . ? C213 C214 H214 126.9 . . ? N211 C215 C214 107.3(3) . . ? N211 C215 C217 122.2(3) . . ? C214 C215 C217 130.5(3) . . ? C213 C216 H21A 109.5 . . ? C213 C216 H21B 109.5 . . ? H21A C216 H21B 109.5 . . ? C213 C216 H21C 109.5 . . ? H21A C216 H21C 109.5 . . ? H21B C216 H21C 109.5 . . ? C215 C217 H21D 109.5 . . ? C215 C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C215 C217 H21F 109.5 . . ? H21D C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? N211 C218 C221 113.8(3) . . ? N211 C218 H21G 108.8 . . ? C221 C218 H21G 108.8 . . ? N211 C218 H21H 108.8 . . ? C221 C218 H21H 108.8 . . ? H21G C218 H21H 107.7 . . ? C223 C221 C222 119.3(3) . . ? C223 C221 C218 122.0(3) . . ? C222 C221 C218 118.7(3) . . ? C232 C222 C222 119.1(4) . 2_767 ? C232 C222 C221 121.9(3) . . ? C222 C222 C221 119.0(4) 2_767 . ? C221 C223 C231 121.5(3) . 2_767 ? C221 C223 H223 119.3 . . ? C231 C223 H223 119.3 2_767 . ? C232 C231 C223 120.7(3) . 2_767 ? C232 C231 H231 119.6 . . ? C223 C231 H231 119.6 2_767 . ? C231 C232 C222 120.4(3) . . ? C231 C232 H232 119.8 . . ? C222 C232 H232 119.8 . . ? N312 N311 C315 111.7(3) . . ? N312 N311 C318 120.1(3) . . ? C315 N311 C318 127.2(3) . . ? C313 N312 N311 105.3(3) . . ? C313 N312 Ag1 131.6(2) . . ? N311 N312 Ag1 123.0(2) . . ? N312 C313 C314 110.5(3) . . ? N312 C313 C316 121.1(3) . . ? C314 C313 C316 128.5(3) . . ? C315 C314 C313 106.3(3) . . ? C315 C314 H314 126.8 . . ? C313 C314 H314 126.8 . . ? N311 C315 C314 106.2(3) . . ? N311 C315 C317 121.9(3) . . ? C314 C315 C317 131.9(3) . . ? C313 C316 H31A 109.5 . . ? C313 C316 H31B 109.5 . . ? H31A C316 H31B 109.5 . . ? C313 C316 H31C 109.5 . . ? H31A C316 H31C 109.5 . . ? H31B C316 H31C 109.5 . . ? C315 C317 H31D 109.5 . . ? C315 C317 H31E 109.5 . . ? H31D C317 H31E 109.5 . . ? C315 C317 H31F 109.5 . . ? H31D C317 H31F 109.5 . . ? H31E C317 H31F 109.5 . . ? N311 C318 C321 112.6(3) . . ? N311 C318 H31G 109.1 . . ? C321 C318 H31G 109.1 . . ? N311 C318 H31H 109.1 . . ? C321 C318 H31H 109.1 . . ? H31G C318 H31H 107.8 . . ? C323 C321 C322 119.6(3) . . ? C323 C321 C318 121.0(3) . . ? C322 C321 C318 119.4(3) . . ? C321 C322 C322 119.6(4) . 2_766 ? C321 C322 C332 122.2(3) . . ? C322 C322 C332 118.2(4) 2_766 . ? C321 C323 C331 120.9(3) . 2_766 ? C321 C323 H323 119.5 . . ? C331 C323 H323 119.5 2_766 . ? C332 C331 C323 120.8(3) . 2_766 ? C332 C331 H331 119.6 . . ? C323 C331 H331 119.6 2_766 . ? C331 C332 C322 120.8(3) . . ? C331 C332 H332 119.6 . . ? C322 C332 H332 119.6 . . ? C412 N411 Ag1 175.7(3) . . ? N411 C412 C413 178.9(4) . . ? C412 C413 H41A 109.5 . . ? C412 C413 H41B 109.5 . . ? H41A C413 H41B 109.5 . . ? C412 C413 H41C 109.5 . . ? H41A C413 H41C 109.5 . . ? H41B C413 H41C 109.5 . . ? O2 S1 O3 115.20(17) . . ? O2 S1 O1 114.29(17) . . ? O3 S1 O1 115.99(18) . . ? O2 S1 C1 103.34(18) . . ? O3 S1 C1 102.61(18) . . ? O1 S1 C1 102.79(19) . . ? F2 C1 F1 106.6(4) . . ? F2 C1 F3 107.3(3) . . ? F1 C1 F3 106.6(3) . . ? F2 C1 S1 112.8(3) . . ? F1 C1 S1 112.4(3) . . ? F3 C1 S1 110.7(3) . . ? N1S C1S C1S 169.7(9) . 2_756 ? 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 C115 N111 N112 C113 -0.6(4) . . . . ? C118 N111 N112 C113 -177.6(3) . . . . ? C115 N111 N112 Ag1 -175.8(2) . . . . ? C118 N111 N112 Ag1 7.2(4) . . . . ? N212 Ag1 N112 C113 173.5(3) . . . . ? N312 Ag1 N112 C113 -41.1(3) . . . . ? N411 Ag1 N112 C113 70.0(3) . . . . ? N212 Ag1 N112 N111 -12.2(3) . . . . ? N312 Ag1 N112 N111 133.2(3) . . . . ? N411 Ag1 N112 N111 -115.7(3) . . . . ? N111 N112 C113 C114 0.4(4) . . . . ? Ag1 N112 C113 C114 175.7(2) . . . . ? N111 N112 C113 C116 179.8(3) . . . . ? Ag1 N112 C113 C116 -4.9(5) . . . . ? N112 C113 C114 C115 0.0(4) . . . . ? C116 C113 C114 C115 -179.4(4) . . . . ? N112 N111 C115 C114 0.6(4) . . . . ? C118 N111 C115 C114 177.2(3) . . . . ? N112 N111 C115 C117 -177.7(3) . . . . ? C118 N111 C115 C117 -1.0(5) . . . . ? C113 C114 C115 N111 -0.3(4) . . . . ? C113 C114 C115 C117 177.7(4) . . . . ? C115 N111 C118 C121 104.7(4) . . . . ? N112 N111 C118 C121 -78.9(4) . . . . ? N111 C118 C121 C122 6.1(5) . . . . ? N111 C118 C121 C123 -175.6(3) . . . . ? C123 C121 C122 C131 -2.1(5) . . . 2_777 ? C118 C121 C122 C131 176.2(3) . . . 2_777 ? C122 C121 C123 C123 1.3(6) . . . 2_777 ? C118 C121 C123 C123 -177.1(4) . . . 2_777 ? C122 C121 C123 C132 -178.7(3) . . . . ? C118 C121 C123 C132 3.0(5) . . . . ? C122 C131 C132 C123 0.3(5) 2_777 . . . ? C123 C123 C132 C131 0.5(6) 2_777 . . . ? C121 C123 C132 C131 -179.5(3) . . . . ? C215 N211 N212 C213 -1.0(4) . . . . ? C218 N211 N212 C213 -175.8(3) . . . . ? C215 N211 N212 Ag1 -170.1(2) . . . . ? C218 N211 N212 Ag1 15.1(4) . . . . ? N112 Ag1 N212 C213 -59.4(3) . . . . ? N312 Ag1 N212 C213 154.3(3) . . . . ? N411 Ag1 N212 C213 39.3(3) . . . . ? N112 Ag1 N212 N211 107.0(3) . . . . ? N312 Ag1 N212 N211 -39.3(3) . . . . ? N411 Ag1 N212 N211 -154.3(2) . . . . ? N211 N212 C213 C214 0.6(4) . . . . ? Ag1 N212 C213 C214 169.1(2) . . . . ? N211 N212 C213 C216 178.7(3) . . . . ? Ag1 N212 C213 C216 -12.8(5) . . . . ? N212 C213 C214 C215 -0.1(4) . . . . ? C216 C213 C214 C215 -178.0(4) . . . . ? N212 N211 C215 C214 0.9(4) . . . . ? C218 N211 C215 C214 175.1(3) . . . . ? N212 N211 C215 C217 -178.4(3) . . . . ? C218 N211 C215 C217 -4.1(6) . . . . ? C213 C214 C215 N211 -0.5(4) . . . . ? C213 C214 C215 C217 178.7(4) . . . . ? C215 N211 C218 C221 -84.8(4) . . . . ? N212 N211 C218 C221 89.0(3) . . . . ? N211 C218 C221 C223 -1.5(4) . . . . ? N211 C218 C221 C222 178.9(3) . . . . ? C223 C221 C222 C232 179.6(3) . . . . ? C218 C221 C222 C232 -0.9(4) . . . . ? C223 C221 C222 C222 -0.3(5) . . . 2_767 ? C218 C221 C222 C222 179.3(3) . . . 2_767 ? C222 C221 C223 C231 0.4(5) . . . 2_767 ? C218 C221 C223 C231 -179.1(3) . . . 2_767 ? C223 C231 C232 C222 0.2(5) 2_767 . . . ? C222 C222 C232 C231 -0.4(5) 2_767 . . . ? C221 C222 C232 C231 179.8(3) . . . . ? C315 N311 N312 C313 1.2(4) . . . . ? C318 N311 N312 C313 171.2(3) . . . . ? C315 N311 N312 Ag1 176.6(2) . . . . ? C318 N311 N312 Ag1 -13.4(4) . . . . ? N212 Ag1 N312 C313 107.6(3) . . . . ? N112 Ag1 N312 C313 -40.2(3) . . . . ? N411 Ag1 N312 C313 -141.8(3) . . . . ? N212 Ag1 N312 N311 -66.5(3) . . . . ? N112 Ag1 N312 N311 145.8(2) . . . . ? N411 Ag1 N312 N311 44.1(3) . . . . ? N311 N312 C313 C314 -0.9(4) . . . . ? Ag1 N312 C313 C314 -175.7(2) . . . . ? N311 N312 C313 C316 177.5(3) . . . . ? Ag1 N312 C313 C316 2.6(5) . . . . ? N312 C313 C314 C315 0.2(4) . . . . ? C316 C313 C314 C315 -178.0(3) . . . . ? N312 N311 C315 C314 -1.1(4) . . . . ? C318 N311 C315 C314 -170.2(3) . . . . ? N312 N311 C315 C317 179.0(3) . . . . ? C318 N311 C315 C317 9.9(5) . . . . ? C313 C314 C315 N311 0.5(4) . . . . ? C313 C314 C315 C317 -179.7(4) . . . . ? N312 N311 C318 C321 -85.3(3) . . . . ? C315 N311 C318 C321 83.0(4) . . . . ? N311 C318 C321 C323 6.3(4) . . . . ? N311 C318 C321 C322 -175.1(3) . . . . ? C323 C321 C322 C322 0.0(5) . . . 2_766 ? C318 C321 C322 C322 -178.7(3) . . . 2_766 ? C323 C321 C322 C332 -179.4(3) . . . . ? C318 C321 C322 C332 1.9(5) . . . . ? C322 C321 C323 C331 -0.6(5) . . . 2_766 ? C318 C321 C323 C331 178.0(3) . . . 2_766 ? C323 C331 C332 C322 0.1(5) 2_766 . . . ? C321 C322 C332 C331 179.9(3) . . . . ? C322 C322 C332 C331 0.5(5) 2_766 . . . ? N212 Ag1 N411 C412 16(4) . . . . ? N112 Ag1 N411 C412 138(4) . . . . ? N312 Ag1 N411 C412 -104(4) . . . . ? Ag1 N411 C412 C413 33(26) . . . . ? O2 S1 C1 F2 62.0(3) . . . . ? O3 S1 C1 F2 -58.0(3) . . . . ? O1 S1 C1 F2 -178.8(3) . . . . ? O2 S1 C1 F1 -58.5(3) . . . . ? O3 S1 C1 F1 -178.6(3) . . . . ? O1 S1 C1 F1 60.6(3) . . . . ? O2 S1 C1 F3 -177.6(3) . . . . ? O3 S1 C1 F3 62.3(3) . . . . ? O1 S1 C1 F3 -58.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.079 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.087 #===END data_imw1173p21c _database_code_depnum_ccdc_archive 'CCDC 797104' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H90 Ag2 N20 O6' _chemical_formula_weight 1619.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.899(10) _cell_length_b 11.673(6) _cell_length_c 18.918(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.356(12) _cell_angle_gamma 90.00 _cell_volume 3692(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7028 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.41 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8896 _exptl_absorpt_correction_T_max 0.9940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34388 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.85 _reflns_number_total 8725 _reflns_number_gt 6245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. All hydrogens were added in geometrically calculated positions. The free nitrate counter ion (O31 O32 O33 N34) is disordered over two sites and has been left isotropic. The model was improved by the application of geometric and displacement restraints. Displacement restraints were also used to improved the appearance of the free acetonitrile solvent molecules (N11S C12S C13S, N21S C22S C23S). 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^)+(0.0385P)^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 8725 _refine_ls_number_parameters 484 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.023 _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 0.779169(11) 0.278380(17) 0.513271(10) 0.01970(6) Uani 1 1 d . . . N111 N 0.70352(11) 0.45280(17) 0.39006(10) 0.0153(4) Uani 1 1 d . . . N112 N 0.77173(11) 0.42614(17) 0.43346(10) 0.0168(4) Uani 1 1 d . . . C113 C 0.82843(14) 0.4867(2) 0.40859(13) 0.0174(5) Uani 1 1 d . . . C114 C 0.79648(14) 0.5525(2) 0.35073(13) 0.0184(5) Uani 1 1 d . . . H114 H 0.8246 0.6031 0.3239 0.022 Uiso 1 1 calc R . . C115 C 0.71625(14) 0.5301(2) 0.33997(12) 0.0174(5) Uani 1 1 d . . . C116 C 0.91309(14) 0.4782(2) 0.44324(14) 0.0234(6) Uani 1 1 d . . . H11A H 0.9182 0.4159 0.4783 0.035 Uiso 1 1 calc R . . H11B H 0.9293 0.5505 0.4673 0.035 Uiso 1 1 calc R . . H11C H 0.9475 0.4624 0.4069 0.035 Uiso 1 1 calc R . . C117 C 0.65091(14) 0.5749(2) 0.28718(13) 0.0243(6) Uani 1 1 d . . . H11F H 0.6141 0.6198 0.3117 0.036 Uiso 1 1 calc R . . H11D H 0.6219 0.5108 0.2619 0.036 Uiso 1 1 calc R . . H11E H 0.6732 0.6237 0.2528 0.036 Uiso 1 1 calc R . . C118 C 0.62788(13) 0.4121(2) 0.40656(12) 0.0161(5) Uani 1 1 d . . . H11G H 0.6350 0.3341 0.4271 0.019 Uiso 1 1 calc R . . H11H H 0.5895 0.4070 0.3619 0.019 Uiso 1 1 calc R . . C121 C 0.59366(13) 0.4888(2) 0.45850(12) 0.0147(5) Uani 1 1 d . . . C122 C 0.63437(14) 0.5807(2) 0.48839(13) 0.0176(5) Uani 1 1 d . . . H122 H 0.6863 0.5964 0.4773 0.021 Uiso 1 1 calc R . . C123 C 0.51661(13) 0.4634(2) 0.47621(12) 0.0141(5) Uani 1 1 d . . . C131 C 0.39856(14) 0.3469(2) 0.46472(13) 0.0198(5) Uani 1 1 d . . . H131 H 0.3690 0.2826 0.4446 0.024 Uiso 1 1 calc R . . C132 C 0.47241(14) 0.3680(2) 0.44785(12) 0.0174(5) Uani 1 1 d . . . H132 H 0.4945 0.3176 0.4165 0.021 Uiso 1 1 calc R . . N211 N 0.74172(11) 0.01760(17) 0.45228(11) 0.0181(4) Uani 1 1 d . . . N212 N 0.78380(11) 0.11589(17) 0.44954(10) 0.0177(4) Uani 1 1 d . . . C213 C 0.82596(14) 0.1010(2) 0.39607(13) 0.0196(5) Uani 1 1 d . . . C214 C 0.81007(14) -0.0051(2) 0.36475(14) 0.0232(6) Uani 1 1 d . . . H214 H 0.8323 -0.0360 0.3256 0.028 Uiso 1 1 calc R . . C215 C 0.75616(14) -0.0564(2) 0.40136(14) 0.0228(6) Uani 1 1 d . . . C216 C 0.88211(15) 0.1901(2) 0.37811(14) 0.0251(6) Uani 1 1 d . . . H21A H 0.8551 0.2646 0.3743 0.038 Uiso 1 1 calc R . . H21B H 0.8998 0.1713 0.3324 0.038 Uiso 1 1 calc R . . H21C H 0.9285 0.1934 0.4157 0.038 Uiso 1 1 calc R . . C217 C 0.71794(17) -0.1704(2) 0.39315(17) 0.0362(7) Uani 1 1 d . . . H21D H 0.7312 -0.2138 0.4376 0.054 Uiso 1 1 calc R . . H21E H 0.7375 -0.2118 0.3541 0.054 Uiso 1 1 calc R . . H21F H 0.6598 -0.1612 0.3823 0.054 Uiso 1 1 calc R . . C218 C 0.68727(13) 0.0027(2) 0.50366(13) 0.0195(5) Uani 1 1 d . . . H21G H 0.7021 0.0569 0.5437 0.023 Uiso 1 1 calc R . . H21H H 0.6933 -0.0759 0.5233 0.023 Uiso 1 1 calc R . . C221 C 0.60080(14) 0.0219(2) 0.47293(13) 0.0174(5) Uani 1 1 d . . . C222 C 0.54074(13) -0.0085(2) 0.51448(13) 0.0162(5) Uani 1 1 d . . . C231 C 0.55870(14) -0.0547(2) 0.58353(13) 0.0179(5) Uani 1 1 d . . . H231 H 0.6130 -0.0656 0.6037 0.022 Uiso 1 1 calc R . . C232 C 0.49993(14) -0.0840(2) 0.62190(13) 0.0201(5) Uani 1 1 d . . . H232 H 0.5134 -0.1157 0.6683 0.024 Uiso 1 1 calc R . . C233 C 0.41958(14) -0.0677(2) 0.59336(13) 0.0188(5) Uani 1 1 d . . . H233 H 0.3788 -0.0888 0.6206 0.023 Uiso 1 1 calc R . . N311 N 0.91925(11) 0.24048(17) 0.64609(10) 0.0174(4) Uani 1 1 d . . . N312 N 0.87273(12) 0.32091(18) 0.60867(10) 0.0184(4) Uani 1 1 d . . . C313 C 0.89000(14) 0.4182(2) 0.64342(13) 0.0189(5) Uani 1 1 d . . . C314 C 0.94782(15) 0.3995(2) 0.70213(13) 0.0220(6) Uani 1 1 d . . . H314 H 0.9706 0.4554 0.7356 0.026 Uiso 1 1 calc R . . C315 C 0.96569(14) 0.2864(2) 0.70270(12) 0.0202(5) Uani 1 1 d . . . C316 C 0.84993(16) 0.5266(2) 0.61787(14) 0.0263(6) Uani 1 1 d . . . H31A H 0.8881 0.5761 0.5980 0.039 Uiso 1 1 calc R . . H31B H 0.8305 0.5656 0.6579 0.039 Uiso 1 1 calc R . . H31C H 0.8047 0.5096 0.5808 0.039 Uiso 1 1 calc R . . C317 C 1.02141(16) 0.2176(2) 0.75272(15) 0.0315(6) Uani 1 1 d . . . H31D H 0.9914 0.1595 0.7752 0.047 Uiso 1 1 calc R . . H31E H 1.0497 0.2677 0.7896 0.047 Uiso 1 1 calc R . . H31F H 1.0602 0.1799 0.7266 0.047 Uiso 1 1 calc R . . C318 C 0.91941(14) 0.1257(2) 0.61856(13) 0.0187(5) Uani 1 1 d . . . H31G H 0.8646 0.1056 0.5959 0.022 Uiso 1 1 calc R . . H31H H 0.9348 0.0720 0.6587 0.022 Uiso 1 1 calc R . . C321 C 0.97626(14) 0.1109(2) 0.56438(13) 0.0181(5) Uani 1 1 d . . . C322 C 1.02851(14) 0.1949(2) 0.55217(13) 0.0213(6) Uani 1 1 d . . . H322 H 1.0301 0.2644 0.5784 0.026 Uiso 1 1 calc R . . C323 C 1.07993(14) 0.1797(2) 0.50132(13) 0.0203(5) Uani 1 1 d . . . H323 H 1.1160 0.2392 0.4935 0.024 Uiso 1 1 calc R . . C324 C 1.07910(14) 0.0821(2) 0.46332(13) 0.0190(5) Uani 1 1 d . . . H324 H 1.1144 0.0733 0.4290 0.023 Uiso 1 1 calc R . . C325 C 1.02610(14) -0.0069(2) 0.47432(13) 0.0168(5) Uani 1 1 d . . . N411 N 0.66007(13) 0.27097(19) 0.56993(11) 0.0256(5) Uani 1 1 d . . . C412 C 0.60202(15) 0.2617(2) 0.59197(13) 0.0212(5) Uani 1 1 d . . . C413 C 0.52758(15) 0.2508(2) 0.62092(15) 0.0286(6) Uani 1 1 d . . . H41A H 0.5391 0.2352 0.6723 0.043 Uiso 1 1 calc R . . H41B H 0.4962 0.1876 0.5970 0.043 Uiso 1 1 calc R . . H41C H 0.4971 0.3223 0.6130 0.043 Uiso 1 1 calc R . . N11S N 0.65327(17) 0.2298(2) 0.27891(13) 0.0412(6) Uani 1 1 d . . . C12S C 0.70187(17) 0.2747(3) 0.25474(14) 0.0287(6) Uani 1 1 d . . . C13S C 0.76314(17) 0.3314(3) 0.22163(16) 0.0394(8) Uani 1 1 d . . . H13A H 0.7837 0.2786 0.1884 0.059 Uiso 1 1 calc R . . H13B H 0.8069 0.3550 0.2585 0.059 Uiso 1 1 calc R . . H13C H 0.7403 0.3991 0.1955 0.059 Uiso 1 1 calc R . . N21S N 0.46805(17) 0.4018(3) 0.25997(15) 0.0603(9) Uani 1 1 d . . . C22S C 0.40978(18) 0.4296(3) 0.27659(15) 0.0374(7) Uani 1 1 d . . . C23S C 0.33518(17) 0.4652(3) 0.29794(17) 0.0377(7) Uani 1 1 d . . . H23A H 0.3025 0.3976 0.3041 0.057 Uiso 1 1 calc R . . H23B H 0.3065 0.5149 0.2611 0.057 Uiso 1 1 calc R . . H23C H 0.3458 0.5072 0.3432 0.057 Uiso 1 1 calc R . . O31X O 0.7981(3) 0.9233(3) 0.6657(2) 0.0298(11) Uiso 0.665(11) 1 d PDU A 1 O32X O 0.7789(3) 0.7567(3) 0.7107(2) 0.0295(11) Uiso 0.665(11) 1 d PDU A 1 O33X O 0.7689(2) 0.7776(3) 0.59747(19) 0.0240(10) Uiso 0.665(11) 1 d PDU A 1 N34X N 0.7814(3) 0.8204(4) 0.6580(3) 0.0216(11) Uiso 0.665(11) 1 d PDU A 1 O31Y O 0.8324(6) 0.9086(6) 0.6830(4) 0.032(2) Uiso 0.335(11) 1 d PDU A 2 O32Y O 0.7966(5) 0.7558(6) 0.7245(4) 0.0203(19) Uiso 0.335(11) 1 d PDU A 2 O33Y O 0.7537(7) 0.7950(10) 0.6153(7) 0.072(3) Uiso 0.335(11) 1 d PDU A 2 N34Y N 0.7947(6) 0.8199(7) 0.6755(5) 0.023(2) Uiso 0.335(11) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02188(10) 0.01840(11) 0.01917(10) 0.00083(8) 0.00424(7) -0.00069(8) N111 0.0125(9) 0.0180(11) 0.0163(10) -0.0007(8) 0.0046(8) -0.0002(8) N112 0.0145(10) 0.0176(11) 0.0184(10) 0.0014(9) 0.0031(8) 0.0016(8) C113 0.0161(12) 0.0174(13) 0.0197(13) -0.0009(10) 0.0059(10) 0.0016(10) C114 0.0187(12) 0.0186(13) 0.0194(13) 0.0009(10) 0.0076(10) -0.0022(10) C115 0.0216(12) 0.0182(13) 0.0137(12) 0.0004(10) 0.0065(10) -0.0002(10) C116 0.0201(13) 0.0245(15) 0.0256(14) 0.0032(11) 0.0033(11) -0.0027(11) C117 0.0222(13) 0.0306(16) 0.0208(13) 0.0050(12) 0.0049(10) 0.0006(12) C118 0.0138(11) 0.0173(13) 0.0178(12) 0.0002(10) 0.0039(9) -0.0023(10) C121 0.0147(11) 0.0151(13) 0.0147(12) 0.0026(10) 0.0030(9) 0.0018(9) C122 0.0145(11) 0.0196(13) 0.0196(13) 0.0037(10) 0.0060(10) -0.0008(10) C123 0.0155(11) 0.0138(13) 0.0131(12) 0.0020(9) 0.0021(9) 0.0010(9) C131 0.0185(12) 0.0191(14) 0.0223(13) -0.0014(11) 0.0043(10) -0.0027(10) C132 0.0202(12) 0.0166(13) 0.0160(12) -0.0017(10) 0.0048(10) -0.0005(10) N211 0.0165(10) 0.0161(11) 0.0226(11) -0.0014(9) 0.0056(9) -0.0031(8) N212 0.0148(10) 0.0168(11) 0.0222(11) 0.0000(9) 0.0051(8) -0.0021(8) C213 0.0166(12) 0.0209(14) 0.0219(13) 0.0005(11) 0.0045(10) 0.0022(10) C214 0.0209(13) 0.0259(15) 0.0234(14) -0.0031(11) 0.0056(11) 0.0033(11) C215 0.0187(13) 0.0198(14) 0.0301(15) -0.0058(11) 0.0041(11) 0.0024(11) C216 0.0246(13) 0.0240(15) 0.0298(15) 0.0012(11) 0.0142(11) -0.0012(11) C217 0.0322(15) 0.0218(15) 0.057(2) -0.0118(14) 0.0136(14) -0.0067(13) C218 0.0161(12) 0.0215(14) 0.0219(13) 0.0036(11) 0.0065(10) -0.0023(10) C221 0.0193(12) 0.0115(12) 0.0223(13) -0.0029(10) 0.0063(10) -0.0001(10) C222 0.0180(12) 0.0117(12) 0.0197(12) -0.0036(10) 0.0054(10) -0.0020(10) C231 0.0183(12) 0.0149(13) 0.0201(13) -0.0029(10) 0.0012(10) 0.0008(10) C232 0.0246(13) 0.0196(14) 0.0164(12) 0.0018(10) 0.0044(10) 0.0001(11) C233 0.0205(12) 0.0170(13) 0.0207(13) -0.0008(10) 0.0089(10) -0.0016(10) N311 0.0200(10) 0.0147(11) 0.0183(10) -0.0002(8) 0.0055(8) 0.0030(8) N312 0.0202(10) 0.0175(11) 0.0182(10) 0.0011(9) 0.0050(8) 0.0031(9) C313 0.0242(13) 0.0136(13) 0.0205(13) -0.0012(10) 0.0081(10) -0.0009(10) C314 0.0277(13) 0.0170(14) 0.0214(14) -0.0038(11) 0.0036(11) -0.0016(11) C315 0.0202(12) 0.0242(14) 0.0168(12) -0.0003(11) 0.0046(9) 0.0010(11) C316 0.0318(15) 0.0201(14) 0.0265(15) -0.0006(11) 0.0027(12) 0.0055(12) C317 0.0342(15) 0.0296(16) 0.0286(15) 0.0000(13) -0.0021(12) 0.0072(13) C318 0.0240(13) 0.0126(12) 0.0206(13) -0.0023(10) 0.0073(10) 0.0018(10) C321 0.0170(12) 0.0184(13) 0.0197(13) 0.0032(10) 0.0054(10) 0.0042(10) C322 0.0234(13) 0.0164(14) 0.0252(13) -0.0029(10) 0.0069(11) 0.0011(10) C323 0.0214(12) 0.0154(13) 0.0253(14) 0.0016(11) 0.0069(10) -0.0028(10) C324 0.0190(12) 0.0176(13) 0.0213(13) 0.0019(10) 0.0068(10) 0.0013(10) C325 0.0177(12) 0.0140(13) 0.0192(13) 0.0002(10) 0.0048(10) 0.0023(10) N411 0.0253(11) 0.0280(13) 0.0248(12) 0.0021(10) 0.0075(9) 0.0037(10) C412 0.0250(13) 0.0208(14) 0.0183(12) 0.0040(10) 0.0044(10) 0.0047(11) C413 0.0215(13) 0.0364(17) 0.0298(15) 0.0053(12) 0.0101(11) 0.0048(12) N11S 0.0567(17) 0.0384(16) 0.0312(14) 0.0003(12) 0.0155(13) 0.0019(14) C12S 0.0361(15) 0.0300(16) 0.0205(13) -0.0040(13) 0.0053(12) 0.0078(14) C13S 0.0366(17) 0.049(2) 0.0339(17) -0.0137(15) 0.0094(14) -0.0065(15) N21S 0.0430(17) 0.105(3) 0.0325(16) 0.0068(17) 0.0044(13) 0.0076(18) C22S 0.0335(17) 0.053(2) 0.0250(16) 0.0082(14) 0.0000(13) -0.0029(15) C23S 0.0327(16) 0.0323(18) 0.0464(19) 0.0072(15) 0.0001(14) -0.0010(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 N212 2.255(2) . ? Ag1 N312 2.275(2) . ? Ag1 N112 2.284(2) . ? Ag1 N411 2.415(2) . ? N111 C115 1.349(3) . ? N111 N112 1.351(3) . ? N111 C118 1.440(3) . ? N112 C113 1.331(3) . ? C113 C114 1.381(3) . ? C113 C116 1.488(3) . ? C114 C115 1.367(3) . ? C114 H114 0.9500 . ? C115 C117 1.473(3) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11F 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C118 C121 1.505(3) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.353(3) . ? C121 C123 1.422(3) . ? C122 C131 1.398(3) 3_666 ? C122 H122 0.9500 . ? C123 C132 1.404(3) . ? C123 C123 1.414(4) 3_666 ? C131 C132 1.355(3) . ? C131 C122 1.398(3) 3_666 ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? N211 C215 1.343(3) . ? N211 N212 1.355(3) . ? N211 C218 1.443(3) . ? N212 C213 1.330(3) . ? C213 C214 1.382(4) . ? C213 C216 1.480(3) . ? C214 C215 1.361(4) . ? C214 H214 0.9500 . ? C215 C217 1.477(4) . ? C216 H21A 0.9800 . ? C216 H21B 0.9800 . ? C216 H21C 0.9800 . ? C217 H21D 0.9800 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C218 C221 1.509(3) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C221 C233 1.361(3) 3_656 ? C221 C222 1.416(3) . ? C222 C231 1.405(3) . ? C222 C222 1.420(5) 3_656 ? C231 C232 1.356(3) . ? C231 H231 0.9500 . ? C232 C233 1.399(3) . ? C232 H232 0.9500 . ? C233 C221 1.361(3) 3_656 ? C233 H233 0.9500 . ? N311 C315 1.344(3) . ? N311 N312 1.356(3) . ? N311 C318 1.438(3) . ? N312 C313 1.324(3) . ? C313 C314 1.386(4) . ? C313 C316 1.482(3) . ? C314 C315 1.355(4) . ? C314 H314 0.9500 . ? C315 C317 1.472(4) . ? C316 H31A 0.9800 . ? C316 H31B 0.9800 . ? C316 H31C 0.9800 . ? C317 H31D 0.9800 . ? C317 H31E 0.9800 . ? C317 H31F 0.9800 . ? C318 C321 1.513(3) . ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? C321 C322 1.362(3) . ? C321 C325 1.414(3) 3_756 ? C322 C323 1.398(3) . ? C322 H322 0.9500 . ? C323 C324 1.346(3) . ? C323 H323 0.9500 . ? C324 C325 1.407(3) . ? C324 H324 0.9500 . ? C325 C325 1.413(4) 3_756 ? C325 C321 1.414(3) 3_756 ? N411 C412 1.125(3) . ? C412 C413 1.449(3) . ? C413 H41A 0.9800 . ? C413 H41B 0.9800 . ? C413 H41C 0.9800 . ? N11S C12S 1.126(4) . ? C12S C13S 1.446(4) . ? C13S H13A 0.9800 . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? N21S C22S 1.124(4) . ? C22S C23S 1.440(4) . ? C23S H23A 0.9800 . ? C23S H23B 0.9800 . ? C23S H23C 0.9800 . ? O31X N34X 1.238(5) . ? O32X N34X 1.250(5) . ? O33X N34X 1.240(6) . ? O31Y N34Y 1.213(8) . ? O32Y N34Y 1.188(9) . ? O33Y N34Y 1.278(10) . ? 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 N212 Ag1 N312 122.25(7) . . ? N212 Ag1 N112 106.54(8) . . ? N312 Ag1 N112 108.96(8) . . ? N212 Ag1 N411 107.64(7) . . ? N312 Ag1 N411 100.58(8) . . ? N112 Ag1 N411 110.55(7) . . ? C115 N111 N112 111.85(19) . . ? C115 N111 C118 127.6(2) . . ? N112 N111 C118 119.88(19) . . ? C113 N112 N111 104.91(19) . . ? C113 N112 Ag1 131.45(16) . . ? N111 N112 Ag1 122.41(14) . . ? N112 C113 C114 110.9(2) . . ? N112 C113 C116 120.3(2) . . ? C114 C113 C116 128.8(2) . . ? C115 C114 C113 106.1(2) . . ? C115 C114 H114 127.0 . . ? C113 C114 H114 127.0 . . ? N111 C115 C114 106.2(2) . . ? N111 C115 C117 122.2(2) . . ? C114 C115 C117 131.5(2) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11F 109.5 . . ? C115 C117 H11D 109.5 . . ? H11F C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11F C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? N111 C118 C121 112.5(2) . . ? N111 C118 H11G 109.1 . . ? C121 C118 H11G 109.1 . . ? N111 C118 H11H 109.1 . . ? C121 C118 H11H 109.1 . . ? H11G C118 H11H 107.8 . . ? C122 C121 C123 119.6(2) . . ? C122 C121 C118 121.6(2) . . ? C123 C121 C118 118.8(2) . . ? C121 C122 C131 121.3(2) . 3_666 ? C121 C122 H122 119.4 . . ? C131 C122 H122 119.4 3_666 . ? C132 C123 C123 118.9(3) . 3_666 ? C132 C123 C121 122.0(2) . . ? C123 C123 C121 119.1(3) 3_666 . ? C132 C131 C122 120.3(2) . 3_666 ? C132 C131 H131 119.8 . . ? C122 C131 H131 119.8 3_666 . ? C131 C132 C123 120.7(2) . . ? C131 C132 H132 119.6 . . ? C123 C132 H132 119.6 . . ? C215 N211 N212 111.5(2) . . ? C215 N211 C218 127.3(2) . . ? N212 N211 C218 121.15(19) . . ? C213 N212 N211 105.09(19) . . ? C213 N212 Ag1 125.48(16) . . ? N211 N212 Ag1 129.25(14) . . ? N212 C213 C214 110.5(2) . . ? N212 C213 C216 121.0(2) . . ? C214 C213 C216 128.5(2) . . ? C215 C214 C213 106.2(2) . . ? C215 C214 H214 126.9 . . ? C213 C214 H214 126.9 . . ? N211 C215 C214 106.7(2) . . ? N211 C215 C217 122.2(2) . . ? C214 C215 C217 131.1(2) . . ? C213 C216 H21A 109.5 . . ? C213 C216 H21B 109.5 . . ? H21A C216 H21B 109.5 . . ? C213 C216 H21C 109.5 . . ? H21A C216 H21C 109.5 . . ? H21B C216 H21C 109.5 . . ? C215 C217 H21D 109.5 . . ? C215 C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C215 C217 H21F 109.5 . . ? H21D C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? N211 C218 C221 113.5(2) . . ? N211 C218 H21G 108.9 . . ? C221 C218 H21G 108.9 . . ? N211 C218 H21H 108.9 . . ? C221 C218 H21H 108.9 . . ? H21G C218 H21H 107.7 . . ? C233 C221 C222 120.3(2) 3_656 . ? C233 C221 C218 121.0(2) 3_656 . ? C222 C221 C218 118.8(2) . . ? C231 C222 C221 122.5(2) . . ? C231 C222 C222 118.6(3) . 3_656 ? C221 C222 C222 118.9(3) . 3_656 ? C232 C231 C222 121.2(2) . . ? C232 C231 H231 119.4 . . ? C222 C231 H231 119.4 . . ? C231 C232 C233 120.3(2) . . ? C231 C232 H232 119.9 . . ? C233 C232 H232 119.9 . . ? C221 C233 C232 120.7(2) 3_656 . ? C221 C233 H233 119.7 3_656 . ? C232 C233 H233 119.7 . . ? C315 N311 N312 111.5(2) . . ? C315 N311 C318 128.9(2) . . ? N312 N311 C318 119.2(2) . . ? C313 N312 N311 105.4(2) . . ? C313 N312 Ag1 131.23(17) . . ? N311 N312 Ag1 123.13(15) . . ? N312 C313 C314 110.0(2) . . ? N312 C313 C316 120.9(2) . . ? C314 C313 C316 129.2(2) . . ? C315 C314 C313 106.9(2) . . ? C315 C314 H314 126.6 . . ? C313 C314 H314 126.6 . . ? N311 C315 C314 106.2(2) . . ? N311 C315 C317 122.7(2) . . ? C314 C315 C317 131.1(2) . . ? C313 C316 H31A 109.5 . . ? C313 C316 H31B 109.5 . . ? H31A C316 H31B 109.5 . . ? C313 C316 H31C 109.5 . . ? H31A C316 H31C 109.5 . . ? H31B C316 H31C 109.5 . . ? C315 C317 H31D 109.5 . . ? C315 C317 H31E 109.5 . . ? H31D C317 H31E 109.5 . . ? C315 C317 H31F 109.5 . . ? H31D C317 H31F 109.5 . . ? H31E C317 H31F 109.5 . . ? N311 C318 C321 112.7(2) . . ? N311 C318 H31G 109.0 . . ? C321 C318 H31G 109.0 . . ? N311 C318 H31H 109.0 . . ? C321 C318 H31H 109.0 . . ? H31G C318 H31H 107.8 . . ? C322 C321 C325 120.0(2) . 3_756 ? C322 C321 C318 121.6(2) . . ? C325 C321 C318 118.4(2) 3_756 . ? C321 C322 C323 120.6(2) . . ? C321 C322 H322 119.7 . . ? C323 C322 H322 119.7 . . ? C324 C323 C322 121.0(2) . . ? C324 C323 H323 119.5 . . ? C322 C323 H323 119.5 . . ? C323 C324 C325 120.3(2) . . ? C323 C324 H324 119.9 . . ? C325 C324 H324 119.9 . . ? C324 C325 C325 119.4(3) . 3_756 ? C324 C325 C321 121.8(2) . 3_756 ? C325 C325 C321 118.7(3) 3_756 3_756 ? C412 N411 Ag1 174.4(2) . . ? N411 C412 C413 179.4(3) . . ? C412 C413 H41A 109.5 . . ? C412 C413 H41B 109.5 . . ? H41A C413 H41B 109.5 . . ? C412 C413 H41C 109.5 . . ? H41A C413 H41C 109.5 . . ? H41B C413 H41C 109.5 . . ? N11S C12S C13S 178.3(3) . . ? C12S C13S H13A 109.5 . . ? C12S C13S H13B 109.5 . . ? H13A C13S H13B 109.5 . . ? C12S C13S H13C 109.5 . . ? H13A C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? N21S C22S C23S 179.9(4) . . ? C22S C23S H23A 109.5 . . ? C22S C23S H23B 109.5 . . ? H23A C23S H23B 109.5 . . ? C22S C23S H23C 109.5 . . ? H23A C23S H23C 109.5 . . ? H23B C23S H23C 109.5 . . ? O31X N34X O33X 120.3(4) . . ? O31X N34X O32X 121.2(5) . . ? O33X N34X O32X 118.5(4) . . ? O32Y N34Y O31Y 119.4(8) . . ? O32Y N34Y O33Y 120.1(9) . . ? O31Y N34Y O33Y 120.4(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 C115 N111 N112 C113 -1.3(3) . . . . ? C118 N111 N112 C113 -172.9(2) . . . . ? C115 N111 N112 Ag1 -170.00(15) . . . . ? C118 N111 N112 Ag1 18.5(3) . . . . ? N212 Ag1 N112 C113 -89.0(2) . . . . ? N312 Ag1 N112 C113 44.7(2) . . . . ? N411 Ag1 N112 C113 154.4(2) . . . . ? N212 Ag1 N112 N111 76.35(17) . . . . ? N312 Ag1 N112 N111 -149.97(16) . . . . ? N411 Ag1 N112 N111 -40.33(19) . . . . ? N111 N112 C113 C114 0.9(3) . . . . ? Ag1 N112 C113 C114 168.12(16) . . . . ? N111 N112 C113 C116 -179.4(2) . . . . ? Ag1 N112 C113 C116 -12.2(3) . . . . ? N112 C113 C114 C115 -0.2(3) . . . . ? C116 C113 C114 C115 -179.9(2) . . . . ? N112 N111 C115 C114 1.2(3) . . . . ? C118 N111 C115 C114 172.0(2) . . . . ? N112 N111 C115 C117 -178.7(2) . . . . ? C118 N111 C115 C117 -8.0(4) . . . . ? C113 C114 C115 N111 -0.6(3) . . . . ? C113 C114 C115 C117 179.3(3) . . . . ? C115 N111 C118 C121 -85.5(3) . . . . ? N112 N111 C118 C121 84.6(3) . . . . ? N111 C118 C121 C122 -4.0(3) . . . . ? N111 C118 C121 C123 175.9(2) . . . . ? C123 C121 C122 C131 -1.4(4) . . . 3_666 ? C118 C121 C122 C131 178.5(2) . . . 3_666 ? C122 C121 C123 C132 -178.8(2) . . . . ? C118 C121 C123 C132 1.3(3) . . . . ? C122 C121 C123 C123 1.3(4) . . . 3_666 ? C118 C121 C123 C123 -178.6(3) . . . 3_666 ? C122 C131 C132 C123 -0.9(4) 3_666 . . . ? C123 C123 C132 C131 1.1(4) 3_666 . . . ? C121 C123 C132 C131 -178.9(2) . . . . ? C215 N211 N212 C213 -0.8(3) . . . . ? C218 N211 N212 C213 -178.9(2) . . . . ? C215 N211 N212 Ag1 174.49(17) . . . . ? C218 N211 N212 Ag1 -3.6(3) . . . . ? N312 Ag1 N212 C213 -84.6(2) . . . . ? N112 Ag1 N212 C213 41.5(2) . . . . ? N411 Ag1 N212 C213 160.06(19) . . . . ? N312 Ag1 N212 N211 101.0(2) . . . . ? N112 Ag1 N212 N211 -132.97(19) . . . . ? N411 Ag1 N212 N211 -14.4(2) . . . . ? N211 N212 C213 C214 0.7(3) . . . . ? Ag1 N212 C213 C214 -174.87(16) . . . . ? N211 N212 C213 C216 -177.9(2) . . . . ? Ag1 N212 C213 C216 6.5(3) . . . . ? N212 C213 C214 C215 -0.3(3) . . . . ? C216 C213 C214 C215 178.2(3) . . . . ? N212 N211 C215 C214 0.7(3) . . . . ? C218 N211 C215 C214 178.6(2) . . . . ? N212 N211 C215 C217 179.7(2) . . . . ? C218 N211 C215 C217 -2.5(4) . . . . ? C213 C214 C215 N211 -0.2(3) . . . . ? C213 C214 C215 C217 -179.1(3) . . . . ? C215 N211 C218 C221 -77.6(3) . . . . ? N212 N211 C218 C221 100.1(3) . . . . ? N211 C218 C221 C233 -10.5(3) . . . 3_656 ? N211 C218 C221 C222 169.6(2) . . . . ? C233 C221 C222 C231 -179.2(2) 3_656 . . . ? C218 C221 C222 C231 0.7(4) . . . . ? C233 C221 C222 C222 0.7(4) 3_656 . . 3_656 ? C218 C221 C222 C222 -179.5(3) . . . 3_656 ? C221 C222 C231 C232 -179.4(2) . . . . ? C222 C222 C231 C232 0.7(4) 3_656 . . . ? C222 C231 C232 C233 -0.5(4) . . . . ? C231 C232 C233 C221 -0.3(4) . . . 3_656 ? C315 N311 N312 C313 -0.8(2) . . . . ? C318 N311 N312 C313 -174.88(19) . . . . ? C315 N311 N312 Ag1 -175.76(15) . . . . ? C318 N311 N312 Ag1 10.2(3) . . . . ? N212 Ag1 N312 C313 164.68(19) . . . . ? N112 Ag1 N312 C313 39.8(2) . . . . ? N411 Ag1 N312 C313 -76.5(2) . . . . ? N212 Ag1 N312 N311 -21.84(19) . . . . ? N112 Ag1 N312 N311 -146.77(16) . . . . ? N411 Ag1 N312 N311 97.00(17) . . . . ? N311 N312 C313 C314 0.6(3) . . . . ? Ag1 N312 C313 C314 174.97(16) . . . . ? N311 N312 C313 C316 -179.8(2) . . . . ? Ag1 N312 C313 C316 -5.5(3) . . . . ? N312 C313 C314 C315 -0.2(3) . . . . ? C316 C313 C314 C315 -179.7(2) . . . . ? N312 N311 C315 C314 0.7(3) . . . . ? C318 N311 C315 C314 174.0(2) . . . . ? N312 N311 C315 C317 179.4(2) . . . . ? C318 N311 C315 C317 -7.3(4) . . . . ? C313 C314 C315 N311 -0.3(3) . . . . ? C313 C314 C315 C317 -178.8(3) . . . . ? C315 N311 C318 C321 -89.0(3) . . . . ? N312 N311 C318 C321 83.9(3) . . . . ? N311 C318 C321 C322 8.5(3) . . . . ? N311 C318 C321 C325 -171.1(2) . . . 3_756 ? C325 C321 C322 C323 0.3(4) 3_756 . . . ? C318 C321 C322 C323 -179.3(2) . . . . ? C321 C322 C323 C324 0.0(4) . . . . ? C322 C323 C324 C325 0.0(4) . . . . ? C323 C324 C325 C325 -0.1(4) . . . 3_756 ? C323 C324 C325 C321 -179.7(2) . . . 3_756 ? N212 Ag1 N411 C412 -26(2) . . . . ? N312 Ag1 N411 C412 -155(2) . . . . ? N112 Ag1 N411 C412 90(2) . . . . ? Ag1 N411 C412 C413 -172(100) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.745 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.112 #===END data_imw1178p21c _database_code_depnum_ccdc_archive 'CCDC 797105' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H90 Ag2 B2 F8 N18' _chemical_formula_weight 1669.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3463(8) _cell_length_b 11.8598(5) _cell_length_c 19.2250(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.584(3) _cell_angle_gamma 90.00 _cell_volume 3899.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8333 _cell_measurement_theta_min 3.942 _cell_measurement_theta_max 25.768 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8933 _exptl_absorpt_correction_T_max 0.9717 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42555 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.62 _reflns_number_total 9028 _reflns_number_gt 6618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. All hydrogens were added in geometrically calculated positions. The Fluorines F2 > F4 of the BF4 anion (B1 F1 F2 F3 F4) are disordered over three sites and have thus been left isotropic. The model was improved by the application of geometric and displacement restraints. Displacement restraints improved the appearance of the free acetonitrile solvent molecules (N11S C12S C13S, N21S C22S C23S). 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^)+(0.0344P)^2^+3.4313P] 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 9028 _refine_ls_number_parameters 483 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.086 _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 0.276941(13) 0.773504(17) 0.015902(12) 0.02038(7) Uani 1 1 d . . . N111 N 0.20005(13) 0.95002(18) -0.10467(12) 0.0170(5) Uani 1 1 d . . . N112 N 0.26817(13) 0.92142(18) -0.06266(13) 0.0175(5) Uani 1 1 d . . . C113 C 0.32373(17) 0.9825(2) -0.08655(16) 0.0195(6) Uani 1 1 d . . . C114 C 0.28996(17) 1.0504(2) -0.14276(16) 0.0206(6) Uani 1 1 d . . . H114 H 0.3164 1.1013 -0.1689 0.025 Uiso 1 1 calc R . . C115 C 0.21099(17) 1.0293(2) -0.15291(15) 0.0191(6) Uani 1 1 d . . . C116 C 0.40743(17) 0.9719(3) -0.05360(17) 0.0269(7) Uani 1 1 d . . . H11A H 0.4129 0.9123 -0.0178 0.040 Uiso 1 1 calc R . . H11B H 0.4256 1.0436 -0.0314 0.040 Uiso 1 1 calc R . . H11C H 0.4388 0.9529 -0.0899 0.040 Uiso 1 1 calc R . . C117 C 0.14441(18) 1.0763(3) -0.20362(16) 0.0268(7) Uani 1 1 d . . . H11D H 0.1162 1.0148 -0.2308 0.040 Uiso 1 1 calc R . . H11E H 0.1644 1.1288 -0.2358 0.040 Uiso 1 1 calc R . . H11F H 0.1088 1.1164 -0.1776 0.040 Uiso 1 1 calc R . . C118 C 0.12623(16) 0.9089(2) -0.08886(15) 0.0181(6) Uani 1 1 d . . . H11G H 0.1340 0.8325 -0.0680 0.022 Uiso 1 1 calc R . . H11H H 0.0883 0.9027 -0.1333 0.022 Uiso 1 1 calc R . . C121 C 0.09264(16) 0.9856(2) -0.03801(15) 0.0165(6) Uani 1 1 d . . . C122 C 0.13449(17) 1.0754(2) -0.00666(15) 0.0189(6) Uani 1 1 d . . . H122 H 0.1857 1.0891 -0.0160 0.023 Uiso 1 1 calc R . . C123 C 0.10252(17) 1.1478(2) 0.03933(16) 0.0201(6) Uani 1 1 d . . . H123 H 0.1324 1.2096 0.0606 0.024 Uiso 1 1 calc R . . C124 C 0.01610(16) 0.9636(2) -0.02333(14) 0.0149(6) Uani 1 1 d . . . C131 C -0.02895(17) 0.8704(2) -0.05349(15) 0.0182(6) Uani 1 1 d . . . H131 H -0.0077 0.8202 -0.0838 0.022 Uiso 1 1 calc R . . N211 N 0.23980(13) 0.51061(18) -0.03859(13) 0.0188(5) Uani 1 1 d . . . N212 N 0.27799(13) 0.60982(18) -0.04566(13) 0.0179(5) Uani 1 1 d . . . C213 C 0.31785(16) 0.5924(2) -0.09850(15) 0.0194(6) Uani 1 1 d . . . C214 C 0.30457(17) 0.4836(2) -0.12541(17) 0.0238(7) Uani 1 1 d . . . H214 H 0.3259 0.4507 -0.1631 0.029 Uiso 1 1 calc R . . C215 C 0.25444(17) 0.4335(2) -0.08647(17) 0.0247(7) Uani 1 1 d . . . C216 C 0.36915(19) 0.6817(3) -0.12011(17) 0.0266(7) Uani 1 1 d . . . H21A H 0.3430 0.7549 -0.1201 0.040 Uiso 1 1 calc R . . H21B H 0.3798 0.6654 -0.1676 0.040 Uiso 1 1 calc R . . H21C H 0.4185 0.6837 -0.0869 0.040 Uiso 1 1 calc R . . C217 C 0.2197(2) 0.3183(3) -0.0894(2) 0.0420(10) Uani 1 1 d . . . H21D H 0.2385 0.2786 -0.0451 0.063 Uiso 1 1 calc R . . H21E H 0.2351 0.2763 -0.1287 0.063 Uiso 1 1 calc R . . H21F H 0.1625 0.3242 -0.0961 0.063 Uiso 1 1 calc R . . C218 C 0.18537(16) 0.5000(2) 0.01080(16) 0.0206(6) Uani 1 1 d . . . H21G H 0.1998 0.5550 0.0495 0.025 Uiso 1 1 calc R . . H21H H 0.1902 0.4235 0.0317 0.025 Uiso 1 1 calc R . . C221 C 0.10084(16) 0.5198(2) -0.02306(16) 0.0176(6) Uani 1 1 d . . . C222 C 0.08233(17) 0.5653(2) -0.08901(16) 0.0201(6) Uani 1 1 d . . . H222 H 0.1230 0.5857 -0.1141 0.024 Uiso 1 1 calc R . . C223 C 0.03982(16) 0.4910(2) 0.01607(15) 0.0168(6) Uani 1 1 d . . . C231 C -0.00406(17) 0.4177(2) 0.12024(16) 0.0204(6) Uani 1 1 d . . . H231 H 0.0076 0.3865 0.1663 0.024 Uiso 1 1 calc R . . C232 C 0.05563(17) 0.4455(2) 0.08507(15) 0.0189(6) Uani 1 1 d . . . H232 H 0.1083 0.4342 0.1072 0.023 Uiso 1 1 calc R . . N311 N 0.41455(13) 0.72314(18) 0.14887(12) 0.0167(5) Uani 1 1 d . . . N312 N 0.36981(14) 0.80595(18) 0.11217(13) 0.0181(5) Uani 1 1 d . . . C313 C 0.38639(17) 0.8997(2) 0.15051(16) 0.0208(6) Uani 1 1 d . . . C314 C 0.44158(18) 0.8766(2) 0.21040(16) 0.0232(7) Uani 1 1 d . . . H314 H 0.4632 0.9288 0.2458 0.028 Uiso 1 1 calc R . . C315 C 0.45854(17) 0.7633(2) 0.20811(15) 0.0203(6) Uani 1 1 d . . . C316 C 0.3477(2) 1.0085(2) 0.12727(17) 0.0299(8) Uani 1 1 d . . . H31A H 0.3845 1.0568 0.1075 0.045 Uiso 1 1 calc R . . H31B H 0.3314 1.0463 0.1678 0.045 Uiso 1 1 calc R . . H31C H 0.3018 0.9940 0.0912 0.045 Uiso 1 1 calc R . . C317 C 0.51146(19) 0.6899(3) 0.25782(18) 0.0306(7) Uani 1 1 d . . . H31D H 0.4813 0.6279 0.2737 0.046 Uiso 1 1 calc R . . H31E H 0.5355 0.7344 0.2987 0.046 Uiso 1 1 calc R . . H31F H 0.5524 0.6590 0.2338 0.046 Uiso 1 1 calc R . . C318 C 0.41632(17) 0.6123(2) 0.11727(16) 0.0186(6) Uani 1 1 d . . . H31G H 0.3630 0.5927 0.0932 0.022 Uiso 1 1 calc R . . H31H H 0.4320 0.5561 0.1550 0.022 Uiso 1 1 calc R . . C321 C 0.47219(16) 0.6053(2) 0.06454(15) 0.0175(6) Uani 1 1 d . . . C322 C 0.51874(17) 0.6947(2) 0.05309(16) 0.0202(6) Uani 1 1 d . . . H322 H 0.5174 0.7619 0.0797 0.024 Uiso 1 1 calc R . . C323 C 0.56852(17) 0.6877(2) 0.00227(17) 0.0227(7) Uani 1 1 d . . . H323 H 0.6001 0.7506 -0.0052 0.027 Uiso 1 1 calc R . . C324 C 0.57187(16) 0.5918(2) -0.03629(16) 0.0199(6) Uani 1 1 d . . . H324 H 0.6055 0.5886 -0.0705 0.024 Uiso 1 1 calc R . . C325 C 0.47460(16) 0.5033(2) 0.02561(15) 0.0170(6) Uani 1 1 d . . . N411 N 0.15990(16) 0.7707(2) 0.07204(14) 0.0281(6) Uani 1 1 d . . . C412 C 0.10274(18) 0.7628(2) 0.09301(16) 0.0238(6) Uani 1 1 d . . . C413 C 0.02936(19) 0.7531(3) 0.12025(18) 0.0308(8) Uani 1 1 d . . . H41A H -0.0043 0.8175 0.1040 0.046 Uiso 1 1 calc R . . H41B H 0.0402 0.7523 0.1719 0.046 Uiso 1 1 calc R . . H41C H 0.0029 0.6830 0.1031 0.046 Uiso 1 1 calc R . . N11S N 0.1592(2) 0.7688(3) 0.28142(16) 0.0440(8) Uani 1 1 d . . . C12S C 0.2035(2) 0.7197(3) 0.25667(18) 0.0318(7) Uani 1 1 d . . . C13S C 0.2600(2) 0.6580(3) 0.2238(2) 0.0403(9) Uani 1 1 d . . . H13A H 0.2353 0.5903 0.2008 0.060 Uiso 1 1 calc R . . H13B H 0.3043 0.6361 0.2598 0.060 Uiso 1 1 calc R . . H13C H 0.2786 0.7060 0.1885 0.060 Uiso 1 1 calc R . . N21S N 0.9683(2) 0.6133(3) 0.2579(2) 0.0705(11) Uiso 1 1 d . . . C22S C 0.9106(2) 0.5806(3) 0.2704(2) 0.0424(9) Uiso 1 1 d . . . C23S C 0.8381(2) 0.5385(3) 0.2871(2) 0.0406(9) Uiso 1 1 d . . . H23A H 0.8168 0.4813 0.2524 0.061 Uiso 1 1 calc R . . H23B H 0.8007 0.6007 0.2860 0.061 Uiso 1 1 calc R . . H23C H 0.8473 0.5048 0.3343 0.061 Uiso 1 1 calc R . . B1 B 0.7038(2) 0.8212(3) 0.3256(2) 0.0256(8) Uiso 1 1 d D . . F1 F 0.70593(11) 0.74496(15) 0.27155(10) 0.0381(5) Uiso 1 1 d D A . F2X F 0.6417(5) 0.8948(8) 0.3020(5) 0.0272(15) Uiso 0.383(16) 1 d PDU A 1 F4X F 0.7766(5) 0.8777(12) 0.3349(4) 0.0293(14) Uiso 0.383(16) 1 d PDU A 1 F3X F 0.6932(7) 0.7614(7) 0.3854(4) 0.0268(15) Uiso 0.383(16) 1 d PDU A 1 F2Y F 0.6342(3) 0.8832(5) 0.3095(4) 0.0340(14) Uiso 0.454(17) 1 d PDU A 2 F3Y F 0.7076(5) 0.7738(5) 0.3923(2) 0.0308(13) Uiso 0.454(17) 1 d PDU A 2 F4Y F 0.7610(4) 0.9077(6) 0.3332(3) 0.0330(12) Uiso 0.454(17) 1 d PDU A 2 F2Z F 0.6655(9) 0.9243(8) 0.3118(7) 0.0359(17) Uiso 0.163(8) 1 d PDU A 3 F3Z F 0.6763(9) 0.7658(11) 0.3802(5) 0.027(2) Uiso 0.163(8) 1 d PDU A 3 F4Z F 0.7859(2) 0.8348(14) 0.3440(6) 0.032(2) Uiso 0.163(8) 1 d PDU A 3 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 0.02120(12) 0.01926(10) 0.02017(12) -0.00015(10) 0.00195(9) 0.00040(9) N111 0.0144(13) 0.0196(11) 0.0176(13) 0.0000(9) 0.0040(10) -0.0006(9) N112 0.0138(12) 0.0190(11) 0.0193(13) 0.0000(10) 0.0016(10) 0.0008(9) C113 0.0166(15) 0.0193(13) 0.0232(17) -0.0045(12) 0.0049(13) -0.0002(11) C114 0.0196(16) 0.0224(13) 0.0215(17) 0.0022(12) 0.0080(13) -0.0006(11) C115 0.0222(16) 0.0196(13) 0.0159(15) 0.0007(11) 0.0049(12) 0.0025(11) C116 0.0184(16) 0.0286(15) 0.0328(19) 0.0010(14) 0.0018(14) -0.0028(12) C117 0.0244(18) 0.0340(16) 0.0225(18) 0.0055(13) 0.0055(14) 0.0049(13) C118 0.0147(15) 0.0204(13) 0.0194(16) -0.0016(11) 0.0031(12) -0.0013(11) C121 0.0177(15) 0.0160(12) 0.0157(15) 0.0028(11) 0.0025(12) 0.0020(11) C122 0.0153(15) 0.0217(13) 0.0202(16) 0.0019(11) 0.0041(12) -0.0002(11) C123 0.0193(16) 0.0190(13) 0.0216(17) -0.0019(11) 0.0027(13) -0.0030(11) C124 0.0154(14) 0.0162(12) 0.0127(14) 0.0035(10) 0.0013(12) 0.0014(10) C131 0.0195(15) 0.0182(13) 0.0166(16) 0.0008(11) 0.0021(12) 0.0014(11) N211 0.0134(13) 0.0184(11) 0.0250(14) -0.0002(10) 0.0041(11) -0.0021(9) N212 0.0153(13) 0.0178(11) 0.0203(14) -0.0005(10) 0.0025(10) -0.0019(9) C213 0.0143(15) 0.0262(14) 0.0171(16) 0.0013(12) 0.0009(12) 0.0020(11) C214 0.0195(16) 0.0274(15) 0.0250(18) -0.0054(13) 0.0048(14) 0.0034(12) C215 0.0167(16) 0.0214(14) 0.0357(19) -0.0095(13) 0.0033(14) 0.0019(11) C216 0.0278(18) 0.0291(15) 0.0254(18) 0.0006(13) 0.0122(14) -0.0008(13) C217 0.031(2) 0.0232(15) 0.074(3) -0.0156(17) 0.0163(19) -0.0065(14) C218 0.0157(15) 0.0221(13) 0.0243(17) 0.0023(12) 0.0041(13) -0.0001(11) C221 0.0158(15) 0.0151(12) 0.0221(16) -0.0020(11) 0.0041(12) -0.0009(10) C222 0.0167(15) 0.0212(13) 0.0234(17) 0.0006(12) 0.0059(13) -0.0015(11) C223 0.0172(15) 0.0144(12) 0.0187(15) -0.0014(11) 0.0024(12) -0.0022(10) C231 0.0215(16) 0.0217(13) 0.0177(16) 0.0017(11) 0.0023(13) 0.0004(11) C232 0.0146(15) 0.0201(13) 0.0205(16) -0.0010(11) -0.0014(12) -0.0002(11) N311 0.0153(12) 0.0145(10) 0.0204(13) 0.0007(10) 0.0030(10) 0.0019(9) N312 0.0171(13) 0.0153(10) 0.0219(14) 0.0004(9) 0.0030(10) 0.0026(9) C313 0.0217(16) 0.0183(13) 0.0229(17) -0.0018(12) 0.0053(13) 0.0004(11) C314 0.0286(17) 0.0187(13) 0.0205(17) -0.0038(12) -0.0005(14) -0.0020(12) C315 0.0176(15) 0.0247(13) 0.0179(15) 0.0009(12) 0.0012(12) -0.0028(11) C316 0.037(2) 0.0204(14) 0.0304(19) -0.0062(13) -0.0005(15) 0.0068(13) C317 0.0273(18) 0.0282(15) 0.032(2) 0.0046(14) -0.0064(15) -0.0015(13) C318 0.0189(15) 0.0136(12) 0.0234(17) -0.0013(11) 0.0044(13) 0.0009(11) C321 0.0143(15) 0.0165(12) 0.0215(16) 0.0016(11) 0.0024(12) 0.0024(10) C322 0.0210(16) 0.0154(12) 0.0247(17) -0.0031(11) 0.0047(13) 0.0002(11) C323 0.0190(16) 0.0159(12) 0.0342(19) 0.0010(12) 0.0076(14) -0.0038(11) C324 0.0160(15) 0.0187(13) 0.0263(17) 0.0002(12) 0.0073(13) 0.0007(11) C325 0.0129(14) 0.0161(12) 0.0219(16) 0.0017(11) 0.0024(12) 0.0019(10) N411 0.0262(15) 0.0315(13) 0.0274(15) 0.0050(12) 0.0068(12) 0.0056(12) C412 0.0249(17) 0.0258(14) 0.0204(16) 0.0042(12) 0.0024(13) 0.0042(12) C413 0.0243(17) 0.0390(18) 0.0313(19) 0.0072(14) 0.0110(15) 0.0056(13) N11S 0.054(2) 0.0456(17) 0.0326(18) 0.0043(15) 0.0095(16) -0.0009(16) C12S 0.035(2) 0.0365(17) 0.0232(18) 0.0082(15) 0.0018(15) -0.0052(16) C13S 0.034(2) 0.051(2) 0.037(2) 0.0120(17) 0.0080(17) 0.0043(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N312 2.275(2) . ? Ag1 N212 2.275(2) . ? Ag1 N112 2.303(2) . ? Ag1 N411 2.453(3) . ? N111 C115 1.356(3) . ? N111 N112 1.359(3) . ? N111 C118 1.449(3) . ? N112 C113 1.346(3) . ? C113 C114 1.396(4) . ? C113 C116 1.490(4) . ? C114 C115 1.374(4) . ? C114 H114 0.9500 . ? C115 C117 1.490(4) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C118 C121 1.521(4) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.371(4) . ? C121 C124 1.426(4) . ? C122 C123 1.410(4) . ? C122 H122 0.9500 . ? C123 C131 1.365(4) 3_575 ? C123 H123 0.9500 . ? C124 C131 1.421(4) . ? C124 C124 1.424(5) 3_575 ? C131 C123 1.365(4) 3_575 ? C131 H131 0.9500 . ? N211 C215 1.351(4) . ? N211 N212 1.368(3) . ? N211 C218 1.452(4) . ? N212 C213 1.337(4) . ? C213 C214 1.395(4) . ? C213 C216 1.487(4) . ? C214 C215 1.373(4) . ? C214 H214 0.9500 . ? C215 C217 1.491(4) . ? C216 H21A 0.9800 . ? C216 H21B 0.9800 . ? C216 H21C 0.9800 . ? C217 H21D 0.9800 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C218 C221 1.520(4) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C221 C222 1.366(4) . ? C221 C223 1.438(4) . ? C222 C231 1.405(4) 3_565 ? C222 H222 0.9500 . ? C223 C232 1.416(4) . ? C223 C223 1.432(6) 3_565 ? C231 C232 1.368(4) . ? C231 C222 1.405(4) 3_565 ? C231 H231 0.9500 . ? C232 H232 0.9500 . ? N311 C315 1.348(4) . ? N311 N312 1.372(3) . ? N311 C318 1.450(3) . ? N312 C313 1.338(3) . ? C313 C314 1.396(4) . ? C313 C316 1.488(4) . ? C314 C315 1.377(4) . ? C314 H314 0.9500 . ? C315 C317 1.491(4) . ? C316 H31A 0.9800 . ? C316 H31B 0.9800 . ? C316 H31C 0.9800 . ? C317 H31D 0.9800 . ? C317 H31E 0.9800 . ? C317 H31F 0.9800 . ? C318 C321 1.517(4) . ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? C321 C322 1.372(4) . ? C321 C325 1.427(4) . ? C322 C323 1.410(4) . ? C322 H322 0.9500 . ? C323 C324 1.364(4) . ? C323 H323 0.9500 . ? C324 C325 1.421(4) 3_665 ? C324 H324 0.9500 . ? C325 C324 1.421(4) 3_665 ? C325 C325 1.429(5) 3_665 ? N411 C412 1.135(4) . ? C412 C413 1.459(4) . ? C413 H41A 0.9800 . ? C413 H41B 0.9800 . ? C413 H41C 0.9800 . ? N11S C12S 1.132(4) . ? C12S C13S 1.449(5) . ? C13S H13A 0.9800 . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? N21S C22S 1.135(5) . ? C22S C23S 1.439(5) . ? C23S H23A 0.9800 . ? C23S H23B 0.9800 . ? C23S H23C 0.9800 . ? B1 F1 1.383(4) . ? B1 F3X 1.389(4) . ? B1 F3Z 1.390(4) . ? B1 F3Y 1.391(4) . ? B1 F2Z 1.396(4) . ? B1 F2X 1.401(4) . ? B1 F2Y 1.403(4) . ? B1 F4X 1.415(4) . ? B1 F4Y 1.418(4) . ? B1 F4Z 1.419(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N312 Ag1 N212 120.11(8) . . ? N312 Ag1 N112 111.41(8) . . ? N212 Ag1 N112 108.30(8) . . ? N312 Ag1 N411 99.80(9) . . ? N212 Ag1 N411 107.23(9) . . ? N112 Ag1 N411 109.25(8) . . ? C115 N111 N112 111.9(2) . . ? C115 N111 C118 127.3(2) . . ? N112 N111 C118 120.2(2) . . ? C113 N112 N111 105.3(2) . . ? C113 N112 Ag1 131.36(19) . . ? N111 N112 Ag1 122.40(16) . . ? N112 C113 C114 110.0(3) . . ? N112 C113 C116 120.8(3) . . ? C114 C113 C116 129.1(3) . . ? C115 C114 C113 106.5(3) . . ? C115 C114 H114 126.7 . . ? C113 C114 H114 126.7 . . ? N111 C115 C114 106.2(2) . . ? N111 C115 C117 121.7(3) . . ? C114 C115 C117 132.1(3) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C115 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? N111 C118 C121 112.3(2) . . ? N111 C118 H11G 109.1 . . ? C121 C118 H11G 109.1 . . ? N111 C118 H11H 109.1 . . ? C121 C118 H11H 109.1 . . ? H11G C118 H11H 107.9 . . ? C122 C121 C124 119.8(3) . . ? C122 C121 C118 121.1(3) . . ? C124 C121 C118 119.1(2) . . ? C121 C122 C123 120.9(3) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C131 C123 C122 120.5(3) 3_575 . ? C131 C123 H123 119.8 3_575 . ? C122 C123 H123 119.8 . . ? C131 C124 C124 118.8(3) . 3_575 ? C131 C124 C121 121.9(2) . . ? C124 C124 C121 119.3(3) 3_575 . ? C123 C131 C124 120.7(3) 3_575 . ? C123 C131 H131 119.7 3_575 . ? C124 C131 H131 119.7 . . ? C215 N211 N212 111.4(2) . . ? C215 N211 C218 127.1(2) . . ? N212 N211 C218 121.2(2) . . ? C213 N212 N211 105.2(2) . . ? C213 N212 Ag1 125.27(18) . . ? N211 N212 Ag1 129.51(17) . . ? N212 C213 C214 110.5(2) . . ? N212 C213 C216 120.8(2) . . ? C214 C213 C216 128.7(3) . . ? C215 C214 C213 106.2(3) . . ? C215 C214 H214 126.9 . . ? C213 C214 H214 126.9 . . ? N211 C215 C214 106.6(2) . . ? N211 C215 C217 121.7(3) . . ? C214 C215 C217 131.7(3) . . ? C213 C216 H21A 109.5 . . ? C213 C216 H21B 109.5 . . ? H21A C216 H21B 109.5 . . ? C213 C216 H21C 109.5 . . ? H21A C216 H21C 109.5 . . ? H21B C216 H21C 109.5 . . ? C215 C217 H21D 109.5 . . ? C215 C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C215 C217 H21F 109.5 . . ? H21D C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? N211 C218 C221 113.1(2) . . ? N211 C218 H21G 109.0 . . ? C221 C218 H21G 109.0 . . ? N211 C218 H21H 109.0 . . ? C221 C218 H21H 109.0 . . ? H21G C218 H21H 107.8 . . ? C222 C221 C223 120.0(3) . . ? C222 C221 C218 121.3(3) . . ? C223 C221 C218 118.7(2) . . ? C221 C222 C231 121.0(3) . 3_565 ? C221 C222 H222 119.5 . . ? C231 C222 H222 119.5 3_565 . ? C232 C223 C223 118.9(3) . 3_565 ? C232 C223 C221 122.4(3) . . ? C223 C223 C221 118.7(3) 3_565 . ? C232 C231 C222 120.7(3) . 3_565 ? C232 C231 H231 119.6 . . ? C222 C231 H231 119.6 3_565 . ? C231 C232 C223 120.7(3) . . ? C231 C232 H232 119.7 . . ? C223 C232 H232 119.7 . . ? C315 N311 N312 111.9(2) . . ? C315 N311 C318 128.7(2) . . ? N312 N311 C318 118.9(2) . . ? C313 N312 N311 105.1(2) . . ? C313 N312 Ag1 130.30(19) . . ? N311 N312 Ag1 124.09(16) . . ? N312 C313 C314 110.3(2) . . ? N312 C313 C316 120.7(3) . . ? C314 C313 C316 129.1(3) . . ? C315 C314 C313 106.6(3) . . ? C315 C314 H314 126.7 . . ? C313 C314 H314 126.7 . . ? N311 C315 C314 106.1(2) . . ? N311 C315 C317 122.5(3) . . ? C314 C315 C317 131.4(3) . . ? C313 C316 H31A 109.5 . . ? C313 C316 H31B 109.5 . . ? H31A C316 H31B 109.5 . . ? C313 C316 H31C 109.5 . . ? H31A C316 H31C 109.5 . . ? H31B C316 H31C 109.5 . . ? C315 C317 H31D 109.5 . . ? C315 C317 H31E 109.5 . . ? H31D C317 H31E 109.5 . . ? C315 C317 H31F 109.5 . . ? H31D C317 H31F 109.5 . . ? H31E C317 H31F 109.5 . . ? N311 C318 C321 112.9(2) . . ? N311 C318 H31G 109.0 . . ? C321 C318 H31G 109.0 . . ? N311 C318 H31H 109.0 . . ? C321 C318 H31H 109.0 . . ? H31G C318 H31H 107.8 . . ? C322 C321 C325 120.1(3) . . ? C322 C321 C318 121.6(2) . . ? C325 C321 C318 118.3(2) . . ? C321 C322 C323 120.7(3) . . ? C321 C322 H322 119.6 . . ? C323 C322 H322 119.6 . . ? C324 C323 C322 120.8(3) . . ? C324 C323 H323 119.6 . . ? C322 C323 H323 119.6 . . ? C323 C324 C325 120.4(3) . 3_665 ? C323 C324 H324 119.8 . . ? C325 C324 H324 119.8 3_665 . ? C324 C325 C321 122.0(2) 3_665 . ? C324 C325 C325 119.1(3) 3_665 3_665 ? C321 C325 C325 118.9(3) . 3_665 ? C412 N411 Ag1 173.5(3) . . ? N411 C412 C413 179.7(4) . . ? C412 C413 H41A 109.5 . . ? C412 C413 H41B 109.5 . . ? H41A C413 H41B 109.5 . . ? C412 C413 H41C 109.5 . . ? H41A C413 H41C 109.5 . . ? H41B C413 H41C 109.5 . . ? N11S C12S C13S 178.9(4) . . ? C12S C13S H13A 109.5 . . ? C12S C13S H13B 109.5 . . ? H13A C13S H13B 109.5 . . ? C12S C13S H13C 109.5 . . ? H13A C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? N21S C22S C23S 179.3(5) . . ? C22S C23S H23A 109.5 . . ? C22S C23S H23B 109.5 . . ? H23A C23S H23B 109.5 . . ? C22S C23S H23C 109.5 . . ? H23A C23S H23C 109.5 . . ? H23B C23S H23C 109.5 . . ? F1 B1 F3X 108.2(5) . . ? F1 B1 F3Z 108.3(6) . . ? F3X B1 F3Z 12.3(8) . . ? F1 B1 F3Y 115.2(4) . . ? F3X B1 F3Y 12.4(5) . . ? F3Z B1 F3Y 23.3(6) . . ? F1 B1 F2Z 120.1(7) . . ? F3X B1 F2Z 118.7(7) . . ? F3Z B1 F2Z 110.2(7) . . ? F3Y B1 F2Z 118.5(6) . . ? F1 B1 F2X 106.2(5) . . ? F3X B1 F2X 112.7(5) . . ? F3Z B1 F2X 101.4(8) . . ? F3Y B1 F2X 117.8(5) . . ? F2Z B1 F2X 22.7(6) . . ? F1 B1 F2Y 107.9(4) . . ? F3X B1 F2Y 102.9(5) . . ? F3Z B1 F2Y 91.4(7) . . ? F3Y B1 F2Y 108.8(4) . . ? F2Z B1 F2Y 30.0(8) . . ? F2X B1 F2Y 10.3(6) . . ? F1 B1 F4X 105.6(5) . . ? F3X B1 F4X 112.0(5) . . ? F3Z B1 F4X 122.7(7) . . ? F3Y B1 F4X 99.8(5) . . ? F2Z B1 F4X 89.8(7) . . ? F2X B1 F4X 111.6(5) . . ? F2Y B1 F4X 119.8(7) . . ? F1 B1 F4Y 116.4(4) . . ? F3X B1 F4Y 118.1(6) . . ? F3Z B1 F4Y 126.0(7) . . ? F3Y B1 F4Y 105.8(4) . . ? F2Z B1 F4Y 71.9(8) . . ? F2X B1 F4Y 94.0(5) . . ? F2Y B1 F4Y 101.8(4) . . ? F4X B1 F4Y 18.1(4) . . ? F1 B1 F4Z 96.3(5) . . ? F3X B1 F4Z 96.7(7) . . ? F3Z B1 F4Z 108.8(7) . . ? F3Y B1 F4Z 85.7(7) . . ? F2Z B1 F4Z 112.0(7) . . ? F2X B1 F4Z 134.1(7) . . ? F2Y B1 F4Z 141.9(8) . . ? F4X B1 F4Z 22.5(6) . . ? F4Y B1 F4Z 40.1(7) . . ? 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 C115 N111 N112 C113 -1.6(3) . . . . ? C118 N111 N112 C113 -173.2(2) . . . . ? C115 N111 N112 Ag1 -171.74(17) . . . . ? C118 N111 N112 Ag1 16.6(3) . . . . ? N312 Ag1 N112 C113 43.7(3) . . . . ? N212 Ag1 N112 C113 -90.5(2) . . . . ? N411 Ag1 N112 C113 153.0(2) . . . . ? N312 Ag1 N112 N111 -148.99(18) . . . . ? N212 Ag1 N112 N111 76.8(2) . . . . ? N411 Ag1 N112 N111 -39.7(2) . . . . ? N111 N112 C113 C114 0.9(3) . . . . ? Ag1 N112 C113 C114 169.80(19) . . . . ? N111 N112 C113 C116 -179.0(2) . . . . ? Ag1 N112 C113 C116 -10.1(4) . . . . ? N112 C113 C114 C115 0.1(3) . . . . ? C116 C113 C114 C115 180.0(3) . . . . ? N112 N111 C115 C114 1.7(3) . . . . ? C118 N111 C115 C114 172.5(2) . . . . ? N112 N111 C115 C117 -178.3(2) . . . . ? C118 N111 C115 C117 -7.4(4) . . . . ? C113 C114 C115 N111 -1.0(3) . . . . ? C113 C114 C115 C117 178.9(3) . . . . ? C115 N111 C118 C121 -82.7(3) . . . . ? N112 N111 C118 C121 87.5(3) . . . . ? N111 C118 C121 C122 -6.5(4) . . . . ? N111 C118 C121 C124 173.1(2) . . . . ? C124 C121 C122 C123 -0.9(4) . . . . ? C118 C121 C122 C123 178.7(3) . . . . ? C121 C122 C123 C131 0.0(4) . . . 3_575 ? C122 C121 C124 C131 -178.8(3) . . . . ? C118 C121 C124 C131 1.6(4) . . . . ? C122 C121 C124 C124 0.6(5) . . . 3_575 ? C118 C121 C124 C124 -178.9(3) . . . 3_575 ? C124 C124 C131 C123 1.5(5) 3_575 . . 3_575 ? C121 C124 C131 C123 -179.1(3) . . . 3_575 ? C215 N211 N212 C213 -0.9(3) . . . . ? C218 N211 N212 C213 -175.4(2) . . . . ? C215 N211 N212 Ag1 178.73(19) . . . . ? C218 N211 N212 Ag1 4.2(4) . . . . ? N312 Ag1 N212 C213 -87.5(2) . . . . ? N112 Ag1 N212 C213 42.0(2) . . . . ? N411 Ag1 N212 C213 159.8(2) . . . . ? N312 Ag1 N212 N211 93.0(2) . . . . ? N112 Ag1 N212 N211 -137.5(2) . . . . ? N411 Ag1 N212 N211 -19.7(2) . . . . ? N211 N212 C213 C214 0.7(3) . . . . ? Ag1 N212 C213 C214 -178.99(19) . . . . ? N211 N212 C213 C216 -178.0(3) . . . . ? Ag1 N212 C213 C216 2.4(4) . . . . ? N212 C213 C214 C215 -0.2(3) . . . . ? C216 C213 C214 C215 178.3(3) . . . . ? N212 N211 C215 C214 0.8(3) . . . . ? C218 N211 C215 C214 174.9(3) . . . . ? N212 N211 C215 C217 179.8(3) . . . . ? C218 N211 C215 C217 -6.1(5) . . . . ? C213 C214 C215 N211 -0.3(3) . . . . ? C213 C214 C215 C217 -179.2(3) . . . . ? C215 N211 C218 C221 -78.5(3) . . . . ? N212 N211 C218 C221 95.1(3) . . . . ? N211 C218 C221 C222 -12.6(4) . . . . ? N211 C218 C221 C223 168.3(2) . . . . ? C223 C221 C222 C231 -1.4(4) . . . 3_565 ? C218 C221 C222 C231 179.4(2) . . . 3_565 ? C222 C221 C223 C232 -178.8(3) . . . . ? C218 C221 C223 C232 0.3(4) . . . . ? C222 C221 C223 C223 1.2(4) . . . 3_565 ? C218 C221 C223 C223 -179.6(3) . . . 3_565 ? C222 C231 C232 C223 -0.7(4) 3_565 . . . ? C223 C223 C232 C231 0.9(5) 3_565 . . . ? C221 C223 C232 C231 -179.1(2) . . . . ? C315 N311 N312 C313 -0.6(3) . . . . ? C318 N311 N312 C313 -173.6(2) . . . . ? C315 N311 N312 Ag1 -172.89(18) . . . . ? C318 N311 N312 Ag1 14.1(3) . . . . ? N212 Ag1 N312 C313 170.7(2) . . . . ? N112 Ag1 N312 C313 42.6(3) . . . . ? N411 Ag1 N312 C313 -72.7(3) . . . . ? N212 Ag1 N312 N311 -19.0(2) . . . . ? N112 Ag1 N312 N311 -147.16(19) . . . . ? N411 Ag1 N312 N311 97.6(2) . . . . ? N311 N312 C313 C314 0.6(3) . . . . ? Ag1 N312 C313 C314 172.2(2) . . . . ? N311 N312 C313 C316 -179.4(3) . . . . ? Ag1 N312 C313 C316 -7.8(4) . . . . ? N312 C313 C314 C315 -0.4(4) . . . . ? C316 C313 C314 C315 179.6(3) . . . . ? N312 N311 C315 C314 0.3(3) . . . . ? C318 N311 C315 C314 172.4(3) . . . . ? N312 N311 C315 C317 179.1(3) . . . . ? C318 N311 C315 C317 -8.8(5) . . . . ? C313 C314 C315 N311 0.1(3) . . . . ? C313 C314 C315 C317 -178.6(3) . . . . ? C315 N311 C318 C321 -90.4(3) . . . . ? N312 N311 C318 C321 81.2(3) . . . . ? N311 C318 C321 C322 3.9(4) . . . . ? N311 C318 C321 C325 -175.0(2) . . . . ? C325 C321 C322 C323 0.9(4) . . . . ? C318 C321 C322 C323 -178.0(3) . . . . ? C321 C322 C323 C324 -0.4(5) . . . . ? C322 C323 C324 C325 -0.3(5) . . . 3_665 ? C322 C321 C325 C324 179.2(3) . . . 3_665 ? C318 C321 C325 C324 -1.8(4) . . . 3_665 ? C322 C321 C325 C325 -0.7(5) . . . 3_665 ? C318 C321 C325 C325 178.3(3) . . . 3_665 ? N312 Ag1 N411 C412 -152(2) . . . . ? N212 Ag1 N411 C412 -26(2) . . . . ? N112 Ag1 N411 C412 91(2) . . . . ? Ag1 N411 C412 C413 -174(100) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.908 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.081 #===END data_imw1188p41212 _database_code_depnum_ccdc_archive 'CCDC 797106' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H78 Ag2 B2 F8 N14' _chemical_formula_weight 1504.82 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'x+1/2, -y+1/2, -z+3/4' _cell_length_a 20.379(3) _cell_length_b 20.379 _cell_length_c 16.588(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6889.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1873 _cell_measurement_theta_min 6.18 _cell_measurement_theta_max 21.64 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9097 _exptl_absorpt_correction_T_max 0.9326 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83365 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7917 _reflns_number_gt 6415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; [AG2(L)3](BF4)2.2MeCN The data was solved by direct methods. All hydrogens have been included in calculated positions. The lattice contains a CH3CN as free solvent (N1S C2S C3S). The solvent molecule is disordered over three sites (28:38:34). Site occupancies were established experimentally. The model beneffited from the application of geometric and displacement restraints. 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^)+(0.0544P)^2^+4.4263P] 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 0.00(3) _refine_ls_number_reflns 7917 _refine_ls_number_parameters 447 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.067 _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 0.985926(15) 0.232561(15) 0.093633(19) 0.03486(10) Uani 1 1 d . . . N111 N 0.83519(16) 0.20203(16) 0.0409(2) 0.0271(7) Uani 1 1 d . . . N112 N 0.89716(17) 0.17777(16) 0.0520(2) 0.0307(8) Uani 1 1 d . . . C113 C 0.8946(2) 0.11502(19) 0.0267(3) 0.0322(9) Uani 1 1 d . . . C114 C 0.8310(2) 0.1007(2) 0.0002(3) 0.0334(9) Uani 1 1 d . . . H114 H 0.8161 0.0600 -0.0209 0.040 Uiso 1 1 calc R . . C115 C 0.7945(2) 0.15656(19) 0.0103(2) 0.0297(9) Uani 1 1 d . . . C116 C 0.9540(2) 0.0732(2) 0.0285(3) 0.0415(11) Uani 1 1 d . . . H11A H 0.9670 0.0622 -0.0267 0.062 Uiso 1 1 calc R . . H11B H 0.9446 0.0328 0.0584 0.062 Uiso 1 1 calc R . . H11C H 0.9898 0.0969 0.0552 0.062 Uiso 1 1 calc R . . C117 C 0.7243(2) 0.1701(2) -0.0060(3) 0.0417(11) Uani 1 1 d . . . H11D H 0.7014 0.1781 0.0450 0.063 Uiso 1 1 calc R . . H11E H 0.7046 0.1322 -0.0331 0.063 Uiso 1 1 calc R . . H11F H 0.7205 0.2088 -0.0406 0.063 Uiso 1 1 calc R . . C118 C 0.8210(2) 0.26830(19) 0.0670(2) 0.0300(9) Uani 1 1 d . . . H11G H 0.8428 0.2759 0.1195 0.036 Uiso 1 1 calc R . . H11H H 0.7731 0.2724 0.0756 0.036 Uiso 1 1 calc R . . C121 C 0.84276(18) 0.32152(18) 0.0085(2) 0.0255(8) Uani 1 1 d . . . C122 C 0.84917(19) 0.3085(2) -0.0712(2) 0.0288(9) Uani 1 1 d . . . H122 H 0.8417 0.2652 -0.0903 0.035 Uiso 1 1 calc R . . C123 C 0.8668(2) 0.35843(18) -0.1263(2) 0.0297(9) Uani 1 1 d . . . H123 H 0.8697 0.3485 -0.1821 0.036 Uiso 1 1 calc R . . C124 C 0.87972(17) 0.42103(19) -0.1003(3) 0.0290(9) Uani 1 1 d . . . C125 C 0.87602(17) 0.43589(19) -0.0168(2) 0.0247(8) Uani 1 1 d . . . C126 C 0.85434(17) 0.38624(18) 0.0383(2) 0.0250(8) Uani 1 1 d . . . C131 C 0.89136(19) 0.49913(18) 0.0150(3) 0.0294(9) Uani 1 1 d . . . H131 H 0.9071 0.5323 -0.0202 0.035 Uiso 1 1 calc R . . C132 C 0.88388(17) 0.5128(2) 0.0950(3) 0.0317(9) Uani 1 1 d . . . H132 H 0.8951 0.5551 0.1147 0.038 Uiso 1 1 calc R . . C133 C 0.85980(18) 0.46538(19) 0.1482(3) 0.0306(9) Uani 1 1 d . . . H133 H 0.8527 0.4759 0.2033 0.037 Uiso 1 1 calc R . . C134 C 0.84656(19) 0.4032(2) 0.1201(2) 0.0294(8) Uani 1 1 d . . . H134 H 0.8317 0.3708 0.1569 0.035 Uiso 1 1 calc R . . N211 N 1.03987(16) 0.20180(16) 0.27107(19) 0.0294(7) Uani 1 1 d . . . N212 N 1.05569(16) 0.20812(16) 0.1920(2) 0.0293(7) Uani 1 1 d . . . C213 C 1.1170(2) 0.1865(2) 0.1849(3) 0.0339(10) Uani 1 1 d . . . C214 C 1.1406(2) 0.1658(2) 0.2590(3) 0.0349(10) Uani 1 1 d . . . H214 H 1.1828 0.1480 0.2700 0.042 Uiso 1 1 calc R . . C215 C 1.0908(2) 0.1761(2) 0.3133(3) 0.0334(10) Uani 1 1 d . . . C216 C 1.1497(2) 0.1859(2) 0.1042(3) 0.0428(11) Uani 1 1 d . . . H21A H 1.1367 0.1464 0.0746 0.064 Uiso 1 1 calc R . . H21B H 1.1975 0.1861 0.1114 0.064 Uiso 1 1 calc R . . H21C H 1.1365 0.2249 0.0736 0.064 Uiso 1 1 calc R . . C217 C 1.0861(2) 0.1638(3) 0.4018(3) 0.0468(11) Uani 1 1 d . . . H21D H 1.0816 0.2056 0.4302 0.070 Uiso 1 1 calc R . . H21E H 1.1260 0.1414 0.4202 0.070 Uiso 1 1 calc R . . H21F H 1.0479 0.1361 0.4130 0.070 Uiso 1 1 calc R . . C218 C 0.97537(19) 0.21959(19) 0.2972(2) 0.0308(9) Uani 1 1 d . . . H21G H 0.9636 0.2625 0.2734 0.037 Uiso 1 1 calc R . . H21H H 0.9754 0.2246 0.3566 0.037 Uiso 1 1 calc R . . C221 C 0.92409(19) 0.16946(19) 0.2737(2) 0.0273(8) Uani 1 1 d . . . C222 C 0.94148(19) 0.10609(19) 0.2614(2) 0.0278(9) Uani 1 1 d . . . H222 H 0.9860 0.0933 0.2679 0.033 Uiso 1 1 calc R . . C223 C 0.85671(19) 0.18921(19) 0.2640(2) 0.0251(8) Uani 1 1 d . . . C231 C 0.7714(2) 0.2724(2) 0.2668(2) 0.0341(9) Uani 1 1 d . . . H231 H 0.7573 0.3156 0.2800 0.041 Uiso 1 1 calc R . . C232 C 0.8350(2) 0.25432(19) 0.2814(2) 0.0302(9) Uani 1 1 d . . . H232 H 0.8649 0.2853 0.3032 0.036 Uiso 1 1 calc R . . N311 N 1.03398(16) 0.37022(17) 0.0102(2) 0.0313(8) Uani 1 1 d . . . N312 N 1.01853(17) 0.30567(17) -0.0012(2) 0.0323(8) Uani 1 1 d . . . C313 C 1.0311(2) 0.2938(2) -0.0779(3) 0.0401(11) Uani 1 1 d . . . C314 C 1.0558(2) 0.3496(3) -0.1152(3) 0.0436(11) Uani 1 1 d . . . H314 H 1.0692 0.3536 -0.1699 0.052 Uiso 1 1 calc R . . C315 C 1.0570(2) 0.3975(3) -0.0581(3) 0.0420(11) Uani 1 1 d . . . C316 C 1.0162(3) 0.2272(3) -0.1138(3) 0.0539(12) Uani 1 1 d . . . H31A H 1.0289 0.1928 -0.0756 0.081 Uiso 1 1 calc R . . H31B H 1.0408 0.2218 -0.1641 0.081 Uiso 1 1 calc R . . H31C H 0.9691 0.2239 -0.1250 0.081 Uiso 1 1 calc R . . C317 C 1.0778(3) 0.4691(3) -0.0612(3) 0.0554(14) Uani 1 1 d . . . H31D H 1.0443 0.4963 -0.0351 0.083 Uiso 1 1 calc R . . H31E H 1.0828 0.4827 -0.1176 0.083 Uiso 1 1 calc R . . H31F H 1.1197 0.4744 -0.0331 0.083 Uiso 1 1 calc R . . C318 C 1.02583(19) 0.3987(2) 0.0898(3) 0.0338(9) Uani 1 1 d . . . H31G H 0.9828 0.3849 0.1116 0.041 Uiso 1 1 calc R . . H31H H 1.0251 0.4471 0.0846 0.041 Uiso 1 1 calc R . . F1 F 0.77829(17) 0.44500(19) 0.44709(17) 0.0753(10) Uani 1 1 d . . . F2 F 0.72030(13) 0.42554(18) 0.3338(2) 0.0684(9) Uani 1 1 d . . . F3 F 0.83047(12) 0.40996(13) 0.3350(2) 0.0571(7) Uani 1 1 d . . . F4 F 0.78871(16) 0.51179(14) 0.3383(2) 0.0666(9) Uani 1 1 d . . . B1 B 0.7787(2) 0.4487(3) 0.3642(3) 0.0382(11) Uani 1 1 d . . . N1SX N 0.9723(9) 0.0445(7) 0.8124(10) 0.095(3) Uiso 0.38 1 d PDU A -1 C2SX C 0.9711(11) 0.0804(9) 0.7626(11) 0.092(3) Uiso 0.38 1 d PDU A -1 C3SX C 0.9702(10) 0.1306(9) 0.6986(11) 0.090(3) Uiso 0.38 1 d PDU A -1 H3S1 H 0.9344 0.1617 0.7089 0.135 Uiso 0.38 1 calc PR A -1 H3S2 H 0.9633 0.1094 0.6463 0.135 Uiso 0.38 1 calc PR A -1 H3S3 H 1.0121 0.1541 0.6982 0.135 Uiso 0.38 1 calc PR A -1 N1SY N 1.0187(11) 0.0744(10) 0.8282(12) 0.090(3) Uiso 0.28 1 d PDU B -2 C2SY C 1.0120(14) 0.0950(13) 0.7672(12) 0.091(3) Uiso 0.28 1 d PDU B -2 C3SY C 0.9997(14) 0.1192(14) 0.6849(12) 0.090(3) Uiso 0.28 1 d PDU B -2 H3S4 H 1.0330 0.1014 0.6482 0.136 Uiso 0.28 1 calc PR B -2 H3S5 H 1.0019 0.1672 0.6845 0.136 Uiso 0.28 1 calc PR B -2 H3S6 H 0.9561 0.1051 0.6672 0.136 Uiso 0.28 1 calc PR B -2 N1SZ N 0.7781(6) 0.1958(6) 0.7599(10) 0.060(3) Uiso 0.34 1 d PDU C -3 C2SZ C 0.8286(6) 0.2038(8) 0.7377(11) 0.060(3) Uiso 0.34 1 d PDU C -3 C3SZ C 0.8974(6) 0.2166(9) 0.7157(11) 0.067(3) Uiso 0.34 1 d PDU C -3 H3S7 H 0.8991 0.2503 0.6737 0.101 Uiso 0.34 1 calc PR C -3 H3S8 H 0.9175 0.1761 0.6955 0.101 Uiso 0.34 1 calc PR C -3 H3S9 H 0.9215 0.2318 0.7633 0.101 Uiso 0.34 1 calc PR C -3 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 0.03530(17) 0.04080(18) 0.02847(16) -0.00036(14) -0.00300(13) 0.00054(14) N111 0.0257(17) 0.0293(17) 0.0263(19) 0.0031(14) -0.0017(14) 0.0006(14) N112 0.0365(19) 0.0295(18) 0.0259(19) 0.0056(14) -0.0005(15) 0.0029(15) C113 0.032(2) 0.031(2) 0.033(2) 0.0073(17) 0.0018(18) 0.0017(16) C114 0.041(2) 0.026(2) 0.034(2) -0.0012(17) 0.0017(18) -0.0003(18) C115 0.035(2) 0.026(2) 0.028(2) 0.0045(17) -0.0038(17) -0.0034(17) C116 0.046(3) 0.029(2) 0.049(3) 0.004(2) 0.003(2) 0.004(2) C117 0.036(2) 0.039(2) 0.050(3) 0.004(2) -0.006(2) -0.005(2) C118 0.038(2) 0.0259(19) 0.026(2) 0.0026(17) 0.0020(16) 0.0006(18) C121 0.0236(19) 0.026(2) 0.027(2) 0.0025(16) -0.0009(16) 0.0009(16) C122 0.030(2) 0.028(2) 0.029(2) 0.0041(16) 0.0011(16) 0.0015(16) C123 0.035(2) 0.028(2) 0.025(2) 0.0018(16) 0.0038(16) 0.0011(17) C124 0.0195(18) 0.032(2) 0.035(2) 0.0099(18) 0.0003(17) 0.0018(15) C125 0.0182(18) 0.027(2) 0.029(2) 0.0008(16) -0.0028(15) 0.0031(15) C126 0.0177(18) 0.027(2) 0.030(2) 0.0064(16) -0.0019(15) 0.0007(14) C131 0.029(2) 0.027(2) 0.032(2) 0.0052(16) 0.0010(16) 0.0005(16) C132 0.0273(19) 0.0268(18) 0.041(2) -0.006(2) -0.0069(18) 0.0033(16) C133 0.029(2) 0.032(2) 0.030(2) -0.0043(18) -0.0016(18) 0.0052(16) C134 0.026(2) 0.034(2) 0.028(2) -0.0003(17) 0.0001(16) 0.0032(16) N211 0.0315(18) 0.0305(18) 0.0262(18) 0.0021(14) -0.0041(14) -0.0084(14) N212 0.0316(18) 0.0307(17) 0.0254(18) 0.0018(14) -0.0047(14) -0.0043(14) C213 0.038(2) 0.030(2) 0.034(2) 0.0017(17) -0.0016(18) -0.0086(18) C214 0.025(2) 0.039(2) 0.040(3) 0.006(2) -0.0071(19) -0.0064(18) C215 0.032(2) 0.038(2) 0.031(2) 0.0047(18) -0.0059(17) -0.0120(18) C216 0.045(3) 0.046(3) 0.037(3) 0.001(2) 0.007(2) 0.000(2) C217 0.042(3) 0.064(3) 0.035(2) 0.016(2) -0.009(2) -0.012(2) C218 0.032(2) 0.033(2) 0.028(2) 0.0009(16) -0.0015(16) -0.0055(16) C221 0.034(2) 0.032(2) 0.0157(18) 0.0025(16) -0.0007(16) -0.0081(16) C222 0.026(2) 0.030(2) 0.028(2) -0.0002(17) 0.0007(16) -0.0020(16) C223 0.032(2) 0.030(2) 0.0133(19) 0.0040(15) 0.0033(16) -0.0039(16) C231 0.044(2) 0.031(2) 0.027(2) 0.0037(17) 0.0111(19) 0.0026(19) C232 0.037(2) 0.027(2) 0.027(2) 0.0054(16) 0.0041(17) -0.0022(17) N311 0.0318(19) 0.038(2) 0.0242(18) 0.0076(15) -0.0020(14) -0.0019(15) N312 0.0300(17) 0.044(2) 0.0228(18) 0.0046(15) -0.0027(15) 0.0006(16) C313 0.034(2) 0.060(3) 0.027(2) 0.001(2) -0.0024(17) 0.004(2) C314 0.036(2) 0.069(3) 0.026(2) 0.007(2) 0.0010(19) 0.001(2) C315 0.027(2) 0.061(3) 0.039(3) 0.020(2) -0.0049(19) 0.000(2) C316 0.052(3) 0.072(3) 0.038(3) -0.013(2) 0.002(2) 0.003(3) C317 0.054(3) 0.059(3) 0.052(3) 0.027(3) -0.007(2) -0.006(2) C318 0.029(2) 0.037(2) 0.035(2) 0.002(2) -0.0021(19) 0.0007(17) F1 0.080(2) 0.114(3) 0.0318(16) 0.0036(17) -0.0024(15) -0.024(2) F2 0.0389(16) 0.105(3) 0.061(2) -0.0337(19) -0.0065(14) -0.0064(16) F3 0.0386(15) 0.0500(16) 0.083(2) -0.0035(16) 0.0033(15) 0.0044(12) F4 0.079(2) 0.0466(16) 0.074(2) 0.0148(17) -0.0067(17) 0.0167(15) B1 0.036(3) 0.044(3) 0.035(3) -0.004(2) -0.006(2) -0.004(2) _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 N212 2.221(3) . ? Ag1 N112 2.235(4) . ? Ag1 N312 2.266(3) . ? N111 C115 1.343(5) . ? N111 N112 1.369(5) . ? N111 C118 1.447(5) . ? N112 C113 1.347(5) . ? C113 C114 1.399(6) . ? C113 C116 1.482(6) . ? C114 C115 1.371(6) . ? C114 H114 0.9500 . ? C115 C117 1.482(6) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C118 C121 1.522(5) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.354(6) . ? C121 C126 1.428(5) . ? C122 C123 1.414(5) . ? C122 H122 0.9500 . ? C123 C124 1.372(6) . ? C123 H123 0.9500 . ? C124 C125 1.420(6) . ? C124 C318 1.520(5) 5_564 ? C125 C131 1.427(5) . ? C125 C126 1.434(5) . ? C126 C134 1.408(5) . ? C131 C132 1.363(6) . ? C131 H131 0.9500 . ? C132 C133 1.399(6) . ? C132 H132 0.9500 . ? C133 C134 1.377(6) . ? C133 H133 0.9500 . ? C134 H134 0.9500 . ? N211 N212 1.356(5) . ? N211 C215 1.357(5) . ? N211 C218 1.431(5) . ? N212 C213 1.330(5) . ? C213 C214 1.386(6) . ? C213 C216 1.496(6) . ? C214 C215 1.375(6) . ? C214 H214 0.9500 . ? C215 C217 1.491(6) . ? C216 H21A 0.9800 . ? C216 H21B 0.9800 . ? C216 H21C 0.9800 . ? C217 H21D 0.9800 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C218 C221 1.512(5) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C221 C222 1.355(6) . ? C221 C223 1.440(6) . ? C222 C222 1.422(8) 7_665 ? C222 H222 0.9500 . ? C223 C223 1.403(8) 7_665 ? C223 C232 1.428(6) . ? C231 C232 1.368(6) . ? C231 C231 1.382(9) 7_665 ? C231 H231 0.9500 . ? C232 H232 0.9500 . ? N311 C315 1.346(5) . ? N311 N312 1.366(5) . ? N311 C318 1.452(6) . ? N312 C313 1.320(5) . ? C313 C314 1.388(7) . ? C313 C316 1.513(7) . ? C314 C315 1.362(7) . ? C314 H314 0.9500 . ? C315 C317 1.520(7) . ? C316 H31A 0.9800 . ? C316 H31B 0.9800 . ? C316 H31C 0.9800 . ? C317 H31D 0.9800 . ? C317 H31E 0.9800 . ? C317 H31F 0.9800 . ? C318 C124 1.520(5) 3_645 ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? F1 B1 1.376(6) . ? F2 B1 1.377(6) . ? F3 B1 1.403(6) . ? F4 B1 1.372(6) . ? N1SX C2SX 1.1044(17) . ? C2SX C3SX 1.4729(17) . ? C3SX H3S1 0.9800 . ? C3SX H3S2 0.9800 . ? C3SX H3S3 0.9800 . ? N1SY C2SY 1.1040(18) . ? C2SY C3SY 1.4733(18) . ? C3SY H3S4 0.9800 . ? C3SY H3S5 0.9800 . ? C3SY H3S6 0.9800 . ? N1SZ C2SZ 1.1045(18) . ? C2SZ C3SZ 1.4736(18) . ? C3SZ H3S7 0.9800 . ? C3SZ H3S8 0.9800 . ? C3SZ H3S9 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 N212 Ag1 N112 129.29(12) . . ? N212 Ag1 N312 118.03(12) . . ? N112 Ag1 N312 110.55(12) . . ? C115 N111 N112 111.8(3) . . ? C115 N111 C118 129.3(3) . . ? N112 N111 C118 118.8(3) . . ? C113 N112 N111 105.4(3) . . ? C113 N112 Ag1 127.0(3) . . ? N111 N112 Ag1 127.4(2) . . ? N112 C113 C114 109.4(4) . . ? N112 C113 C116 120.6(4) . . ? C114 C113 C116 130.0(4) . . ? C115 C114 C113 106.9(4) . . ? C115 C114 H114 126.6 . . ? C113 C114 H114 126.6 . . ? N111 C115 C114 106.6(4) . . ? N111 C115 C117 122.4(4) . . ? C114 C115 C117 131.0(4) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C115 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? N111 C118 C121 114.6(3) . . ? N111 C118 H11G 108.6 . . ? C121 C118 H11G 108.6 . . ? N111 C118 H11H 108.6 . . ? C121 C118 H11H 108.6 . . ? H11G C118 H11H 107.6 . . ? C122 C121 C126 120.2(4) . . ? C122 C121 C118 120.7(4) . . ? C126 C121 C118 119.0(4) . . ? C121 C122 C123 121.0(4) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C124 C123 C122 121.0(4) . . ? C124 C123 H123 119.5 . . ? C122 C123 H123 119.5 . . ? C123 C124 C125 119.6(4) . . ? C123 C124 C318 120.4(4) . 5_564 ? C125 C124 C318 120.0(4) . 5_564 ? C124 C125 C131 122.8(4) . . ? C124 C125 C126 119.2(3) . . ? C131 C125 C126 118.0(4) . . ? C134 C126 C121 122.8(4) . . ? C134 C126 C125 118.4(4) . . ? C121 C126 C125 118.8(3) . . ? C132 C131 C125 121.3(4) . . ? C132 C131 H131 119.3 . . ? C125 C131 H131 119.3 . . ? C131 C132 C133 120.8(4) . . ? C131 C132 H132 119.6 . . ? C133 C132 H132 119.6 . . ? C134 C133 C132 119.3(4) . . ? C134 C133 H133 120.3 . . ? C132 C133 H133 120.3 . . ? C133 C134 C126 122.1(4) . . ? C133 C134 H134 119.0 . . ? C126 C134 H134 119.0 . . ? N212 N211 C215 110.8(3) . . ? N212 N211 C218 119.2(3) . . ? C215 N211 C218 130.0(3) . . ? C213 N212 N211 106.1(3) . . ? C213 N212 Ag1 127.6(3) . . ? N211 N212 Ag1 125.4(2) . . ? N212 C213 C214 110.4(4) . . ? N212 C213 C216 120.1(4) . . ? C214 C213 C216 129.5(4) . . ? C215 C214 C213 106.2(4) . . ? C215 C214 H214 126.9 . . ? C213 C214 H214 126.9 . . ? N211 C215 C214 106.5(4) . . ? N211 C215 C217 121.7(4) . . ? C214 C215 C217 131.8(4) . . ? C213 C216 H21A 109.5 . . ? C213 C216 H21B 109.5 . . ? H21A C216 H21B 109.5 . . ? C213 C216 H21C 109.5 . . ? H21A C216 H21C 109.5 . . ? H21B C216 H21C 109.5 . . ? C215 C217 H21D 109.5 . . ? C215 C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C215 C217 H21F 109.5 . . ? H21D C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? N211 C218 C221 112.7(3) . . ? N211 C218 H21G 109.1 . . ? C221 C218 H21G 109.1 . . ? N211 C218 H21H 109.1 . . ? C221 C218 H21H 109.1 . . ? H21G C218 H21H 107.8 . . ? C222 C221 C223 119.9(3) . . ? C222 C221 C218 120.1(4) . . ? C223 C221 C218 119.9(4) . . ? C221 C222 C222 120.8(2) . 7_665 ? C221 C222 H222 119.6 . . ? C222 C222 H222 119.6 7_665 . ? C223 C223 C232 118.7(2) 7_665 . ? C223 C223 C221 119.1(2) 7_665 . ? C232 C223 C221 122.2(4) . . ? C232 C231 C231 120.6(2) . 7_665 ? C232 C231 H231 119.7 . . ? C231 C231 H231 119.7 7_665 . ? C231 C232 C223 120.6(4) . . ? C231 C232 H232 119.7 . . ? C223 C232 H232 119.7 . . ? C315 N311 N312 111.3(4) . . ? C315 N311 C318 129.8(4) . . ? N312 N311 C318 119.0(3) . . ? C313 N312 N311 105.3(3) . . ? C313 N312 Ag1 127.3(3) . . ? N311 N312 Ag1 127.2(2) . . ? N312 C313 C314 110.5(4) . . ? N312 C313 C316 120.3(4) . . ? C314 C313 C316 129.2(4) . . ? C315 C314 C313 106.5(4) . . ? C315 C314 H314 126.8 . . ? C313 C314 H314 126.8 . . ? N311 C315 C314 106.4(4) . . ? N311 C315 C317 121.6(5) . . ? C314 C315 C317 132.0(4) . . ? C313 C316 H31A 109.5 . . ? C313 C316 H31B 109.5 . . ? H31A C316 H31B 109.5 . . ? C313 C316 H31C 109.5 . . ? H31A C316 H31C 109.5 . . ? H31B C316 H31C 109.5 . . ? C315 C317 H31D 109.5 . . ? C315 C317 H31E 109.5 . . ? H31D C317 H31E 109.5 . . ? C315 C317 H31F 109.5 . . ? H31D C317 H31F 109.5 . . ? H31E C317 H31F 109.5 . . ? N311 C318 C124 114.3(3) . 3_645 ? N311 C318 H31G 108.7 . . ? C124 C318 H31G 108.7 3_645 . ? N311 C318 H31H 108.7 . . ? C124 C318 H31H 108.7 3_645 . ? H31G C318 H31H 107.6 . . ? F4 B1 F1 111.4(4) . . ? F4 B1 F2 109.5(4) . . ? F1 B1 F2 110.0(4) . . ? F4 B1 F3 107.9(4) . . ? F1 B1 F3 108.7(4) . . ? F2 B1 F3 109.3(4) . . ? N1SX C2SX C3SX 177(2) . . ? C2SX C3SX H3S1 109.5 . . ? C2SX C3SX H3S2 109.5 . . ? H3S1 C3SX H3S2 109.5 . . ? C2SX C3SX H3S3 109.5 . . ? H3S1 C3SX H3S3 109.5 . . ? H3S2 C3SX H3S3 109.5 . . ? N1SY C2SY C3SY 176(3) . . ? C2SY C3SY H3S4 109.5 . . ? C2SY C3SY H3S5 109.5 . . ? H3S4 C3SY H3S5 109.5 . . ? C2SY C3SY H3S6 109.5 . . ? H3S4 C3SY H3S6 109.5 . . ? H3S5 C3SY H3S6 109.5 . . ? N1SZ C2SZ C3SZ 174.7(17) . . ? C2SZ C3SZ H3S7 109.5 . . ? C2SZ C3SZ H3S8 109.5 . . ? H3S7 C3SZ H3S8 109.5 . . ? C2SZ C3SZ H3S9 109.5 . . ? H3S7 C3SZ H3S9 109.5 . . ? H3S8 C3SZ H3S9 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 C115 N111 N112 C113 0.4(4) . . . . ? C118 N111 N112 C113 176.5(3) . . . . ? C115 N111 N112 Ag1 175.9(3) . . . . ? C118 N111 N112 Ag1 -8.0(5) . . . . ? N212 Ag1 N112 C113 -56.6(4) . . . . ? N312 Ag1 N112 C113 106.2(3) . . . . ? N212 Ag1 N112 N111 128.8(3) . . . . ? N312 Ag1 N112 N111 -68.4(3) . . . . ? N111 N112 C113 C114 -0.1(4) . . . . ? Ag1 N112 C113 C114 -175.6(3) . . . . ? N111 N112 C113 C116 178.9(4) . . . . ? Ag1 N112 C113 C116 3.4(6) . . . . ? N112 C113 C114 C115 -0.3(5) . . . . ? C116 C113 C114 C115 -179.1(4) . . . . ? N112 N111 C115 C114 -0.6(5) . . . . ? C118 N111 C115 C114 -176.2(4) . . . . ? N112 N111 C115 C117 178.9(4) . . . . ? C118 N111 C115 C117 3.3(6) . . . . ? C113 C114 C115 N111 0.5(5) . . . . ? C113 C114 C115 C117 -178.9(4) . . . . ? C115 N111 C118 C121 -103.8(5) . . . . ? N112 N111 C118 C121 80.9(4) . . . . ? N111 C118 C121 C122 25.3(5) . . . . ? N111 C118 C121 C126 -156.7(3) . . . . ? C126 C121 C122 C123 -0.6(6) . . . . ? C118 C121 C122 C123 177.4(4) . . . . ? C121 C122 C123 C124 1.9(6) . . . . ? C122 C123 C124 C125 0.6(6) . . . . ? C122 C123 C124 C318 179.9(4) . . . 5_564 ? C123 C124 C125 C131 177.4(4) . . . . ? C318 C124 C125 C131 -1.9(5) 5_564 . . . ? C123 C124 C125 C126 -4.3(5) . . . . ? C318 C124 C125 C126 176.4(3) 5_564 . . . ? C122 C121 C126 C134 178.0(4) . . . . ? C118 C121 C126 C134 0.1(5) . . . . ? C122 C121 C126 C125 -3.2(5) . . . . ? C118 C121 C126 C125 178.8(3) . . . . ? C124 C125 C126 C134 -175.6(3) . . . . ? C131 C125 C126 C134 2.8(5) . . . . ? C124 C125 C126 C121 5.6(5) . . . . ? C131 C125 C126 C121 -176.1(3) . . . . ? C124 C125 C131 C132 176.4(4) . . . . ? C126 C125 C131 C132 -1.9(5) . . . . ? C125 C131 C132 C133 -1.1(6) . . . . ? C131 C132 C133 C134 3.1(6) . . . . ? C132 C133 C134 C126 -2.2(6) . . . . ? C121 C126 C134 C133 178.0(3) . . . . ? C125 C126 C134 C133 -0.8(5) . . . . ? C215 N211 N212 C213 -0.3(4) . . . . ? C218 N211 N212 C213 -178.2(3) . . . . ? C215 N211 N212 Ag1 169.8(3) . . . . ? C218 N211 N212 Ag1 -8.1(5) . . . . ? N112 Ag1 N212 C213 107.2(3) . . . . ? N312 Ag1 N212 C213 -54.5(4) . . . . ? N112 Ag1 N212 N211 -60.8(3) . . . . ? N312 Ag1 N212 N211 137.6(3) . . . . ? N211 N212 C213 C214 0.5(5) . . . . ? Ag1 N212 C213 C214 -169.3(3) . . . . ? N211 N212 C213 C216 179.2(4) . . . . ? Ag1 N212 C213 C216 9.4(6) . . . . ? N212 C213 C214 C215 -0.5(5) . . . . ? C216 C213 C214 C215 -179.0(4) . . . . ? N212 N211 C215 C214 0.0(4) . . . . ? C218 N211 C215 C214 177.6(4) . . . . ? N212 N211 C215 C217 -179.7(4) . . . . ? C218 N211 C215 C217 -2.1(7) . . . . ? C213 C214 C215 N211 0.3(5) . . . . ? C213 C214 C215 C217 180.0(5) . . . . ? N212 N211 C218 C221 75.0(4) . . . . ? C215 N211 C218 C221 -102.4(4) . . . . ? N211 C218 C221 C222 25.3(5) . . . . ? N211 C218 C221 C223 -154.3(3) . . . . ? C223 C221 C222 C222 0.1(7) . . . 7_665 ? C218 C221 C222 C222 -179.5(4) . . . 7_665 ? C222 C221 C223 C223 -4.6(6) . . . 7_665 ? C218 C221 C223 C223 174.9(4) . . . 7_665 ? C222 C221 C223 C232 175.8(4) . . . . ? C218 C221 C223 C232 -4.6(5) . . . . ? C231 C231 C232 C223 -1.6(7) 7_665 . . . ? C223 C223 C232 C231 -3.5(6) 7_665 . . . ? C221 C223 C232 C231 176.0(4) . . . . ? C315 N311 N312 C313 -1.2(4) . . . . ? C318 N311 N312 C313 -179.6(3) . . . . ? C315 N311 N312 Ag1 174.5(3) . . . . ? C318 N311 N312 Ag1 -4.0(5) . . . . ? N212 Ag1 N312 C313 111.6(4) . . . . ? N112 Ag1 N312 C313 -53.3(4) . . . . ? N212 Ag1 N312 N311 -63.2(3) . . . . ? N112 Ag1 N312 N311 131.9(3) . . . . ? N311 N312 C313 C314 1.3(5) . . . . ? Ag1 N312 C313 C314 -174.3(3) . . . . ? N311 N312 C313 C316 -176.7(4) . . . . ? Ag1 N312 C313 C316 7.7(6) . . . . ? N312 C313 C314 C315 -1.0(5) . . . . ? C316 C313 C314 C315 176.8(5) . . . . ? N312 N311 C315 C314 0.6(5) . . . . ? C318 N311 C315 C314 178.8(4) . . . . ? N312 N311 C315 C317 -179.9(4) . . . . ? C318 N311 C315 C317 -1.7(7) . . . . ? C313 C314 C315 N311 0.2(5) . . . . ? C313 C314 C315 C317 -179.2(5) . . . . ? C315 N311 C318 C124 -101.8(5) . . . 3_645 ? N312 N311 C318 C124 76.3(4) . . . 3_645 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.621 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.073 #===END data_imw1191p212121 _database_code_depnum_ccdc_archive 'CCDC 797107' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H75 Ag2 N15 O6' _chemical_formula_weight 1414.17 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 Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 16.3239(18) _cell_length_b 19.566(2) _cell_length_c 20.852(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6660.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9636 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.37 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8287 _exptl_absorpt_correction_T_max 0.8808 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 119532 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13604 _reflns_number_gt 12662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data processing was carried out to a resolution of 0.8 angstrom as the data was only complete to this resolution. Hydrogen atoms were added in geometrically calculated positions. The lattice contains an acetonitrile molecule that is disordered over three sites and has been modelled as such (N1S C2S C3S; 40:35:25). Geometric and displacement restraints were applied to the disordered molecules to improve the model. The solvent molecule components were left isotropic due to the disorder. One nitrate counterion (N2 O4 O5 O6) is disordered over two sites and has been modelled as such (85:15). Geometric and displacement rrestraints have been applied to improve the model. The oxygen atoms have been left isotropic due to the disorder. 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^)+(0.0727P)^2^+8.2884P] 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 -0.01(2) _refine_ls_number_reflns 13604 _refine_ls_number_parameters 842 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.071 _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 0.711946(19) 0.248082(17) 0.753856(15) 0.03160(9) Uani 1 1 d . . . Ag2 Ag 1.030610(19) 0.025699(18) 0.985514(16) 0.03145(9) Uani 1 1 d . . . N111 N 0.8867(2) 0.30738(19) 0.79640(18) 0.0280(8) Uani 1 1 d . . . N112 N 0.8065(2) 0.32236(19) 0.78470(17) 0.0268(7) Uani 1 1 d . . . C115 C 0.9254(3) 0.3614(2) 0.8236(2) 0.0299(9) Uani 1 1 d . . . C114 C 0.8696(3) 0.4126(2) 0.8304(2) 0.0287(9) Uani 1 1 d . . . H114 H 0.8782 0.4567 0.8483 0.034 Uiso 1 1 calc R . . C113 C 0.7965(3) 0.3860(2) 0.8051(2) 0.0292(9) Uani 1 1 d . . . C117 C 1.0141(3) 0.3583(3) 0.8420(3) 0.0412(12) Uani 1 1 d . . . H11A H 1.0226 0.3212 0.8728 0.062 Uiso 1 1 calc R . . H11B H 1.0303 0.4018 0.8616 0.062 Uiso 1 1 calc R . . H11C H 1.0474 0.3500 0.8037 0.062 Uiso 1 1 calc R . . C116 C 0.7151(3) 0.4211(3) 0.7995(2) 0.0375(10) Uani 1 1 d . . . H11D H 0.6754 0.3899 0.7799 0.056 Uiso 1 1 calc R . . H11E H 0.7208 0.4620 0.7727 0.056 Uiso 1 1 calc R . . H11F H 0.6960 0.4343 0.8423 0.056 Uiso 1 1 calc R . . C118 C 0.9173(3) 0.2396(2) 0.7805(2) 0.0297(9) Uani 1 1 d . . . H11G H 0.9778 0.2412 0.7774 0.036 Uiso 1 1 calc R . . H11H H 0.8956 0.2259 0.7380 0.036 Uiso 1 1 calc R . . N121 N 0.8470(2) 0.05568(18) 1.03601(18) 0.0270(7) Uani 1 1 d . . . N122 N 0.9277(2) 0.05069(17) 1.05165(17) 0.0240(7) Uani 1 1 d . . . C125 C 0.8030(3) 0.0819(2) 1.0852(2) 0.0304(9) Uani 1 1 d . . . C124 C 0.8577(3) 0.0938(2) 1.1349(2) 0.0324(10) Uani 1 1 d . . . H124 H 0.8457 0.1119 1.1761 0.039 Uiso 1 1 calc R . . C123 C 0.9339(3) 0.0737(2) 1.1115(2) 0.0283(9) Uani 1 1 d . . . C127 C 0.7131(3) 0.0934(3) 1.0822(3) 0.0428(11) Uani 1 1 d . . . H12A H 0.7013 0.1306 1.0521 0.064 Uiso 1 1 calc R . . H12B H 0.6927 0.1055 1.1249 0.064 Uiso 1 1 calc R . . H12C H 0.6859 0.0515 1.0675 0.064 Uiso 1 1 calc R . . C126 C 1.0158(3) 0.0761(3) 1.1431(2) 0.0367(11) Uani 1 1 d . . . H12D H 1.0479 0.0360 1.1303 0.055 Uiso 1 1 calc R . . H12E H 1.0087 0.0761 1.1898 0.055 Uiso 1 1 calc R . . H12F H 1.0446 0.1178 1.1300 0.055 Uiso 1 1 calc R . . C128 C 0.8208(3) 0.0369(2) 0.9721(2) 0.0302(9) Uani 1 1 d . . . H12G H 0.7605 0.0315 0.9719 0.036 Uiso 1 1 calc R . . H12H H 0.8452 -0.0079 0.9609 0.036 Uiso 1 1 calc R . . C131 C 0.8927(2) 0.1867(2) 0.8299(2) 0.0268(9) Uani 1 1 d . . . C132 C 0.8787(3) 0.2053(2) 0.8921(2) 0.0297(9) Uani 1 1 d . . . H132 H 0.8839 0.2520 0.9041 0.036 Uiso 1 1 calc R . . C133 C 0.8564(3) 0.1563(2) 0.9389(2) 0.0287(9) Uani 1 1 d . . . H133 H 0.8495 0.1701 0.9822 0.034 Uiso 1 1 calc R . . C134 C 0.8447(2) 0.0885(2) 0.9220(2) 0.0253(8) Uani 1 1 d . . . C135 C 0.8570(2) 0.0679(2) 0.8574(2) 0.0256(8) Uani 1 1 d . . . C136 C 0.8848(2) 0.1171(2) 0.8107(2) 0.0260(8) Uani 1 1 d . . . C141 C 0.8416(3) -0.0008(2) 0.8366(2) 0.0289(9) Uani 1 1 d . . . H141 H 0.8199 -0.0330 0.8661 0.035 Uiso 1 1 calc R . . C142 C 0.8576(3) -0.0208(2) 0.7747(2) 0.0339(9) Uani 1 1 d . . . H142 H 0.8468 -0.0665 0.7617 0.041 Uiso 1 1 calc R . . C143 C 0.8904(3) 0.0268(3) 0.7304(2) 0.0336(9) Uani 1 1 d . . . H143 H 0.9042 0.0125 0.6882 0.040 Uiso 1 1 calc R . . C144 C 0.9025(2) 0.0940(2) 0.7484(2) 0.0307(9) Uani 1 1 d . . . H144 H 0.9233 0.1255 0.7178 0.037 Uiso 1 1 calc R . . N211 N 0.6229(2) 0.29390(19) 0.62072(18) 0.0317(8) Uani 1 1 d . . . N212 N 0.6130(2) 0.27389(18) 0.68300(18) 0.0292(8) Uani 1 1 d . . . C215 C 0.5505(3) 0.3140(2) 0.5940(2) 0.0392(11) Uani 1 1 d . . . C214 C 0.4924(3) 0.3074(2) 0.6406(3) 0.0414(12) Uani 1 1 d . . . H214 H 0.4358 0.3179 0.6369 0.050 Uiso 1 1 calc R . . C213 C 0.5332(3) 0.2819(2) 0.6953(2) 0.0335(9) Uani 1 1 d . . . C217 C 0.5465(4) 0.3365(3) 0.5259(3) 0.0572(16) Uani 1 1 d . . . H21A H 0.5855 0.3738 0.5189 0.086 Uiso 1 1 calc R . . H21B H 0.4909 0.3524 0.5162 0.086 Uiso 1 1 calc R . . H21C H 0.5603 0.2980 0.4978 0.086 Uiso 1 1 calc R . . C216 C 0.4984(3) 0.2626(3) 0.7582(3) 0.0454(12) Uani 1 1 d . . . H21D H 0.4618 0.2233 0.7529 0.068 Uiso 1 1 calc R . . H21E H 0.4674 0.3012 0.7758 0.068 Uiso 1 1 calc R . . H21F H 0.5428 0.2505 0.7877 0.068 Uiso 1 1 calc R . . C218 C 0.7023(3) 0.2857(2) 0.5913(2) 0.0354(10) Uani 1 1 d . . . H21G H 0.6961 0.2888 0.5442 0.042 Uiso 1 1 calc R . . H21H H 0.7233 0.2394 0.6014 0.042 Uiso 1 1 calc R . . N221 N 0.9168(2) 0.56216(19) 0.66202(18) 0.0271(8) Uani 1 1 d . . . N222 N 0.9309(2) 0.58438(18) 0.60181(17) 0.0267(7) Uani 1 1 d . . . C225 C 0.8888(3) 0.6110(2) 0.7013(2) 0.0320(9) Uani 1 1 d . . . C224 C 0.8828(3) 0.6694(2) 0.6647(2) 0.0340(10) Uani 1 1 d . . . H224 H 0.8644 0.7132 0.6783 0.041 Uiso 1 1 calc R . . C223 C 0.9093(3) 0.6510(2) 0.6034(2) 0.0313(9) Uani 1 1 d . . . C227 C 0.8674(4) 0.5992(3) 0.7707(2) 0.0447(12) Uani 1 1 d . . . H22A H 0.8236 0.5651 0.7737 0.067 Uiso 1 1 calc R . . H22B H 0.8488 0.6422 0.7900 0.067 Uiso 1 1 calc R . . H22C H 0.9159 0.5827 0.7937 0.067 Uiso 1 1 calc R . . C226 C 0.9147(3) 0.6937(3) 0.5436(2) 0.0428(12) Uani 1 1 d . . . H22D H 0.9460 0.6689 0.5109 0.064 Uiso 1 1 calc R . . H22E H 0.9422 0.7369 0.5534 0.064 Uiso 1 1 calc R . . H22F H 0.8594 0.7030 0.5275 0.064 Uiso 1 1 calc R . . C228 C 0.9394(3) 0.4909(2) 0.6776(2) 0.0284(9) Uani 1 1 d . . . H22G H 0.9445 0.4865 0.7247 0.034 Uiso 1 1 calc R . . H22H H 0.9938 0.4810 0.6587 0.034 Uiso 1 1 calc R . . C231 C 0.7652(3) 0.3382(2) 0.61286(19) 0.0279(9) Uani 1 1 d . . . C232 C 0.7406(3) 0.4040(2) 0.6248(2) 0.0296(9) Uani 1 1 d . . . H232 H 0.6845 0.4159 0.6199 0.036 Uiso 1 1 calc R . . C233 C 0.7978(3) 0.4545(2) 0.6442(2) 0.0278(9) Uani 1 1 d . . . H233 H 0.7800 0.5003 0.6506 0.033 Uiso 1 1 calc R . . C234 C 0.8790(3) 0.4379(2) 0.65381(19) 0.0251(8) Uani 1 1 d . . . C235 C 0.9060(3) 0.3694(2) 0.64262(19) 0.0251(8) Uani 1 1 d . . . C236 C 0.8489(3) 0.3200(2) 0.62016(19) 0.0277(9) Uani 1 1 d . . . C241 C 0.9881(3) 0.3496(2) 0.6537(2) 0.0307(9) Uani 1 1 d . . . H241 H 1.0256 0.3823 0.6701 0.037 Uiso 1 1 calc R . . C242 C 1.0152(3) 0.2843(3) 0.6415(2) 0.0365(11) Uani 1 1 d . . . H242 H 1.0707 0.2725 0.6494 0.044 Uiso 1 1 calc R . . C243 C 0.9606(3) 0.2353(2) 0.6175(2) 0.0386(11) Uani 1 1 d . . . H243 H 0.9789 0.1901 0.6088 0.046 Uiso 1 1 calc R . . C244 C 0.8792(3) 0.2536(3) 0.6065(2) 0.0344(9) Uani 1 1 d . . . H244 H 0.8428 0.2205 0.5892 0.041 Uiso 1 1 calc R . . N311 N 0.6648(2) 0.08819(18) 0.78909(18) 0.0290(8) Uani 1 1 d . . . N312 N 0.6747(2) 0.15427(19) 0.80982(18) 0.0298(8) Uani 1 1 d . . . C315 C 0.6363(3) 0.0465(2) 0.8357(2) 0.0335(10) Uani 1 1 d . . . C314 C 0.6264(3) 0.0877(3) 0.8895(2) 0.0365(10) Uani 1 1 d . . . H314 H 0.6070 0.0740 0.9305 0.044 Uiso 1 1 calc R . . C313 C 0.6507(3) 0.1532(2) 0.8710(2) 0.0316(9) Uani 1 1 d . . . C317 C 0.6199(3) -0.0277(3) 0.8261(3) 0.0482(12) Uani 1 1 d . . . H31A H 0.5769 -0.0334 0.7938 0.072 Uiso 1 1 calc R . . H31B H 0.6020 -0.0480 0.8667 0.072 Uiso 1 1 calc R . . H31C H 0.6701 -0.0504 0.8115 0.072 Uiso 1 1 calc R . . C316 C 0.6524(3) 0.2178(3) 0.9095(2) 0.0414(11) Uani 1 1 d . . . H31D H 0.6701 0.2558 0.8821 0.062 Uiso 1 1 calc R . . H31E H 0.6907 0.2127 0.9453 0.062 Uiso 1 1 calc R . . H31F H 0.5974 0.2273 0.9261 0.062 Uiso 1 1 calc R . . C318 C 0.6884(3) 0.0718(3) 0.7235(2) 0.0336(10) Uani 1 1 d . . . H31G H 0.6992 0.0221 0.7206 0.040 Uiso 1 1 calc R . . H31H H 0.7402 0.0959 0.7134 0.040 Uiso 1 1 calc R . . C321 C 0.6253(3) 0.0907(2) 0.6735(2) 0.0261(8) Uani 1 1 d . . . C322 C 0.5439(3) 0.0951(2) 0.6891(2) 0.0274(8) Uani 1 1 d . . . H322 H 0.5269 0.0864 0.7319 0.033 Uiso 1 1 calc R . . C323 C 0.4846(3) 0.1124(2) 0.6420(2) 0.0306(9) Uani 1 1 d . . . H323 H 0.4284 0.1139 0.6536 0.037 Uiso 1 1 calc R . . C324 C 0.5066(3) 0.1268(2) 0.5804(2) 0.0296(9) Uani 1 1 d . . . C325 C 0.5909(3) 0.1251(2) 0.5628(2) 0.0284(9) Uani 1 1 d . . . C326 C 0.6509(3) 0.1045(2) 0.6090(2) 0.0272(9) Uani 1 1 d . . . C331 C 0.6196(3) 0.1429(2) 0.5002(2) 0.0343(10) Uani 1 1 d . . . H331 H 0.5818 0.1592 0.4691 0.041 Uiso 1 1 calc R . . C332 C 0.7009(3) 0.1368(2) 0.4843(2) 0.0397(11) Uani 1 1 d . . . H332 H 0.7185 0.1490 0.4424 0.048 Uiso 1 1 calc R . . C333 C 0.7581(3) 0.1131(2) 0.5285(2) 0.0377(11) Uani 1 1 d . . . H333 H 0.8139 0.1080 0.5165 0.045 Uiso 1 1 calc R . . C334 C 0.7335(3) 0.0972(2) 0.5893(2) 0.0328(10) Uani 1 1 d . . . H334 H 0.7728 0.0808 0.6192 0.039 Uiso 1 1 calc R . . N411 N 1.1353(2) -0.04040(19) 1.02127(18) 0.0315(8) Uani 1 1 d . . . N412 N 1.1336(2) -0.1078(2) 1.03956(19) 0.0347(9) Uani 1 1 d . . . C413 C 1.2069(3) -0.1281(3) 1.0639(2) 0.0408(11) Uani 1 1 d . . . C414 C 1.2575(3) -0.0721(3) 1.0609(2) 0.0427(12) Uani 1 1 d . . . H414 H 1.3131 -0.0701 1.0741 0.051 Uiso 1 1 calc R . . C415 C 1.2111(3) -0.0185(3) 1.0346(2) 0.0366(10) Uani 1 1 d . . . C416 C 1.2205(4) -0.1984(3) 1.0879(3) 0.0583(16) Uani 1 1 d . . . H41F H 1.1837 -0.2073 1.1241 0.087 Uiso 1 1 calc R . . H41G H 1.2774 -0.2033 1.1020 0.087 Uiso 1 1 calc R . . H41H H 1.2093 -0.2312 1.0535 0.087 Uiso 1 1 calc R . . C417 C 1.2356(3) 0.0542(3) 1.0205(3) 0.0499(13) Uani 1 1 d . . . H41A H 1.2348 0.0619 0.9740 0.075 Uiso 1 1 calc R . . H41B H 1.2909 0.0626 1.0370 0.075 Uiso 1 1 calc R . . H41C H 1.1969 0.0855 1.0412 0.075 Uiso 1 1 calc R . . C418 C 1.0576(3) -0.1459(3) 1.0305(2) 0.0378(11) Uani 1 1 d . . . H41D H 1.0692 -0.1955 1.0335 0.045 Uiso 1 1 calc R . . H41E H 1.0358 -0.1365 0.9871 0.045 Uiso 1 1 calc R . . N1 N 0.7620(2) 0.8168(2) 0.77963(19) 0.0353(9) Uani 1 1 d . . . O1 O 0.7926(3) 0.8327(3) 0.8316(2) 0.0703(14) Uani 1 1 d . . . O2 O 0.6878(3) 0.8094(3) 0.7762(3) 0.0700(13) Uani 1 1 d . . . O3 O 0.8044(3) 0.8152(2) 0.7300(2) 0.0596(11) Uani 1 1 d . . . N2 N 0.5260(2) 0.96621(16) 0.05548(15) 0.0573(12) Uani 1 1 d D . . O4X O 0.4549(3) 0.9876(3) 0.0641(3) 0.0855(17) Uiso 0.849(6) 1 d PDU A 1 O5X O 0.5570(3) 0.9250(3) 0.0941(2) 0.0746(15) Uiso 0.849(6) 1 d PDU A 1 O6X O 0.5658(3) 0.9852(2) 0.0076(2) 0.0608(13) Uiso 0.849(6) 1 d PDU A 1 O4Y O 0.4917(10) 1.0078(4) 0.0190(6) 0.076(2) Uiso 0.151(6) 1 d PDU A 2 O5Y O 0.4888(10) 0.9437(7) 0.1033(4) 0.077(2) Uiso 0.151(6) 1 d PDU A 2 O6Y O 0.5974(3) 0.9469(7) 0.0440(8) 0.071(2) Uiso 0.151(6) 1 d PDU A 2 N1SX N 0.6616(9) 0.6057(7) 0.7167(7) 0.063(3) Uiso 0.402(3) 1 d PDU B 1 C2SX C 0.6714(8) 0.6540(6) 0.6860(6) 0.037(2) Uiso 0.402(3) 1 d PDU B 1 C3SX C 0.6800(7) 0.7168(5) 0.6398(5) 0.0264(19) Uiso 0.402(3) 1 d PDU B 1 H3S1 H 0.7188 0.7057 0.6055 0.040 Uiso 0.402(3) 1 calc PR B 1 H3S2 H 0.7001 0.7564 0.6639 0.040 Uiso 0.402(3) 1 calc PR B 1 H3S3 H 0.6264 0.7275 0.6211 0.040 Uiso 0.402(3) 1 calc PR B 1 N1SY N 0.5535(8) 0.6617(6) 0.5129(7) 0.045(3) Uiso 0.330(7) 1 d PD C 2 C2SY C 0.5661(8) 0.6150(6) 0.5380(6) 0.028(2) Uiso 0.330(7) 1 d PDU C 2 C3SY C 0.5797(8) 0.5476(6) 0.5716(7) 0.028(2) Uiso 0.330(7) 1 d PDU C 2 H3S4 H 0.5277 0.5311 0.5891 0.043 Uiso 0.330(7) 1 calc PR C 2 H3S5 H 0.6191 0.5539 0.6066 0.043 Uiso 0.330(7) 1 calc PR C 2 H3S6 H 0.6013 0.5142 0.5410 0.043 Uiso 0.330(7) 1 calc PR C 2 N1SZ N 0.6208(12) 0.5550(10) 0.7123(8) 0.058(3) Uiso 0.268(7) 1 d PDU D 3 C2SZ C 0.6012(10) 0.5457(8) 0.6662(7) 0.030(3) Uiso 0.268(7) 1 d PDU D 3 C3SZ C 0.5794(10) 0.5365(9) 0.5980(8) 0.031(2) Uiso 0.268(7) 1 d PDU D 3 H3S7 H 0.5589 0.5798 0.5807 0.046 Uiso 0.268(7) 1 calc PR D 3 H3S8 H 0.5367 0.5014 0.5943 0.046 Uiso 0.268(7) 1 calc PR D 3 H3S9 H 0.6279 0.5221 0.5739 0.046 Uiso 0.268(7) 1 calc PR D 3 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 0.02589(15) 0.03655(17) 0.03237(16) -0.00406(15) -0.00196(13) -0.00283(13) Ag2 0.02367(14) 0.03966(17) 0.03103(15) -0.00223(14) 0.00173(13) -0.00002(14) N111 0.0235(17) 0.0310(19) 0.0295(18) 0.0098(15) -0.0001(14) -0.0033(14) N112 0.0184(16) 0.0349(19) 0.0271(17) 0.0059(15) -0.0006(13) -0.0007(14) C115 0.026(2) 0.035(2) 0.029(2) 0.0119(18) -0.0018(17) -0.0125(18) C114 0.030(2) 0.029(2) 0.027(2) 0.0073(17) -0.0027(17) -0.0081(17) C113 0.031(2) 0.032(2) 0.0251(19) 0.0019(16) 0.0017(17) -0.0067(18) C117 0.025(2) 0.043(3) 0.055(3) 0.016(2) -0.009(2) -0.0059(19) C116 0.031(2) 0.043(3) 0.038(2) -0.003(2) -0.001(2) 0.000(2) C118 0.027(2) 0.030(2) 0.032(2) 0.0106(18) 0.0042(16) -0.0011(17) N121 0.0218(16) 0.0269(17) 0.0322(18) 0.0078(14) 0.0022(14) 0.0022(14) N122 0.0158(15) 0.0284(17) 0.0279(17) 0.0053(14) 0.0002(13) -0.0007(13) C125 0.025(2) 0.033(2) 0.034(2) 0.0077(18) 0.0056(17) 0.0007(17) C124 0.034(2) 0.032(2) 0.030(2) 0.0045(18) 0.0078(19) 0.0051(19) C123 0.027(2) 0.027(2) 0.031(2) 0.0068(17) 0.0024(17) -0.0038(17) C127 0.024(2) 0.053(3) 0.051(3) 0.008(2) 0.009(2) 0.006(2) C126 0.032(3) 0.049(3) 0.029(2) 0.001(2) 0.0003(18) -0.003(2) C128 0.0231(18) 0.032(2) 0.036(2) 0.0067(18) 0.0002(16) -0.0036(17) C131 0.0181(18) 0.032(2) 0.031(2) 0.0122(17) -0.0029(16) -0.0037(16) C132 0.027(2) 0.027(2) 0.035(2) 0.0022(18) -0.0025(18) -0.0009(17) C133 0.031(2) 0.030(2) 0.026(2) 0.0046(17) 0.0005(17) -0.0031(18) C134 0.0182(18) 0.024(2) 0.033(2) 0.0055(17) -0.0001(16) 0.0029(16) C135 0.0190(19) 0.026(2) 0.032(2) 0.0070(17) -0.0033(16) -0.0001(16) C136 0.0198(19) 0.032(2) 0.027(2) 0.0040(17) -0.0032(16) 0.0024(16) C141 0.020(2) 0.030(2) 0.038(2) 0.0015(17) -0.0042(17) -0.0024(16) C142 0.027(2) 0.027(2) 0.047(2) -0.0038(19) -0.0107(18) 0.0007(18) C143 0.027(2) 0.039(2) 0.035(2) -0.002(2) -0.0036(17) 0.008(2) C144 0.0212(19) 0.037(2) 0.034(2) 0.007(2) -0.0025(18) 0.0051(16) N211 0.035(2) 0.0288(19) 0.0316(19) -0.0003(15) -0.0038(16) -0.0087(15) N212 0.0278(18) 0.0256(17) 0.0342(19) -0.0008(14) -0.0044(15) -0.0046(14) C215 0.045(3) 0.026(2) 0.047(3) 0.0010(19) -0.022(2) -0.0055(19) C214 0.033(2) 0.031(2) 0.060(3) -0.003(2) -0.017(2) 0.0035(19) C213 0.032(2) 0.026(2) 0.042(2) -0.0068(18) -0.004(2) 0.0006(19) C217 0.077(4) 0.042(3) 0.053(3) 0.009(2) -0.019(3) -0.007(3) C216 0.030(2) 0.053(3) 0.053(3) -0.010(3) 0.008(2) -0.001(2) C218 0.043(3) 0.030(2) 0.033(2) -0.0039(18) -0.001(2) -0.007(2) N221 0.0224(17) 0.0292(18) 0.0298(18) 0.0020(15) 0.0004(14) -0.0057(14) N222 0.0282(18) 0.0262(18) 0.0259(17) 0.0019(14) -0.0051(14) -0.0071(14) C225 0.030(2) 0.033(2) 0.033(2) -0.0018(18) 0.0001(18) -0.0060(18) C224 0.034(2) 0.032(2) 0.036(2) -0.0020(19) -0.0002(19) -0.0018(19) C223 0.026(2) 0.028(2) 0.040(2) 0.0028(18) -0.0048(18) -0.0064(17) C227 0.046(3) 0.052(3) 0.036(3) 0.000(2) 0.009(2) -0.004(2) C226 0.051(3) 0.039(3) 0.038(3) 0.011(2) -0.006(2) -0.008(2) C228 0.028(2) 0.028(2) 0.029(2) 0.0016(16) -0.0013(16) -0.0010(16) C231 0.038(2) 0.026(2) 0.0199(18) 0.0022(15) 0.0015(16) -0.0085(17) C232 0.022(2) 0.038(2) 0.028(2) 0.0021(18) -0.0024(16) -0.0048(17) C233 0.027(2) 0.027(2) 0.030(2) -0.0002(16) -0.0001(17) -0.0035(17) C234 0.026(2) 0.026(2) 0.0237(19) 0.0047(16) -0.0002(16) -0.0019(16) C235 0.029(2) 0.028(2) 0.0182(18) 0.0027(15) 0.0015(16) -0.0044(17) C236 0.037(2) 0.027(2) 0.0192(18) 0.0039(16) 0.0020(17) 0.0008(18) C241 0.027(2) 0.036(2) 0.029(2) 0.0044(18) 0.0050(17) 0.0010(18) C242 0.035(3) 0.042(3) 0.033(2) 0.010(2) 0.0095(19) 0.012(2) C243 0.050(3) 0.035(3) 0.031(2) 0.0013(17) 0.009(2) 0.008(2) C244 0.049(3) 0.029(2) 0.0252(19) -0.0005(19) 0.0064(18) -0.002(2) N311 0.0292(19) 0.0251(18) 0.0328(19) -0.0064(15) -0.0102(15) -0.0028(14) N312 0.0311(19) 0.0269(18) 0.0313(19) -0.0046(15) -0.0070(15) -0.0035(15) C315 0.028(2) 0.034(2) 0.038(2) 0.0035(19) -0.0090(18) -0.0043(18) C314 0.037(3) 0.041(3) 0.032(2) 0.006(2) -0.0037(19) -0.005(2) C313 0.025(2) 0.035(2) 0.035(2) -0.0045(19) -0.0035(18) 0.0003(18) C317 0.047(3) 0.036(3) 0.061(3) 0.001(3) -0.013(2) -0.009(2) C316 0.051(3) 0.041(3) 0.032(2) -0.007(2) -0.001(2) 0.005(2) C318 0.028(2) 0.041(3) 0.032(2) -0.0081(19) -0.0078(17) 0.0043(18) C321 0.029(2) 0.024(2) 0.0253(19) -0.0070(16) -0.0086(17) 0.0025(16) C322 0.028(2) 0.027(2) 0.0274(19) -0.0046(15) -0.0062(17) 0.0004(17) C323 0.026(2) 0.032(2) 0.034(2) -0.0020(18) -0.0041(17) 0.0035(17) C324 0.034(2) 0.022(2) 0.032(2) -0.0020(16) -0.0099(18) 0.0051(17) C325 0.039(2) 0.0167(18) 0.030(2) -0.0051(16) -0.0033(18) -0.0033(17) C326 0.030(2) 0.0183(19) 0.033(2) -0.0072(16) -0.0030(17) -0.0012(16) C331 0.046(3) 0.025(2) 0.032(3) -0.0017(16) -0.0065(19) -0.0048(19) C332 0.055(3) 0.030(2) 0.034(2) -0.010(2) 0.009(2) -0.012(2) C333 0.036(2) 0.031(2) 0.046(3) -0.012(2) 0.007(2) -0.0061(19) C334 0.031(2) 0.030(2) 0.038(2) -0.0129(18) -0.0054(19) -0.0012(18) N411 0.0246(17) 0.038(2) 0.0323(19) 0.0063(16) 0.0072(15) 0.0036(15) N412 0.0273(19) 0.044(2) 0.0333(19) -0.0011(17) 0.0095(16) 0.0078(16) C413 0.040(3) 0.052(3) 0.031(2) 0.005(2) 0.007(2) 0.016(2) C414 0.027(2) 0.071(4) 0.031(2) 0.002(2) -0.0014(18) 0.012(2) C415 0.027(2) 0.055(3) 0.028(2) 0.004(2) 0.0022(17) 0.005(2) C416 0.064(4) 0.050(3) 0.061(3) 0.009(3) 0.011(3) 0.030(3) C417 0.037(3) 0.067(4) 0.045(3) 0.010(3) -0.009(2) -0.017(2) C418 0.038(2) 0.040(3) 0.036(2) -0.0085(19) 0.0099(19) 0.002(2) N1 0.0292(19) 0.041(2) 0.035(2) 0.0050(17) -0.0015(16) -0.0008(16) O1 0.083(3) 0.086(3) 0.041(2) 0.013(2) -0.013(2) -0.029(3) O2 0.035(2) 0.091(4) 0.084(3) 0.005(3) -0.002(2) -0.003(2) O3 0.066(3) 0.050(2) 0.063(3) -0.0171(19) 0.026(2) -0.015(2) N2 0.073(3) 0.050(3) 0.049(3) -0.008(2) -0.003(2) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N112 2.216(4) . ? Ag1 N212 2.247(4) . ? Ag1 N312 2.259(4) . ? Ag2 N122 2.228(3) . ? Ag2 N222 2.243(4) 3_746 ? Ag2 N411 2.269(4) . ? N111 C115 1.355(6) . ? N111 N112 1.364(5) . ? N111 C118 1.454(6) . ? N112 C113 1.325(6) . ? C115 C114 1.362(7) . ? C115 C117 1.499(6) . ? C114 C113 1.405(6) . ? C114 H114 0.9500 . ? C113 C116 1.501(7) . ? C117 H11A 0.9800 . ? C117 H11B 0.9800 . ? C117 H11C 0.9800 . ? C116 H11D 0.9800 . ? C116 H11E 0.9800 . ? C116 H11F 0.9800 . ? C118 C131 1.516(5) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? N121 C125 1.352(6) . ? N121 N122 1.360(5) . ? N121 C128 1.446(6) . ? N122 C123 1.331(6) . ? C125 C124 1.388(7) . ? C125 C127 1.487(6) . ? C124 C123 1.392(6) . ? C124 H124 0.9500 . ? C123 C126 1.492(6) . ? C127 H12A 0.9800 . ? C127 H12B 0.9800 . ? C127 H12C 0.9800 . ? C126 H12D 0.9800 . ? C126 H12E 0.9800 . ? C126 H12F 0.9800 . ? C128 C134 1.504(6) . ? C128 H12G 0.9900 . ? C128 H12H 0.9900 . ? C131 C132 1.367(6) . ? C131 C136 1.424(6) . ? C132 C133 1.415(6) . ? C132 H132 0.9500 . ? C133 C134 1.387(6) . ? C133 H133 0.9500 . ? C134 C135 1.421(6) . ? C135 C141 1.433(6) . ? C135 C136 1.444(6) . ? C136 C144 1.405(6) . ? C141 C142 1.374(7) . ? C141 H141 0.9500 . ? C142 C143 1.418(7) . ? C142 H142 0.9500 . ? C143 C144 1.381(7) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? N211 C215 1.364(6) . ? N211 N212 1.366(5) . ? N211 C218 1.444(6) . ? N212 C213 1.337(6) . ? C215 C214 1.364(8) . ? C215 C217 1.487(7) . ? C214 C213 1.412(7) . ? C214 H214 0.9500 . ? C213 C216 1.479(7) . ? C217 H21A 0.9800 . ? C217 H21B 0.9800 . ? C217 H21C 0.9800 . ? C216 H21D 0.9800 . ? C216 H21E 0.9800 . ? C216 H21F 0.9800 . ? C218 C231 1.520(6) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? N221 C225 1.340(6) . ? N221 N222 1.348(5) . ? N221 C228 1.479(5) . ? N222 C223 1.350(6) . ? N222 Ag2 2.243(4) 3_756 ? C225 C224 1.377(7) . ? C225 C227 1.508(7) . ? C224 C223 1.396(7) . ? C224 H224 0.9500 . ? C223 C226 1.504(6) . ? C227 H22A 0.9800 . ? C227 H22B 0.9800 . ? C227 H22C 0.9800 . ? C226 H22D 0.9800 . ? C226 H22E 0.9800 . ? C226 H22F 0.9800 . ? C228 C234 1.515(6) . ? C228 H22G 0.9900 . ? C228 H22H 0.9900 . ? C231 C232 1.371(6) . ? C231 C236 1.419(7) . ? C232 C233 1.420(6) . ? C232 H232 0.9500 . ? C233 C234 1.378(6) . ? C233 H233 0.9500 . ? C234 C235 1.430(6) . ? C235 C241 1.414(6) . ? C235 C236 1.422(6) . ? C236 C244 1.420(6) . ? C241 C242 1.375(7) . ? C241 H241 0.9500 . ? C242 C243 1.402(7) . ? C242 H242 0.9500 . ? C243 C244 1.395(7) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? N311 C315 1.351(6) . ? N311 N312 1.373(5) . ? N311 C318 1.457(6) . ? N312 C313 1.336(6) . ? C315 C314 1.390(7) . ? C315 C317 1.489(7) . ? C314 C313 1.396(7) . ? C314 H314 0.9500 . ? C313 C316 1.497(7) . ? C317 H31A 0.9800 . ? C317 H31B 0.9800 . ? C317 H31C 0.9800 . ? C316 H31D 0.9800 . ? C316 H31E 0.9800 . ? C316 H31F 0.9800 . ? C318 C321 1.511(6) . ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? C321 C322 1.370(6) . ? C321 C326 1.434(6) . ? C322 C323 1.420(6) . ? C322 H322 0.9500 . ? C323 C324 1.363(7) . ? C323 H323 0.9500 . ? C324 C325 1.424(7) . ? C324 C418 1.524(6) 2_654 ? C325 C331 1.429(6) . ? C325 C326 1.432(6) . ? C326 C334 1.417(6) . ? C331 C332 1.374(7) . ? C331 H331 0.9500 . ? C332 C333 1.390(8) . ? C332 H332 0.9500 . ? C333 C334 1.367(7) . ? C333 H333 0.9500 . ? C334 H334 0.9500 . ? N411 C415 1.339(6) . ? N411 N412 1.373(5) . ? N412 C413 1.359(6) . ? N412 C418 1.459(7) . ? C413 C414 1.372(8) . ? C413 C416 1.481(7) . ? C414 C415 1.405(7) . ? C414 H414 0.9500 . ? C415 C417 1.508(7) . ? C416 H41F 0.9800 . ? C416 H41G 0.9800 . ? C416 H41H 0.9800 . ? C417 H41A 0.9800 . ? C417 H41B 0.9800 . ? C417 H41C 0.9800 . ? C418 C324 1.524(6) 2_655 ? C418 H41D 0.9900 . ? C418 H41E 0.9900 . ? N1 O2 1.221(6) . ? N1 O1 1.234(6) . ? N1 O3 1.245(6) . ? N2 O4X 1.247(3) . ? N2 O6Y 1.247(3) . ? N2 O5X 1.247(3) . ? N2 O4Y 1.247(3) . ? N2 O5Y 1.247(3) . ? N2 O6X 1.248(3) . ? N1SX C2SX 1.151(14) . ? C2SX C3SX 1.568(12) . ? C3SX H3S1 0.9800 . ? C3SX H3S2 0.9800 . ? C3SX H3S3 0.9800 . ? N1SY C2SY 1.071(13) . ? C2SY C3SY 1.511(14) . ? C3SY H3S4 0.9800 . ? C3SY H3S5 0.9800 . ? C3SY H3S6 0.9800 . ? N1SZ C2SZ 1.030(16) . ? C2SZ C3SZ 1.476(15) . ? C3SZ H3S7 0.9800 . ? C3SZ H3S8 0.9800 . ? C3SZ H3S9 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 N112 Ag1 N212 122.99(13) . . ? N112 Ag1 N312 124.80(13) . . ? N212 Ag1 N312 109.20(13) . . ? N122 Ag2 N222 126.99(12) . 3_746 ? N122 Ag2 N411 119.32(12) . . ? N222 Ag2 N411 110.32(13) 3_746 . ? C115 N111 N112 110.8(4) . . ? C115 N111 C118 130.3(4) . . ? N112 N111 C118 118.9(4) . . ? C113 N112 N111 105.2(4) . . ? C113 N112 Ag1 128.5(3) . . ? N111 N112 Ag1 125.5(3) . . ? N111 C115 C114 107.8(4) . . ? N111 C115 C117 121.8(4) . . ? C114 C115 C117 130.4(5) . . ? C115 C114 C113 104.8(4) . . ? C115 C114 H114 127.6 . . ? C113 C114 H114 127.6 . . ? N112 C113 C114 111.4(4) . . ? N112 C113 C116 121.0(4) . . ? C114 C113 C116 127.7(4) . . ? C115 C117 H11A 109.5 . . ? C115 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C115 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C113 C116 H11D 109.5 . . ? C113 C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? C113 C116 H11F 109.5 . . ? H11D C116 H11F 109.5 . . ? H11E C116 H11F 109.5 . . ? N111 C118 C131 112.2(4) . . ? N111 C118 H11G 109.2 . . ? C131 C118 H11G 109.2 . . ? N111 C118 H11H 109.2 . . ? C131 C118 H11H 109.2 . . ? H11G C118 H11H 107.9 . . ? C125 N121 N122 111.0(4) . . ? C125 N121 C128 129.6(4) . . ? N122 N121 C128 119.2(3) . . ? C123 N122 N121 105.9(3) . . ? C123 N122 Ag2 126.7(3) . . ? N121 N122 Ag2 126.7(3) . . ? N121 C125 C124 106.8(4) . . ? N121 C125 C127 123.3(4) . . ? C124 C125 C127 129.9(4) . . ? C125 C124 C123 105.4(4) . . ? C125 C124 H124 127.3 . . ? C123 C124 H124 127.3 . . ? N122 C123 C124 110.9(4) . . ? N122 C123 C126 119.6(4) . . ? C124 C123 C126 129.6(4) . . ? C125 C127 H12A 109.5 . . ? C125 C127 H12B 109.5 . . ? H12A C127 H12B 109.5 . . ? C125 C127 H12C 109.5 . . ? H12A C127 H12C 109.5 . . ? H12B C127 H12C 109.5 . . ? C123 C126 H12D 109.5 . . ? C123 C126 H12E 109.5 . . ? H12D C126 H12E 109.5 . . ? C123 C126 H12F 109.5 . . ? H12D C126 H12F 109.5 . . ? H12E C126 H12F 109.5 . . ? N121 C128 C134 113.1(4) . . ? N121 C128 H12G 109.0 . . ? C134 C128 H12G 109.0 . . ? N121 C128 H12H 109.0 . . ? C134 C128 H12H 109.0 . . ? H12G C128 H12H 107.8 . . ? C132 C131 C136 120.5(4) . . ? C132 C131 C118 120.5(4) . . ? C136 C131 C118 119.1(4) . . ? C131 C132 C133 121.1(4) . . ? C131 C132 H132 119.5 . . ? C133 C132 H132 119.5 . . ? C134 C133 C132 120.7(4) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.5(4) . . ? C133 C134 C128 120.2(4) . . ? C135 C134 C128 120.3(4) . . ? C134 C135 C141 121.9(4) . . ? C134 C135 C136 119.7(4) . . ? C141 C135 C136 118.4(4) . . ? C144 C136 C131 123.3(4) . . ? C144 C136 C135 118.2(4) . . ? C131 C136 C135 118.4(4) . . ? C142 C141 C135 121.3(4) . . ? C142 C141 H141 119.4 . . ? C135 C141 H141 119.4 . . ? C141 C142 C143 119.8(4) . . ? C141 C142 H142 120.1 . . ? C143 C142 H142 120.1 . . ? C144 C143 C142 120.1(4) . . ? C144 C143 H143 119.9 . . ? C142 C143 H143 119.9 . . ? C143 C144 C136 121.9(4) . . ? C143 C144 H144 119.0 . . ? C136 C144 H144 119.0 . . ? C215 N211 N212 111.7(4) . . ? C215 N211 C218 129.5(4) . . ? N212 N211 C218 118.6(4) . . ? C213 N212 N211 105.3(4) . . ? C213 N212 Ag1 126.9(3) . . ? N211 N212 Ag1 127.2(3) . . ? N211 C215 C214 106.5(4) . . ? N211 C215 C217 120.9(5) . . ? C214 C215 C217 132.6(5) . . ? C215 C214 C213 106.3(4) . . ? C215 C214 H214 126.8 . . ? C213 C214 H214 126.8 . . ? N212 C213 C214 110.2(4) . . ? N212 C213 C216 121.0(4) . . ? C214 C213 C216 128.8(5) . . ? C215 C217 H21A 109.5 . . ? C215 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C215 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C213 C216 H21D 109.5 . . ? C213 C216 H21E 109.5 . . ? H21D C216 H21E 109.5 . . ? C213 C216 H21F 109.5 . . ? H21D C216 H21F 109.5 . . ? H21E C216 H21F 109.5 . . ? N211 C218 C231 114.0(4) . . ? N211 C218 H21G 108.8 . . ? C231 C218 H21G 108.8 . . ? N211 C218 H21H 108.8 . . ? C231 C218 H21H 108.8 . . ? H21G C218 H21H 107.7 . . ? C225 N221 N222 113.4(4) . . ? C225 N221 C228 128.6(4) . . ? N222 N221 C228 117.8(4) . . ? N221 N222 C223 104.1(4) . . ? N221 N222 Ag2 129.7(3) . 3_756 ? C223 N222 Ag2 126.0(3) . 3_756 ? N221 C225 C224 106.1(4) . . ? N221 C225 C227 123.8(4) . . ? C224 C225 C227 130.0(5) . . ? C225 C224 C223 105.7(4) . . ? C225 C224 H224 127.1 . . ? C223 C224 H224 127.1 . . ? N222 C223 C224 110.6(4) . . ? N222 C223 C226 120.0(4) . . ? C224 C223 C226 129.3(4) . . ? C225 C227 H22A 109.5 . . ? C225 C227 H22B 109.5 . . ? H22A C227 H22B 109.5 . . ? C225 C227 H22C 109.5 . . ? H22A C227 H22C 109.5 . . ? H22B C227 H22C 109.5 . . ? C223 C226 H22D 109.5 . . ? C223 C226 H22E 109.5 . . ? H22D C226 H22E 109.5 . . ? C223 C226 H22F 109.5 . . ? H22D C226 H22F 109.5 . . ? H22E C226 H22F 109.5 . . ? N221 C228 C234 114.3(3) . . ? N221 C228 H22G 108.7 . . ? C234 C228 H22G 108.7 . . ? N221 C228 H22H 108.7 . . ? C234 C228 H22H 108.7 . . ? H22G C228 H22H 107.6 . . ? C232 C231 C236 119.9(4) . . ? C232 C231 C218 119.3(4) . . ? C236 C231 C218 120.8(4) . . ? C231 C232 C233 120.9(4) . . ? C231 C232 H232 119.6 . . ? C233 C232 H232 119.6 . . ? C234 C233 C232 120.6(4) . . ? C234 C233 H233 119.7 . . ? C232 C233 H233 119.7 . . ? C233 C234 C235 119.6(4) . . ? C233 C234 C228 120.8(4) . . ? C235 C234 C228 119.6(4) . . ? C241 C235 C236 119.3(4) . . ? C241 C235 C234 121.5(4) . . ? C236 C235 C234 119.3(4) . . ? C231 C236 C244 122.9(4) . . ? C231 C236 C235 119.7(4) . . ? C244 C236 C235 117.4(4) . . ? C242 C241 C235 121.9(4) . . ? C242 C241 H241 119.0 . . ? C235 C241 H241 119.0 . . ? C241 C242 C243 119.8(4) . . ? C241 C242 H242 120.1 . . ? C243 C242 H242 120.1 . . ? C244 C243 C242 119.2(4) . . ? C244 C243 H243 120.4 . . ? C242 C243 H243 120.4 . . ? C243 C244 C236 122.3(4) . . ? C243 C244 H244 118.9 . . ? C236 C244 H244 118.9 . . ? C315 N311 N312 112.5(4) . . ? C315 N311 C318 129.3(4) . . ? N312 N311 C318 118.1(4) . . ? C313 N312 N311 104.6(4) . . ? C313 N312 Ag1 125.8(3) . . ? N311 N312 Ag1 129.4(3) . . ? N311 C315 C314 105.7(4) . . ? N311 C315 C317 123.6(5) . . ? C314 C315 C317 130.7(5) . . ? C315 C314 C313 106.1(4) . . ? C315 C314 H314 127.0 . . ? C313 C314 H314 127.0 . . ? N312 C313 C314 111.1(4) . . ? N312 C313 C316 119.5(4) . . ? C314 C313 C316 129.3(4) . . ? C315 C317 H31A 109.5 . . ? C315 C317 H31B 109.5 . . ? H31A C317 H31B 109.5 . . ? C315 C317 H31C 109.5 . . ? H31A C317 H31C 109.5 . . ? H31B C317 H31C 109.5 . . ? C313 C316 H31D 109.5 . . ? C313 C316 H31E 109.5 . . ? H31D C316 H31E 109.5 . . ? C313 C316 H31F 109.5 . . ? H31D C316 H31F 109.5 . . ? H31E C316 H31F 109.5 . . ? N311 C318 C321 114.4(4) . . ? N311 C318 H31G 108.7 . . ? C321 C318 H31G 108.7 . . ? N311 C318 H31H 108.7 . . ? C321 C318 H31H 108.7 . . ? H31G C318 H31H 107.6 . . ? C322 C321 C326 119.6(4) . . ? C322 C321 C318 120.9(4) . . ? C326 C321 C318 119.6(4) . . ? C321 C322 C323 120.7(4) . . ? C321 C322 H322 119.6 . . ? C323 C322 H322 119.6 . . ? C324 C323 C322 121.5(4) . . ? C324 C323 H323 119.3 . . ? C322 C323 H323 119.3 . . ? C323 C324 C325 119.5(4) . . ? C323 C324 C418 120.8(4) . 2_654 ? C325 C324 C418 119.7(4) . 2_654 ? C324 C325 C331 123.1(4) . . ? C324 C325 C326 119.6(4) . . ? C331 C325 C326 117.3(4) . . ? C334 C326 C325 118.9(4) . . ? C334 C326 C321 122.0(4) . . ? C325 C326 C321 119.0(4) . . ? C332 C331 C325 121.0(5) . . ? C332 C331 H331 119.5 . . ? C325 C331 H331 119.5 . . ? C331 C332 C333 121.2(5) . . ? C331 C332 H332 119.4 . . ? C333 C332 H332 119.4 . . ? C334 C333 C332 119.5(5) . . ? C334 C333 H333 120.2 . . ? C332 C333 H333 120.2 . . ? C333 C334 C326 121.7(5) . . ? C333 C334 H334 119.1 . . ? C326 C334 H334 119.1 . . ? C415 N411 N412 105.6(4) . . ? C415 N411 Ag2 125.6(3) . . ? N412 N411 Ag2 128.6(3) . . ? C413 N412 N411 111.5(4) . . ? C413 N412 C418 130.4(4) . . ? N411 N412 C418 118.2(4) . . ? N412 C413 C414 106.3(4) . . ? N412 C413 C416 121.9(5) . . ? C414 C413 C416 131.8(5) . . ? C413 C414 C415 106.8(4) . . ? C413 C414 H414 126.6 . . ? C415 C414 H414 126.6 . . ? N411 C415 C414 109.9(5) . . ? N411 C415 C417 120.4(4) . . ? C414 C415 C417 129.7(5) . . ? C413 C416 H41F 109.5 . . ? C413 C416 H41G 109.5 . . ? H41F C416 H41G 109.5 . . ? C413 C416 H41H 109.5 . . ? H41F C416 H41H 109.5 . . ? H41G C416 H41H 109.5 . . ? C415 C417 H41A 109.5 . . ? C415 C417 H41B 109.5 . . ? H41A C417 H41B 109.5 . . ? C415 C417 H41C 109.5 . . ? H41A C417 H41C 109.5 . . ? H41B C417 H41C 109.5 . . ? N412 C418 C324 111.8(4) . 2_655 ? N412 C418 H41D 109.3 . . ? C324 C418 H41D 109.3 2_655 . ? N412 C418 H41E 109.3 . . ? C324 C418 H41E 109.3 2_655 . ? H41D C418 H41E 107.9 . . ? O2 N1 O1 118.9(5) . . ? O2 N1 O3 120.0(5) . . ? O1 N1 O3 120.7(4) . . ? O4X N2 O6Y 176.7(9) . . ? O4X N2 O5X 120.06(7) . . ? O6Y N2 O5X 63.2(9) . . ? O4X N2 O4Y 56.7(9) . . ? O6Y N2 O4Y 120.02(7) . . ? O5X N2 O4Y 176.7(8) . . ? O4X N2 O5Y 63.3(9) . . ? O6Y N2 O5Y 120.01(7) . . ? O5X N2 O5Y 56.8(9) . . ? O4Y N2 O5Y 119.97(7) . . ? O4X N2 O6X 120.01(7) . . ? O6Y N2 O6X 56.7(8) . . ? O5X N2 O6X 119.92(7) . . ? O4Y N2 O6X 63.3(9) . . ? O5Y N2 O6X 176.2(8) . . ? N1SX C2SX C3SX 175.0(14) . . ? C2SX C3SX H3S1 109.5 . . ? C2SX C3SX H3S2 109.5 . . ? H3S1 C3SX H3S2 109.5 . . ? C2SX C3SX H3S3 109.5 . . ? H3S1 C3SX H3S3 109.5 . . ? H3S2 C3SX H3S3 109.5 . . ? N1SY C2SY C3SY 176.9(16) . . ? C2SY C3SY H3S4 109.5 . . ? C2SY C3SY H3S5 109.5 . . ? H3S4 C3SY H3S5 109.5 . . ? C2SY C3SY H3S6 109.5 . . ? H3S4 C3SY H3S6 109.5 . . ? H3S5 C3SY H3S6 109.5 . . ? N1SZ C2SZ C3SZ 175(2) . . ? C2SZ C3SZ H3S7 109.5 . . ? C2SZ C3SZ H3S8 109.5 . . ? H3S7 C3SZ H3S8 109.5 . . ? C2SZ C3SZ H3S9 109.5 . . ? H3S7 C3SZ H3S9 109.5 . . ? H3S8 C3SZ H3S9 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 C115 N111 N112 C113 -0.1(4) . . . . ? C118 N111 N112 C113 178.7(3) . . . . ? C115 N111 N112 Ag1 -170.7(3) . . . . ? C118 N111 N112 Ag1 8.0(5) . . . . ? N212 Ag1 N112 C113 49.3(4) . . . . ? N312 Ag1 N112 C113 -109.0(4) . . . . ? N212 Ag1 N112 N111 -142.3(3) . . . . ? N312 Ag1 N112 N111 59.5(4) . . . . ? N112 N111 C115 C114 0.4(5) . . . . ? C118 N111 C115 C114 -178.1(4) . . . . ? N112 N111 C115 C117 179.4(4) . . . . ? C118 N111 C115 C117 0.9(7) . . . . ? N111 C115 C114 C113 -0.6(5) . . . . ? C117 C115 C114 C113 -179.5(5) . . . . ? N111 N112 C113 C114 -0.3(5) . . . . ? Ag1 N112 C113 C114 170.0(3) . . . . ? N111 N112 C113 C116 179.4(4) . . . . ? Ag1 N112 C113 C116 -10.4(6) . . . . ? C115 C114 C113 N112 0.5(5) . . . . ? C115 C114 C113 C116 -179.1(4) . . . . ? C115 N111 C118 C131 100.3(5) . . . . ? N112 N111 C118 C131 -78.1(5) . . . . ? C125 N121 N122 C123 0.4(5) . . . . ? C128 N121 N122 C123 177.5(4) . . . . ? C125 N121 N122 Ag2 -170.5(3) . . . . ? C128 N121 N122 Ag2 6.7(5) . . . . ? N222 Ag2 N122 C123 -108.9(3) 3_746 . . . ? N411 Ag2 N122 C123 48.3(4) . . . . ? N222 Ag2 N122 N121 60.1(4) 3_746 . . . ? N411 Ag2 N122 N121 -142.7(3) . . . . ? N122 N121 C125 C124 -0.4(5) . . . . ? C128 N121 C125 C124 -177.2(4) . . . . ? N122 N121 C125 C127 179.9(4) . . . . ? C128 N121 C125 C127 3.2(7) . . . . ? N121 C125 C124 C123 0.3(5) . . . . ? C127 C125 C124 C123 179.9(5) . . . . ? N121 N122 C123 C124 -0.2(5) . . . . ? Ag2 N122 C123 C124 170.7(3) . . . . ? N121 N122 C123 C126 -179.0(4) . . . . ? Ag2 N122 C123 C126 -8.2(6) . . . . ? C125 C124 C123 N122 -0.1(5) . . . . ? C125 C124 C123 C126 178.6(5) . . . . ? C125 N121 C128 C134 103.0(5) . . . . ? N122 N121 C128 C134 -73.5(5) . . . . ? N111 C118 C131 C132 -27.3(6) . . . . ? N111 C118 C131 C136 152.9(4) . . . . ? C136 C131 C132 C133 0.4(6) . . . . ? C118 C131 C132 C133 -179.5(4) . . . . ? C131 C132 C133 C134 -3.0(7) . . . . ? C132 C133 C134 C135 1.5(6) . . . . ? C132 C133 C134 C128 -179.8(4) . . . . ? N121 C128 C134 C133 -26.0(5) . . . . ? N121 C128 C134 C135 152.7(4) . . . . ? C133 C134 C135 C141 -176.6(4) . . . . ? C128 C134 C135 C141 4.7(6) . . . . ? C133 C134 C135 C136 2.5(6) . . . . ? C128 C134 C135 C136 -176.2(4) . . . . ? C132 C131 C136 C144 -176.6(4) . . . . ? C118 C131 C136 C144 3.2(6) . . . . ? C132 C131 C136 C135 3.6(6) . . . . ? C118 C131 C136 C135 -176.6(4) . . . . ? C134 C135 C136 C144 175.2(4) . . . . ? C141 C135 C136 C144 -5.7(6) . . . . ? C134 C135 C136 C131 -5.0(6) . . . . ? C141 C135 C136 C131 174.2(4) . . . . ? C134 C135 C141 C142 -176.8(4) . . . . ? C136 C135 C141 C142 4.1(6) . . . . ? C135 C141 C142 C143 0.3(6) . . . . ? C141 C142 C143 C144 -3.2(6) . . . . ? C142 C143 C144 C136 1.4(6) . . . . ? C131 C136 C144 C143 -176.8(4) . . . . ? C135 C136 C144 C143 3.0(6) . . . . ? C215 N211 N212 C213 -0.2(5) . . . . ? C218 N211 N212 C213 -174.9(4) . . . . ? C215 N211 N212 Ag1 -172.0(3) . . . . ? C218 N211 N212 Ag1 13.3(5) . . . . ? N112 Ag1 N212 C213 -109.1(4) . . . . ? N312 Ag1 N212 C213 52.1(4) . . . . ? N112 Ag1 N212 N211 61.0(4) . . . . ? N312 Ag1 N212 N211 -137.8(3) . . . . ? N212 N211 C215 C214 0.6(5) . . . . ? C218 N211 C215 C214 174.5(4) . . . . ? N212 N211 C215 C217 -178.6(4) . . . . ? C218 N211 C215 C217 -4.7(7) . . . . ? N211 C215 C214 C213 -0.7(5) . . . . ? C217 C215 C214 C213 178.4(5) . . . . ? N211 N212 C213 C214 -0.2(5) . . . . ? Ag1 N212 C213 C214 171.6(3) . . . . ? N211 N212 C213 C216 177.6(4) . . . . ? Ag1 N212 C213 C216 -10.6(6) . . . . ? C215 C214 C213 N212 0.6(5) . . . . ? C215 C214 C213 C216 -177.0(5) . . . . ? C215 N211 C218 C231 111.0(5) . . . . ? N212 N211 C218 C231 -75.5(5) . . . . ? C225 N221 N222 C223 -0.8(5) . . . . ? C228 N221 N222 C223 -176.3(3) . . . . ? C225 N221 N222 Ag2 -175.5(3) . . . 3_756 ? C228 N221 N222 Ag2 9.1(5) . . . 3_756 ? N222 N221 C225 C224 0.8(5) . . . . ? C228 N221 C225 C224 175.7(4) . . . . ? N222 N221 C225 C227 179.2(4) . . . . ? C228 N221 C225 C227 -5.9(7) . . . . ? N221 C225 C224 C223 -0.4(5) . . . . ? C227 C225 C224 C223 -178.8(5) . . . . ? N221 N222 C223 C224 0.5(5) . . . . ? Ag2 N222 C223 C224 175.4(3) 3_756 . . . ? N221 N222 C223 C226 -178.6(4) . . . . ? Ag2 N222 C223 C226 -3.7(6) 3_756 . . . ? C225 C224 C223 N222 -0.1(5) . . . . ? C225 C224 C223 C226 179.0(5) . . . . ? C225 N221 C228 C234 107.1(5) . . . . ? N222 N221 C228 C234 -78.2(5) . . . . ? N211 C218 C231 C232 -36.1(6) . . . . ? N211 C218 C231 C236 144.5(4) . . . . ? C236 C231 C232 C233 0.2(6) . . . . ? C218 C231 C232 C233 -179.2(4) . . . . ? C231 C232 C233 C234 -2.4(6) . . . . ? C232 C233 C234 C235 1.5(6) . . . . ? C232 C233 C234 C228 -177.1(4) . . . . ? N221 C228 C234 C233 -25.8(6) . . . . ? N221 C228 C234 C235 155.6(4) . . . . ? C233 C234 C235 C241 -178.1(4) . . . . ? C228 C234 C235 C241 0.5(6) . . . . ? C233 C234 C235 C236 1.6(6) . . . . ? C228 C234 C235 C236 -179.9(4) . . . . ? C232 C231 C236 C244 -177.7(4) . . . . ? C218 C231 C236 C244 1.7(6) . . . . ? C232 C231 C236 C235 2.9(6) . . . . ? C218 C231 C236 C235 -177.7(4) . . . . ? C241 C235 C236 C231 175.9(4) . . . . ? C234 C235 C236 C231 -3.8(6) . . . . ? C241 C235 C236 C244 -3.6(6) . . . . ? C234 C235 C236 C244 176.7(4) . . . . ? C236 C235 C241 C242 2.1(6) . . . . ? C234 C235 C241 C242 -178.2(4) . . . . ? C235 C241 C242 C243 -0.1(7) . . . . ? C241 C242 C243 C244 -0.2(6) . . . . ? C242 C243 C244 C236 -1.5(6) . . . . ? C231 C236 C244 C243 -176.1(4) . . . . ? C235 C236 C244 C243 3.4(6) . . . . ? C315 N311 N312 C313 -0.7(5) . . . . ? C318 N311 N312 C313 -178.2(4) . . . . ? C315 N311 N312 Ag1 -175.7(3) . . . . ? C318 N311 N312 Ag1 6.8(5) . . . . ? N112 Ag1 N312 C313 53.4(4) . . . . ? N212 Ag1 N312 C313 -107.4(4) . . . . ? N112 Ag1 N312 N311 -132.6(3) . . . . ? N212 Ag1 N312 N311 66.7(4) . . . . ? N312 N311 C315 C314 0.6(5) . . . . ? C318 N311 C315 C314 177.8(4) . . . . ? N312 N311 C315 C317 179.9(4) . . . . ? C318 N311 C315 C317 -2.9(7) . . . . ? N311 C315 C314 C313 -0.3(5) . . . . ? C317 C315 C314 C313 -179.5(5) . . . . ? N311 N312 C313 C314 0.5(5) . . . . ? Ag1 N312 C313 C314 175.7(3) . . . . ? N311 N312 C313 C316 -179.3(4) . . . . ? Ag1 N312 C313 C316 -4.1(6) . . . . ? C315 C314 C313 N312 -0.1(5) . . . . ? C315 C314 C313 C316 179.6(5) . . . . ? C315 N311 C318 C321 102.1(5) . . . . ? N312 N311 C318 C321 -80.9(5) . . . . ? N311 C318 C321 C322 -25.7(6) . . . . ? N311 C318 C321 C326 154.1(4) . . . . ? C326 C321 C322 C323 0.7(6) . . . . ? C318 C321 C322 C323 -179.6(4) . . . . ? C321 C322 C323 C324 -1.6(6) . . . . ? C322 C323 C324 C325 -0.6(6) . . . . ? C322 C323 C324 C418 -179.4(4) . . . 2_654 ? C323 C324 C325 C331 -176.7(4) . . . . ? C418 C324 C325 C331 2.1(6) 2_654 . . . ? C323 C324 C325 C326 3.6(6) . . . . ? C418 C324 C325 C326 -177.6(4) 2_654 . . . ? C324 C325 C326 C334 174.4(4) . . . . ? C331 C325 C326 C334 -5.3(6) . . . . ? C324 C325 C326 C321 -4.4(6) . . . . ? C331 C325 C326 C321 175.8(4) . . . . ? C322 C321 C326 C334 -176.5(4) . . . . ? C318 C321 C326 C334 3.7(6) . . . . ? C322 C321 C326 C325 2.3(6) . . . . ? C318 C321 C326 C325 -177.5(4) . . . . ? C324 C325 C331 C332 -176.3(4) . . . . ? C326 C325 C331 C332 3.5(6) . . . . ? C325 C331 C332 C333 0.0(7) . . . . ? C331 C332 C333 C334 -1.7(7) . . . . ? C332 C333 C334 C326 -0.3(7) . . . . ? C325 C326 C334 C333 3.9(6) . . . . ? C321 C326 C334 C333 -177.3(4) . . . . ? N122 Ag2 N411 C415 -107.6(4) . . . . ? N222 Ag2 N411 C415 53.1(4) 3_746 . . . ? N122 Ag2 N411 N412 65.6(4) . . . . ? N222 Ag2 N411 N412 -133.7(3) 3_746 . . . ? C415 N411 N412 C413 0.0(5) . . . . ? Ag2 N411 N412 C413 -174.3(3) . . . . ? C415 N411 N412 C418 -179.8(4) . . . . ? Ag2 N411 N412 C418 6.0(6) . . . . ? N411 N412 C413 C414 -0.2(5) . . . . ? C418 N412 C413 C414 179.5(4) . . . . ? N411 N412 C413 C416 179.1(4) . . . . ? C418 N412 C413 C416 -1.2(8) . . . . ? N412 C413 C414 C415 0.4(5) . . . . ? C416 C413 C414 C415 -178.8(5) . . . . ? N412 N411 C415 C414 0.3(5) . . . . ? Ag2 N411 C415 C414 174.8(3) . . . . ? N412 N411 C415 C417 179.9(4) . . . . ? Ag2 N411 C415 C417 -5.6(6) . . . . ? C413 C414 C415 N411 -0.5(5) . . . . ? C413 C414 C415 C417 180.0(5) . . . . ? C413 N412 C418 C324 105.0(5) . . . 2_655 ? N411 N412 C418 C324 -75.3(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.988 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.097 #===END data_imw1192cubic _database_code_depnum_ccdc_archive 'CCDC 797108' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H72 Ag2 F12 N12 P2' _chemical_formula_weight 1539.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P4(1)32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' _cell_length_a 19.8931(6) _cell_length_b 19.8931(6) _cell_length_c 19.8931(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7872.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.64 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7926 _exptl_absorpt_correction_T_max 0.8383 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 147176 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.38 _reflns_number_total 3307 _reflns_number_gt 2386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. All hydrogens were added in calculated positions. The structure contains a disordered PF6 anion (P1 F1 > F6). The ion sits on a special position and exhibits rotational disorder about the F1-P1-F2 pivot causing the equitorial fluorines to be dosordered over three sites. The model had beneffited from the application of geometric and displacement restraints. 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^)+(0.1899P)^2^+11.6538P] 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 -0.18(14) _refine_ls_number_reflns 3307 _refine_ls_number_parameters 146 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.3221 _refine_ls_wR_factor_gt 0.2651 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.232 _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 1.00297(3) 0.00297(3) 0.00297(3) 0.0606(4) Uani 1 3 d S . . N111 N 0.9567(3) -0.0403(3) 0.1536(3) 0.0531(13) Uani 1 1 d . . . N112 N 0.9669(3) -0.0598(3) 0.0895(3) 0.0556(14) Uani 1 1 d . . . C113 C 0.9435(4) -0.1226(4) 0.0862(5) 0.066(2) Uani 1 1 d . . . C114 C 0.9173(4) -0.1407(4) 0.1504(5) 0.071(2) Uani 1 1 d . . . H114 H 0.8972 -0.1824 0.1621 0.085 Uiso 1 1 calc R . . C115 C 0.9262(4) -0.0881(3) 0.1909(4) 0.0556(16) Uani 1 1 d . . . C116 C 0.9466(7) -0.1625(5) 0.0223(6) 0.095(3) Uani 1 1 d . . . H11A H 0.9021 -0.1812 0.0124 0.143 Uiso 1 1 calc R . . H11B H 0.9790 -0.1993 0.0274 0.143 Uiso 1 1 calc R . . H11C H 0.9607 -0.1332 -0.0147 0.143 Uiso 1 1 calc R . . C117 C 0.9079(5) -0.0782(5) 0.2630(5) 0.072(2) Uani 1 1 d . . . H11D H 0.9485 -0.0679 0.2890 0.108 Uiso 1 1 calc R . . H11E H 0.8872 -0.1193 0.2805 0.108 Uiso 1 1 calc R . . H11F H 0.8760 -0.0408 0.2669 0.108 Uiso 1 1 calc R . . C118 C 0.9744(3) 0.0279(3) 0.1719(4) 0.0519(14) Uani 1 1 d . . . H11G H 1.0189 0.0388 0.1526 0.062 Uiso 1 1 calc R . . H11H H 0.9783 0.0307 0.2215 0.062 Uiso 1 1 calc R . . C121 C 0.9238(3) 0.0800(3) 0.1482(3) 0.0440(12) Uani 1 1 d . . . C122 C 0.8600(3) 0.0616(3) 0.1364(4) 0.0510(15) Uani 1 1 d . . . H122 H 0.8468 0.0162 0.1432 0.061 Uiso 1 1 calc R . . C123 C 0.9450(3) 0.1476(3) 0.1378(3) 0.0406(12) Uani 1 1 d . . . C131 C 1.0311(3) 0.2349(3) 0.1395(3) 0.0485(14) Uani 1 1 d . . . H131 H 1.0755 0.2491 0.1499 0.058 Uiso 1 1 calc R . . C132 C 1.0119(3) 0.1699(3) 0.1525(3) 0.0455(13) Uani 1 1 d . . . H132 H 1.0434 0.1393 0.1714 0.055 Uiso 1 1 calc R . . P1 P 0.47397(11) 0.02603(11) 0.97397(11) 0.0655(9) Uiso 1 3 d SD . . F1 F 0.5174(4) -0.0174(4) 1.0174(4) 0.208(10) Uiso 1 3 d SD A . F2 F 0.4276(2) 0.0724(2) 0.9276(2) 0.086(3) Uiso 1 3 d SD A . F3 F 0.5367(8) 0.0710(13) 0.9615(16) 0.086(7) Uiso 0.287(15) 1 d PDU A 1 F4 F 0.5220(16) 0.0867(9) 0.986(2) 0.096(8) Uiso 0.287(15) 1 d PDU A 1 F5 F 0.4899(16) 0.0943(6) 1.0120(13) 0.101(6) Uiso 0.380(15) 1 d PDU A 2 F6 F 0.4557(16) 0.0781(12) 1.0327(8) 0.117(7) Uiso 0.380(15) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0606(4) 0.0606(4) 0.0606(4) 0.0018(2) 0.0018(2) 0.0018(2) N111 0.050(3) 0.049(3) 0.060(3) 0.008(2) 0.002(2) 0.007(2) N112 0.054(3) 0.050(3) 0.063(3) 0.001(2) -0.001(3) 0.009(2) C113 0.074(5) 0.048(4) 0.076(5) 0.008(3) 0.001(4) 0.001(3) C114 0.073(5) 0.049(4) 0.089(6) 0.009(4) 0.003(4) 0.001(4) C115 0.051(4) 0.048(3) 0.068(4) 0.014(3) 0.003(3) 0.006(3) C116 0.124(9) 0.065(5) 0.097(7) -0.015(5) -0.007(7) 0.002(6) C117 0.079(5) 0.065(5) 0.073(5) 0.012(4) 0.012(4) 0.003(4) C118 0.045(3) 0.046(3) 0.064(4) 0.007(3) -0.002(3) 0.006(3) C121 0.039(3) 0.045(3) 0.049(3) 0.002(2) -0.004(2) 0.008(2) C122 0.042(3) 0.041(3) 0.070(4) 0.010(3) 0.000(3) 0.005(3) C123 0.039(3) 0.043(3) 0.040(3) -0.002(2) 0.001(2) -0.001(2) C131 0.040(3) 0.056(3) 0.050(3) -0.004(3) 0.003(2) -0.004(3) C132 0.043(3) 0.047(3) 0.047(3) -0.006(2) 0.002(2) -0.003(2) _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 N112 2.244(6) . ? Ag1 N112 2.244(6) 9_654 ? Ag1 N112 2.244(6) 5_645 ? N111 N112 1.348(9) . ? N111 C115 1.351(9) . ? N111 C118 1.448(9) . ? N112 C113 1.336(10) . ? C113 C114 1.425(12) . ? C113 C116 1.500(14) . ? C114 C115 1.333(11) . ? C114 H114 0.9500 . ? C115 C117 1.493(11) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C118 C121 1.520(8) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.342(9) . ? C121 C123 1.425(8) . ? C122 C122 1.437(12) 13_545 ? C122 H122 0.9500 . ? C123 C123 1.426(12) 13_545 ? C123 C132 1.433(8) . ? C131 C132 1.373(9) . ? C131 C131 1.421(13) 13_545 ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? P1 F1 1.497(14) . ? P1 F3 1.556(12) 6_456 ? P1 F3 1.556(12) . ? P1 F3 1.556(12) 12_565 ? P1 F4 1.557(12) . ? P1 F4 1.557(12) 6_456 ? P1 F4 1.557(12) 12_565 ? P1 F5 1.587(11) . ? P1 F5 1.587(11) 6_456 ? P1 F5 1.587(11) 12_565 ? P1 F2 1.598(9) . ? P1 F6 1.603(12) 12_565 ? F3 F4 0.64(4) . ? F5 F6 0.86(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N112 Ag1 N112 119.61(4) . 9_654 ? N112 Ag1 N112 119.61(4) . 5_645 ? N112 Ag1 N112 119.61(4) 9_654 5_645 ? N112 N111 C115 112.6(6) . . ? N112 N111 C118 118.2(6) . . ? C115 N111 C118 129.0(6) . . ? C113 N112 N111 105.3(6) . . ? C113 N112 Ag1 126.5(6) . . ? N111 N112 Ag1 127.8(4) . . ? N112 C113 C114 108.7(8) . . ? N112 C113 C116 121.5(8) . . ? C114 C113 C116 129.8(8) . . ? C115 C114 C113 107.1(7) . . ? C115 C114 H114 126.4 . . ? C113 C114 H114 126.4 . . ? C114 C115 N111 106.3(7) . . ? C114 C115 C117 130.7(7) . . ? N111 C115 C117 123.0(7) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C115 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? N111 C118 C121 113.6(6) . . ? N111 C118 H11G 108.9 . . ? C121 C118 H11G 108.9 . . ? N111 C118 H11H 108.9 . . ? C121 C118 H11H 108.9 . . ? H11G C118 H11H 107.7 . . ? C122 C121 C123 120.8(5) . . ? C122 C121 C118 119.6(6) . . ? C123 C121 C118 119.6(5) . . ? C121 C122 C122 120.4(4) . 13_545 ? C121 C122 H122 119.8 . . ? C122 C122 H122 119.8 13_545 . ? C121 C123 C123 118.7(3) . 13_545 ? C121 C123 C132 122.4(5) . . ? C123 C123 C132 118.9(4) 13_545 . ? C132 C131 C131 120.4(4) . 13_545 ? C132 C131 H131 119.8 . . ? C131 C131 H131 119.8 13_545 . ? C131 C132 C123 120.7(6) . . ? C131 C132 H132 119.7 . . ? C123 C132 H132 119.7 . . ? F1 P1 F3 87.8(4) . 6_456 ? F1 P1 F3 87.8(4) . . ? F3 P1 F3 119.85(6) 6_456 . ? F1 P1 F3 87.8(4) . 12_565 ? F3 P1 F3 119.85(6) 6_456 12_565 ? F3 P1 F3 119.85(6) . 12_565 ? F1 P1 F4 90.4(4) . . ? F3 P1 F4 143.7(14) 6_456 . ? F3 P1 F4 23.9(14) . . ? F3 P1 F4 96.2(14) 12_565 . ? F1 P1 F4 90.4(4) . 6_456 ? F3 P1 F4 23.9(14) 6_456 6_456 ? F3 P1 F4 96.2(14) . 6_456 ? F3 P1 F4 143.7(14) 12_565 6_456 ? F4 P1 F4 119.996(19) . 6_456 ? F1 P1 F4 90.4(4) . 12_565 ? F3 P1 F4 96.2(14) 6_456 12_565 ? F3 P1 F4 143.7(14) . 12_565 ? F3 P1 F4 23.9(14) 12_565 12_565 ? F4 P1 F4 119.996(9) . 12_565 ? F4 P1 F4 119.996(17) 6_456 12_565 ? F1 P1 F5 96.0(4) . . ? F3 P1 F5 173.1(12) 6_456 . ? F3 P1 F5 54.7(13) . . ? F3 P1 F5 66.2(13) 12_565 . ? F4 P1 F5 30.9(11) . . ? F4 P1 F5 149.8(11) 6_456 . ? F4 P1 F5 89.5(11) 12_565 . ? F1 P1 F5 96.0(4) . 6_456 ? F3 P1 F5 54.7(13) 6_456 6_456 ? F3 P1 F5 66.2(13) . 6_456 ? F3 P1 F5 173.1(12) 12_565 6_456 ? F4 P1 F5 89.5(11) . 6_456 ? F4 P1 F5 30.9(11) 6_456 6_456 ? F4 P1 F5 149.8(11) 12_565 6_456 ? F5 P1 F5 118.94(15) . 6_456 ? F1 P1 F5 96.0(4) . 12_565 ? F3 P1 F5 66.2(13) 6_456 12_565 ? F3 P1 F5 173.1(12) . 12_565 ? F3 P1 F5 54.7(13) 12_565 12_565 ? F4 P1 F5 149.8(11) . 12_565 ? F4 P1 F5 89.5(11) 6_456 12_565 ? F4 P1 F5 30.9(11) 12_565 12_565 ? F5 P1 F5 118.94(15) . 12_565 ? F5 P1 F5 118.94(15) 6_456 12_565 ? F1 P1 F2 180.0(5) . . ? F3 P1 F2 92.2(4) 6_456 . ? F3 P1 F2 92.2(4) . . ? F3 P1 F2 92.2(4) 12_565 . ? F4 P1 F2 89.6(4) . . ? F4 P1 F2 89.6(4) 6_456 . ? F4 P1 F2 89.6(4) 12_565 . ? F5 P1 F2 84.0(4) . . ? F5 P1 F2 84.0(4) 6_456 . ? F5 P1 F2 84.0(4) 12_565 . ? F1 P1 F6 94.8(5) . 12_565 ? F3 P1 F6 35.1(11) 6_456 12_565 ? F3 P1 F6 154.4(11) . 12_565 ? F3 P1 F6 85.8(11) 12_565 12_565 ? F4 P1 F6 174.6(7) . 12_565 ? F4 P1 F6 58.3(16) 6_456 12_565 ? F4 P1 F6 61.9(16) 12_565 12_565 ? F5 P1 F6 149.5(12) . 12_565 ? F5 P1 F6 88.2(12) 6_456 12_565 ? F5 P1 F6 31.2(12) 12_565 12_565 ? F2 P1 F6 85.2(5) . 12_565 ? F4 F3 P1 78.1(15) . . ? F3 F4 P1 78.0(15) . . ? F6 F5 P1 75.4(11) . . ? F5 F6 P1 73.3(11) . . ? 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 C115 N111 N112 C113 -1.5(8) . . . . ? C118 N111 N112 C113 -177.0(6) . . . . ? C115 N111 N112 Ag1 171.5(4) . . . . ? C118 N111 N112 Ag1 -4.1(8) . . . . ? N112 Ag1 N112 C113 107.9(6) 9_654 . . . ? N112 Ag1 N112 C113 -59.7(7) 5_645 . . . ? N112 Ag1 N112 N111 -63.7(7) 9_654 . . . ? N112 Ag1 N112 N111 128.8(5) 5_645 . . . ? N111 N112 C113 C114 1.1(8) . . . . ? Ag1 N112 C113 C114 -172.0(5) . . . . ? N111 N112 C113 C116 -179.3(9) . . . . ? Ag1 N112 C113 C116 7.6(12) . . . . ? N112 C113 C114 C115 -0.5(9) . . . . ? C116 C113 C114 C115 180.0(10) . . . . ? C113 C114 C115 N111 -0.4(9) . . . . ? C113 C114 C115 C117 179.2(8) . . . . ? N112 N111 C115 C114 1.2(8) . . . . ? C118 N111 C115 C114 176.2(7) . . . . ? N112 N111 C115 C117 -178.5(7) . . . . ? C118 N111 C115 C117 -3.5(11) . . . . ? N112 N111 C118 C121 76.6(8) . . . . ? C115 N111 C118 C121 -98.2(8) . . . . ? N111 C118 C121 C122 24.1(9) . . . . ? N111 C118 C121 C123 -154.9(6) . . . . ? C123 C121 C122 C122 -0.7(13) . . . 13_545 ? C118 C121 C122 C122 -179.7(8) . . . 13_545 ? C122 C121 C123 C123 -2.2(11) . . . 13_545 ? C118 C121 C123 C123 176.8(7) . . . 13_545 ? C122 C121 C123 C132 177.4(6) . . . . ? C118 C121 C123 C132 -3.6(9) . . . . ? C131 C131 C132 C123 -0.7(11) 13_545 . . . ? C121 C123 C132 C131 177.7(6) . . . . ? C123 C123 C132 C131 -2.8(10) 13_545 . . . ? F1 P1 F3 F4 -96.0(7) . . . . ? F3 P1 F3 F4 177.9(8) 6_456 . . . ? F3 P1 F3 F4 -9.9(12) 12_565 . . . ? F4 P1 F3 F4 173.9(10) 6_456 . . . ? F4 P1 F3 F4 -8.4(13) 12_565 . . . ? F5 P1 F3 F4 2.9(7) . . . . ? F5 P1 F3 F4 166.5(10) 6_456 . . . ? F5 P1 F3 F4 27(8) 12_565 . . . ? F2 P1 F3 F4 84.0(7) . . . . ? F6 P1 F3 F4 167.7(16) 12_565 . . . ? F1 P1 F4 F3 83.6(7) . . . . ? F3 P1 F4 F3 -3.1(12) 6_456 . . . ? F3 P1 F4 F3 171.4(10) 12_565 . . . ? F4 P1 F4 F3 -7.0(11) 6_456 . . . ? F4 P1 F4 F3 174.3(9) 12_565 . . . ? F5 P1 F4 F3 -175.3(11) . . . . ? F5 P1 F4 F3 -12.3(9) 6_456 . . . ? F5 P1 F4 F3 -173.8(13) 12_565 . . . ? F2 P1 F4 F3 -96.4(7) . . . . ? F6 P1 F4 F3 -77(17) 12_565 . . . ? F1 P1 F5 F6 -89.4(11) . . . . ? F3 P1 F5 F6 148(7) 6_456 . . . ? F3 P1 F5 F6 -172.4(13) . . . . ? F3 P1 F5 F6 -4.5(11) 12_565 . . . ? F4 P1 F5 F6 -170.0(17) . . . . ? F4 P1 F5 F6 169.6(14) 6_456 . . . ? F4 P1 F5 F6 0.9(12) 12_565 . . . ? F5 P1 F5 F6 170.4(9) 6_456 . . . ? F5 P1 F5 F6 10.8(16) 12_565 . . . ? F2 P1 F5 F6 90.6(11) . . . . ? F6 P1 F5 F6 20.6(15) 12_565 . . . ? F1 P1 F6 F5 93.6(11) . . . . ? F3 P1 F6 F5 -171.6(14) 6_456 . . . ? F3 P1 F6 F5 6.3(11) . . . . ? F3 P1 F6 F5 172.9(18) 12_565 . . . ? F4 P1 F6 F5 5.8(10) . . . . ? F4 P1 F6 F5 -106(17) 6_456 . . . ? F4 P1 F6 F5 -178.9(14) 12_565 . . . ? F5 P1 F6 F5 -16.6(17) 6_456 . . . ? F5 P1 F6 F5 -170.5(14) 12_565 . . . ? F2 P1 F6 F5 -86.4(11) . . . . ? F6 P1 F6 F5 -168.2(8) 12_565 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.907 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.128 #===END data_imw1193p21n_0802s6_unknown_solv _database_code_depnum_ccdc_archive 'CCDC 797109' #TrackingRef '- Ward_silvernetworks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Ag N5 O3' _chemical_formula_weight 514.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0339(8) _cell_length_b 12.3064(9) _cell_length_c 17.8158(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.880(3) _cell_angle_gamma 90.00 _cell_volume 2135.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9045 _cell_measurement_theta_min 2.355 _cell_measurement_theta_max 27.451 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7579 _exptl_absorpt_correction_T_max 0.8284 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36979 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4373 _reflns_number_gt 3916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data processing was carried out to a resolution of 0.8 Angstroms as the data was only complete to this resolution. The uncoordinated oxgen atom (O13) of the nitrate anion (N11 O11 O12 O13) has a larger isotropic perameter than the other 'bound' oxygens. The data did not suggest that the entire anion needed splitting and so no action was taken. The higher isotropic parameter is most likely a reflection of the higher movement of the uncoordinated oxygen compared to the 'bound'. 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^)+(0.0309P)^2^+1.7842P] 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 4373 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.945351(16) 0.837241(12) 0.082612(8) 0.02367(6) Uani 1 1 d . . . N111 N 0.93918(17) 1.04396(13) 0.18712(9) 0.0207(3) Uani 1 1 d . . . N112 N 1.00557(17) 0.98759(13) 0.14156(9) 0.0203(3) Uani 1 1 d . . . C113 C 1.1294(2) 1.03326(15) 0.15133(11) 0.0202(4) Uani 1 1 d . . . C114 C 1.1419(2) 1.11933(16) 0.20352(11) 0.0222(4) Uani 1 1 d . . . H114 H 1.2196 1.1649 0.2207 0.027 Uiso 1 1 calc R . . C115 C 1.0190(2) 1.12518(16) 0.22526(11) 0.0216(4) Uani 1 1 d . . . C116 C 1.2322(2) 0.98936(17) 0.11062(12) 0.0262(4) Uani 1 1 d . . . H11A H 1.2394 0.9104 0.1177 0.039 Uiso 1 1 calc R . . H11B H 1.3219 1.0228 0.1322 0.039 Uiso 1 1 calc R . . H11C H 1.2027 1.0061 0.0553 0.039 Uiso 1 1 calc R . . C117 C 0.9728(2) 1.20211(19) 0.27879(13) 0.0313(5) Uani 1 1 d . . . H11D H 0.8850 1.2347 0.2523 0.047 Uiso 1 1 calc R . . H11E H 1.0416 1.2594 0.2945 0.047 Uiso 1 1 calc R . . H11F H 0.9615 1.1626 0.3246 0.047 Uiso 1 1 calc R . . C118 C 0.8033(2) 1.00876(17) 0.19264(11) 0.0234(4) Uani 1 1 d . . . H11G H 0.7748 1.0520 0.2330 0.028 Uiso 1 1 calc R . . H11H H 0.8078 0.9316 0.2087 0.028 Uiso 1 1 calc R . . C121 C 0.6197(2) 0.93510(17) 0.08507(11) 0.0234(4) Uani 1 1 d . . . H121 H 0.6375 0.8654 0.1081 0.028 Uiso 1 1 calc R . . C122 C 0.6973(2) 1.02097(17) 0.11746(11) 0.0234(4) Uani 1 1 d . . . C123 C 0.5113(2) 0.94764(16) 0.01669(11) 0.0216(4) Uani 1 1 d . . . C131 C 0.3265(2) 0.87468(17) -0.08226(12) 0.0261(4) Uani 1 1 d . . . H131 H 0.2710 0.8149 -0.1044 0.031 Uiso 1 1 calc R . . C132 C 0.4287(2) 0.85989(17) -0.01686(12) 0.0252(4) Uani 1 1 d . . . H132 H 0.4439 0.7899 0.0060 0.030 Uiso 1 1 calc R . . N211 N 0.85431(17) 0.69244(13) -0.06809(9) 0.0201(3) Uani 1 1 d . . . N212 N 0.95116(17) 0.71405(13) -0.00152(9) 0.0214(3) Uani 1 1 d . . . C213 C 1.0625(2) 0.65703(16) -0.00674(12) 0.0244(4) Uani 1 1 d . . . C214 C 1.0362(2) 0.59866(17) -0.07597(12) 0.0263(4) Uani 1 1 d . . . H214 H 1.0979 0.5521 -0.0936 0.032 Uiso 1 1 calc R . . C215 C 0.9028(2) 0.62243(16) -0.11358(12) 0.0238(4) Uani 1 1 d . . . C216 C 1.1905(2) 0.66192(18) 0.05646(14) 0.0309(5) Uani 1 1 d . . . H21A H 1.2438 0.7262 0.0494 0.046 Uiso 1 1 calc R . . H21B H 1.2453 0.5964 0.0549 0.046 Uiso 1 1 calc R . . H21C H 1.1663 0.6663 0.1065 0.046 Uiso 1 1 calc R . . C217 C 0.8161(2) 0.58152(18) -0.18810(12) 0.0298(5) Uani 1 1 d . . . H21D H 0.7407 0.5377 -0.1780 0.045 Uiso 1 1 calc R . . H21E H 0.8722 0.5367 -0.2141 0.045 Uiso 1 1 calc R . . H21F H 0.7784 0.6432 -0.2212 0.045 Uiso 1 1 calc R . . C218 C 0.7143(2) 0.73141(15) -0.07864(11) 0.0214(4) Uani 1 1 d . . . H21G H 0.6794 0.7553 -0.1329 0.026 Uiso 1 1 calc R . . H21H H 0.7138 0.7951 -0.0448 0.026 Uiso 1 1 calc R . . C231 C 0.64756(19) 0.59583(15) 0.01064(11) 0.0192(4) Uani 1 1 d . . . H231 H 0.7273 0.6165 0.0486 0.023 Uiso 1 1 calc R . . C232 C 0.6194(2) 0.64502(15) -0.06010(11) 0.0191(4) Uani 1 1 d . . . C233 C 0.4997(2) 0.61581(17) -0.11687(11) 0.0232(4) Uani 1 1 d . . . H233 H 0.4801 0.6500 -0.1661 0.028 Uiso 1 1 calc R . . C234 C 0.56010(19) 0.51462(15) 0.02841(11) 0.0178(4) Uani 1 1 d . . . C241 C 0.5876(2) 0.46150(16) 0.10099(11) 0.0221(4) Uani 1 1 d . . . H241 H 0.6679 0.4798 0.1393 0.027 Uiso 1 1 calc R . . O11 O 0.83645(17) 0.70735(17) 0.17452(9) 0.0424(4) Uani 1 1 d . . . O12 O 1.05370(15) 0.73457(13) 0.21654(9) 0.0343(4) Uani 1 1 d . . . O13 O 0.9615(2) 0.59557(18) 0.25571(15) 0.0717(7) Uani 1 1 d . . . N11 N 0.95033(19) 0.67746(14) 0.21566(10) 0.0270(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 0.02392(9) 0.02483(9) 0.02169(9) -0.00480(6) 0.00436(6) -0.00126(6) N111 0.0184(8) 0.0244(8) 0.0192(8) -0.0013(7) 0.0043(6) 0.0012(7) N112 0.0207(8) 0.0217(8) 0.0186(8) 0.0000(6) 0.0049(6) 0.0024(7) C113 0.0217(10) 0.0187(9) 0.0206(9) 0.0052(7) 0.0060(8) 0.0019(7) C114 0.0235(10) 0.0193(9) 0.0236(10) 0.0019(8) 0.0054(8) -0.0023(8) C115 0.0249(10) 0.0194(9) 0.0200(9) 0.0017(8) 0.0047(8) 0.0016(8) C116 0.0256(11) 0.0238(10) 0.0316(11) 0.0000(8) 0.0115(9) 0.0006(8) C117 0.0337(12) 0.0301(11) 0.0327(12) -0.0077(9) 0.0132(10) -0.0030(10) C118 0.0186(10) 0.0311(11) 0.0205(9) 0.0008(8) 0.0047(8) -0.0014(8) C121 0.0205(10) 0.0283(10) 0.0231(10) 0.0038(8) 0.0087(8) 0.0026(8) C122 0.0159(9) 0.0348(11) 0.0210(10) -0.0011(8) 0.0072(8) 0.0038(8) C123 0.0201(10) 0.0222(10) 0.0260(10) 0.0018(8) 0.0125(8) 0.0027(8) C131 0.0228(10) 0.0264(10) 0.0295(11) -0.0029(9) 0.0070(8) 0.0006(8) C132 0.0230(10) 0.0229(10) 0.0307(11) 0.0028(8) 0.0083(8) 0.0023(8) N211 0.0210(8) 0.0193(8) 0.0207(8) -0.0005(6) 0.0062(7) -0.0044(6) N212 0.0209(8) 0.0219(8) 0.0219(8) -0.0011(7) 0.0061(7) -0.0050(7) C213 0.0228(10) 0.0233(10) 0.0280(11) 0.0007(8) 0.0078(8) -0.0028(8) C214 0.0271(11) 0.0228(10) 0.0319(11) -0.0029(8) 0.0128(9) -0.0012(8) C215 0.0303(11) 0.0175(9) 0.0263(10) -0.0019(8) 0.0125(9) -0.0040(8) C216 0.0238(11) 0.0321(12) 0.0361(12) -0.0056(9) 0.0059(9) 0.0008(9) C217 0.0358(12) 0.0264(11) 0.0275(11) -0.0059(9) 0.0080(9) -0.0020(9) C218 0.0231(10) 0.0184(9) 0.0228(10) 0.0005(7) 0.0059(8) -0.0008(8) C231 0.0183(9) 0.0195(9) 0.0191(9) -0.0030(7) 0.0032(7) -0.0002(7) C232 0.0194(10) 0.0170(9) 0.0220(9) -0.0022(7) 0.0072(8) 0.0005(7) C233 0.0247(10) 0.0256(10) 0.0185(9) 0.0034(8) 0.0034(8) -0.0009(8) C234 0.0179(9) 0.0177(9) 0.0180(9) -0.0019(7) 0.0050(7) 0.0016(7) C241 0.0203(10) 0.0258(10) 0.0182(9) -0.0001(8) 0.0009(7) -0.0025(8) O11 0.0246(8) 0.0681(12) 0.0323(9) 0.0016(8) 0.0021(7) -0.0072(8) O12 0.0242(8) 0.0410(9) 0.0343(9) 0.0025(7) 0.0005(7) -0.0051(7) O13 0.0632(14) 0.0598(14) 0.1100(19) 0.0500(14) 0.0559(14) 0.0212(11) N11 0.0297(10) 0.0289(9) 0.0258(9) -0.0001(7) 0.0134(8) 0.0039(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N112 2.1417(16) . ? Ag1 N212 2.1425(16) . ? Ag1 O12 2.6883(16) . ? Ag1 O11 2.6998(18) . ? N111 C115 1.357(3) . ? N111 N112 1.358(2) . ? N111 C118 1.456(2) . ? N112 C113 1.336(3) . ? C113 C114 1.395(3) . ? C113 C116 1.497(3) . ? C114 C115 1.380(3) . ? C114 H114 0.9500 . ? C115 C117 1.494(3) . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C118 C122 1.505(3) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C121 C122 1.357(3) . ? C121 C123 1.434(3) . ? C121 H121 0.9500 . ? C122 C131 1.424(3) 3_675 ? C123 C132 1.405(3) . ? C123 C123 1.415(4) 3_675 ? C131 C132 1.367(3) . ? C131 C122 1.424(3) 3_675 ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? N211 C215 1.351(3) . ? N211 N212 1.367(2) . ? N211 C218 1.454(3) . ? N212 C213 1.341(3) . ? C213 C214 1.397(3) . ? C213 C216 1.492(3) . ? C214 C215 1.378(3) . ? C214 H214 0.9500 . ? C215 C217 1.489(3) . ? C216 H21A 0.9800 . ? C216 H21B 0.9800 . ? C216 H21C 0.9800 . ? C217 H21D 0.9800 . ? C217 H21E 0.9800 . ? C217 H21F 0.9800 . ? C218 C232 1.515(3) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C231 C232 1.365(3) . ? C231 C234 1.415(3) . ? C231 H231 0.9500 . ? C232 C233 1.418(3) . ? C233 C241 1.368(3) 3_665 ? C233 H233 0.9500 . ? C234 C241 1.416(3) . ? C234 C234 1.422(4) 3_665 ? C241 C233 1.368(3) 3_665 ? C241 H241 0.9500 . ? O11 N11 1.255(3) . ? O12 N11 1.250(2) . ? O13 N11 1.224(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N112 Ag1 N212 154.49(6) . . ? N112 Ag1 O12 87.96(5) . . ? N212 Ag1 O12 102.43(6) . . ? N112 Ag1 O11 108.77(6) . . ? N212 Ag1 O11 95.06(6) . . ? O12 Ag1 O11 47.14(5) . . ? C115 N111 N112 111.13(16) . . ? C115 N111 C118 129.42(17) . . ? N112 N111 C118 119.34(16) . . ? C113 N112 N111 106.34(15) . . ? C113 N112 Ag1 124.85(13) . . ? N111 N112 Ag1 127.83(13) . . ? N112 C113 C114 109.76(17) . . ? N112 C113 C116 120.81(17) . . ? C114 C113 C116 129.40(18) . . ? C115 C114 C113 106.46(18) . . ? C115 C114 H114 126.8 . . ? C113 C114 H114 126.8 . . ? N111 C115 C114 106.30(17) . . ? N111 C115 C117 123.38(19) . . ? C114 C115 C117 130.32(19) . . ? C113 C116 H11A 109.5 . . ? C113 C116 H11B 109.5 . . ? H11A C116 H11B 109.5 . . ? C113 C116 H11C 109.5 . . ? H11A C116 H11C 109.5 . . ? H11B C116 H11C 109.5 . . ? C115 C117 H11D 109.5 . . ? C115 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C115 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? N111 C118 C122 112.55(16) . . ? N111 C118 H11G 109.1 . . ? C122 C118 H11G 109.1 . . ? N111 C118 H11H 109.1 . . ? C122 C118 H11H 109.1 . . ? H11G C118 H11H 107.8 . . ? C122 C121 C123 121.25(19) . . ? C122 C121 H121 119.4 . . ? C123 C121 H121 119.4 . . ? C121 C122 C131 119.77(18) . 3_675 ? C121 C122 C118 120.79(19) . . ? C131 C122 C118 119.35(19) 3_675 . ? C132 C123 C123 120.2(2) . 3_675 ? C132 C123 C121 121.93(18) . . ? C123 C123 C121 117.9(2) 3_675 . ? C132 C131 C122 120.5(2) . 3_675 ? C132 C131 H131 119.7 . . ? C122 C131 H131 119.7 3_675 . ? C131 C132 C123 120.38(19) . . ? C131 C132 H132 119.8 . . ? C123 C132 H132 119.8 . . ? C215 N211 N212 111.18(17) . . ? C215 N211 C218 127.49(17) . . ? N212 N211 C218 120.80(16) . . ? C213 N212 N211 105.58(16) . . ? C213 N212 Ag1 125.57(13) . . ? N211 N212 Ag1 127.71(13) . . ? N212 C213 C214 110.27(18) . . ? N212 C213 C216 120.45(19) . . ? C214 C213 C216 129.3(2) . . ? C215 C214 C213 106.01(19) . . ? C215 C214 H214 127.0 . . ? C213 C214 H214 127.0 . . ? N211 C215 C214 106.94(18) . . ? N211 C215 C217 122.23(19) . . ? C214 C215 C217 130.79(19) . . ? C213 C216 H21A 109.5 . . ? C213 C216 H21B 109.5 . . ? H21A C216 H21B 109.5 . . ? C213 C216 H21C 109.5 . . ? H21A C216 H21C 109.5 . . ? H21B C216 H21C 109.5 . . ? C215 C217 H21D 109.5 . . ? C215 C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C215 C217 H21F 109.5 . . ? H21D C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? N211 C218 C232 112.25(15) . . ? N211 C218 H21G 109.2 . . ? C232 C218 H21G 109.2 . . ? N211 C218 H21H 109.2 . . ? C232 C218 H21H 109.2 . . ? H21G C218 H21H 107.9 . . ? C232 C231 C234 121.17(17) . . ? C232 C231 H231 119.4 . . ? C234 C231 H231 119.4 . . ? C231 C232 C233 119.89(18) . . ? C231 C232 C218 120.70(17) . . ? C233 C232 C218 119.41(17) . . ? C241 C233 C232 120.23(18) 3_665 . ? C241 C233 H233 119.9 3_665 . ? C232 C233 H233 119.9 . . ? C231 C234 C241 122.35(17) . . ? C231 C234 C234 119.0(2) . 3_665 ? C241 C234 C234 118.6(2) . 3_665 ? C233 C241 C234 121.05(18) 3_665 . ? C233 C241 H241 119.5 3_665 . ? C234 C241 H241 119.5 . . ? N11 O11 Ag1 94.78(12) . . ? N11 O12 Ag1 95.47(11) . . ? O13 N11 O12 119.7(2) . . ? O13 N11 O11 121.6(2) . . ? O12 N11 O11 118.62(18) . . ? 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 C115 N111 N112 C113 0.4(2) . . . . ? C118 N111 N112 C113 -176.19(16) . . . . ? C115 N111 N112 Ag1 169.37(13) . . . . ? C118 N111 N112 Ag1 -7.2(2) . . . . ? N212 Ag1 N112 C113 -29.6(2) . . . . ? O12 Ag1 N112 C113 85.60(15) . . . . ? O11 Ag1 N112 C113 128.62(15) . . . . ? N212 Ag1 N112 N111 163.32(14) . . . . ? O12 Ag1 N112 N111 -81.50(15) . . . . ? O11 Ag1 N112 N111 -38.47(16) . . . . ? N111 N112 C113 C114 0.0(2) . . . . ? Ag1 N112 C113 C114 -169.39(12) . . . . ? N111 N112 C113 C116 178.58(17) . . . . ? Ag1 N112 C113 C116 9.2(2) . . . . ? N112 C113 C114 C115 -0.4(2) . . . . ? C116 C113 C114 C115 -178.79(19) . . . . ? N112 N111 C115 C114 -0.6(2) . . . . ? C118 N111 C115 C114 175.51(18) . . . . ? N112 N111 C115 C117 179.05(18) . . . . ? C118 N111 C115 C117 -4.8(3) . . . . ? C113 C114 C115 N111 0.6(2) . . . . ? C113 C114 C115 C117 -179.0(2) . . . . ? C115 N111 C118 C122 118.0(2) . . . . ? N112 N111 C118 C122 -66.1(2) . . . . ? C123 C121 C122 C131 -1.5(3) . . . 3_675 ? C123 C121 C122 C118 175.12(18) . . . . ? N111 C118 C122 C121 125.3(2) . . . . ? N111 C118 C122 C131 -58.1(2) . . . 3_675 ? C122 C121 C123 C132 -179.01(19) . . . . ? C122 C121 C123 C123 0.8(3) . . . 3_675 ? C122 C131 C132 C123 0.2(3) 3_675 . . . ? C123 C123 C132 C131 0.5(4) 3_675 . . . ? C121 C123 C132 C131 -179.75(19) . . . . ? C215 N211 N212 C213 0.8(2) . . . . ? C218 N211 N212 C213 173.12(16) . . . . ? C215 N211 N212 Ag1 169.03(13) . . . . ? C218 N211 N212 Ag1 -18.7(2) . . . . ? N112 Ag1 N212 C213 59.0(2) . . . . ? O12 Ag1 N212 C213 -53.20(16) . . . . ? O11 Ag1 N212 C213 -100.37(16) . . . . ? N112 Ag1 N212 N211 -107.02(18) . . . . ? O12 Ag1 N212 N211 140.82(14) . . . . ? O11 Ag1 N212 N211 93.64(15) . . . . ? N211 N212 C213 C214 -0.5(2) . . . . ? Ag1 N212 C213 C214 -169.04(13) . . . . ? N211 N212 C213 C216 179.51(18) . . . . ? Ag1 N212 C213 C216 11.0(3) . . . . ? N212 C213 C214 C215 0.0(2) . . . . ? C216 C213 C214 C215 -180.0(2) . . . . ? N212 N211 C215 C214 -0.8(2) . . . . ? C218 N211 C215 C214 -172.46(18) . . . . ? N212 N211 C215 C217 177.32(18) . . . . ? C218 N211 C215 C217 5.7(3) . . . . ? C213 C214 C215 N211 0.5(2) . . . . ? C213 C214 C215 C217 -177.5(2) . . . . ? C215 N211 C218 C232 73.2(2) . . . . ? N212 N211 C218 C232 -97.7(2) . . . . ? C234 C231 C232 C233 0.8(3) . . . . ? C234 C231 C232 C218 -179.63(17) . . . . ? N211 C218 C232 C231 56.6(2) . . . . ? N211 C218 C232 C233 -123.88(19) . . . . ? C231 C232 C233 C241 0.0(3) . . . 3_665 ? C218 C232 C233 C241 -179.58(18) . . . 3_665 ? C232 C231 C234 C241 179.33(18) . . . . ? C232 C231 C234 C234 -0.9(3) . . . 3_665 ? C231 C234 C241 C233 179.21(19) . . . 3_665 ? C234 C234 C241 C233 -0.6(3) 3_665 . . 3_665 ? N112 Ag1 O11 N11 -79.61(14) . . . . ? N212 Ag1 O11 N11 91.16(13) . . . . ? O12 Ag1 O11 N11 -11.12(11) . . . . ? N112 Ag1 O12 N11 129.37(12) . . . . ? N212 Ag1 O12 N11 -74.15(12) . . . . ? O11 Ag1 O12 N11 11.18(11) . . . . ? Ag1 O12 N11 O13 161.1(2) . . . . ? Ag1 O12 N11 O11 -20.38(19) . . . . ? Ag1 O11 N11 O13 -161.2(2) . . . . ? Ag1 O11 N11 O12 20.27(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.680 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.063 #===END