# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c2c _database_code_depnum_ccdc_archive 'CCDC 798512' #TrackingRef 'cif file upate-798512.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag5 I7, C14 H18 N2' _chemical_formula_sum 'C14 H18 Ag5 I7 N2' _chemical_formula_weight 1641.95 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' I I -0.4742 1.8119 '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 _symmetry_space_group_name_Hall -C2yc 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 18.407(4) _cell_length_b 15.378(3) _cell_length_c 13.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.44(3) _cell_angle_gamma 90.00 _cell_volume 2986.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6630 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 10.463 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.009 _exptl_absorpt_correction_T_max 0.124 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 6630 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3427 _reflns_number_gt 2632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.0791P)^2^+7.5580P] 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 SHELXL _refine_ls_extinction_coef 0.00117(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3427 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 I1 I 0.07022(4) 0.40637(4) 0.47272(5) 0.0486(2) Uani 1 1 d . . . I2 I 0.14310(4) 0.19494(4) 0.29102(5) 0.0524(2) Uani 1 1 d . . . I3 I 0.25499(4) 0.48720(4) 0.36455(5) 0.04592(19) Uani 1 1 d . . . I4 I 0.0000 0.66236(5) 0.2500 0.0456(2) Uani 1 2 d S . . Ag1 Ag 0.0000 0.30559(9) 0.2500 0.0671(3) Uani 1 2 d S . . Ag2 Ag 0.21027(6) 0.34773(6) 0.44881(8) 0.0666(3) Uani 1 1 d . . . Ag3 Ag 0.06889(7) 0.52176(9) 0.20517(14) 0.1175(6) Uani 1 1 d . . . N1 N 0.3192(5) 0.3489(4) 0.2098(6) 0.0403(15) Uani 1 1 d . . . C1 C 0.3569(7) 0.4231(6) 0.2095(8) 0.052(2) Uani 1 1 d . . . H1 H 0.3249 0.4577 0.1372 0.062 Uiso 1 1 calc R . . C2 C 0.4438(7) 0.4485(7) 0.3172(10) 0.056(2) Uani 1 1 d . . . H2 H 0.4703 0.5003 0.3181 0.067 Uiso 1 1 calc R . . C3 C 0.4898(7) 0.3960(7) 0.4219(10) 0.057(2) Uani 1 1 d . . . H3 H 0.5487 0.4113 0.4941 0.069 Uiso 1 1 calc R . . C4 C 0.4494(7) 0.3220(6) 0.4203(8) 0.053(2) Uani 1 1 d . . . H4 H 0.4795 0.2874 0.4925 0.064 Uiso 1 1 calc R . . C5 C 0.3640(6) 0.2980(6) 0.3122(7) 0.0459(19) Uani 1 1 d . . . H5 H 0.3372 0.2461 0.3102 0.055 Uiso 1 1 calc R . . C6 C 0.2242(6) 0.3217(6) 0.0945(8) 0.050(2) Uani 1 1 d . . . H6A H 0.1956 0.3694 0.0344 0.060 Uiso 1 1 calc R . . H6B H 0.1858 0.3088 0.1192 0.060 Uiso 1 1 calc R . . C7 C 0.2282(6) 0.2425(6) 0.0313(7) 0.0436(18) Uani 1 1 d . . . H7A H 0.2627 0.1973 0.0945 0.052 Uiso 1 1 calc R . . H7B H 0.1656 0.2213 -0.0319 0.052 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 I1 0.0559(4) 0.0506(4) 0.0406(3) 0.0052(2) 0.0306(3) 0.0150(3) I2 0.0464(3) 0.0493(4) 0.0396(3) -0.0046(2) 0.0159(3) 0.0060(2) I3 0.0422(3) 0.0471(3) 0.0489(3) -0.0068(2) 0.0285(3) -0.0020(2) I4 0.0374(4) 0.0444(4) 0.0468(4) 0.000 0.0222(3) 0.000 Ag1 0.0531(6) 0.0862(9) 0.0512(6) 0.000 0.0271(5) 0.000 Ag2 0.0642(5) 0.0628(5) 0.0600(5) -0.0023(4) 0.0323(4) -0.0075(4) Ag3 0.0498(5) 0.1120(9) 0.1305(10) -0.0654(8) 0.0264(6) 0.0027(5) N1 0.038(3) 0.040(4) 0.039(3) -0.002(3) 0.022(3) 0.005(3) C1 0.071(6) 0.043(5) 0.044(5) 0.003(4) 0.037(5) 0.003(4) C2 0.069(6) 0.053(5) 0.065(6) -0.015(5) 0.051(6) -0.018(5) C3 0.049(5) 0.060(6) 0.055(6) -0.013(4) 0.028(5) -0.004(4) C4 0.052(5) 0.052(5) 0.034(4) -0.002(4) 0.016(4) 0.000(4) C5 0.050(5) 0.040(4) 0.036(4) 0.000(3) 0.021(4) 0.005(4) C6 0.042(4) 0.059(5) 0.031(4) -0.003(4) 0.013(4) 0.012(4) C7 0.047(4) 0.043(4) 0.031(4) -0.005(3) 0.020(4) -0.002(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 I1 Ag3 2.7963(15) 2 ? I1 Ag1 2.8728(12) . ? I1 Ag2 2.9317(12) . ? I2 Ag2 2.8701(17) 7_556 ? I2 Ag2 2.8811(12) . ? I2 Ag1 2.8860(12) . ? I3 Ag3 2.7353(17) . ? I3 Ag2 2.7800(11) . ? I4 Ag3 2.7569(13) 2 ? I4 Ag3 2.7569(13) . ? Ag1 I1 2.8728(12) 2 ? Ag1 I2 2.8860(12) 2 ? Ag1 Ag2 3.1120(17) . ? Ag1 Ag2 3.1120(17) 2 ? Ag2 I2 2.8701(17) 7_556 ? Ag2 Ag2 3.2509(19) 7_556 ? Ag3 I1 2.7963(15) 2 ? N1 C5 1.335(10) . ? N1 C1 1.336(12) . ? N1 C6 1.507(10) . ? C1 C2 1.390(14) . ? C1 H1 0.9300 . ? C2 C3 1.368(15) . ? C2 H2 0.9300 . ? C3 C4 1.353(14) . ? C3 H3 0.9300 . ? C4 C5 1.372(12) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.514(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C7 1.500(17) 7 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? 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 Ag3 I1 Ag1 82.50(6) 2 . ? Ag3 I1 Ag2 120.02(4) 2 . ? Ag1 I1 Ag2 64.83(3) . . ? Ag2 I2 Ag2 68.84(4) 7_556 . ? Ag2 I2 Ag1 114.97(3) 7_556 . ? Ag2 I2 Ag1 65.32(4) . . ? Ag3 I3 Ag2 85.76(5) . . ? Ag3 I4 Ag3 76.68(8) 2 . ? I1 Ag1 I1 114.70(6) . 2 ? I1 Ag1 I2 106.41(3) . 2 ? I1 Ag1 I2 110.71(4) 2 2 ? I1 Ag1 I2 110.71(4) . . ? I1 Ag1 I2 106.41(3) 2 . ? I2 Ag1 I2 107.74(6) 2 . ? I1 Ag1 Ag2 58.50(3) . . ? I1 Ag1 Ag2 107.33(5) 2 . ? I2 Ag1 Ag2 141.84(4) 2 . ? I2 Ag1 Ag2 57.27(3) . . ? I1 Ag1 Ag2 107.33(5) . 2 ? I1 Ag1 Ag2 58.50(3) 2 2 ? I2 Ag1 Ag2 57.27(3) 2 2 ? I2 Ag1 Ag2 141.84(4) . 2 ? Ag2 Ag1 Ag2 155.96(6) . 2 ? I3 Ag2 I2 112.49(4) . 7_556 ? I3 Ag2 I2 115.35(4) . . ? I2 Ag2 I2 111.16(4) 7_556 . ? I3 Ag2 I1 108.14(4) . . ? I2 Ag2 I1 99.19(4) 7_556 . ? I2 Ag2 I1 109.18(4) . . ? I3 Ag2 Ag1 109.56(4) . . ? I2 Ag2 Ag1 136.52(4) 7_556 . ? I2 Ag2 Ag1 57.42(3) . . ? I1 Ag2 Ag1 56.67(3) . . ? I3 Ag2 Ag2 135.83(5) . 7_556 ? I2 Ag2 Ag2 55.74(3) 7_556 7_556 ? I2 Ag2 Ag2 55.42(4) . 7_556 ? I1 Ag2 Ag2 115.61(4) . 7_556 ? Ag1 Ag2 Ag2 99.40(5) . 7_556 ? I3 Ag3 I4 120.17(4) . . ? I3 Ag3 I1 125.60(5) . 2 ? I4 Ag3 I1 112.62(4) . 2 ? C5 N1 C1 121.1(7) . . ? C5 N1 C6 118.5(7) . . ? C1 N1 C6 120.4(7) . . ? N1 C1 C2 120.0(8) . . ? N1 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C3 C2 C1 118.9(9) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 119.9(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.9(9) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 120.2(9) . . ? N1 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N1 C6 C7 111.8(7) . . ? N1 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N1 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C7 C7 C6 115.1(9) 7 . ? C7 C7 H7A 108.5 7 . ? C6 C7 H7A 108.5 . . ? C7 C7 H7B 108.5 7 . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.817 _refine_diff_density_min -4.139 _refine_diff_density_rms 0.478 data_p32 _database_code_depnum_ccdc_archive 'CCDC 798513' #TrackingRef 'cif file update-798513.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag5 I7, C18 H26 N2' _chemical_formula_sum 'C18 H26 Ag5 I7 N2' _chemical_formula_weight 1698.06 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P32 _symmetry_space_group_name_Hall P32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 12.0730(17) _cell_length_b 12.0730(17) _cell_length_c 20.906(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2639.0(7) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11507 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.54 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2262 _exptl_absorpt_coefficient_mu 8.887 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.125 _exptl_absorpt_correction_T_max 0.396 _exptl_absorpt_process_details 'TEXRAY software (Molecular Structure Corporation, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotor target' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Weissenberg IP' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean None _diffrn_standards_number None _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 11507 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7768 _reflns_number_gt 5270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'TEXRAY software (Molecular Structure Corporation, 1999)' _computing_cell_refinement 'TEXRAY software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material "SHELXL-97/2 (Sheldrick,1997)')" _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^)+(0.1172P)^2^+0.9695P] 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 SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.63(8) _refine_ls_number_reflns 7768 _refine_ls_number_parameters 211 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.003 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 I1 I 0.80958(15) 0.8646(2) 0.02195(10) 0.0995(6) Uani 1 1 d . . . I2 I 0.59090(19) 0.44101(19) 0.10441(8) 0.0883(5) Uani 1 1 d . . . I3 I 0.37242(13) 0.54873(13) -0.03587(6) 0.0655(3) Uani 1 1 d . . . I4 I 0.48339(13) 0.76677(12) 0.15467(6) 0.0656(3) Uani 1 1 d . . . I5 I 0.49294(13) 0.51872(13) 0.30968(6) 0.0675(3) Uani 1 1 d . . . I6 I 0.16703(15) 0.34040(14) 0.15026(8) 0.0794(4) Uani 1 1 d . . . I7 I 0.08162(12) 0.65710(13) 0.07175(7) 0.0672(3) Uani 1 1 d . . . Ag1 Ag 0.5782(2) 0.6540(2) 0.05997(11) 0.0891(5) Uani 1 1 d . . . Ag2 Ag 0.43397(19) 0.5010(2) 0.17671(9) 0.0844(5) Uani 1 1 d . . . Ag3 Ag 0.2269(2) 0.3982(2) 0.28227(10) 0.0942(6) Uani 1 1 d . . . Ag4 Ag 0.2120(2) 0.5934(2) 0.16384(10) 0.0892(5) Uani 1 1 d . . . Ag5 Ag 0.3307(2) 0.7307(2) 0.03250(13) 0.0981(6) Uani 1 1 d . . . N1 N 1.199(3) 1.075(2) -0.0080(12) 0.104(4) Uani 1 1 d . . . N2 N 1.470(3) 1.228(3) 0.4767(11) 0.100(3) Uani 1 1 d . . . C1 C 1.152(4) 0.972(3) -0.0477(14) 0.104(4) Uani 1 1 d . . . H1 H 1.1067 0.8902 -0.0304 0.125 Uiso 1 1 calc R . . C2 C 1.171(4) 0.986(3) -0.1124(14) 0.104(4) Uani 1 1 d . . . H2 H 1.1345 0.9150 -0.1394 0.125 Uiso 1 1 calc R . . C3 C 1.244(4) 1.107(3) -0.1365(15) 0.104(4) Uani 1 1 d . . . H3 H 1.2656 1.1203 -0.1797 0.125 Uiso 1 1 calc R . . C4 C 1.287(4) 1.211(3) -0.0947(14) 0.104(4) Uani 1 1 d . . . H4 H 1.3260 1.2945 -0.1102 0.125 Uiso 1 1 calc R . . C5 C 1.269(4) 1.187(3) -0.0304(14) 0.104(4) Uani 1 1 d . . . H5 H 1.3102 1.2546 -0.0020 0.125 Uiso 1 1 calc R . . C6 C 1.169(3) 1.050(3) 0.0616(11) 0.089(7) Uani 1 1 d . . . H6A H 1.1473 1.1112 0.0790 0.106 Uiso 1 1 calc R . . H6B H 1.0954 0.9648 0.0673 0.106 Uiso 1 1 calc R . . C7 C 1.273(3) 1.059(3) 0.0935(13) 0.089(7) Uiso 1 1 d . . . H7A H 1.3466 1.1428 0.0855 0.107 Uiso 1 1 calc R . . H7B H 1.2921 0.9958 0.0762 0.107 Uiso 1 1 calc R . . C8 C 1.255(5) 1.040(5) 0.165(3) 0.151(15) Uiso 1 1 d . . . H8A H 1.2583 1.1152 0.1831 0.181 Uiso 1 1 calc R . . H8B H 1.1692 0.9685 0.1725 0.181 Uiso 1 1 calc R . . C9 C 1.345(6) 1.015(6) 0.200(3) 0.18(2) Uiso 1 1 d . . . H9A H 1.4324 1.0846 0.1972 0.219 Uiso 1 1 calc R . . H9B H 1.3404 0.9351 0.1874 0.219 Uiso 1 1 calc R . . C10 C 1.279(6) 1.005(7) 0.274(3) 0.18(2) Uiso 1 1 d . . . H10A H 1.2003 1.0075 0.2716 0.221 Uiso 1 1 calc R . . H10B H 1.2638 0.9285 0.2972 0.221 Uiso 1 1 calc R . . C11 C 1.388(6) 1.127(5) 0.3041(14) 0.159(19) Uani 1 1 d . . . H11A H 1.3907 1.2014 0.2850 0.190 Uiso 1 1 calc R . . H11B H 1.4695 1.1315 0.2954 0.190 Uiso 1 1 calc R . . C12 C 1.369(4) 1.128(3) 0.3781(13) 0.125(13) Uani 1 1 d . . . H12A H 1.3007 1.1461 0.3869 0.150 Uiso 1 1 calc R . . H12B H 1.3440 1.0441 0.3957 0.150 Uiso 1 1 calc R . . C13 C 1.484(3) 1.221(3) 0.4070(13) 0.112(11) Uani 1 1 d . . . H13A H 1.5089 1.3043 0.3883 0.135 Uiso 1 1 calc R . . H13B H 1.5509 1.2018 0.3982 0.135 Uiso 1 1 calc R . . C14 C 1.501(4) 1.162(3) 0.5139(13) 0.100(3) Uani 1 1 d . . . H14 H 1.5264 1.1067 0.4970 0.120 Uiso 1 1 calc R . . C15 C 1.495(3) 1.176(3) 0.5826(13) 0.100(3) Uani 1 1 d . . . H15 H 1.5285 1.1400 0.6107 0.120 Uiso 1 1 calc R . . C16 C 1.441(3) 1.240(3) 0.6040(14) 0.100(3) Uani 1 1 d . . . H16 H 1.4312 1.2450 0.6479 0.120 Uiso 1 1 calc R . . C17 C 1.401(3) 1.298(3) 0.5651(14) 0.100(3) Uani 1 1 d . . . H17 H 1.3554 1.3360 0.5796 0.120 Uiso 1 1 calc R . . C18 C 1.431(3) 1.298(3) 0.4992(14) 0.100(3) Uani 1 1 d . . . H18 H 1.4211 1.3525 0.4716 0.120 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 I1 0.0607(8) 0.1200(14) 0.1048(12) 0.0306(11) -0.0022(8) 0.0355(8) I2 0.1046(12) 0.1052(11) 0.0821(9) 0.0109(8) 0.0175(8) 0.0726(10) I3 0.0748(8) 0.0637(7) 0.0588(6) -0.0024(5) 0.0005(6) 0.0352(6) I4 0.0650(7) 0.0602(7) 0.0669(7) -0.0026(5) -0.0048(6) 0.0279(6) I5 0.0727(8) 0.0741(8) 0.0612(7) -0.0037(6) -0.0091(6) 0.0409(6) I6 0.0815(9) 0.0755(8) 0.0837(9) -0.0200(7) -0.0199(7) 0.0410(7) I7 0.0619(7) 0.0694(7) 0.0704(7) 0.0040(6) -0.0030(6) 0.0330(6) Ag1 0.0911(12) 0.0886(12) 0.0859(11) 0.0135(10) 0.0109(10) 0.0435(10) Ag2 0.0856(11) 0.1018(13) 0.0691(9) 0.0002(9) 0.0078(9) 0.0493(11) Ag3 0.0775(11) 0.1034(14) 0.0816(11) 0.0048(10) 0.0090(9) 0.0301(10) Ag4 0.0851(11) 0.0959(13) 0.0868(12) 0.0052(10) -0.0076(9) 0.0453(10) Ag5 0.0947(13) 0.0928(13) 0.1080(15) 0.0086(11) 0.0231(12) 0.0476(12) N1 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) N2 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(8) C1 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) C2 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) C3 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) C4 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) C5 0.152(11) 0.082(6) 0.084(6) -0.006(5) -0.006(7) 0.063(7) C6 0.100(18) 0.107(18) 0.066(12) -0.010(13) 0.014(12) 0.058(16) C11 0.25(6) 0.18(4) 0.057(15) 0.02(2) 0.01(2) 0.11(4) C12 0.15(3) 0.096(19) 0.064(13) -0.017(14) -0.038(16) 0.015(19) C13 0.11(2) 0.11(2) 0.072(14) 0.020(14) 0.016(14) 0.018(17) C14 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(8) C15 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(8) C16 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(8) C17 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(8) C18 0.146(10) 0.111(8) 0.076(6) 0.016(5) 0.008(6) 0.089(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 I1 Ag3 2.779(3) 2_664 ? I1 Ag1 2.793(3) . ? I2 Ag2 2.788(2) . ? I2 Ag1 2.810(3) . ? I3 Ag5 2.869(3) . ? I3 Ag4 2.888(3) 2_664 ? I3 Ag1 2.940(3) . ? I3 Ag3 3.136(3) 2_664 ? I4 Ag4 2.880(3) . ? I4 Ag1 2.940(3) . ? I4 Ag2 2.991(3) . ? I4 Ag5 3.051(3) . ? I5 Ag5 2.825(3) 3_565 ? I5 Ag3 2.844(3) . ? I5 Ag2 2.851(2) . ? I6 Ag4 2.837(3) . ? I6 Ag3 2.850(3) . ? I6 Ag2 2.864(3) . ? I7 Ag5 2.799(3) . ? I7 Ag4 2.826(2) . ? Ag1 Ag2 3.030(3) . ? Ag1 Ag3 3.052(3) 2_664 ? Ag2 Ag3 3.091(3) . ? Ag3 I1 2.779(3) 3_565 ? Ag3 Ag1 3.052(3) 3_565 ? Ag3 I3 3.136(3) 3_565 ? Ag3 Ag5 3.360(3) 3_565 ? Ag4 I3 2.888(3) 3_565 ? Ag4 Ag5 3.157(3) . ? Ag5 I5 2.825(3) 2_664 ? Ag5 Ag3 3.360(3) 2_664 ? N1 C5 1.27(4) . ? N1 C1 1.36(4) . ? N1 C6 1.50(3) . ? N2 C18 1.24(4) . ? N2 C14 1.30(3) . ? N2 C13 1.47(4) . ? C1 C2 1.37(4) . ? C1 H1 0.9300 . ? C2 C3 1.38(4) . ? C2 H2 0.9300 . ? C3 C4 1.40(4) . ? C3 H3 0.9300 . ? C4 C5 1.37(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.38(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.51(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.47(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.72(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.54(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.57(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.42(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.45(4) . ? C14 H14 0.9300 . ? C15 C16 1.32(4) . ? C15 H15 0.9300 . ? C16 C17 1.31(4) . ? C16 H16 0.9300 . ? C17 C18 1.42(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 Ag3 I1 Ag1 66.44(8) 2_664 . ? Ag2 I2 Ag1 65.55(7) . . ? Ag5 I3 Ag4 108.20(8) . 2_664 ? Ag5 I3 Ag1 76.31(8) . . ? Ag4 I3 Ag1 124.51(8) 2_664 . ? Ag5 I3 Ag3 67.88(7) . 2_664 ? Ag4 I3 Ag3 70.54(7) 2_664 2_664 ? Ag1 I3 Ag3 60.21(6) . 2_664 ? Ag4 I4 Ag1 105.84(7) . . ? Ag4 I4 Ag2 70.48(6) . . ? Ag1 I4 Ag2 61.45(6) . . ? Ag4 I4 Ag5 64.25(7) . . ? Ag1 I4 Ag5 73.58(7) . . ? Ag2 I4 Ag5 101.17(7) . . ? Ag5 I5 Ag3 72.70(7) 3_565 . ? Ag5 I5 Ag2 106.78(8) 3_565 . ? Ag3 I5 Ag2 65.76(6) . . ? Ag4 I6 Ag3 75.57(7) . . ? Ag4 I6 Ag2 72.95(7) . . ? Ag3 I6 Ag2 65.51(6) . . ? Ag5 I7 Ag4 68.28(8) . . ? I1 Ag1 I2 116.10(10) . . ? I1 Ag1 I4 102.34(9) . . ? I2 Ag1 I4 114.41(9) . . ? I1 Ag1 I3 116.36(9) . . ? I2 Ag1 I3 104.53(9) . . ? I4 Ag1 I3 102.63(8) . . ? I1 Ag1 Ag2 142.42(11) . . ? I2 Ag1 Ag2 56.88(6) . . ? I4 Ag1 Ag2 60.11(6) . . ? I3 Ag1 Ag2 100.47(8) . . ? I1 Ag1 Ag3 56.56(7) . 2_664 ? I2 Ag1 Ag3 148.76(10) . 2_664 ? I4 Ag1 Ag3 96.64(8) . 2_664 ? I3 Ag1 Ag3 63.08(7) . 2_664 ? Ag2 Ag1 Ag3 149.35(10) . 2_664 ? I2 Ag2 I5 111.80(8) . . ? I2 Ag2 I6 113.59(9) . . ? I5 Ag2 I6 113.16(8) . . ? I2 Ag2 I4 113.47(8) . . ? I5 Ag2 I4 99.29(7) . . ? I6 Ag2 I4 104.47(7) . . ? I2 Ag2 Ag1 57.57(7) . . ? I5 Ag2 Ag1 133.93(9) . . ? I6 Ag2 Ag1 111.48(8) . . ? I4 Ag2 Ag1 58.44(6) . . ? I2 Ag2 Ag3 143.21(10) . . ? I5 Ag2 Ag3 57.01(6) . . ? I6 Ag2 Ag3 57.03(6) . . ? I4 Ag2 Ag3 103.20(8) . . ? Ag1 Ag2 Ag3 157.29(10) . . ? I1 Ag3 I5 119.59(10) 3_565 . ? I1 Ag3 I6 109.11(9) 3_565 . ? I5 Ag3 I6 113.81(8) . . ? I1 Ag3 Ag1 57.00(7) 3_565 3_565 ? I5 Ag3 Ag1 111.95(8) . 3_565 ? I6 Ag3 Ag1 131.99(10) . 3_565 ? I1 Ag3 Ag2 147.51(11) 3_565 . ? I5 Ag3 Ag2 57.23(6) . . ? I6 Ag3 Ag2 57.47(6) . . ? Ag1 Ag3 Ag2 155.00(11) 3_565 . ? I1 Ag3 I3 110.75(9) 3_565 3_565 ? I5 Ag3 I3 101.33(8) . 3_565 ? I6 Ag3 I3 100.18(8) . 3_565 ? Ag1 Ag3 I3 56.71(6) 3_565 3_565 ? Ag2 Ag3 I3 101.13(8) . 3_565 ? I1 Ag3 Ag5 114.44(9) 3_565 3_565 ? I5 Ag3 Ag5 53.39(6) . 3_565 ? I6 Ag3 Ag5 134.43(9) . 3_565 ? Ag1 Ag3 Ag5 67.87(8) 3_565 3_565 ? Ag2 Ag3 Ag5 89.76(8) . 3_565 ? I3 Ag3 Ag5 52.27(6) 3_565 3_565 ? I7 Ag4 I6 113.07(8) . . ? I7 Ag4 I4 110.06(8) . . ? I6 Ag4 I4 108.16(8) . . ? I7 Ag4 I3 118.48(9) . 3_565 ? I6 Ag4 I3 106.79(8) . 3_565 ? I4 Ag4 I3 99.06(7) . 3_565 ? I7 Ag4 Ag5 55.45(6) . . ? I6 Ag4 Ag5 105.70(9) . . ? I4 Ag4 Ag5 60.51(7) . . ? I3 Ag4 Ag5 145.83(10) 3_565 . ? I7 Ag5 I5 118.84(9) . 2_664 ? I7 Ag5 I3 118.35(9) . . ? I5 Ag5 I3 108.79(9) 2_664 . ? I7 Ag5 I4 106.04(9) . . ? I5 Ag5 I4 99.85(8) 2_664 . ? I3 Ag5 I4 101.63(8) . . ? I7 Ag5 Ag4 56.27(6) . . ? I5 Ag5 Ag4 142.64(10) 2_664 . ? I3 Ag5 Ag4 103.80(9) . . ? I4 Ag5 Ag4 55.24(7) . . ? I7 Ag5 Ag3 165.22(11) . 2_664 ? I5 Ag5 Ag3 53.91(6) 2_664 2_664 ? I3 Ag5 Ag3 59.85(7) . 2_664 ? I4 Ag5 Ag3 88.42(8) . 2_664 ? Ag4 Ag5 Ag3 138.04(10) . 2_664 ? C5 N1 C1 120(3) . . ? C5 N1 C6 123(2) . . ? C1 N1 C6 117(2) . . ? C18 N2 C14 121(3) . . ? C18 N2 C13 120(3) . . ? C14 N2 C13 119(3) . . ? N1 C1 C2 121(3) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 118(3) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 119(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118(3) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 123(3) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C7 C6 N1 110(2) . . ? C7 C6 H6A 109.8 . . ? N1 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? N1 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C8 114(3) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 118(4) . . ? C9 C8 H8A 107.9 . . ? C7 C8 H8A 107.9 . . ? C9 C8 H8B 108.0 . . ? C7 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 C10 96(5) . . ? C8 C9 H9A 112.6 . . ? C10 C9 H9A 112.7 . . ? C8 C9 H9B 112.5 . . ? C10 C9 H9B 112.5 . . ? H9A C9 H9B 110.1 . . ? C11 C10 C9 99(4) . . ? C11 C10 H10A 112.1 . . ? C9 C10 H10A 112.1 . . ? C11 C10 H10B 111.9 . . ? C9 C10 H10B 112.0 . . ? H10A C10 H10B 109.7 . . ? C10 C11 C12 110(4) . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C13 C12 C11 110(3) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 C13 N2 112(3) . . ? C12 C13 H13A 109.2 . . ? N2 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? N2 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N2 C14 C15 118(3) . . ? N2 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 118(3) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C17 C16 C15 122(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 116(3) . . ? C16 C17 H17 122.0 . . ? C18 C17 H17 122.0 . . ? N2 C18 C17 123(3) . . ? N2 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.362 _refine_diff_density_min -2.061 _refine_diff_density_rms 0.460