# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1445 data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 Ag2 N10 O13' _chemical_formula_weight 1056.68 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 rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 15.627(3) _cell_length_b 15.627(3) _cell_length_c 31.583(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6679(2) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3011 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1316 _reflns_number_gt 1011 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The [Ag~2~(n3F)]^2+^ cation shows 32 point symmetry, the silver ions lie on the threefold axis and each furan oxygen atom is bisected by a twofold axis. The two nitrate ions associated with each cation are disordered over three equivalent positions on the twofold axes. 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^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1316 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.6667 0.3333 0.035079(11) 0.02330(17) Uani 1 3 d S . . N1 N 0.6667 0.3333 -0.04428(15) 0.0316(10) Uani 1 3 d S . . C1 C 0.5875(3) 0.3512(3) -0.05941(10) 0.0362(8) Uani 1 1 d . . . H1A H 0.5251 0.2895 -0.0589 0.040 Uiso 1 1 calc R . . H1B H 0.6010 0.3740 -0.0885 0.049 Uiso 1 1 calc R . . C2 C 0.5784(2) 0.4271(2) -0.03277(10) 0.0361(8) Uani 1 1 d . . . H2A H 0.5636 0.4675 -0.0513 0.035 Uiso 1 1 calc R . . H2B H 0.6417 0.4702 -0.0195 0.044 Uiso 1 1 calc R . . C3 C 0.4998(3) 0.3837(3) 0.00152(10) 0.0366(8) Uani 1 1 d . . . H3A H 0.5056 0.4368 0.0195 0.043 Uiso 1 1 calc R . . H3B H 0.4351 0.3527 -0.0116 0.031 Uiso 1 1 calc R . . N2 N 0.50772(19) 0.31062(19) 0.02779(7) 0.0290(6) Uani 1 1 d . . . C4 C 0.4283(2) 0.2309(2) 0.03511(10) 0.0310(7) Uani 1 1 d . . . H4 H 0.3701 0.2216 0.0229 0.032 Uiso 1 1 calc R . . C5 C 0.4244(2) 0.1544(2) 0.06140(9) 0.0292(7) Uani 1 1 d . . . C6 C 0.3526(2) 0.0593(2) 0.06924(10) 0.0356(8) Uani 1 1 d . . . H6 H 0.2891 0.0271 0.0580 0.043 Uiso 1 1 calc R . . O1 O 0.50807(16) 0.17474(16) 0.0833 0.0268(6) Uani 1 2 d S . . N11 N 0.0977(12) -0.2356(12) 0.0833 0.094(4) Uani 0.67 2 d SP . . O11 O 0.0341(5) -0.2602(6) 0.0580(2) 0.137(3) Uani 0.67 1 d P . . O12 O 0.1655(4) -0.1679(4) 0.0833 0.078(3) Uani 0.67 2 d SP . . O13 O 0.0704(6) -0.1253(6) 0.0077(2) 0.125(3) Uani 0.67 1 d P . . H13A H 0.0678 -0.1627 0.0297 0.050 Uiso 1 1 d . . . H13B H 0.0059 -0.1383 0.0028 0.050 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 Ag 0.0215(2) 0.0215(2) 0.0269(3) 0.000 0.000 0.01075(10) N1 0.0322(15) 0.0322(15) 0.030(2) 0.000 0.000 0.0161(8) C1 0.0371(17) 0.0391(18) 0.0318(17) 0.0000(15) -0.0049(14) 0.0185(15) C2 0.0411(19) 0.0354(18) 0.0382(17) -0.0020(15) -0.0152(15) 0.0241(16) C3 0.0391(18) 0.045(2) 0.0375(17) -0.0045(15) -0.0089(14) 0.0299(17) N2 0.0292(14) 0.0331(14) 0.0309(13) -0.0061(11) -0.0037(11) 0.0203(13) C4 0.0269(17) 0.0394(18) 0.0316(16) -0.0112(14) -0.0055(14) 0.0203(15) C5 0.0218(15) 0.0334(17) 0.0338(16) -0.0109(13) 0.0007(13) 0.0149(14) C6 0.0224(15) 0.0330(17) 0.0447(19) -0.0155(14) 0.0059(14) 0.0090(14) O1 0.0217(11) 0.0217(11) 0.0342(15) -0.0020(6) 0.0020(6) 0.0089(13) N11 0.145(10) 0.145(10) 0.061(6) -0.004(2) 0.004(2) 0.125(11) O11 0.118(5) 0.175(7) 0.150(6) -0.073(6) -0.040(5) 0.097(5) O12 0.037(2) 0.037(2) 0.152(8) -0.003(2) 0.003(2) 0.012(3) O13 0.138(5) 0.152(6) 0.106(4) -0.058(4) 0.028(4) 0.088(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N2 2.338(2) 2_655 ? Ag N2 2.338(3) 3_665 ? Ag N2 2.338(3) . y Ag N1 2.506(5) . y Ag Ag 3.0480(10) 16_544 y N1 C1 1.477(4) 2_655 ? N1 C1 1.477(4) 3_665 ? N1 C1 1.477(4) . ? C1 C2 1.518(5) . ? C2 C3 1.519(5) . ? C3 N2 1.466(4) . ? N2 C4 1.264(4) . ? C4 C5 1.432(4) . ? C5 C6 1.365(4) . ? C5 O1 1.369(3) . ? C6 C6 1.402(7) 16_544 ? O1 C5 1.369(3) 16_544 ? N11 O12 1.059(15) . ? N11 O11 1.179(10) 16_544 ? N11 O11 1.180(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 N2 Ag N2 119.04(2) 2_655 3_665 ? N2 Ag N2 119.04(2) 2_655 . y N2 Ag N2 119.04(2) 3_665 . ? N2 Ag N1 84.35(6) 2_655 . ? N2 Ag N1 84.35(6) 3_665 . ? N2 Ag N1 84.35(6) . . y N2 Ag Ag 95.65(6) 2_655 16_544 ? N2 Ag Ag 95.65(6) 3_665 16_544 ? N2 Ag Ag 95.65(6) . 16_544 y N1 Ag Ag 180.0 . 16_544 ? C1 N1 C1 110.1(2) 2_655 3_665 ? C1 N1 C1 110.1(2) 2_655 . ? C1 N1 C1 110.1(2) 3_665 . ? C1 N1 Ag 108.9(2) 2_655 . ? C1 N1 Ag 108.9(2) 3_665 . ? C1 N1 Ag 108.9(2) . . ? N1 C1 C2 112.5(3) . . ? C1 C2 C3 114.7(3) . . ? N2 C3 C2 112.8(2) . . ? C4 N2 C3 116.6(3) . . ? C4 N2 Ag 125.2(2) . . ? C3 N2 Ag 115.75(19) . . ? N2 C4 C5 122.6(3) . . ? C6 C5 O1 109.3(3) . . ? C6 C5 C4 133.1(3) . . ? O1 C5 C4 117.6(3) . . ? C5 C6 C6 107.08(19) . 16_544 ? C5 O1 C5 107.2(3) . 16_544 ? O12 N11 O11 125.7(9) . 16_544 ? O12 N11 O11 125.7(9) . . ? O11 N11 O11 108.5(18) 16_544 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.661 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.076 data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 Ag2 B2 F8 N10' _chemical_formula_weight 1058.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 22.869(2) _cell_length_b 11.1337(10) _cell_length_c 18.9368(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.520(6) _cell_angle_gamma 90.00 _cell_volume 4454.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.66 _cell_measurement_theta_max 12.54 _exptl_crystal_description rhomb _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7489 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4466 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3921 _reflns_number_gt 3365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXL-97' _refine_special_details ; The asymmetric unit contains half of the cation, one BF~4~^-^ anion and one acetonitrile solvate molecule. The cation lies on a twofold axis which passes through C(18), C(19) and the mid-point of the Ag-Ag vector. 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^)+(0.0255P)^2^+12.3476P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3921 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.124 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.418368(10) 0.934604(19) 0.211721(12) 0.02855(8) Uani 1 1 d . . . N1 N 0.29758(11) 0.9330(2) 0.15129(14) 0.0323(5) Uani 1 1 d . . . C1 C 0.27852(14) 1.0518(3) 0.16830(19) 0.0370(7) Uani 1 1 d . . . H1A H 0.2726 1.0484 0.2174 0.044 Uiso 1 1 calc R . . H1B H 0.2375 1.0743 0.1277 0.044 Uiso 1 1 calc R . . C2 C 0.32763(14) 1.1468(3) 0.17342(19) 0.0391(7) Uani 1 1 d . . . H2A H 0.3357 1.1474 0.1256 0.047 Uiso 1 1 calc R . . H2B H 0.3117 1.2271 0.1799 0.047 Uiso 1 1 calc R . . N3 N 0.38680(11) 1.1205(2) 0.23889(15) 0.0320(6) Uani 1 1 d . . . C3 C 0.39825(14) 1.1830(3) 0.29830(18) 0.0347(7) Uani 1 1 d . . . H3 H 0.3696 1.2463 0.2955 0.042 Uiso 1 1 calc R . . C4 C 0.45167(14) 1.1666(3) 0.37104(18) 0.0343(7) Uani 1 1 d . . . C5 C 0.45448(17) 1.2401(3) 0.4319(2) 0.0468(9) Uani 1 1 d . . . H5 H 0.4229 1.2995 0.4247 0.056 Uiso 1 1 calc R . . C6 C 0.50293(18) 1.2267(3) 0.5026(2) 0.0525(10) Uani 1 1 d . . . H6 H 0.5048 1.2774 0.5437 0.063 Uiso 1 1 calc R . . C7 C 0.54861(16) 1.1404(3) 0.51357(19) 0.0468(9) Uani 1 1 d . . . H7 H 0.5815 1.1310 0.5625 0.056 Uiso 1 1 calc R . . C8 C 0.54701(14) 1.0663(3) 0.45334(17) 0.0358(7) Uani 1 1 d . . . C9 C 0.49833(13) 1.0803(3) 0.38236(17) 0.0331(7) Uani 1 1 d . . . H9 H 0.4969 1.0305 0.3410 0.040 Uiso 1 1 calc R . . C10 C 0.59752(14) 0.9770(3) 0.46865(18) 0.0380(7) Uani 1 1 d . . . H10 H 0.6238 0.9620 0.5206 0.046 Uiso 1 1 calc R . . N4 N 0.60880(11) 0.9182(2) 0.41796(14) 0.0345(6) Uani 1 1 d . . . C11 C 0.66697(14) 0.8445(3) 0.44525(19) 0.0409(8) Uani 1 1 d . . . H11A H 0.6590 0.7667 0.4178 0.049 Uiso 1 1 calc R . . H11B H 0.6802 0.8281 0.5006 0.049 Uiso 1 1 calc R . . C12 C 0.71886(14) 0.9127(3) 0.43061(18) 0.0409(8) Uani 1 1 d . . . H12A H 0.7258 0.9911 0.4573 0.049 Uiso 1 1 calc R . . H12B H 0.7588 0.8665 0.4518 0.049 Uiso 1 1 calc R . . C13 C 0.27830(14) 0.8345(3) 0.18897(18) 0.0356(7) Uani 1 1 d . . . H13A H 0.2737 0.7600 0.1588 0.043 Uiso 1 1 calc R . . H13B H 0.2366 0.8535 0.1909 0.043 Uiso 1 1 calc R . . C14 C 0.32627(13) 0.8140(3) 0.26951(18) 0.0362(7) Uani 1 1 d . . . H14A H 0.3324 0.8890 0.2996 0.043 Uiso 1 1 calc R . . H14B H 0.3107 0.7513 0.2950 0.043 Uiso 1 1 calc R . . N5 N 0.38681(11) 0.7760(2) 0.26588(14) 0.0309(5) Uani 1 1 d . . . C15 C 0.39936(14) 0.6648(3) 0.27498(18) 0.0363(7) Uani 1 1 d . . . H15 H 0.3722 0.6158 0.2902 0.044 Uiso 1 1 calc R . . C16 C 0.45253(14) 0.6059(3) 0.2638(2) 0.0431(8) Uani 1 1 d . . . C17 C 0.45347(18) 0.4816(3) 0.2640(4) 0.093(2) Uani 1 1 d . . . H17 H 0.4216 0.4384 0.2739 0.111 Uiso 1 1 calc R . . C18 C 0.5000 0.4198(5) 0.2500 0.132(4) Uani 1 2 d S . . H18 H 0.5000 0.3345 0.2500 0.158 Uiso 1 2 calc SR . . C19 C 0.5000 0.6670(4) 0.2500 0.0344(10) Uani 1 2 d S . . H19 H 0.5000 0.7524 0.2500 0.041 Uiso 1 2 calc SR . . B1 B 0.25938(17) 0.4881(3) 0.1366(2) 0.0361(8) Uani 1 1 d . . . F1 F 0.21150(8) 0.55784(17) 0.14424(11) 0.0443(4) Uani 1 1 d . . . F2 F 0.29694(8) 0.44054(17) 0.20745(10) 0.0448(4) Uani 1 1 d . . . F3 F 0.29612(9) 0.55936(18) 0.10976(12) 0.0508(5) Uani 1 1 d . . . F4 F 0.23228(10) 0.39516(18) 0.08551(12) 0.0532(5) Uani 1 1 d . . . N20 N 0.3921(2) 1.5099(5) 0.4441(4) 0.1105(18) Uani 1 1 d . . . C21 C 0.3869(3) 1.5576(6) 0.4930(4) 0.103(2) Uani 1 1 d . . . C22 C 0.3751(4) 1.6304(8) 0.5478(5) 0.225(6) Uani 1 1 d . . . H22A H 0.4020 1.7020 0.5584 0.050 Uiso 1 1 calc R . . H22B H 0.3846 1.5847 0.5951 0.050 Uiso 1 1 calc R . . H22C H 0.3305 1.6548 0.5276 0.050 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 Ag 0.02927(12) 0.02405(12) 0.03552(12) -0.00028(10) 0.01595(9) -0.00060(10) N1 0.0305(12) 0.0326(13) 0.0368(13) -0.0006(12) 0.0161(11) -0.0006(11) C1 0.0302(15) 0.0373(18) 0.0435(17) 0.0040(15) 0.0142(13) 0.0072(14) C2 0.0383(17) 0.0286(16) 0.052(2) 0.0077(14) 0.0186(15) 0.0079(14) N3 0.0312(13) 0.0227(12) 0.0452(15) 0.0040(12) 0.0180(12) 0.0006(10) C3 0.0331(16) 0.0224(15) 0.057(2) -0.0010(14) 0.0261(15) 0.0025(12) C4 0.0362(16) 0.0275(16) 0.0483(18) -0.0092(14) 0.0265(14) -0.0066(13) C5 0.048(2) 0.0381(19) 0.067(2) -0.0162(17) 0.0366(19) -0.0059(15) C6 0.058(2) 0.055(2) 0.058(2) -0.0271(19) 0.0366(19) -0.0151(19) C7 0.0455(19) 0.061(2) 0.0406(19) -0.0150(17) 0.0233(16) -0.0149(17) C8 0.0329(15) 0.0421(17) 0.0392(16) -0.0074(15) 0.0213(13) -0.0073(14) C9 0.0325(15) 0.0340(17) 0.0392(16) -0.0092(14) 0.0208(13) -0.0063(13) C10 0.0318(16) 0.052(2) 0.0326(16) 0.0015(15) 0.0150(13) -0.0049(14) N4 0.0324(13) 0.0377(15) 0.0368(14) 0.0055(12) 0.0170(11) 0.0002(11) C11 0.0368(17) 0.048(2) 0.0408(18) 0.0101(16) 0.0183(14) 0.0096(15) C12 0.0309(16) 0.052(2) 0.0401(18) 0.0036(15) 0.0134(14) 0.0062(15) C13 0.0303(15) 0.0319(16) 0.0521(19) -0.0056(15) 0.0242(14) -0.0044(13) C14 0.0375(16) 0.0338(17) 0.0483(18) 0.0012(15) 0.0286(15) -0.0015(14) N5 0.0324(13) 0.0274(13) 0.0359(13) 0.0009(11) 0.0166(11) -0.0010(10) C15 0.0299(15) 0.0298(17) 0.0479(19) 0.0054(14) 0.0133(14) -0.0056(13) C16 0.0280(16) 0.0236(15) 0.073(2) 0.0074(16) 0.0141(16) -0.0001(13) C17 0.038(2) 0.0276(19) 0.219(6) 0.021(3) 0.057(3) 0.0023(17) C18 0.057(4) 0.019(3) 0.335(14) 0.000 0.093(6) 0.000 C19 0.031(2) 0.020(2) 0.050(3) 0.000 0.0130(19) 0.000 B1 0.0414(19) 0.0321(18) 0.0386(19) 0.0022(16) 0.0195(16) 0.0022(16) F1 0.0453(10) 0.0410(10) 0.0532(11) 0.0030(9) 0.0261(9) 0.0082(9) F2 0.0421(10) 0.0470(11) 0.0449(10) 0.0071(9) 0.0163(8) 0.0034(9) F3 0.0598(12) 0.0478(11) 0.0601(12) 0.0055(10) 0.0401(10) -0.0011(10) F4 0.0624(13) 0.0397(11) 0.0531(12) -0.0091(9) 0.0172(10) -0.0017(10) N20 0.078(3) 0.086(3) 0.152(5) -0.039(3) 0.028(3) 0.020(3) C21 0.077(3) 0.103(5) 0.134(5) -0.050(4) 0.045(4) -0.040(3) C22 0.302(12) 0.256(11) 0.223(9) -0.152(8) 0.220(9) -0.227(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N5 2.293(2) . y Ag N4 2.298(2) 2_655 y Ag N3 2.313(2) . y Ag N1 2.553(2) . y Ag Ag 3.4491(5) 2_655 y N1 C13 1.465(4) . ? N1 C1 1.467(4) . ? N1 C12 1.467(4) 2_655 ? C1 C2 1.519(4) . ? C2 N3 1.473(4) . ? N3 C3 1.262(4) . ? C3 C4 1.461(4) . ? C4 C9 1.390(4) . ? C4 C5 1.394(4) . ? C5 C6 1.380(5) . ? C6 C7 1.376(5) . ? C7 C8 1.397(4) . ? C8 C9 1.387(4) . ? C8 C10 1.466(4) . ? C10 N4 1.267(4) . ? N4 C11 1.478(4) . ? N4 Ag 2.298(2) 2_655 ? C11 C12 1.522(4) . ? C12 N1 1.467(4) 2_655 ? C13 C14 1.517(4) . ? C14 N5 1.474(4) . ? N5 C15 1.268(4) . ? C15 C16 1.467(4) . ? C16 C17 1.384(5) . ? C16 C19 1.389(4) . ? C17 C18 1.376(5) . ? C18 C17 1.376(5) 2_655 ? C19 C16 1.389(4) 2_655 ? B1 F3 1.386(4) . ? B1 F4 1.390(4) . ? B1 F2 1.391(4) . ? B1 F1 1.394(4) . ? N20 C21 1.113(7) . ? C21 C22 1.422(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag N4 114.46(9) . 2_655 y N5 Ag N3 114.26(9) . . y N4 Ag N3 109.21(9) 2_655 . y N5 Ag N1 73.94(8) . . y N4 Ag N1 73.57(8) 2_655 . y N3 Ag N1 74.31(8) . . y N5 Ag Ag 106.71(6) . 2_655 ? N4 Ag Ag 104.79(6) 2_655 2_655 ? N3 Ag Ag 106.64(6) . 2_655 ? N1 Ag Ag 178.34(5) . 2_655 ? C13 N1 C1 113.4(2) . . ? C13 N1 C12 113.4(2) . 2_655 ? C1 N1 C12 113.2(2) . 2_655 ? C13 N1 Ag 105.22(17) . . ? C1 N1 Ag 104.88(17) . . ? C12 N1 Ag 105.68(16) 2_655 . ? N1 C1 C2 111.6(2) . . ? N3 C2 C1 109.5(2) . . ? C3 N3 C2 116.8(3) . . ? C3 N3 Ag 135.7(2) . . ? C2 N3 Ag 104.80(18) . . ? N3 C3 C4 125.8(3) . . ? C9 C4 C5 119.2(3) . . ? C9 C4 C3 123.1(3) . . ? C5 C4 C3 117.6(3) . . ? C6 C5 C4 120.3(3) . . ? C7 C6 C5 120.2(3) . . ? C6 C7 C8 120.5(3) . . ? C9 C8 C7 119.0(3) . . ? C9 C8 C10 123.2(3) . . ? C7 C8 C10 117.8(3) . . ? C8 C9 C4 120.7(3) . . ? N4 C10 C8 125.0(3) . . ? C10 N4 C11 116.0(3) . . ? C10 N4 Ag 135.9(2) . 2_655 ? C11 N4 Ag 104.87(18) . 2_655 ? N4 C11 C12 108.6(3) . . ? N1 C12 C11 111.6(3) 2_655 . ? N1 C13 C14 111.5(2) . . ? N5 C14 C13 109.1(2) . . ? C15 N5 C14 116.2(3) . . ? C15 N5 Ag 136.0(2) . . ? C14 N5 Ag 105.17(17) . . ? N5 C15 C16 125.1(3) . . ? C17 C16 C19 118.6(3) . . ? C17 C16 C15 117.4(3) . . ? C19 C16 C15 124.0(3) . . ? C18 C17 C16 120.8(4) . . ? C17 C18 C17 120.0(5) . 2_655 ? C16 C19 C16 121.3(4) . 2_655 ? F3 B1 F4 110.0(3) . . ? F3 B1 F2 109.5(3) . . ? F4 B1 F2 109.5(3) . . ? F3 B1 F1 109.2(3) . . ? F4 B1 F1 109.2(3) . . ? F2 B1 F1 109.4(3) . . ? N20 C21 C22 172.0(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.711 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.062 data_2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Ag2 N10 O6' _chemical_formula_weight 1010.69 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 rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 15.821(3) _cell_length_b 15.821(3) _cell_length_c 34.581(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7496(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 2 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3108 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3309 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2957 _reflns_number_gt 1802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; The structure was initially solved in R-3c which revealed the cation but not the anions; the nitrate anions were only located in the lower symmetry space group R3c. The cation lies on the threefold axis, which passes through the silver ions. The symmetry of the space group requires that the two nitrate ions associated with each cation are disordered over three equivalent positions about the threefold axis but these sites are further disordered. Consequently, each asymmetric unit contains one third of a cation and two thirds of a nitrate ion disordered over two 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^)+(0.1140P)^2^+28.2924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.30(15) _refine_ls_number_reflns 2957 _refine_ls_number_parameters 184 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.0000 0.08207(3) 0.0566(6) Uani 1 3 d S . . Ag2 Ag 0.0000 0.0000 -0.02708(3) 0.0613(7) Uani 1 3 d S . . N1 N 0.0000 0.0000 0.1516(8) 0.081(8) Uani 1 3 d SDU . . C1 C -0.0919(9) -0.0847(12) 0.1635(5) 0.083(4) Uani 1 1 d DU . . H1A H -0.0933 -0.1467 0.1637 0.080 Uiso 1 1 d R . . H1B H -0.1004 -0.0698 0.1900 0.080 Uiso 1 1 d R . . C2 C -0.1746(12) -0.0816(13) 0.1401(4) 0.098(6) Uani 1 1 d DU . . H2A H -0.1570 -0.0189 0.1287 0.080 Uiso 1 1 d R . . H2B H -0.2303 -0.1001 0.1569 0.080 Uiso 1 1 d R . . C3 C -0.2127(11) -0.1577(13) 0.1064(5) 0.101(5) Uani 1 1 d DU . . H3A H -0.2589 -0.1516 0.0898 0.080 Uiso 1 1 d R . . H3B H -0.2478 -0.2215 0.1184 0.080 Uiso 1 1 d R . . N3 N -0.1322(9) -0.1546(8) 0.0845(3) 0.065(3) Uani 1 1 d DU . . C4 C -0.1330(12) -0.2323(11) 0.0763(5) 0.080(4) Uani 1 1 d DU . . H4 H -0.1796 -0.2910 0.0873 0.080 Uiso 1 1 d R . . C10 C 0.0066(12) -0.1650(9) 0.0293(5) 0.068(3) Uani 1 1 d DU . . H10 H 0.0032 -0.1080 0.0300 0.080 Uiso 1 1 d R . . C5 C -0.0623(13) -0.2404(10) 0.0508(4) 0.081(4) Uani 1 1 d DU . . C6 C -0.0658(14) -0.3307(10) 0.0510(5) 0.098(4) Uani 1 1 d DU . . H6 H -0.1065 -0.3859 0.0655 0.080 Uiso 1 1 d R . . C7 C -0.0074(15) -0.3482(12) 0.0252(6) 0.107(4) Uani 1 1 d DU . . H7 H -0.0042 -0.4052 0.0242 0.080 Uiso 1 1 d R . . C8 C 0..0653(14) -0.2686(12) 0.0059(6) 0.103(5) Uani 1 1 d DU . . H8 H 0.1117 -0.2724 -0.0093 0.080 Uiso 1 1 d R . . C9 C 0.0666(9) -0.1784(9) 0.0049(5) 0.073(3) Uani 1 1 d DU . . C11 C 0.1399(13) -0.0993(12) -0.0192(5) 0.084(4) Uani 1 1 d DU . . H11 H 0.1966 -0.0983 -0.0271 0.080 Uiso 1 1 d R . . N4 N 0.1342(10) -0.0261(10) -0.0297(4) 0.086(4) Uani 1 1 d DU . . C12 C 0.2171(10) 0.0431(13) -0.0546(4) 0.092(4) Uani 1 1 d DU . . H12A H 0.2622 0.0959 -0.0381 0.080 Uiso 1 1 d R . . H12B H 0.2506 0.0110 -0.0652 0.080 Uiso 1 1 d R . . C13 C 0.1853(11) 0.0883(9) -0.0869(5) 0.081(4) Uani 1 1 d DU . . H13A H 0.2402 0.1247 -0.1041 0.080 Uiso 1 1 d R . . H13B H 0.1692 0.1347 -0.0756 0.080 Uiso 1 1 d R . . C14 C 0.0974(9) 0.0249(13) -0.1125(4) 0.075(4) Uani 1 1 d DU . . H14A H 0.1075 0.0492 -0.1388 0.080 Uiso 1 1 d R . . H14B H 0.0947 -0.0377 -0.1129 0.080 Uiso 1 1 d R . . N2 N 0.0000 0.0000 -0.0975(6) 0.065(6) Uani 1 3 d SDU . . N11 N 0.2830(14) 0.4815(16) -0.0713(7) 0.074(7) Uiso 0.351(5) 1 d PD A 1 O11 O 0.2135(14) 0.4705(18) -0.0652(8) 0.100 Uiso 0.351(5) 1 d PD A 1 O12 O 0.3388(15) 0.5425(17) -0.0630(8) 0.100 Uiso 0.351(5) 1 d PD A 1 O13 O 0.2861(17) 0.4332(16) -0.0894(7) 0.100 Uiso 0.351(5) 1 d PD A 1 N21 N 0.263(2) 0.329(3) -0.1393(8) 0.092(8) Uiso 0.315(5) 1 d PD A 2 O21 O 0.2185(18) 0.329(2) -0.1612(7) 0.100 Uiso 0.315(5) 1 d PD A 2 O22 O 0.279(2) 0.375(2) -0.1164(7) 0.100 Uiso 0.315(5) 1 d PD A 2 O23 O 0.319(2) 0.318(2) -0.1484(8) 0.100 Uiso 0.315(5) 1 d PD 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 0.0605(8) 0.0605(8) 0.0489(14) 0.000 0.000 0.0302(4) Ag2 0.0679(10) 0.0679(10) 0.0483(15) 0.000 0.000 0.0339(5) N1 0.091(10) 0.091(10) 0.06(2) 0.000 0.000 0.046(5) C1 0.107(11) 0.098(10) 0.057(9) 0.000(8) 0.019(6) 0.062(9) C2 0.088(9) 0.136(15) 0.050(8) 0.021(7) 0.021(7) 0.040(9) C3 0.079(11) 0.092(11) 0.092(12) 0.013(8) 0.020(7) 0.013(9) N3 0.072(8) 0.074(7) 0.042(6) 0.019(5) -0.002(5) 0.032(7) C4 0.082(11) 0.059(9) 0.067(11) 0.007(8) -0.017(6) 0.012(8) C10 0.097(7) 0.074(8) 0.052(5) -0.003(7) -0.021(4) 0.057(8) C5 0.131(13) 0.072(9) 0.045(8) -0.003(6) -0.021(6) 0.054(9) C6 0.137(14) 0.067(9) 0.089(13) -0.014(8) -0.058(7) 0.050(10) C7 0.155(13) 0.106(10) 0.098(9) -0.021(10) -0.066(8) 0.095(11) C8 0.128(15) 0.125(12) 0.105(16) -0.038(10) -0.053(8) 0.100(12) C9 0.060(8) 0.086(9) 0.088(11) -0.027(7) -0.040(5) 0.048(7) C11 0.101(12) 0.128(12) 0.056(10) -0.024(8) -0.020(6) 0.082(10) N4 0.066(8) 0.119(12) 0.080(10) 0.003(8) -0.004(7) 0.051(9) C12 0.067(9) 0.133(12) 0.059(8) -0.014(7) 0.008(6) 0.038(8) C13 0.071(7) 0.086(11) 0.083(11) -0.009(7) 0.029(7) 0.036(7) C14 0.091(9) 0.093(10) 0.045(7) 0.018(6) 0.020(5) 0.049(8) N2 0.078(8) 0.078(8) 0.040(17) 0.000 0.000 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.291(12) . y Ag1 N3 2.291(12) 2 ? Ag1 N3 2.291(12) 3 ? Ag1 N1 2.41(3) . y Ag1 Ag2 3.775(2) . y Ag2 N4 2.358(13) 2 ? Ag2 N4 2.358(13) 3 ? Ag2 N4 2.358(13) . y Ag2 N2 2.43(2) . y N1 C1 1.459(12) 3 ? N1 C1 1.459(12) 2 ? N1 C1 1.459(12) . ? C1 C2 1.560(15) . ? C2 C3 1.565(14) . ? C3 N3 1.462(13) . ? N3 C4 1.254(12) . ? C4 C5 1.481(14) . ? C10 C9 1.363(12) . ? C10 C5 1.365(12) . ? C5 C6 1.402(13) . ? C6 C7 1.406(14) . ? C7 C8 1.381(14) . ? C8 C9 1.417(13) . ? C9 C11 1.468(14) . ? C11 N4 1.260(13) . ? N4 C12 1.493(12) . ? C12 C13 1.539(14) . ? C13 C14 1.526(14) . ? C14 N2 1.480(11) . ? N2 C14 1.480(11) 3 ? N2 C14 1.480(11) 2 ? N11 O12 0.971(15) . ? N11 O13 1.006(15) . ? N11 O11 1.046(12) . ? O11 O12 1.725(19) . ? O11 O13 1.745(19) . ? O12 O13 1.75(2) . ? N21 O22 1.018(17) . ? N21 O21 1.028(17) . ? N21 O23 1.037(16) . ? O21 O23 1.74(2) . ? O21 O22 1.77(2) . ? O22 O23 1.73(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N3 119.87(4) . 2 y N3 Ag1 N3 119.87(4) . 3 ? N3 Ag1 N3 119.87(4) 2 3 ? N3 Ag1 N1 87.9(3) . . y N3 Ag1 N1 87.9(3) 2 . ? N3 Ag1 N1 87.9(3) 3 . ? N3 Ag1 Ag2 92.1(3) . . y N3 Ag1 Ag2 92.1(3) 2 . ? N3 Ag1 Ag2 92.1(3) 3 . ? N1 Ag1 Ag2 180.000(1) . . ? N4 Ag2 N4 119.86(5) 2 3 ? N4 Ag2 N4 119.86(5) 2 . y N4 Ag2 N4 119.86(5) 3 . ? N4 Ag2 N2 87.8(3) 2 . ? N4 Ag2 N2 87.8(3) 3 . ? N4 Ag2 N2 87.8(3) . . y N4 Ag2 Ag1 92.2(3) 2 . ? N4 Ag2 Ag1 92.2(3) 3 . ? N4 Ag2 Ag1 92.2(3) . . y N2 Ag2 Ag1 180.0 . . ? C1 N1 C1 112.4(10) 3 2 ? C1 N1 C1 112.4(10) 3 . ? C1 N1 C1 112.4(10) 2 . ? C1 N1 Ag1 106.4(12) 3 . ? C1 N1 Ag1 106.4(12) 2 . ? C1 N1 Ag1 106.4(12) . . ? N1 C1 C2 106.9(12) . . ? C1 C2 C3 111.7(13) . . ? N3 C3 C2 111.5(12) . . ? C4 N3 C3 120.2(12) . . ? C4 N3 Ag1 126.5(10) . . ? C3 N3 Ag1 111.7(9) . . ? N3 C4 C5 125.6(13) . . ? C9 C10 C5 120.9(9) . . ? C10 C5 C6 120.1(12) . . ? C10 C5 C4 123.8(11) . . ? C6 C5 C4 116.0(13) . . ? C5 C6 C7 120.0(13) . . ? C8 C7 C6 117.2(12) . . ? C7 C8 C9 121.0(13) . . ? C10 C9 C8 118.8(12) . . ? C10 C9 C11 122.2(11) . . ? C8 C9 C11 118.7(13) . . ? N4 C11 C9 123.9(14) . . ? C11 N4 C12 113.5(13) . . ? C11 N4 Ag2 129.4(11) . . ? C12 N4 Ag2 115.6(9) . . ? N4 C12 C13 112.9(11) . . ? C14 C13 C12 121.1(11) . . ? N2 C14 C13 117.2(12) . . ? C14 N2 C14 108.4(10) 3 . ? C14 N2 C14 108.4(10) 3 2 ? C14 N2 C14 108.4(10) . 2 ? C14 N2 Ag2 110.5(9) 3 . ? C14 N2 Ag2 110.5(9) . . ? C14 N2 Ag2 110.5(9) 2 . ? O12 N11 O13 125.0(17) . . ? O12 N11 O11 117.6(17) . . ? O13 N11 O11 116.5(16) . . ? N11 O11 O12 29.9(9) . . ? N11 O11 O13 31.1(9) . . ? O12 O11 O13 60.7(6) . . ? N11 O12 O11 32.5(9) . . ? N11 O12 O13 28.0(9) . . ? O11 O12 O13 60.2(7) . . ? N11 O13 O11 32.4(9) . . ? N11 O13 O12 27.0(9) . . ? O11 O13 O12 59.1(6) . . ? O22 N21 O21 120(2) . . ? O22 N21 O23 115(2) . . ? O21 N21 O23 115(2) . . ? N21 O21 O23 32.9(12) . . ? N21 O21 O22 29.7(13) . . ? O23 O21 O22 59.2(6) . . ? N21 O22 O23 32.8(12) . . ? N21 O22 O21 30.0(13) . . ? O23 O22 O21 59.4(6) . . ? N21 O23 O21 32.5(12) . . ? N21 O23 O22 32.2(12) . . ? O21 O23 O22 61.5(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.740 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.122