# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global #====================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 182 _publ_contact_author_name 'John P. Fackler' _publ_contact_author_address ; Department of Chemistry Texas A&M University College Station, TX 77843 ; _publ_contact_author_email fackler@mail.chem.tamu.edu _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; ? ; #========================================================================= #2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and X-Ray Structures of Silver and Gold Guanidinate-Like Complexes. A Au(II) Complex with 2.47 Au-Au Distance" ; loop_ _publ_author_name _publ_author_address M.D.Irwin ; Department of Chemistry Texas A&M University College Station 77843, TX ; 'Hanan E. Abdou' ; Department of Chemistry Texas A&M University College Station 77843, TX ; 'Ahmed A. Mohamed' ; Department of Chemistry Texas A&M University College Station 77843, TX ; 'Fackler Junior,John P.' ; Department of Chemistry Texas A&M University College Station 77843, TX ; #=================================================================== data_Auhpp _database_code_CSD 217313 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Au2 Cl2 N6' _chemical_formula_weight 741.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 22.220(4) _cell_length_b 10.838(2) _cell_length_c 8.0990(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.27(3) _cell_angle_gamma 90.00 _cell_volume 1817.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 16.428 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7093 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2130 _reflns_number_gt 1683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+85.2809P] 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 2130 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.2217(9) 0.577(2) 0.231(7) 0.20(2) Uani 1 1 d . . . H2A H 0.2644 0.5612 0.3174 0.242 Uiso 1 1 calc R . . H2B H 0.2192 0.5416 0.1186 0.242 Uiso 1 1 calc R . . Au1 Au 0.03897(2) 0.41337(4) 0.03901(8) 0.0425(2) Uani 1 1 d . . . N2 N -0.0387(6) 0.302(2) -0.043(5) 0.21(2) Uani 1 1 d . . . N1 N 0.1102(5) 0.5488(14) 0.112(2) 0.065(4) Uani 1 1 d . . . Cl1 Cl 0.11701(17) 0.2490(3) 0.1181(10) 0.097(2) Uani 1 1 d . . . N3 N 0.1451(4) 0.7413(10) 0.1451(16) 0.041(2) Uani 1 1 d . . . C4 C 0.1355(7) 0.8743(13) 0.137(3) 0.058(4) Uani 1 1 d . . . H4A H 0.1563 0.9096 0.0608 0.070 Uiso 1 1 calc R . . H4B H 0.1561 0.9087 0.2542 0.070 Uiso 1 1 calc R . . C7 C 0.0973(6) 0.6588(12) 0.0981(18) 0.041(3) Uani 1 1 d . . . C3 C 0.2108(7) 0.707(2) 0.211(5) 0.133(13) Uani 1 1 d . . . H3 H 0.2443 0.7637 0.2399 0.159 Uiso 1 1 calc R . . C6 C -0.0358(10) 0.190(4) -0.038(15) 0.80(15) Uani 1 1 d . . . H6A H -0.0081 0.1774 0.0843 0.955 Uiso 1 1 calc R . . H6B H -0.0078 0.1761 -0.1046 0.955 Uiso 1 1 calc R . . C5 C 0.0676(8) 0.9092(12) 0.069(3) 0.082(7) Uani 1 1 d . . . H5 H 0.0510 0.9889 0.0520 0.098 Uiso 1 1 calc R . . C1 C 0.1648(18) 0.513(4) 0.298(5) 0.170(15) Uiso 1 1 d . . . H1A H 0.1700 0.4245 0.3180 0.204 Uiso 1 1 calc R . . H1B H 0.1600 0.5540 0.3989 0.204 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 C2 0.014(7) 0.068(15) 0.46(7) 0.01(2) 0.010(17) 0.003(8) Au1 0.0204(3) 0.0193(3) 0.0788(4) 0.0009(2) 0.0072(2) 0.00234(14) N2 0.013(6) 0.059(12) 0.48(6) -0.004(19) 0.012(15) 0.005(7) N1 0.021(5) 0.073(9) 0.091(10) 0.012(8) 0.007(6) 0.037(6) Cl1 0.0260(15) 0.0222(15) 0.215(6) 0.002(2) 0.008(2) 0.0072(13) N3 0.022(4) 0.036(5) 0.059(6) -0.002(5) 0.006(4) -0.003(4) C4 0.046(8) 0.029(6) 0.090(11) -0.003(7) 0.014(8) -0.015(6) C7 0.028(6) 0.036(6) 0.054(7) 0.002(5) 0.008(5) -0.003(5) C3 0.017(7) 0.073(14) 0.27(4) -0.010(18) 0.005(13) -0.013(7) C6 0.005(10) 0.10(3) 2.0(4) 0.01(8) 0.02(5) -0.013(12) C5 0.043(9) 0.016(6) 0.17(2) -0.003(8) 0.019(10) 0.000(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 C2 C3 1.42(3) . ? C2 C1 1.70(5) . ? Au1 N2 2.010(17) . ? Au1 N1 2.081(16) . ? Au1 Cl1 2.405(3) . ? Au1 Au1 2.4759(9) 5_565 ? N2 C6 1.21(5) . ? N2 C7 1.286(18) 5_565 ? N1 C7 1.222(19) . ? N1 C1 1.60(4) . ? N3 C7 1.334(15) . ? N3 C3 1.412(19) . ? N3 C4 1.455(17) . ? C4 C5 1.46(2) . ? C7 N2 1.286(18) 5_565 ? C6 C5 1.26(4) 5_565 ? C5 C6 1.26(4) 5_565 ? 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 C3 C2 C1 109(3) . . ? N2 Au1 N1 172.0(6) . . ? N2 Au1 Cl1 95.4(5) . . ? N1 Au1 Cl1 92.6(3) . . ? N2 Au1 Au1 86.2(5) . 5_565 ? N1 Au1 Au1 85.8(3) . 5_565 ? Cl1 Au1 Au1 178.45(9) . 5_565 ? C6 N2 C7 112.1(18) . 5_565 ? C6 N2 Au1 123.9(14) . . ? C7 N2 Au1 123.9(15) 5_565 . ? C7 N1 C1 113(2) . . ? C7 N1 Au1 122.2(8) . . ? C1 N1 Au1 109.5(18) . . ? C7 N3 C3 122.4(13) . . ? C7 N3 C4 124.2(11) . . ? C3 N3 C4 113.4(13) . . ? N3 C4 C5 113.0(11) . . ? N1 C7 N2 121.8(15) . 5_565 ? N1 C7 N3 119.5(12) . . ? N2 C7 N3 118.7(15) 5_565 . ? N3 C3 C2 114.5(15) . . ? N2 C6 C5 146(2) . 5_565 ? C6 C5 C4 106.3(17) 5_565 . ? N1 C1 C2 90(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 3.713 _refine_diff_density_min -2.859 _refine_diff_density_rms 0.306 data_aghpp _database_code_CSD 217314 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 Ag4 N12' _chemical_formula_weight 980.03 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 16.2031(9) _cell_length_b 16.2031(9) _cell_length_c 12.7823(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3355.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.339 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11033 _diffrn_reflns_av_R_equivalents 0.1019 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3833 _reflns_number_gt 3669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+7.3917P] 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 -0.04(5) _refine_ls_number_reflns 3833 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.10533(3) 0.93699(2) 0.52060(3) 0.03077(12) Uani 1 1 d . . . Ag2 Ag 0.38765(3) 0.05552(2) 0.23605(3) 0.03147(12) Uani 1 1 d . . . N3 N 0.1547(3) 0.9489(3) 0.3715(3) 0.0318(9) Uani 1 1 d . . . C8 C 0.2929(4) 0.1243(5) 0.4251(5) 0.0406(13) Uani 1 1 d . . . H8A H 0.2523 0.1070 0.3738 0.049 Uiso 1 1 calc R . . H8B H 0.2865 0.1832 0.4361 0.049 Uiso 1 1 calc R . . N5 N 0.4204(3) 0.1281(3) 0.5580(3) 0.0357(10) Uani 1 1 d . . . C1 C 0.1199(4) 0.9474(4) 0.7585(5) 0.0422(13) Uani 1 1 d . . . H1A H 0.0918 0.9937 0.7909 0.051 Uiso 1 1 calc R . . H1B H 0.1721 0.9669 0.7308 0.051 Uiso 1 1 calc R . . N6 N 0.3851(3) 0.0160(3) 0.0808(4) 0.0324(10) Uani 1 1 d . . . C5 C 0.2159(4) 0.8892(4) 0.3380(5) 0.0377(12) Uani 1 1 d . . . H5A H 0.2252 0.8492 0.3932 0.045 Uiso 1 1 calc R . . H5B H 0.2677 0.9170 0.3237 0.045 Uiso 1 1 calc R . . N1 N 0.0689(3) 0.9135(3) 0.6734(3) 0.0321(9) Uani 1 1 d . . . N4 N 0.3763(3) 0.1069(3) 0.3856(3) 0.0312(10) Uani 1 1 d . . . C4 C 0.0031(3) 0.8702(3) 0.7003(4) 0.0260(10) Uani 1 1 d . . . C6 C 0.1860(4) 0.8453(4) 0.2398(5) 0.0427(13) Uani 1 1 d . . . H6A H 0.1333 0.8186 0.2528 0.051 Uiso 1 1 calc R . . H6B H 0.2255 0.8035 0.2186 0.051 Uiso 1 1 calc R . . C13 C 0.3900(6) 0.0813(4) 0.0015(5) 0.0509(17) Uani 1 1 d . . . H13A H 0.4467 0.0863 -0.0220 0.061 Uiso 1 1 calc R . . H13B H 0.3742 0.1334 0.0331 0.061 Uiso 1 1 calc R . . C10 C 0.3416(4) 0.1117(5) 0.6046(5) 0.0443(15) Uani 1 1 d . . . H10A H 0.3208 0.1621 0.6358 0.053 Uiso 1 1 calc R . . H10B H 0.3486 0.0715 0.6602 0.053 Uiso 1 1 calc R . . N2 N -0.0101(3) 0.8493(3) 0.8032(3) 0.0356(10) Uani 1 1 d . . . C7 C 0.1770(4) 0.9107(4) 0.1548(5) 0.0398(13) Uani 1 1 d . . . H7A H 0.2295 0.9175 0.1194 0.048 Uiso 1 1 calc R . . H7B H 0.1370 0.8920 0.1035 0.048 Uiso 1 1 calc R . . C9 C 0.2780(4) 0.0791(4) 0.5270(5) 0.0418(13) Uani 1 1 d . . . H9A H 0.2848 0.0201 0.5173 0.050 Uiso 1 1 calc R . . H9B H 0.2226 0.0896 0.5523 0.050 Uiso 1 1 calc R . . C12 C 0.4382(3) 0.1160(3) 0.4522(4) 0.0270(10) Uani 1 1 d . . . C11 C 0.4832(4) 0.1425(5) 0.6361(4) 0.0438(15) Uani 1 1 d . . . H11A H 0.4891 0.0933 0.6787 0.053 Uiso 1 1 calc R . . H11B H 0.4654 0.1871 0.6815 0.053 Uiso 1 1 calc R . . C2 C 0.1352(4) 0.8799(5) 0.8398(5) 0.0475(16) Uani 1 1 d . . . H2A H 0.1616 0.8326 0.8075 0.057 Uiso 1 1 calc R . . H2B H 0.1707 0.9003 0.8951 0.057 Uiso 1 1 calc R . . C14 C 0.3360(6) 0.0650(5) -0.0903(6) 0.0516(17) Uani 1 1 d . . . H14 H 0.2953 0.1004 -0.1152 0.062 Uiso 1 1 calc R . . C3 C 0.0531(5) 0.8561(5) 0.8831(4) 0.0495(17) Uani 1 1 d . . . H3A H 0.0583 0.8035 0.9189 0.059 Uiso 1 1 calc R . . H3B H 0.0362 0.8969 0.9342 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0398(2) 0.0364(2) 0.0161(2) 0.00276(14) 0.00210(15) -0.00324(16) Ag2 0.0440(2) 0.0351(2) 0.01534(19) -0.00440(14) -0.00484(14) -0.00289(16) N3 0.036(2) 0.043(2) 0.0165(19) 0.0028(18) 0.0025(17) -0.003(2) C8 0.035(3) 0.060(4) 0.027(3) 0.001(3) 0.001(2) -0.003(3) N5 0.032(2) 0.060(3) 0.015(2) -0.008(2) 0.0040(17) -0.001(2) C1 0.051(3) 0.050(3) 0.026(3) 0.001(3) -0.003(3) -0.006(3) N6 0.051(3) 0.031(2) 0.0158(19) -0.0026(16) -0.0032(18) -0.006(2) C5 0.035(3) 0.052(3) 0.026(3) 0.004(3) -0.001(2) 0.001(3) N1 0.043(3) 0.038(2) 0.0155(18) 0.0031(17) -0.0017(17) -0.0041(19) N4 0.034(2) 0.045(3) 0.0149(18) -0.0064(18) -0.0005(16) -0.002(2) C4 0.039(3) 0.024(2) 0.015(2) 0.0051(17) 0.0009(19) 0.0078(19) C6 0.046(3) 0.052(3) 0.030(3) 0.000(3) 0.004(3) 0.006(3) C13 0.084(5) 0.040(3) 0.028(3) 0.005(3) -0.007(3) -0.014(3) C10 0.039(3) 0.071(5) 0.023(3) -0.001(3) 0.004(2) 0.006(3) N2 0.051(3) 0.041(3) 0.015(2) 0.0073(18) -0.0021(19) 0.001(2) C7 0.045(3) 0.056(4) 0.018(2) -0.004(2) 0.005(2) 0.008(3) C9 0.036(3) 0.057(4) 0.032(3) 0.005(3) 0.004(2) -0.002(3) C12 0.039(3) 0.031(2) 0.0110(19) -0.0003(17) 0.0008(18) 0.002(2) C11 0.049(3) 0.065(4) 0.017(2) -0.012(3) -0.006(2) 0.005(3) C2 0.046(3) 0.071(5) 0.026(3) 0.006(3) -0.011(3) -0.002(3) C14 0.075(5) 0.047(4) 0.033(3) 0.001(3) -0.003(3) 0.009(3) C3 0.063(4) 0.071(5) 0.015(2) 0.014(3) -0.006(3) -0.015(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 N1 2.076(4) . ? Ag1 N3 2.076(4) . ? Ag1 Ag1 2.8614(6) 3_466 ? Ag1 Ag1 2.8614(6) 4_666 ? Ag2 N6 2.086(4) . ? Ag2 N4 2.093(4) . ? Ag2 Ag2 2.8937(6) 7 ? Ag2 Ag2 2.8937(6) 8_545 ? N3 C4 1.332(7) 4_666 ? N3 C5 1.449(8) . ? C8 N4 1.471(8) . ? C8 C9 1.513(8) . ? N5 C12 1.397(6) . ? N5 C10 1.434(8) . ? N5 C11 1.444(7) . ? C1 N1 1.473(7) . ? C1 C2 1.529(9) . ? N6 C12 1.328(7) 8_545 ? N6 C13 1.467(7) . ? C5 C6 1.522(9) . ? N1 C4 1.322(7) . ? N4 C12 1.324(7) . ? C4 N3 1.332(7) 3_466 ? C4 N2 1.375(6) . ? C6 C7 1.526(9) . ? C13 C14 1.488(10) . ? C10 C9 1.523(9) . ? N2 C3 1.450(8) . ? N2 C7 1.456(8) 3_466 ? C7 N2 1.456(8) 4_666 ? C12 N6 1.328(7) 7 ? C11 C14 1.492(10) 7 ? C2 C3 1.490(10) . ? C14 C11 1.492(10) 8_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 172.1(2) . . ? N1 Ag1 Ag1 81.84(14) . 3_466 ? N3 Ag1 Ag1 102.75(14) . 3_466 ? N1 Ag1 Ag1 106.25(14) . 4_666 ? N3 Ag1 Ag1 80.48(14) . 4_666 ? Ag1 Ag1 Ag1 88.058(5) 3_466 4_666 ? N6 Ag2 N4 171.63(19) . . ? N6 Ag2 Ag2 103.51(14) . 7 ? N4 Ag2 Ag2 80.99(13) . 7 ? N6 Ag2 Ag2 80.49(13) . 8_545 ? N4 Ag2 Ag2 106.82(14) . 8_545 ? Ag2 Ag2 Ag2 89.130(4) 7 8_545 ? C4 N3 C5 116.3(4) 4_666 . ? C4 N3 Ag1 125.2(4) 4_666 . ? C5 N3 Ag1 118.2(4) . . ? N4 C8 C9 110.4(5) . . ? C12 N5 C10 124.1(5) . . ? C12 N5 C11 123.1(5) . . ? C10 N5 C11 111.8(5) . . ? N1 C1 C2 109.0(5) . . ? C12 N6 C13 117.8(5) 8_545 . ? C12 N6 Ag2 126.4(4) 8_545 . ? C13 N6 Ag2 115.7(4) . . ? N3 C5 C6 109.8(5) . . ? C4 N1 C1 117.3(5) . . ? C4 N1 Ag1 124.8(4) . . ? C1 N1 Ag1 117.9(4) . . ? C12 N4 C8 117.0(4) . . ? C12 N4 Ag2 124.4(4) . . ? C8 N4 Ag2 118.1(4) . . ? N1 C4 N3 120.9(5) . 3_466 ? N1 C4 N2 120.3(5) . . ? N3 C4 N2 118.9(5) 3_466 . ? C5 C6 C7 107.0(5) . . ? N6 C13 C14 112.6(6) . . ? N5 C10 C9 113.3(5) . . ? C4 N2 C3 123.1(5) . . ? C4 N2 C7 124.2(5) . 3_466 ? C3 N2 C7 112.7(5) . 3_466 ? N2 C7 C6 112.2(5) 4_666 . ? C8 C9 C10 106.6(5) . . ? N4 C12 N6 120.9(4) . 7 ? N4 C12 N5 118.8(5) . . ? N6 C12 N5 120.4(5) 7 . ? N5 C11 C14 113.1(5) . 7 ? C3 C2 C1 107.0(6) . . ? C13 C14 C11 109.2(6) . 8_545 ? N2 C3 C2 112.8(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.028 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.131