# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2257 data_global _audit_creation_method SHELXL-97 _publ_requested_journal 'Dalton' _publ_contact_author_name 'Andreas A. Danopoulos' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield SO17 1BJ United Kingdom ; _publ_contact_author_email ad1@soton.ac.uk _publ_contact_author_fax '+44 (23) 80 59 68 05' _publ_contact_author_phone '+44 (23) 80 59 67 42' _publ_section_title ; N-Functionalised heterocyclic carbene complexes of silver ; loop_ _publ_author_name _publ_author_address 'Kleinhenz, Sven' ; Department of Chemistry University of Southampton Highfield SO17 1BJ United Kingdom ; 'Tulloch, Arran A. D.' ; Department of Chemistry University of Southampton Highfield SO17 1BJ United Kingdom ; 'Danopoulos, Andreas A.' ; Department of Chemistry University of Southampton Highfield SO17 1BJ United Kingdom ; 'Scott Winston' ; Department of Chemistry University of Southampton Highfield SO17 1BJ United Kingdom ; 'Graham Eastham' ; Ineos Acrylics PO Box 90 Middlesbrough TS90 8JE United Kingdom ; data_7b _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-mesityl-1-(2-picolyl)-imidazol-2-ylidene silver bromide ; _chemical_name_common 00skl024 _chemical_melting_point ? _chemical_formula_moiety 'C18 H19 Ag1 Br1 N3' _chemical_formula_sum 'C18 H19 Ag Br N3' _chemical_formula_weight 465.14 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' 'Br' 'Br' -0.2901 2.4595 '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 'P 2/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 9.7752(13) _cell_length_b 16.867(3) _cell_length_c 10.909(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.115(12) _cell_angle_gamma 90.00 _cell_volume 1791.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 55198 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description prism _exptl_crystal_colour clorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 3.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; SORTAV - multi-scan from symmetry-related measurements (Blessing, 1995-1997) ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 13805 _diffrn_reflns_av_R_equivalents 0.2641 _diffrn_reflns_av_sigmaI/netI 0.1859 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.54 _reflns_number_total 3686 _reflns_number_gt 1916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.017(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3686 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2842 _refine_ls_R_factor_gt 0.2056 _refine_ls_wR_factor_ref 0.5351 _refine_ls_wR_factor_gt 0.4992 _refine_ls_goodness_of_fit_ref 1.586 _refine_ls_restrained_S_all 1.586 _refine_ls_shift/su_max 0.258 _refine_ls_shift/su_mean 0.060 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 0.4384(2) 0.03910(12) 0.3642(3) 0.1080(14) Uani 1 1 d . . . Br2 Br 0.5066(4) 0.0977(2) 0.6173(3) 0.1106(15) Uani 1 1 d . . . N3 N 0.4032(15) 0.1856(10) 0.1979(14) 0.059(4) Uani 1 1 d . . . N2 N 0.2461(18) 0.1812(11) 0.3164(16) 0.070(5) Uani 1 1 d . . . N1 N -0.0650(15) 0.1158(11) 0.4427(16) 0.065(4) Uani 1 1 d . . . C1 C 0.3622(16) 0.1467(10) 0.2972(18) 0.055(5) Uani 1 1 d . . . C9 C 0.317(2) 0.2531(13) 0.170(2) 0.077(6) Uani 1 1 d . . . H9 H 0.3318 0.2944 0.1166 0.092 Uiso 1 1 calc R . . C5 C 0.047(2) 0.0467(13) 0.293(2) 0.070(6) Uani 1 1 d . . . H5 H 0.1269 0.0365 0.2552 0.084 Uiso 1 1 calc R . . C7 C 0.160(2) 0.1551(14) 0.421(2) 0.080(7) Uani 1 1 d . . . H7A H 0.2189 0.1257 0.4815 0.095 Uiso 1 1 calc R . . H7B H 0.1282 0.2020 0.4613 0.095 Uiso 1 1 calc R . . C13 C 0.759(3) 0.1359(18) 0.022(3) 0.094(8) Uiso 1 1 d . . . C6 C 0.0445(17) 0.1069(10) 0.3807(15) 0.046(4) Uiso 1 1 d . . . C11 C 0.514(3) 0.1259(12) 0.031(3) 0.085(8) Uani 1 1 d . . . C4 C -0.074(2) 0.0007(13) 0.262(2) 0.068(5) Uiso 1 1 d . . . H4 H -0.0794 -0.0362 0.1987 0.081 Uiso 1 1 calc R . . C2 C -0.179(4) 0.0713(15) 0.410(3) 0.121(14) Uani 1 1 d . . . H2 H -0.2591 0.0827 0.4471 0.145 Uiso 1 1 calc R . . C12 C 0.648(3) 0.1158(13) -0.0181(17) 0.075(7) Uani 1 1 d . . . H12 H 0.6445 0.0891 -0.0929 0.090 Uiso 1 1 calc R . . C15 C 0.648(2) 0.2030(14) 0.191(2) 0.070(6) Uani 1 1 d . . . C14 C 0.771(2) 0.1809(18) 0.135(3) 0.096(8) Uani 1 1 d . . . H14 H 0.8571 0.1955 0.1715 0.115 Uiso 1 1 calc R . . C10 C 0.532(2) 0.1734(11) 0.1470(18) 0.060(5) Uani 1 1 d . . . C8 C 0.215(2) 0.2444(13) 0.236(2) 0.065(5) Uani 1 1 d . . . H8 H 0.1348 0.2746 0.2300 0.078 Uiso 1 1 calc R . . C3 C -0.181(2) 0.0134(19) 0.331(3) 0.096(10) Uani 1 1 d . . . H3 H -0.2580 -0.0195 0.3203 0.116 Uiso 1 1 calc R . . C17 C 0.660(3) 0.2498(17) 0.296(3) 0.095(8) Uani 1 1 d . . . H17A H 0.7553 0.2623 0.3164 0.143 Uiso 1 1 calc R . . H17B H 0.6250 0.2218 0.3625 0.143 Uiso 1 1 calc R . . H17C H 0.6092 0.2980 0.2802 0.143 Uiso 1 1 calc R . . C18 C 0.891(3) 0.121(2) -0.047(4) 0.149(15) Uani 1 1 d . . . H18A H 0.9701 0.1422 0.0007 0.224 Uiso 1 1 calc R . . H18B H 0.8812 0.1474 -0.1260 0.224 Uiso 1 1 calc R . . H18C H 0.9032 0.0654 -0.0594 0.224 Uiso 1 1 calc R . . C16 C 0.373(3) 0.0949(18) -0.025(3) 0.106(9) Uani 1 1 d . . . H16A H 0.3035 0.1099 0.0278 0.159 Uiso 1 1 calc R . . H16B H 0.3759 0.0382 -0.0310 0.159 Uiso 1 1 calc R . . H16C H 0.3520 0.1174 -0.1049 0.159 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 0.0949(18) 0.0763(16) 0.160(3) 0.0318(13) 0.0539(15) 0.0097(10) Br2 0.123(2) 0.126(3) 0.087(2) -0.0206(16) 0.0344(16) -0.0451(19) N3 0.058(9) 0.067(10) 0.054(9) 0.011(8) 0.024(7) 0.010(7) N2 0.077(11) 0.075(11) 0.062(10) -0.023(9) 0.035(8) -0.037(10) N1 0.047(8) 0.078(11) 0.074(11) -0.008(9) 0.030(7) -0.014(8) C1 0.036(9) 0.050(10) 0.079(13) -0.016(9) -0.006(9) 0.010(8) C9 0.058(12) 0.054(12) 0.113(18) -0.005(12) -0.016(12) 0.004(10) C5 0.069(12) 0.080(14) 0.064(13) -0.012(10) 0.027(10) -0.004(10) C7 0.084(14) 0.083(15) 0.080(15) -0.032(12) 0.058(12) -0.022(12) C11 0.106(18) 0.040(11) 0.10(2) 0.036(12) -0.016(15) 0.006(11) C2 0.18(3) 0.053(13) 0.15(3) 0.008(16) 0.13(3) 0.000(17) C12 0.13(2) 0.071(13) 0.029(10) 0.015(9) 0.022(11) 0.045(13) C15 0.084(15) 0.070(13) 0.061(13) -0.001(11) 0.039(11) 0.005(12) C14 0.059(12) 0.11(2) 0.12(2) 0.018(17) 0.031(13) 0.021(12) C10 0.086(14) 0.046(10) 0.055(11) 0.022(9) 0.043(11) 0.017(10) C8 0.049(11) 0.064(13) 0.082(15) -0.011(11) 0.008(10) -0.013(9) C3 0.052(12) 0.11(2) 0.12(2) 0.07(2) 0.000(13) -0.023(13) C17 0.074(15) 0.097(19) 0.12(2) -0.003(16) 0.035(14) 0.015(13) C18 0.11(2) 0.13(3) 0.22(5) 0.04(3) 0.05(3) 0.05(2) C16 0.14(2) 0.088(19) 0.090(19) 0.014(15) -0.014(17) 0.005(17) _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 C1 2.070(18) . ? Ag1 Br2 2.373(4) 3_656 ? Ag1 Br2 2.952(4) . ? Ag1 Ag1 3.367(6) 3_656 ? Br2 Ag1 2.373(4) 3_656 ? N3 C9 1.43(3) . ? N3 C1 1.36(2) . ? N3 C10 1.44(2) . ? N2 C1 1.31(2) . ? N2 C8 1.40(3) . ? N2 C7 1.54(2) . ? N1 C6 1.32(2) . ? N1 C2 1.36(4) . ? C9 C8 1.29(3) . ? C5 C6 1.40(3) . ? C5 C4 1.43(3) . ? C7 C6 1.43(3) . ? C13 C12 1.19(4) . ? C13 C14 1.45(4) . ? C13 C18 1.57(4) . ? C11 C12 1.46(4) . ? C11 C10 1.50(4) . ? C11 C16 1.55(4) . ? C4 C3 1.35(4) . ? C2 C3 1.31(4) . ? C15 C10 1.29(3) . ? C15 C17 1.38(3) . ? C15 C14 1.45(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 C1 Ag1 Br2 162.5(5) . 3_656 ? C1 Ag1 Br2 94.6(5) . . ? Br2 Ag1 Br2 102.40(13) 3_656 . ? C1 Ag1 Ag1 138.0(5) . 3_656 ? Br2 Ag1 Ag1 58.91(10) 3_656 3_656 ? Br2 Ag1 Ag1 43.49(11) . 3_656 ? Ag1 Br2 Ag1 77.60(13) 3_656 . ? C9 N3 C1 110.0(16) . . ? C9 N3 C10 123.6(17) . . ? C1 N3 C10 124.7(15) . . ? C1 N2 C8 112.5(16) . . ? C1 N2 C7 122(2) . . ? C8 N2 C7 125.6(19) . . ? C6 N1 C2 119.0(18) . . ? N2 C1 N3 103.5(16) . . ? N2 C1 Ag1 128.6(16) . . ? N3 C1 Ag1 125.7(12) . . ? C8 C9 N3 105(2) . . ? C6 C5 C4 119.2(18) . . ? C6 C7 N2 113.7(17) . . ? C12 C13 C14 118(3) . . ? C12 C13 C18 123(3) . . ? C14 C13 C18 119(3) . . ? N1 C6 C5 119.8(16) . . ? N1 C6 C7 115.6(15) . . ? C5 C6 C7 124.1(17) . . ? C12 C11 C10 109(2) . . ? C12 C11 C16 128(3) . . ? C10 C11 C16 123(2) . . ? C3 C4 C5 117(2) . . ? N1 C2 C3 123(2) . . ? C13 C12 C11 131(2) . . ? C10 C15 C17 123(2) . . ? C10 C15 C14 118(2) . . ? C17 C15 C14 119(2) . . ? C15 C14 C13 119(3) . . ? C15 C10 N3 124.7(19) . . ? C15 C10 C11 124.0(18) . . ? N3 C10 C11 111(2) . . ? C9 C8 N2 107.3(19) . . ? C4 C3 C2 121(2) . . ? 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 C1 Ag1 Br2 Ag1 176.2(5) . . . 3_656 ? Br2 Ag1 Br2 Ag1 0.0 3_656 . . 3_656 ? C8 N2 C1 N3 -3(2) . . . . ? C7 N2 C1 N3 179.2(16) . . . . ? C8 N2 C1 Ag1 -166.8(14) . . . . ? C7 N2 C1 Ag1 16(3) . . . . ? C9 N3 C1 N2 9(2) . . . . ? C10 N3 C1 N2 174.6(18) . . . . ? C9 N3 C1 Ag1 173.2(13) . . . . ? C10 N3 C1 Ag1 -21(3) . . . . ? Br2 Ag1 C1 N2 94(2) 3_656 . . . ? Br2 Ag1 C1 N2 -73.5(16) . . . . ? Ag1 Ag1 C1 N2 -69.6(18) 3_656 . . . ? Br2 Ag1 C1 N3 -66(2) 3_656 . . . ? Br2 Ag1 C1 N3 126.3(15) . . . . ? Ag1 Ag1 C1 N3 130.2(14) 3_656 . . . ? C1 N3 C9 C8 -12(2) . . . . ? C10 N3 C9 C8 -178(2) . . . . ? C1 N2 C7 C6 -102(2) . . . . ? C8 N2 C7 C6 81(2) . . . . ? C2 N1 C6 C5 -7(3) . . . . ? C2 N1 C6 C7 -179(2) . . . . ? C4 C5 C6 N1 7(3) . . . . ? C4 C5 C6 C7 178(2) . . . . ? N2 C7 C6 N1 -146.8(18) . . . . ? N2 C7 C6 C5 41(3) . . . . ? C6 C5 C4 C3 -7(3) . . . . ? C6 N1 C2 C3 8(4) . . . . ? C14 C13 C12 C11 -3(4) . . . . ? C18 C13 C12 C11 -178(2) . . . . ? C10 C11 C12 C13 3(3) . . . . ? C16 C11 C12 C13 -177(3) . . . . ? C10 C15 C14 C13 9(4) . . . . ? C17 C15 C14 C13 -176(3) . . . . ? C12 C13 C14 C15 -3(4) . . . . ? C18 C13 C14 C15 172(3) . . . . ? C17 C15 C10 N3 1(3) . . . . ? C14 C15 C10 N3 175.7(19) . . . . ? C17 C15 C10 C11 177(2) . . . . ? C14 C15 C10 C11 -8(3) . . . . ? C9 N3 C10 C15 85(3) . . . . ? C1 N3 C10 C15 -79(3) . . . . ? C9 N3 C10 C11 -92(2) . . . . ? C1 N3 C10 C11 104(2) . . . . ? C12 C11 C10 C15 3(3) . . . . ? C16 C11 C10 C15 -176(2) . . . . ? C12 C11 C10 N3 179.4(14) . . . . ? C16 C11 C10 N3 0(3) . . . . ? N3 C9 C8 N2 9(2) . . . . ? C1 N2 C8 C9 -4(2) . . . . ? C7 N2 C8 C9 173.2(19) . . . . ? C5 C4 C3 C2 8(4) . . . . ? N1 C2 C3 C4 -9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 5.162 _refine_diff_density_min -1.319 _refine_diff_density_rms 0.284 data_7c _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-(2,6-di-isopropylphenyl)-1-(2-picolyl)-imidazol-2-ylidene silver bromide ; _chemical_name_common 00skl020 _chemical_melting_point ? _chemical_formula_moiety 'C42 H50 Ag2 Br2 N6' _chemical_formula_sum 'C42 H50 Ag2 Br2 N6' _chemical_formula_weight 1014.44 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 'P 21 n b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z' 'x+1/2, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' _cell_length_a 12.77370(10) _cell_length_b 16.55300(10) _cell_length_c 20.1344(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4257.28(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30414 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 2.833 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7096 _exptl_absorpt_correction_T_max 0.8713 _exptl_absorpt_process_details ; SORTAV - multi-scan from symmetry-related measurements (R.H. Blessing, 1995-1997 ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 37682 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.38 _reflns_number_total 8211 _reflns_number_gt 7205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0580P)^2^+1.2641P] 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 0.00080(12) _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 0.016(8) _refine_ls_number_reflns 8211 _refine_ls_number_parameters 470 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.56404(3) 0.48834(2) 0.259989(17) 0.02309(11) Uani 1 1 d . . . Ag2 Ag 0.09619(4) 0.62307(2) 0.20967(2) 0.03468(13) Uani 1 1 d . . . Br1 Br 0.00591(5) 0.64870(3) 0.31728(3) 0.04151(17) Uani 1 1 d . . . Br2 Br 0.13602(6) 0.64932(4) 0.08957(3) 0.05024(19) Uani 1 1 d . . . N5 N 0.5843(3) 0.4664(2) 0.10623(19) 0.0207(9) Uani 1 1 d . . . N6 N 0.5243(3) 0.4858(2) 0.4109(2) 0.0229(9) Uani 1 1 d . . . N7 N 0.6836(3) 0.5177(2) 0.3922(2) 0.0205(9) Uani 1 1 d . . . N8 N 0.4333(3) 0.5082(2) 0.1328(2) 0.0257(10) Uani 1 1 d . . . N9 N 0.1773(4) 0.4879(2) 0.2134(2) 0.0267(10) Uani 1 1 d . . . N10 N 0.8955(3) 0.4318(3) 0.4092(2) 0.0315(11) Uani 1 1 d . . . C11 C 0.5701(5) 0.4977(3) 0.4726(2) 0.0261(11) Uani 1 1 d . . . H11A H 0.5371 0.4931 0.5148 0.031 Uiso 1 1 calc R . . C12 C 0.7657(4) 0.5109(3) 0.1054(3) 0.0244(12) Uani 1 1 d . . . C13 C 0.4161(4) 0.4634(3) 0.4001(3) 0.0242(11) Uani 1 1 d . . . C14 C 0.2109(5) 0.3276(4) 0.1836(3) 0.0457(16) Uani 1 1 d . . . H14A H 0.2226 0.2723 0.1733 0.055 Uiso 1 1 calc R . . C15 C 0.6955(4) 0.4467(3) 0.1092(2) 0.0222(11) Uani 1 1 d . . . C16 C 0.3420(4) 0.5319(3) 0.1716(3) 0.0305(12) Uani 1 1 d . . . H16A H 0.3048 0.5757 0.1478 0.037 Uiso 1 1 calc R . . H16B H 0.3660 0.5539 0.2147 0.037 Uiso 1 1 calc R . . C17 C 0.7314(5) 0.5978(3) 0.1031(3) 0.0331(13) Uani 1 1 d . . . H17A H 0.6540 0.5980 0.0957 0.040 Uiso 1 1 calc R . . C18 C 0.7837(4) 0.5308(3) 0.3602(3) 0.0266(12) Uani 1 1 d . . . H18A H 0.8249 0.5704 0.3861 0.032 Uiso 1 1 calc R . . H18B H 0.7722 0.5534 0.3152 0.032 Uiso 1 1 calc R . . C19 C 0.2668(4) 0.4646(3) 0.1845(3) 0.0254(11) Uani 1 1 d . . . C20 C 0.5279(4) 0.4866(3) 0.1598(2) 0.0216(11) Uani 1 1 d . . . C21 C 0.5301(4) 0.4748(3) 0.0479(3) 0.0293(12) Uani 1 1 d . . . H21A H 0.5552 0.4636 0.0045 0.035 Uiso 1 1 calc R . . C22 C 0.4349(4) 0.5020(3) 0.0643(3) 0.0314(13) Uani 1 1 d . . . H22A H 0.3793 0.5145 0.0347 0.038 Uiso 1 1 calc R . . C23 C 0.3433(4) 0.5248(3) 0.3923(3) 0.0247(11) Uani 1 1 d . . . C24 C 0.2852(5) 0.3845(3) 0.1686(3) 0.0399(15) Uani 1 1 d . . . H24A H 0.3487 0.3692 0.1475 0.048 Uiso 1 1 calc R . . C25 C 0.6641(6) 0.2301(4) 0.0700(3) 0.0551(18) Uani 1 1 d . . . H25A H 0.6590 0.2530 0.0253 0.083 Uiso 1 1 calc R . . H25B H 0.6101 0.1887 0.0758 0.083 Uiso 1 1 calc R . . H25C H 0.7334 0.2057 0.0761 0.083 Uiso 1 1 calc R . . C26 C 0.9052(4) 0.4128(4) 0.1087(3) 0.0358(13) Uani 1 1 d . . . H26A H 0.9779 0.4007 0.1075 0.043 Uiso 1 1 calc R . . C27 C 0.7259(4) 0.3659(3) 0.1137(3) 0.0254(11) Uani 1 1 d . . . C28 C 0.3913(4) 0.3814(3) 0.3976(3) 0.0301(12) Uani 1 1 d . . . C29 C 0.6483(5) 0.2967(3) 0.1212(3) 0.0321(12) Uani 1 1 d . . . H29A H 0.5763 0.3192 0.1150 0.039 Uiso 1 1 calc R . . C30 C 0.1060(4) 0.4322(3) 0.2275(3) 0.0318(12) Uani 1 1 d . . . H30A H 0.0429 0.4492 0.2481 0.038 Uiso 1 1 calc R . . C31 C 0.6709(4) 0.5170(3) 0.4608(3) 0.0263(12) Uani 1 1 d . . . H31A H 0.7232 0.5281 0.4931 0.032 Uiso 1 1 calc R . . C32 C 0.1184(5) 0.3515(3) 0.2139(3) 0.0374(14) Uani 1 1 d . . . H32A H 0.0656 0.3134 0.2249 0.045 Uiso 1 1 calc R . . C33 C 0.8435(4) 0.4530(3) 0.3548(2) 0.0224(11) Uani 1 1 d . . . C34 C 0.8330(4) 0.3502(3) 0.1133(3) 0.0314(13) Uani 1 1 d . . . H34A H 0.8570 0.2960 0.1162 0.038 Uiso 1 1 calc R . . C35 C 0.2868(5) 0.3616(3) 0.3856(3) 0.0357(14) Uani 1 1 d . . . H35A H 0.2663 0.3064 0.3844 0.043 Uiso 1 1 calc R . . C36 C 0.4725(5) 0.3147(3) 0.4069(3) 0.0425(15) Uani 1 1 d . . . H36A H 0.5435 0.3402 0.4072 0.051 Uiso 1 1 calc R . . C37 C 0.8734(5) 0.4912(3) 0.1058(3) 0.0341(13) Uani 1 1 d . . . H37A H 0.9241 0.5331 0.1041 0.041 Uiso 1 1 calc R . . C38 C 0.2130(5) 0.4211(4) 0.3754(3) 0.0370(14) Uani 1 1 d . . . H38A H 0.1426 0.4064 0.3662 0.044 Uiso 1 1 calc R . . C39 C 0.3716(5) 0.6129(3) 0.3974(3) 0.0333(13) Uani 1 1 d . . . H39A H 0.4408 0.6163 0.4205 0.040 Uiso 1 1 calc R . . C40 C 0.2397(5) 0.5010(3) 0.3782(3) 0.0326(13) Uani 1 1 d . . . H40A H 0.1877 0.5410 0.3706 0.039 Uiso 1 1 calc R . . C41 C 0.2925(5) 0.6614(4) 0.4389(3) 0.0425(15) Uani 1 1 d . . . H41A H 0.2847 0.6361 0.4827 0.064 Uiso 1 1 calc R . . H41B H 0.2247 0.6620 0.4162 0.064 Uiso 1 1 calc R . . H41C H 0.3178 0.7169 0.4444 0.064 Uiso 1 1 calc R . . C42 C 0.7515(6) 0.6393(4) 0.1700(3) 0.0457(16) Uani 1 1 d . . . H42A H 0.7175 0.6086 0.2055 0.069 Uiso 1 1 calc R . . H42B H 0.7229 0.6942 0.1688 0.069 Uiso 1 1 calc R . . H42C H 0.8271 0.6418 0.1782 0.069 Uiso 1 1 calc R . . C43 C 0.7810(6) 0.6455(4) 0.0459(3) 0.0507(17) Uani 1 1 d . . . H43A H 0.7662 0.6182 0.0037 0.076 Uiso 1 1 calc R . . H43B H 0.8569 0.6487 0.0525 0.076 Uiso 1 1 calc R . . H43C H 0.7516 0.7002 0.0449 0.076 Uiso 1 1 calc R . . C44 C 0.3845(5) 0.6523(3) 0.3295(3) 0.0398(15) Uani 1 1 d . . . H44A H 0.4351 0.6213 0.3032 0.060 Uiso 1 1 calc R . . H44B H 0.4099 0.7077 0.3350 0.060 Uiso 1 1 calc R . . H44C H 0.3169 0.6530 0.3065 0.060 Uiso 1 1 calc R . . C45 C 0.4564(7) 0.2722(5) 0.4727(4) 0.084(3) Uani 1 1 d . . . H45A H 0.5094 0.2299 0.4779 0.126 Uiso 1 1 calc R . . H45B H 0.3865 0.2479 0.4737 0.126 Uiso 1 1 calc R . . H45C H 0.4629 0.3113 0.5090 0.126 Uiso 1 1 calc R . . C46 C 0.9400(4) 0.3078(3) 0.3550(3) 0.0358(14) Uani 1 1 d . . . H46A H 0.9753 0.2573 0.3568 0.043 Uiso 1 1 calc R . . C47 C 0.5940(4) 0.4977(3) 0.3609(3) 0.0219(11) Uani 1 1 d . . . C48 C 0.9426(5) 0.3588(3) 0.4079(3) 0.0350(14) Uani 1 1 d . . . H48A H 0.9797 0.3420 0.4464 0.042 Uiso 1 1 calc R . . C49 C 0.4685(8) 0.2546(5) 0.3500(5) 0.078(3) Uani 1 1 d . . . H49A H 0.5216 0.2127 0.3570 0.117 Uiso 1 1 calc R . . H49B H 0.4823 0.2826 0.3081 0.117 Uiso 1 1 calc R . . H49C H 0.3990 0.2296 0.3483 0.117 Uiso 1 1 calc R . . C50 C 0.8862(5) 0.3300(4) 0.2991(3) 0.0381(14) Uani 1 1 d . . . H50A H 0.8832 0.2952 0.2616 0.046 Uiso 1 1 calc R . . C51 C 0.6547(7) 0.2618(5) 0.1907(4) 0.061(2) Uani 1 1 d . . . H51A H 0.6440 0.3050 0.2233 0.092 Uiso 1 1 calc R . . H51B H 0.7237 0.2374 0.1974 0.092 Uiso 1 1 calc R . . H51C H 0.6004 0.2205 0.1962 0.092 Uiso 1 1 calc R . . C52 C 0.8356(4) 0.4052(3) 0.2984(3) 0.0308(12) Uani 1 1 d . . . H52A H 0.7972 0.4228 0.2607 0.037 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 0.02167(19) 0.02926(19) 0.01833(19) -0.00057(14) 0.00209(18) -0.00005(18) Ag2 0.0314(2) 0.0314(2) 0.0412(3) -0.00301(18) 0.0034(2) 0.00170(19) Br1 0.0358(3) 0.0380(3) 0.0507(4) 0.0031(3) 0.0136(3) 0.0010(3) Br2 0.0552(4) 0.0506(4) 0.0449(4) -0.0008(3) -0.0047(3) 0.0016(3) N5 0.018(2) 0.0252(19) 0.018(2) -0.0018(16) 0.0019(18) -0.0022(17) N6 0.021(2) 0.025(2) 0.022(2) 0.0003(16) -0.0008(19) 0.0014(17) N7 0.019(2) 0.026(2) 0.016(2) -0.0038(17) 0.0014(19) 0.0050(17) N8 0.022(2) 0.030(2) 0.026(3) -0.0083(18) -0.001(2) -0.0019(18) N9 0.026(2) 0.025(2) 0.029(3) 0.0023(18) 0.004(2) 0.0054(18) N10 0.023(2) 0.037(2) 0.035(3) 0.003(2) 0.003(2) 0.004(2) C11 0.029(3) 0.034(3) 0.016(2) -0.0018(19) -0.002(3) 0.005(2) C12 0.023(3) 0.031(3) 0.019(3) -0.002(2) 0.003(2) 0.000(2) C13 0.019(2) 0.030(3) 0.023(3) 0.002(2) 0.004(2) 0.002(2) C14 0.043(4) 0.027(3) 0.067(5) -0.005(3) 0.011(3) 0.003(3) C15 0.023(3) 0.030(3) 0.014(2) -0.003(2) 0.000(2) -0.003(2) C16 0.027(3) 0.026(3) 0.039(3) -0.008(2) 0.002(3) 0.003(2) C17 0.036(3) 0.032(3) 0.032(3) 0.003(2) 0.006(3) -0.005(3) C18 0.018(3) 0.033(3) 0.029(3) 0.004(2) 0.001(2) 0.001(2) C19 0.019(2) 0.031(3) 0.026(3) -0.004(2) -0.002(2) 0.005(2) C20 0.022(3) 0.027(2) 0.016(3) 0.0008(19) -0.002(2) -0.004(2) C21 0.031(3) 0.037(3) 0.020(3) -0.003(2) -0.003(2) -0.004(2) C22 0.023(3) 0.041(3) 0.030(3) 0.004(2) -0.010(3) 0.002(2) C23 0.024(3) 0.031(3) 0.019(3) -0.003(2) 0.001(2) 0.001(2) C24 0.032(3) 0.033(3) 0.055(4) -0.005(3) 0.005(3) 0.003(3) C25 0.074(5) 0.044(4) 0.047(4) -0.005(3) -0.002(4) -0.010(3) C26 0.022(3) 0.055(4) 0.031(3) -0.001(3) 0.002(2) 0.011(3) C27 0.026(3) 0.031(3) 0.019(3) -0.001(2) 0.001(2) 0.003(2) C28 0.032(3) 0.031(3) 0.027(3) 0.003(2) 0.012(3) -0.001(2) C29 0.035(3) 0.026(3) 0.035(3) 0.002(2) -0.007(3) 0.000(2) C30 0.024(3) 0.037(3) 0.035(3) 0.007(2) 0.004(2) 0.002(3) C31 0.026(3) 0.032(3) 0.021(3) -0.006(2) -0.003(2) 0.003(2) C32 0.034(4) 0.039(3) 0.039(3) -0.002(2) 0.005(3) -0.006(3) C33 0.016(2) 0.025(2) 0.026(3) 0.001(2) 0.005(2) -0.005(2) C34 0.029(3) 0.036(3) 0.030(3) -0.003(2) 0.000(3) 0.008(2) C35 0.038(3) 0.034(3) 0.035(3) -0.005(2) 0.007(3) -0.010(3) C36 0.041(3) 0.034(3) 0.053(4) 0.007(3) 0.012(3) 0.002(3) C37 0.027(3) 0.047(3) 0.028(3) -0.003(3) 0.004(3) -0.006(3) C38 0.028(3) 0.053(4) 0.030(3) -0.007(3) -0.001(3) -0.008(3) C39 0.033(3) 0.038(3) 0.029(3) -0.003(2) 0.000(3) 0.005(3) C40 0.028(3) 0.048(3) 0.022(3) -0.001(2) -0.001(3) 0.004(3) C41 0.057(4) 0.040(3) 0.031(3) -0.005(2) 0.000(3) 0.018(3) C42 0.057(4) 0.036(3) 0.044(4) -0.009(3) -0.002(3) -0.007(3) C43 0.065(5) 0.046(4) 0.042(4) 0.011(3) 0.014(4) -0.001(3) C44 0.047(4) 0.035(3) 0.038(4) -0.005(3) 0.012(3) 0.005(3) C45 0.084(6) 0.079(6) 0.089(6) 0.042(5) 0.024(5) 0.030(5) C46 0.023(3) 0.029(3) 0.055(4) 0.001(3) 0.014(3) 0.005(2) C47 0.019(3) 0.023(2) 0.024(3) 0.0024(18) 0.002(2) 0.005(2) C48 0.028(3) 0.041(3) 0.036(4) 0.008(3) 0.004(3) 0.008(2) C49 0.075(5) 0.056(4) 0.103(7) -0.020(4) 0.022(5) 0.017(4) C50 0.029(3) 0.038(3) 0.047(4) -0.016(3) 0.010(3) -0.004(3) C51 0.070(5) 0.067(5) 0.046(4) 0.016(3) 0.004(4) -0.037(4) C52 0.024(3) 0.038(3) 0.030(3) -0.006(2) 0.005(2) -0.001(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 C20 2.069(5) . ? Ag1 C47 2.074(5) . ? Ag2 N9 2.467(4) . ? Ag2 Br1 2.4909(7) . ? Ag2 Br2 2.5090(8) . ? N5 C20 1.339(6) . ? N5 C21 1.370(7) . ? N5 C15 1.459(6) . ? N6 C47 1.358(7) . ? N6 C11 1.388(7) . ? N6 C13 1.447(7) . ? N7 C47 1.348(7) . ? N7 C31 1.390(7) . ? N7 C18 1.449(7) . ? N8 C20 1.373(7) . ? N8 C22 1.383(8) . ? N8 C16 1.457(7) . ? N9 C30 1.326(7) . ? N9 C19 1.340(7) . ? N10 C33 1.326(7) . ? N10 C48 1.350(7) . ? C11 C31 1.348(8) . ? C11 H11A 0.9500 . ? C12 C15 1.392(7) . ? C12 C37 1.415(8) . ? C12 C17 1.505(7) . ? C13 C23 1.387(7) . ? C13 C28 1.395(8) . ? C14 C24 1.372(9) . ? C14 C32 1.387(9) . ? C14 H14A 0.9500 . ? C15 C27 1.395(7) . ? C16 C19 1.493(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C42 1.533(8) . ? C17 C43 1.534(8) . ? C17 H17A 1.0000 . ? C18 C33 1.502(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.383(8) . ? C21 C22 1.338(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C40 1.410(8) . ? C23 C39 1.506(7) . ? C24 H24A 0.9500 . ? C25 C29 1.522(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C37 1.360(8) . ? C26 C34 1.392(8) . ? C26 H26A 0.9500 . ? C27 C34 1.393(8) . ? C27 C29 1.522(7) . ? C28 C35 1.395(9) . ? C28 C36 1.526(8) . ? C29 C51 1.516(9) . ? C29 H29A 1.0000 . ? C30 C32 1.374(8) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C52 1.388(7) . ? C34 H34A 0.9500 . ? C35 C38 1.379(9) . ? C35 H35A 0.9500 . ? C36 C45 1.514(9) . ? C36 C49 1.518(10) . ? C36 H36A 1.0000 . ? C37 H37A 0.9500 . ? C38 C40 1.367(8) . ? C38 H38A 0.9500 . ? C39 C44 1.524(8) . ? C39 C41 1.537(8) . ? C39 H39A 1.0000 . ? C40 H40A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.360(8) . ? C46 C50 1.369(9) . ? C46 H46A 0.9500 . ? C48 H48A 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.403(8) . ? C50 H50A 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 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 C20 Ag1 C47 175.90(19) . . ? N9 Ag2 Br1 108.82(11) . . ? N9 Ag2 Br2 95.80(11) . . ? Br1 Ag2 Br2 154.52(3) . . ? C20 N5 C21 113.2(4) . . ? C20 N5 C15 123.1(4) . . ? C21 N5 C15 123.4(4) . . ? C47 N6 C11 111.5(4) . . ? C47 N6 C13 123.5(4) . . ? C11 N6 C13 125.0(4) . . ? C47 N7 C31 111.3(4) . . ? C47 N7 C18 125.3(4) . . ? C31 N7 C18 123.1(4) . . ? C20 N8 C22 111.2(5) . . ? C20 N8 C16 124.2(5) . . ? C22 N8 C16 124.5(5) . . ? C30 N9 C19 118.6(4) . . ? C30 N9 Ag2 110.4(3) . . ? C19 N9 Ag2 127.3(3) . . ? C33 N10 C48 116.3(5) . . ? C31 C11 N6 106.2(4) . . ? C31 C11 H11A 126.9 . . ? N6 C11 H11A 126.9 . . ? C15 C12 C37 116.8(5) . . ? C15 C12 C17 122.9(5) . . ? C37 C12 C17 120.3(5) . . ? C23 C13 C28 123.9(5) . . ? C23 C13 N6 117.9(4) . . ? C28 C13 N6 118.2(5) . . ? C24 C14 C32 119.3(5) . . ? C24 C14 H14A 120.3 . . ? C32 C14 H14A 120.3 . . ? C12 C15 C27 123.8(5) . . ? C12 C15 N5 117.0(4) . . ? C27 C15 N5 119.2(4) . . ? N8 C16 C19 114.0(4) . . ? N8 C16 H16A 108.7 . . ? C19 C16 H16A 108.7 . . ? N8 C16 H16B 108.7 . . ? C19 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C12 C17 C42 110.7(5) . . ? C12 C17 C43 113.3(5) . . ? C42 C17 C43 111.0(5) . . ? C12 C17 H17A 107.2 . . ? C42 C17 H17A 107.2 . . ? C43 C17 H17A 107.2 . . ? N7 C18 C33 110.6(4) . . ? N7 C18 H18A 109.5 . . ? C33 C18 H18A 109.5 . . ? N7 C18 H18B 109.5 . . ? C33 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N9 C19 C24 121.4(5) . . ? N9 C19 C16 114.2(4) . . ? C24 C19 C16 124.4(5) . . ? N5 C20 N8 102.7(4) . . ? N5 C20 Ag1 132.0(4) . . ? N8 C20 Ag1 125.4(4) . . ? C22 C21 N5 106.4(5) . . ? C22 C21 H21A 126.8 . . ? N5 C21 H21A 126.8 . . ? C21 C22 N8 106.5(5) . . ? C21 C22 H22A 126.7 . . ? N8 C22 H22A 126.7 . . ? C13 C23 C40 116.5(5) . . ? C13 C23 C39 122.8(5) . . ? C40 C23 C39 120.7(5) . . ? C14 C24 C19 119.3(6) . . ? C14 C24 H24A 120.3 . . ? C19 C24 H24A 120.3 . . ? C29 C25 H25A 109.5 . . ? C29 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C29 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C37 C26 C34 121.0(5) . . ? C37 C26 H26A 119.5 . . ? C34 C26 H26A 119.5 . . ? C34 C27 C15 116.9(5) . . ? C34 C27 C29 119.9(5) . . ? C15 C27 C29 123.2(5) . . ? C13 C28 C35 116.9(5) . . ? C13 C28 C36 123.0(5) . . ? C35 C28 C36 120.1(5) . . ? C51 C29 C27 110.0(5) . . ? C51 C29 C25 110.0(5) . . ? C27 C29 C25 113.1(5) . . ? C51 C29 H29A 107.8 . . ? C27 C29 H29A 107.8 . . ? C25 C29 H29A 107.8 . . ? N9 C30 C32 123.7(5) . . ? N9 C30 H30A 118.2 . . ? C32 C30 H30A 118.2 . . ? C11 C31 N7 106.8(5) . . ? C11 C31 H31A 126.6 . . ? N7 C31 H31A 126.6 . . ? C30 C32 C14 117.6(6) . . ? C30 C32 H32A 121.2 . . ? C14 C32 H32A 121.2 . . ? N10 C33 C52 124.2(5) . . ? N10 C33 C18 115.0(4) . . ? C52 C33 C18 120.6(5) . . ? C26 C34 C27 120.8(5) . . ? C26 C34 H34A 119.6 . . ? C27 C34 H34A 119.6 . . ? C38 C35 C28 120.8(5) . . ? C38 C35 H35A 119.6 . . ? C28 C35 H35A 119.6 . . ? C45 C36 C49 110.5(6) . . ? C45 C36 C28 110.6(5) . . ? C49 C36 C28 111.0(6) . . ? C45 C36 H36A 108.2 . . ? C49 C36 H36A 108.2 . . ? C28 C36 H36A 108.2 . . ? C26 C37 C12 120.7(5) . . ? C26 C37 H37A 119.6 . . ? C12 C37 H37A 119.6 . . ? C40 C38 C35 121.0(6) . . ? C40 C38 H38A 119.5 . . ? C35 C38 H38A 119.5 . . ? C23 C39 C44 112.2(5) . . ? C23 C39 C41 112.6(5) . . ? C44 C39 C41 109.6(5) . . ? C23 C39 H39A 107.4 . . ? C44 C39 H39A 107.4 . . ? C41 C39 H39A 107.4 . . ? C38 C40 C23 120.8(5) . . ? C38 C40 H40A 119.6 . . ? C23 C40 H40A 119.6 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C17 C42 H42A 109.5 . . ? C17 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C17 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C17 C43 H43A 109.5 . . ? C17 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C17 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C36 C45 H45A 109.5 . . ? C36 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C36 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C50 119.3(5) . . ? C48 C46 H46A 120.3 . . ? C50 C46 H46A 120.3 . . ? N7 C47 N6 104.3(4) . . ? N7 C47 Ag1 129.3(4) . . ? N6 C47 Ag1 126.4(4) . . ? N10 C48 C46 124.0(5) . . ? N10 C48 H48A 118.0 . . ? C46 C48 H48A 118.0 . . ? C36 C49 H49A 109.5 . . ? C36 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C36 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C46 C50 C52 118.5(5) . . ? C46 C50 H50A 120.7 . . ? C52 C50 H50A 120.7 . . ? C29 C51 H51A 109.5 . . ? C29 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C29 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C33 C52 C50 117.6(5) . . ? C33 C52 H52A 121.2 . . ? C50 C52 H52A 121.2 . . ? 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 Br1 Ag2 N9 C30 55.9(4) . . . . ? Br2 Ag2 N9 C30 -117.5(4) . . . . ? Br1 Ag2 N9 C19 -146.4(4) . . . . ? Br2 Ag2 N9 C19 40.3(4) . . . . ? C47 N6 C11 C31 -0.3(6) . . . . ? C13 N6 C11 C31 179.5(4) . . . . ? C47 N6 C13 C23 -89.3(6) . . . . ? C11 N6 C13 C23 90.9(6) . . . . ? C47 N6 C13 C28 90.1(6) . . . . ? C11 N6 C13 C28 -89.7(6) . . . . ? C37 C12 C15 C27 0.4(8) . . . . ? C17 C12 C15 C27 -177.7(5) . . . . ? C37 C12 C15 N5 -177.7(5) . . . . ? C17 C12 C15 N5 4.2(7) . . . . ? C20 N5 C15 C12 -86.3(6) . . . . ? C21 N5 C15 C12 86.2(6) . . . . ? C20 N5 C15 C27 95.5(6) . . . . ? C21 N5 C15 C27 -92.0(6) . . . . ? C20 N8 C16 C19 -95.6(6) . . . . ? C22 N8 C16 C19 82.1(7) . . . . ? C15 C12 C17 C42 105.5(6) . . . . ? C37 C12 C17 C42 -72.5(7) . . . . ? C15 C12 C17 C43 -129.0(6) . . . . ? C37 C12 C17 C43 52.9(7) . . . . ? C47 N7 C18 C33 -88.8(6) . . . . ? C31 N7 C18 C33 84.9(6) . . . . ? C30 N9 C19 C24 0.8(8) . . . . ? Ag2 N9 C19 C24 -155.4(4) . . . . ? C30 N9 C19 C16 -179.3(5) . . . . ? Ag2 N9 C19 C16 24.5(7) . . . . ? N8 C16 C19 N9 -172.7(5) . . . . ? N8 C16 C19 C24 7.2(8) . . . . ? C21 N5 C20 N8 0.4(5) . . . . ? C15 N5 C20 N8 173.6(4) . . . . ? C21 N5 C20 Ag1 -179.3(4) . . . . ? C15 N5 C20 Ag1 -6.1(7) . . . . ? C22 N8 C20 N5 -0.9(5) . . . . ? C16 N8 C20 N5 177.0(4) . . . . ? C22 N8 C20 Ag1 178.7(3) . . . . ? C16 N8 C20 Ag1 -3.3(7) . . . . ? C47 Ag1 C20 N5 141(3) . . . . ? C47 Ag1 C20 N8 -38(3) . . . . ? C20 N5 C21 C22 0.3(6) . . . . ? C15 N5 C21 C22 -172.9(4) . . . . ? N5 C21 C22 N8 -0.9(6) . . . . ? C20 N8 C22 C21 1.1(6) . . . . ? C16 N8 C22 C21 -176.8(4) . . . . ? C28 C13 C23 C40 -2.7(8) . . . . ? N6 C13 C23 C40 176.6(5) . . . . ? C28 C13 C23 C39 178.1(5) . . . . ? N6 C13 C23 C39 -2.6(8) . . . . ? C32 C14 C24 C19 0.5(10) . . . . ? N9 C19 C24 C14 -0.9(9) . . . . ? C16 C19 C24 C14 179.1(6) . . . . ? C12 C15 C27 C34 -1.0(8) . . . . ? N5 C15 C27 C34 177.1(5) . . . . ? C12 C15 C27 C29 177.0(5) . . . . ? N5 C15 C27 C29 -4.9(7) . . . . ? C23 C13 C28 C35 0.8(8) . . . . ? N6 C13 C28 C35 -178.5(5) . . . . ? C23 C13 C28 C36 -179.5(5) . . . . ? N6 C13 C28 C36 1.2(8) . . . . ? C34 C27 C29 C51 69.2(7) . . . . ? C15 C27 C29 C51 -108.7(6) . . . . ? C34 C27 C29 C25 -54.3(7) . . . . ? C15 C27 C29 C25 127.8(6) . . . . ? C19 N9 C30 C32 -0.2(8) . . . . ? Ag2 N9 C30 C32 159.8(5) . . . . ? N6 C11 C31 N7 0.9(5) . . . . ? C47 N7 C31 C11 -1.3(5) . . . . ? C18 N7 C31 C11 -175.8(4) . . . . ? N9 C30 C32 C14 -0.2(9) . . . . ? C24 C14 C32 C30 0.0(10) . . . . ? C48 N10 C33 C52 -0.1(7) . . . . ? C48 N10 C33 C18 174.4(5) . . . . ? N7 C18 C33 N10 -82.2(5) . . . . ? N7 C18 C33 C52 92.5(6) . . . . ? C37 C26 C34 C27 1.4(9) . . . . ? C15 C27 C34 C26 0.1(8) . . . . ? C29 C27 C34 C26 -178.0(5) . . . . ? C13 C28 C35 C38 1.4(9) . . . . ? C36 C28 C35 C38 -178.3(5) . . . . ? C13 C28 C36 C45 109.3(7) . . . . ? C35 C28 C36 C45 -71.0(8) . . . . ? C13 C28 C36 C49 -127.7(6) . . . . ? C35 C28 C36 C49 52.1(8) . . . . ? C34 C26 C37 C12 -2.0(9) . . . . ? C15 C12 C37 C26 1.1(8) . . . . ? C17 C12 C37 C26 179.2(5) . . . . ? C28 C35 C38 C40 -1.5(9) . . . . ? C13 C23 C39 C44 100.2(6) . . . . ? C40 C23 C39 C44 -78.9(7) . . . . ? C13 C23 C39 C41 -135.5(6) . . . . ? C40 C23 C39 C41 45.4(7) . . . . ? C35 C38 C40 C23 -0.6(9) . . . . ? C13 C23 C40 C38 2.6(8) . . . . ? C39 C23 C40 C38 -178.2(5) . . . . ? C31 N7 C47 N6 1.1(5) . . . . ? C18 N7 C47 N6 175.5(4) . . . . ? C31 N7 C47 Ag1 180.0(3) . . . . ? C18 N7 C47 Ag1 -5.6(7) . . . . ? C11 N6 C47 N7 -0.5(5) . . . . ? C13 N6 C47 N7 179.7(4) . . . . ? C11 N6 C47 Ag1 -179.4(3) . . . . ? C13 N6 C47 Ag1 0.8(6) . . . . ? C20 Ag1 C47 N7 -108(3) . . . . ? C20 Ag1 C47 N6 71(3) . . . . ? C33 N10 C48 C46 0.6(8) . . . . ? C50 C46 C48 N10 -0.7(9) . . . . ? C48 C46 C50 C52 0.2(8) . . . . ? N10 C33 C52 C50 -0.3(8) . . . . ? C18 C33 C52 C50 -174.5(5) . . . . ? C46 C50 C52 C33 0.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.741 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.142 data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-(2,6-di-isopropylphenyl)-1-(2-pyridyl)-imidazol-2-ylidene silver bromide ; _chemical_name_common 'Compound X' _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 Ag1 Br1 N3' _chemical_formula_sum 'C20 H23 Ag Br N3' _chemical_formula_weight 493.19 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' 'Br' 'Br' -0.2901 2.4595 '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 'P 21/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 10.8837(4) _cell_length_b 16.4154(6) _cell_length_c 11.4127(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.155(2) _cell_angle_gamma 90.000(2) _cell_volume 1985.49(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2474 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 3.035 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5175 _exptl_absorpt_correction_T_max 0.7933 _exptl_absorpt_process_details ; SORTAV - multi-scan from symmetry-related measurements (R.H. Blessing, 1995-1997 ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 2801 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2167 _reflns_number_gt 1913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0849P)^2^+1.8357P] 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 SHELXL _refine_ls_extinction_coef 0.0086(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2167 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.004 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 0.06743(5) 0.17981(3) 0.29062(4) 0.0266(3) Uani 1 1 d . . . Br2 Br 0.28322(8) 0.14986(6) 0.39205(7) 0.0468(4) Uani 1 1 d . . . C16 C -0.1933(7) 0.2361(4) 0.4738(5) 0.0244(16) Uani 1 1 d . . . C6 C -0.0193(7) 0.1463(4) -0.0057(6) 0.0274(17) Uani 1 1 d . . . C7 C 0.0262(10) 0.1041(5) -0.0873(6) 0.0334(19) Uani 1 1 d . . . C8 C -0.1368(6) 0.1271(4) 0.0097(5) 0.0221(15) Uani 1 1 d . . . C9 C -0.1279(7) 0.4003(4) 0.4731(6) 0.0305(17) Uani 1 1 d . . . C10 C -0.0476(7) 0.0441(4) -0.1540(5) 0.0312(17) Uani 1 1 d . . . H10 H -0.0168 0.0122 -0.2107 0.037 Uiso 1 1 calc R . . C11 C -0.3174(7) 0.1831(4) 0.0845(6) 0.0273(18) Uani 1 1 d . . . C12 C -0.3290(8) 0.2230(4) 0.1830(6) 0.0269(16) Uani 1 1 d . . . N1 N -0.1907(6) 0.1678(3) 0.0990(5) 0.0234(14) Uani 1 1 d . . . C14 C -0.1378(7) 0.3632(4) 0.5798(6) 0.0315(17) Uani 1 1 d . . . N3 N -0.2126(5) 0.0720(3) -0.0529(4) 0.0262(13) Uani 1 1 d . . . N2 N -0.2103(5) 0.2320(3) 0.2562(4) 0.0233(13) Uani 1 1 d . . . C18 C -0.1702(7) 0.2815(4) 0.5784(6) 0.0306(17) Uani 1 1 d . . . C20 C -0.1832(7) 0.2763(4) 0.3693(5) 0.0246(16) Uani 1 1 d . . . C19 C -0.1495(6) 0.3588(4) 0.3662(6) 0.0245(16) Uani 1 1 d . . . C17 C -0.1664(8) 0.0323(4) -0.1357(6) 0.0301(18) Uani 1 1 d . . . C5 C -0.1416(7) 0.4014(4) 0.2492(6) 0.0283(16) Uani 1 1 d . . . C2 C -0.2233(8) 0.1456(4) 0.4754(6) 0.0351(19) Uani 1 1 d . . . C1 C -0.1208(7) 0.1974(4) 0.2065(5) 0.0224(16) Uani 1 1 d . . . C4 C -0.1015(8) 0.1004(5) 0.5362(6) 0.044(2) Uani 1 1 d . . . H4A H -0.1187 0.0419 0.5383 0.065 Uiso 1 1 calc R . . H4B H -0.0715 0.1207 0.6185 0.065 Uiso 1 1 calc R . . H4C H -0.0368 0.1098 0.4905 0.065 Uiso 1 1 calc R . . C3 C -0.3302(10) 0.1258(6) 0.5364(11) 0.057(3) Uani 1 1 d . . . C13 C -0.2554(10) 0.4540(6) 0.2052(8) 0.066(3) Uani 1 1 d . . . H13A H -0.3321 0.4215 0.1996 0.100 Uiso 1 1 calc R . . H13B H -0.2538 0.4759 0.1257 0.100 Uiso 1 1 calc R . . H13C H -0.2548 0.4991 0.2616 0.100 Uiso 1 1 calc R . . C15 C -0.0262(11) 0.4518(9) 0.2578(9) 0.097(5) Uani 1 1 d . . . H15A H 0.0488 0.4182 0.2875 0.145 Uiso 1 1 calc R . . H15B H -0.0270 0.4971 0.3135 0.145 Uiso 1 1 calc R . . H15C H -0.0244 0.4733 0.1781 0.145 Uiso 1 1 calc R . . H7 H -0.115(7) 0.390(5) 0.669(6) 0.039(19) Uiso 1 1 d . . . H5 H -0.385(7) 0.246(4) 0.201(5) 0.015(19) Uiso 1 1 d . . . H6 H -0.180(7) 0.266(5) 0.654(7) 0.04(2) Uiso 1 1 d . . . H4 H -0.392(8) 0.163(4) 0.014(6) 0.031(19) Uiso 1 1 d . . . H8 H -0.106(6) 0.458(4) 0.467(5) 0.026(16) Uiso 1 1 d . . . H10 H -0.250(6) 0.124(4) 0.385(5) 0.016(15) Uiso 1 1 d . . . H1 H 0.016(8) 0.186(5) 0.030(6) 0.03(2) Uiso 1 1 d . . . H3 H -0.223(7) 0.002(4) -0.171(5) 0.019(18) Uiso 1 1 d . . . H2 H 0.094(7) 0.113(4) -0.092(5) 0.010(19) Uiso 1 1 d . . . H9 H -0.132(10) 0.361(7) 0.196(8) 0.08(3) Uiso 1 1 d . . . H18 H -0.327(7) 0.146(4) 0.589(6) 0.01(2) Uiso 1 1 d . . . H17 H -0.430(12) 0.152(6) 0.489(9) 0.08(3) Uiso 1 1 d . . . H19 H -0.378(12) 0.069(8) 0.515(9) 0.10(4) 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 0.0195(6) 0.0331(4) 0.0256(4) -0.00469(18) 0.0014(3) 0.00247(19) Br2 0.0309(7) 0.0673(6) 0.0383(5) -0.0054(4) -0.0003(4) 0.0078(4) C16 0.015(4) 0.028(3) 0.027(3) -0.001(3) -0.002(3) 0.004(3) C6 0.031(5) 0.027(4) 0.025(4) -0.006(3) 0.008(3) -0.004(3) C7 0.021(5) 0.046(5) 0.034(4) 0.006(3) 0.010(4) -0.002(4) C8 0.019(4) 0.026(3) 0.021(3) 0.004(3) 0.006(3) 0.005(3) C9 0.021(5) 0.032(4) 0.038(4) -0.003(3) 0.006(3) 0.006(3) C10 0.039(5) 0.035(4) 0.022(3) 0.003(3) 0.012(3) 0.002(3) C11 0.012(5) 0.037(4) 0.029(4) 0.007(3) -0.003(3) -0.005(3) C12 0.017(5) 0.034(4) 0.028(4) -0.005(3) 0.001(4) 0.003(3) N1 0.019(4) 0.026(3) 0.024(3) 0.000(2) 0.002(3) -0.004(2) C14 0.024(5) 0.039(4) 0.031(4) -0.008(3) 0.005(3) 0.002(3) N3 0.025(4) 0.026(3) 0.028(3) -0.002(2) 0.007(3) -0.008(2) N2 0.023(4) 0.027(3) 0.020(3) 0.001(2) 0.004(3) -0.001(2) C18 0.024(5) 0.039(4) 0.029(4) -0.003(3) 0.005(3) 0.011(3) C20 0.021(4) 0.027(3) 0.025(3) -0.005(3) 0.003(3) 0.003(3) C19 0.013(4) 0.028(3) 0.031(4) -0.007(3) 0.001(3) 0.004(3) C17 0.038(5) 0.029(4) 0.025(4) -0.011(3) 0.012(4) -0.007(4) C5 0.026(5) 0.031(3) 0.029(4) 0.003(3) 0.008(3) -0.003(3) C2 0.041(6) 0.030(4) 0.032(4) 0.002(3) 0.004(4) -0.006(3) C1 0.020(5) 0.027(3) 0.021(3) 0.001(3) 0.008(3) 0.004(3) C4 0.049(6) 0.037(4) 0.042(4) 0.003(3) 0.004(4) 0.013(4) C3 0.057(8) 0.050(5) 0.066(7) -0.012(5) 0.020(6) -0.007(5) C13 0.060(7) 0.080(6) 0.067(5) 0.050(5) 0.029(5) 0.035(5) C15 0.051(7) 0.180(14) 0.056(6) 0.031(7) 0.007(5) -0.054(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 C1 2.075(7) . ? Ag1 Br2 2.4208(10) . ? C16 C18 1.382(10) . ? C16 C20 1.389(9) . ? C16 C2 1.522(9) . ? C6 C7 1.343(11) . ? C6 C8 1.367(10) . ? C6 H1 0.81(8) . ? C7 C10 1.384(11) . ? C7 H2 0.76(7) . ? C8 N3 1.319(8) . ? C8 N1 1.450(9) . ? C9 C19 1.370(9) . ? C9 C14 1.387(10) . ? C9 H8 0.98(7) . ? C10 C17 1.370(10) . ? C10 H10 0.9500 . ? C11 C12 1.331(11) . ? C11 N1 1.374(10) . ? C11 H4 1.06(8) . ? C12 N2 1.377(9) . ? C12 H5 0.78(7) . ? N1 C1 1.377(9) . ? C14 C18 1.385(10) . ? C14 H7 1.09(7) . ? N3 C17 1.337(9) . ? N2 C1 1.358(9) . ? N2 C20 1.451(8) . ? C18 H6 0.93(7) . ? C20 C19 1.406(9) . ? C19 C5 1.527(9) . ? C17 H3 0.83(7) . ? C5 C15 1.489(12) . ? C5 C13 1.500(11) . ? C5 H9 0.92(10) . ? C2 C3 1.521(14) . ? C2 C4 1.540(11) . ? C2 H10 1.06(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 H18 0.68(6) . ? C3 H17 1.18(12) . ? C3 H19 1.08(13) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 C1 Ag1 Br2 176.06(17) . . ? C18 C16 C20 116.8(6) . . ? C18 C16 C2 120.9(6) . . ? C20 C16 C2 122.2(5) . . ? C7 C6 C8 118.3(7) . . ? C7 C6 H1 124(6) . . ? C8 C6 H1 118(6) . . ? C6 C7 C10 119.3(9) . . ? C6 C7 H2 117(5) . . ? C10 C7 H2 123(5) . . ? N3 C8 C6 125.2(6) . . ? N3 C8 N1 113.2(6) . . ? C6 C8 N1 121.6(6) . . ? C19 C9 C14 122.1(6) . . ? C19 C9 H8 114(3) . . ? C14 C9 H8 124(3) . . ? C17 C10 C7 117.8(7) . . ? C17 C10 H10 121.1 . . ? C7 C10 H10 121.1 . . ? C12 C11 N1 105.9(6) . . ? C12 C11 H4 127(4) . . ? N1 C11 H4 127(4) . . ? C11 C12 N2 108.0(7) . . ? C11 C12 H5 133(5) . . ? N2 C12 H5 118(5) . . ? C11 N1 C1 112.2(6) . . ? C11 N1 C8 123.7(5) . . ? C1 N1 C8 124.0(6) . . ? C18 C14 C9 119.0(6) . . ? C18 C14 H7 114(4) . . ? C9 C14 H7 127(4) . . ? C8 N3 C17 115.4(6) . . ? C1 N2 C12 111.4(5) . . ? C1 N2 C20 124.1(6) . . ? C12 N2 C20 124.5(6) . . ? C16 C18 C14 121.9(7) . . ? C16 C18 H6 129(4) . . ? C14 C18 H6 109(4) . . ? C16 C20 C19 123.4(5) . . ? C16 C20 N2 119.1(5) . . ? C19 C20 N2 117.5(5) . . ? C9 C19 C20 116.7(6) . . ? C9 C19 C5 121.3(6) . . ? C20 C19 C5 122.0(5) . . ? N3 C17 C10 123.9(7) . . ? N3 C17 H3 106(5) . . ? C10 C17 H3 130(5) . . ? C15 C5 C13 108.8(9) . . ? C15 C5 C19 114.3(6) . . ? C13 C5 C19 110.5(6) . . ? C15 C5 H9 103(7) . . ? C13 C5 H9 114(7) . . ? C19 C5 H9 106(6) . . ? C16 C2 C3 113.7(7) . . ? C16 C2 C4 108.1(6) . . ? C3 C2 C4 111.1(7) . . ? C16 C2 H10 109(3) . . ? C3 C2 H10 108(3) . . ? C4 C2 H10 107(3) . . ? N2 C1 N1 102.5(6) . . ? N2 C1 Ag1 126.3(4) . . ? N1 C1 Ag1 130.6(5) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C3 H18 115(7) . . ? C2 C3 H17 115(5) . . ? H18 C3 H17 95(8) . . ? C2 C3 H19 118(6) . . ? H18 C3 H19 123(9) . . ? H17 C3 H19 83(8) . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C15 H15A 109.5 . . ? C5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 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 C8 C6 C7 C10 1.1(10) . . . . ? C7 C6 C8 N3 -2.8(10) . . . . ? C7 C6 C8 N1 177.7(6) . . . . ? C6 C7 C10 C17 1.9(10) . . . . ? N1 C11 C12 N2 0.2(7) . . . . ? C12 C11 N1 C1 0.2(7) . . . . ? C12 C11 N1 C8 -178.2(6) . . . . ? N3 C8 N1 C11 -32.5(8) . . . . ? C6 C8 N1 C11 147.0(6) . . . . ? N3 C8 N1 C1 149.3(5) . . . . ? C6 C8 N1 C1 -31.2(9) . . . . ? C19 C9 C14 C18 0.3(11) . . . . ? C6 C8 N3 C17 1.1(9) . . . . ? N1 C8 N3 C17 -179.4(5) . . . . ? C11 C12 N2 C1 -0.5(7) . . . . ? C11 C12 N2 C20 176.6(6) . . . . ? C20 C16 C18 C14 -0.3(11) . . . . ? C2 C16 C18 C14 177.4(7) . . . . ? C9 C14 C18 C16 -0.3(11) . . . . ? C18 C16 C20 C19 0.9(10) . . . . ? C2 C16 C20 C19 -176.7(7) . . . . ? C18 C16 C20 N2 -178.2(7) . . . . ? C2 C16 C20 N2 4.2(10) . . . . ? C1 N2 C20 C16 -97.3(8) . . . . ? C12 N2 C20 C16 85.9(8) . . . . ? C1 N2 C20 C19 83.6(8) . . . . ? C12 N2 C20 C19 -93.2(8) . . . . ? C14 C9 C19 C20 0.3(10) . . . . ? C14 C9 C19 C5 178.3(7) . . . . ? C16 C20 C19 C9 -0.9(10) . . . . ? N2 C20 C19 C9 178.1(6) . . . . ? C16 C20 C19 C5 -178.9(7) . . . . ? N2 C20 C19 C5 0.2(10) . . . . ? C8 N3 C17 C10 2.3(9) . . . . ? C7 C10 C17 N3 -3.8(10) . . . . ? C9 C19 C5 C15 48.1(11) . . . . ? C20 C19 C5 C15 -134.0(9) . . . . ? C9 C19 C5 C13 -74.9(9) . . . . ? C20 C19 C5 C13 102.9(8) . . . . ? C18 C16 C2 C3 52.4(10) . . . . ? C20 C16 C2 C3 -130.1(8) . . . . ? C18 C16 C2 C4 -71.5(9) . . . . ? C20 C16 C2 C4 106.0(7) . . . . ? C12 N2 C1 N1 0.6(7) . . . . ? C20 N2 C1 N1 -176.5(5) . . . . ? C12 N2 C1 Ag1 -170.6(5) . . . . ? C20 N2 C1 Ag1 12.3(8) . . . . ? C11 N1 C1 N2 -0.5(6) . . . . ? C8 N1 C1 N2 177.9(5) . . . . ? C11 N1 C1 Ag1 170.2(5) . . . . ? C8 N1 C1 Ag1 -11.4(9) . . . . ? Br2 Ag1 C1 N2 95(3) . . . . ? Br2 Ag1 C1 N1 -73(3) . . . . ? _diffrn_measured_fraction_theta_max 0.602 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.602 _refine_diff_density_max 1.113 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.163 data_9b _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-mesityl-1-(N,N-diethylacetamido) imidazol-2-ylidene silver bromide ; _chemical_name_common 00skl035 _chemical_melting_point ? _chemical_formula_moiety 'C34 H50 Ag1 Br0.65 Cl7.35 N4 O2' _chemical_formula_sum 'C18 H25 Ag Br0.08 Cl0.92 N3 O' _chemical_formula_weight 446.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 26.5398(2) _cell_length_b 10.44890(10) _cell_length_c 16.8853(2) _cell_angle_alpha 90.00 _cell_angle_beta 125.9000(10) _cell_angle_gamma 90.00 _cell_volume 3793.01(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20698 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 1.373 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8205 _exptl_absorpt_correction_T_max 0.9345 _exptl_absorpt_process_details ; SORTAV - multi-scan from symmetry-related measurements (R.H. Blessing, 1995-1997 ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 21107 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5526 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0912P)^2^+12.1639P] 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 5526 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 0.081475(13) 0.62725(3) 0.28795(2) 0.03656(13) Uani 1 1 d . . . O O 0.15358(12) 0.7639(3) 0.1100(2) 0.0373(6) Uani 1 1 d . . . Br1 Br 0.04467(4) 0.65670(12) 0.38760(7) 0.0479(4) Uani 0.081(4) 1 d P . . Cl2 Cl 0.04467(4) 0.65670(12) 0.38760(7) 0.0479(4) Uani 0.919(4) 1 d P . . N1 N 0.12930(14) 0.5441(3) 0.1638(2) 0.0309(6) Uani 1 1 d . . . N2 N 0.19475(14) 0.4997(3) 0.3147(2) 0.0321(6) Uani 1 1 d . . . C2 C 0.22977(18) 0.5056(4) 0.4194(3) 0.0342(8) Uani 1 1 d . . . C3 C 0.07861(17) 0.6032(4) 0.0740(3) 0.0354(8) Uani 1 1 d . . . H3A H 0.0437 0.6206 0.0784 0.043 Uiso 1 1 calc R . . H3B H 0.0636 0.5439 0.0186 0.043 Uiso 1 1 calc R . . C5 C 0.21650(18) 0.4417(4) 0.2662(3) 0.0360(8) Uani 1 1 d . . . H5 H 0.2533 0.3920 0.2944 0.043 Uiso 1 1 calc R . . C6 C 0.10016(17) 0.7289(4) 0.0555(3) 0.0371(8) Uani 1 1 d . . . C7 C 0.2149(2) 0.4233(4) 0.4680(3) 0.0420(9) Uani 1 1 d . . . C8 C 0.2781(2) 0.5943(4) 0.4682(3) 0.0394(8) Uani 1 1 d . . . C9 C 0.17492(18) 0.4701(4) 0.1709(3) 0.0376(8) Uani 1 1 d . . . H9 H 0.1766 0.4441 0.1186 0.045 Uiso 1 1 calc R . . C11 C 0.3136(2) 0.5964(5) 0.5697(3) 0.0465(10) Uani 1 1 d . . . H11 H 0.3467 0.6561 0.6048 0.056 Uiso 1 1 calc R . . C12 C 0.14050(17) 0.5631(3) 0.2516(3) 0.0313(7) Uani 1 1 d . . . C13 C 0.2523(2) 0.4299(5) 0.5701(3) 0.0493(11) Uani 1 1 d . . . H13 H 0.2433 0.3751 0.6052 0.059 Uiso 1 1 calc R . . C14 C 0.3017(2) 0.5130(5) 0.6214(3) 0.0509(12) Uani 1 1 d . . . C15 C 0.2917(2) 0.6845(4) 0.4139(3) 0.0470(10) Uani 1 1 d . . . H15A H 0.2619 0.6701 0.3434 0.070 Uiso 1 1 calc R . . H15B H 0.3340 0.6695 0.4333 0.070 Uiso 1 1 calc R . . H15C H 0.2881 0.7729 0.4294 0.070 Uiso 1 1 calc R . . C17 C 0.3427(3) 0.5168(7) 0.7321(4) 0.0716(18) Uani 1 1 d . . . H17A H 0.3750 0.5820 0.7549 0.107 Uiso 1 1 calc R . . H17B H 0.3622 0.4330 0.7578 0.107 Uiso 1 1 calc R . . H17C H 0.3174 0.5381 0.7552 0.107 Uiso 1 1 calc R . . C18 C 0.1617(2) 0.3308(5) 0.4139(4) 0.0513(11) Uani 1 1 d . . . H18A H 0.1590 0.2817 0.4608 0.077 Uiso 1 1 calc R . . H18B H 0.1684 0.2722 0.3756 0.077 Uiso 1 1 calc R . . H18C H 0.1228 0.3781 0.3700 0.077 Uiso 1 1 calc R . . N3 N 0.0574(2) 0.7955(7) -0.0232(4) 0.103(3) Uani 1 1 d . . . C20 C 0.0729(3) 0.9244(12) -0.0429(7) 0.159(6) Uani 1 1 d . . . H20A H 0.0715 0.9855 0.0006 0.191 Uiso 1 1 calc R . . H20B H 0.1169 0.9198 -0.0193 0.191 Uiso 1 1 calc R . . C21 C -0.0239(7) 0.7739(9) -0.0823(8) 0.178(7) Uani 1 1 d . . . H21A H -0.0345 0.7280 -0.0427 0.214 Uiso 1 1 calc R . . H21B H -0.0490 0.8527 -0.1118 0.214 Uiso 1 1 calc R . . C25 C -0.0217(6) 0.7044(6) -0.1407(7) 0.126(4) Uani 1 1 d . . . H25A H -0.0633 0.6703 -0.1902 0.188 Uiso 1 1 calc R . . H25B H 0.0072 0.6335 -0.1049 0.188 Uiso 1 1 calc R . . H25C H -0.0074 0.7552 -0.1728 0.188 Uiso 1 1 calc R . . C22 C 0.0465(4) 0.9719(12) -0.1179(13) 0.267(12) Uani 1 1 d . . . H22A H 0.0629 1.0584 -0.1114 0.400 Uiso 1 1 calc R . . H22B H 0.0022 0.9768 -0.1453 0.400 Uiso 1 1 calc R . . H22C H 0.0518 0.9212 -0.1614 0.400 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 0.0402(2) 0.03953(19) 0.0460(2) 0.00605(11) 0.03431(16) 0.00873(11) O 0.0347(13) 0.0391(14) 0.0372(13) -0.0035(11) 0.0205(11) -0.0069(11) Br1 0.0355(5) 0.0848(8) 0.0340(5) 0.0016(4) 0.0262(4) 0.0043(4) Cl2 0.0355(5) 0.0848(8) 0.0340(5) 0.0016(4) 0.0262(4) 0.0043(4) N1 0.0308(14) 0.0364(15) 0.0314(14) 0.0016(12) 0.0216(12) -0.0002(12) N2 0.0363(15) 0.0379(15) 0.0333(15) 0.0079(12) 0.0266(13) 0.0108(12) C2 0.0391(18) 0.0398(18) 0.0332(17) 0.0122(14) 0.0264(16) 0.0179(15) C3 0.0297(17) 0.046(2) 0.0297(17) 0.0014(14) 0.0171(14) -0.0070(15) C5 0.0407(19) 0.0399(19) 0.0427(19) 0.0044(15) 0.0329(17) 0.0083(15) C6 0.0323(17) 0.046(2) 0.0344(18) 0.0034(15) 0.0205(15) -0.0059(15) C7 0.052(2) 0.045(2) 0.045(2) 0.0158(17) 0.037(2) 0.0220(18) C8 0.045(2) 0.0396(19) 0.0395(19) 0.0063(16) 0.0281(18) 0.0144(17) C9 0.042(2) 0.043(2) 0.042(2) -0.0038(16) 0.0323(17) 0.0010(16) C11 0.055(3) 0.050(2) 0.037(2) 0.0026(18) 0.029(2) 0.017(2) C12 0.0352(17) 0.0360(17) 0.0338(17) 0.0056(13) 0.0265(15) 0.0056(14) C13 0.065(3) 0.057(3) 0.045(2) 0.021(2) 0.043(2) 0.031(2) C14 0.062(3) 0.067(3) 0.0332(19) 0.0146(19) 0.033(2) 0.034(2) C15 0.050(2) 0.048(2) 0.043(2) 0.0068(18) 0.027(2) 0.0036(19) C17 0.074(4) 0.106(5) 0.037(2) 0.015(3) 0.035(3) 0.039(3) C18 0.062(3) 0.051(2) 0.061(3) 0.018(2) 0.047(3) 0.013(2) N3 0.032(2) 0.128(5) 0.091(4) 0.074(4) 0.004(2) -0.023(3) C20 0.056(4) 0.201(9) 0.117(6) 0.115(7) -0.007(4) -0.060(5) C21 0.385(19) 0.105(6) 0.186(10) 0.104(7) 0.246(13) 0.147(10) C25 0.272(13) 0.049(3) 0.149(8) 0.021(4) 0.175(9) 0.012(5) C22 0.066(5) 0.144(10) 0.35(2) 0.170(12) -0.012(8) -0.037(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 Ag1 C12 2.099(3) . ? Ag1 Br1 2.4099(9) . ? Ag1 Cl2 2.9071(10) 6_556 ? Ag1 Br1 2.9071(10) 6_556 ? O C6 1.208(4) . ? Br1 Ag1 2.9071(10) 6_556 ? N1 C12 1.346(4) . ? N1 C9 1.381(5) . ? N1 C3 1.448(5) . ? N2 C12 1.359(5) . ? N2 C5 1.389(4) . ? N2 C2 1.438(5) . ? C2 C7 1.394(5) . ? C2 C8 1.395(6) . ? C3 C6 1.536(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C9 1.346(6) . ? C5 H5 0.9500 . ? C6 N3 1.330(6) . ? C7 C13 1.399(6) . ? C7 C18 1.501(7) . ? C8 C11 1.390(6) . ? C8 C15 1.499(6) . ? C9 H9 0.9500 . ? C11 C14 1.393(7) . ? C11 H11 0.9500 . ? C13 C14 1.375(8) . ? C13 H13 0.9500 . ? C14 C17 1.515(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N3 C20 1.502(9) . ? N3 C21 1.783(16) . ? C20 C22 1.140(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.254(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C12 Ag1 Br1 157.27(10) . . ? C12 Ag1 Cl2 110.26(10) . 6_556 ? Br1 Ag1 Cl2 90.14(3) . 6_556 ? C12 Ag1 Br1 110.26(10) . 6_556 ? Br1 Ag1 Br1 90.14(3) . 6_556 ? Cl2 Ag1 Br1 0.00(4) 6_556 6_556 ? Ag1 Br1 Ag1 88.31(3) . 6_556 ? C12 N1 C9 111.7(3) . . ? C12 N1 C3 124.1(3) . . ? C9 N1 C3 124.0(3) . . ? C12 N2 C5 111.5(3) . . ? C12 N2 C2 124.6(3) . . ? C5 N2 C2 123.5(3) . . ? C7 C2 C8 122.8(4) . . ? C7 C2 N2 119.7(4) . . ? C8 C2 N2 117.5(3) . . ? N1 C3 C6 110.4(3) . . ? N1 C3 H3A 109.6 . . ? C6 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C6 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C9 C5 N2 106.0(3) . . ? C9 C5 H5 127.0 . . ? N2 C5 H5 127.0 . . ? O C6 N3 122.4(4) . . ? O C6 C3 121.0(3) . . ? N3 C6 C3 116.7(3) . . ? C2 C7 C13 117.0(5) . . ? C2 C7 C18 121.9(4) . . ? C13 C7 C18 121.0(4) . . ? C11 C8 C2 117.5(4) . . ? C11 C8 C15 120.9(4) . . ? C2 C8 C15 121.6(4) . . ? C5 C9 N1 106.9(3) . . ? C5 C9 H9 126.5 . . ? N1 C9 H9 126.5 . . ? C8 C11 C14 121.6(5) . . ? C8 C11 H11 119.2 . . ? C14 C11 H11 119.2 . . ? N1 C12 N2 103.9(3) . . ? N1 C12 Ag1 130.5(3) . . ? N2 C12 Ag1 123.7(2) . . ? C14 C13 C7 122.1(4) . . ? C14 C13 H13 118.9 . . ? C7 C13 H13 118.9 . . ? C13 C14 C11 118.9(4) . . ? C13 C14 C17 121.5(5) . . ? C11 C14 C17 119.5(5) . . ? C8 C15 H15A 109.5 . . ? C8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C18 H18A 109.5 . . ? C7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C6 N3 C20 120.4(4) . . ? C6 N3 C21 122.5(4) . . ? C20 N3 C21 112.8(5) . . ? C22 C20 N3 124.5(9) . . ? C22 C20 H20A 106.2 . . ? N3 C20 H20A 106.2 . . ? C22 C20 H20B 106.2 . . ? N3 C20 H20B 106.2 . . ? H20A C20 H20B 106.4 . . ? C25 C21 N3 85.1(9) . . ? C25 C21 H21A 114.5 . . ? N3 C21 H21A 114.5 . . ? C25 C21 H21B 114.5 . . ? N3 C21 H21B 114.5 . . ? H21A C21 H21B 111.6 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 C12 Ag1 Br1 Ag1 -142.4(3) . . . 6_556 ? Cl2 Ag1 Br1 Ag1 12.06(5) 6_556 . . 6_556 ? Br1 Ag1 Br1 Ag1 12.06(5) 6_556 . . 6_556 ? C12 N2 C2 C7 85.6(5) . . . . ? C5 N2 C2 C7 -103.0(4) . . . . ? C12 N2 C2 C8 -94.9(4) . . . . ? C5 N2 C2 C8 76.5(5) . . . . ? C12 N1 C3 C6 92.6(4) . . . . ? C9 N1 C3 C6 -81.9(4) . . . . ? C12 N2 C5 C9 0.2(4) . . . . ? C2 N2 C5 C9 -172.2(4) . . . . ? N1 C3 C6 O 2.7(5) . . . . ? N1 C3 C6 N3 -177.7(5) . . . . ? C8 C2 C7 C13 -2.1(5) . . . . ? N2 C2 C7 C13 177.4(3) . . . . ? C8 C2 C7 C18 178.4(4) . . . . ? N2 C2 C7 C18 -2.1(5) . . . . ? C7 C2 C8 C11 2.0(6) . . . . ? N2 C2 C8 C11 -177.5(3) . . . . ? C7 C2 C8 C15 -178.0(4) . . . . ? N2 C2 C8 C15 2.6(5) . . . . ? N2 C5 C9 N1 0.1(4) . . . . ? C12 N1 C9 C5 -0.3(4) . . . . ? C3 N1 C9 C5 174.7(3) . . . . ? C2 C8 C11 C14 0.2(6) . . . . ? C15 C8 C11 C14 -179.9(4) . . . . ? C9 N1 C12 N2 0.4(4) . . . . ? C3 N1 C12 N2 -174.6(3) . . . . ? C9 N1 C12 Ag1 -163.9(3) . . . . ? C3 N1 C12 Ag1 21.1(5) . . . . ? C5 N2 C12 N1 -0.4(4) . . . . ? C2 N2 C12 N1 171.9(3) . . . . ? C5 N2 C12 Ag1 165.3(3) . . . . ? C2 N2 C12 Ag1 -22.4(5) . . . . ? Br1 Ag1 C12 N1 157.7(2) . . . . ? Cl2 Ag1 C12 N1 5.1(4) 6_556 . . . ? Br1 Ag1 C12 N1 5.1(4) 6_556 . . . ? Br1 Ag1 C12 N2 -4.0(5) . . . . ? Cl2 Ag1 C12 N2 -156.6(3) 6_556 . . . ? Br1 Ag1 C12 N2 -156.6(3) 6_556 . . . ? C2 C7 C13 C14 -0.1(6) . . . . ? C18 C7 C13 C14 179.4(4) . . . . ? C7 C13 C14 C11 2.1(6) . . . . ? C7 C13 C14 C17 -178.6(4) . . . . ? C8 C11 C14 C13 -2.2(6) . . . . ? C8 C11 C14 C17 178.5(4) . . . . ? O C6 N3 C20 -5.3(12) . . . . ? C3 C6 N3 C20 175.2(9) . . . . ? O C6 N3 C21 -160.4(6) . . . . ? C3 C6 N3 C21 20.0(9) . . . . ? C6 N3 C20 C22 158.0(18) . . . . ? C21 N3 C20 C22 -45(2) . . . . ? C6 N3 C21 C25 -98.4(8) . . . . ? C20 N3 C21 C25 104.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.858 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.208 data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-tert-butyl-1-(4,6-di-tertbutyl-o-toluidyl-phenylimine)- imidazol-2-ylidene silver bromide ; _chemical_name_common 00skl033 _chemical_melting_point ? _chemical_formula_moiety 'C29 H39 Ag1 Cl1 N3' _chemical_formula_sum 'C29 H39 Ag Cl N3' _chemical_formula_weight 572.95 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6884(2) _cell_length_b 11.4709(2) _cell_length_c 13.7750(2) _cell_angle_alpha 71.9370(10) _cell_angle_beta 85.7790(10) _cell_angle_gamma 76.9490(10) _cell_volume 1417.83(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14099 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9002 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details ; SORTAV (Blessing, 1995-1997) ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 14216 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 29.97 _reflns_number_total 7942 _reflns_number_gt 6214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0586P)^2^+0.2498P] 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 7942 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.008 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 0.886629(19) 0.893239(18) 0.580981(16) 0.03187(8) Uani 1 1 d . . . Cl1 Cl 1.10106(6) 0.92747(6) 0.62831(5) 0.02846(14) Uani 1 1 d . . . N2 N 0.6155(2) 0.85047(17) 0.50516(14) 0.0215(4) Uani 1 1 d . . . N3 N 0.5949(2) 0.82917(19) 0.66561(15) 0.0245(4) Uani 1 1 d . . . N1 N 0.7193(2) 0.80195(18) 0.21156(15) 0.0257(4) Uani 1 1 d . . . C9 C 0.7605(2) 0.5737(2) 0.29378(17) 0.0219(5) Uani 1 1 d . . . C8 C 0.7781(2) 0.4743(2) 0.38501(18) 0.0219(5) Uani 1 1 d . . . H8 H 0.7976 0.3909 0.3811 0.026 Uiso 1 1 calc R . . C5 C 0.7196(2) 0.7166(2) 0.39712(17) 0.0215(5) Uani 1 1 d . . . C1 C 0.6877(2) 0.8478(2) 0.58623(18) 0.0227(5) Uani 1 1 d . . . C6 C 0.7366(2) 0.6138(2) 0.48522(17) 0.0219(5) Uani 1 1 d . . . H6 H 0.7259 0.6281 0.5500 0.026 Uiso 1 1 calc R . . C2 C 0.4657(3) 0.8231(2) 0.6315(2) 0.0283(5) Uani 1 1 d . . . H2 H 0.3828 0.8120 0.6714 0.034 Uiso 1 1 calc R . . C3 C 0.4806(3) 0.8356(2) 0.5320(2) 0.0276(5) Uani 1 1 d . . . H3 H 0.4103 0.8345 0.4879 0.033 Uiso 1 1 calc R . . C10 C 0.7355(3) 0.6962(2) 0.30164(17) 0.0227(5) Uani 1 1 d . . . C11 C 0.7840(2) 0.3826(2) 0.58083(17) 0.0213(5) Uani 1 1 d . . . C7 C 0.7685(2) 0.4918(2) 0.48114(17) 0.0200(4) Uani 1 1 d . . . C4 C 0.6806(3) 0.8493(2) 0.40635(18) 0.0267(5) Uani 1 1 d . . . H4A H 0.7670 0.8840 0.3978 0.032 Uiso 1 1 calc R . . H4B H 0.6139 0.9035 0.3512 0.032 Uiso 1 1 calc R . . C18 C 0.8593(3) 0.2578(2) 0.5642(2) 0.0330(6) Uani 1 1 d . . . H18A H 0.9548 0.2637 0.5374 0.049 Uiso 1 1 calc R . . H18B H 0.8056 0.2392 0.5153 0.049 Uiso 1 1 calc R . . H18C H 0.8657 0.1907 0.6294 0.049 Uiso 1 1 calc R . . C16 C 0.8721(3) 0.4070(2) 0.6580(2) 0.0340(6) Uani 1 1 d . . . H16A H 0.9670 0.4131 0.6300 0.051 Uiso 1 1 calc R . . H16B H 0.8797 0.3376 0.7219 0.051 Uiso 1 1 calc R . . H16C H 0.8257 0.4857 0.6715 0.051 Uiso 1 1 calc R . . C19 C 0.7699(3) 0.5465(2) 0.18988(18) 0.0261(5) Uani 1 1 d . . . C24 C 0.8074(3) 0.8727(2) 0.19740(18) 0.0270(5) Uani 1 1 d . . . H24 H 0.8808 0.8521 0.2458 0.032 Uiso 1 1 calc R . . C22 C 0.8919(3) 0.5957(3) 0.1244(2) 0.0376(7) Uani 1 1 d . . . H22A H 0.9815 0.5552 0.1608 0.056 Uiso 1 1 calc R . . H22B H 0.8758 0.6867 0.1109 0.056 Uiso 1 1 calc R . . H22C H 0.8960 0.5765 0.0595 0.056 Uiso 1 1 calc R . . C17 C 0.6359(3) 0.3722(3) 0.6247(2) 0.0375(7) Uani 1 1 d . . . H17A H 0.5880 0.4515 0.6365 0.056 Uiso 1 1 calc R . . H17B H 0.6440 0.3042 0.6894 0.056 Uiso 1 1 calc R . . H17C H 0.5809 0.3541 0.5762 0.056 Uiso 1 1 calc R . . C25 C 0.7994(3) 0.9861(2) 0.10788(19) 0.0315(6) Uani 1 1 d . . . C21 C 0.6286(3) 0.6086(3) 0.1330(2) 0.0403(7) Uani 1 1 d . . . H21A H 0.6068 0.6986 0.1253 0.060 Uiso 1 1 calc R . . H21B H 0.5528 0.5704 0.1720 0.060 Uiso 1 1 calc R . . H21C H 0.6362 0.5961 0.0654 0.060 Uiso 1 1 calc R . . C20 C 0.7970(4) 0.4059(3) 0.2035(2) 0.0413(7) Uani 1 1 d . . . H20A H 0.8860 0.3637 0.2404 0.062 Uiso 1 1 calc R . . H20B H 0.8033 0.3923 0.1364 0.062 Uiso 1 1 calc R . . H20C H 0.7189 0.3715 0.2425 0.062 Uiso 1 1 calc R . . C12 C 0.6288(3) 0.8114(3) 0.7737(2) 0.0372(6) Uani 1 1 d . . . C15 C 0.6600(4) 0.9314(4) 0.7829(3) 0.0581(10) Uani 1 1 d . . . H15A H 0.5780 1.0006 0.7593 0.087 Uiso 1 1 calc R . . H15B H 0.7429 0.9507 0.7409 0.087 Uiso 1 1 calc R . . H15C H 0.6793 0.9204 0.8544 0.087 Uiso 1 1 calc R . . C14 C 0.7568(4) 0.7014(4) 0.8060(2) 0.0569(10) Uani 1 1 d . . . H14A H 0.7339 0.6255 0.7989 0.085 Uiso 1 1 calc R . . H14B H 0.7799 0.6873 0.8774 0.085 Uiso 1 1 calc R . . H14C H 0.8382 0.7211 0.7625 0.085 Uiso 1 1 calc R . . C13 C 0.5022(4) 0.7771(4) 0.8417(2) 0.0594(10) Uani 1 1 d . . . H13A H 0.4184 0.8450 0.8202 0.089 Uiso 1 1 calc R . . H13B H 0.5239 0.7651 0.9130 0.089 Uiso 1 1 calc R . . H13C H 0.4835 0.6994 0.8353 0.089 Uiso 1 1 calc R . . C26 C 0.7059(4) 1.0121(3) 0.0284(2) 0.0409(7) Uani 1 1 d . . . H26 H 0.6469 0.9557 0.0300 0.049 Uiso 1 1 calc R . . C30 C 0.8869(4) 1.0673(3) 0.1049(2) 0.0425(7) Uani 1 1 d . . . H30 H 0.9530 1.0485 0.1582 0.051 Uiso 1 1 calc R . . C29 C 0.8772(5) 1.1770(3) 0.0231(3) 0.0591(11) Uani 1 1 d . . . H29 H 0.9354 1.2342 0.0210 0.071 Uiso 1 1 calc R . . C27 C 0.6988(5) 1.1205(3) -0.0530(2) 0.0545(10) Uani 1 1 d . . . H27 H 0.6353 1.1381 -0.1076 0.065 Uiso 1 1 calc R . . C28 C 0.7831(5) 1.2022(3) -0.0548(3) 0.0662(13) Uani 1 1 d . . . H28 H 0.7766 1.2770 -0.1103 0.079 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 0.02247(12) 0.03431(13) 0.04427(14) -0.01756(9) -0.00024(8) -0.00894(9) Cl1 0.0225(3) 0.0272(3) 0.0351(3) -0.0043(2) -0.0073(2) -0.0092(2) N2 0.0245(10) 0.0173(9) 0.0229(10) -0.0053(7) -0.0025(8) -0.0053(8) N3 0.0228(10) 0.0259(10) 0.0244(10) -0.0090(8) 0.0007(8) -0.0025(8) N1 0.0356(12) 0.0204(10) 0.0194(10) -0.0042(8) -0.0035(8) -0.0039(9) C9 0.0225(11) 0.0238(11) 0.0192(11) -0.0054(9) -0.0016(8) -0.0058(9) C8 0.0229(11) 0.0189(11) 0.0256(12) -0.0072(9) -0.0015(9) -0.0062(9) C5 0.0233(11) 0.0189(11) 0.0223(12) -0.0051(9) -0.0048(9) -0.0050(9) C1 0.0217(11) 0.0190(11) 0.0279(12) -0.0086(9) -0.0008(9) -0.0029(9) C6 0.0256(12) 0.0226(11) 0.0178(11) -0.0059(9) -0.0027(9) -0.0053(10) C2 0.0188(11) 0.0264(12) 0.0376(15) -0.0076(10) 0.0013(10) -0.0038(10) C3 0.0234(12) 0.0222(12) 0.0391(15) -0.0098(10) -0.0084(10) -0.0055(10) C10 0.0251(12) 0.0213(11) 0.0211(11) -0.0031(9) -0.0017(9) -0.0081(9) C11 0.0234(11) 0.0202(11) 0.0186(11) -0.0035(8) -0.0017(9) -0.0044(9) C7 0.0182(11) 0.0209(11) 0.0197(11) -0.0035(8) -0.0023(8) -0.0046(9) C4 0.0394(14) 0.0197(11) 0.0204(12) -0.0045(9) -0.0020(10) -0.0068(11) C18 0.0441(16) 0.0221(12) 0.0269(13) -0.0035(10) -0.0034(11) 0.0002(11) C16 0.0432(16) 0.0291(13) 0.0271(14) -0.0042(10) -0.0116(11) -0.0053(12) C19 0.0334(14) 0.0267(12) 0.0196(12) -0.0080(9) 0.0000(9) -0.0078(11) C24 0.0326(13) 0.0240(12) 0.0226(12) -0.0050(9) 0.0001(10) -0.0050(11) C22 0.0460(17) 0.0413(16) 0.0280(14) -0.0136(12) 0.0108(12) -0.0136(14) C17 0.0299(14) 0.0382(15) 0.0360(15) 0.0016(12) 0.0044(11) -0.0096(12) C25 0.0469(16) 0.0217(12) 0.0234(13) -0.0069(9) 0.0107(11) -0.0058(11) C21 0.0460(17) 0.0500(18) 0.0302(15) -0.0192(13) -0.0132(12) -0.0070(14) C20 0.074(2) 0.0304(14) 0.0246(14) -0.0135(11) -0.0013(13) -0.0133(15) C12 0.0367(15) 0.0482(17) 0.0222(13) -0.0128(12) -0.0026(11) 0.0038(13) C15 0.075(3) 0.068(2) 0.0408(19) -0.0324(17) -0.0144(17) -0.008(2) C14 0.052(2) 0.070(2) 0.0271(16) -0.0072(15) -0.0056(14) 0.0214(18) C13 0.051(2) 0.085(3) 0.0311(17) -0.0151(17) 0.0121(14) -0.0008(19) C26 0.067(2) 0.0275(14) 0.0244(14) -0.0058(11) -0.0013(13) -0.0048(14) C30 0.0535(19) 0.0374(16) 0.0377(16) -0.0099(12) 0.0174(14) -0.0194(15) C29 0.094(3) 0.0359(17) 0.051(2) -0.0127(15) 0.035(2) -0.0325(19) C27 0.097(3) 0.0301(16) 0.0254(15) -0.0032(12) 0.0008(16) 0.0006(17) C28 0.129(4) 0.0266(16) 0.0306(18) -0.0011(12) 0.028(2) -0.013(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 C1 2.098(2) . ? Ag1 Cl1 2.3710(6) . ? N2 C1 1.349(3) . ? N2 C3 1.366(3) . ? N2 C4 1.460(3) . ? N3 C1 1.359(3) . ? N3 C2 1.392(3) . ? N3 C12 1.490(3) . ? N1 C24 1.271(3) . ? N1 C10 1.430(3) . ? C9 C8 1.401(3) . ? C9 C10 1.407(3) . ? C9 C19 1.549(3) . ? C8 C7 1.393(3) . ? C8 H8 0.9500 . ? C5 C6 1.394(3) . ? C5 C10 1.398(3) . ? C5 C4 1.526(3) . ? C6 C7 1.381(3) . ? C6 H6 0.9500 . ? C2 C3 1.333(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C11 C18 1.529(3) . ? C11 C17 1.530(3) . ? C11 C16 1.538(3) . ? C11 C7 1.535(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C19 C20 1.527(4) . ? C19 C22 1.535(4) . ? C19 C21 1.539(4) . ? C24 C25 1.481(3) . ? C24 H24 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C25 C30 1.384(4) . ? C25 C26 1.389(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C12 C15 1.517(5) . ? C12 C14 1.534(4) . ? C12 C13 1.535(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C30 C29 1.395(4) . ? C30 H30 0.9500 . ? C29 C28 1.377(6) . ? C29 H29 0.9500 . ? C27 C28 1.369(6) . ? C27 H27 0.9500 . ? C28 H28 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 C1 Ag1 Cl1 162.92(7) . . ? C1 N2 C3 111.1(2) . . ? C1 N2 C4 123.8(2) . . ? C3 N2 C4 124.4(2) . . ? C1 N3 C2 109.7(2) . . ? C1 N3 C12 125.0(2) . . ? C2 N3 C12 125.2(2) . . ? C24 N1 C10 117.4(2) . . ? C8 C9 C10 117.2(2) . . ? C8 C9 C19 120.1(2) . . ? C10 C9 C19 122.7(2) . . ? C7 C8 C9 123.2(2) . . ? C7 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C6 C5 C10 119.3(2) . . ? C6 C5 C4 119.6(2) . . ? C10 C5 C4 121.1(2) . . ? N2 C1 N3 104.8(2) . . ? N2 C1 Ag1 125.78(17) . . ? N3 C1 Ag1 128.66(18) . . ? C7 C6 C5 122.0(2) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C3 C2 N3 107.0(2) . . ? C3 C2 H2 126.5 . . ? N3 C2 H2 126.5 . . ? C2 C3 N2 107.3(2) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C5 C10 C9 120.7(2) . . ? C5 C10 N1 119.0(2) . . ? C9 C10 N1 120.2(2) . . ? C18 C11 C17 109.3(2) . . ? C18 C11 C16 107.3(2) . . ? C17 C11 C16 109.6(2) . . ? C18 C11 C7 112.12(19) . . ? C17 C11 C7 108.43(19) . . ? C16 C11 C7 110.05(19) . . ? C6 C7 C8 117.5(2) . . ? C6 C7 C11 119.5(2) . . ? C8 C7 C11 122.9(2) . . ? N2 C4 C5 111.40(19) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C19 C22 106.9(2) . . ? C20 C19 C21 107.7(2) . . ? C22 C19 C21 110.0(2) . . ? C20 C19 C9 111.8(2) . . ? C22 C19 C9 111.1(2) . . ? C21 C19 C9 109.3(2) . . ? N1 C24 C25 122.1(2) . . ? N1 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C30 C25 C26 120.1(3) . . ? C30 C25 C24 118.6(3) . . ? C26 C25 C24 121.3(3) . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C12 C15 109.6(2) . . ? N3 C12 C14 108.2(2) . . ? C15 C12 C14 111.3(3) . . ? N3 C12 C13 109.0(3) . . ? C15 C12 C13 110.3(3) . . ? C14 C12 C13 108.4(3) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C27 C26 C25 119.8(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C25 C30 C29 119.4(3) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.7(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C9 C8 C7 1.6(3) . . . . ? C19 C9 C8 C7 -178.8(2) . . . . ? C3 N2 C1 N3 0.8(3) . . . . ? C4 N2 C1 N3 -170.23(19) . . . . ? C3 N2 C1 Ag1 -170.17(16) . . . . ? C4 N2 C1 Ag1 18.8(3) . . . . ? C2 N3 C1 N2 -1.1(3) . . . . ? C12 N3 C1 N2 176.0(2) . . . . ? C2 N3 C1 Ag1 169.46(17) . . . . ? C12 N3 C1 Ag1 -13.4(3) . . . . ? Cl1 Ag1 C1 N2 -177.89(12) . . . . ? Cl1 Ag1 C1 N3 13.3(4) . . . . ? C10 C5 C6 C7 -0.2(4) . . . . ? C4 C5 C6 C7 178.4(2) . . . . ? C1 N3 C2 C3 1.1(3) . . . . ? C12 N3 C2 C3 -176.0(2) . . . . ? N3 C2 C3 N2 -0.6(3) . . . . ? C1 N2 C3 C2 -0.1(3) . . . . ? C4 N2 C3 C2 170.8(2) . . . . ? C6 C5 C10 C9 3.6(3) . . . . ? C4 C5 C10 C9 -175.0(2) . . . . ? C6 C5 C10 N1 -179.4(2) . . . . ? C4 C5 C10 N1 2.0(3) . . . . ? C8 C9 C10 C5 -4.2(3) . . . . ? C19 C9 C10 C5 176.2(2) . . . . ? C8 C9 C10 N1 178.8(2) . . . . ? C19 C9 C10 N1 -0.8(4) . . . . ? C24 N1 C10 C5 63.4(3) . . . . ? C24 N1 C10 C9 -119.5(3) . . . . ? C5 C6 C7 C8 -2.4(3) . . . . ? C5 C6 C7 C11 -179.2(2) . . . . ? C9 C8 C7 C6 1.6(3) . . . . ? C9 C8 C7 C11 178.3(2) . . . . ? C18 C11 C7 C6 -163.7(2) . . . . ? C17 C11 C7 C6 75.6(3) . . . . ? C16 C11 C7 C6 -44.3(3) . . . . ? C18 C11 C7 C8 19.7(3) . . . . ? C17 C11 C7 C8 -101.0(3) . . . . ? C16 C11 C7 C8 139.1(2) . . . . ? C1 N2 C4 C5 95.7(3) . . . . ? C3 N2 C4 C5 -74.1(3) . . . . ? C6 C5 C4 N2 -21.3(3) . . . . ? C10 C5 C4 N2 157.2(2) . . . . ? C8 C9 C19 C20 0.8(3) . . . . ? C10 C9 C19 C20 -179.7(2) . . . . ? C8 C9 C19 C22 -118.6(3) . . . . ? C10 C9 C19 C22 60.9(3) . . . . ? C8 C9 C19 C21 119.8(3) . . . . ? C10 C9 C19 C21 -60.6(3) . . . . ? C10 N1 C24 C25 -178.9(2) . . . . ? N1 C24 C25 C30 171.4(3) . . . . ? N1 C24 C25 C26 -8.1(4) . . . . ? C1 N3 C12 C15 66.1(3) . . . . ? C2 N3 C12 C15 -117.2(3) . . . . ? C1 N3 C12 C14 -55.4(4) . . . . ? C2 N3 C12 C14 121.3(3) . . . . ? C1 N3 C12 C13 -173.1(3) . . . . ? C2 N3 C12 C13 3.6(4) . . . . ? C30 C25 C26 C27 -1.0(4) . . . . ? C24 C25 C26 C27 178.5(3) . . . . ? C26 C25 C30 C29 1.9(4) . . . . ? C24 C25 C30 C29 -177.7(3) . . . . ? C25 C30 C29 C28 -1.3(5) . . . . ? C25 C26 C27 C28 -0.4(5) . . . . ? C26 C27 C28 C29 1.0(6) . . . . ? C30 C29 C28 C27 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.682 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.176 data_11b _audit_creation_method SHELXL-97 _chemical_name_systematic ; a,a’-bis(3-mesityl-imidazol-2-ylidene)-o-xylene bis(silver bromide) ; _chemical_name_common 00skl036 _chemical_melting_point ? _chemical_formula_moiety 'C42 H44 Ag2 Cl2 N4' _chemical_formula_sum 'C32.50 H35 Ag2 Cl3 N4' _chemical_formula_weight 803.73 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.2853(3) _cell_length_b 12.7079(3) _cell_length_c 18.5879(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.4070(10) _cell_angle_gamma 90.0000(10) _cell_volume 3624.73(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51246 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 30.508 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8787 _exptl_absorpt_correction_T_max 0.9366 _exptl_absorpt_process_details ; SORTAV - multi-scan from symmetry-related measurements (Blessing, 1995-1997) ; _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 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method '\p and \q scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 35356 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1081 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 30.50 _reflns_number_total 9486 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1278P)^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 9486 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2093 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.005 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 Ag2 Ag 0.75713(4) 0.83276(5) 0.79553(3) 0.0669(2) Uani 1 1 d . . . Ag1 Ag 0.17093(4) 0.76188(4) 0.56683(3) 0.0596(2) Uani 1 1 d . . . Cl2 Cl 0.85763(10) 0.90273(13) 0.75288(9) 0.0498(4) Uani 1 1 d . . . Cl1 Cl 0.09236(13) 0.64421(14) 0.60526(13) 0.0665(5) Uani 1 1 d . . . N6 N 0.7468(4) 0.7323(4) 0.9398(3) 0.0547(14) Uani 1 1 d . . . C32 C 0.8379(5) 0.7512(6) 0.9857(4) 0.063(2) Uani 1 1 d . . . N1 N 0.2013(4) 0.9323(4) 0.4656(3) 0.0542(14) Uani 1 1 d . . . N3 N 0.6194(4) 0.7313(5) 0.8411(3) 0.0542(14) Uani 1 1 d . . . C9 C 0.5002(7) 1.0180(7) 0.8370(5) 0.080(2) Uani 1 1 d . . . H9 H 0.5258 1.0617 0.8837 0.096 Uiso 1 1 calc R . . C27 C 1.0129(6) 0.8093(9) 1.0752(5) 0.087(3) Uani 1 1 d . . . C29 C 0.9506(6) 0.8590(8) 1.0852(5) 0.089(3) Uani 1 1 d . . . H29 H 0.9687 0.9149 1.1235 0.107 Uiso 1 1 calc R . . C2 C 0.7026(5) 0.7622(5) 0.8634(4) 0.0597(19) Uani 1 1 d . . . C21 C 0.0752(5) 1.0389(5) 0.4423(4) 0.0542(17) Uani 1 1 d . . . C12 C 0.5438(5) 0.7558(6) 0.7657(4) 0.066(2) Uani 1 1 d . . . H12A H 0.5003 0.6989 0.7529 0.079 Uiso 1 1 calc R . . H12B H 0.5612 0.7575 0.7219 0.079 Uiso 1 1 calc R . . N2 N 0.3230(4) 0.8728(5) 0.5538(4) 0.0619(15) Uani 1 1 d . . . C4 C 0.3423(4) 0.9425(6) 0.5085(4) 0.0598(19) Uani 1 1 d . . . H4 H 0.3987 0.9590 0.5149 0.072 Uiso 1 1 calc R . . C10 C 0.5371(5) 0.9272(6) 0.8348(4) 0.065(2) Uani 1 1 d . . . H10 H 0.5894 0.9067 0.8806 0.078 Uiso 1 1 calc R . . C13 C 0.6135(6) 0.6802(6) 0.9050(5) 0.073(2) Uani 1 1 d . . . H13 H 0.5629 0.6509 0.9048 0.088 Uiso 1 1 calc R . . C20 C -0.0112(5) 1.0609(6) 0.3959(4) 0.0615(19) Uani 1 1 d . . . H20 H -0.0351 1.1196 0.4104 0.074 Uiso 1 1 calc R . . C3 C 0.2670(5) 0.9830(7) 0.4534(5) 0.069(2) Uani 1 1 d . . . H3 H 0.2592 1.0353 0.4141 0.083 Uiso 1 1 calc R . . C11 C 0.5014(4) 0.8604(5) 0.7669(4) 0.0556(17) Uani 1 1 d . . . C8 C 0.4227(7) 1.0483(7) 0.7692(6) 0.087(3) Uani 1 1 d . . . H8 H 0.3953 1.1126 0.7703 0.105 Uiso 1 1 calc R . . C16 C 0.0605(5) 0.8915(6) 0.3520(5) 0.0615(18) Uani 1 1 d . . . C15 C 0.0969(6) 0.7996(8) 0.3301(6) 0.095(3) Uani 1 1 d . . . H15A H 0.0520 0.7678 0.2804 0.143 Uiso 1 1 calc R . . H15B H 0.1170 0.7480 0.3742 0.143 Uiso 1 1 calc R . . H15C H 0.1462 0.8219 0.3213 0.143 Uiso 1 1 calc R . . C19 C -0.1601(5) 1.0268(8) 0.2836(5) 0.088(3) Uani 1 1 d . . . H19A H -0.1726 1.0891 0.3076 0.132 Uiso 1 1 calc R . . H19B H -0.1943 0.9670 0.2868 0.132 Uiso 1 1 calc R . . H19C H -0.1757 1.0409 0.2267 0.132 Uiso 1 1 calc R . . C24 C 0.8715(6) 0.6040(8) 0.9174(6) 0.093(3) Uani 1 1 d . . . H24A H 0.9234 0.5730 0.9172 0.139 Uiso 1 1 calc R . . H24B H 0.8315 0.6283 0.8627 0.139 Uiso 1 1 calc R . . H24C H 0.8424 0.5511 0.9347 0.139 Uiso 1 1 calc R . . C31 C 0.7945(7) 0.8980(8) 1.0583(6) 0.109(3) Uani 1 1 d . . . H31A H 0.7373 0.8673 1.0233 0.163 Uiso 1 1 calc R . . H31B H 0.7948 0.9721 1.0441 0.163 Uiso 1 1 calc R . . H31C H 0.8062 0.8927 1.1151 0.163 Uiso 1 1 calc R . . C14 C 0.6964(5) 0.6814(7) 0.9680(5) 0.070(2) Uani 1 1 d . . . H14 H 0.7151 0.6527 1.0206 0.083 Uiso 1 1 calc R . . C6 C 0.4255(5) 0.8910(6) 0.6976(5) 0.0616(19) Uani 1 1 d . . . C7 C 0.3855(6) 0.9846(6) 0.7000(5) 0.072(2) Uani 1 1 d . . . H7 H 0.3329 1.0055 0.6547 0.087 Uiso 1 1 calc R . . C23 C 0.1094(5) 0.9527(5) 0.4187(4) 0.0544(17) Uani 1 1 d . . . C18 C -0.0660(5) 1.0015(6) 0.3285(5) 0.064(2) Uani 1 1 d . . . C30 C 0.8647(7) 0.8384(6) 1.0468(5) 0.075(2) Uani 1 1 d . . . C1 C 0.2371(5) 0.8629(5) 0.5278(4) 0.0516(16) Uani 1 1 d . . . C26 C 0.9874(6) 0.7244(8) 1.0202(5) 0.077(2) Uani 1 1 d . . . H26 H 1.0302 0.6856 1.0130 0.092 Uiso 1 1 calc R . . C17 C -0.0289(5) 0.9183(7) 0.3094(5) 0.072(2) Uani 1 1 d . . . H17 H -0.0655 0.8756 0.2646 0.086 Uiso 1 1 calc R . . C5 C 0.3879(5) 0.8213(6) 0.6268(4) 0.0589(18) Uani 1 1 d . . . H5A H 0.4354 0.7942 0.6162 0.071 Uiso 1 1 calc R . . H5B H 0.3605 0.7603 0.6393 0.071 Uiso 1 1 calc R . . C25 C 0.8985(5) 0.6967(7) 0.9756(4) 0.0640(19) Uani 1 1 d . . . C22 C 0.1298(6) 1.1057(7) 0.5120(5) 0.081(2) Uani 1 1 d . . . H22A H 0.0941 1.1618 0.5176 0.121 Uiso 1 1 calc R . . H22B H 0.1768 1.1368 0.5035 0.121 Uiso 1 1 calc R . . H22C H 0.1549 1.0629 0.5614 0.121 Uiso 1 1 calc R . . C28 C 1.1066(7) 0.8383(11) 1.1195(6) 0.137(5) Uani 1 1 d . . . H28A H 1.1138 0.8983 1.1552 0.205 Uiso 1 1 calc R . . H28B H 1.1277 0.8575 1.0805 0.205 Uiso 1 1 calc R . . H28C H 1.1402 0.7783 1.1520 0.205 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 Ag2 0.0702(4) 0.0744(4) 0.0647(4) 0.0149(3) 0.0384(3) 0.0078(3) Ag1 0.0608(4) 0.0575(4) 0.0718(4) 0.0094(3) 0.0401(3) 0.0046(3) Cl2 0.0431(9) 0.0660(10) 0.0516(9) 0.0198(8) 0.0316(8) 0.0052(8) Cl1 0.0719(12) 0.0572(11) 0.0978(14) 0.0087(9) 0.0624(12) 0.0022(9) N6 0.050(3) 0.068(4) 0.043(3) 0.015(3) 0.019(3) 0.006(3) C32 0.064(5) 0.075(5) 0.049(4) 0.010(4) 0.024(4) -0.004(4) N1 0.052(3) 0.052(3) 0.063(4) 0.005(3) 0.030(3) -0.001(3) N3 0.043(3) 0.073(4) 0.051(3) 0.002(3) 0.025(3) 0.003(3) C9 0.110(7) 0.063(5) 0.078(6) -0.003(4) 0.052(6) -0.003(5) C27 0.052(5) 0.140(9) 0.054(5) 0.004(5) 0.012(4) -0.015(6) C29 0.070(6) 0.122(8) 0.061(5) -0.028(5) 0.018(5) -0.041(6) C2 0.070(5) 0.054(4) 0.052(4) -0.001(3) 0.025(4) 0.008(4) C21 0.060(5) 0.051(4) 0.049(4) 0.011(3) 0.023(4) 0.010(3) C12 0.054(5) 0.081(5) 0.063(5) 0.001(4) 0.026(4) 0.003(4) N2 0.040(3) 0.076(4) 0.071(4) 0.012(3) 0.026(3) 0.005(3) C4 0.041(4) 0.085(5) 0.048(4) 0.005(4) 0.016(3) -0.006(4) C10 0.069(5) 0.074(5) 0.056(4) 0.004(4) 0.031(4) 0.009(4) C13 0.066(5) 0.084(6) 0.075(5) 0.005(4) 0.039(5) 0.008(4) C20 0.070(5) 0.055(4) 0.067(5) 0.011(4) 0.038(4) 0.015(4) C3 0.066(5) 0.083(6) 0.067(5) 0.006(4) 0.039(4) -0.015(4) C11 0.046(4) 0.056(4) 0.066(5) 0.006(4) 0.027(4) 0.004(3) C8 0.126(8) 0.058(5) 0.102(7) -0.002(5) 0.074(7) 0.018(5) C16 0.055(5) 0.058(4) 0.070(5) -0.010(4) 0.028(4) -0.005(4) C15 0.088(7) 0.094(7) 0.105(7) -0.036(6) 0.046(6) 0.002(6) C19 0.056(5) 0.109(7) 0.079(6) 0.017(5) 0.014(4) 0.016(5) C24 0.073(6) 0.101(7) 0.104(7) -0.018(6) 0.041(5) 0.013(5) C31 0.125(9) 0.091(7) 0.093(7) -0.031(6) 0.035(6) -0.006(6) C14 0.070(5) 0.091(6) 0.059(5) 0.011(4) 0.039(4) 0.010(5) C6 0.074(5) 0.059(5) 0.073(5) 0.004(4) 0.052(4) -0.002(4) C7 0.084(6) 0.056(5) 0.084(6) 0.020(4) 0.045(5) 0.022(4) C23 0.055(4) 0.056(4) 0.055(4) 0.015(3) 0.027(4) 0.006(3) C18 0.071(5) 0.064(5) 0.067(5) 0.017(4) 0.040(4) 0.015(4) C30 0.108(7) 0.064(5) 0.059(5) -0.003(4) 0.044(5) -0.002(5) C1 0.059(5) 0.051(4) 0.049(4) 0.013(3) 0.028(3) 0.012(3) C26 0.060(5) 0.108(7) 0.061(5) 0.008(5) 0.026(4) -0.002(5) C17 0.060(5) 0.088(6) 0.058(5) 0.003(4) 0.020(4) -0.010(4) C5 0.057(4) 0.066(5) 0.059(4) 0.000(4) 0.031(4) 0.003(4) C25 0.054(5) 0.083(5) 0.054(4) 0.008(4) 0.024(4) 0.001(4) C22 0.089(6) 0.073(5) 0.075(5) -0.008(4) 0.034(5) 0.010(5) C28 0.095(8) 0.241(16) 0.066(6) -0.038(7) 0.030(6) -0.062(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 C2 2.092(8) . ? Ag2 Cl2 2.3886(15) . ? Ag1 C1 2.061(7) . ? Ag1 Cl1 2.3419(18) . ? N6 C2 1.321(8) . ? N6 C14 1.368(9) . ? N6 C32 1.424(9) . ? C32 C25 1.339(11) . ? C32 C30 1.500(11) . ? N1 C1 1.355(8) . ? N1 C3 1.412(9) . ? N1 C23 1.442(8) . ? N3 C2 1.360(9) . ? N3 C13 1.397(9) . ? N3 C12 1.443(9) . ? C9 C10 1.328(10) . ? C9 C8 1.407(12) . ? C9 H9 0.9500 . ? C27 C29 1.333(13) . ? C27 C26 1.411(13) . ? C27 C28 1.487(12) . ? C29 C30 1.343(12) . ? C29 H29 0.9500 . ? C21 C20 1.366(9) . ? C21 C23 1.407(9) . ? C21 C22 1.472(10) . ? C12 C11 1.523(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N2 C1 1.339(8) . ? N2 C4 1.365(9) . ? N2 C5 1.458(9) . ? C4 C3 1.334(10) . ? C4 H4 0.9500 . ? C10 C11 1.407(10) . ? C10 H10 0.9500 . ? C13 C14 1.371(11) . ? C13 H13 0.9500 . ? C20 C18 1.394(10) . ? C20 H20 0.9500 . ? C3 H3 0.9500 . ? C11 C6 1.405(10) . ? C8 C7 1.400(12) . ? C8 H8 0.9500 . ? C16 C23 1.375(10) . ? C16 C17 1.415(10) . ? C16 C15 1.470(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 C18 1.481(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C24 C25 1.520(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 C30 1.528(13) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C14 H14 0.9500 . ? C6 C7 1.386(10) . ? C6 C5 1.467(10) . ? C7 H7 0.9500 . ? C18 C17 1.367(11) . ? C26 C25 1.414(11) . ? C26 H26 0.9500 . ? C17 H17 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 C2 Ag2 Cl2 163.3(2) . . ? C1 Ag1 Cl1 177.4(2) . . ? C2 N6 C14 113.1(7) . . ? C2 N6 C32 121.8(6) . . ? C14 N6 C32 125.0(6) . . ? C25 C32 N6 123.4(7) . . ? C25 C32 C30 119.9(8) . . ? N6 C32 C30 116.7(7) . . ? C1 N1 C3 110.4(6) . . ? C1 N1 C23 125.2(5) . . ? C3 N1 C23 124.3(6) . . ? C2 N3 C13 110.9(6) . . ? C2 N3 C12 126.2(6) . . ? C13 N3 C12 122.6(6) . . ? C10 C9 C8 118.9(8) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C29 C27 C26 117.4(8) . . ? C29 C27 C28 123.4(10) . . ? C26 C27 C28 119.2(10) . . ? C27 C29 C30 126.8(9) . . ? C27 C29 H29 116.6 . . ? C30 C29 H29 116.6 . . ? N6 C2 N3 104.5(6) . . ? N6 C2 Ag2 125.0(6) . . ? N3 C2 Ag2 130.4(5) . . ? C20 C21 C23 117.1(7) . . ? C20 C21 C22 120.6(7) . . ? C23 C21 C22 122.2(7) . . ? N3 C12 C11 113.6(6) . . ? N3 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? N3 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C1 N2 C4 112.5(6) . . ? C1 N2 C5 123.0(6) . . ? C4 N2 C5 124.3(6) . . ? C3 C4 N2 107.2(6) . . ? C3 C4 H4 126.4 . . ? N2 C4 H4 126.4 . . ? C9 C10 C11 122.3(8) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C14 C13 N3 105.3(7) . . ? C14 C13 H13 127.3 . . ? N3 C13 H13 127.3 . . ? C21 C20 C18 123.4(7) . . ? C21 C20 H20 118.3 . . ? C18 C20 H20 118.3 . . ? C4 C3 N1 105.8(6) . . ? C4 C3 H3 127.1 . . ? N1 C3 H3 127.1 . . ? C6 C11 C10 119.6(7) . . ? C6 C11 C12 118.8(6) . . ? C10 C11 C12 121.6(6) . . ? C7 C8 C9 120.6(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C23 C16 C17 115.4(7) . . ? C23 C16 C15 122.3(7) . . ? C17 C16 C15 122.2(7) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C14 C13 106.1(7) . . ? N6 C14 H14 126.9 . . ? C13 C14 H14 126.9 . . ? C7 C6 C11 118.5(7) . . ? C7 C6 C5 121.7(7) . . ? C11 C6 C5 119.7(7) . . ? C6 C7 C8 120.1(8) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C16 C23 C21 123.3(7) . . ? C16 C23 N1 119.5(6) . . ? C21 C23 N1 117.1(6) . . ? C17 C18 C20 116.5(7) . . ? C17 C18 C19 123.1(8) . . ? C20 C18 C19 120.3(7) . . ? C29 C30 C32 115.4(8) . . ? C29 C30 C31 125.7(8) . . ? C32 C30 C31 118.9(8) . . ? N2 C1 N1 104.0(6) . . ? N2 C1 Ag1 129.3(5) . . ? N1 C1 Ag1 126.6(5) . . ? C27 C26 C25 120.6(9) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C18 C17 C16 124.2(8) . . ? C18 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? N2 C5 C6 113.4(6) . . ? N2 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C32 C25 C26 119.9(8) . . ? C32 C25 C24 119.8(7) . . ? C26 C25 C24 120.3(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C2 N6 C32 C25 -74.5(10) . . . . ? C14 N6 C32 C25 104.4(9) . . . . ? C2 N6 C32 C30 104.4(8) . . . . ? C14 N6 C32 C30 -76.7(9) . . . . ? C26 C27 C29 C30 -1.6(16) . . . . ? C28 C27 C29 C30 179.0(10) . . . . ? C14 N6 C2 N3 1.2(8) . . . . ? C32 N6 C2 N3 -179.7(6) . . . . ? C14 N6 C2 Ag2 -175.5(5) . . . . ? C32 N6 C2 Ag2 3.5(9) . . . . ? C13 N3 C2 N6 -1.0(8) . . . . ? C12 N3 C2 N6 172.8(6) . . . . ? C13 N3 C2 Ag2 175.5(5) . . . . ? C12 N3 C2 Ag2 -10.6(11) . . . . ? Cl2 Ag2 C2 N6 5.3(11) . . . . ? Cl2 Ag2 C2 N3 -170.6(4) . . . . ? C2 N3 C12 C11 -86.6(8) . . . . ? C13 N3 C12 C11 86.5(8) . . . . ? C1 N2 C4 C3 2.9(9) . . . . ? C5 N2 C4 C3 -172.1(7) . . . . ? C8 C9 C10 C11 0.1(13) . . . . ? C2 N3 C13 C14 0.5(8) . . . . ? C12 N3 C13 C14 -173.6(7) . . . . ? C23 C21 C20 C18 1.2(10) . . . . ? C22 C21 C20 C18 179.2(7) . . . . ? N2 C4 C3 N1 -2.0(8) . . . . ? C1 N1 C3 C4 0.5(8) . . . . ? C23 N1 C3 C4 -180.0(6) . . . . ? C9 C10 C11 C6 1.9(11) . . . . ? C9 C10 C11 C12 -179.2(7) . . . . ? N3 C12 C11 C6 -177.9(6) . . . . ? N3 C12 C11 C10 3.2(10) . . . . ? C10 C9 C8 C7 -0.8(13) . . . . ? C2 N6 C14 C13 -1.0(9) . . . . ? C32 N6 C14 C13 -179.9(7) . . . . ? N3 C13 C14 N6 0.3(8) . . . . ? C10 C11 C6 C7 -3.1(10) . . . . ? C12 C11 C6 C7 177.9(7) . . . . ? C10 C11 C6 C5 -179.8(7) . . . . ? C12 C11 C6 C5 1.2(10) . . . . ? C11 C6 C7 C8 2.4(11) . . . . ? C5 C6 C7 C8 179.1(7) . . . . ? C9 C8 C7 C6 -0.5(13) . . . . ? C17 C16 C23 C21 -2.5(11) . . . . ? C15 C16 C23 C21 -177.8(8) . . . . ? C17 C16 C23 N1 -179.4(6) . . . . ? C15 C16 C23 N1 5.2(11) . . . . ? C20 C21 C23 C16 0.5(10) . . . . ? C22 C21 C23 C16 -177.5(7) . . . . ? C20 C21 C23 N1 177.5(6) . . . . ? C22 C21 C23 N1 -0.5(10) . . . . ? C1 N1 C23 C16 -87.2(8) . . . . ? C3 N1 C23 C16 93.3(8) . . . . ? C1 N1 C23 C21 95.6(8) . . . . ? C3 N1 C23 C21 -83.9(8) . . . . ? C21 C20 C18 C17 -0.6(11) . . . . ? C21 C20 C18 C19 176.9(7) . . . . ? C27 C29 C30 C32 -1.0(14) . . . . ? C27 C29 C30 C31 -178.9(10) . . . . ? C25 C32 C30 C29 3.2(11) . . . . ? N6 C32 C30 C29 -175.7(7) . . . . ? C25 C32 C30 C31 -178.8(8) . . . . ? N6 C32 C30 C31 2.3(10) . . . . ? C4 N2 C1 N1 -2.5(8) . . . . ? C5 N2 C1 N1 172.6(6) . . . . ? C4 N2 C1 Ag1 174.7(5) . . . . ? C5 N2 C1 Ag1 -10.2(10) . . . . ? C3 N1 C1 N2 1.2(7) . . . . ? C23 N1 C1 N2 -178.4(6) . . . . ? C3 N1 C1 Ag1 -176.2(5) . . . . ? C23 N1 C1 Ag1 4.3(9) . . . . ? Cl1 Ag1 C1 N2 -122(4) . . . . ? Cl1 Ag1 C1 N1 54(5) . . . . ? C29 C27 C26 C25 2.3(13) . . . . ? C28 C27 C26 C25 -178.4(9) . . . . ? C20 C18 C17 C16 -1.7(11) . . . . ? C19 C18 C17 C16 -179.1(7) . . . . ? C23 C16 C17 C18 3.2(11) . . . . ? C15 C16 C17 C18 178.5(9) . . . . ? C1 N2 C5 C6 -99.3(8) . . . . ? C4 N2 C5 C6 75.2(9) . . . . ? C7 C6 C5 N2 17.3(10) . . . . ? C11 C6 C5 N2 -166.1(6) . . . . ? N6 C32 C25 C26 176.2(7) . . . . ? C30 C32 C25 C26 -2.6(11) . . . . ? N6 C32 C25 C24 -4.9(12) . . . . ? C30 C32 C25 C24 176.3(7) . . . . ? C27 C26 C25 C32 -0.1(12) . . . . ? C27 C26 C25 C24 -179.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 1.982 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.172