# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Ag Cl N8 O4' _chemical_formula_sum 'C44 H40 Ag Cl N8 O4' _chemical_formula_weight 888.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.556(5) _cell_length_b 11.468(5) _cell_length_c 22.267(5) _cell_angle_alpha 93.896(5) _cell_angle_beta 98.182(5) _cell_angle_gamma 100.288(5) _cell_volume 2365.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8575 _exptl_absorpt_correction_T_max 0.9016 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16709 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8225 _reflns_number_gt 3678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8225 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1734 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2455 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.99444(7) 0.26130(5) 0.49367(3) 0.0721(3) Uani 1 1 d . . . C1 C 1.5920(9) -0.6987(9) 0.9014(4) 0.081(3) Uani 1 1 d . . . C2 C 1.5511(9) -0.6039(7) 0.8682(4) 0.071(2) Uani 1 1 d . . . C3 C 1.6584(10) -0.5397(10) 0.8399(5) 0.102(4) Uani 1 1 d . . . C4 C 1.4150(8) -0.5818(6) 0.8623(3) 0.0543(19) Uani 1 1 d . . . C5 C 1.3020(8) -0.6531(6) 0.8915(3) 0.057(2) Uani 1 1 d . . . H5A H 1.3474 -0.6791 0.9287 0.068 Uiso 1 1 calc R . . H5B H 1.2567 -0.7236 0.8643 0.068 Uiso 1 1 calc R . . C6 C 1.1882(8) -0.5864(6) 0.9064(3) 0.055(2) Uani 1 1 d . . . C7 C 1.2496(10) -0.4909(7) 0.9581(3) 0.079(3) Uani 1 1 d . . . H7A H 1.3012 -0.5244 0.9908 0.119 Uiso 1 1 calc R . . H7B H 1.1727 -0.4593 0.9726 0.119 Uiso 1 1 calc R . . H7C H 1.3140 -0.4283 0.9440 0.119 Uiso 1 1 calc R . . C8 C 1.0654(9) -0.6723(8) 0.9266(5) 0.101(3) Uani 1 1 d . . . H8A H 0.9946 -0.6288 0.9380 0.151 Uiso 1 1 calc R . . H8B H 1.1029 -0.7101 0.9608 0.151 Uiso 1 1 calc R . . H8C H 1.0216 -0.7316 0.8935 0.151 Uiso 1 1 calc R . . C9 C 1.1272(8) -0.5349(7) 0.8498(3) 0.062(2) Uani 1 1 d . . . H9A H 1.0657 -0.5990 0.8224 0.075 Uiso 1 1 calc R . . H9B H 1.0674 -0.4798 0.8614 0.075 Uiso 1 1 calc R . . C10 C 1.2383(8) -0.4714(6) 0.8163(3) 0.0519(19) Uani 1 1 d . . . C11 C 1.3728(8) -0.4943(7) 0.8253(3) 0.062(2) Uani 1 1 d . . . H11 H 1.4420 -0.4502 0.8062 0.074 Uiso 1 1 calc R . . C12 C 1.2012(9) -0.3853(6) 0.7743(3) 0.060(2) Uani 1 1 d . . . H12 H 1.2757 -0.3450 0.7565 0.072 Uiso 1 1 calc R . . C13 C 1.0728(9) -0.3586(6) 0.7591(3) 0.061(2) Uani 1 1 d . . . H13 H 0.9984 -0.3995 0.7767 0.073 Uiso 1 1 calc R . . C14 C 1.0353(8) -0.2726(7) 0.7180(3) 0.058(2) Uani 1 1 d . . . C15 C 0.8942(8) -0.2559(8) 0.7079(4) 0.076(3) Uani 1 1 d . . . H15 H 0.8262 -0.2992 0.7280 0.091 Uiso 1 1 calc R . . C16 C 0.8527(9) -0.1755(8) 0.6684(4) 0.082(3) Uani 1 1 d . . . H16 H 0.7576 -0.1650 0.6622 0.098 Uiso 1 1 calc R . . C17 C 0.9531(9) -0.1108(6) 0.6381(3) 0.056(2) Uani 1 1 d . . . C18 C 1.0908(8) -0.1257(7) 0.6478(3) 0.061(2) Uani 1 1 d . . . H18 H 1.1580 -0.0823 0.6275 0.074 Uiso 1 1 calc R . . C19 C 1.1333(8) -0.2039(6) 0.6872(3) 0.062(2) Uani 1 1 d . . . H19 H 1.2294 -0.2116 0.6936 0.075 Uiso 1 1 calc R . . C20 C 0.7704(9) -0.0300(8) 0.5683(4) 0.096(3) Uani 1 1 d . . . H20 H 0.6885 -0.0849 0.5720 0.115 Uiso 1 1 calc R . . C21 C 0.7742(9) 0.0599(8) 0.5346(4) 0.095(3) Uani 1 1 d . . . H21 H 0.6948 0.0806 0.5116 0.114 Uiso 1 1 calc R . . C22 C 0.9890(9) 0.0616(6) 0.5768(3) 0.058(2) Uani 1 1 d . . . H22 H 1.0883 0.0827 0.5882 0.070 Uiso 1 1 calc R . . C23 C 1.2187(11) 0.4531(10) 0.4514(5) 0.119(4) Uani 1 1 d . . . H23 H 1.2952 0.4276 0.4739 0.142 Uiso 1 1 calc R . . C24 C 1.2300(10) 0.5432(9) 0.4158(5) 0.113(4) Uani 1 1 d . . . H24 H 1.3149 0.5902 0.4088 0.136 Uiso 1 1 calc R . . C25 C 1.0080(9) 0.4660(7) 0.4124(3) 0.062(2) Uani 1 1 d . . . H25 H 0.9083 0.4485 0.4022 0.075 Uiso 1 1 calc R . . C26 C 1.0489(8) 0.6368(6) 0.3508(3) 0.058(2) Uani 1 1 d . . . C27 C 1.1525(8) 0.7115(8) 0.3268(4) 0.080(3) Uani 1 1 d . . . H27 H 1.2491 0.7074 0.3372 0.096 Uiso 1 1 calc R . . C28 C 1.1132(8) 0.7924(7) 0.2874(4) 0.079(3) Uani 1 1 d . . . H28 H 1.1833 0.8395 0.2699 0.094 Uiso 1 1 calc R . . C29 C 0.9707(9) 0.8043(6) 0.2735(3) 0.058(2) Uani 1 1 d . . . C30 C 0.8689(8) 0.7278(7) 0.2988(3) 0.067(2) Uani 1 1 d . . . H30 H 0.7724 0.7333 0.2897 0.081 Uiso 1 1 calc R . . C31 C 0.9064(9) 0.6435(7) 0.3372(4) 0.069(2) Uani 1 1 d . . . H31 H 0.8364 0.5931 0.3532 0.083 Uiso 1 1 calc R . . C32 C 0.9323(9) 0.8902(6) 0.2327(3) 0.061(2) Uani 1 1 d . . . H32 H 1.0058 0.9297 0.2142 0.073 Uiso 1 1 calc R . . C33 C 0.8039(9) 0.9190(7) 0.2187(3) 0.062(2) Uani 1 1 d . . . H33 H 0.7312 0.8828 0.2387 0.074 Uiso 1 1 calc R . . C34 C 0.7658(9) 1.0000(6) 0.1760(3) 0.059(2) Uani 1 1 d . . . C35 C 0.8718(8) 1.0566(7) 0.1378(3) 0.064(2) Uani 1 1 d . . . H35A H 0.9326 1.0005 0.1287 0.077 Uiso 1 1 calc R . . H35B H 0.9332 1.1256 0.1616 0.077 Uiso 1 1 calc R . . C36 C 0.8046(8) 1.0952(7) 0.0782(3) 0.056(2) Uani 1 1 d . . . C37 C 0.7364(10) 0.9907(7) 0.0330(3) 0.077(3) Uani 1 1 d . . . H37A H 0.8097 0.9513 0.0208 0.116 Uiso 1 1 calc R . . H37B H 0.6852 1.0177 -0.0020 0.116 Uiso 1 1 calc R . . H37C H 0.6705 0.9363 0.0514 0.116 Uiso 1 1 calc R . . C38 C 0.9200(9) 1.1721(8) 0.0502(4) 0.091(3) Uani 1 1 d . . . H38A H 0.9726 1.2348 0.0801 0.136 Uiso 1 1 calc R . . H38B H 0.8756 1.2060 0.0159 0.136 Uiso 1 1 calc R . . H38C H 0.9847 1.1242 0.0371 0.136 Uiso 1 1 calc R . . C39 C 0.6919(8) 1.1681(6) 0.0928(3) 0.059(2) Uani 1 1 d . . . H39A H 0.7411 1.2428 0.1154 0.071 Uiso 1 1 calc R . . H39B H 0.6408 1.1864 0.0548 0.071 Uiso 1 1 calc R . . C40 C 0.5847(7) 1.1073(6) 0.1287(3) 0.0472(18) Uani 1 1 d . . . C41 C 0.6320(8) 1.0270(6) 0.1686(3) 0.057(2) Uani 1 1 d . . . H41 H 0.5664 0.9896 0.1916 0.068 Uiso 1 1 calc R . . C42 C 0.4512(9) 1.1328(8) 0.1252(3) 0.067(2) Uani 1 1 d . . . C43 C 0.3451(10) 1.0747(10) 0.1584(5) 0.092(3) Uani 1 1 d . . . C44 C 0.4057(9) 1.2200(8) 0.0878(4) 0.070(2) Uani 1 1 d . . . Cl1 Cl 0.4038(4) 0.2139(5) 0.5925(2) 0.0779(13) Uani 0.50 1 d P . . Cl2 Cl 0.4131(4) 0.7051(5) 0.5920(2) 0.0726(12) Uani 0.50 1 d P . . N1 N 1.6274(9) -0.7740(8) 0.9269(4) 0.108(3) Uani 1 1 d . . . N2 N 1.7474(10) -0.4858(10) 0.8183(5) 0.140(4) Uani 1 1 d . . . N3 N 0.9064(6) -0.0293(5) 0.5967(3) 0.0563(16) Uani 1 1 d . . . N4 N 0.9121(7) 0.1177(6) 0.5390(3) 0.0679(18) Uani 1 1 d . . . N5 N 1.0814(8) 0.4067(5) 0.4491(3) 0.0654(18) Uani 1 1 d . . . N6 N 1.0906(7) 0.5529(5) 0.3914(3) 0.0657(18) Uani 1 1 d . . . N7 N 0.2673(11) 1.0297(10) 0.1861(5) 0.139(4) Uani 1 1 d . . . N8 N 0.3683(9) 1.2892(7) 0.0586(4) 0.101(3) Uani 1 1 d . . . O1 O 0.2870(16) 0.2488(14) 0.5537(7) 0.124(5) Uani 0.50 1 d P . . O2 O 0.5120(16) 0.1913(14) 0.5577(7) 0.125(5) Uani 0.50 1 d P . . O3 O 0.4618(12) 0.3103(11) 0.6400(6) 0.092(4) Uani 0.50 1 d P . . O4 O 0.3497(16) 0.1085(11) 0.6194(6) 0.115(5) Uani 0.50 1 d P . . O5 O 0.5172(16) 0.6856(14) 0.5597(7) 0.120(5) Uani 0.50 1 d P . . O6 O 0.2996(18) 0.7319(16) 0.5547(8) 0.147(6) Uani 0.50 1 d P . . O7 O 0.4657(15) 0.8008(14) 0.6347(8) 0.123(5) Uani 0.50 1 d P . . O8 O 0.3661(17) 0.6073(13) 0.6195(7) 0.127(5) Uani 0.50 1 d P . . 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 0.0819(5) 0.0625(5) 0.0758(5) 0.0248(3) 0.0184(4) 0.0126(3) C1 0.072(6) 0.087(7) 0.084(7) 0.010(6) 0.005(5) 0.021(5) C2 0.055(6) 0.079(6) 0.081(6) 0.027(5) 0.009(4) 0.014(5) C3 0.042(6) 0.140(10) 0.138(9) 0.049(8) 0.038(6) 0.019(6) C4 0.048(5) 0.055(5) 0.057(5) 0.005(4) 0.008(4) 0.003(4) C5 0.066(5) 0.043(4) 0.062(5) 0.010(4) 0.013(4) 0.008(4) C6 0.054(5) 0.052(5) 0.068(5) 0.025(4) 0.023(4) 0.016(4) C7 0.116(8) 0.073(6) 0.056(5) 0.011(5) 0.014(5) 0.036(6) C8 0.074(6) 0.106(7) 0.148(9) 0.078(7) 0.055(6) 0.030(6) C9 0.066(5) 0.061(5) 0.067(5) 0.021(4) 0.024(4) 0.014(4) C10 0.067(5) 0.050(4) 0.039(4) 0.005(4) 0.011(4) 0.010(4) C11 0.055(5) 0.066(5) 0.068(5) 0.020(4) 0.018(4) 0.013(4) C12 0.068(6) 0.059(5) 0.053(5) 0.009(4) 0.015(4) 0.008(4) C13 0.080(6) 0.061(5) 0.045(4) 0.012(4) 0.010(4) 0.019(4) C14 0.058(5) 0.065(5) 0.049(4) 0.012(4) 0.008(4) 0.008(4) C15 0.048(5) 0.102(7) 0.085(6) 0.044(5) 0.015(4) 0.017(5) C16 0.056(5) 0.097(7) 0.101(7) 0.052(6) 0.015(5) 0.019(5) C17 0.073(6) 0.050(5) 0.043(4) 0.008(4) 0.000(4) 0.010(4) C18 0.050(5) 0.075(5) 0.061(5) 0.023(4) 0.009(4) 0.009(4) C19 0.063(5) 0.063(5) 0.060(5) 0.015(4) 0.003(4) 0.011(4) C20 0.059(6) 0.102(7) 0.117(7) 0.069(6) -0.013(5) -0.011(5) C21 0.059(6) 0.103(7) 0.115(8) 0.068(6) -0.013(5) -0.009(5) C22 0.065(5) 0.052(5) 0.057(5) 0.015(4) 0.011(4) 0.003(4) C23 0.079(7) 0.123(9) 0.144(9) 0.086(8) -0.016(6) -0.007(6) C24 0.060(6) 0.129(8) 0.144(9) 0.102(7) -0.013(6) -0.011(6) C25 0.058(5) 0.059(5) 0.069(5) 0.018(4) 0.005(4) 0.008(4) C26 0.061(6) 0.050(5) 0.055(5) 0.015(4) -0.004(4) -0.001(4) C27 0.045(5) 0.091(6) 0.111(7) 0.040(6) 0.021(5) 0.012(5) C28 0.046(5) 0.088(6) 0.105(7) 0.055(6) 0.016(4) 0.004(4) C29 0.070(6) 0.053(5) 0.051(4) 0.016(4) 0.009(4) 0.004(4) C30 0.052(5) 0.066(5) 0.077(6) 0.014(5) 0.002(4) -0.002(4) C31 0.062(6) 0.065(5) 0.077(6) 0.026(5) 0.010(4) -0.002(4) C32 0.070(6) 0.058(5) 0.053(5) 0.012(4) 0.011(4) 0.007(4) C33 0.067(6) 0.071(5) 0.049(5) 0.014(4) 0.015(4) 0.011(4) C34 0.068(6) 0.054(5) 0.055(5) 0.007(4) 0.013(4) 0.008(4) C35 0.066(5) 0.064(5) 0.066(5) 0.020(4) 0.017(4) 0.015(4) C36 0.055(5) 0.057(5) 0.059(5) 0.020(4) 0.015(4) 0.012(4) C37 0.114(8) 0.075(6) 0.048(5) 0.005(5) 0.014(5) 0.033(6) C38 0.085(7) 0.092(7) 0.112(7) 0.056(6) 0.046(5) 0.022(5) C39 0.065(5) 0.052(5) 0.062(5) 0.015(4) 0.016(4) 0.009(4) C40 0.048(5) 0.050(4) 0.041(4) 0.004(4) 0.007(3) 0.003(4) C41 0.059(5) 0.053(5) 0.062(5) 0.010(4) 0.022(4) 0.011(4) C42 0.057(5) 0.081(6) 0.062(5) 0.010(5) 0.004(4) 0.014(5) C43 0.060(6) 0.120(8) 0.108(8) 0.042(7) 0.035(6) 0.019(6) C44 0.062(6) 0.075(6) 0.067(6) 0.003(5) 0.006(4) 0.006(5) Cl1 0.044(3) 0.091(4) 0.095(3) 0.018(3) 0.015(2) -0.002(2) Cl2 0.039(2) 0.087(3) 0.094(3) 0.008(3) 0.024(2) 0.007(2) N1 0.118(7) 0.095(6) 0.117(7) 0.028(5) 0.002(5) 0.042(6) N2 0.073(6) 0.182(10) 0.188(10) 0.063(8) 0.054(6) 0.041(7) N3 0.054(4) 0.059(4) 0.055(4) 0.013(3) 0.006(3) 0.006(3) N4 0.072(5) 0.066(4) 0.066(4) 0.020(4) 0.009(4) 0.012(4) N5 0.071(5) 0.056(4) 0.063(4) 0.007(4) 0.002(4) 0.004(4) N6 0.057(4) 0.059(4) 0.074(4) 0.015(4) 0.005(3) -0.005(3) N7 0.096(7) 0.184(11) 0.161(9) 0.068(8) 0.057(7) 0.040(7) N8 0.103(6) 0.087(6) 0.114(7) 0.022(5) -0.004(5) 0.030(5) O1 0.100(11) 0.132(12) 0.138(12) 0.035(10) -0.001(9) 0.021(9) O2 0.103(11) 0.136(13) 0.138(12) -0.005(10) 0.036(10) 0.019(10) O3 0.055(7) 0.074(8) 0.143(11) 0.006(8) 0.037(7) -0.012(6) O4 0.139(13) 0.079(9) 0.116(11) 0.020(8) 0.010(9) -0.004(9) O5 0.100(11) 0.133(12) 0.132(12) -0.001(10) 0.042(9) 0.024(9) O6 0.123(13) 0.169(16) 0.156(15) 0.038(13) 0.010(11) 0.047(12) O7 0.082(10) 0.115(11) 0.172(15) -0.021(11) 0.062(10) -0.001(9) O8 0.141(14) 0.102(11) 0.136(13) 0.029(10) 0.025(10) 0.010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.083(6) . ? Ag1 N5 2.103(6) . ? C1 N1 1.140(10) . ? C1 C2 1.434(12) . ? C2 C4 1.359(10) . ? C2 C3 1.404(12) . ? C3 N2 1.142(12) . ? C4 C11 1.417(9) . ? C4 C5 1.487(9) . ? C5 C6 1.499(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.509(10) . ? C6 C9 1.514(9) . ? C6 C8 1.531(10) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.496(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.348(10) . ? C10 C12 1.460(9) . ? C11 H11 0.9300 . ? C12 C13 1.321(10) . ? C12 H12 0.9300 . ? C13 C14 1.447(9) . ? C13 H13 0.9300 . ? C14 C15 1.385(10) . ? C14 C19 1.401(10) . ? C15 C16 1.387(10) . ? C15 H15 0.9300 . ? C16 C17 1.387(10) . ? C16 H16 0.9300 . ? C17 C18 1.346(10) . ? C17 N3 1.440(8) . ? C18 C19 1.368(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.313(10) . ? C20 N3 1.361(9) . ? C20 H20 0.9300 . ? C21 N4 1.352(10) . ? C21 H21 0.9300 . ? C22 N4 1.314(9) . ? C22 N3 1.332(8) . ? C22 H22 0.9300 . ? C23 N5 1.316(11) . ? C23 C24 1.342(11) . ? C23 H23 0.9300 . ? C24 N6 1.391(10) . ? C24 H24 0.9300 . ? C25 N5 1.305(9) . ? C25 N6 1.312(9) . ? C25 H25 0.9300 . ? C26 C31 1.369(10) . ? C26 C27 1.382(10) . ? C26 N6 1.434(9) . ? C27 C28 1.384(10) . ? C27 H27 0.9300 . ? C28 C29 1.385(10) . ? C28 H28 0.9300 . ? C29 C30 1.397(10) . ? C29 C32 1.445(9) . ? C30 C31 1.393(10) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.328(10) . ? C32 H32 0.9300 . ? C33 C34 1.427(10) . ? C33 H33 0.9300 . ? C34 C41 1.359(10) . ? C34 C35 1.503(10) . ? C35 C36 1.521(9) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.497(10) . ? C36 C38 1.518(10) . ? C36 C39 1.533(10) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.493(9) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C42 1.352(10) . ? C40 C41 1.409(9) . ? C41 H41 0.9300 . ? C42 C44 1.431(12) . ? C42 C43 1.434(12) . ? C43 N7 1.112(11) . ? C44 N8 1.136(10) . ? Cl1 O2 1.425(15) . ? Cl1 O4 1.431(13) . ? Cl1 O1 1.444(14) . ? Cl1 O3 1.450(13) . ? Cl2 O5 1.350(14) . ? Cl2 O8 1.351(14) . ? Cl2 O6 1.363(15) . ? Cl2 O7 1.372(15) . ? 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 N4 Ag1 N5 178.9(3) . . ? N1 C1 C2 178.3(11) . . ? C4 C2 C3 122.3(8) . . ? C4 C2 C1 121.9(8) . . ? C3 C2 C1 115.7(8) . . ? N2 C3 C2 178.1(14) . . ? C2 C4 C11 121.4(7) . . ? C2 C4 C5 121.3(7) . . ? C11 C4 C5 117.2(6) . . ? C4 C5 C6 113.6(6) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 110.2(6) . . ? C5 C6 C9 109.1(6) . . ? C7 C6 C9 111.8(6) . . ? C5 C6 C8 109.5(6) . . ? C7 C6 C8 108.1(7) . . ? C9 C6 C8 108.0(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 114.4(6) . . ? C10 C9 H9A 108.7 . . ? C6 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C6 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C12 120.4(7) . . ? C11 C10 C9 119.4(6) . . ? C12 C10 C9 120.2(7) . . ? C10 C11 C4 123.8(7) . . ? C10 C11 H11 118.1 . . ? C4 C11 H11 118.1 . . ? C13 C12 C10 126.7(7) . . ? C13 C12 H12 116.7 . . ? C10 C12 H12 116.7 . . ? C12 C13 C14 127.1(8) . . ? C12 C13 H13 116.5 . . ? C14 C13 H13 116.5 . . ? C15 C14 C19 117.1(7) . . ? C15 C14 C13 118.8(7) . . ? C19 C14 C13 124.1(7) . . ? C14 C15 C16 120.9(7) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 120.0(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.6(7) . . ? C18 C17 N3 121.7(7) . . ? C16 C17 N3 118.7(7) . . ? C17 C18 C19 120.9(7) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 121.5(7) . . ? C18 C19 H19 119.3 . . ? C14 C19 H19 119.3 . . ? C21 C20 N3 108.5(7) . . ? C21 C20 H20 125.8 . . ? N3 C20 H20 125.8 . . ? C20 C21 N4 109.0(7) . . ? C20 C21 H21 125.5 . . ? N4 C21 H21 125.5 . . ? N4 C22 N3 111.3(7) . . ? N4 C22 H22 124.3 . . ? N3 C22 H22 124.3 . . ? N5 C23 C24 108.9(8) . . ? N5 C23 H23 125.6 . . ? C24 C23 H23 125.6 . . ? C23 C24 N6 107.0(8) . . ? C23 C24 H24 126.5 . . ? N6 C24 H24 126.5 . . ? N5 C25 N6 112.5(7) . . ? N5 C25 H25 123.7 . . ? N6 C25 H25 123.7 . . ? C31 C26 C27 120.7(7) . . ? C31 C26 N6 119.4(7) . . ? C27 C26 N6 119.9(7) . . ? C26 C27 C28 120.3(7) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 120.8(7) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 117.2(7) . . ? C28 C29 C32 119.9(7) . . ? C30 C29 C32 122.8(7) . . ? C31 C30 C29 122.5(7) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C26 C31 C30 118.3(7) . . ? C26 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C33 C32 C29 127.4(7) . . ? C33 C32 H32 116.3 . . ? C29 C32 H32 116.3 . . ? C32 C33 C34 126.8(7) . . ? C32 C33 H33 116.6 . . ? C34 C33 H33 116.6 . . ? C41 C34 C33 120.8(7) . . ? C41 C34 C35 118.3(7) . . ? C33 C34 C35 121.0(7) . . ? C34 C35 C36 114.8(6) . . ? C34 C35 H35A 108.6 . . ? C36 C35 H35A 108.6 . . ? C34 C35 H35B 108.6 . . ? C36 C35 H35B 108.6 . . ? H35A C35 H35B 107.5 . . ? C37 C36 C38 108.0(7) . . ? C37 C36 C35 111.7(6) . . ? C38 C36 C35 109.6(6) . . ? C37 C36 C39 110.4(6) . . ? C38 C36 C39 109.6(6) . . ? C35 C36 C39 107.5(6) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C36 114.3(6) . . ? C40 C39 H39A 108.7 . . ? C36 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C36 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C42 C40 C41 121.8(7) . . ? C42 C40 C39 121.4(6) . . ? C41 C40 C39 116.8(6) . . ? C34 C41 C40 125.2(7) . . ? C34 C41 H41 117.4 . . ? C40 C41 H41 117.4 . . ? C40 C42 C44 122.0(7) . . ? C40 C42 C43 122.7(8) . . ? C44 C42 C43 115.2(7) . . ? N7 C43 C42 177.1(12) . . ? N8 C44 C42 179.1(10) . . ? O2 Cl1 O4 109.6(10) . . ? O2 Cl1 O1 110.0(10) . . ? O4 Cl1 O1 109.3(9) . . ? O2 Cl1 O3 110.6(8) . . ? O4 Cl1 O3 109.6(8) . . ? O1 Cl1 O3 107.7(9) . . ? O5 Cl2 O8 110.3(10) . . ? O5 Cl2 O6 110.3(11) . . ? O8 Cl2 O6 108.8(11) . . ? O5 Cl2 O7 109.5(9) . . ? O8 Cl2 O7 110.3(10) . . ? O6 Cl2 O7 107.6(11) . . ? C22 N3 C20 105.3(6) . . ? C22 N3 C17 126.9(6) . . ? C20 N3 C17 127.8(6) . . ? C22 N4 C21 105.9(6) . . ? C22 N4 Ag1 125.3(6) . . ? C21 N4 Ag1 128.7(5) . . ? C25 N5 C23 107.2(7) . . ? C25 N5 Ag1 125.8(6) . . ? C23 N5 Ag1 127.0(6) . . ? C25 N6 C24 104.3(6) . . ? C25 N6 C26 128.4(7) . . ? C24 N6 C26 127.2(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 N1 C1 C2 C4 159(37) . . . . ? N1 C1 C2 C3 -17(38) . . . . ? C4 C2 C3 N2 104(36) . . . . ? C1 C2 C3 N2 -79(36) . . . . ? C3 C2 C4 C11 1.9(14) . . . . ? C1 C2 C4 C11 -174.8(8) . . . . ? C3 C2 C4 C5 178.4(8) . . . . ? C1 C2 C4 C5 1.8(13) . . . . ? C2 C4 C5 C6 152.2(8) . . . . ? C11 C4 C5 C6 -31.1(9) . . . . ? C4 C5 C6 C7 -70.2(8) . . . . ? C4 C5 C6 C9 53.0(8) . . . . ? C4 C5 C6 C8 171.0(7) . . . . ? C5 C6 C9 C10 -47.7(9) . . . . ? C7 C6 C9 C10 74.5(8) . . . . ? C8 C6 C9 C10 -166.7(7) . . . . ? C6 C9 C10 C11 20.3(10) . . . . ? C6 C9 C10 C12 -159.5(6) . . . . ? C12 C10 C11 C4 -175.9(7) . . . . ? C9 C10 C11 C4 4.2(12) . . . . ? C2 C4 C11 C10 177.8(8) . . . . ? C5 C4 C11 C10 1.2(11) . . . . ? C11 C10 C12 C13 176.6(8) . . . . ? C9 C10 C12 C13 -3.6(11) . . . . ? C10 C12 C13 C14 179.4(7) . . . . ? C12 C13 C14 C15 -179.4(8) . . . . ? C12 C13 C14 C19 0.6(13) . . . . ? C19 C14 C15 C16 0.8(13) . . . . ? C13 C14 C15 C16 -179.2(8) . . . . ? C14 C15 C16 C17 0.2(14) . . . . ? C15 C16 C17 C18 -0.7(13) . . . . ? C15 C16 C17 N3 179.1(7) . . . . ? C16 C17 C18 C19 0.0(12) . . . . ? N3 C17 C18 C19 -179.8(7) . . . . ? C17 C18 C19 C14 1.0(12) . . . . ? C15 C14 C19 C18 -1.4(12) . . . . ? C13 C14 C19 C18 178.6(7) . . . . ? N3 C20 C21 N4 2.0(12) . . . . ? N5 C23 C24 N6 1.0(14) . . . . ? C31 C26 C27 C28 -1.6(13) . . . . ? N6 C26 C27 C28 179.7(8) . . . . ? C26 C27 C28 C29 3.2(14) . . . . ? C27 C28 C29 C30 -2.8(13) . . . . ? C27 C28 C29 C32 179.4(8) . . . . ? C28 C29 C30 C31 0.9(12) . . . . ? C32 C29 C30 C31 178.7(7) . . . . ? C27 C26 C31 C30 -0.3(12) . . . . ? N6 C26 C31 C30 178.4(7) . . . . ? C29 C30 C31 C26 0.6(12) . . . . ? C28 C29 C32 C33 -174.3(8) . . . . ? C30 C29 C32 C33 8.0(13) . . . . ? C29 C32 C33 C34 -176.8(7) . . . . ? C32 C33 C34 C41 -176.0(8) . . . . ? C32 C33 C34 C35 4.5(12) . . . . ? C41 C34 C35 C36 -24.5(10) . . . . ? C33 C34 C35 C36 154.9(7) . . . . ? C34 C35 C36 C37 -71.6(9) . . . . ? C34 C35 C36 C38 168.7(7) . . . . ? C34 C35 C36 C39 49.7(9) . . . . ? C37 C36 C39 C40 69.6(8) . . . . ? C38 C36 C39 C40 -171.5(6) . . . . ? C35 C36 C39 C40 -52.5(8) . . . . ? C36 C39 C40 C42 -153.4(7) . . . . ? C36 C39 C40 C41 29.8(9) . . . . ? C33 C34 C41 C40 178.7(7) . . . . ? C35 C34 C41 C40 -1.9(12) . . . . ? C42 C40 C41 C34 -177.7(8) . . . . ? C39 C40 C41 C34 -1.0(11) . . . . ? C41 C40 C42 C44 175.8(7) . . . . ? C39 C40 C42 C44 -0.8(12) . . . . ? C41 C40 C42 C43 -4.4(13) . . . . ? C39 C40 C42 C43 179.0(8) . . . . ? C40 C42 C43 N7 38(27) . . . . ? C44 C42 C43 N7 -143(27) . . . . ? C40 C42 C44 N8 -161(100) . . . . ? C43 C42 C44 N8 19(70) . . . . ? N4 C22 N3 C20 1.1(9) . . . . ? N4 C22 N3 C17 179.6(6) . . . . ? C21 C20 N3 C22 -1.9(11) . . . . ? C21 C20 N3 C17 179.7(8) . . . . ? C18 C17 N3 C22 -20.0(11) . . . . ? C16 C17 N3 C22 160.2(8) . . . . ? C18 C17 N3 C20 158.1(9) . . . . ? C16 C17 N3 C20 -21.7(12) . . . . ? N3 C22 N4 C21 0.1(10) . . . . ? N3 C22 N4 Ag1 -177.5(5) . . . . ? C20 C21 N4 C22 -1.3(12) . . . . ? C20 C21 N4 Ag1 176.2(7) . . . . ? N5 Ag1 N4 C22 -15(13) . . . . ? N5 Ag1 N4 C21 168(12) . . . . ? N6 C25 N5 C23 -2.0(11) . . . . ? N6 C25 N5 Ag1 179.6(5) . . . . ? C24 C23 N5 C25 0.5(13) . . . . ? C24 C23 N5 Ag1 178.8(7) . . . . ? N4 Ag1 N5 C25 -164(13) . . . . ? N4 Ag1 N5 C23 18(13) . . . . ? N5 C25 N6 C24 2.6(10) . . . . ? N5 C25 N6 C26 -179.4(7) . . . . ? C23 C24 N6 C25 -2.1(12) . . . . ? C23 C24 N6 C26 179.9(9) . . . . ? C31 C26 N6 C25 10.6(12) . . . . ? C27 C26 N6 C25 -170.7(8) . . . . ? C31 C26 N6 C24 -171.9(9) . . . . ? C27 C26 N6 C24 6.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.323 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 917019' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 Ag N9 O3' _chemical_formula_weight 850.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.727(5) _cell_length_b 32.015(5) _cell_length_c 8.917(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 112.829(5) _cell_angle_gamma 90.000(5) _cell_volume 2033.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8530 _exptl_absorpt_correction_T_max 0.8984 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14283 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3572 _reflns_number_gt 2927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+1.8340P] 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 3572 _refine_ls_number_parameters 306 _refine_ls_number_restraints 417 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.0000 2.0000 0.0801(3) Uani 1 2 d S . . N3 N 0.3998(4) 0.04779(10) 1.5293(4) 0.0499(7) Uani 1 1 d . . . C17 C 0.4666(5) 0.06302(12) 1.4107(5) 0.0513(9) Uani 1 1 d U . . C2 C 0.4373(6) 0.18506(14) 0.3975(6) 0.0647(10) Uani 1 1 d U . . C11 C 0.5303(6) 0.15629(13) 0.6680(5) 0.0607(10) Uani 1 1 d U A . H11 H 0.4070 0.1475 0.6402 0.073 Uiso 1 1 calc R . . C4 C 0.5739(6) 0.17764(13) 0.5464(5) 0.0557(9) Uani 1 1 d U . . N4 N 0.3997(5) 0.02577(11) 1.7628(4) 0.0603(9) Uani 1 1 d . . . C18 C 0.6559(6) 0.07088(16) 1.4536(6) 0.0680(11) Uani 1 1 d U . . H18 H 0.7405 0.0652 1.5589 0.082 Uiso 1 1 calc R . . C14 C 0.6001(7) 0.09610(16) 1.1869(6) 0.0721(11) Uani 1 1 d U A . C19 C 0.7194(7) 0.08694(17) 1.3422(6) 0.0761(12) Uani 1 1 d U . . H19 H 0.8473 0.0917 1.3730 0.091 Uiso 1 1 calc R . . C16 C 0.3424(6) 0.07083(14) 1.2552(5) 0.0638(10) Uani 1 1 d U . . H16 H 0.2152 0.0652 1.2247 0.077 Uiso 1 1 calc R . . C12 C 0.5818(7) 0.12668(16) 0.9284(6) 0.0720(11) Uani 1 1 d U A . H12 H 0.4542 0.1205 0.8876 0.086 Uiso 1 1 calc R . . C20 C 0.2172(7) 0.0421(2) 1.5108(6) 0.0836(15) Uani 1 1 d U . . H20 H 0.1113 0.0466 1.4163 0.100 Uiso 1 1 calc R . . C1 C 0.4701(8) 0.20592(17) 0.2699(7) 0.0842(14) Uani 1 1 d U . . C22 C 0.5050(6) 0.03716(12) 1.6846(5) 0.0561(9) Uani 1 1 d U . . H22 H 0.6355 0.0378 1.7303 0.067 Uiso 1 1 calc R . . C3 C 0.2479(8) 0.17218(18) 0.3581(7) 0.0823(14) Uani 1 1 d U . . C10 C 0.6517(7) 0.14801(17) 0.8168(6) 0.0738(11) Uani 1 1 d U . . C15 C 0.4097(7) 0.08740(15) 1.1422(5) 0.0710(11) Uani 1 1 d U . . H15 H 0.3262 0.0926 1.0362 0.085 Uiso 1 1 calc R . . C13 C 0.6774(8) 0.1157(2) 1.0754(6) 0.0877(15) Uani 1 1 d U . . H13 H 0.8063 0.1203 1.1157 0.105 Uiso 1 1 calc R A . C21 C 0.2194(7) 0.02893(19) 1.6542(6) 0.0822(14) Uani 1 1 d U . . H21 H 0.1137 0.0229 1.6760 0.099 Uiso 1 1 calc R . . N1 N 0.4951(9) 0.2221(2) 0.1668(7) 0.137(3) Uani 1 1 d . . . N2 N 0.0973(7) 0.1611(2) 0.3296(8) 0.127(2) Uani 1 1 d . . . N5 N 1.0000 0.0000 1.0000 0.103(3) Uani 1 2 d SD . . O3 O 0.9066(14) 0.0208(4) 1.0750(13) 0.109(3) Uani 0.50 1 d PDU . . O2 O 0.9577(15) 0.0155(5) 0.8593(12) 0.124(4) Uani 0.50 1 d PDU . . O1 O 1.079(3) -0.0327(5) 1.060(3) 0.202(7) Uani 0.50 1 d PDU . . C6 C 0.9114(6) 0.18418(16) 0.7578(6) 0.0665(10) Uani 1 1 d U . . C5 C 0.7687(7) 0.1918(2) 0.5872(6) 0.0874(15) Uani 1 1 d U A . H5A H 0.7652 0.2216 0.5667 0.105 Uiso 1 1 calc R . . H5B H 0.8145 0.1785 0.5121 0.105 Uiso 1 1 calc R . . C7 C 0.8633(12) 0.1466(3) 0.8504(10) 0.0669(18) Uani 0.549(6) 1 d PU A 1 H7A H 0.8941 0.1203 0.8128 0.080 Uiso 0.549(6) 1 calc PR A 1 H7B H 0.9366 0.1489 0.9663 0.080 Uiso 0.549(6) 1 calc PR A 1 C8 C 0.8927(15) 0.2238(3) 0.8487(14) 0.092(3) Uani 0.549(6) 1 d PU A 1 H8A H 0.7687 0.2251 0.8488 0.137 Uiso 0.549(6) 1 calc PR A 1 H8B H 0.9145 0.2480 0.7952 0.137 Uiso 0.549(6) 1 calc PR A 1 H8C H 0.9834 0.2229 0.9588 0.137 Uiso 0.549(6) 1 calc PR A 1 C9 C 1.1138(13) 0.1801(4) 0.7763(13) 0.087(3) Uani 0.549(6) 1 d PU A 1 H9A H 1.1932 0.1777 0.8896 0.130 Uiso 0.549(6) 1 calc PR A 1 H9B H 1.1491 0.2043 0.7314 0.130 Uiso 0.549(6) 1 calc PR A 1 H9C H 1.1274 0.1556 0.7198 0.130 Uiso 0.549(6) 1 calc PR A 1 C8' C 0.9893(16) 0.1431(4) 0.7231(16) 0.084(3) Uani 0.451(6) 1 d PU A 2 H8'1 H 1.1047 0.1366 0.8123 0.126 Uiso 0.451(6) 1 calc PR A 2 H8'2 H 1.0124 0.1459 0.6252 0.126 Uiso 0.451(6) 1 calc PR A 2 H8'3 H 0.8999 0.1212 0.7099 0.126 Uiso 0.451(6) 1 calc PR A 2 C7' C 0.8263(16) 0.1803(4) 0.8815(13) 0.075(2) Uani 0.451(6) 1 d PU A 2 H7'1 H 0.7830 0.2074 0.9009 0.090 Uiso 0.451(6) 1 calc PR A 2 H7'2 H 0.9198 0.1703 0.9834 0.090 Uiso 0.451(6) 1 calc PR A 2 C9' C 1.0681(19) 0.2180(5) 0.8064(17) 0.102(4) Uani 0.451(6) 1 d PU A 2 H9'1 H 1.0154 0.2447 0.8147 0.154 Uiso 0.451(6) 1 calc PR A 2 H9'2 H 1.1206 0.2194 0.7250 0.154 Uiso 0.451(6) 1 calc PR A 2 H9'3 H 1.1648 0.2109 0.9094 0.154 Uiso 0.451(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1155(5) 0.0822(4) 0.0471(3) 0.0125(2) 0.0365(3) -0.0022(3) N3 0.0496(17) 0.0594(18) 0.0433(17) 0.0091(14) 0.0208(14) 0.0009(14) C17 0.059(2) 0.0537(19) 0.047(2) 0.0083(16) 0.0262(17) 0.0015(16) C2 0.062(2) 0.068(2) 0.060(2) 0.0090(19) 0.0189(18) -0.0022(19) C11 0.061(2) 0.068(2) 0.060(2) 0.0106(18) 0.0306(18) 0.0001(19) C4 0.058(2) 0.061(2) 0.052(2) 0.0039(17) 0.0256(16) -0.0024(17) N4 0.075(2) 0.066(2) 0.0429(18) 0.0057(15) 0.0263(17) -0.0043(17) C18 0.060(2) 0.089(3) 0.060(2) 0.008(2) 0.0286(19) -0.006(2) C14 0.075(2) 0.082(3) 0.072(3) 0.007(2) 0.041(2) -0.002(2) C19 0.067(2) 0.099(3) 0.069(3) 0.009(2) 0.034(2) -0.005(2) C16 0.063(2) 0.076(2) 0.054(2) 0.0135(19) 0.0246(18) 0.002(2) C12 0.067(2) 0.090(3) 0.060(2) 0.009(2) 0.027(2) 0.005(2) C20 0.055(2) 0.133(4) 0.065(3) 0.035(3) 0.026(2) 0.007(3) C1 0.085(3) 0.089(3) 0.064(3) 0.016(2) 0.012(2) -0.013(3) C22 0.058(2) 0.064(2) 0.045(2) 0.0066(17) 0.0178(18) -0.0042(18) C3 0.069(3) 0.094(3) 0.072(3) 0.011(3) 0.015(2) -0.001(2) C10 0.070(2) 0.098(3) 0.061(2) 0.014(2) 0.0333(19) -0.003(2) C15 0.081(3) 0.080(3) 0.049(2) 0.019(2) 0.022(2) 0.012(2) C13 0.075(3) 0.122(4) 0.068(3) 0.017(3) 0.031(2) -0.008(3) C21 0.061(3) 0.122(4) 0.072(3) 0.031(3) 0.035(2) 0.005(3) N1 0.146(5) 0.163(6) 0.076(3) 0.048(4) 0.015(3) -0.049(4) N2 0.067(3) 0.187(6) 0.106(4) 0.013(4) 0.011(3) -0.020(3) N5 0.070(4) 0.134(7) 0.090(6) -0.004(5) 0.015(4) -0.037(4) O3 0.101(5) 0.143(7) 0.110(6) -0.005(5) 0.071(5) -0.020(5) O2 0.105(6) 0.191(8) 0.097(6) 0.015(6) 0.063(5) -0.017(6) O1 0.169(10) 0.187(10) 0.206(11) -0.016(9) 0.023(8) 0.031(8) C6 0.059(2) 0.083(3) 0.055(2) 0.0059(19) 0.0197(18) -0.0055(19) C5 0.071(3) 0.130(4) 0.059(2) 0.020(2) 0.023(2) -0.024(3) C7 0.071(3) 0.077(4) 0.051(3) 0.009(3) 0.022(3) 0.005(3) C8 0.090(5) 0.084(5) 0.095(5) -0.012(4) 0.029(4) -0.004(4) C9 0.067(4) 0.114(6) 0.079(5) 0.011(5) 0.028(4) 0.003(4) C8' 0.064(5) 0.106(6) 0.081(6) 0.011(5) 0.027(4) 0.011(4) C7' 0.079(4) 0.087(5) 0.058(4) 0.010(4) 0.024(3) -0.002(4) C9' 0.088(6) 0.115(6) 0.087(6) 0.013(5) 0.016(5) -0.028(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.117(3) 3_659 ? Ag1 N4 2.117(3) . ? N3 C22 1.349(5) . ? N3 C20 1.368(6) . ? N3 C17 1.430(5) . ? C17 C16 1.369(6) . ? C17 C18 1.384(6) . ? C2 C4 1.359(6) . ? C2 C1 1.424(7) . ? C2 C3 1.427(7) . ? C11 C10 1.321(6) . ? C11 C4 1.428(6) . ? C11 H11 0.9300 . ? C4 C5 1.476(6) . ? N4 C22 1.312(5) . ? N4 C21 1.357(6) . ? C18 C19 1.368(6) . ? C18 H18 0.9300 . ? C14 C19 1.365(7) . ? C14 C15 1.395(7) . ? C14 C13 1.483(7) . ? C19 H19 0.9300 . ? C16 C15 1.404(6) . ? C16 H16 0.9300 . ? C12 C13 1.279(7) . ? C12 C10 1.471(6) . ? C12 H12 0.9300 . ? C20 C21 1.341(6) . ? C20 H20 0.9300 . ? C1 N1 1.135(7) . ? C22 H22 0.9300 . ? C3 N2 1.147(7) . ? C10 C7 1.544(10) . ? C10 C7' 1.618(13) . ? C15 H15 0.9300 . ? C13 H13 0.9300 . ? C21 H21 0.9300 . ? N5 O1 1.225(13) 3_757 ? N5 O1 1.225(13) . ? N5 O2 1.268(10) 3_757 ? N5 O2 1.268(10) . ? N5 O3 1.337(8) . ? N5 O3 1.337(8) 3_757 ? O3 O1 1.31(2) 3_757 ? O3 O2 1.522(17) 3_757 ? O2 O1 1.026(19) 3_757 ? O2 O3 1.522(17) 3_757 ? O1 O2 1.026(19) 3_757 ? O1 O3 1.31(2) 3_757 ? C6 C7' 1.493(12) . ? C6 C5 1.512(7) . ? C6 C9 1.513(10) . ? C6 C8' 1.526(13) . ? C6 C8 1.542(11) . ? C6 C9' 1.556(13) . ? C6 C7 1.582(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? 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 N4 Ag1 N4 180.000(1) 3_659 . ? C22 N3 C20 105.9(3) . . ? C22 N3 C17 126.8(3) . . ? C20 N3 C17 127.4(3) . . ? C16 C17 C18 119.8(4) . . ? C16 C17 N3 120.0(4) . . ? C18 C17 N3 120.2(4) . . ? C4 C2 C1 123.5(4) . . ? C4 C2 C3 121.6(4) . . ? C1 C2 C3 115.0(4) . . ? C10 C11 C4 125.0(4) . . ? C10 C11 H11 117.5 . . ? C4 C11 H11 117.5 . . ? C2 C4 C11 120.2(4) . . ? C2 C4 C5 121.2(4) . . ? C11 C4 C5 118.6(4) . . ? C22 N4 C21 106.1(3) . . ? C22 N4 Ag1 125.3(3) . . ? C21 N4 Ag1 128.2(3) . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C19 C14 C15 118.0(4) . . ? C19 C14 C13 118.8(5) . . ? C15 C14 C13 123.2(5) . . ? C14 C19 C18 121.7(5) . . ? C14 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C13 C12 C10 127.1(5) . . ? C13 C12 H12 116.5 . . ? C10 C12 H12 116.5 . . ? C21 C20 N3 107.2(4) . . ? C21 C20 H20 126.4 . . ? N3 C20 H20 126.4 . . ? N1 C1 C2 179.0(7) . . ? N4 C22 N3 111.4(4) . . ? N4 C22 H22 124.3 . . ? N3 C22 H22 124.3 . . ? N2 C3 C2 178.2(7) . . ? C11 C10 C12 118.0(4) . . ? C11 C10 C7 119.0(5) . . ? C12 C10 C7 119.7(5) . . ? C11 C10 C7' 113.5(5) . . ? C12 C10 C7' 122.0(6) . . ? C7 C10 C7' 43.5(5) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C12 C13 C14 125.5(5) . . ? C12 C13 H13 117.3 . . ? C14 C13 H13 117.3 . . ? C20 C21 N4 109.5(4) . . ? C20 C21 H21 125.3 . . ? N4 C21 H21 125.3 . . ? O1 N5 O1 180.0(7) 3_757 . ? O1 N5 O2 131.5(9) 3_757 3_757 ? O1 N5 O2 48.5(9) . 3_757 ? O1 N5 O2 48.5(9) 3_757 . ? O1 N5 O2 131.5(9) . . ? O2 N5 O2 180.000(4) 3_757 . ? O1 N5 O3 61.4(10) 3_757 . ? O1 N5 O3 118.6(10) . . ? O2 N5 O3 71.5(7) 3_757 . ? O2 N5 O3 108.5(7) . . ? O1 N5 O3 118.6(10) 3_757 3_757 ? O1 N5 O3 61.4(10) . 3_757 ? O2 N5 O3 108.5(7) 3_757 3_757 ? O2 N5 O3 71.5(7) . 3_757 ? O3 N5 O3 180.0(10) . 3_757 ? O1 O3 N5 55.1(7) 3_757 . ? O1 O3 O2 106.4(10) 3_757 3_757 ? N5 O3 O2 52.2(5) . 3_757 ? O1 O2 N5 63.5(11) 3_757 . ? O1 O2 O3 118.4(15) 3_757 3_757 ? N5 O2 O3 56.4(6) . 3_757 ? O2 O1 N5 67.9(10) 3_757 . ? O2 O1 O3 129.2(17) 3_757 3_757 ? N5 O1 O3 63.5(9) . 3_757 ? C7' C6 C5 113.5(6) . . ? C7' C6 C9 130.1(7) . . ? C5 C6 C9 116.3(5) . . ? C7' C6 C8' 113.5(8) . . ? C5 C6 C8' 97.2(6) . . ? C9 C6 C8' 58.3(7) . . ? C7' C6 C8 61.5(6) . . ? C5 C6 C8 102.5(6) . . ? C9 C6 C8 108.5(7) . . ? C8' C6 C8 160.0(7) . . ? C7' C6 C9' 111.8(8) . . ? C5 C6 C9' 110.6(6) . . ? C9 C6 C9' 51.0(7) . . ? C8' C6 C9' 109.3(8) . . ? C8 C6 C9' 60.1(7) . . ? C7' C6 C7 44.8(5) . . ? C5 C6 C7 114.9(5) . . ? C9 C6 C7 108.6(6) . . ? C8' C6 C7 69.1(6) . . ? C8 C6 C7 105.1(6) . . ? C9' C6 C7 134.3(7) . . ? C4 C5 C6 118.3(4) . . ? C4 C5 H5A 107.7 . . ? C6 C5 H5A 107.7 . . ? C4 C5 H5B 107.7 . . ? C6 C5 H5B 107.7 . . ? H5A C5 H5B 107.1 . . ? C10 C7 C6 108.8(6) . . ? C10 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? C10 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? C6 C8' H8'1 109.5 . . ? C6 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C6 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C6 C7' C10 109.6(8) . . ? C6 C7' H7'1 109.8 . . ? C10 C7' H7'1 109.8 . . ? C6 C7' H7'2 109.8 . . ? C10 C7' H7'2 109.8 . . ? H7'1 C7' H7'2 108.2 . . ? C6 C9' H9'1 109.5 . . ? C6 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C6 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? 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 C22 N3 C17 C16 177.2(4) . . . . ? C20 N3 C17 C16 -4.9(7) . . . . ? C22 N3 C17 C18 -4.4(6) . . . . ? C20 N3 C17 C18 173.6(5) . . . . ? C1 C2 C4 C11 -179.6(5) . . . . ? C3 C2 C4 C11 0.4(7) . . . . ? C1 C2 C4 C5 1.2(8) . . . . ? C3 C2 C4 C5 -178.8(5) . . . . ? C10 C11 C4 C2 -179.1(5) . . . . ? C10 C11 C4 C5 0.1(8) . . . . ? N4 Ag1 N4 C22 -55(100) 3_659 . . . ? N4 Ag1 N4 C21 116(100) 3_659 . . . ? C16 C17 C18 C19 0.9(7) . . . . ? N3 C17 C18 C19 -177.5(4) . . . . ? C15 C14 C19 C18 -2.0(8) . . . . ? C13 C14 C19 C18 176.6(5) . . . . ? C17 C18 C19 C14 0.6(8) . . . . ? C18 C17 C16 C15 -1.0(7) . . . . ? N3 C17 C16 C15 177.4(4) . . . . ? C22 N3 C20 C21 0.7(6) . . . . ? C17 N3 C20 C21 -177.6(4) . . . . ? C4 C2 C1 N1 124(46) . . . . ? C3 C2 C1 N1 -56(46) . . . . ? C21 N4 C22 N3 0.2(5) . . . . ? Ag1 N4 C22 N3 172.7(3) . . . . ? C20 N3 C22 N4 -0.6(5) . . . . ? C17 N3 C22 N4 177.7(4) . . . . ? C4 C2 C3 N2 -22(27) . . . . ? C1 C2 C3 N2 158(26) . . . . ? C4 C11 C10 C12 178.4(4) . . . . ? C4 C11 C10 C7 -22.3(8) . . . . ? C4 C11 C10 C7' 26.2(8) . . . . ? C13 C12 C10 C11 179.1(6) . . . . ? C13 C12 C10 C7 19.9(10) . . . . ? C13 C12 C10 C7' -31.2(10) . . . . ? C19 C14 C15 C16 1.8(8) . . . . ? C13 C14 C15 C16 -176.7(5) . . . . ? C17 C16 C15 C14 -0.3(7) . . . . ? C10 C12 C13 C14 176.7(5) . . . . ? C19 C14 C13 C12 -178.5(6) . . . . ? C15 C14 C13 C12 0.0(10) . . . . ? N3 C20 C21 N4 -0.5(7) . . . . ? C22 N4 C21 C20 0.2(6) . . . . ? Ag1 N4 C21 C20 -172.0(4) . . . . ? O1 N5 O3 O1 180.000(13) . . . 3_757 ? O2 N5 O3 O1 167.9(13) 3_757 . . 3_757 ? O2 N5 O3 O1 -12.1(13) . . . 3_757 ? O3 N5 O3 O1 -14(100) 3_757 . . 3_757 ? O1 N5 O3 O2 -167.9(13) 3_757 . . 3_757 ? O1 N5 O3 O2 12.1(13) . . . 3_757 ? O2 N5 O3 O2 180.000(10) . . . 3_757 ? O3 N5 O3 O2 178(100) 3_757 . . 3_757 ? O1 N5 O2 O1 180.000(15) . . . 3_757 ? O2 N5 O2 O1 -85(100) 3_757 . . 3_757 ? O3 N5 O2 O1 14.2(16) . . . 3_757 ? O3 N5 O2 O1 -165.8(16) 3_757 . . 3_757 ? O1 N5 O2 O3 165.8(16) 3_757 . . 3_757 ? O1 N5 O2 O3 -14.2(16) . . . 3_757 ? O2 N5 O2 O3 81(100) 3_757 . . 3_757 ? O3 N5 O2 O3 180.000(7) . . . 3_757 ? O1 N5 O1 O2 29(100) 3_757 . . 3_757 ? O2 N5 O1 O2 180.000(15) . . . 3_757 ? O3 N5 O1 O2 -15.3(17) . . . 3_757 ? O3 N5 O1 O2 164.7(17) 3_757 . . 3_757 ? O1 N5 O1 O3 -135(100) 3_757 . . 3_757 ? O2 N5 O1 O3 -164.7(17) 3_757 . . 3_757 ? O2 N5 O1 O3 15.3(17) . . . 3_757 ? O3 N5 O1 O3 180.000(11) . . . 3_757 ? C2 C4 C5 C6 177.3(5) . . . . ? C11 C4 C5 C6 -1.9(8) . . . . ? C7' C6 C5 C4 -25.0(9) . . . . ? C9 C6 C5 C4 152.8(7) . . . . ? C8' C6 C5 C4 94.6(7) . . . . ? C8 C6 C5 C4 -89.0(7) . . . . ? C9' C6 C5 C4 -151.5(8) . . . . ? C7 C6 C5 C4 24.4(8) . . . . ? C11 C10 C7 C6 42.0(8) . . . . ? C12 C10 C7 C6 -159.0(5) . . . . ? C7' C10 C7 C6 -52.5(7) . . . . ? C7' C6 C7 C10 57.1(8) . . . . ? C5 C6 C7 C10 -41.9(8) . . . . ? C9 C6 C7 C10 -174.1(7) . . . . ? C8' C6 C7 C10 -130.3(8) . . . . ? C8 C6 C7 C10 69.9(7) . . . . ? C9' C6 C7 C10 132.7(11) . . . . ? C5 C6 C7' C10 48.6(9) . . . . ? C9 C6 C7' C10 -128.7(9) . . . . ? C8' C6 C7' C10 -61.2(10) . . . . ? C8 C6 C7' C10 140.4(10) . . . . ? C9' C6 C7' C10 174.6(8) . . . . ? C7 C6 C7' C10 -53.7(7) . . . . ? C11 C10 C7' C6 -50.6(9) . . . . ? C12 C10 C7' C6 158.5(6) . . . . ? C7 C10 C7' C6 57.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.588 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 917020' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H46 Ag N9 O3' _chemical_formula_sum 'C50 H46 Ag N9 O3' _chemical_formula_weight 928.83 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' Ag Ag -0.8971 1.1015 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.991(14) _cell_length_b 13.22(3) _cell_length_c 13.23(3) _cell_angle_alpha 80.11(2) _cell_angle_beta 81.34(2) _cell_angle_gamma 77.57(2) _cell_volume 1168(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4265 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.35 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8085 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8274 _diffrn_reflns_av_R_equivalents 0.1074 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4059 _reflns_number_gt 3625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.2207P] 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 4059 _refine_ls_number_parameters 303 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.5000 -0.5000 0.5000 0.06006(18) Uani 1 2 d S . . C1 C 1.5709(5) -0.2647(2) 0.5054(3) 0.0534(6) Uani 1 1 d U . . H1 H 1.7024 -0.2809 0.4779 0.064 Uiso 1 1 calc R . . C2 C 1.2776(4) -0.2804(2) 0.5613(2) 0.0447(6) Uani 1 1 d . . . H2 H 1.1615 -0.3058 0.5818 0.054 Uiso 1 1 calc R . . C3 C 1.4885(4) -0.1718(2) 0.5299(2) 0.0458(5) Uani 1 1 d U . . H3 H 1.5452 -0.1133 0.5244 0.055 Uiso 1 1 calc R . . C4 C 0.5642(5) 0.3327(2) 0.7524(2) 0.0480(7) Uani 1 1 d . . . C5 C 0.7252(5) 0.2521(2) 0.7124(2) 0.0511(7) Uani 1 1 d . . . H5 H 0.8423 0.2728 0.6824 0.061 Uiso 1 1 calc R . . C6 C 0.4390(5) 0.5169(2) 0.7805(2) 0.0491(7) Uani 1 1 d . . . C7 C 0.5906(5) 0.4337(3) 0.7419(2) 0.0514(7) Uani 1 1 d . . . H7 H 0.7097 0.4499 0.7089 0.062 Uiso 1 1 calc R . . C8 C 0.7155(5) 0.1515(3) 0.7160(2) 0.0526(7) Uani 1 1 d . . . H8 H 0.5975 0.1322 0.7465 0.063 Uiso 1 1 calc R . . C9 C 0.2368(5) 0.4922(3) 0.8151(3) 0.0571(8) Uani 1 1 d . . . H9A H 0.1670 0.5007 0.7552 0.069 Uiso 1 1 calc R . . H9B H 0.1633 0.5415 0.8601 0.069 Uiso 1 1 calc R . . C10 C 1.1534(4) -0.0967(2) 0.6022(2) 0.0436(6) Uani 1 1 d . . . C11 C 0.8716(5) 0.0673(2) 0.6768(2) 0.0492(7) Uani 1 1 d . . . C12 C 0.9589(5) -0.1076(2) 0.6253(3) 0.0596(8) Uani 1 1 d . . . H12 H 0.9211 -0.1683 0.6160 0.071 Uiso 1 1 calc R . . C13 C 0.3710(5) 0.3010(3) 0.8029(3) 0.0559(8) Uani 1 1 d . . . H13A H 0.4001 0.2321 0.8431 0.067 Uiso 1 1 calc R . . H13B H 0.2943 0.2963 0.7492 0.067 Uiso 1 1 calc R . . C14 C 0.2459(5) 0.3779(3) 0.8738(2) 0.0549(8) Uani 1 1 d . . . C15 C 0.4788(5) 0.6142(2) 0.7834(2) 0.0532(7) Uani 1 1 d . . . C16 C 1.2113(5) -0.0048(3) 0.6141(3) 0.0608(8) Uani 1 1 d . . . H16 H 1.3424 0.0021 0.5975 0.073 Uiso 1 1 calc R . . C17 C 0.6739(6) 0.6395(3) 0.7490(3) 0.0618(9) Uani 1 1 d . . . C18 C 0.8193(5) -0.0254(3) 0.6632(3) 0.0613(9) Uani 1 1 d . . . H18 H 0.6884 -0.0327 0.6796 0.074 Uiso 1 1 calc R . . C19 C 1.0692(5) 0.0766(3) 0.6514(3) 0.0632(9) Uani 1 1 d . . . H19 H 1.1069 0.1378 0.6593 0.076 Uiso 1 1 calc R . . C20 C 0.3432(7) 0.3694(3) 0.9741(3) 0.0758(11) Uani 1 1 d . . . H20A H 0.3433 0.3013 1.0135 0.114 Uiso 1 1 calc R . . H20B H 0.2699 0.4218 1.0146 0.114 Uiso 1 1 calc R . . H20C H 0.4765 0.3800 0.9561 0.114 Uiso 1 1 calc R . . C21 C 0.0371(6) 0.3537(4) 0.9003(4) 0.0840(12) Uani 1 1 d . . . H21A H -0.0212 0.3598 0.8377 0.126 Uiso 1 1 calc R . . H21B H -0.0423 0.4023 0.9433 0.126 Uiso 1 1 calc R . . H21C H 0.0444 0.2837 0.9364 0.126 Uiso 1 1 calc R . . C22 C 0.3301(6) 0.6988(3) 0.8208(3) 0.0633(9) Uani 1 1 d . . . N1 N 1.4493(4) -0.33620(19) 0.52335(18) 0.0477(6) Uani 1 1 d . . . N3 N 0.8270(6) 0.6586(3) 0.7206(3) 0.0833(10) Uani 1 1 d . . . N4 N 0.2127(7) 0.7650(3) 0.8507(3) 0.0917(11) Uani 1 1 d . . . N2 N 1.2981(3) -0.18224(18) 0.56542(18) 0.0438(5) Uani 1 1 d U . . C34 C 0.483(3) 0.0614(9) 0.0744(8) 0.176(5) Uani 1 1 d . . . H34 H 0.4713 0.1026 0.1262 0.211 Uiso 1 1 calc R . . C33 C 0.663(3) 0.0185(14) 0.0333(12) 0.196(6) Uani 1 1 d . . . H33 H 0.7749 0.0316 0.0548 0.235 Uiso 1 1 calc R . . C35 C 0.319(2) 0.0461(10) 0.0423(12) 0.179(4) Uani 1 1 d . . . H35 H 0.1946 0.0780 0.0702 0.215 Uiso 1 1 calc R . . N5 N 1.0000 0.5000 0.5000 0.0715(13) Uani 1 2 d SD . . O3 O 0.9968(17) 0.4124(7) 0.5450(9) 0.118(4) Uani 0.50 1 d PD . . O1 O 0.8744(12) 0.5281(11) 0.4231(6) 0.113(3) Uani 0.50 1 d PD . . O2 O 1.0998(15) 0.5579(10) 0.5005(12) 0.122(4) Uani 0.50 1 d PD . . 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 0.0727(3) 0.0333(2) 0.0713(3) -0.02315(16) -0.00743(18) 0.00751(16) C1 0.0459(13) 0.0417(13) 0.0677(15) -0.0120(12) 0.0040(12) -0.0021(11) C2 0.0494(15) 0.0292(13) 0.0526(15) -0.0100(11) -0.0028(12) -0.0002(12) C3 0.0401(10) 0.0321(10) 0.0639(12) -0.0109(10) 0.0030(10) -0.0072(9) C4 0.0564(17) 0.0390(16) 0.0429(14) -0.0119(12) -0.0021(12) 0.0053(13) C5 0.0582(18) 0.0393(16) 0.0490(15) -0.0116(12) 0.0026(13) 0.0034(14) C6 0.0636(18) 0.0378(16) 0.0392(13) -0.0076(12) -0.0097(13) 0.0087(14) C7 0.0578(18) 0.0432(17) 0.0468(15) -0.0112(13) 0.0016(13) 0.0022(14) C8 0.0577(18) 0.0405(16) 0.0527(16) -0.0100(13) 0.0043(14) 0.0009(14) C9 0.0616(19) 0.0458(18) 0.0581(17) -0.0166(14) -0.0078(15) 0.0103(15) C10 0.0528(16) 0.0258(13) 0.0469(14) -0.0081(11) 0.0000(12) 0.0021(12) C11 0.0573(17) 0.0335(15) 0.0504(15) -0.0082(12) 0.0014(13) 0.0012(13) C12 0.0560(18) 0.0301(15) 0.091(2) -0.0181(15) 0.0077(17) -0.0086(14) C13 0.0637(19) 0.0421(17) 0.0582(17) -0.0176(14) 0.0042(15) -0.0018(15) C14 0.0586(18) 0.0469(18) 0.0524(16) -0.0148(13) 0.0033(14) 0.0041(15) C15 0.069(2) 0.0389(16) 0.0457(15) -0.0084(12) -0.0112(14) 0.0066(15) C16 0.0503(17) 0.0422(17) 0.091(2) -0.0264(17) 0.0042(16) -0.0071(15) C17 0.083(3) 0.0349(16) 0.0630(19) -0.0057(14) -0.0128(18) 0.0012(17) C18 0.0520(18) 0.0398(17) 0.087(2) -0.0162(16) 0.0101(16) -0.0047(14) C19 0.067(2) 0.0338(16) 0.091(2) -0.0271(16) 0.0037(18) -0.0076(15) C20 0.101(3) 0.068(2) 0.0484(18) -0.0077(17) -0.0026(18) -0.001(2) C21 0.066(2) 0.077(3) 0.104(3) -0.032(2) 0.015(2) -0.007(2) C22 0.090(2) 0.0385(17) 0.0572(18) -0.0146(15) -0.0098(17) 0.0050(18) N1 0.0568(14) 0.0323(12) 0.0517(13) -0.0149(10) -0.0056(11) 0.0027(11) N3 0.088(2) 0.0522(19) 0.106(3) -0.0045(18) -0.009(2) -0.0139(18) N4 0.116(3) 0.0506(19) 0.098(2) -0.0270(18) -0.006(2) 0.015(2) N2 0.0440(10) 0.0291(10) 0.0552(12) -0.0087(9) -0.0004(9) -0.0021(9) C34 0.313(17) 0.115(7) 0.116(6) -0.001(5) -0.007(10) -0.099(11) C33 0.298(19) 0.169(12) 0.147(9) 0.011(8) -0.028(10) -0.126(13) C35 0.235(13) 0.127(8) 0.157(9) 0.023(7) 0.013(9) -0.053(8) N5 0.051(2) 0.059(3) 0.098(3) -0.032(3) 0.027(2) -0.007(2) O3 0.101(7) 0.080(6) 0.134(7) 0.019(6) 0.038(6) 0.003(5) O1 0.082(5) 0.152(9) 0.101(5) -0.042(5) -0.018(4) 0.012(6) O2 0.092(6) 0.100(8) 0.202(13) -0.085(8) 0.005(6) -0.045(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 N1 2.186(5) 2_846 ? Ag1 N1 2.186(5) . ? C1 C3 1.312(5) . ? C1 N1 1.371(4) . ? C1 H1 0.9300 . ? C2 N1 1.342(4) . ? C2 N2 1.347(5) . ? C2 H2 0.9300 . ? C3 N2 1.371(4) . ? C3 H3 0.9300 . ? C4 C7 1.369(5) . ? C4 C5 1.477(5) . ? C4 C13 1.523(5) . ? C5 C8 1.338(6) . ? C5 H5 0.9300 . ? C6 C15 1.382(5) . ? C6 C7 1.456(5) . ? C6 C9 1.505(6) . ? C7 H7 0.9300 . ? C8 C11 1.485(5) . ? C8 H8 0.9300 . ? C9 C14 1.569(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.381(5) . ? C10 C16 1.401(5) . ? C10 N2 1.445(4) . ? C11 C18 1.398(5) . ? C11 C19 1.399(6) . ? C12 C18 1.402(5) . ? C12 H12 0.9300 . ? C13 C14 1.542(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C21 1.539(6) . ? C14 C20 1.557(6) . ? C15 C22 1.452(5) . ? C15 C17 1.462(6) . ? C16 C19 1.400(5) . ? C16 H16 0.9300 . ? C17 N3 1.146(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.143(5) . ? C34 C33 1.339(17) . ? C34 C35 1.350(15) . ? C34 H34 0.9300 . ? C33 C35 1.397(16) 2_655 ? C33 H33 0.9300 . ? C35 C33 1.397(16) 2_655 ? C35 H35 0.9300 . ? N5 O2 1.143(7) . ? N5 O2 1.143(7) 2_766 ? N5 O3 1.212(8) 2_766 ? N5 O3 1.212(8) . ? N5 O1 1.394(7) 2_766 ? N5 O1 1.394(7) . ? O3 O2 0.949(12) 2_766 ? O3 O1 1.463(15) 2_766 ? O1 O2 1.386(15) 2_766 ? O1 O3 1.463(15) 2_766 ? O2 O3 0.949(12) 2_766 ? O2 O1 1.386(15) 2_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.00(14) 2_846 . ? C3 C1 N1 115.2(3) . . ? C3 C1 H1 122.4 . . ? N1 C1 H1 122.4 . . ? N1 C2 N2 110.0(3) . . ? N1 C2 H2 125.0 . . ? N2 C2 H2 125.0 . . ? C1 C3 N2 102.8(3) . . ? C1 C3 H3 128.6 . . ? N2 C3 H3 128.6 . . ? C7 C4 C5 119.5(3) . . ? C7 C4 C13 121.7(3) . . ? C5 C4 C13 118.8(3) . . ? C8 C5 C4 125.1(3) . . ? C8 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? C15 C6 C7 121.3(3) . . ? C15 C6 C9 121.8(3) . . ? C7 C6 C9 116.9(3) . . ? C4 C7 C6 122.4(3) . . ? C4 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C5 C8 C11 127.5(3) . . ? C5 C8 H8 116.3 . . ? C11 C8 H8 116.3 . . ? C6 C9 C14 112.1(3) . . ? C6 C9 H9A 109.2 . . ? C14 C9 H9A 109.2 . . ? C6 C9 H9B 109.2 . . ? C14 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C12 C10 C16 121.1(3) . . ? C12 C10 N2 118.9(3) . . ? C16 C10 N2 120.0(3) . . ? C18 C11 C19 118.1(3) . . ? C18 C11 C8 118.8(3) . . ? C19 C11 C8 123.1(3) . . ? C10 C12 C18 118.8(3) . . ? C10 C12 H12 120.6 . . ? C18 C12 H12 120.6 . . ? C4 C13 C14 113.5(3) . . ? C4 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C4 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C21 C14 C13 109.1(3) . . ? C21 C14 C20 110.5(3) . . ? C13 C14 C20 110.5(3) . . ? C21 C14 C9 110.2(3) . . ? C13 C14 C9 108.4(3) . . ? C20 C14 C9 108.0(3) . . ? C6 C15 C22 122.5(3) . . ? C6 C15 C17 122.3(3) . . ? C22 C15 C17 115.2(3) . . ? C19 C16 C10 119.1(3) . . ? C19 C16 H16 120.4 . . ? C10 C16 H16 120.4 . . ? N3 C17 C15 178.9(4) . . ? C11 C18 C12 121.8(3) . . ? C11 C18 H18 119.1 . . ? C12 C18 H18 119.1 . . ? C11 C19 C16 121.1(3) . . ? C11 C19 H19 119.5 . . ? C16 C19 H19 119.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C15 179.6(5) . . ? C2 N1 C1 102.3(3) . . ? C2 N1 Ag1 125.5(2) . . ? C1 N1 Ag1 132.1(2) . . ? C2 N2 C3 109.6(2) . . ? C2 N2 C10 128.9(3) . . ? C3 N2 C10 121.5(3) . . ? C33 C34 C35 121.4(13) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C33 C35 119.4(13) . 2_655 ? C34 C33 H33 120.3 . . ? C35 C33 H33 120.3 2_655 . ? C34 C35 C33 119.1(13) . 2_655 ? C34 C35 H35 120.5 . . ? C33 C35 H35 120.4 2_655 . ? O2 N5 O2 180.000(2) . 2_766 ? O2 N5 O3 47.4(6) . 2_766 ? O2 N5 O3 132.6(6) 2_766 2_766 ? O2 N5 O3 132.6(6) . . ? O2 N5 O3 47.4(6) 2_766 . ? O3 N5 O3 180.0(4) 2_766 . ? O2 N5 O1 65.4(7) . 2_766 ? O2 N5 O1 114.6(7) 2_766 2_766 ? O3 N5 O1 112.1(7) 2_766 2_766 ? O3 N5 O1 67.9(7) . 2_766 ? O2 N5 O1 114.6(7) . . ? O2 N5 O1 65.4(7) 2_766 . ? O3 N5 O1 67.9(7) 2_766 . ? O3 N5 O1 112.1(7) . . ? O1 N5 O1 180.000(2) 2_766 . ? O2 O3 N5 62.5(7) 2_766 . ? O2 O3 O1 123.6(12) 2_766 2_766 ? N5 O3 O1 62.0(6) . 2_766 ? O2 O1 N5 48.5(4) 2_766 . ? O2 O1 O3 98.3(6) 2_766 2_766 ? N5 O1 O3 50.1(4) . 2_766 ? O3 O2 N5 70.1(8) 2_766 . ? O3 O2 O1 135.1(12) 2_766 2_766 ? N5 O2 O1 66.1(7) . 2_766 ? 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 N1 C1 C3 N2 -0.7(4) . . . . ? C7 C4 C5 C8 -178.4(3) . . . . ? C13 C4 C5 C8 0.5(5) . . . . ? C5 C4 C7 C6 -179.3(3) . . . . ? C13 C4 C7 C6 1.8(5) . . . . ? C15 C6 C7 C4 169.9(3) . . . . ? C9 C6 C7 C4 -11.2(4) . . . . ? C4 C5 C8 C11 179.7(3) . . . . ? C15 C6 C9 C14 -142.0(3) . . . . ? C7 C6 C9 C14 39.1(4) . . . . ? C5 C8 C11 C18 -163.7(3) . . . . ? C5 C8 C11 C19 15.4(5) . . . . ? C16 C10 C12 C18 -1.2(5) . . . . ? N2 C10 C12 C18 178.6(3) . . . . ? C7 C4 C13 C14 -21.4(4) . . . . ? C5 C4 C13 C14 159.7(3) . . . . ? C4 C13 C14 C21 167.0(3) . . . . ? C4 C13 C14 C20 -71.2(4) . . . . ? C4 C13 C14 C9 47.0(4) . . . . ? C6 C9 C14 C21 -175.7(3) . . . . ? C6 C9 C14 C13 -56.4(4) . . . . ? C6 C9 C14 C20 63.4(4) . . . . ? C7 C6 C15 C22 179.5(3) . . . . ? C9 C6 C15 C22 0.7(5) . . . . ? C7 C6 C15 C17 -0.4(4) . . . . ? C9 C6 C15 C17 -179.3(3) . . . . ? C12 C10 C16 C19 0.8(5) . . . . ? N2 C10 C16 C19 -179.0(3) . . . . ? C6 C15 C17 N3 46(22) . . . . ? C22 C15 C17 N3 -134(22) . . . . ? C19 C11 C18 C12 0.1(5) . . . . ? C8 C11 C18 C12 179.3(3) . . . . ? C10 C12 C18 C11 0.8(6) . . . . ? C18 C11 C19 C16 -0.5(5) . . . . ? C8 C11 C19 C16 -179.7(3) . . . . ? C10 C16 C19 C11 0.1(6) . . . . ? C6 C15 C22 N4 44(85) . . . . ? C17 C15 C22 N4 -136(100) . . . . ? N2 C2 N1 C1 -0.1(3) . . . . ? N2 C2 N1 Ag1 179.99(18) . . . . ? C3 C1 N1 C2 0.6(4) . . . . ? C3 C1 N1 Ag1 -179.6(2) . . . . ? N1 Ag1 N1 C2 -97(100) 2_846 . . . ? N1 Ag1 N1 C1 83(100) 2_846 . . . ? N1 C2 N2 C3 -0.3(3) . . . . ? N1 C2 N2 C10 -179.0(3) . . . . ? C1 C3 N2 C2 0.6(3) . . . . ? C1 C3 N2 C10 179.4(3) . . . . ? C12 C10 N2 C2 -9.2(5) . . . . ? C16 C10 N2 C2 170.7(3) . . . . ? C12 C10 N2 C3 172.3(3) . . . . ? C16 C10 N2 C3 -7.9(4) . . . . ? C35 C34 C33 C35 -1.9(18) . . . 2_655 ? C33 C34 C35 C33 1.9(18) . . . 2_655 ? O2 N5 O3 O2 180.000(3) . . . 2_766 ? O3 N5 O3 O2 -79(100) 2_766 . . 2_766 ? O1 N5 O3 O2 169.8(10) 2_766 . . 2_766 ? O1 N5 O3 O2 -10.2(10) . . . 2_766 ? O2 N5 O3 O1 10.2(10) . . . 2_766 ? O2 N5 O3 O1 -169.8(10) 2_766 . . 2_766 ? O3 N5 O3 O1 111(100) 2_766 . . 2_766 ? O1 N5 O3 O1 180.000(3) . . . 2_766 ? O2 N5 O1 O2 180.000(2) . . . 2_766 ? O3 N5 O1 O2 -171.8(8) 2_766 . . 2_766 ? O3 N5 O1 O2 8.2(8) . . . 2_766 ? O1 N5 O1 O2 -2(100) 2_766 . . 2_766 ? O2 N5 O1 O3 -8.2(8) . . . 2_766 ? O2 N5 O1 O3 171.8(8) 2_766 . . 2_766 ? O3 N5 O1 O3 180.000(3) . . . 2_766 ? O1 N5 O1 O3 170(100) 2_766 . . 2_766 ? O2 N5 O2 O3 -42(100) 2_766 . . 2_766 ? O3 N5 O2 O3 180.000(4) . . . 2_766 ? O1 N5 O2 O3 -169.6(11) 2_766 . . 2_766 ? O1 N5 O2 O3 10.4(11) . . . 2_766 ? O2 N5 O2 O1 127(100) 2_766 . . 2_766 ? O3 N5 O2 O1 169.6(11) 2_766 . . 2_766 ? O3 N5 O2 O1 -10.4(11) . . . 2_766 ? O1 N5 O2 O1 180.000(2) . . . 2_766 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.685 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 917021' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H46 Ag F3 N8 O2' _chemical_formula_sum 'C52 H46 Ag F3 N8 O2' _chemical_formula_weight 979.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.667(5) _cell_length_b 11.899(5) _cell_length_c 21.743(5) _cell_angle_alpha 93.227(5) _cell_angle_beta 99.083(5) _cell_angle_gamma 100.103(5) _cell_volume 2422.3(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8390 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.90 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8704 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17293 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8460 _reflns_number_gt 6802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1525P)^2^+2.7893P] 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 8460 _refine_ls_number_parameters 599 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2303 _refine_ls_wR_factor_gt 0.2099 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.97373(5) 0.27083(3) 0.483501(18) 0.0707(2) Uani 1 1 d . . . C1 C 0.3621(6) 1.0901(6) 0.1593(3) 0.0763(15) Uani 1 1 d . . . C2 C 0.4625(5) 1.1446(4) 0.1223(2) 0.0569(11) Uani 1 1 d . . . C3 C 0.4129(6) 1.2282(5) 0.0829(3) 0.0650(13) Uani 1 1 d . . . C4 C 0.5942(5) 1.1180(4) 0.1239(2) 0.0484(9) Uani 1 1 d . . . C5 C 0.6964(5) 1.1765(4) 0.0858(2) 0.0536(10) Uani 1 1 d . . . H5A H 0.7482 1.2476 0.1087 0.064 Uiso 1 1 calc R . . H5B H 0.6431 1.1955 0.0474 0.064 Uiso 1 1 calc R . . C6 C 0.8043(5) 1.1031(4) 0.0694(2) 0.0568(11) Uani 1 1 d . . . C7 C 0.7290(7) 1.0007(5) 0.0236(3) 0.0770(15) Uani 1 1 d . . . H7A H 0.6780 1.0272 -0.0126 0.115 Uiso 1 1 calc R . . H7B H 0.6632 0.9510 0.0434 0.115 Uiso 1 1 calc R . . H7C H 0.7983 0.9594 0.0112 0.115 Uiso 1 1 calc R . . C8 C 0.9168(7) 1.1776(6) 0.0394(3) 0.0854(19) Uani 1 1 d . . . H8A H 0.9623 1.2431 0.0678 0.128 Uiso 1 1 calc R . . H8B H 0.8718 1.2026 0.0014 0.128 Uiso 1 1 calc R . . H8C H 0.9867 1.1338 0.0304 0.128 Uiso 1 1 calc R . . C9 C 0.8760(5) 1.0636(4) 0.1307(2) 0.0572(11) Uani 1 1 d . . . H9A H 0.9350 1.0093 0.1208 0.069 Uiso 1 1 calc R . . H9B H 0.9381 1.1292 0.1552 0.069 Uiso 1 1 calc R . . C10 C 0.7727(5) 1.0092(4) 0.1693(2) 0.0492(9) Uani 1 1 d . . . C11 C 0.6409(5) 1.0360(4) 0.1642(2) 0.0556(11) Uani 1 1 d . . . H11 H 0.5777 0.9993 0.1880 0.067 Uiso 1 1 calc R . . C12 C 0.8111(5) 0.9271(4) 0.2119(2) 0.0527(10) Uani 1 1 d . . . H12 H 0.7393 0.8906 0.2317 0.063 Uiso 1 1 calc R . . C13 C 0.9372(5) 0.8980(4) 0.2258(2) 0.0524(10) Uani 1 1 d . . . H13 H 1.0104 0.9355 0.2071 0.063 Uiso 1 1 calc R . . C14 C 0.9719(5) 0.8107(4) 0.2686(2) 0.0496(10) Uani 1 1 d . . . C15 C 1.1123(5) 0.8001(5) 0.2855(3) 0.0727(16) Uani 1 1 d . . . H15 H 1.1830 0.8476 0.2697 0.087 Uiso 1 1 calc R . . C16 C 1.1495(5) 0.7196(6) 0.3257(3) 0.0771(17) Uani 1 1 d . . . H16 H 1.2448 0.7142 0.3372 0.093 Uiso 1 1 calc R . . C17 C 1.0466(5) 0.6486(4) 0.3482(2) 0.0513(10) Uani 1 1 d . . . C18 C 0.9053(5) 0.6577(4) 0.3320(2) 0.0591(12) Uani 1 1 d . . . H18 H 0.8346 0.6097 0.3476 0.071 Uiso 1 1 calc R . . C19 C 0.8703(5) 0.7391(4) 0.2924(2) 0.0594(12) Uani 1 1 d . . . H19 H 0.7751 0.7454 0.2816 0.071 Uiso 1 1 calc R . . C20 C 1.2145(6) 0.5737(7) 0.4286(4) 0.107(3) Uani 1 1 d . . . H20 H 1.2944 0.6315 0.4317 0.129 Uiso 1 1 calc R . . C21 C 1.2020(7) 0.4813(7) 0.4602(4) 0.100(2) Uani 1 1 d . . . H21 H 1.2752 0.4632 0.4888 0.120 Uiso 1 1 calc R . . C22 C 1.0020(5) 0.4729(4) 0.4043(2) 0.0580(11) Uani 1 1 d . . . H22 H 0.9063 0.4498 0.3867 0.070 Uiso 1 1 calc R . . C23 C 0.7705(6) 0.0760(5) 0.5294(3) 0.0760(16) Uani 1 1 d . . . H23 H 0.6924 0.0979 0.5058 0.091 Uiso 1 1 calc R . . C24 C 0.7638(6) -0.0117(5) 0.5653(3) 0.0763(16) Uani 1 1 d . . . H24 H 0.6820 -0.0617 0.5706 0.092 Uiso 1 1 calc R . . C25 C 0.9844(6) 0.0723(4) 0.5708(2) 0.0579(11) Uani 1 1 d . . . H25 H 1.0833 0.0896 0.5813 0.070 Uiso 1 1 calc R . . C26 C 0.9473(5) -0.0926(4) 0.6358(2) 0.0503(10) Uani 1 1 d . . . C27 C 0.8520(6) -0.1496(5) 0.6685(3) 0.0709(15) Uani 1 1 d . . . H27 H 0.7592 -0.1361 0.6640 0.085 Uiso 1 1 calc R . . C28 C 0.8959(6) -0.2289(5) 0.7090(3) 0.0691(14) Uani 1 1 d . . . H28 H 0.8312 -0.2683 0.7312 0.083 Uiso 1 1 calc R . . C29 C 1.0331(5) -0.2497(4) 0.7165(2) 0.0514(10) Uani 1 1 d . . . C30 C 1.1281(5) -0.1879(4) 0.6838(2) 0.0550(11) Uani 1 1 d . . . H30 H 1.2221 -0.1989 0.6892 0.066 Uiso 1 1 calc R . . C31 C 1.0859(5) -0.1105(4) 0.6432(2) 0.0545(11) Uani 1 1 d . . . H31 H 1.1505 -0.0706 0.6210 0.065 Uiso 1 1 calc R . . C32 C 1.0715(5) -0.3373(4) 0.7580(2) 0.0531(10) Uani 1 1 d . . . H32 H 0.9992 -0.3764 0.7766 0.064 Uiso 1 1 calc R . . C33 C 1.1994(5) -0.3659(4) 0.7715(2) 0.0547(11) Uani 1 1 d . . . H33 H 1.2722 -0.3266 0.7532 0.066 Uiso 1 1 calc R . . C34 C 1.2356(5) -0.4531(4) 0.8122(2) 0.0489(10) Uani 1 1 d . . . C35 C 1.1222(5) -0.5196(4) 0.8432(2) 0.0572(11) Uani 1 1 d . . . H35A H 1.0627 -0.5786 0.8131 0.069 Uiso 1 1 calc R . . H35B H 1.0622 -0.4683 0.8559 0.069 Uiso 1 1 calc R . . C36 C 1.1833(5) -0.5764(4) 0.9011(2) 0.0575(11) Uani 1 1 d . . . C37 C 1.2471(7) -0.4878(5) 0.9564(2) 0.0740(15) Uani 1 1 d . . . H37A H 1.2756 -0.5262 0.9926 0.111 Uiso 1 1 calc R . . H37B H 1.1771 -0.4434 0.9647 0.111 Uiso 1 1 calc R . . H37C H 1.3287 -0.4379 0.9466 0.111 Uiso 1 1 calc R . . C38 C 1.0625(7) -0.6633(6) 0.9189(3) 0.0870(19) Uani 1 1 d . . . H38A H 1.0287 -0.7231 0.8857 0.131 Uiso 1 1 calc R . . H38B H 0.9857 -0.6255 0.9259 0.131 Uiso 1 1 calc R . . H38C H 1.0973 -0.6958 0.9564 0.131 Uiso 1 1 calc R . . C39 C 1.2973(5) -0.6397(4) 0.8836(2) 0.0577(11) Uani 1 1 d . . . H39A H 1.3415 -0.6705 0.9205 0.069 Uiso 1 1 calc R . . H39B H 1.2525 -0.7036 0.8532 0.069 Uiso 1 1 calc R . . C40 C 1.4118(5) -0.5638(4) 0.8567(2) 0.0525(10) Uani 1 1 d . . . C41 C 1.3689(5) -0.4746(4) 0.8206(2) 0.0540(10) Uani 1 1 d . . . H41 H 1.4367 -0.4294 0.8021 0.065 Uiso 1 1 calc R . . C42 C 1.5466(6) -0.5844(5) 0.8642(2) 0.0645(12) Uani 1 1 d . . . C43 C 1.5863(7) -0.6799(6) 0.8961(3) 0.0780(16) Uani 1 1 d . . . C44 C 1.6578(7) -0.5151(6) 0.8388(3) 0.0851(18) Uani 1 1 d . . . C45 C 0.6015(11) 0.2688(9) 0.4114(4) 0.111(2) Uani 1 1 d . . . C46 C 0.5355(12) 0.3434(10) 0.3684(5) 0.122(3) Uani 1 1 d . . . C47 C 0.4391(10) 0.0989(9) 0.6176(6) 0.124(3) Uani 1 1 d . . . H47 H 0.4190 0.0283 0.5942 0.149 Uiso 1 1 calc R . . C48 C 0.4921(8) 0.0978(9) 0.6822(5) 0.111(3) Uani 1 1 d . . . H48 H 0.5088 0.0315 0.7004 0.133 Uiso 1 1 calc R . . C49 C 0.5177(8) 0.2066(10) 0.7168(5) 0.116(3) Uani 1 1 d . . . H49 H 0.5536 0.2145 0.7594 0.139 Uiso 1 1 calc R . . C50 C 0.4873(8) 0.3036(10) 0.6849(6) 0.122(3) Uani 1 1 d . . . H50 H 0.5000 0.3743 0.7076 0.146 Uiso 1 1 calc R . . C51 C 0.4378(9) 0.2945(10) 0.6190(6) 0.123(3) Uani 1 1 d . . . H51 H 0.4210 0.3578 0.5978 0.147 Uiso 1 1 calc R . . C52 C 0.4158(11) 0.1830(12) 0.5879(5) 0.127(3) Uani 1 1 d . . . H52 H 0.3838 0.1722 0.5449 0.153 Uiso 1 1 calc R . . F1 F 0.6300(7) 0.4279(5) 0.3529(3) 0.1417(18) Uani 1 1 d . . . F2 F 0.4817(7) 0.2844(6) 0.3103(3) 0.145(2) Uani 1 1 d . . . F3 F 0.4236(7) 0.3733(6) 0.3787(3) 0.148(2) Uani 1 1 d . . . N1 N 0.2844(7) 1.0465(7) 0.1876(4) 0.120(2) Uani 1 1 d . . . N2 N 0.3737(6) 1.2942(5) 0.0526(3) 0.0899(16) Uani 1 1 d . . . N3 N 1.0854(4) 0.5665(4) 0.39034(19) 0.0560(9) Uani 1 1 d . . . N4 N 1.0707(5) 0.4174(4) 0.4457(2) 0.0600(10) Uani 1 1 d . . . N5 N 0.9088(5) 0.1284(3) 0.53263(19) 0.0631(10) Uani 1 1 d . . . N6 N 0.9015(4) -0.0134(3) 0.59297(18) 0.0550(9) Uani 1 1 d . . . N7 N 1.6161(7) -0.7573(6) 0.9194(3) 0.110(2) Uani 1 1 d . . . N9 N 1.7453(7) -0.4618(8) 0.8170(4) 0.133(3) Uani 1 1 d . . . O1 O 0.7280(7) 0.2870(5) 0.4255(3) 0.1099(16) Uani 1 1 d . . . O2 O 0.5229(8) 0.1935(7) 0.4299(3) 0.142(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0959(4) 0.0536(3) 0.0702(3) 0.0320(2) 0.0203(2) 0.0206(2) C1 0.063(3) 0.091(4) 0.084(4) 0.030(3) 0.015(3) 0.032(3) C2 0.059(3) 0.059(3) 0.057(3) 0.015(2) 0.009(2) 0.022(2) C3 0.064(3) 0.063(3) 0.071(3) 0.013(3) 0.002(2) 0.023(2) C4 0.055(2) 0.044(2) 0.048(2) 0.0123(18) 0.0081(18) 0.0154(18) C5 0.065(3) 0.046(2) 0.054(2) 0.0187(19) 0.012(2) 0.017(2) C6 0.063(3) 0.059(3) 0.057(2) 0.025(2) 0.021(2) 0.020(2) C7 0.098(4) 0.076(4) 0.062(3) 0.002(3) 0.014(3) 0.032(3) C8 0.078(4) 0.101(5) 0.097(4) 0.058(4) 0.040(3) 0.031(3) C9 0.053(2) 0.059(3) 0.066(3) 0.025(2) 0.015(2) 0.016(2) C10 0.052(2) 0.047(2) 0.052(2) 0.0167(18) 0.0091(18) 0.0130(18) C11 0.058(3) 0.056(3) 0.060(3) 0.025(2) 0.017(2) 0.016(2) C12 0.057(3) 0.050(2) 0.057(2) 0.021(2) 0.014(2) 0.014(2) C13 0.053(2) 0.044(2) 0.062(3) 0.0213(19) 0.010(2) 0.0083(18) C14 0.050(2) 0.046(2) 0.055(2) 0.0171(19) 0.0080(19) 0.0101(18) C15 0.049(3) 0.076(3) 0.103(4) 0.054(3) 0.023(3) 0.016(2) C16 0.042(2) 0.095(4) 0.104(4) 0.060(4) 0.018(3) 0.020(2) C17 0.049(2) 0.047(2) 0.063(3) 0.026(2) 0.0129(19) 0.0125(18) C18 0.048(2) 0.059(3) 0.076(3) 0.034(2) 0.018(2) 0.010(2) C19 0.041(2) 0.065(3) 0.076(3) 0.031(2) 0.009(2) 0.013(2) C20 0.053(3) 0.123(6) 0.146(6) 0.091(5) 0.000(3) 0.004(3) C21 0.066(4) 0.115(5) 0.121(5) 0.075(5) -0.002(3) 0.022(4) C22 0.060(3) 0.049(2) 0.070(3) 0.028(2) 0.014(2) 0.012(2) C23 0.077(4) 0.067(3) 0.078(3) 0.030(3) -0.010(3) 0.010(3) C24 0.062(3) 0.073(3) 0.087(4) 0.039(3) -0.012(3) 0.006(3) C25 0.067(3) 0.048(2) 0.059(3) 0.022(2) 0.006(2) 0.013(2) C26 0.059(3) 0.046(2) 0.047(2) 0.0184(18) 0.0021(18) 0.0114(19) C27 0.056(3) 0.079(3) 0.085(3) 0.049(3) 0.010(2) 0.019(2) C28 0.058(3) 0.076(3) 0.082(3) 0.049(3) 0.018(2) 0.020(2) C29 0.057(2) 0.051(2) 0.047(2) 0.0197(19) 0.0045(18) 0.0106(19) C30 0.054(2) 0.061(3) 0.054(2) 0.020(2) 0.0084(19) 0.019(2) C31 0.059(3) 0.054(3) 0.054(2) 0.024(2) 0.012(2) 0.010(2) C32 0.056(3) 0.053(3) 0.053(2) 0.023(2) 0.0077(19) 0.013(2) C33 0.062(3) 0.056(3) 0.049(2) 0.023(2) 0.010(2) 0.012(2) C34 0.052(2) 0.051(2) 0.046(2) 0.0155(18) 0.0066(18) 0.0131(19) C35 0.057(3) 0.062(3) 0.059(3) 0.028(2) 0.015(2) 0.018(2) C36 0.065(3) 0.054(3) 0.061(3) 0.028(2) 0.018(2) 0.017(2) C37 0.107(4) 0.067(3) 0.058(3) 0.023(2) 0.022(3) 0.031(3) C38 0.084(4) 0.080(4) 0.112(5) 0.058(4) 0.039(4) 0.020(3) C39 0.068(3) 0.050(2) 0.058(3) 0.022(2) 0.008(2) 0.017(2) C40 0.056(3) 0.053(2) 0.051(2) 0.0117(19) 0.0064(19) 0.017(2) C41 0.059(3) 0.054(2) 0.053(2) 0.022(2) 0.0114(19) 0.012(2) C42 0.063(3) 0.070(3) 0.065(3) 0.021(2) 0.007(2) 0.024(2) C43 0.079(4) 0.089(4) 0.076(3) 0.020(3) 0.007(3) 0.042(3) C44 0.063(3) 0.101(5) 0.102(5) 0.030(4) 0.020(3) 0.035(3) C45 0.104(6) 0.114(7) 0.115(6) 0.012(5) 0.015(5) 0.023(5) C46 0.117(7) 0.123(8) 0.127(8) 0.019(6) 0.019(6) 0.026(6) C47 0.094(6) 0.116(7) 0.160(10) 0.006(7) 0.037(6) 0.002(5) C48 0.076(4) 0.141(8) 0.130(7) 0.040(6) 0.045(5) 0.026(5) C49 0.068(4) 0.167(9) 0.114(6) 0.005(6) 0.046(4) 0.001(5) C50 0.072(5) 0.144(8) 0.159(9) 0.017(7) 0.050(5) 0.019(5) C51 0.076(5) 0.137(8) 0.162(9) 0.036(7) 0.041(5) 0.015(5) C52 0.118(7) 0.148(10) 0.114(7) 0.018(7) 0.014(5) 0.022(7) F1 0.144(4) 0.133(4) 0.148(4) 0.033(4) 0.024(4) 0.017(4) F2 0.145(5) 0.151(5) 0.132(4) 0.020(4) 0.008(4) 0.020(4) F3 0.129(4) 0.146(5) 0.176(5) 0.022(4) 0.024(4) 0.047(4) N1 0.084(4) 0.163(7) 0.138(6) 0.070(5) 0.057(4) 0.041(4) N2 0.097(4) 0.079(3) 0.098(4) 0.026(3) -0.003(3) 0.041(3) N3 0.050(2) 0.057(2) 0.067(2) 0.0298(19) 0.0134(17) 0.0154(17) N4 0.068(3) 0.056(2) 0.062(2) 0.0244(19) 0.0159(19) 0.0191(19) N5 0.078(3) 0.051(2) 0.061(2) 0.0233(18) 0.005(2) 0.013(2) N6 0.062(2) 0.047(2) 0.056(2) 0.0232(17) 0.0033(17) 0.0111(17) N7 0.118(5) 0.119(5) 0.110(5) 0.042(4) 0.006(4) 0.071(4) N9 0.076(4) 0.169(7) 0.177(7) 0.076(6) 0.051(4) 0.038(4) O1 0.103(4) 0.114(4) 0.113(4) 0.013(3) 0.013(3) 0.025(3) O2 0.138(6) 0.138(6) 0.146(6) 0.034(5) 0.017(4) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.104(4) . ? Ag1 N5 2.110(4) . ? Ag1 O1 2.552(6) . ? C1 N1 1.121(8) . ? C1 C2 1.448(8) . ? C2 C4 1.360(7) . ? C2 C3 1.445(7) . ? C3 N2 1.130(7) . ? C4 C11 1.431(6) . ? C4 C5 1.493(6) . ? C5 C6 1.543(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.526(8) . ? C6 C8 1.531(7) . ? C6 C9 1.541(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.489(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.356(7) . ? C10 C12 1.440(6) . ? C11 H11 0.9300 . ? C12 C13 1.320(6) . ? C12 H12 0.9300 . ? C13 C14 1.480(6) . ? C13 H13 0.9300 . ? C14 C19 1.368(6) . ? C14 C15 1.379(7) . ? C15 C16 1.388(7) . ? C15 H15 0.9300 . ? C16 C17 1.361(7) . ? C16 H16 0.9300 . ? C17 C18 1.380(7) . ? C17 N3 1.434(5) . ? C18 C19 1.384(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.327(9) . ? C20 N3 1.372(7) . ? C20 H20 0.9300 . ? C21 N4 1.340(8) . ? C21 H21 0.9300 . ? C22 N4 1.312(6) . ? C22 N3 1.335(6) . ? C22 H22 0.9300 . ? C23 C24 1.336(8) . ? C23 N5 1.362(8) . ? C23 H23 0.9300 . ? C24 N6 1.376(7) . ? C24 H24 0.9300 . ? C25 N5 1.307(6) . ? C25 N6 1.343(6) . ? C25 H25 0.9300 . ? C26 C27 1.362(7) . ? C26 C31 1.379(7) . ? C26 N6 1.438(5) . ? C27 C28 1.400(7) . ? C27 H27 0.9300 . ? C28 C29 1.378(7) . ? C28 H28 0.9300 . ? C29 C30 1.385(6) . ? C29 C32 1.474(6) . ? C30 C31 1.380(6) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.334(7) . ? C32 H32 0.9300 . ? C33 C34 1.454(6) . ? C33 H33 0.9300 . ? C34 C41 1.343(7) . ? C34 C35 1.508(6) . ? C35 C36 1.545(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C39 1.523(7) . ? C36 C37 1.528(8) . ? C36 C38 1.533(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.515(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C42 1.354(7) . ? C40 C41 1.435(6) . ? C41 H41 0.9300 . ? C42 C44 1.438(9) . ? C42 C43 1.441(8) . ? C43 N7 1.135(8) . ? C44 N9 1.146(9) . ? C45 O1 1.191(10) . ? C45 O2 1.200(11) . ? C45 C46 1.473(14) . ? C46 F3 1.245(11) . ? C46 F1 1.332(12) . ? C46 F2 1.388(12) . ? C47 C52 1.255(15) . ? C47 C48 1.419(14) . ? C47 H47 0.9300 . ? C48 C49 1.422(13) . ? C48 H48 0.9300 . ? C49 C50 1.429(14) . ? C49 H49 0.9300 . ? C50 C51 1.429(14) . ? C50 H50 0.9300 . ? C51 C52 1.421(15) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N5 170.24(16) . . ? N4 Ag1 O1 91.59(18) . . ? N5 Ag1 O1 97.74(18) . . ? N1 C1 C2 179.0(8) . . ? C4 C2 C3 122.2(5) . . ? C4 C2 C1 122.3(4) . . ? C3 C2 C1 115.5(5) . . ? N2 C3 C2 179.3(7) . . ? C2 C4 C11 120.8(4) . . ? C2 C4 C5 121.2(4) . . ? C11 C4 C5 118.0(4) . . ? C4 C5 C6 113.2(4) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C8 109.4(5) . . ? C7 C6 C9 111.1(4) . . ? C8 C6 C9 109.6(4) . . ? C7 C6 C5 110.4(4) . . ? C8 C6 C5 108.5(4) . . ? C9 C6 C5 107.8(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 113.5(4) . . ? C10 C9 H9A 108.9 . . ? C6 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C6 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C12 119.3(4) . . ? C11 C10 C9 120.2(4) . . ? C12 C10 C9 120.4(4) . . ? C10 C11 C4 123.3(4) . . ? C10 C11 H11 118.4 . . ? C4 C11 H11 118.4 . . ? C13 C12 C10 126.9(4) . . ? C13 C12 H12 116.5 . . ? C10 C12 H12 116.5 . . ? C12 C13 C14 125.4(4) . . ? C12 C13 H13 117.3 . . ? C14 C13 H13 117.3 . . ? C19 C14 C15 118.1(4) . . ? C19 C14 C13 122.9(4) . . ? C15 C14 C13 119.0(4) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.1(4) . . ? C16 C17 N3 119.9(4) . . ? C18 C17 N3 120.0(4) . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C14 C19 C18 121.8(4) . . ? C14 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 N3 105.8(6) . . ? C21 C20 H20 127.1 . . ? N3 C20 H20 127.1 . . ? C20 C21 N4 111.6(5) . . ? C20 C21 H21 124.2 . . ? N4 C21 H21 124.2 . . ? N4 C22 N3 112.1(5) . . ? N4 C22 H22 123.9 . . ? N3 C22 H22 123.9 . . ? C24 C23 N5 109.9(5) . . ? C24 C23 H23 125.1 . . ? N5 C23 H23 125.1 . . ? C23 C24 N6 106.6(5) . . ? C23 C24 H24 126.7 . . ? N6 C24 H24 126.7 . . ? N5 C25 N6 111.6(5) . . ? N5 C25 H25 124.2 . . ? N6 C25 H25 124.2 . . ? C27 C26 C31 120.9(4) . . ? C27 C26 N6 119.1(4) . . ? C31 C26 N6 120.0(4) . . ? C26 C27 C28 118.9(5) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 121.4(5) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 118.0(4) . . ? C28 C29 C32 118.9(4) . . ? C30 C29 C32 123.1(4) . . ? C31 C30 C29 121.2(4) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C26 C31 C30 119.5(4) . . ? C26 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C33 C32 C29 126.5(4) . . ? C33 C32 H32 116.8 . . ? C29 C32 H32 116.8 . . ? C32 C33 C34 126.0(4) . . ? C32 C33 H33 117.0 . . ? C34 C33 H33 117.0 . . ? C41 C34 C33 119.5(4) . . ? C41 C34 C35 121.1(4) . . ? C33 C34 C35 119.5(4) . . ? C34 C35 C36 113.4(4) . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C39 C36 C37 109.9(4) . . ? C39 C36 C38 108.8(4) . . ? C37 C36 C38 109.6(5) . . ? C39 C36 C35 108.5(4) . . ? C37 C36 C35 111.5(4) . . ? C38 C36 C35 108.5(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C36 112.8(4) . . ? C40 C39 H39A 109.0 . . ? C36 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C36 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C42 C40 C41 122.2(5) . . ? C42 C40 C39 120.5(4) . . ? C41 C40 C39 117.2(4) . . ? C34 C41 C40 123.3(4) . . ? C34 C41 H41 118.4 . . ? C40 C41 H41 118.4 . . ? C40 C42 C44 122.2(5) . . ? C40 C42 C43 122.1(5) . . ? C44 C42 C43 115.7(5) . . ? N7 C43 C42 177.7(8) . . ? N9 C44 C42 178.1(9) . . ? O1 C45 O2 124.5(10) . . ? O1 C45 C46 118.3(10) . . ? O2 C45 C46 117.2(10) . . ? F3 C46 F1 113.7(10) . . ? F3 C46 F2 97.7(9) . . ? F1 C46 F2 100.5(8) . . ? F3 C46 C45 118.5(10) . . ? F1 C46 C45 113.0(9) . . ? F2 C46 C45 110.5(9) . . ? C52 C47 C48 128.3(11) . . ? C52 C47 H47 115.9 . . ? C48 C47 H47 115.9 . . ? C47 C48 C49 114.4(9) . . ? C47 C48 H48 122.8 . . ? C49 C48 H48 122.8 . . ? C48 C49 C50 118.8(9) . . ? C48 C49 H49 120.6 . . ? C50 C49 H49 120.6 . . ? C49 C50 C51 121.6(10) . . ? C49 C50 H50 119.2 . . ? C51 C50 H50 119.2 . . ? C52 C51 C50 116.0(10) . . ? C52 C51 H51 122.0 . . ? C50 C51 H51 122.0 . . ? C47 C52 C51 120.8(11) . . ? C47 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C22 N3 C20 105.8(4) . . ? C22 N3 C17 127.7(4) . . ? C20 N3 C17 126.4(4) . . ? C22 N4 C21 104.6(4) . . ? C22 N4 Ag1 123.6(4) . . ? C21 N4 Ag1 131.5(4) . . ? C25 N5 C23 105.8(4) . . ? C25 N5 Ag1 130.2(4) . . ? C23 N5 Ag1 124.0(3) . . ? C25 N6 C24 106.1(4) . . ? C25 N6 C26 127.1(4) . . ? C24 N6 C26 126.8(4) . . ? C45 O1 Ag1 158.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C4 -61(42) . . . . ? N1 C1 C2 C3 119(42) . . . . ? C4 C2 C3 N2 -130(64) . . . . ? C1 C2 C3 N2 51(64) . . . . ? C3 C2 C4 C11 179.0(5) . . . . ? C1 C2 C4 C11 -1.7(8) . . . . ? C3 C2 C4 C5 1.4(7) . . . . ? C1 C2 C4 C5 -179.3(5) . . . . ? C2 C4 C5 C6 -153.5(4) . . . . ? C11 C4 C5 C6 28.8(6) . . . . ? C4 C5 C6 C7 68.7(5) . . . . ? C4 C5 C6 C8 -171.3(4) . . . . ? C4 C5 C6 C9 -52.8(5) . . . . ? C7 C6 C9 C10 -69.8(6) . . . . ? C8 C6 C9 C10 169.1(5) . . . . ? C5 C6 C9 C10 51.3(6) . . . . ? C6 C9 C10 C11 -25.8(7) . . . . ? C6 C9 C10 C12 153.7(4) . . . . ? C12 C10 C11 C4 178.9(4) . . . . ? C9 C10 C11 C4 -1.6(7) . . . . ? C2 C4 C11 C10 -177.6(5) . . . . ? C5 C4 C11 C10 0.1(7) . . . . ? C11 C10 C12 C13 -174.6(5) . . . . ? C9 C10 C12 C13 5.9(8) . . . . ? C10 C12 C13 C14 -178.2(5) . . . . ? C12 C13 C14 C19 9.0(8) . . . . ? C12 C13 C14 C15 -171.2(5) . . . . ? C19 C14 C15 C16 -0.3(9) . . . . ? C13 C14 C15 C16 179.9(6) . . . . ? C14 C15 C16 C17 1.0(11) . . . . ? C15 C16 C17 C18 -1.1(10) . . . . ? C15 C16 C17 N3 -179.2(6) . . . . ? C16 C17 C18 C19 0.6(8) . . . . ? N3 C17 C18 C19 178.6(5) . . . . ? C15 C14 C19 C18 -0.2(8) . . . . ? C13 C14 C19 C18 179.6(5) . . . . ? C17 C18 C19 C14 0.1(9) . . . . ? N3 C20 C21 N4 -2.0(11) . . . . ? N5 C23 C24 N6 1.2(8) . . . . ? C31 C26 C27 C28 -1.3(9) . . . . ? N6 C26 C27 C28 178.4(5) . . . . ? C26 C27 C28 C29 0.3(10) . . . . ? C27 C28 C29 C30 1.4(9) . . . . ? C27 C28 C29 C32 -177.7(5) . . . . ? C28 C29 C30 C31 -2.1(8) . . . . ? C32 C29 C30 C31 177.0(5) . . . . ? C27 C26 C31 C30 0.6(8) . . . . ? N6 C26 C31 C30 -179.0(4) . . . . ? C29 C30 C31 C26 1.1(8) . . . . ? C28 C29 C32 C33 -178.3(5) . . . . ? C30 C29 C32 C33 2.6(8) . . . . ? C29 C32 C33 C34 -179.5(5) . . . . ? C32 C33 C34 C41 178.6(5) . . . . ? C32 C33 C34 C35 -0.1(8) . . . . ? C41 C34 C35 C36 21.5(7) . . . . ? C33 C34 C35 C36 -159.8(4) . . . . ? C34 C35 C36 C39 -48.6(6) . . . . ? C34 C35 C36 C37 72.6(6) . . . . ? C34 C35 C36 C38 -166.7(5) . . . . ? C37 C36 C39 C40 -67.9(5) . . . . ? C38 C36 C39 C40 172.1(5) . . . . ? C35 C36 C39 C40 54.3(5) . . . . ? C36 C39 C40 C42 150.4(5) . . . . ? C36 C39 C40 C41 -32.9(6) . . . . ? C33 C34 C41 C40 -176.0(4) . . . . ? C35 C34 C41 C40 2.7(7) . . . . ? C42 C40 C41 C34 179.6(5) . . . . ? C39 C40 C41 C34 2.9(7) . . . . ? C41 C40 C42 C44 2.8(8) . . . . ? C39 C40 C42 C44 179.3(5) . . . . ? C41 C40 C42 C43 -174.7(5) . . . . ? C39 C40 C42 C43 1.8(8) . . . . ? C40 C42 C43 N7 84(20) . . . . ? C44 C42 C43 N7 -93(20) . . . . ? C40 C42 C44 N9 -89(22) . . . . ? C43 C42 C44 N9 89(22) . . . . ? O1 C45 C46 F3 -140.0(10) . . . . ? O2 C45 C46 F3 40.0(15) . . . . ? O1 C45 C46 F1 -3.2(14) . . . . ? O2 C45 C46 F1 176.8(9) . . . . ? O1 C45 C46 F2 108.5(10) . . . . ? O2 C45 C46 F2 -71.5(12) . . . . ? C52 C47 C48 C49 1.8(14) . . . . ? C47 C48 C49 C50 0.8(10) . . . . ? C48 C49 C50 C51 -2.7(11) . . . . ? C49 C50 C51 C52 2.3(11) . . . . ? C48 C47 C52 C51 -2.2(17) . . . . ? C50 C51 C52 C47 0.1(14) . . . . ? N4 C22 N3 C20 -3.6(7) . . . . ? N4 C22 N3 C17 -178.7(5) . . . . ? C21 C20 N3 C22 3.3(9) . . . . ? C21 C20 N3 C17 178.5(6) . . . . ? C16 C17 N3 C22 -161.4(6) . . . . ? C18 C17 N3 C22 20.6(8) . . . . ? C16 C17 N3 C20 24.4(9) . . . . ? C18 C17 N3 C20 -153.6(7) . . . . ? N3 C22 N4 C21 2.4(7) . . . . ? N3 C22 N4 Ag1 176.5(3) . . . . ? C20 C21 N4 C22 -0.1(9) . . . . ? C20 C21 N4 Ag1 -173.7(6) . . . . ? N5 Ag1 N4 C22 -167.2(8) . . . . ? O1 Ag1 N4 C22 -4.4(4) . . . . ? N5 Ag1 N4 C21 5.3(13) . . . . ? O1 Ag1 N4 C21 168.1(6) . . . . ? N6 C25 N5 C23 -0.6(6) . . . . ? N6 C25 N5 Ag1 179.4(3) . . . . ? C24 C23 N5 C25 -0.4(7) . . . . ? C24 C23 N5 Ag1 179.6(4) . . . . ? N4 Ag1 N5 C25 -19.4(12) . . . . ? O1 Ag1 N5 C25 178.0(5) . . . . ? N4 Ag1 N5 C23 160.5(8) . . . . ? O1 Ag1 N5 C23 -2.1(5) . . . . ? N5 C25 N6 C24 1.3(6) . . . . ? N5 C25 N6 C26 -179.9(4) . . . . ? C23 C24 N6 C25 -1.5(7) . . . . ? C23 C24 N6 C26 179.8(5) . . . . ? C27 C26 N6 C25 159.5(5) . . . . ? C31 C26 N6 C25 -20.8(7) . . . . ? C27 C26 N6 C24 -21.9(8) . . . . ? C31 C26 N6 C24 157.7(5) . . . . ? O2 C45 O1 Ag1 -9(2) . . . . ? C46 C45 O1 Ag1 170.8(12) . . . . ? N4 Ag1 O1 C45 -168.0(17) . . . . ? N5 Ag1 O1 C45 9.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.174 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 917022' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H40 Ag F6 N8 P' _chemical_formula_sum 'C50 H40 Ag F6 N8 P' _chemical_formula_weight 1005.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.738(2) _cell_length_b 11.756(2) _cell_length_c 21.462(4) _cell_angle_alpha 94.268(3) _cell_angle_beta 96.334(3) _cell_angle_gamma 98.170(3) _cell_volume 2407.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2319 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 19.63 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8601 _exptl_absorpt_correction_T_max 0.9035 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17215 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8383 _reflns_number_gt 4499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8383 _refine_ls_number_parameters 599 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1330 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.052 _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 0.02110(6) 0.22984(4) 0.51384(2) 0.0650(3) Uani 1 1 d . . . P1 P 0.4531(2) 0.18562(19) 0.60275(11) 0.0712(6) Uani 1 1 d . . . N3 N -0.0746(5) -0.0574(4) 0.6156(2) 0.0495(13) Uani 1 1 d . . . C17 C -0.0369(6) -0.1399(5) 0.6572(3) 0.0476(15) Uani 1 1 d . . . N6 N 0.0938(5) 0.5098(4) 0.4024(2) 0.0502(13) Uani 1 1 d . . . N4 N -0.0614(5) 0.0889(4) 0.5576(2) 0.0515(13) Uani 1 1 d . . . C47 C 0.4397(11) 0.7977(11) 0.6139(8) 0.116(4) Uani 1 1 d . . . C14 C 0.0357(6) -0.3059(5) 0.7360(3) 0.0456(15) Uani 1 1 d . . . C26 C 0.0485(6) 0.5904(5) 0.3607(3) 0.0458(15) Uani 1 1 d . . . C4 C 0.4116(7) -0.6167(5) 0.8751(3) 0.0497(16) Uani 1 1 d . . . C13 C 0.0695(6) -0.3932(5) 0.7778(3) 0.0484(16) Uani 1 1 d . . . H13 H -0.0021 -0.4283 0.7984 0.058 Uiso 1 1 calc R . . C34 C -0.2441(7) 0.9530(5) 0.1875(3) 0.0484(16) Uani 1 1 d . . . C35 C -0.1348(7) 1.0147(6) 0.1532(3) 0.0554(17) Uani 1 1 d . . . H35A H -0.0764 0.9602 0.1390 0.066 Uiso 1 1 calc R . . H35B H -0.0759 1.0735 0.1823 0.066 Uiso 1 1 calc R . . N5 N 0.0911(6) 0.3683(5) 0.4639(2) 0.0593(15) Uani 1 1 d . . . C28 C -0.1316(7) 0.6852(5) 0.3149(3) 0.0515(16) Uani 1 1 d . . . H28 H -0.2251 0.6952 0.3103 0.062 Uiso 1 1 calc R . . C29 C -0.0409(7) 0.7494(5) 0.2817(3) 0.0474(16) Uani 1 1 d . . . C32 C -0.0805(7) 0.8362(5) 0.2408(3) 0.0486(16) Uani 1 1 d . . . H32 H -0.0102 0.8749 0.2208 0.058 Uiso 1 1 calc R . . C11 C 0.3636(7) -0.5348(5) 0.8349(3) 0.0529(17) Uani 1 1 d . . . H11 H 0.4250 -0.4988 0.8096 0.063 Uiso 1 1 calc R . . C16 C -0.1365(7) -0.2044(7) 0.6849(4) 0.076(2) Uani 1 1 d . . . H16 H -0.2292 -0.1932 0.6771 0.091 Uiso 1 1 calc R . . C2 C 0.5439(7) -0.6437(6) 0.8757(3) 0.0565(17) Uani 1 1 d . . . C41 C -0.5528(7) 1.0895(6) 0.1401(3) 0.0640(19) Uani 1 1 d . . . F4 F 0.5755(6) 0.1366(6) 0.6409(3) 0.153(2) Uani 1 1 d . . . C5 C 0.3113(6) -0.6743(5) 0.9150(3) 0.0514(16) Uani 1 1 d . . . H5A H 0.3634 -0.6933 0.9530 0.062 Uiso 1 1 calc R . . H5B H 0.2636 -0.7460 0.8923 0.062 Uiso 1 1 calc R . . C9 C 0.1314(7) -0.5590(6) 0.8737(3) 0.0583(18) Uani 1 1 d . . . H9A H 0.0701 -0.6237 0.8499 0.070 Uiso 1 1 calc R . . H9B H 0.0742 -0.5018 0.8857 0.070 Uiso 1 1 calc R . . C6 C 0.2021(7) -0.6006(5) 0.9333(3) 0.0526(17) Uani 1 1 d . . . C40 C -0.4181(7) 1.0667(5) 0.1456(3) 0.0505(16) Uani 1 1 d . . . C20 C 0.0066(6) 0.0311(5) 0.5977(3) 0.0499(16) Uani 1 1 d . . . H20 H 0.1014 0.0505 0.6120 0.060 Uiso 1 1 calc R . . C43 C -0.6635(9) 1.0231(8) 0.1676(4) 0.084(2) Uani 1 1 d . . . C30 C 0.0972(7) 0.7304(6) 0.2882(3) 0.0583(18) Uani 1 1 d . . . H30 H 0.1612 0.7726 0.2663 0.070 Uiso 1 1 calc R . . C33 C -0.2079(7) 0.8654(5) 0.2292(3) 0.0482(16) Uani 1 1 d . . . H33 H -0.2790 0.8274 0.2490 0.058 Uiso 1 1 calc R . . C36 C -0.1948(7) 1.0726(6) 0.0956(3) 0.0566(17) Uani 1 1 d . . . C44 C -0.3764(7) 0.9775(5) 0.1823(3) 0.0543(17) Uani 1 1 d . . . H44 H -0.4423 0.9351 0.2031 0.065 Uiso 1 1 calc R . . C27 C -0.0898(6) 0.6066(5) 0.3547(3) 0.0492(16) Uani 1 1 d . . . H27 H -0.1534 0.5653 0.3771 0.059 Uiso 1 1 calc R . . C31 C 0.1417(7) 0.6497(6) 0.3267(3) 0.0602(18) Uani 1 1 d . . . H31 H 0.2338 0.6359 0.3295 0.072 Uiso 1 1 calc R . . C1 C 0.5911(7) -0.7298(6) 0.9142(3) 0.0634(19) Uani 1 1 d . . . F5 F 0.3240(7) 0.2287(7) 0.5695(3) 0.173(3) Uani 1 1 d . . . C10 C 0.2336(6) -0.5074(5) 0.8322(3) 0.0469(15) Uani 1 1 d . . . F3 F 0.3418(6) 0.1083(6) 0.6343(3) 0.157(3) Uani 1 1 d . . . C19 C 0.1352(7) -0.2387(6) 0.7075(3) 0.0575(18) Uani 1 1 d . . . H19 H 0.2281 -0.2497 0.7148 0.069 Uiso 1 1 calc R . . N1 N 0.6303(8) -0.7955(6) 0.9439(3) 0.099(2) Uani 1 1 d . . . C18 C 0.1007(6) -0.1556(6) 0.6686(3) 0.0563(18) Uani 1 1 d . . . H18 H 0.1696 -0.1111 0.6504 0.068 Uiso 1 1 calc R . . F6 F 0.5658(8) 0.2618(7) 0.5750(3) 0.202(4) Uani 1 1 d . . . C39 C -0.3097(7) 1.1398(5) 0.1165(3) 0.0572(18) Uani 1 1 d . . . H39A H -0.2668 1.2042 0.1465 0.069 Uiso 1 1 calc R . . H39B H -0.3541 1.1710 0.0802 0.069 Uiso 1 1 calc R . . F1 F 0.4506(7) 0.0921(7) 0.5490(3) 0.178(3) Uani 1 1 d . . . F2 F 0.4611(7) 0.2783(7) 0.6590(4) 0.173(3) Uani 1 1 d . . . C24 C 0.2315(7) 0.5019(7) 0.4246(4) 0.078(2) Uani 1 1 d . . . H24 H 0.3114 0.5483 0.4159 0.093 Uiso 1 1 calc R . . C7 C 0.2724(8) -0.4969(6) 0.9781(3) 0.077(2) Uani 1 1 d . . . H7A H 0.3342 -0.4472 0.9565 0.115 Uiso 1 1 calc R . . H7B H 0.3248 -0.5230 1.0134 0.115 Uiso 1 1 calc R . . H7C H 0.2024 -0.4552 0.9927 0.115 Uiso 1 1 calc R . . C12 C 0.1935(7) -0.4266(5) 0.7888(3) 0.0498(16) Uani 1 1 d . . . H12 H 0.2626 -0.3943 0.7659 0.060 Uiso 1 1 calc R . . C38 C -0.0780(8) 1.1570(7) 0.0754(4) 0.083(2) Uani 1 1 d . . . H38A H -0.0031 1.1166 0.0654 0.125 Uiso 1 1 calc R . . H38B H -0.0440 1.2161 0.1091 0.125 Uiso 1 1 calc R . . H38C H -0.1131 1.1917 0.0390 0.125 Uiso 1 1 calc R . . C8 C 0.0903(8) -0.6736(7) 0.9652(4) 0.082(2) Uani 1 1 d . . . H8A H 0.0192 -0.6284 0.9744 0.123 Uiso 1 1 calc R . . H8B H 0.1329 -0.6975 1.0035 0.123 Uiso 1 1 calc R . . H8C H 0.0492 -0.7404 0.9374 0.123 Uiso 1 1 calc R . . N2 N 0.7199(8) -0.5419(8) 0.8094(4) 0.114(3) Uani 1 1 d . . . C15 C -0.1020(7) -0.2860(6) 0.7241(4) 0.072(2) Uani 1 1 d . . . H15 H -0.1715 -0.3284 0.7430 0.086 Uiso 1 1 calc R . . C25 C 0.0152(7) 0.4262(5) 0.4274(3) 0.0565(17) Uani 1 1 d . . . H25 H -0.0818 0.4110 0.4198 0.068 Uiso 1 1 calc R . . C3 C 0.6415(9) -0.5882(7) 0.8379(4) 0.075(2) Uani 1 1 d . . . C49 C 0.5122(9) 0.7084(14) 0.7067(5) 0.104(3) Uani 1 1 d . . . C37 C -0.2565(8) 0.9828(6) 0.0414(3) 0.073(2) Uani 1 1 d . . . H37A H -0.2902 1.0206 0.0059 0.109 Uiso 1 1 calc R . . H37B H -0.3325 0.9321 0.0542 0.109 Uiso 1 1 calc R . . H37C H -0.1858 0.9389 0.0298 0.109 Uiso 1 1 calc R . . C23 C 0.2258(8) 0.4123(7) 0.4619(4) 0.080(2) Uani 1 1 d . . . H23 H 0.3027 0.3860 0.4825 0.096 Uiso 1 1 calc R . . C50 C 0.4830(10) 0.6028(11) 0.6745(7) 0.105(3) Uani 1 1 d . . . C21 C -0.2037(8) -0.0572(7) 0.5836(4) 0.088(3) Uani 1 1 d U . . H21 H -0.2835 -0.1100 0.5857 0.106 Uiso 1 1 calc R . . C48 C 0.4881(10) 0.8078(11) 0.6778(8) 0.112(4) Uani 1 1 d . . . C45 C 0.4329(11) 0.5889(10) 0.6124(7) 0.115(4) Uani 1 1 d . . . C22 C -0.1947(8) 0.0320(7) 0.5491(4) 0.084(3) Uani 1 1 d . . . H22 H -0.2683 0.0524 0.5231 0.101 Uiso 1 1 calc R . . N7 N -0.7506(9) 0.9691(9) 0.1892(5) 0.127(3) Uani 1 1 d . . . C42 C -0.5903(8) 1.1855(7) 0.1085(4) 0.075(2) Uani 1 1 d . . . N8 N -0.6197(9) 1.2631(7) 0.0842(4) 0.115(3) Uani 1 1 d . . . C46 C 0.4076(10) 0.6904(14) 0.5813(5) 0.113(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0801(4) 0.0492(4) 0.0685(4) 0.0265(3) 0.0052(3) 0.0114(3) P1 0.0525(12) 0.0716(14) 0.0882(16) 0.0078(12) 0.0104(11) 0.0030(10) N3 0.035(3) 0.049(3) 0.067(3) 0.027(3) 0.002(2) 0.007(2) C17 0.038(4) 0.045(4) 0.062(4) 0.018(3) 0.005(3) 0.007(3) N6 0.055(3) 0.045(3) 0.050(3) 0.016(2) 0.001(3) 0.006(3) N4 0.048(3) 0.046(3) 0.061(3) 0.016(3) 0.002(3) 0.007(3) C47 0.066(7) 0.098(9) 0.193(14) 0.033(9) 0.045(8) 0.010(6) C14 0.048(4) 0.039(4) 0.052(4) 0.010(3) 0.006(3) 0.008(3) C26 0.043(4) 0.046(4) 0.048(4) 0.012(3) -0.005(3) 0.010(3) C4 0.062(4) 0.044(4) 0.048(4) 0.012(3) 0.011(3) 0.015(3) C13 0.041(4) 0.048(4) 0.058(4) 0.019(3) 0.008(3) 0.005(3) C34 0.059(4) 0.040(4) 0.048(4) 0.010(3) 0.004(3) 0.012(3) C35 0.063(4) 0.054(4) 0.056(4) 0.024(3) 0.014(3) 0.013(3) N5 0.067(4) 0.055(3) 0.058(4) 0.025(3) -0.003(3) 0.014(3) C28 0.053(4) 0.058(4) 0.046(4) 0.010(3) 0.004(3) 0.016(3) C29 0.056(4) 0.046(4) 0.042(4) 0.014(3) 0.001(3) 0.011(3) C32 0.054(4) 0.048(4) 0.046(4) 0.017(3) 0.005(3) 0.011(3) C11 0.061(4) 0.048(4) 0.054(4) 0.022(3) 0.012(3) 0.012(3) C16 0.028(4) 0.092(6) 0.117(6) 0.062(5) 0.015(4) 0.010(4) C2 0.055(4) 0.054(4) 0.062(4) 0.014(3) 0.000(3) 0.013(3) C41 0.060(5) 0.066(5) 0.071(5) 0.022(4) 0.005(4) 0.021(4) F4 0.095(4) 0.175(6) 0.189(6) 0.033(5) -0.017(4) 0.046(4) C5 0.062(4) 0.043(4) 0.051(4) 0.011(3) 0.006(3) 0.013(3) C9 0.060(4) 0.054(4) 0.064(4) 0.019(3) 0.010(3) 0.010(3) C6 0.066(4) 0.046(4) 0.050(4) 0.018(3) 0.014(3) 0.012(3) C40 0.054(4) 0.043(4) 0.054(4) 0.009(3) -0.001(3) 0.010(3) C20 0.037(3) 0.050(4) 0.063(4) 0.019(3) -0.003(3) 0.005(3) C43 0.067(6) 0.095(7) 0.096(7) 0.024(5) 0.002(5) 0.031(5) C30 0.047(4) 0.068(5) 0.065(4) 0.034(4) 0.009(3) 0.011(3) C33 0.059(4) 0.041(4) 0.046(4) 0.013(3) 0.010(3) 0.008(3) C36 0.066(4) 0.049(4) 0.057(4) 0.020(3) 0.008(3) 0.007(3) C44 0.053(4) 0.056(4) 0.057(4) 0.022(3) 0.006(3) 0.011(3) C27 0.051(4) 0.047(4) 0.051(4) 0.023(3) 0.007(3) 0.005(3) C31 0.042(4) 0.068(5) 0.076(5) 0.035(4) 0.008(3) 0.011(3) C1 0.066(5) 0.051(4) 0.077(5) 0.008(4) 0.006(4) 0.020(4) F5 0.151(6) 0.186(7) 0.184(6) 0.036(5) -0.052(5) 0.078(5) C10 0.050(4) 0.044(4) 0.049(4) 0.011(3) 0.007(3) 0.012(3) F3 0.094(4) 0.186(7) 0.187(6) 0.043(5) 0.047(4) -0.029(4) C19 0.041(4) 0.063(4) 0.072(5) 0.029(4) 0.005(3) 0.011(3) N1 0.112(6) 0.072(5) 0.116(6) 0.030(4) -0.015(5) 0.039(4) C18 0.038(4) 0.063(4) 0.074(5) 0.032(4) 0.014(3) 0.012(3) F6 0.192(7) 0.220(8) 0.165(6) 0.040(6) 0.051(5) -0.100(6) C39 0.068(5) 0.044(4) 0.060(4) 0.016(3) 0.000(3) 0.012(3) F1 0.122(5) 0.212(8) 0.176(6) -0.100(6) 0.011(4) 0.015(5) F2 0.122(5) 0.185(7) 0.192(7) -0.087(6) -0.013(5) 0.033(5) C24 0.044(4) 0.078(5) 0.111(6) 0.047(5) -0.005(4) 0.000(4) C7 0.098(6) 0.079(6) 0.055(5) -0.006(4) 0.010(4) 0.029(5) C12 0.053(4) 0.048(4) 0.052(4) 0.019(3) 0.015(3) 0.010(3) C38 0.068(5) 0.079(6) 0.113(7) 0.056(5) 0.035(5) 0.006(4) C8 0.074(5) 0.086(6) 0.098(6) 0.051(5) 0.026(4) 0.018(4) N2 0.086(6) 0.131(7) 0.143(8) 0.045(6) 0.053(5) 0.029(5) C15 0.039(4) 0.082(5) 0.103(6) 0.054(4) 0.019(4) 0.007(4) C25 0.061(4) 0.049(4) 0.061(4) 0.017(3) 0.005(3) 0.008(3) C3 0.063(5) 0.081(6) 0.089(6) 0.024(5) 0.013(5) 0.028(5) C49 0.063(6) 0.141(10) 0.109(8) -0.002(8) 0.036(5) 0.006(7) C37 0.116(7) 0.054(5) 0.054(4) 0.019(4) 0.007(4) 0.027(4) C23 0.065(5) 0.072(5) 0.099(6) 0.039(4) -0.020(4) 0.009(4) C50 0.072(7) 0.132(10) 0.125(10) 0.033(8) 0.051(7) 0.021(6) C21 0.046(4) 0.098(6) 0.121(6) 0.057(5) -0.004(4) 0.002(4) C48 0.050(6) 0.113(10) 0.170(12) -0.014(9) 0.040(7) -0.004(6) C45 0.095(8) 0.107(9) 0.153(11) 0.019(8) 0.056(8) 0.011(6) C22 0.057(5) 0.093(6) 0.108(6) 0.056(5) -0.002(4) 0.017(4) N7 0.082(6) 0.147(8) 0.167(9) 0.057(7) 0.043(6) 0.026(6) C42 0.071(5) 0.082(6) 0.077(5) 0.011(4) 0.001(4) 0.030(4) N8 0.133(7) 0.108(6) 0.119(6) 0.040(5) 0.003(5) 0.067(6) C46 0.074(7) 0.170(12) 0.103(8) 0.030(8) 0.038(6) 0.008(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 N4 2.072(5) . ? Ag1 N5 2.090(5) . ? P1 F6 1.518(6) . ? P1 F1 1.528(6) . ? P1 F5 1.543(6) . ? P1 F2 1.553(6) . ? P1 F3 1.560(6) . ? P1 F4 1.573(6) . ? N3 C20 1.323(7) . ? N3 C21 1.365(8) . ? N3 C17 1.424(7) . ? C17 C16 1.362(8) . ? C17 C18 1.376(8) . ? N6 C25 1.341(8) . ? N6 C24 1.390(8) . ? N6 C26 1.433(7) . ? N4 C20 1.315(7) . ? N4 C22 1.359(9) . ? C47 C46 1.374(16) . ? C47 C48 1.391(16) . ? C14 C19 1.386(8) . ? C14 C15 1.393(8) . ? C14 C13 1.462(8) . ? C26 C31 1.372(8) . ? C26 C27 1.380(8) . ? C4 C2 1.370(9) . ? C4 C11 1.432(8) . ? C4 C5 1.493(8) . ? C13 C12 1.324(8) . ? C13 H13 0.9300 . ? C34 C44 1.354(8) . ? C34 C33 1.468(8) . ? C34 C35 1.495(8) . ? C35 C36 1.554(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? N5 C25 1.311(7) . ? N5 C23 1.347(9) . ? C28 C29 1.374(8) . ? C28 C27 1.378(8) . ? C28 H28 0.9300 . ? C29 C30 1.388(8) . ? C29 C32 1.459(8) . ? C32 C33 1.336(8) . ? C32 H32 0.9300 . ? C11 C10 1.345(8) . ? C11 H11 0.9300 . ? C16 C15 1.376(9) . ? C16 H16 0.9300 . ? C2 C3 1.435(11) . ? C2 C1 1.446(9) . ? C41 C40 1.370(9) . ? C41 C42 1.429(10) . ? C41 C43 1.445(12) . ? C5 C6 1.529(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C9 C10 1.502(8) . ? C9 C6 1.533(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C6 C7 1.524(9) . ? C6 C8 1.541(9) . ? C40 C44 1.435(8) . ? C40 C39 1.487(9) . ? C20 H20 0.9300 . ? C43 N7 1.146(11) . ? C30 C31 1.388(8) . ? C30 H30 0.9300 . ? C33 H33 0.9300 . ? C36 C37 1.520(9) . ? C36 C38 1.523(9) . ? C36 C39 1.545(9) . ? C44 H44 0.9300 . ? C27 H27 0.9300 . ? C31 H31 0.9300 . ? C1 N1 1.120(8) . ? C10 C12 1.442(8) . ? C19 C18 1.385(8) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C24 C23 1.367(9) . ? C24 H24 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C12 H12 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N2 C3 1.134(10) . ? C15 H15 0.9300 . ? C25 H25 0.9300 . ? C49 C50 1.353(14) . ? C49 C48 1.400(15) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C23 H23 0.9300 . ? C50 C45 1.357(14) . ? C21 C22 1.327(10) . ? C21 H21 0.9300 . ? C45 C46 1.447(15) . ? C22 H22 0.9300 . ? C42 N8 1.139(9) . ? 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 N4 Ag1 N5 175.4(2) . . ? F6 P1 F1 89.6(4) . . ? F6 P1 F5 98.5(5) . . ? F1 P1 F5 91.9(4) . . ? F6 P1 F2 90.2(5) . . ? F1 P1 F2 177.4(4) . . ? F5 P1 F2 90.8(4) . . ? F6 P1 F3 177.2(4) . . ? F1 P1 F3 92.1(4) . . ? F5 P1 F3 83.6(4) . . ? F2 P1 F3 88.0(4) . . ? F6 P1 F4 86.6(4) . . ? F1 P1 F4 89.6(4) . . ? F5 P1 F4 174.7(4) . . ? F2 P1 F4 87.7(4) . . ? F3 P1 F4 91.3(4) . . ? C20 N3 C21 105.5(5) . . ? C20 N3 C17 128.2(5) . . ? C21 N3 C17 126.2(5) . . ? C16 C17 C18 119.9(6) . . ? C16 C17 N3 120.4(5) . . ? C18 C17 N3 119.7(5) . . ? C25 N6 C24 105.7(5) . . ? C25 N6 C26 128.1(5) . . ? C24 N6 C26 126.2(5) . . ? C20 N4 C22 104.7(5) . . ? C20 N4 Ag1 127.0(4) . . ? C22 N4 Ag1 128.2(4) . . ? C46 C47 C48 119.7(11) . . ? C19 C14 C15 117.1(5) . . ? C19 C14 C13 123.2(5) . . ? C15 C14 C13 119.7(6) . . ? C31 C26 C27 120.7(5) . . ? C31 C26 N6 120.1(5) . . ? C27 C26 N6 119.2(5) . . ? C2 C4 C11 121.2(6) . . ? C2 C4 C5 121.0(5) . . ? C11 C4 C5 117.8(6) . . ? C12 C13 C14 125.5(6) . . ? C12 C13 H13 117.3 . . ? C14 C13 H13 117.3 . . ? C44 C34 C33 118.6(6) . . ? C44 C34 C35 121.5(5) . . ? C33 C34 C35 119.9(6) . . ? C34 C35 C36 114.0(5) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C25 N5 C23 106.9(6) . . ? C25 N5 Ag1 127.5(5) . . ? C23 N5 Ag1 125.5(4) . . ? C29 C28 C27 122.7(6) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C28 C29 C30 117.4(5) . . ? C28 C29 C32 124.2(6) . . ? C30 C29 C32 118.5(6) . . ? C33 C32 C29 126.4(6) . . ? C33 C32 H32 116.8 . . ? C29 C32 H32 116.8 . . ? C10 C11 C4 123.0(6) . . ? C10 C11 H11 118.5 . . ? C4 C11 H11 118.5 . . ? C17 C16 C15 121.0(6) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C4 C2 C3 121.4(6) . . ? C4 C2 C1 121.4(6) . . ? C3 C2 C1 117.1(6) . . ? C40 C41 C42 120.9(7) . . ? C40 C41 C43 123.2(6) . . ? C42 C41 C43 115.9(7) . . ? C4 C5 C6 113.6(5) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C10 C9 C6 113.2(5) . . ? C10 C9 H9A 108.9 . . ? C6 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C6 C9 H9B 108.9 . . ? H9A C9 H9B 107.8 . . ? C7 C6 C5 109.9(6) . . ? C7 C6 C9 109.6(5) . . ? C5 C6 C9 108.9(5) . . ? C7 C6 C8 109.9(6) . . ? C5 C6 C8 109.7(5) . . ? C9 C6 C8 108.8(5) . . ? C41 C40 C44 121.4(6) . . ? C41 C40 C39 120.0(6) . . ? C44 C40 C39 118.6(6) . . ? N4 C20 N3 112.6(5) . . ? N4 C20 H20 123.7 . . ? N3 C20 H20 123.7 . . ? N7 C43 C41 179.1(11) . . ? C29 C30 C31 121.2(6) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C33 C34 124.9(6) . . ? C32 C33 H33 117.6 . . ? C34 C33 H33 117.6 . . ? C37 C36 C38 110.3(6) . . ? C37 C36 C39 109.8(6) . . ? C38 C36 C39 109.1(6) . . ? C37 C36 C35 111.0(5) . . ? C38 C36 C35 108.7(6) . . ? C39 C36 C35 107.9(5) . . ? C34 C44 C40 122.1(6) . . ? C34 C44 H44 119.0 . . ? C40 C44 H44 119.0 . . ? C28 C27 C26 118.6(6) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C26 C31 C30 119.4(6) . . ? C26 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? N1 C1 C2 178.6(9) . . ? C11 C10 C12 118.9(6) . . ? C11 C10 C9 121.0(5) . . ? C12 C10 C9 120.1(5) . . ? C18 C19 C14 122.1(6) . . ? C18 C19 H19 119.0 . . ? C14 C19 H19 119.0 . . ? C17 C18 C19 119.1(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C40 C39 C36 112.7(5) . . ? C40 C39 H39A 109.1 . . ? C36 C39 H39A 109.1 . . ? C40 C39 H39B 109.1 . . ? C36 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C23 C24 N6 106.2(6) . . ? C23 C24 H24 126.9 . . ? N6 C24 H24 126.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C12 C10 127.3(6) . . ? C13 C12 H12 116.3 . . ? C10 C12 H12 116.3 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C15 C14 120.8(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N5 C25 N6 112.0(6) . . ? N5 C25 H25 124.0 . . ? N6 C25 H25 124.0 . . ? N2 C3 C2 178.0(10) . . ? C50 C49 C48 121.2(11) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C23 C24 109.1(6) . . ? N5 C23 H23 125.4 . . ? C24 C23 H23 125.4 . . ? C49 C50 C45 121.6(11) . . ? C22 C21 N3 107.5(7) . . ? C22 C21 H21 126.2 . . ? N3 C21 H21 126.2 . . ? C47 C48 C49 119.0(11) . . ? C50 C45 C46 118.2(11) . . ? C21 C22 N4 109.6(6) . . ? C21 C22 H22 125.2 . . ? N4 C22 H22 125.2 . . ? N8 C42 C41 178.8(10) . . ? C47 C46 C45 120.1(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 N3 C17 C16 160.9(7) . . . . ? C21 N3 C17 C16 -22.0(11) . . . . ? C20 N3 C17 C18 -20.2(10) . . . . ? C21 N3 C17 C18 157.0(7) . . . . ? N5 Ag1 N4 C20 155(2) . . . . ? N5 Ag1 N4 C22 -22(3) . . . . ? C25 N6 C26 C31 -162.8(6) . . . . ? C24 N6 C26 C31 16.0(10) . . . . ? C25 N6 C26 C27 16.6(10) . . . . ? C24 N6 C26 C27 -164.5(7) . . . . ? C19 C14 C13 C12 -6.8(10) . . . . ? C15 C14 C13 C12 174.3(7) . . . . ? C44 C34 C35 C36 -20.7(9) . . . . ? C33 C34 C35 C36 160.7(5) . . . . ? N4 Ag1 N5 C25 32(3) . . . . ? N4 Ag1 N5 C23 -146(2) . . . . ? C27 C28 C29 C30 1.7(10) . . . . ? C27 C28 C29 C32 -177.8(6) . . . . ? C28 C29 C32 C33 -0.5(10) . . . . ? C30 C29 C32 C33 -180.0(6) . . . . ? C2 C4 C11 C10 178.8(6) . . . . ? C5 C4 C11 C10 0.5(10) . . . . ? C18 C17 C16 C15 -0.3(12) . . . . ? N3 C17 C16 C15 178.7(7) . . . . ? C11 C4 C2 C3 2.2(11) . . . . ? C5 C4 C2 C3 -179.5(6) . . . . ? C11 C4 C2 C1 -177.4(6) . . . . ? C5 C4 C2 C1 0.9(10) . . . . ? C2 C4 C5 C6 152.6(6) . . . . ? C11 C4 C5 C6 -29.1(8) . . . . ? C4 C5 C6 C7 -68.0(7) . . . . ? C4 C5 C6 C9 52.1(7) . . . . ? C4 C5 C6 C8 171.1(6) . . . . ? C10 C9 C6 C7 71.3(7) . . . . ? C10 C9 C6 C5 -48.9(7) . . . . ? C10 C9 C6 C8 -168.4(6) . . . . ? C42 C41 C40 C44 174.0(7) . . . . ? C43 C41 C40 C44 -3.2(11) . . . . ? C42 C41 C40 C39 -2.2(11) . . . . ? C43 C41 C40 C39 -179.4(7) . . . . ? C22 N4 C20 N3 -0.6(8) . . . . ? Ag1 N4 C20 N3 -177.6(4) . . . . ? C21 N3 C20 N4 1.0(8) . . . . ? C17 N3 C20 N4 178.6(6) . . . . ? C40 C41 C43 N7 -43(67) . . . . ? C42 C41 C43 N7 140(67) . . . . ? C28 C29 C30 C31 0.0(10) . . . . ? C32 C29 C30 C31 179.5(6) . . . . ? C29 C32 C33 C34 -179.8(6) . . . . ? C44 C34 C33 C32 -177.1(6) . . . . ? C35 C34 C33 C32 1.5(10) . . . . ? C34 C35 C36 C37 -73.0(8) . . . . ? C34 C35 C36 C38 165.4(6) . . . . ? C34 C35 C36 C39 47.2(7) . . . . ? C33 C34 C44 C40 176.2(6) . . . . ? C35 C34 C44 C40 -2.4(10) . . . . ? C41 C40 C44 C34 179.2(6) . . . . ? C39 C40 C44 C34 -4.6(10) . . . . ? C29 C28 C27 C26 -1.1(10) . . . . ? C31 C26 C27 C28 -1.2(10) . . . . ? N6 C26 C27 C28 179.3(5) . . . . ? C27 C26 C31 C30 2.9(10) . . . . ? N6 C26 C31 C30 -177.7(6) . . . . ? C29 C30 C31 C26 -2.3(11) . . . . ? C4 C2 C1 N1 -158(36) . . . . ? C3 C2 C1 N1 23(36) . . . . ? C4 C11 C10 C12 -178.0(6) . . . . ? C4 C11 C10 C9 2.4(10) . . . . ? C6 C9 C10 C11 23.3(9) . . . . ? C6 C9 C10 C12 -156.3(6) . . . . ? C15 C14 C19 C18 -0.4(10) . . . . ? C13 C14 C19 C18 -179.3(6) . . . . ? C16 C17 C18 C19 1.0(11) . . . . ? N3 C17 C18 C19 -177.9(6) . . . . ? C14 C19 C18 C17 -0.7(11) . . . . ? C41 C40 C39 C36 -149.5(6) . . . . ? C44 C40 C39 C36 34.2(8) . . . . ? C37 C36 C39 C40 67.3(7) . . . . ? C38 C36 C39 C40 -171.7(6) . . . . ? C35 C36 C39 C40 -53.8(7) . . . . ? C25 N6 C24 C23 0.2(8) . . . . ? C26 N6 C24 C23 -178.9(6) . . . . ? C14 C13 C12 C10 176.2(6) . . . . ? C11 C10 C12 C13 177.0(7) . . . . ? C9 C10 C12 C13 -3.4(10) . . . . ? C17 C16 C15 C14 -0.9(13) . . . . ? C19 C14 C15 C16 1.2(11) . . . . ? C13 C14 C15 C16 -179.8(7) . . . . ? C23 N5 C25 N6 -1.9(8) . . . . ? Ag1 N5 C25 N6 -179.8(4) . . . . ? C24 N6 C25 N5 1.0(8) . . . . ? C26 N6 C25 N5 -179.9(6) . . . . ? C4 C2 C3 N2 88(25) . . . . ? C1 C2 C3 N2 -92(25) . . . . ? C25 N5 C23 C24 1.9(9) . . . . ? Ag1 N5 C23 C24 180.0(5) . . . . ? N6 C24 C23 N5 -1.3(10) . . . . ? C48 C49 C50 C45 1.9(15) . . . . ? C20 N3 C21 C22 -1.0(9) . . . . ? C17 N3 C21 C22 -178.7(7) . . . . ? C46 C47 C48 C49 4.2(15) . . . . ? C50 C49 C48 C47 -3.2(15) . . . . ? C49 C50 C45 C46 -1.6(15) . . . . ? N3 C21 C22 N4 0.7(10) . . . . ? C20 N4 C22 C21 0.0(9) . . . . ? Ag1 N4 C22 C21 176.8(6) . . . . ? C40 C41 C42 N8 -91(48) . . . . ? C43 C41 C42 N8 86(48) . . . . ? C48 C47 C46 C45 -4.0(15) . . . . ? C50 C45 C46 C47 2.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.919 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 917023' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 Ag N11 O3' _chemical_formula_sum 'C42 H38 Ag N11 O3' _chemical_formula_weight 852.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.621(5) _cell_length_b 7.851(5) _cell_length_c 18.755(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 92.618(5) _cell_angle_gamma 90.000(5) _cell_volume 3916(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6856 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.56 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.8945 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13435 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3445 _reflns_number_gt 3078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+4.9915P] 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 3445 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.85871(5) 1.2500 0.05975(17) Uani 1 2 d S . . N3 N 0.45061(7) 0.7092(3) 1.04147(11) 0.0358(4) Uani 1 1 d . . . C3 C 0.43575(9) 0.5918(3) 0.98623(13) 0.0348(5) Uani 1 1 d . . . N1 N 0.47646(8) 0.8261(3) 1.14137(12) 0.0429(5) Uani 1 1 d . . . N2 N 0.45102(10) 0.8801(3) 1.02855(13) 0.0486(6) Uani 1 1 d . . . C4 C 0.43188(10) 0.4193(3) 1.00079(14) 0.0405(6) Uani 1 1 d . . . H4 H 0.4397 0.3778 1.0464 0.049 Uiso 1 1 calc R . . C17 C 0.32525(10) 0.1320(3) 0.57459(15) 0.0392(6) Uani 1 1 d . . . C8 C 0.42472(11) 0.6536(3) 0.91815(15) 0.0443(6) Uani 1 1 d . . . H8 H 0.4278 0.7693 0.9085 0.053 Uiso 1 1 calc R . . C18 C 0.31388(9) 0.2027(4) 0.50973(14) 0.0407(6) Uani 1 1 d . . . C10 C 0.37267(11) 0.2884(3) 0.75527(15) 0.0449(6) Uani 1 1 d . . . H10 H 0.3757 0.4024 0.7428 0.054 Uiso 1 1 calc R . . C21 C 0.34018(10) 0.2371(3) 0.63473(14) 0.0427(6) Uani 1 1 d . . . H21 H 0.3407 0.3546 0.6285 0.051 Uiso 1 1 calc R . . C11 C 0.35350(10) 0.1737(3) 0.69966(14) 0.0399(6) Uani 1 1 d . . . C12 C 0.34997(11) -0.0145(3) 0.71454(14) 0.0439(6) Uani 1 1 d . . . H12A H 0.3392 -0.0307 0.7628 0.053 Uiso 1 1 calc R . . H12B H 0.3831 -0.0649 0.7117 0.053 Uiso 1 1 calc R . . C5 C 0.41613(10) 0.3093(3) 0.94618(14) 0.0418(6) Uani 1 1 d . . . H5 H 0.4136 0.1935 0.9557 0.050 Uiso 1 1 calc R . . C9 C 0.38626(10) 0.2476(3) 0.82206(14) 0.0417(6) Uani 1 1 d . . . H9 H 0.3843 0.1333 0.8347 0.050 Uiso 1 1 calc R . . C6 C 0.40414(10) 0.3681(3) 0.87783(15) 0.0395(6) Uani 1 1 d . . . C16 C 0.32513(11) -0.0584(3) 0.58581(14) 0.0450(6) Uani 1 1 d . . . H16A H 0.3578 -0.1039 0.5751 0.054 Uiso 1 1 calc R . . H16B H 0.3003 -0.1096 0.5529 0.054 Uiso 1 1 calc R . . C13 C 0.31323(11) -0.1077(3) 0.66244(15) 0.0439(6) Uani 1 1 d . . . C7 C 0.40912(11) 0.5428(3) 0.86485(14) 0.0456(6) Uani 1 1 d . . . H7 H 0.4017 0.5847 0.8192 0.055 Uiso 1 1 calc R . . N5 N 0.30724(10) 0.5286(4) 0.49280(15) 0.0598(7) Uani 1 1 d . . . C2 C 0.46606(10) 0.6794(3) 1.10910(14) 0.0408(6) Uani 1 1 d . . . H2 H 0.4690 0.5725 1.1302 0.049 Uiso 1 1 calc R . . C19 C 0.30464(11) 0.1045(4) 0.44607(16) 0.0507(7) Uani 1 1 d . . . C1 C 0.46684(11) 0.9430(4) 1.08971(14) 0.0487(7) Uani 1 1 d . . . H1 H 0.4712 1.0593 1.0972 0.058 Uiso 1 1 calc R . . C20 C 0.31108(10) 0.3849(4) 0.49956(15) 0.0438(6) Uani 1 1 d . . . C14 C 0.32142(14) -0.3000(4) 0.67189(19) 0.0626(8) Uani 1 1 d . . . H14A H 0.3153 -0.3315 0.7202 0.094 Uiso 1 1 calc R . . H14B H 0.3554 -0.3282 0.6615 0.094 Uiso 1 1 calc R . . H14C H 0.2986 -0.3607 0.6399 0.094 Uiso 1 1 calc R . . N4 N 0.29820(12) 0.0295(5) 0.39437(15) 0.0780(9) Uani 1 1 d . . . C15 C 0.25888(12) -0.0630(5) 0.67757(18) 0.0620(8) Uani 1 1 d . . . H15A H 0.2365 -0.1246 0.6453 0.093 Uiso 1 1 calc R . . H15B H 0.2537 0.0571 0.6711 0.093 Uiso 1 1 calc R . . H15C H 0.2523 -0.0935 0.7258 0.093 Uiso 1 1 calc R . . N11 N 0.5000 0.3126(5) 0.2500 0.0677(11) Uani 1 2 d S . . O3 O 0.5000 0.4581(5) 0.2500 0.1057(16) Uani 1 2 d S . . O6 O 0.5242(2) 0.2468(9) 0.2974(3) 0.231(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0764(3) 0.0741(3) 0.0272(2) 0.000 -0.01372(15) 0.000 N3 0.0391(11) 0.0399(11) 0.0279(10) -0.0003(8) -0.0035(8) -0.0005(9) C3 0.0345(12) 0.0430(13) 0.0266(12) -0.0035(10) -0.0019(9) -0.0009(10) N1 0.0488(13) 0.0495(12) 0.0297(12) -0.0025(9) -0.0068(9) 0.0002(10) N2 0.0724(16) 0.0386(12) 0.0336(13) 0.0031(9) -0.0116(11) -0.0074(10) C4 0.0448(14) 0.0462(14) 0.0298(13) 0.0019(11) -0.0053(10) 0.0015(11) C17 0.0403(13) 0.0441(14) 0.0330(14) -0.0067(10) 0.0004(10) -0.0038(10) C8 0.0583(16) 0.0402(13) 0.0338(15) 0.0023(10) -0.0047(12) -0.0050(11) C18 0.0382(13) 0.0505(14) 0.0333(14) -0.0035(11) 0.0016(10) -0.0055(11) C10 0.0571(16) 0.0388(13) 0.0382(15) -0.0052(11) -0.0050(12) -0.0021(12) C21 0.0545(15) 0.0348(13) 0.0382(14) -0.0040(11) -0.0049(11) -0.0019(11) C11 0.0443(14) 0.0402(13) 0.0350(14) -0.0063(10) -0.0017(11) -0.0012(11) C12 0.0551(15) 0.0401(13) 0.0363(14) -0.0024(11) -0.0022(11) -0.0024(11) C5 0.0477(14) 0.0389(13) 0.0385(14) -0.0008(11) -0.0013(11) 0.0003(11) C9 0.0480(14) 0.0402(13) 0.0364(14) -0.0046(11) -0.0033(11) -0.0048(11) C6 0.0407(13) 0.0448(14) 0.0325(14) -0.0050(10) -0.0024(10) -0.0015(10) C16 0.0574(16) 0.0414(14) 0.0361(14) -0.0102(11) -0.0008(12) -0.0038(12) C13 0.0530(15) 0.0388(13) 0.0397(15) -0.0037(11) -0.0016(12) -0.0046(11) C7 0.0608(16) 0.0485(15) 0.0268(13) 0.0015(11) -0.0070(11) -0.0049(12) N5 0.0588(16) 0.0609(17) 0.0595(17) 0.0117(13) -0.0003(12) -0.0017(12) C2 0.0496(14) 0.0437(13) 0.0284(13) -0.0007(10) -0.0051(11) 0.0026(11) C19 0.0512(16) 0.0652(18) 0.0359(16) -0.0047(13) 0.0038(12) -0.0067(13) C1 0.0670(18) 0.0413(14) 0.0367(15) -0.0013(11) -0.0085(12) -0.0065(13) C20 0.0397(14) 0.0576(18) 0.0341(14) 0.0019(11) -0.0003(11) -0.0048(11) C14 0.092(2) 0.0378(14) 0.0571(19) -0.0024(13) -0.0035(17) -0.0107(15) N4 0.090(2) 0.100(2) 0.0441(16) -0.0236(16) 0.0049(14) -0.0105(18) C15 0.0570(18) 0.076(2) 0.0538(19) -0.0056(16) 0.0055(14) -0.0134(16) N11 0.089(3) 0.046(2) 0.069(3) 0.000 0.017(2) 0.000 O3 0.174(5) 0.047(2) 0.100(3) 0.000 0.046(3) 0.000 O6 0.231(6) 0.244(6) 0.226(6) 0.171(6) 0.089(5) 0.146(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 N1 2.120(2) . ? Ag1 N1 2.120(2) 2_657 ? N3 C2 1.336(3) . ? N3 N2 1.364(3) . ? N3 C3 1.429(3) . ? C3 C8 1.385(4) . ? C3 C4 1.386(4) . ? N1 C2 1.324(4) . ? N1 C1 1.351(4) . ? N2 C1 1.301(4) . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C17 C18 1.359(4) . ? C17 C21 1.439(4) . ? C17 C16 1.510(4) . ? C8 C7 1.375(4) . ? C8 H8 0.9300 . ? C18 C19 1.433(4) . ? C18 C20 1.445(4) . ? C10 C9 1.327(4) . ? C10 C11 1.453(4) . ? C10 H10 0.9300 . ? C21 C11 1.348(4) . ? C21 H21 0.9300 . ? C11 C12 1.508(4) . ? C12 C13 1.536(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C5 C6 1.386(4) . ? C5 H5 0.9300 . ? C9 C6 1.473(4) . ? C9 H9 0.9300 . ? C6 C7 1.400(4) . ? C16 C13 1.535(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C13 C15 1.528(4) . ? C13 C14 1.535(4) . ? C7 H7 0.9300 . ? N5 C20 1.139(4) . ? C2 H2 0.9300 . ? C19 N4 1.141(4) . ? C1 H1 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? N11 O3 1.142(6) . ? N11 O6 1.191(5) 2_655 ? N11 O6 1.191(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 166.12(13) . 2_657 ? C2 N3 N2 109.6(2) . . ? C2 N3 C3 129.7(2) . . ? N2 N3 C3 120.7(2) . . ? C8 C3 C4 120.6(2) . . ? C8 C3 N3 118.8(2) . . ? C4 C3 N3 120.5(2) . . ? C2 N1 C1 103.6(2) . . ? C2 N1 Ag1 126.21(18) . . ? C1 N1 Ag1 130.20(19) . . ? C1 N2 N3 102.8(2) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C18 C17 C21 120.6(2) . . ? C18 C17 C16 121.8(2) . . ? C21 C17 C16 117.5(2) . . ? C7 C8 C3 119.5(2) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? C17 C18 C19 123.3(3) . . ? C17 C18 C20 122.1(2) . . ? C19 C18 C20 114.6(3) . . ? C9 C10 C11 126.8(3) . . ? C9 C10 H10 116.6 . . ? C11 C10 H10 116.6 . . ? C11 C21 C17 123.2(2) . . ? C11 C21 H21 118.4 . . ? C17 C21 H21 118.4 . . ? C21 C11 C10 119.3(2) . . ? C21 C11 C12 120.9(2) . . ? C10 C11 C12 119.8(2) . . ? C11 C12 C13 113.1(2) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C10 C9 C6 125.5(3) . . ? C10 C9 H9 117.3 . . ? C6 C9 H9 117.3 . . ? C5 C6 C7 117.8(2) . . ? C5 C6 C9 119.8(2) . . ? C7 C6 C9 122.4(2) . . ? C17 C16 C13 112.4(2) . . ? C17 C16 H16A 109.1 . . ? C13 C16 H16A 109.1 . . ? C17 C16 H16B 109.1 . . ? C13 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C15 C13 C14 109.6(3) . . ? C15 C13 C16 110.7(2) . . ? C14 C13 C16 108.8(2) . . ? C15 C13 C12 110.7(2) . . ? C14 C13 C12 108.2(2) . . ? C16 C13 C12 108.8(2) . . ? C8 C7 C6 121.4(2) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N1 C2 N3 109.3(2) . . ? N1 C2 H2 125.3 . . ? N3 C2 H2 125.3 . . ? N4 C19 C18 178.0(4) . . ? N2 C1 N1 114.7(2) . . ? N2 C1 H1 122.7 . . ? N1 C1 H1 122.7 . . ? N5 C20 C18 177.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 N11 O6 115.7(5) . 2_655 ? O3 N11 O6 115.7(5) . . ? O6 N11 O6 128.5(9) 2_655 . ? 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 N3 C3 C8 -175.1(3) . . . . ? N2 N3 C3 C8 3.9(4) . . . . ? C2 N3 C3 C4 5.6(4) . . . . ? N2 N3 C3 C4 -175.3(2) . . . . ? N1 Ag1 N1 C2 4.7(2) 2_657 . . . ? N1 Ag1 N1 C1 -177.7(2) 2_657 . . . ? C2 N3 N2 C1 0.0(3) . . . . ? C3 N3 N2 C1 -179.2(2) . . . . ? C8 C3 C4 C5 -0.8(4) . . . . ? N3 C3 C4 C5 178.4(2) . . . . ? C4 C3 C8 C7 0.9(4) . . . . ? N3 C3 C8 C7 -178.3(2) . . . . ? C21 C17 C18 C19 172.3(3) . . . . ? C16 C17 C18 C19 -4.8(4) . . . . ? C21 C17 C18 C20 -6.5(4) . . . . ? C16 C17 C18 C20 176.3(2) . . . . ? C18 C17 C21 C11 -177.7(3) . . . . ? C16 C17 C21 C11 -0.4(4) . . . . ? C17 C21 C11 C10 174.1(2) . . . . ? C17 C21 C11 C12 -4.4(4) . . . . ? C9 C10 C11 C21 178.3(3) . . . . ? C9 C10 C11 C12 -3.2(4) . . . . ? C21 C11 C12 C13 -21.7(4) . . . . ? C10 C11 C12 C13 159.9(2) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C11 C10 C9 C6 -178.0(3) . . . . ? C4 C5 C6 C7 1.0(4) . . . . ? C4 C5 C6 C9 -178.3(2) . . . . ? C10 C9 C6 C5 178.6(3) . . . . ? C10 C9 C6 C7 -0.7(5) . . . . ? C18 C17 C16 C13 -151.9(3) . . . . ? C21 C17 C16 C13 30.9(3) . . . . ? C17 C16 C13 C15 67.7(3) . . . . ? C17 C16 C13 C14 -171.9(3) . . . . ? C17 C16 C13 C12 -54.2(3) . . . . ? C11 C12 C13 C15 -72.3(3) . . . . ? C11 C12 C13 C14 167.6(2) . . . . ? C11 C12 C13 C16 49.6(3) . . . . ? C3 C8 C7 C6 -0.1(4) . . . . ? C5 C6 C7 C8 -0.9(4) . . . . ? C9 C6 C7 C8 178.4(3) . . . . ? C1 N1 C2 N3 -0.5(3) . . . . ? Ag1 N1 C2 N3 177.61(16) . . . . ? N2 N3 C2 N1 0.3(3) . . . . ? C3 N3 C2 N1 179.4(2) . . . . ? C17 C18 C19 N4 -133(12) . . . . ? C20 C18 C19 N4 46(12) . . . . ? N3 N2 C1 N1 -0.3(3) . . . . ? C2 N1 C1 N2 0.5(4) . . . . ? Ag1 N1 C1 N2 -177.4(2) . . . . ? C17 C18 C20 N5 -73(8) . . . . ? C19 C18 C20 N5 108(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 917024' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 Ag2 F6 N10 O4' _chemical_formula_sum 'C46 H38 Ag2 F6 N10 O4' _chemical_formula_weight 1124.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.750(5) _cell_length_b 12.813(5) _cell_length_c 20.012(5) _cell_angle_alpha 73.540(5) _cell_angle_beta 80.240(5) _cell_angle_gamma 65.257(5) _cell_volume 2396.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8940 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.89 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7754 _exptl_absorpt_correction_T_max 0.8415 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16562 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8307 _reflns_number_gt 6617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+2.2143P] 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 8307 _refine_ls_number_parameters 617 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.75468(3) 0.24051(3) 0.996329(19) 0.04520(16) Uani 1 1 d . . . Ag2 Ag 1.33776(4) 0.24757(4) 0.85832(3) 0.06568(19) Uani 1 1 d . . . N3 N 1.1406(3) 0.0734(3) 0.89512(18) 0.0330(8) Uani 1 1 d . . . N8 N 0.3838(4) 0.4463(3) 1.0960(2) 0.0374(8) Uani 1 1 d . . . N5 N 0.9672(4) 0.1735(3) 0.9567(2) 0.0386(8) Uani 1 1 d . . . C24 C 0.2986(4) 0.5278(4) 1.1368(2) 0.0358(9) Uani 1 1 d . . . N4 N 1.1756(4) 0.1578(3) 0.9068(2) 0.0428(9) Uani 1 1 d . . . C17 C 1.2301(4) -0.0124(4) 0.8571(2) 0.0341(9) Uani 1 1 d . . . C14 C 1.3998(5) -0.1765(4) 0.7804(2) 0.0378(10) Uani 1 1 d . . . N6 N 0.5559(4) 0.3346(3) 1.0401(2) 0.0393(9) Uani 1 1 d . . . C29 C 0.3454(4) 0.6056(4) 1.1498(2) 0.0378(10) Uani 1 1 d . . . H18 H 0.4315 0.6046 1.1321 0.045 Uiso 1 1 calc R . . C32 C -0.0207(5) 0.9361(4) 1.3160(2) 0.0422(11) Uani 1 1 d . . . C39 C 0.0124(5) 1.0253(5) 1.3198(3) 0.0452(11) Uani 1 1 d . . . H11 H 0.0938 1.0292 1.2971 0.054 Uiso 1 1 calc R . . C28 C 0.2616(5) 0.6850(4) 1.1895(2) 0.0402(10) Uani 1 1 d . . . H19 H 0.2925 0.7374 1.1984 0.048 Uiso 1 1 calc R . . C23 C 0.5188(4) 0.4090(4) 1.0801(2) 0.0361(9) Uani 1 1 d . . . H20 H 0.5780 0.4326 1.0952 0.043 Uiso 1 1 calc R . . C31 C 0.0667(5) 0.8547(4) 1.2734(2) 0.0441(11) Uani 1 1 d . . . H12 H 0.1484 0.8624 1.2540 0.053 Uiso 1 1 calc R . . N7 N 0.3283(4) 0.3950(5) 1.0643(3) 0.0615(13) Uani 1 1 d . . . C33 C -0.1481(5) 0.9225(5) 1.3535(3) 0.0483(12) Uani 1 1 d . . . H9A H -0.1298 0.8389 1.3701 0.058 Uiso 1 1 calc R . . H9B H -0.2198 0.9571 1.3207 0.058 Uiso 1 1 calc R . . C18 C 1.1821(4) -0.0850(4) 0.8406(2) 0.0391(10) Uani 1 1 d . . . H25 H 1.0928 -0.0791 0.8547 0.047 Uiso 1 1 calc R . . C10 C 1.5449(5) -0.4258(4) 0.6829(2) 0.0451(11) Uani 1 1 d . . . C13 C 1.4890(5) -0.2600(4) 0.7382(2) 0.0409(11) Uani 1 1 d . . . H30 H 1.5696 -0.2517 0.7175 0.049 Uiso 1 1 calc R . . C27 C 0.1320(5) 0.6876(4) 1.2166(2) 0.0389(10) Uani 1 1 d . . . C11 C 1.5138(6) -0.5167(5) 0.6825(3) 0.0490(12) Uani 1 1 d . . . H42 H 1.4378 -0.5247 0.7099 0.059 Uiso 1 1 calc R . . C34 C -0.2006(5) 0.9810(5) 1.4160(3) 0.0510(12) Uani 1 1 d . . . C21 C 1.0680(5) 0.2138(4) 0.9445(3) 0.0437(11) Uani 1 1 d . . . H22 H 1.0623 0.2764 0.9613 0.052 Uiso 1 1 calc R . . C15 C 1.4458(5) -0.1036(5) 0.7985(3) 0.0566(14) Uani 1 1 d . . . H28 H 1.5347 -0.1086 0.7843 0.068 Uiso 1 1 calc R . . C25 C 0.1700(5) 0.5290(5) 1.1626(3) 0.0475(12) Uani 1 1 d . . . H16 H 0.1387 0.4773 1.1533 0.057 Uiso 1 1 calc R . . C38 C -0.0716(5) 1.1136(5) 1.3568(2) 0.0446(11) Uani 1 1 d . . . C26 C 0.0899(5) 0.6080(5) 1.2022(3) 0.0480(12) Uani 1 1 d . . . H15 H 0.0041 0.6081 1.2200 0.058 Uiso 1 1 calc R . . C12 C 1.4631(5) -0.3461(4) 0.7275(2) 0.0450(11) Uani 1 1 d . . . H31 H 1.3851 -0.3567 0.7507 0.054 Uiso 1 1 calc R . . C30 C 0.0414(5) 0.7699(4) 1.2592(2) 0.0415(11) Uani 1 1 d . . . H13 H -0.0406 0.7624 1.2779 0.050 Uiso 1 1 calc R . . C4 C 1.5915(6) -0.6019(5) 0.6422(3) 0.0512(13) Uani 1 1 d . . . C20 C 1.0159(4) 0.0859(4) 0.9249(2) 0.0365(10) Uani 1 1 d . . . H23 H 0.9698 0.0394 0.9233 0.044 Uiso 1 1 calc R . . C9 C 1.6632(6) -0.4074(6) 0.6390(3) 0.0587(14) Uani 1 1 d . . . H33A H 1.7427 -0.4441 0.6670 0.070 Uiso 1 1 calc R . . H33B H 1.6426 -0.3232 0.6241 0.070 Uiso 1 1 calc R . . C37 C -0.2042(5) 1.1071(5) 1.3921(3) 0.0486(12) Uani 1 1 d . . . H5A H -0.2768 1.1548 1.3601 0.058 Uiso 1 1 calc R . . H5B H -0.2267 1.1410 1.4324 0.058 Uiso 1 1 calc R . . C2 C 1.5654(7) -0.6991(5) 0.6485(3) 0.0624(16) Uani 1 1 d . . . C19 C 1.2651(5) -0.1665(4) 0.8033(2) 0.0420(11) Uani 1 1 d . . . H26 H 1.2317 -0.2160 0.7929 0.050 Uiso 1 1 calc R . . C16 C 1.3630(5) -0.0224(5) 0.8377(3) 0.0588(15) Uani 1 1 d . . . H29 H 1.3970 0.0245 0.8506 0.071 Uiso 1 1 calc R . . C5 C 1.7105(6) -0.5868(5) 0.5965(3) 0.0617(15) Uani 1 1 d . . . H37A H 1.7188 -0.6155 0.5553 0.074 Uiso 1 1 calc R . . H37B H 1.7936 -0.6352 0.6213 0.074 Uiso 1 1 calc R . . C40 C -0.0374(6) 1.2038(5) 1.3572(3) 0.0548(13) Uani 1 1 d . . . C22 C 0.4360(5) 0.3281(5) 1.0322(3) 0.0561(14) Uani 1 1 d . . . H21 H 0.4311 0.2804 1.0062 0.067 Uiso 1 1 calc R . . C6 C 1.6989(6) -0.4591(6) 0.5736(3) 0.0576(14) Uani 1 1 d . . . C1 C 1.6436(8) -0.7872(6) 0.6092(3) 0.0720(18) Uani 1 1 d . . . C36 C -0.1028(7) 0.9088(6) 1.4763(3) 0.0712(18) Uani 1 1 d . . . H7A H -0.0122 0.9060 1.4604 0.107 Uiso 1 1 calc R . . H7B H -0.1003 0.8299 1.4908 0.107 Uiso 1 1 calc R . . H7C H -0.1353 0.9459 1.5149 0.107 Uiso 1 1 calc R . . C35 C -0.3439(7) 0.9867(7) 1.4403(4) 0.080(2) Uani 1 1 d . . . H8A H -0.3783 1.0273 1.4774 0.120 Uiso 1 1 calc R . . H8B H -0.3416 0.9080 1.4569 0.120 Uiso 1 1 calc R . . H8C H -0.4028 1.0286 1.4021 0.120 Uiso 1 1 calc R . . C8 C 1.5855(8) -0.3868(6) 0.5222(3) 0.0758(19) Uani 1 1 d . . . H35A H 1.6083 -0.4188 0.4817 0.114 Uiso 1 1 calc R . . H35B H 1.5769 -0.3060 0.5084 0.114 Uiso 1 1 calc R . . H35C H 1.5001 -0.3900 0.5441 0.114 Uiso 1 1 calc R . . C42 C 0.0889(8) 1.2124(7) 1.3257(4) 0.0744(18) Uani 1 1 d . . . C41 C -0.1255(7) 1.2987(6) 1.3897(3) 0.0685(16) Uani 1 1 d . . . C7 C 1.8341(8) -0.4542(9) 0.5386(5) 0.102(3) Uani 1 1 d . . . H36A H 1.9040 -0.4951 0.5718 0.153 Uiso 1 1 calc R . . H36B H 1.8239 -0.3731 0.5220 0.153 Uiso 1 1 calc R . . H36C H 1.8597 -0.4911 0.5001 0.153 Uiso 1 1 calc R . . N1 N 1.7049(8) -0.8571(6) 0.5784(4) 0.098(2) Uani 1 1 d . . . N9 N -0.1955(8) 1.3738(6) 1.4147(4) 0.104(2) Uani 1 1 d . . . N10 N 0.1920(8) 1.2172(8) 1.3030(5) 0.118(3) Uani 1 1 d . . . C3 C 1.4616(10) -0.7221(6) 0.6967(4) 0.081(2) Uani 1 1 d . . . N2 N 1.3792(10) -0.7385(6) 0.7376(4) 0.113(3) Uani 1 1 d . . . O2 O 1.5386(4) 0.1620(5) 0.9153(3) 0.0877(15) Uani 1 1 d . . . C43 C 1.1967(5) 0.4962(5) 0.8736(3) 0.0516(13) Uani 1 1 d . . . O3 O 1.3084(4) 0.4994(5) 0.8538(3) 0.0830(14) Uani 1 1 d . . . O1 O 1.7386(4) 0.0734(4) 0.9623(2) 0.0682(11) Uani 1 1 d . . . F6 F 1.1263(5) 0.6645(5) 0.9200(3) 0.126(2) Uani 1 1 d . . . F4 F 0.9772(5) 0.5978(5) 0.9242(4) 0.138(2) Uani 1 1 d . . . F3 F 1.6557(6) 0.0255(6) 0.8217(3) 0.1216(18) Uani 1 1 d . . . C45 C 1.6542(5) 0.0832(5) 0.9251(3) 0.0557(13) Uani 1 1 d . . . C44 C 1.0843(6) 0.6098(6) 0.8889(4) 0.0690(17) Uani 1 1 d . . . C46 C 1.7026(7) -0.0175(6) 0.8869(4) 0.0698(17) Uani 1 1 d . . . F5 F 1.0388(7) 0.6893(6) 0.8304(4) 0.155(3) Uani 1 1 d . . . O4 O 1.1595(5) 0.4155(4) 0.8815(3) 0.0889(15) Uani 1 1 d U . . F1 F 1.8368(5) -0.0661(6) 0.8784(4) 0.142(3) Uani 1 1 d . . . F2 F 1.6586(7) -0.0988(5) 0.9165(4) 0.140(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0307(2) 0.0440(2) 0.0569(3) -0.02434(18) 0.01064(16) -0.00769(17) Ag2 0.0448(3) 0.0676(3) 0.0905(4) -0.0343(3) 0.0141(2) -0.0244(2) N3 0.0269(17) 0.0342(19) 0.0410(19) -0.0189(15) 0.0045(14) -0.0110(15) N8 0.0257(18) 0.041(2) 0.047(2) -0.0213(17) 0.0056(15) -0.0104(16) N5 0.0315(19) 0.037(2) 0.048(2) -0.0182(17) 0.0062(16) -0.0126(17) C24 0.026(2) 0.033(2) 0.045(2) -0.0179(19) -0.0003(17) -0.0043(18) N4 0.033(2) 0.041(2) 0.062(2) -0.0276(19) 0.0135(17) -0.0190(17) C17 0.025(2) 0.032(2) 0.043(2) -0.0156(18) 0.0049(17) -0.0068(17) C14 0.032(2) 0.034(2) 0.045(2) -0.0184(19) 0.0047(18) -0.0067(19) N6 0.034(2) 0.041(2) 0.045(2) -0.0191(17) 0.0050(16) -0.0137(17) C29 0.026(2) 0.042(2) 0.045(2) -0.016(2) 0.0039(17) -0.0103(19) C32 0.034(2) 0.044(3) 0.041(2) -0.017(2) 0.0014(19) -0.005(2) C39 0.035(2) 0.051(3) 0.048(3) -0.023(2) 0.006(2) -0.010(2) C28 0.035(2) 0.042(3) 0.044(2) -0.018(2) -0.0021(19) -0.010(2) C23 0.026(2) 0.036(2) 0.045(2) -0.0182(19) 0.0019(18) -0.0075(18) C31 0.035(2) 0.045(3) 0.045(3) -0.020(2) 0.0064(19) -0.005(2) N7 0.040(2) 0.080(3) 0.088(3) -0.057(3) 0.010(2) -0.027(2) C33 0.040(3) 0.053(3) 0.050(3) -0.026(2) 0.011(2) -0.014(2) C18 0.026(2) 0.043(3) 0.051(3) -0.021(2) 0.0045(18) -0.0129(19) C10 0.044(3) 0.044(3) 0.038(2) -0.016(2) 0.000(2) -0.004(2) C13 0.028(2) 0.042(3) 0.046(3) -0.018(2) 0.0013(18) -0.004(2) C27 0.032(2) 0.041(3) 0.038(2) -0.0165(19) 0.0031(18) -0.0063(19) C11 0.054(3) 0.044(3) 0.041(3) -0.018(2) 0.006(2) -0.010(2) C34 0.048(3) 0.055(3) 0.049(3) -0.027(2) 0.014(2) -0.016(2) C21 0.034(2) 0.038(3) 0.063(3) -0.030(2) 0.010(2) -0.012(2) C15 0.032(3) 0.063(3) 0.087(4) -0.045(3) 0.019(2) -0.021(2) C25 0.031(2) 0.053(3) 0.067(3) -0.034(3) 0.014(2) -0.018(2) C38 0.042(3) 0.047(3) 0.040(2) -0.016(2) -0.001(2) -0.011(2) C26 0.031(2) 0.052(3) 0.065(3) -0.030(2) 0.010(2) -0.014(2) C12 0.045(3) 0.044(3) 0.042(2) -0.021(2) 0.006(2) -0.010(2) C30 0.034(2) 0.047(3) 0.041(2) -0.020(2) 0.0055(19) -0.011(2) C4 0.057(3) 0.045(3) 0.040(3) -0.018(2) -0.006(2) -0.002(2) C20 0.028(2) 0.037(2) 0.046(2) -0.0196(19) 0.0071(18) -0.0125(19) C9 0.045(3) 0.073(4) 0.064(3) -0.042(3) 0.011(2) -0.019(3) C37 0.041(3) 0.049(3) 0.052(3) -0.027(2) 0.010(2) -0.009(2) C2 0.085(4) 0.044(3) 0.049(3) -0.023(2) -0.005(3) -0.008(3) C19 0.039(2) 0.044(3) 0.049(3) -0.021(2) 0.003(2) -0.017(2) C16 0.034(3) 0.057(3) 0.102(4) -0.055(3) 0.021(3) -0.021(2) C5 0.056(3) 0.061(4) 0.059(3) -0.037(3) 0.001(3) -0.001(3) C40 0.061(3) 0.052(3) 0.055(3) -0.027(3) 0.001(3) -0.019(3) C22 0.039(3) 0.072(4) 0.077(4) -0.052(3) 0.016(2) -0.026(3) C6 0.048(3) 0.067(4) 0.057(3) -0.035(3) 0.010(2) -0.013(3) C1 0.087(5) 0.052(3) 0.070(4) -0.029(3) -0.012(3) -0.008(3) C36 0.087(5) 0.066(4) 0.046(3) -0.013(3) -0.003(3) -0.017(3) C35 0.068(4) 0.086(5) 0.092(5) -0.044(4) 0.037(4) -0.037(4) C8 0.087(5) 0.083(5) 0.046(3) -0.016(3) 0.005(3) -0.025(4) C42 0.074(4) 0.075(4) 0.092(5) -0.041(4) 0.008(4) -0.037(4) C41 0.078(4) 0.065(4) 0.072(4) -0.035(3) 0.006(3) -0.029(3) C7 0.073(5) 0.141(8) 0.114(6) -0.083(6) 0.050(4) -0.051(5) N1 0.110(5) 0.074(4) 0.103(5) -0.059(4) -0.007(4) -0.005(4) N9 0.123(6) 0.082(5) 0.116(5) -0.062(4) 0.014(5) -0.031(4) N10 0.096(5) 0.142(7) 0.160(7) -0.068(6) 0.027(5) -0.083(5) C3 0.139(7) 0.050(4) 0.053(4) -0.023(3) 0.008(4) -0.036(4) N2 0.188(9) 0.090(5) 0.076(4) -0.034(4) 0.037(5) -0.076(6) O2 0.045(3) 0.092(4) 0.119(4) -0.043(3) -0.009(2) -0.006(2) C43 0.040(3) 0.053(3) 0.075(3) -0.029(3) 0.010(2) -0.026(2) O3 0.048(2) 0.096(4) 0.125(4) -0.052(3) 0.018(2) -0.040(2) O1 0.063(3) 0.065(3) 0.092(3) -0.027(2) -0.012(2) -0.032(2) F6 0.107(4) 0.110(4) 0.210(6) -0.111(4) 0.013(4) -0.053(3) F4 0.071(3) 0.122(4) 0.255(7) -0.118(5) 0.079(4) -0.056(3) F3 0.124(4) 0.158(5) 0.112(4) -0.072(4) -0.012(3) -0.056(4) C45 0.040(3) 0.053(3) 0.074(4) -0.010(3) 0.004(3) -0.023(3) C44 0.050(3) 0.062(4) 0.110(5) -0.038(4) 0.004(3) -0.029(3) C46 0.056(4) 0.084(5) 0.095(5) -0.043(4) -0.003(3) -0.038(3) F5 0.140(5) 0.101(4) 0.161(6) -0.023(4) -0.048(5) 0.023(4) O4 0.075(3) 0.062(3) 0.146(4) -0.049(3) 0.027(3) -0.039(2) F1 0.058(3) 0.155(5) 0.244(7) -0.144(5) 0.014(3) -0.019(3) F2 0.187(6) 0.106(4) 0.183(6) -0.066(4) 0.037(5) -0.108(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6 2.144(4) . ? Ag1 N5 2.171(4) . ? Ag1 O1 2.501(4) 1_455 ? Ag2 O2 2.304(5) . ? Ag2 O4 2.309(5) . ? Ag2 N2 2.351(7) 1_565 ? Ag2 N4 2.403(4) . ? N3 C20 1.334(6) . ? N3 N4 1.371(5) . ? N3 C17 1.432(5) . ? N8 C23 1.336(6) . ? N8 N7 1.373(6) . ? N8 C24 1.423(5) . ? N5 C20 1.319(6) . ? N5 C21 1.345(6) . ? C24 C25 1.386(6) . ? C24 C29 1.387(6) . ? N4 C21 1.319(6) . ? C17 C18 1.370(6) . ? C17 C16 1.377(6) . ? C14 C15 1.374(7) . ? C14 C19 1.405(7) . ? C14 C13 1.468(6) . ? N6 C23 1.309(6) . ? N6 C22 1.364(6) . ? C29 C28 1.388(6) . ? C29 H18 0.9300 . ? C32 C39 1.355(7) . ? C32 C31 1.453(6) . ? C32 C33 1.499(7) . ? C39 C38 1.427(7) . ? C39 H11 0.9300 . ? C28 C27 1.397(7) . ? C28 H19 0.9300 . ? C23 H20 0.9300 . ? C31 C30 1.336(7) . ? C31 H12 0.9300 . ? N7 C22 1.311(7) . ? C33 C34 1.544(7) . ? C33 H9A 0.9700 . ? C33 H9B 0.9700 . ? C18 C19 1.371(6) . ? C18 H25 0.9300 . ? C10 C11 1.341(8) . ? C10 C12 1.452(6) . ? C10 C9 1.483(8) . ? C13 C12 1.324(7) . ? C13 H30 0.9300 . ? C27 C26 1.388(7) . ? C27 C30 1.469(6) . ? C11 C4 1.431(7) . ? C11 H42 0.9300 . ? C34 C35 1.513(8) . ? C34 C37 1.535(8) . ? C34 C36 1.548(8) . ? C21 H22 0.9300 . ? C15 C16 1.393(7) . ? C15 H28 0.9300 . ? C25 C26 1.373(7) . ? C25 H16 0.9300 . ? C38 C40 1.353(8) . ? C38 C37 1.505(7) . ? C26 H15 0.9300 . ? C12 H31 0.9300 . ? C30 H13 0.9300 . ? C4 C2 1.355(9) . ? C4 C5 1.490(8) . ? C20 H23 0.9300 . ? C9 C6 1.553(7) . ? C9 H33A 0.9700 . ? C9 H33B 0.9700 . ? C37 H5A 0.9700 . ? C37 H5B 0.9700 . ? C2 C3 1.419(11) . ? C2 C1 1.443(8) . ? C19 H26 0.9300 . ? C16 H29 0.9300 . ? C5 C6 1.526(9) . ? C5 H37A 0.9700 . ? C5 H37B 0.9700 . ? C40 C42 1.432(9) . ? C40 C41 1.440(8) . ? C22 H21 0.9300 . ? C6 C7 1.521(9) . ? C6 C8 1.530(9) . ? C1 N1 1.139(8) . ? C36 H7A 0.9600 . ? C36 H7B 0.9600 . ? C36 H7C 0.9600 . ? C35 H8A 0.9600 . ? C35 H8B 0.9600 . ? C35 H8C 0.9600 . ? C8 H35A 0.9600 . ? C8 H35B 0.9600 . ? C8 H35C 0.9600 . ? C42 N10 1.144(9) . ? C41 N9 1.132(9) . ? C7 H36A 0.9600 . ? C7 H36B 0.9600 . ? C7 H36C 0.9600 . ? C3 N2 1.144(10) . ? N2 Ag2 2.351(7) 1_545 ? O2 C45 1.234(7) . ? C43 O3 1.212(6) . ? C43 O4 1.220(7) . ? C43 C44 1.526(8) . ? O1 C45 1.214(7) . ? O1 Ag1 2.501(4) 1_655 ? F6 C44 1.299(7) . ? F4 C44 1.288(8) . ? F3 C46 1.357(8) . ? C45 C46 1.544(9) . ? C44 F5 1.323(9) . ? C46 F2 1.275(8) . ? C46 F1 1.313(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N5 167.74(14) . . ? N6 Ag1 O1 106.51(15) . 1_455 ? N5 Ag1 O1 85.75(15) . 1_455 ? O2 Ag2 O4 121.65(19) . . ? O2 Ag2 N2 111.9(3) . 1_565 ? O4 Ag2 N2 111.2(3) . 1_565 ? O2 Ag2 N4 114.45(18) . . ? O4 Ag2 N4 83.21(15) . . ? N2 Ag2 N4 111.2(2) 1_565 . ? C20 N3 N4 109.0(3) . . ? C20 N3 C17 128.4(4) . . ? N4 N3 C17 122.6(3) . . ? C23 N8 N7 109.4(4) . . ? C23 N8 C24 130.1(4) . . ? N7 N8 C24 120.5(4) . . ? C20 N5 C21 103.2(4) . . ? C20 N5 Ag1 121.4(3) . . ? C21 N5 Ag1 134.2(3) . . ? C25 C24 C29 121.0(4) . . ? C25 C24 N8 119.7(4) . . ? C29 C24 N8 119.3(4) . . ? C21 N4 N3 102.4(4) . . ? C21 N4 Ag2 118.1(3) . . ? N3 N4 Ag2 137.5(3) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 N3 119.2(4) . . ? C16 C17 N3 120.6(4) . . ? C15 C14 C19 117.3(4) . . ? C15 C14 C13 120.5(4) . . ? C19 C14 C13 122.2(4) . . ? C23 N6 C22 103.6(4) . . ? C23 N6 Ag1 130.1(3) . . ? C22 N6 Ag1 126.3(3) . . ? C24 C29 C28 119.0(4) . . ? C24 C29 H18 120.5 . . ? C28 C29 H18 120.5 . . ? C39 C32 C31 119.4(5) . . ? C39 C32 C33 120.9(4) . . ? C31 C32 C33 119.7(4) . . ? C32 C39 C38 123.3(5) . . ? C32 C39 H11 118.3 . . ? C38 C39 H11 118.3 . . ? C29 C28 C27 121.2(4) . . ? C29 C28 H19 119.4 . . ? C27 C28 H19 119.4 . . ? N6 C23 N8 110.3(4) . . ? N6 C23 H20 124.9 . . ? N8 C23 H20 124.9 . . ? C30 C31 C32 126.4(5) . . ? C30 C31 H12 116.8 . . ? C32 C31 H12 116.8 . . ? C22 N7 N8 102.5(4) . . ? C32 C33 C34 113.6(4) . . ? C32 C33 H9A 108.8 . . ? C34 C33 H9A 108.8 . . ? C32 C33 H9B 108.8 . . ? C34 C33 H9B 108.8 . . ? H9A C33 H9B 107.7 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H25 119.9 . . ? C19 C18 H25 119.9 . . ? C11 C10 C12 119.6(5) . . ? C11 C10 C9 120.5(5) . . ? C12 C10 C9 119.9(5) . . ? C12 C13 C14 124.9(5) . . ? C12 C13 H30 117.6 . . ? C14 C13 H30 117.6 . . ? C26 C27 C28 117.6(4) . . ? C26 C27 C30 119.9(4) . . ? C28 C27 C30 122.6(4) . . ? C10 C11 C4 123.4(5) . . ? C10 C11 H42 118.3 . . ? C4 C11 H42 118.3 . . ? C35 C34 C37 109.2(5) . . ? C35 C34 C33 109.7(5) . . ? C37 C34 C33 108.4(4) . . ? C35 C34 C36 110.1(5) . . ? C37 C34 C36 109.7(5) . . ? C33 C34 C36 109.7(5) . . ? N4 C21 N5 114.8(4) . . ? N4 C21 H22 122.6 . . ? N5 C21 H22 122.6 . . ? C14 C15 C16 121.8(5) . . ? C14 C15 H28 119.1 . . ? C16 C15 H28 119.1 . . ? C26 C25 C24 118.7(5) . . ? C26 C25 H16 120.7 . . ? C24 C25 H16 120.7 . . ? C40 C38 C39 121.5(5) . . ? C40 C38 C37 120.8(5) . . ? C39 C38 C37 117.6(5) . . ? C25 C26 C27 122.5(5) . . ? C25 C26 H15 118.7 . . ? C27 C26 H15 118.7 . . ? C13 C12 C10 126.3(5) . . ? C13 C12 H31 116.9 . . ? C10 C12 H31 116.9 . . ? C31 C30 C27 125.5(5) . . ? C31 C30 H13 117.2 . . ? C27 C30 H13 117.2 . . ? C2 C4 C11 121.7(5) . . ? C2 C4 C5 119.8(5) . . ? C11 C4 C5 118.3(5) . . ? N5 C20 N3 110.6(4) . . ? N5 C20 H23 124.7 . . ? N3 C20 H23 124.7 . . ? C10 C9 C6 113.1(5) . . ? C10 C9 H33A 109.0 . . ? C6 C9 H33A 109.0 . . ? C10 C9 H33B 109.0 . . ? C6 C9 H33B 109.0 . . ? H33A C9 H33B 107.8 . . ? C38 C37 C34 113.8(4) . . ? C38 C37 H5A 108.8 . . ? C34 C37 H5A 108.8 . . ? C38 C37 H5B 108.8 . . ? C34 C37 H5B 108.8 . . ? H5A C37 H5B 107.7 . . ? C4 C2 C3 121.2(5) . . ? C4 C2 C1 122.8(6) . . ? C3 C2 C1 116.0(6) . . ? C18 C19 C14 121.2(4) . . ? C18 C19 H26 119.4 . . ? C14 C19 H26 119.4 . . ? C17 C16 C15 119.2(5) . . ? C17 C16 H29 120.4 . . ? C15 C16 H29 120.4 . . ? C4 C5 C6 113.7(5) . . ? C4 C5 H37A 108.8 . . ? C6 C5 H37A 108.8 . . ? C4 C5 H37B 108.8 . . ? C6 C5 H37B 108.8 . . ? H37A C5 H37B 107.7 . . ? C38 C40 C42 122.9(5) . . ? C38 C40 C41 122.5(6) . . ? C42 C40 C41 114.6(5) . . ? N7 C22 N6 114.3(4) . . ? N7 C22 H21 122.9 . . ? N6 C22 H21 122.9 . . ? C7 C6 C5 110.3(6) . . ? C7 C6 C8 109.4(6) . . ? C5 C6 C8 109.4(5) . . ? C7 C6 C9 109.2(5) . . ? C5 C6 C9 108.6(5) . . ? C8 C6 C9 109.8(5) . . ? N1 C1 C2 179.6(10) . . ? C34 C36 H7A 109.5 . . ? C34 C36 H7B 109.5 . . ? H7A C36 H7B 109.5 . . ? C34 C36 H7C 109.5 . . ? H7A C36 H7C 109.5 . . ? H7B C36 H7C 109.5 . . ? C34 C35 H8A 109.5 . . ? C34 C35 H8B 109.5 . . ? H8A C35 H8B 109.5 . . ? C34 C35 H8C 109.5 . . ? H8A C35 H8C 109.5 . . ? H8B C35 H8C 109.5 . . ? C6 C8 H35A 109.5 . . ? C6 C8 H35B 109.5 . . ? H35A C8 H35B 109.5 . . ? C6 C8 H35C 109.5 . . ? H35A C8 H35C 109.5 . . ? H35B C8 H35C 109.5 . . ? N10 C42 C40 177.4(9) . . ? N9 C41 C40 179.3(8) . . ? C6 C7 H36A 109.5 . . ? C6 C7 H36B 109.5 . . ? H36A C7 H36B 109.5 . . ? C6 C7 H36C 109.5 . . ? H36A C7 H36C 109.5 . . ? H36B C7 H36C 109.5 . . ? N2 C3 C2 177.0(8) . . ? C3 N2 Ag2 135.0(8) . 1_545 ? C45 O2 Ag2 149.7(5) . . ? O3 C43 O4 129.2(6) . . ? O3 C43 C44 116.3(5) . . ? O4 C43 C44 114.5(5) . . ? C45 O1 Ag1 125.3(4) . 1_655 ? O1 C45 O2 127.7(6) . . ? O1 C45 C46 113.6(5) . . ? O2 C45 C46 118.6(6) . . ? F4 C44 F6 107.7(6) . . ? F4 C44 F5 105.5(7) . . ? F6 C44 F5 102.9(6) . . ? F4 C44 C43 115.1(5) . . ? F6 C44 C43 113.7(5) . . ? F5 C44 C43 110.9(6) . . ? F2 C46 F1 108.7(7) . . ? F2 C46 F3 105.7(6) . . ? F1 C46 F3 105.8(7) . . ? F2 C46 C45 113.8(6) . . ? F1 C46 C45 112.2(5) . . ? F3 C46 C45 110.2(6) . . ? C43 O4 Ag2 111.6(4) . . ? 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 N6 Ag1 N5 C20 -174.0(6) . . . . ? O1 Ag1 N5 C20 6.0(4) 1_455 . . . ? N6 Ag1 N5 C21 -8.7(10) . . . . ? O1 Ag1 N5 C21 171.3(5) 1_455 . . . ? C23 N8 C24 C25 -162.0(5) . . . . ? N7 N8 C24 C25 19.8(7) . . . . ? C23 N8 C24 C29 18.5(7) . . . . ? N7 N8 C24 C29 -159.8(5) . . . . ? C20 N3 N4 C21 1.2(5) . . . . ? C17 N3 N4 C21 -178.2(4) . . . . ? C20 N3 N4 Ag2 -161.5(4) . . . . ? C17 N3 N4 Ag2 19.1(7) . . . . ? O2 Ag2 N4 C21 104.3(4) . . . . ? O4 Ag2 N4 C21 -17.5(4) . . . . ? N2 Ag2 N4 C21 -127.6(4) 1_565 . . . ? O2 Ag2 N4 N3 -95.0(5) . . . . ? O4 Ag2 N4 N3 143.2(5) . . . . ? N2 Ag2 N4 N3 33.1(5) 1_565 . . . ? C20 N3 C17 C18 8.2(7) . . . . ? N4 N3 C17 C18 -172.5(4) . . . . ? C20 N3 C17 C16 -171.4(5) . . . . ? N4 N3 C17 C16 7.9(7) . . . . ? N5 Ag1 N6 C23 -18.5(9) . . . . ? O1 Ag1 N6 C23 161.5(4) 1_455 . . . ? N5 Ag1 N6 C22 162.2(6) . . . . ? O1 Ag1 N6 C22 -17.8(5) 1_455 . . . ? C25 C24 C29 C28 0.4(7) . . . . ? N8 C24 C29 C28 179.9(4) . . . . ? C31 C32 C39 C38 176.1(4) . . . . ? C33 C32 C39 C38 -2.1(8) . . . . ? C24 C29 C28 C27 0.0(7) . . . . ? C22 N6 C23 N8 0.1(6) . . . . ? Ag1 N6 C23 N8 -179.4(3) . . . . ? N7 N8 C23 N6 -0.7(6) . . . . ? C24 N8 C23 N6 -179.1(4) . . . . ? C39 C32 C31 C30 -173.3(5) . . . . ? C33 C32 C31 C30 4.9(8) . . . . ? C23 N8 N7 C22 1.0(6) . . . . ? C24 N8 N7 C22 179.6(5) . . . . ? C39 C32 C33 C34 -23.2(7) . . . . ? C31 C32 C33 C34 158.7(4) . . . . ? C16 C17 C18 C19 -1.4(8) . . . . ? N3 C17 C18 C19 178.9(4) . . . . ? C15 C14 C13 C12 168.7(5) . . . . ? C19 C14 C13 C12 -12.1(8) . . . . ? C29 C28 C27 C26 0.0(7) . . . . ? C29 C28 C27 C30 179.6(4) . . . . ? C12 C10 C11 C4 -177.7(5) . . . . ? C9 C10 C11 C4 1.3(8) . . . . ? C32 C33 C34 C35 167.5(5) . . . . ? C32 C33 C34 C37 48.4(6) . . . . ? C32 C33 C34 C36 -71.4(6) . . . . ? N3 N4 C21 N5 -1.0(6) . . . . ? Ag2 N4 C21 N5 165.8(3) . . . . ? C20 N5 C21 N4 0.4(6) . . . . ? Ag1 N5 C21 N4 -166.7(3) . . . . ? C19 C14 C15 C16 -0.2(9) . . . . ? C13 C14 C15 C16 179.1(6) . . . . ? C29 C24 C25 C26 -0.8(8) . . . . ? N8 C24 C25 C26 179.7(5) . . . . ? C32 C39 C38 C40 -177.5(5) . . . . ? C32 C39 C38 C37 -1.1(7) . . . . ? C24 C25 C26 C27 0.8(8) . . . . ? C28 C27 C26 C25 -0.4(8) . . . . ? C30 C27 C26 C25 180.0(5) . . . . ? C14 C13 C12 C10 176.2(5) . . . . ? C11 C10 C12 C13 173.3(5) . . . . ? C9 C10 C12 C13 -5.7(8) . . . . ? C32 C31 C30 C27 -179.2(4) . . . . ? C26 C27 C30 C31 -176.1(5) . . . . ? C28 C27 C30 C31 4.3(8) . . . . ? C10 C11 C4 C2 173.3(5) . . . . ? C10 C11 C4 C5 -2.0(8) . . . . ? C21 N5 C20 N3 0.4(5) . . . . ? Ag1 N5 C20 N3 169.6(3) . . . . ? N4 N3 C20 N5 -1.0(5) . . . . ? C17 N3 C20 N5 178.3(4) . . . . ? C11 C10 C9 C6 26.2(7) . . . . ? C12 C10 C9 C6 -154.8(5) . . . . ? C40 C38 C37 C34 -153.9(5) . . . . ? C39 C38 C37 C34 29.7(6) . . . . ? C35 C34 C37 C38 -171.3(5) . . . . ? C33 C34 C37 C38 -51.9(6) . . . . ? C36 C34 C37 C38 68.0(6) . . . . ? C11 C4 C2 C3 -1.5(9) . . . . ? C5 C4 C2 C3 173.7(6) . . . . ? C11 C4 C2 C1 -179.1(5) . . . . ? C5 C4 C2 C1 -3.8(9) . . . . ? C17 C18 C19 C14 -0.8(7) . . . . ? C15 C14 C19 C18 1.6(7) . . . . ? C13 C14 C19 C18 -177.7(4) . . . . ? C18 C17 C16 C15 2.8(9) . . . . ? N3 C17 C16 C15 -177.6(5) . . . . ? C14 C15 C16 C17 -1.9(10) . . . . ? C2 C4 C5 C6 159.2(5) . . . . ? C11 C4 C5 C6 -25.5(7) . . . . ? C39 C38 C40 C42 -5.2(9) . . . . ? C37 C38 C40 C42 178.5(6) . . . . ? C39 C38 C40 C41 175.2(5) . . . . ? C37 C38 C40 C41 -1.1(8) . . . . ? N8 N7 C22 N6 -1.0(7) . . . . ? C23 N6 C22 N7 0.6(7) . . . . ? Ag1 N6 C22 N7 -179.9(4) . . . . ? C4 C5 C6 C7 169.7(5) . . . . ? C4 C5 C6 C8 -69.9(6) . . . . ? C4 C5 C6 C9 50.0(6) . . . . ? C10 C9 C6 C7 -170.8(6) . . . . ? C10 C9 C6 C5 -50.5(7) . . . . ? C10 C9 C6 C8 69.2(7) . . . . ? C4 C2 C1 N1 172(100) . . . . ? C3 C2 C1 N1 -5(100) . . . . ? C38 C40 C42 N10 -93(18) . . . . ? C41 C40 C42 N10 86(18) . . . . ? C38 C40 C41 N9 -75(83) . . . . ? C42 C40 C41 N9 105(83) . . . . ? C4 C2 C3 N2 -34(17) . . . . ? C1 C2 C3 N2 144(17) . . . . ? C2 C3 N2 Ag2 -21(18) . . . 1_545 ? O4 Ag2 O2 C45 179.3(9) . . . . ? N2 Ag2 O2 C45 -45.8(10) 1_565 . . . ? N4 Ag2 O2 C45 82.0(10) . . . . ? Ag1 O1 C45 O2 -25.8(9) 1_655 . . . ? Ag1 O1 C45 C46 154.3(4) 1_655 . . . ? Ag2 O2 C45 O1 175.9(6) . . . . ? Ag2 O2 C45 C46 -4.3(13) . . . . ? O3 C43 C44 F4 -165.0(7) . . . . ? O4 C43 C44 F4 16.7(10) . . . . ? O3 C43 C44 F6 -40.1(9) . . . . ? O4 C43 C44 F6 141.6(7) . . . . ? O3 C43 C44 F5 75.2(8) . . . . ? O4 C43 C44 F5 -103.0(7) . . . . ? O1 C45 C46 F2 98.2(7) . . . . ? O2 C45 C46 F2 -81.6(8) . . . . ? O1 C45 C46 F1 -25.7(9) . . . . ? O2 C45 C46 F1 154.4(7) . . . . ? O1 C45 C46 F3 -143.3(6) . . . . ? O2 C45 C46 F3 36.9(8) . . . . ? O3 C43 O4 Ag2 2.7(9) . . . . ? C44 C43 O4 Ag2 -179.3(4) . . . . ? O2 Ag2 O4 C43 55.9(6) . . . . ? N2 Ag2 O4 C43 -79.3(5) 1_565 . . . ? N4 Ag2 O4 C43 170.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.105 _refine_diff_density_min -1.441 _refine_diff_density_rms 0.209 _database_code_depnum_ccdc_archive 'CCDC 917025' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_8 #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 Ag F6 N10 P' _chemical_formula_sum 'C42 H38 Ag F6 N10 P' _chemical_formula_weight 935.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.768(5) _cell_length_b 7.990(5) _cell_length_c 19.600(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 96.028(5) _cell_angle_gamma 90.000(5) _cell_volume 4169(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5393 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.92 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8421 _exptl_absorpt_correction_T_max 0.8906 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14264 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3669 _reflns_number_gt 2934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+2.6689P] 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 3669 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 1.29597(4) 0.7500 0.07562(17) Uani 1 2 d S . . P1 P 1.0000 0.77579(13) 0.7500 0.0566(3) Uani 1 2 d S . . N3 N 0.94974(8) 1.1823(2) 0.54420(11) 0.0469(5) Uani 1 1 d . . . C2 C 0.81419(9) 0.7124(3) 0.01918(14) 0.0514(6) Uani 1 1 d . . . C17 C 0.93249(9) 1.0722(3) 0.48878(12) 0.0445(5) Uani 1 1 d . . . N5 N 0.97666(9) 1.2854(3) 0.64365(11) 0.0592(6) Uani 1 1 d . . . C4 C 0.82407(9) 0.6404(3) 0.08222(13) 0.0482(6) Uani 1 1 d . . . C16 C 0.91406(9) 1.1402(3) 0.42661(12) 0.0499(6) Uani 1 1 d . . . H16 H 0.9137 1.2556 0.4202 0.060 Uiso 1 1 calc R . . C12 C 0.86539(10) 0.7901(3) 0.26144(13) 0.0517(6) Uani 1 1 d . . . H12 H 0.8679 0.9030 0.2507 0.062 Uiso 1 1 calc R . . C19 C 0.91496(10) 0.7982(3) 0.44559(14) 0.0526(6) Uani 1 1 d . . . H19 H 0.9152 0.6830 0.4525 0.063 Uiso 1 1 calc R . . C13 C 0.87845(10) 0.7470(3) 0.32596(14) 0.0519(6) Uani 1 1 d . . . H13 H 0.8761 0.6342 0.3369 0.062 Uiso 1 1 calc R . . C10 C 0.84741(9) 0.6786(3) 0.20545(13) 0.0473(6) Uani 1 1 d . . . C11 C 0.83695(10) 0.7427(3) 0.14199(14) 0.0504(6) Uani 1 1 d . . . H11 H 0.8381 0.8582 0.1365 0.060 Uiso 1 1 calc R . . C9 C 0.84166(10) 0.4951(3) 0.21913(14) 0.0553(6) Uani 1 1 d . . . H9A H 0.8274 0.4815 0.2623 0.066 Uiso 1 1 calc R . . H9B H 0.8747 0.4436 0.2241 0.066 Uiso 1 1 calc R . . N4 N 0.95470(10) 1.3496(3) 0.53387(12) 0.0683(7) Uani 1 1 d . . . F2 F 0.98184(15) 0.7762(3) 0.67136(14) 0.1484(13) Uani 1 1 d . . . C18 C 0.93314(9) 0.9018(3) 0.49888(13) 0.0531(6) Uani 1 1 d . . . H18 H 0.9457 0.8570 0.5410 0.064 Uiso 1 1 calc R . . C3 C 0.81160(9) 0.8910(4) 0.01060(13) 0.0527(6) Uani 1 1 d . . . C6 C 0.80841(10) 0.4034(3) 0.16269(14) 0.0556(6) Uani 1 1 d . . . C15 C 0.89607(10) 1.0347(3) 0.37398(12) 0.0519(6) Uani 1 1 d . . . H15 H 0.8834 1.0802 0.3320 0.062 Uiso 1 1 calc R . . F3 F 1.03832(10) 0.9183(3) 0.73983(16) 0.1306(10) Uani 1 1 d . . . C14 C 0.89643(9) 0.8614(3) 0.38217(12) 0.0469(6) Uani 1 1 d . . . C5 C 0.82422(11) 0.4537(3) 0.09225(14) 0.0569(7) Uani 1 1 d . . . H5A H 0.8577 0.4109 0.0880 0.068 Uiso 1 1 calc R . . H5B H 0.8014 0.4028 0.0564 0.068 Uiso 1 1 calc R . . N1 N 0.80239(12) 0.5462(4) -0.09385(15) 0.0913(9) Uani 1 1 d . . . N2 N 0.80810(10) 1.0320(4) 0.00463(14) 0.0719(7) Uani 1 1 d . . . C21 C 0.97077(12) 1.4052(4) 0.59491(15) 0.0686(8) Uani 1 1 d . . . H21 H 0.9776 1.5176 0.6040 0.082 Uiso 1 1 calc R . . F1 F 0.96178(8) 0.6360(3) 0.76417(17) 0.1277(10) Uani 1 1 d . . . C20 C 0.96310(11) 1.1486(4) 0.60926(13) 0.0572(7) Uani 1 1 d . . . H20 H 0.9630 1.0421 0.6284 0.069 Uiso 1 1 calc R . . C1 C 0.80684(10) 0.6162(4) -0.04344(14) 0.0613(7) Uani 1 1 d . . . C7 C 0.75317(11) 0.4474(4) 0.16686(17) 0.0739(9) Uani 1 1 d . . . H7A H 0.7326 0.3895 0.1313 0.111 Uiso 1 1 calc R . . H7B H 0.7486 0.5659 0.1611 0.111 Uiso 1 1 calc R . . H7C H 0.7437 0.4144 0.2108 0.111 Uiso 1 1 calc R . . C8 C 0.81606(16) 0.2144(4) 0.17249(19) 0.0840(10) Uani 1 1 d . . . H8A H 0.8506 0.1869 0.1689 0.126 Uiso 1 1 calc R . . H8B H 0.7950 0.1555 0.1377 0.126 Uiso 1 1 calc R . . H8C H 0.8073 0.1825 0.2169 0.126 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 0.1238(3) 0.0575(2) 0.0396(2) 0.000 -0.01968(17) 0.000 P1 0.0659(6) 0.0430(5) 0.0611(6) 0.000 0.0071(5) 0.000 N3 0.0553(12) 0.0428(12) 0.0409(11) -0.0025(9) -0.0030(9) 0.0016(9) C2 0.0488(14) 0.0614(17) 0.0439(14) -0.0099(12) 0.0045(11) -0.0070(12) C17 0.0487(13) 0.0462(14) 0.0373(12) -0.0053(10) -0.0019(10) -0.0016(10) N5 0.0787(15) 0.0545(14) 0.0411(12) -0.0054(10) -0.0093(11) 0.0026(12) C4 0.0489(13) 0.0512(14) 0.0442(14) -0.0068(12) 0.0029(11) -0.0049(11) C16 0.0647(15) 0.0439(14) 0.0405(13) 0.0010(11) 0.0025(11) -0.0007(12) C12 0.0640(15) 0.0452(14) 0.0442(14) -0.0051(11) -0.0034(12) -0.0058(12) C19 0.0659(16) 0.0392(14) 0.0507(15) 0.0010(11) -0.0030(12) 0.0002(12) C13 0.0594(15) 0.0482(14) 0.0461(15) -0.0052(11) -0.0036(12) -0.0048(11) C10 0.0498(13) 0.0461(14) 0.0446(14) -0.0071(11) -0.0026(11) -0.0011(11) C11 0.0602(15) 0.0423(14) 0.0475(15) -0.0059(11) 0.0008(12) -0.0034(11) C9 0.0657(16) 0.0454(14) 0.0517(15) -0.0007(12) -0.0080(12) -0.0005(12) N4 0.1033(18) 0.0477(13) 0.0479(13) 0.0014(11) -0.0205(12) -0.0034(13) F2 0.265(4) 0.0891(17) 0.0777(16) -0.0114(13) -0.044(2) 0.021(2) C18 0.0635(15) 0.0520(15) 0.0403(13) 0.0026(12) -0.0103(11) 0.0026(12) C3 0.0512(15) 0.066(2) 0.0412(14) -0.0007(13) 0.0041(11) -0.0052(13) C6 0.0684(16) 0.0461(14) 0.0502(15) -0.0016(12) -0.0037(12) -0.0095(13) C15 0.0658(16) 0.0546(16) 0.0333(12) 0.0008(11) -0.0039(11) -0.0024(13) F3 0.144(2) 0.0857(16) 0.171(3) -0.0112(16) 0.0608(19) -0.0459(15) C14 0.0486(13) 0.0501(14) 0.0412(13) -0.0070(11) 0.0007(10) -0.0029(11) C5 0.0701(17) 0.0482(15) 0.0512(15) -0.0122(12) 0.0001(13) -0.0024(13) N1 0.112(2) 0.107(2) 0.0555(17) -0.0282(16) 0.0119(15) -0.0151(18) N2 0.0832(18) 0.0686(19) 0.0641(16) 0.0066(14) 0.0086(13) -0.0035(14) C21 0.100(2) 0.0471(16) 0.0523(17) -0.0014(13) -0.0198(15) 0.0004(15) F1 0.0910(14) 0.0864(16) 0.207(3) 0.0242(18) 0.0232(16) -0.0256(13) C20 0.0812(18) 0.0467(15) 0.0408(14) -0.0029(12) -0.0069(12) -0.0004(13) C1 0.0638(17) 0.076(2) 0.0449(16) -0.0060(15) 0.0089(13) -0.0077(15) C7 0.0676(18) 0.083(2) 0.070(2) -0.0028(17) 0.0016(15) -0.0188(16) C8 0.129(3) 0.0470(17) 0.072(2) -0.0024(15) -0.011(2) -0.0122(18) _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 N5 2.114(2) . ? Ag1 N5 2.114(2) 2_756 ? P1 F1 1.559(2) . ? P1 F1 1.559(2) 2_756 ? P1 F3 1.559(2) . ? P1 F3 1.559(2) 2_756 ? P1 F2 1.567(3) 2_756 ? P1 F2 1.567(3) . ? N3 C20 1.316(3) . ? N3 N4 1.361(3) . ? N3 C17 1.436(3) . ? C2 C4 1.363(4) . ? C2 C3 1.438(4) . ? C2 C1 1.444(4) . ? C17 C16 1.378(3) . ? C17 C18 1.376(4) . ? N5 C20 1.316(4) . ? N5 C21 1.349(4) . ? C4 C11 1.440(4) . ? C4 C5 1.505(4) . ? C16 C15 1.379(4) . ? C16 H16 0.9300 . ? C12 C13 1.322(4) . ? C12 C10 1.456(3) . ? C12 H12 0.9300 . ? C19 C14 1.384(4) . ? C19 C18 1.381(4) . ? C19 H19 0.9300 . ? C13 C14 1.473(4) . ? C13 H13 0.9300 . ? C10 C11 1.347(4) . ? C10 C9 1.501(4) . ? C11 H11 0.9300 . ? C9 C6 1.532(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N4 C21 1.306(4) . ? C18 H18 0.9300 . ? C3 N2 1.135(4) . ? C6 C7 1.531(4) . ? C6 C8 1.533(4) . ? C6 C5 1.539(4) . ? C15 C14 1.394(4) . ? C15 H15 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N1 C1 1.131(4) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N5 175.44(13) . 2_756 ? F1 P1 F1 88.5(2) . 2_756 ? F1 P1 F3 177.01(16) . . ? F1 P1 F3 92.74(15) 2_756 . ? F1 P1 F3 92.74(15) . 2_756 ? F1 P1 F3 177.01(16) 2_756 2_756 ? F3 P1 F3 86.2(2) . 2_756 ? F1 P1 F2 88.17(17) . 2_756 ? F1 P1 F2 92.02(17) 2_756 2_756 ? F3 P1 F2 89.07(17) . 2_756 ? F3 P1 F2 90.74(18) 2_756 2_756 ? F1 P1 F2 92.02(17) . . ? F1 P1 F2 88.17(17) 2_756 . ? F3 P1 F2 90.74(18) . . ? F3 P1 F2 89.07(16) 2_756 . ? F2 P1 F2 179.7(2) 2_756 . ? C20 N3 N4 108.9(2) . . ? C20 N3 C17 129.9(2) . . ? N4 N3 C17 121.2(2) . . ? C4 C2 C3 121.8(2) . . ? C4 C2 C1 122.8(3) . . ? C3 C2 C1 115.4(2) . . ? C16 C17 C18 121.1(2) . . ? C16 C17 N3 119.0(2) . . ? C18 C17 N3 120.0(2) . . ? C20 N5 C21 102.8(2) . . ? C20 N5 Ag1 125.1(2) . . ? C21 N5 Ag1 132.09(19) . . ? C2 C4 C11 120.3(2) . . ? C2 C4 C5 122.3(2) . . ? C11 C4 C5 117.3(2) . . ? C17 C16 C15 119.0(2) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C13 C12 C10 126.5(3) . . ? C13 C12 H12 116.7 . . ? C10 C12 H12 116.7 . . ? C14 C19 C18 121.7(2) . . ? C14 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C12 C13 C14 125.9(3) . . ? C12 C13 H13 117.0 . . ? C14 C13 H13 117.0 . . ? C11 C10 C12 118.9(2) . . ? C11 C10 C9 121.4(2) . . ? C12 C10 C9 119.7(2) . . ? C10 C11 C4 122.9(2) . . ? C10 C11 H11 118.5 . . ? C4 C11 H11 118.5 . . ? C10 C9 C6 113.6(2) . . ? C10 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C21 N4 N3 103.0(2) . . ? C17 C18 C19 119.1(2) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N2 C3 C2 177.8(3) . . ? C9 C6 C7 110.0(2) . . ? C9 C6 C8 108.7(2) . . ? C7 C6 C8 109.7(3) . . ? C9 C6 C5 109.2(2) . . ? C7 C6 C5 110.2(2) . . ? C8 C6 C5 108.9(2) . . ? C16 C15 C14 121.6(2) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C19 C14 C15 117.6(2) . . ? C19 C14 C13 120.2(2) . . ? C15 C14 C13 122.2(2) . . ? C4 C5 C6 112.3(2) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N4 C21 N5 114.2(3) . . ? N4 C21 H21 122.9 . . ? N5 C21 H21 122.9 . . ? N3 C20 N5 111.0(3) . . ? N3 C20 H20 124.5 . . ? N5 C20 H20 124.5 . . ? N1 C1 C2 176.8(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 C20 N3 C17 C16 171.1(3) . . . . ? N4 N3 C17 C16 -9.2(4) . . . . ? C20 N3 C17 C18 -7.0(4) . . . . ? N4 N3 C17 C18 172.7(2) . . . . ? N5 Ag1 N5 C20 8.4(2) 2_756 . . . ? N5 Ag1 N5 C21 -172.8(3) 2_756 . . . ? C3 C2 C4 C11 -5.9(4) . . . . ? C1 C2 C4 C11 172.6(2) . . . . ? C3 C2 C4 C5 176.8(2) . . . . ? C1 C2 C4 C5 -4.8(4) . . . . ? C18 C17 C16 C15 0.0(4) . . . . ? N3 C17 C16 C15 -178.1(2) . . . . ? C10 C12 C13 C14 -179.8(2) . . . . ? C13 C12 C10 C11 -178.2(3) . . . . ? C13 C12 C10 C9 0.9(4) . . . . ? C12 C10 C11 C4 173.3(2) . . . . ? C9 C10 C11 C4 -5.7(4) . . . . ? C2 C4 C11 C10 -179.5(2) . . . . ? C5 C4 C11 C10 -2.0(4) . . . . ? C11 C10 C9 C6 -18.3(4) . . . . ? C12 C10 C9 C6 162.7(2) . . . . ? C20 N3 N4 C21 -0.3(3) . . . . ? C17 N3 N4 C21 179.9(2) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? N3 C17 C18 C19 178.0(2) . . . . ? C14 C19 C18 C17 0.4(4) . . . . ? C4 C2 C3 N2 -75(8) . . . . ? C1 C2 C3 N2 107(8) . . . . ? C10 C9 C6 C7 -74.2(3) . . . . ? C10 C9 C6 C8 165.7(3) . . . . ? C10 C9 C6 C5 47.0(3) . . . . ? C17 C16 C15 C14 -0.4(4) . . . . ? C18 C19 C14 C15 -0.8(4) . . . . ? C18 C19 C14 C13 178.5(2) . . . . ? C16 C15 C14 C19 0.8(4) . . . . ? C16 C15 C14 C13 -178.5(2) . . . . ? C12 C13 C14 C19 -171.8(3) . . . . ? C12 C13 C14 C15 7.5(4) . . . . ? C2 C4 C5 C6 -149.7(2) . . . . ? C11 C4 C5 C6 32.9(3) . . . . ? C9 C6 C5 C4 -54.2(3) . . . . ? C7 C6 C5 C4 66.8(3) . . . . ? C8 C6 C5 C4 -172.8(2) . . . . ? N3 N4 C21 N5 0.2(4) . . . . ? C20 N5 C21 N4 0.0(4) . . . . ? Ag1 N5 C21 N4 -179.0(2) . . . . ? N4 N3 C20 N5 0.3(3) . . . . ? C17 N3 C20 N5 -180.0(2) . . . . ? C21 N5 C20 N3 -0.2(3) . . . . ? Ag1 N5 C20 N3 178.92(18) . . . . ? C4 C2 C1 N1 -138(7) . . . . ? C3 C2 C1 N1 40(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.483 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 917026'