Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_address ; School of Chemistry F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_section_title ; Silver(I) complexation of linked 2,2'-dipyridylamine derivatives. Synthetic, solvent extraction, membrane transport and X-ray structural studies ; loop_ _publ_author_name 'Leonard Lindoy' 'Bianca Antonioli' 'David J. Bray' 'Jack K. Clegg' 'Karsten Gloe' 'Kerstin Gloe' ; O.Kataeva ; 'John C. McMurtrie' 'Peter J. Steel' 'Christopher J. Sumby' 'Marco Wenzel' # Attachment 'combinedfinal.cif' data_3cjs _database_code_depnum_ccdc_archive 'CCDC 614167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H39 Ag1.50 Cl F9 N9 O0.50 P1.50' _chemical_formula_weight 1104.54 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.361(5) _cell_length_b 17.001(6) _cell_length_c 20.092(7) _cell_angle_alpha 69.969(4) _cell_angle_beta 73.690(4) _cell_angle_gamma 86.817(5) _cell_volume 4419(2) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2220 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.713277 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31790 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15399 _reflns_number_gt 9151 _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^)+(0.0640P)^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 15399 _refine_ls_number_parameters 1187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.019 _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 1.24307(3) -0.33093(3) 0.65841(2) 0.02893(13) Uani 1 1 d . . . Ag2 Ag 0.83673(3) -0.22287(3) 0.83543(2) 0.03055(13) Uani 1 1 d . . . Ag3 Ag 0.66854(3) 0.15473(3) 0.70378(2) 0.03043(13) Uani 1 1 d . . . C1 C 1.5982(3) -0.3067(4) 0.4342(3) 0.0236(14) Uani 1 1 d . . . C2 C 1.6484(3) -0.3544(3) 0.3919(3) 0.0196(13) Uani 1 1 d . . . C3 C 1.7141(3) -0.3135(4) 0.3228(3) 0.0267(15) Uani 1 1 d . . . H3A H 1.7467 -0.3448 0.2927 0.032 Uiso 1 1 calc R . . C4 C 1.7312(4) -0.2278(4) 0.2986(3) 0.0308(15) Uani 1 1 d . . . H4A H 1.7773 -0.2008 0.2526 0.037 Uiso 1 1 calc R . . C5 C 1.6819(4) -0.1805(4) 0.3407(3) 0.0282(14) Uani 1 1 d . . . H5A H 1.6939 -0.1215 0.3237 0.034 Uiso 1 1 calc R . . C6 C 1.6154(4) -0.2202(4) 0.4074(3) 0.0288(15) Uani 1 1 d . . . H6A H 1.5806 -0.1879 0.4358 0.035 Uiso 1 1 calc R . . N11 N 1.4566(3) -0.2965(3) 0.5364(2) 0.0242(11) Uani 1 1 d . . . C11 C 1.5317(4) -0.3499(3) 0.5102(3) 0.0238(14) Uani 1 1 d . . . H11A H 1.4994 -0.3997 0.5099 0.029 Uiso 1 1 calc R . . H11B H 1.5712 -0.3698 0.5454 0.029 Uiso 1 1 calc R . . C12 C 1.6309(4) -0.4487(3) 0.4189(3) 0.0239(14) Uani 1 1 d . . . H12A H 1.6348 -0.4719 0.4704 0.029 Uiso 1 1 calc R . . H12B H 1.5641 -0.4608 0.4194 0.029 Uiso 1 1 calc R . . N12 N 1.6991(3) -0.4925(3) 0.3748(2) 0.0228(11) Uani 1 1 d . . . N21 N 1.3832(3) -0.2735(3) 0.6496(2) 0.0219(11) Uani 1 1 d . . . C22 C 1.4649(4) -0.2704(3) 0.5944(3) 0.0211(13) Uani 1 1 d . . . C23 C 1.5541(4) -0.2463(4) 0.5956(3) 0.0292(15) Uani 1 1 d . . . H23A H 1.6097 -0.2423 0.5554 0.035 Uiso 1 1 calc R . . C24 C 1.5626(4) -0.2280(4) 0.6555(3) 0.0368(17) Uani 1 1 d . . . H24A H 1.6242 -0.2119 0.6568 0.044 Uiso 1 1 calc R . . C25 C 1.4807(4) -0.2331(4) 0.7139(3) 0.0306(15) Uani 1 1 d . . . H25A H 1.4848 -0.2226 0.7566 0.037 Uiso 1 1 calc R . . C26 C 1.3940(4) -0.2540(4) 0.7071(3) 0.0264(14) Uani 1 1 d . . . H26A H 1.3371 -0.2548 0.7455 0.032 Uiso 1 1 calc R . . N31 N 1.3699(3) -0.3277(3) 0.4667(2) 0.0292(12) Uani 1 1 d . . . C32 C 1.3784(3) -0.2792(3) 0.5046(2) 0.0206(13) Uani 1 1 d . . . C33 C 1.3170(4) -0.2125(4) 0.5102(3) 0.0258(14) Uani 1 1 d . . . H33A H 1.3262 -0.1781 0.5366 0.031 Uiso 1 1 calc R . . C34 C 1.2435(4) -0.1986(4) 0.4764(3) 0.0332(16) Uani 1 1 d . . . H34A H 1.2010 -0.1543 0.4793 0.040 Uiso 1 1 calc R . . C35 C 1.2317(4) -0.2502(4) 0.4377(3) 0.0368(17) Uani 1 1 d . . . H35A H 1.1813 -0.2417 0.4142 0.044 Uiso 1 1 calc R . . C36 C 1.2958(4) -0.3145(4) 0.4347(3) 0.0354(16) Uani 1 1 d . . . H36A H 1.2875 -0.3504 0.4093 0.043 Uiso 1 1 calc R . . N41 N 1.8297(3) -0.5840(3) 0.3763(2) 0.0211(11) Uani 1 1 d . . . C42 C 1.7862(3) -0.5178(3) 0.3934(2) 0.0162(12) Uani 1 1 d . . . C43 C 1.8235(4) -0.4767(4) 0.4308(3) 0.0260(14) Uani 1 1 d . . . H43A H 1.7912 -0.4309 0.4427 0.031 Uiso 1 1 calc R . . C44 C 1.9075(4) -0.5035(4) 0.4499(3) 0.0322(15) Uani 1 1 d . . . H44A H 1.9336 -0.4767 0.4756 0.039 Uiso 1 1 calc R . . C45 C 1.9545(4) -0.5708(4) 0.4310(3) 0.0311(15) Uani 1 1 d . . . H45A H 2.0134 -0.5897 0.4427 0.037 Uiso 1 1 calc R . . C46 C 1.9130(4) -0.6086(4) 0.3953(3) 0.0275(15) Uani 1 1 d . . . H46A H 1.9443 -0.6546 0.3831 0.033 Uiso 1 1 calc R . . N51 N 1.5804(3) -0.5151(3) 0.3227(2) 0.0243(11) Uani 1 1 d . . . C52 C 1.6747(4) -0.5051(3) 0.3148(3) 0.0219(13) Uani 1 1 d . . . C53 C 1.7460(4) -0.5028(4) 0.2500(3) 0.0239(13) Uani 1 1 d . . . H53A H 1.8125 -0.4926 0.2447 0.029 Uiso 1 1 calc R . . C54 C 1.7181(4) -0.5156(4) 0.1943(3) 0.0279(14) Uani 1 1 d . . . H54A H 1.7653 -0.5149 0.1502 0.033 Uiso 1 1 calc R . . C55 C 1.6205(4) -0.5294(4) 0.2029(3) 0.0329(15) Uani 1 1 d . . . H55A H 1.5994 -0.5403 0.1660 0.040 Uiso 1 1 calc R . . C56 C 1.5554(4) -0.5269(4) 0.2670(3) 0.0277(14) Uani 1 1 d . . . H56A H 1.4882 -0.5339 0.2723 0.033 Uiso 1 1 calc R . . C1' C 0.9780(3) -0.5589(3) 0.8677(3) 0.0195(13) Uani 1 1 d . . . C2' C 1.0201(3) -0.6279(4) 0.9087(3) 0.0235(14) Uani 1 1 d . . . C3' C 1.0641(4) -0.6865(4) 0.8766(3) 0.0264(14) Uani 1 1 d . . . H3'A H 1.0929 -0.7333 0.9041 0.032 Uiso 1 1 calc R . . C4' C 1.0661(4) -0.6769(4) 0.8039(3) 0.0302(15) Uani 1 1 d . . . H4'A H 1.0946 -0.7178 0.7829 0.036 Uiso 1 1 calc R . . C5' C 1.0265(3) -0.6077(4) 0.7631(3) 0.0264(14) Uani 1 1 d . . . H5'A H 1.0293 -0.6003 0.7135 0.032 Uiso 1 1 calc R . . C6' C 0.9825(3) -0.5489(4) 0.7944(3) 0.0221(13) Uani 1 1 d . . . H6'A H 0.9552 -0.5016 0.7660 0.027 Uiso 1 1 calc R . . N11' N 0.9005(3) -0.4198(3) 0.8521(2) 0.0226(11) Uani 1 1 d . . . C11' C 0.9280(4) -0.4963(3) 0.9039(3) 0.0251(14) Uani 1 1 d . . . H11C H 0.8688 -0.5241 0.9432 0.030 Uiso 1 1 calc R . . H11D H 0.9720 -0.4801 0.9276 0.030 Uiso 1 1 calc R . . N12' N 1.0722(3) -0.7081(3) 1.0235(2) 0.0247(11) Uani 1 1 d . . . C12' C 1.0185(4) -0.6358(4) 0.9870(3) 0.0259(14) Uani 1 1 d . . . H12C H 1.0471 -0.5834 0.9856 0.031 Uiso 1 1 calc R . . H12D H 0.9501 -0.6418 1.0175 0.031 Uiso 1 1 calc R . . N21' N 0.7661(3) -0.3362(3) 0.8327(2) 0.0240(11) Uani 1 1 d . . . C22' C 0.8035(4) -0.4136(4) 0.8482(3) 0.0244(14) Uani 1 1 d . . . C23' C 0.7482(4) -0.4859(4) 0.8644(3) 0.0275(14) Uani 1 1 d . . . H23B H 0.7758 -0.5393 0.8756 0.033 Uiso 1 1 calc R . . C24' C 0.6528(4) -0.4781(4) 0.8638(3) 0.0376(16) Uani 1 1 d . . . H24B H 0.6137 -0.5267 0.8749 0.045 Uiso 1 1 calc R . . C25' C 0.6131(4) -0.4002(4) 0.8473(3) 0.0341(16) Uani 1 1 d . . . H25B H 0.5471 -0.3943 0.8468 0.041 Uiso 1 1 calc R . . C26' C 0.6714(4) -0.3324(4) 0.8318(3) 0.0305(15) Uani 1 1 d . . . H26B H 0.6444 -0.2787 0.8194 0.037 Uiso 1 1 calc R . . N31' N 1.0504(3) -0.3613(3) 0.8369(2) 0.0278(12) Uani 1 1 d . . . C32' C 0.9738(4) -0.3580(4) 0.8098(3) 0.0225(13) Uani 1 1 d . . . C33' C 0.9697(4) -0.2967(4) 0.7421(3) 0.0270(14) Uani 1 1 d . . . H33B H 0.9158 -0.2961 0.7233 0.032 Uiso 1 1 calc R . . C34' C 1.0456(4) -0.2382(4) 0.7041(3) 0.0329(16) Uani 1 1 d . . . H34B H 1.0447 -0.1968 0.6584 0.040 Uiso 1 1 calc R . . C35' C 1.1247(4) -0.2394(4) 0.7329(3) 0.0324(16) Uani 1 1 d . . . H35B H 1.1768 -0.1985 0.7084 0.039 Uiso 1 1 calc R . . C36' C 1.1228(4) -0.3032(4) 0.7985(3) 0.0327(16) Uani 1 1 d . . . H36B H 1.1767 -0.3059 0.8178 0.039 Uiso 1 1 calc R . . N41' N 1.0496(3) -0.8282(3) 1.1304(2) 0.0237(11) Uani 1 1 d . . . C42' C 1.0192(4) -0.7820(4) 1.0715(3) 0.0244(14) Uani 1 1 d . . . C43' C 0.9343(4) -0.8049(4) 1.0596(3) 0.0320(16) Uani 1 1 d . . . H43B H 0.9140 -0.7716 1.0178 0.038 Uiso 1 1 calc R . . C44' C 0.8809(4) -0.8761(4) 1.1093(3) 0.0395(17) Uani 1 1 d . . . H44B H 0.8228 -0.8922 1.1026 0.047 Uiso 1 1 calc R . . C45' C 0.9130(4) -0.9242(4) 1.1693(3) 0.0376(17) Uani 1 1 d . . . H45B H 0.8781 -0.9742 1.2039 0.045 Uiso 1 1 calc R . . C46' C 0.9963(4) -0.8977(4) 1.1772(3) 0.0327(15) Uani 1 1 d . . . H46B H 1.0177 -0.9306 1.2185 0.039 Uiso 1 1 calc R . . N51' N 1.2037(3) -0.6173(3) 0.9956(2) 0.0275(12) Uani 1 1 d . . . C52' C 1.1725(4) -0.6964(4) 1.0116(3) 0.0283(15) Uani 1 1 d . . . C53' C 1.2351(4) -0.7639(4) 1.0142(3) 0.0266(14) Uani 1 1 d . . . H53B H 1.2113 -0.8187 1.0233 0.032 Uiso 1 1 calc R . . C54' C 1.3326(4) -0.7466(4) 1.0031(3) 0.0387(18) Uani 1 1 d . . . H54B H 1.3769 -0.7904 1.0057 0.046 Uiso 1 1 calc R . . C55' C 1.3659(4) -0.6657(4) 0.9881(3) 0.0368(17) Uani 1 1 d . . . H55B H 1.4325 -0.6533 0.9807 0.044 Uiso 1 1 calc R . . C56' C 1.2995(4) -0.6034(4) 0.9842(3) 0.0333(16) Uani 1 1 d . . . H56B H 1.3226 -0.5477 0.9728 0.040 Uiso 1 1 calc R . . C1" C 0.7305(4) -0.0040(3) 0.9928(3) 0.0224(13) Uani 1 1 d . . . C2" C 0.6887(4) -0.0372(4) 1.0698(3) 0.0257(14) Uani 1 1 d . . . C3" C 0.7458(4) -0.0802(4) 1.1150(3) 0.0288(15) Uani 1 1 d . . . H3"A H 0.7169 -0.1043 1.1666 0.035 Uiso 1 1 calc R . . C4" C 0.8435(4) -0.0888(4) 1.0866(3) 0.0319(15) Uani 1 1 d . . . H4"A H 0.8815 -0.1176 1.1186 0.038 Uiso 1 1 calc R . . C5" C 0.8862(4) -0.0553(4) 1.0110(3) 0.0305(15) Uani 1 1 d . . . H5"A H 0.9537 -0.0603 0.9911 0.037 Uiso 1 1 calc R . . C6" C 0.8291(4) -0.0143(3) 0.9647(3) 0.0258(14) Uani 1 1 d . . . H6"A H 0.8580 0.0071 0.9129 0.031 Uiso 1 1 calc R . . N11" N 0.7193(3) 0.0705(3) 0.8638(2) 0.0240(11) Uani 1 1 d . . . C11" C 0.6672(4) 0.0406(4) 0.9433(2) 0.0261(14) Uani 1 1 d . . . H11E H 0.6127 0.0018 0.9520 0.031 Uiso 1 1 calc R . . H11F H 0.6393 0.0891 0.9574 0.031 Uiso 1 1 calc R . . N12" N 0.5384(3) -0.0787(3) 1.1767(2) 0.0272(12) Uani 1 1 d . . . C12" C 0.5816(4) -0.0224(4) 1.0997(3) 0.0300(15) Uani 1 1 d . . . H12E H 0.5749 0.0365 1.0978 0.036 Uiso 1 1 calc R . . H12F H 0.5449 -0.0312 1.0676 0.036 Uiso 1 1 calc R . . N21" N 0.7549(3) 0.1977(3) 0.7626(2) 0.0237(11) Uani 1 1 d . . . C22" C 0.7561(3) 0.1536(4) 0.8327(3) 0.0222(13) Uani 1 1 d . . . C23" C 0.7877(4) 0.1924(4) 0.8749(3) 0.0284(15) Uani 1 1 d . . . H23C H 0.7891 0.1606 0.9238 0.034 Uiso 1 1 calc R . . C24" C 0.8163(4) 0.2754(4) 0.8458(3) 0.0289(15) Uani 1 1 d . . . H24C H 0.8366 0.3020 0.8744 0.035 Uiso 1 1 calc R . . C25" C 0.8154(4) 0.3198(4) 0.7748(3) 0.0277(14) Uani 1 1 d . . . H25C H 0.8348 0.3776 0.7533 0.033 Uiso 1 1 calc R . . C26" C 0.7858(4) 0.2790(4) 0.7356(3) 0.0277(15) Uani 1 1 d . . . H26C H 0.7870 0.3101 0.6860 0.033 Uiso 1 1 calc R . . N31" N 0.6603(3) -0.0488(3) 0.8547(2) 0.0350(13) Uani 1 1 d . . . C32" C 0.7254(4) 0.0149(4) 0.8254(3) 0.0281(15) Uani 1 1 d . . . C33" C 0.8001(4) 0.0241(4) 0.7592(3) 0.0331(16) Uani 1 1 d . . . H33C H 0.8465 0.0698 0.7386 0.040 Uiso 1 1 calc R . . C34" C 0.8039(5) -0.0348(5) 0.7254(3) 0.0402(17) Uani 1 1 d . . . H34C H 0.8540 -0.0303 0.6815 0.048 Uiso 1 1 calc R . . C35" C 0.7349(5) -0.1002(4) 0.7553(3) 0.0447(19) Uani 1 1 d . . . H35C H 0.7353 -0.1409 0.7325 0.054 Uiso 1 1 calc R . . C36" C 0.6659(5) -0.1036(4) 0.8192(4) 0.0442(18) Uani 1 1 d . . . H36C H 0.6182 -0.1484 0.8400 0.053 Uiso 1 1 calc R . . N41" N 0.4491(3) -0.0742(3) 1.2938(2) 0.0269(12) Uani 1 1 d . . . C42" C 0.5271(4) -0.0467(4) 1.2338(3) 0.0257(14) Uani 1 1 d . . . C43" C 0.5932(4) 0.0139(4) 1.2289(3) 0.0371(16) Uani 1 1 d . . . H43C H 0.6458 0.0352 1.1857 0.045 Uiso 1 1 calc R . . C44" C 0.5819(5) 0.0423(4) 1.2868(4) 0.0450(18) Uani 1 1 d . . . H44C H 0.6276 0.0824 1.2842 0.054 Uiso 1 1 calc R . . C45" C 0.5043(5) 0.0127(4) 1.3488(3) 0.0447(18) Uani 1 1 d . . . H45C H 0.4957 0.0313 1.3895 0.054 Uiso 1 1 calc R . . C46" C 0.4406(4) -0.0440(4) 1.3496(3) 0.0334(16) Uani 1 1 d . . . H46C H 0.3865 -0.0638 1.3919 0.040 Uiso 1 1 calc R . . N51" N 0.4881(3) -0.1718(4) 1.1297(2) 0.0313(13) Uani 1 1 d . . . C52" C 0.5106(3) -0.1612(4) 1.1863(3) 0.0253(14) Uani 1 1 d . . . C53" C 0.5081(4) -0.2286(4) 1.2524(3) 0.0261(14) Uani 1 1 d . . . H53C H 0.5254 -0.2197 1.2916 0.031 Uiso 1 1 calc R . . C54" C 0.4795(4) -0.3077(4) 1.2580(3) 0.0328(16) Uani 1 1 d . . . H54C H 0.4768 -0.3543 1.3015 0.039 Uiso 1 1 calc R . . C55" C 0.4548(4) -0.3183(4) 1.1995(4) 0.0400(17) Uani 1 1 d . . . H55C H 0.4342 -0.3718 1.2024 0.048 Uiso 1 1 calc R . . C56" C 0.4611(4) -0.2487(5) 1.1366(3) 0.0394(17) Uani 1 1 d . . . H56C H 0.4453 -0.2562 1.0963 0.047 Uiso 1 1 calc R . . P1 P 0.65511(11) 0.28229(12) 0.05643(8) 0.0353(4) Uani 1 1 d . . . F1 F 0.7622(2) 0.3188(3) 0.00880(19) 0.0579(12) Uani 1 1 d . . . F2 F 0.6804(3) 0.1963(3) 0.0408(2) 0.0674(13) Uani 1 1 d . . . F3 F 0.6191(3) 0.3188(3) -0.01636(19) 0.0607(12) Uani 1 1 d . . . F4 F 0.5474(2) 0.2466(3) 0.1036(2) 0.0658(13) Uani 1 1 d . . . F5 F 0.6918(3) 0.2455(3) 0.12886(18) 0.0700(14) Uani 1 1 d . . . F6 F 0.6304(3) 0.3671(3) 0.0728(3) 0.0768(14) Uani 1 1 d . . . P2 P 0.24703(11) 0.45886(11) 0.36425(8) 0.0353(4) Uani 1 1 d . . . F7 F 0.1774(2) 0.5309(2) 0.38055(17) 0.0476(10) Uani 1 1 d . . . F8 F 0.1746(2) 0.4362(3) 0.32464(18) 0.0541(11) Uani 1 1 d . . . F9 F 0.1882(2) 0.3935(2) 0.44176(16) 0.0452(10) Uani 1 1 d . . . F10 F 0.3166(2) 0.3858(2) 0.34878(19) 0.0566(12) Uani 1 1 d . . . F11 F 0.3061(2) 0.5235(3) 0.28674(18) 0.0589(12) Uani 1 1 d . . . F12 F 0.3186(3) 0.4823(3) 0.4039(2) 0.0616(12) Uani 1 1 d . . . P3 P 0.7551(2) 1.00191(15) 0.43213(11) 0.0747(8) Uani 1 1 d . . . F13 F 0.8238(4) 1.0781(4) 0.4150(3) 0.115(2) Uani 1 1 d . . . F14 F 0.7277(5) 0.9990(4) 0.5140(3) 0.129(2) Uani 1 1 d . . . F15 F 0.8346(7) 0.9397(5) 0.4459(4) 0.183(4) Uani 1 1 d . . . F16 F 0.7834(5) 1.0056(4) 0.3492(3) 0.123(2) Uani 1 1 d . . . F17 F 0.6797(8) 0.9301(5) 0.4503(4) 0.219(5) Uani 1 1 d . . . F18 F 0.6760(5) 1.0682(5) 0.4146(5) 0.165(3) Uani 1 1 d . . . C60 C 0.0759(8) 0.1938(9) 0.6369(5) 0.122(5) Uani 1 1 d . . . H60A H 0.1438 0.2133 0.6268 0.146 Uiso 1 1 calc R A 1 H60B H 0.0774 0.1518 0.6126 0.146 Uiso 1 1 calc R A 1 Cl61 Cl 0.0153(3) 0.2740(3) 0.5997(2) 0.122(3) Uani 0.691(9) 1 d P B 1 Cl63 Cl -0.0061(17) 0.1792(18) 0.6034(13) 0.276(12) Uiso 0.309(9) 1 d P B 2 Cl62 Cl 0.02698(19) 0.1446(2) 0.73343(17) 0.1157(10) Uani 1 1 d . B . O70 O 0.1976(7) 0.2352(9) 0.3454(5) 0.197(6) Uani 1 1 d . . . H70 H 0.2338 0.1969 0.3376 0.296 Uiso 1 1 calc R . . C71 C 0.1502(8) 0.2124(8) 0.4136(5) 0.120(5) Uani 1 1 d . . . H71A H 0.1892 0.2264 0.4413 0.180 Uiso 1 1 calc R . . H71B H 0.1360 0.1517 0.4325 0.180 Uiso 1 1 calc R . . H71C H 0.0893 0.2415 0.4192 0.180 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 0.0307(2) 0.0277(3) 0.0289(2) -0.0108(2) -0.00702(18) -0.0016(2) Ag2 0.0334(2) 0.0267(3) 0.0309(2) -0.0075(2) -0.01049(18) -0.0007(2) Ag3 0.0285(2) 0.0359(3) 0.0262(2) -0.0100(2) -0.00652(17) -0.0036(2) C1 0.023(3) 0.025(4) 0.018(2) -0.003(2) -0.005(2) 0.005(3) C2 0.022(3) 0.019(3) 0.019(2) -0.004(2) -0.011(2) 0.004(2) C3 0.023(3) 0.032(4) 0.018(3) -0.007(3) 0.001(2) 0.002(3) C4 0.031(3) 0.025(4) 0.023(3) 0.003(3) -0.001(2) 0.001(3) C5 0.030(3) 0.018(4) 0.032(3) -0.001(3) -0.011(2) 0.000(3) C6 0.036(3) 0.025(4) 0.025(3) -0.010(3) -0.009(2) 0.007(3) N11 0.032(2) 0.025(3) 0.017(2) -0.009(2) -0.0063(18) 0.007(2) C11 0.028(3) 0.021(3) 0.019(3) -0.007(2) -0.001(2) 0.006(3) C12 0.025(3) 0.028(4) 0.017(2) -0.011(2) 0.001(2) 0.004(3) N12 0.025(2) 0.025(3) 0.019(2) -0.009(2) -0.0065(18) 0.007(2) N21 0.029(2) 0.020(3) 0.016(2) -0.006(2) -0.0039(18) 0.000(2) C22 0.029(3) 0.017(3) 0.019(3) -0.005(2) -0.009(2) 0.002(3) C23 0.022(3) 0.042(4) 0.026(3) -0.016(3) -0.004(2) 0.002(3) C24 0.024(3) 0.053(5) 0.039(3) -0.020(3) -0.012(2) 0.004(3) C25 0.033(3) 0.040(4) 0.022(3) -0.014(3) -0.010(2) 0.002(3) C26 0.030(3) 0.027(4) 0.021(3) -0.010(3) -0.003(2) 0.003(3) N31 0.039(3) 0.027(3) 0.021(2) -0.009(2) -0.006(2) -0.007(2) C32 0.026(3) 0.017(3) 0.013(2) 0.000(2) -0.002(2) -0.005(3) C33 0.037(3) 0.021(4) 0.018(3) -0.004(2) -0.009(2) 0.005(3) C34 0.034(3) 0.034(4) 0.023(3) -0.002(3) -0.007(2) 0.009(3) C35 0.035(3) 0.046(5) 0.018(3) 0.003(3) -0.005(2) -0.005(3) C36 0.042(3) 0.045(5) 0.020(3) -0.012(3) -0.008(3) -0.007(3) N41 0.022(2) 0.021(3) 0.016(2) -0.004(2) -0.0001(17) -0.002(2) C42 0.019(2) 0.018(3) 0.010(2) -0.003(2) -0.0018(19) -0.002(2) C43 0.031(3) 0.028(4) 0.021(3) -0.008(3) -0.011(2) 0.005(3) C44 0.040(3) 0.040(4) 0.027(3) -0.018(3) -0.016(3) -0.002(3) C45 0.028(3) 0.041(4) 0.027(3) -0.011(3) -0.012(2) 0.010(3) C46 0.026(3) 0.032(4) 0.021(3) -0.007(3) -0.005(2) 0.008(3) N51 0.019(2) 0.027(3) 0.027(2) -0.009(2) -0.0076(18) 0.002(2) C52 0.028(3) 0.014(3) 0.019(3) 0.000(2) -0.008(2) 0.007(3) C53 0.023(3) 0.024(4) 0.023(3) -0.007(2) -0.005(2) -0.001(3) C54 0.030(3) 0.029(4) 0.021(3) -0.008(3) -0.003(2) -0.005(3) C55 0.040(3) 0.036(4) 0.025(3) -0.006(3) -0.018(3) -0.001(3) C56 0.026(3) 0.029(4) 0.028(3) -0.006(3) -0.010(2) -0.001(3) C1' 0.016(2) 0.020(3) 0.020(3) -0.004(2) -0.003(2) -0.001(2) C2' 0.019(3) 0.026(4) 0.024(3) -0.006(3) -0.004(2) -0.003(3) C3' 0.027(3) 0.024(4) 0.028(3) -0.009(3) -0.008(2) 0.004(3) C4' 0.023(3) 0.032(4) 0.034(3) -0.018(3) 0.004(2) -0.002(3) C5' 0.023(3) 0.034(4) 0.019(3) -0.010(3) 0.000(2) -0.002(3) C6' 0.020(3) 0.021(3) 0.021(3) -0.004(2) -0.002(2) -0.007(3) N11' 0.019(2) 0.020(3) 0.025(2) -0.005(2) -0.0023(18) -0.001(2) C11' 0.026(3) 0.022(4) 0.020(3) -0.001(2) -0.006(2) 0.007(3) N12' 0.027(2) 0.020(3) 0.025(2) -0.003(2) -0.0104(19) 0.004(2) C12' 0.032(3) 0.024(4) 0.023(3) -0.008(3) -0.011(2) 0.011(3) N21' 0.023(2) 0.019(3) 0.027(2) -0.004(2) -0.0080(18) 0.003(2) C22' 0.029(3) 0.025(4) 0.015(2) -0.005(2) -0.003(2) 0.005(3) C23' 0.034(3) 0.016(4) 0.030(3) -0.008(3) -0.005(2) 0.002(3) C24' 0.035(3) 0.037(5) 0.043(3) -0.018(3) -0.007(3) -0.003(3) C25' 0.022(3) 0.032(4) 0.051(4) -0.015(3) -0.013(3) -0.002(3) C26' 0.030(3) 0.028(4) 0.041(3) -0.013(3) -0.019(3) 0.008(3) N31' 0.022(2) 0.035(3) 0.028(2) -0.012(2) -0.008(2) 0.005(2) C32' 0.029(3) 0.020(3) 0.021(3) -0.012(2) -0.004(2) 0.007(3) C33' 0.027(3) 0.029(4) 0.023(3) -0.007(3) -0.005(2) 0.000(3) C34' 0.035(3) 0.031(4) 0.023(3) -0.005(3) 0.002(2) 0.002(3) C35' 0.021(3) 0.029(4) 0.040(3) -0.015(3) 0.009(3) -0.008(3) C36' 0.019(3) 0.036(4) 0.041(3) -0.016(3) -0.002(3) 0.003(3) N41' 0.024(2) 0.021(3) 0.024(2) -0.005(2) -0.0074(19) 0.005(2) C42' 0.027(3) 0.022(4) 0.027(3) -0.011(3) -0.008(2) 0.005(3) C43' 0.023(3) 0.037(4) 0.031(3) -0.007(3) -0.006(2) 0.004(3) C44' 0.024(3) 0.044(5) 0.049(4) -0.018(3) -0.005(3) 0.000(3) C45' 0.033(3) 0.025(4) 0.042(3) -0.002(3) -0.001(3) -0.005(3) C46' 0.039(3) 0.022(4) 0.032(3) -0.004(3) -0.010(3) 0.005(3) N51' 0.031(3) 0.024(3) 0.019(2) -0.001(2) -0.0024(19) -0.002(2) C52' 0.025(3) 0.037(4) 0.016(3) -0.003(3) -0.002(2) 0.002(3) C53' 0.028(3) 0.018(4) 0.029(3) -0.007(3) -0.001(2) 0.001(3) C54' 0.030(3) 0.039(5) 0.031(3) 0.000(3) 0.000(3) 0.010(3) C55' 0.025(3) 0.046(5) 0.028(3) -0.002(3) -0.001(2) -0.001(3) C56' 0.039(3) 0.033(4) 0.020(3) -0.003(3) -0.001(2) -0.011(3) C1" 0.028(3) 0.016(3) 0.018(2) -0.001(2) -0.002(2) -0.001(3) C2" 0.029(3) 0.016(3) 0.024(3) 0.000(2) -0.003(2) -0.002(3) C3" 0.030(3) 0.029(4) 0.022(3) -0.003(3) -0.006(2) 0.001(3) C4" 0.037(3) 0.026(4) 0.035(3) -0.011(3) -0.015(3) 0.012(3) C5" 0.022(3) 0.028(4) 0.036(3) -0.007(3) -0.007(2) 0.003(3) C6" 0.030(3) 0.017(3) 0.019(3) 0.001(2) 0.001(2) -0.005(3) N11" 0.035(2) 0.017(3) 0.014(2) -0.001(2) -0.0034(18) -0.002(2) C11" 0.026(3) 0.026(4) 0.016(2) 0.003(2) -0.002(2) 0.001(3) N12" 0.029(2) 0.022(3) 0.022(2) 0.000(2) -0.0023(19) -0.002(2) C12" 0.026(3) 0.031(4) 0.018(3) 0.007(3) -0.003(2) 0.002(3) N21" 0.026(2) 0.025(3) 0.015(2) -0.001(2) -0.0054(17) 0.001(2) C22" 0.019(2) 0.026(4) 0.021(3) -0.009(3) -0.004(2) 0.004(3) C23" 0.034(3) 0.031(4) 0.018(3) -0.006(3) -0.009(2) 0.004(3) C24" 0.034(3) 0.026(4) 0.029(3) -0.011(3) -0.010(2) 0.003(3) C25" 0.033(3) 0.019(4) 0.030(3) -0.006(3) -0.010(2) -0.004(3) C26" 0.028(3) 0.023(4) 0.022(3) 0.005(3) -0.007(2) 0.001(3) N31" 0.046(3) 0.022(3) 0.032(3) -0.002(2) -0.011(2) -0.008(3) C32" 0.034(3) 0.024(4) 0.025(3) -0.001(3) -0.018(2) 0.008(3) C33" 0.035(3) 0.034(4) 0.030(3) -0.009(3) -0.011(2) 0.012(3) C34" 0.043(4) 0.042(5) 0.037(3) -0.017(3) -0.013(3) 0.012(4) C35" 0.067(5) 0.035(5) 0.043(4) -0.019(3) -0.031(3) 0.024(4) C36" 0.059(4) 0.026(4) 0.048(4) -0.004(3) -0.026(3) 0.003(3) N41" 0.033(2) 0.020(3) 0.022(2) -0.002(2) -0.0059(19) -0.002(2) C42" 0.026(3) 0.015(3) 0.030(3) -0.002(3) -0.008(2) 0.004(3) C43" 0.035(3) 0.016(4) 0.055(4) -0.010(3) -0.005(3) -0.008(3) C44" 0.046(4) 0.024(4) 0.073(5) -0.022(4) -0.020(3) -0.004(3) C45" 0.060(4) 0.032(4) 0.047(4) -0.019(3) -0.013(3) -0.003(4) C46" 0.047(4) 0.028(4) 0.023(3) -0.007(3) -0.007(3) -0.004(3) N51" 0.030(3) 0.039(4) 0.026(3) -0.014(2) -0.008(2) 0.006(3) C52" 0.020(3) 0.031(4) 0.020(3) -0.006(3) -0.001(2) 0.000(3) C53" 0.023(3) 0.028(4) 0.025(3) -0.006(3) -0.007(2) 0.001(3) C54" 0.031(3) 0.027(4) 0.035(3) -0.006(3) -0.004(3) 0.000(3) C55" 0.031(3) 0.033(4) 0.056(4) -0.023(4) -0.001(3) -0.002(3) C56" 0.030(3) 0.053(5) 0.040(4) -0.027(4) -0.005(3) 0.007(3) P1 0.0308(8) 0.0502(13) 0.0279(8) -0.0194(8) -0.0063(6) 0.0061(8) F1 0.0332(18) 0.080(3) 0.050(2) -0.015(2) -0.0038(16) -0.003(2) F2 0.095(3) 0.050(3) 0.053(2) -0.025(2) -0.008(2) 0.015(2) F3 0.056(2) 0.085(3) 0.042(2) -0.012(2) -0.0286(18) 0.007(2) F4 0.038(2) 0.092(4) 0.056(2) -0.019(2) 0.0003(17) -0.015(2) F5 0.059(2) 0.122(4) 0.0299(19) -0.025(2) -0.0184(17) 0.023(3) F6 0.068(3) 0.079(4) 0.101(3) -0.064(3) -0.012(2) 0.013(3) P2 0.0312(8) 0.0388(11) 0.0261(7) -0.0013(7) -0.0060(6) 0.0057(8) F7 0.045(2) 0.043(3) 0.0414(19) -0.0059(18) -0.0037(16) 0.0111(18) F8 0.043(2) 0.085(3) 0.0371(19) -0.022(2) -0.0142(16) 0.002(2) F9 0.052(2) 0.040(2) 0.0291(17) 0.0010(16) -0.0037(15) -0.0016(18) F10 0.049(2) 0.052(3) 0.054(2) -0.013(2) -0.0015(17) 0.019(2) F11 0.045(2) 0.059(3) 0.041(2) 0.0074(19) 0.0064(16) 0.001(2) F12 0.048(2) 0.078(3) 0.064(2) -0.022(2) -0.0266(19) 0.000(2) P3 0.132(2) 0.0322(14) 0.0519(12) -0.0151(10) -0.0096(13) -0.0071(16) F13 0.139(5) 0.093(5) 0.092(4) -0.007(3) -0.022(3) -0.044(4) F14 0.216(6) 0.102(5) 0.058(3) -0.043(3) 0.007(3) -0.038(5) F15 0.301(10) 0.151(7) 0.134(6) -0.083(5) -0.104(6) 0.145(8) F16 0.190(6) 0.108(5) 0.060(3) -0.030(3) -0.013(3) -0.002(4) F17 0.376(13) 0.132(7) 0.120(5) -0.055(5) 0.023(7) -0.154(8) F18 0.181(7) 0.156(7) 0.268(9) -0.150(7) -0.152(7) 0.088(6) C60 0.106(8) 0.203(15) 0.091(7) -0.075(9) -0.052(6) 0.020(9) Cl61 0.080(3) 0.120(5) 0.101(3) 0.020(3) 0.000(2) 0.009(2) Cl62 0.0989(19) 0.116(3) 0.126(2) -0.0222(19) -0.0404(17) -0.0195(18) O70 0.138(7) 0.381(17) 0.169(9) -0.183(11) -0.101(7) 0.129(9) C71 0.126(9) 0.149(11) 0.048(5) 0.026(6) -0.031(6) -0.049(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 N21 2.221(5) . ? Ag1 N41 2.222(5) 2_846 ? Ag2 N21' 2.250(5) . ? Ag2 N41' 2.253(5) 2_747 ? Ag3 N41" 2.213(5) 2_657 ? Ag3 N21" 2.232(5) . ? C1 C6 1.392(8) . ? C1 C2 1.401(7) . ? C1 C11 1.508(6) . ? C2 C3 1.405(7) . ? C2 C12 1.516(8) . ? C3 C4 1.381(8) . ? C4 C5 1.389(8) . ? C5 C6 1.377(7) . ? N11 C32 1.411(7) . ? N11 C22 1.417(7) . ? N11 C11 1.471(6) . ? C12 N12 1.478(6) . ? N12 C42 1.407(6) . ? N12 C52 1.431(7) . ? N21 C26 1.355(7) . ? N21 C22 1.359(6) . ? C22 C23 1.375(7) . ? C23 C24 1.378(8) . ? C24 C25 1.391(7) . ? C25 C26 1.370(8) . ? N31 C32 1.331(7) . ? N31 C36 1.361(7) . ? C32 C33 1.412(7) . ? C33 C34 1.378(8) . ? C34 C35 1.399(9) . ? C35 C36 1.396(8) . ? N41 C42 1.357(7) . ? N41 C46 1.357(6) . ? N41 Ag1 2.222(5) 2_846 ? C42 C43 1.403(8) . ? C43 C44 1.375(7) . ? C44 C45 1.407(8) . ? C45 C46 1.373(8) . ? N51 C52 1.331(6) . ? N51 C56 1.345(7) . ? C52 C53 1.402(6) . ? C53 C54 1.374(7) . ? C54 C55 1.386(7) . ? C55 C56 1.376(7) . ? C1' C2' 1.400(7) . ? C1' C6' 1.407(7) . ? C1' C11' 1.526(7) . ? C2' C3' 1.397(8) . ? C2' C12' 1.527(7) . ? C3' C4' 1.405(7) . ? C4' C5' 1.380(8) . ? C5' C6' 1.390(8) . ? N11' C32' 1.393(7) . ? N11' C22' 1.413(6) . ? N11' C11' 1.475(6) . ? N12' C42' 1.398(7) . ? N12' C52' 1.407(7) . ? N12' C12' 1.494(6) . ? N21' C22' 1.361(7) . ? N21' C26' 1.364(7) . ? C22' C23' 1.392(8) . ? C23' C24' 1.372(8) . ? C24' C25' 1.382(8) . ? C25' C26' 1.357(8) . ? N31' C36' 1.339(7) . ? N31' C32' 1.347(7) . ? C32' C33' 1.417(7) . ? C33' C34' 1.376(8) . ? C34' C35' 1.407(8) . ? C35' C36' 1.386(8) . ? N41' C46' 1.342(7) . ? N41' C42' 1.351(6) . ? N41' Ag2 2.253(5) 2_747 ? C42' C43' 1.406(8) . ? C43' C44' 1.378(8) . ? C44' C45' 1.389(8) . ? C45' C46' 1.370(8) . ? N51' C52' 1.342(8) . ? N51' C56' 1.351(7) . ? C52' C53' 1.414(8) . ? C53' C54' 1.387(8) . ? C54' C55' 1.385(9) . ? C55' C56' 1.381(8) . ? C1" C6" 1.394(7) . ? C1" C2" 1.411(7) . ? C1" C11" 1.517(7) . ? C2" C3" 1.389(7) . ? C2" C12" 1.527(7) . ? C3" C4" 1.379(7) . ? C4" C5" 1.389(7) . ? C5" C6" 1.395(7) . ? N11" C32" 1.396(7) . ? N11" C22" 1.400(7) . ? N11" C11" 1.477(6) . ? N12" C42" 1.398(7) . ? N12" C52" 1.413(7) . ? N12" C12" 1.485(6) . ? N21" C26" 1.350(7) . ? N21" C22" 1.355(6) . ? C22" C23" 1.411(8) . ? C23" C24" 1.367(8) . ? C24" C25" 1.370(7) . ? C25" C26" 1.370(8) . ? N31" C32" 1.327(7) . ? N31" C36" 1.341(8) . ? C32" C33" 1.421(7) . ? C33" C34" 1.380(9) . ? C34" C35" 1.382(9) . ? C35" C36" 1.369(9) . ? N41" C42" 1.358(6) . ? N41" C46" 1.358(7) . ? N41" Ag3 2.213(5) 2_657 ? C42" C43" 1.399(8) . ? C43" C44" 1.373(9) . ? C44" C45" 1.378(9) . ? C45" C46" 1.359(9) . ? N51" C52" 1.334(7) . ? N51" C56" 1.335(8) . ? C52" C53" 1.419(7) . ? C53" C54" 1.387(8) . ? C54" C55" 1.387(9) . ? C55" C56" 1.389(9) . ? P1 F6 1.587(5) . ? P1 F1 1.594(4) . ? P1 F4 1.596(4) . ? P1 F5 1.599(4) . ? P1 F2 1.599(4) . ? P1 F3 1.600(4) . ? P2 F11 1.594(3) . ? P2 F9 1.598(3) . ? P2 F7 1.601(4) . ? P2 F12 1.603(4) . ? P2 F8 1.607(4) . ? P2 F10 1.609(4) . ? P3 F15 1.529(7) . ? P3 F17 1.554(8) . ? P3 F13 1.554(6) . ? P3 F14 1.565(5) . ? P3 F16 1.581(5) . ? P3 F18 1.580(6) . ? C60 Cl61 1.58(2) . ? C60 Cl61 1.647(12) . ? C60 Cl62 1.773(10) . ? O70 C71 1.277(11) . ? 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 N21 Ag1 N41 146.11(14) . 2_846 ? N21' Ag2 N41' 147.49(15) . 2_747 ? N41" Ag3 N21" 150.23(15) 2_657 . ? C6 C1 C2 119.3(4) . . ? C6 C1 C11 120.7(5) . . ? C2 C1 C11 119.9(5) . . ? C1 C2 C3 119.1(5) . . ? C1 C2 C12 120.8(4) . . ? C3 C2 C12 120.0(5) . . ? C4 C3 C2 120.1(5) . . ? C3 C4 C5 120.9(5) . . ? C6 C5 C4 119.1(6) . . ? C5 C6 C1 121.5(5) . . ? C32 N11 C22 124.8(4) . . ? C32 N11 C11 117.2(4) . . ? C22 N11 C11 117.9(4) . . ? N11 C11 C1 114.0(4) . . ? N12 C12 C2 115.1(4) . . ? C42 N12 C52 123.6(4) . . ? C42 N12 C12 117.7(4) . . ? C52 N12 C12 118.6(4) . . ? C26 N21 C22 116.8(5) . . ? C26 N21 Ag1 119.6(3) . . ? C22 N21 Ag1 122.5(4) . . ? N21 C22 C23 121.8(5) . . ? N21 C22 N11 117.8(5) . . ? C23 C22 N11 120.3(4) . . ? C22 C23 C24 119.8(5) . . ? C23 C24 C25 119.9(5) . . ? C26 C25 C24 116.7(5) . . ? N21 C26 C25 124.9(4) . . ? C32 N31 C36 118.1(5) . . ? N31 C32 C33 122.9(5) . . ? N31 C32 N11 115.1(5) . . ? C33 C32 N11 121.9(5) . . ? C34 C33 C32 118.4(6) . . ? C33 C34 C35 119.6(6) . . ? C36 C35 C34 118.3(6) . . ? N31 C36 C35 122.6(6) . . ? C42 N41 C46 117.5(5) . . ? C42 N41 Ag1 123.1(3) . 2_846 ? C46 N41 Ag1 118.1(4) . 2_846 ? N41 C42 C43 122.1(5) . . ? N41 C42 N12 117.9(5) . . ? C43 C42 N12 119.9(5) . . ? C44 C43 C42 119.0(5) . . ? C43 C44 C45 119.5(6) . . ? C46 C45 C44 118.1(5) . . ? N41 C46 C45 123.7(5) . . ? C52 N51 C56 117.5(4) . . ? N51 C52 C53 122.2(5) . . ? N51 C52 N12 116.2(4) . . ? C53 C52 N12 121.5(5) . . ? C54 C53 C52 118.9(5) . . ? C53 C54 C55 119.5(5) . . ? C56 C55 C54 117.5(5) . . ? N51 C56 C55 124.3(5) . . ? C2' C1' C6' 119.4(5) . . ? C2' C1' C11' 119.0(4) . . ? C6' C1' C11' 121.6(5) . . ? C3' C2' C1' 119.4(5) . . ? C3' C2' C12' 121.8(5) . . ? C1' C2' C12' 118.8(5) . . ? C2' C3' C4' 120.7(5) . . ? C5' C4' C3' 119.7(5) . . ? C4' C5' C6' 120.2(5) . . ? C5' C6' C1' 120.6(5) . . ? C32' N11' C22' 124.4(4) . . ? C32' N11' C11' 116.6(4) . . ? C22' N11' C11' 118.9(4) . . ? N11' C11' C1' 113.8(4) . . ? C42' N12' C52' 123.2(4) . . ? C42' N12' C12' 118.4(4) . . ? C52' N12' C12' 118.3(5) . . ? N12' C12' C2' 114.2(4) . . ? C22' N21' C26' 116.5(5) . . ? C22' N21' Ag2 123.9(4) . . ? C26' N21' Ag2 117.9(4) . . ? N21' C22' C23' 122.4(5) . . ? N21' C22' N11' 117.7(5) . . ? C23' C22' N11' 119.8(5) . . ? C24' C23' C22' 118.3(5) . . ? C23' C24' C25' 120.6(6) . . ? C26' C25' C24' 117.9(5) . . ? C25' C26' N21' 124.3(6) . . ? C36' N31' C32' 118.0(5) . . ? N31' C32' N11' 115.5(4) . . ? N31' C32' C33' 121.9(5) . . ? N11' C32' C33' 122.7(5) . . ? C34' C33' C32' 118.5(5) . . ? C33' C34' C35' 120.2(5) . . ? C36' C35' C34' 116.7(5) . . ? N31' C36' C35' 124.7(6) . . ? C46' N41' C42' 117.5(5) . . ? C46' N41' Ag2 119.5(4) . 2_747 ? C42' N41' Ag2 121.5(4) . 2_747 ? N41' C42' N12' 118.3(5) . . ? N41' C42' C43' 121.7(5) . . ? N12' C42' C43' 120.0(5) . . ? C44' C43' C42' 119.0(5) . . ? C43' C44' C45' 119.3(6) . . ? C46' C45' C44' 118.1(6) . . ? N41' C46' C45' 124.3(5) . . ? C52' N51' C56' 117.3(5) . . ? N51' C52' N12' 115.4(5) . . ? N51' C52' C53' 123.3(5) . . ? N12' C52' C53' 121.2(6) . . ? C54' C53' C52' 117.0(6) . . ? C53' C54' C55' 120.4(6) . . ? C56' C55' C54' 118.2(6) . . ? N51' C56' C55' 123.6(6) . . ? C6" C1" C2" 118.4(5) . . ? C6" C1" C11" 122.3(4) . . ? C2" C1" C11" 119.3(4) . . ? C3" C2" C1" 119.4(4) . . ? C3" C2" C12" 122.9(4) . . ? C1" C2" C12" 117.6(5) . . ? C4" C3" C2" 121.5(5) . . ? C3" C4" C5" 119.8(5) . . ? C4" C5" C6" 119.3(5) . . ? C1" C6" C5" 121.5(4) . . ? C32" N11" C22" 125.2(4) . . ? C32" N11" C11" 117.8(5) . . ? C22" N11" C11" 116.9(4) . . ? N11" C11" C1" 114.0(4) . . ? C42" N12" C52" 124.9(4) . . ? C42" N12" C12" 118.4(5) . . ? C52" N12" C12" 116.8(5) . . ? N12" C12" C2" 112.8(4) . . ? C26" N21" C22" 117.0(5) . . ? C26" N21" Ag3 118.0(4) . . ? C22" N21" Ag3 122.7(4) . . ? N21" C22" N11" 118.4(5) . . ? N21" C22" C23" 120.7(5) . . ? N11" C22" C23" 120.8(5) . . ? C24" C23" C22" 120.3(5) . . ? C23" C24" C25" 118.9(6) . . ? C24" C25" C26" 118.7(6) . . ? N21" C26" C25" 124.4(5) . . ? C32" N31" C36" 118.0(5) . . ? N31" C32" N11" 117.1(5) . . ? N31" C32" C33" 121.1(6) . . ? N11" C32" C33" 121.8(6) . . ? C34" C33" C32" 118.8(6) . . ? C33" C34" C35" 120.0(6) . . ? C36" C35" C34" 116.9(7) . . ? N31" C36" C35" 125.2(7) . . ? C42" N41" C46" 117.7(5) . . ? C42" N41" Ag3 121.3(4) . 2_657 ? C46" N41" Ag3 120.7(4) . 2_657 ? N41" C42" C43" 120.3(5) . . ? N41" C42" N12" 118.5(5) . . ? C43" C42" N12" 121.2(5) . . ? C44" C43" C42" 119.8(5) . . ? C43" C44" C45" 120.0(7) . . ? C46" C45" C44" 117.8(6) . . ? N41" C46" C45" 124.3(5) . . ? C52" N51" C56" 118.2(5) . . ? N51" C52" N12" 116.3(5) . . ? N51" C52" C53" 122.4(6) . . ? N12" C52" C53" 121.3(5) . . ? C54" C53" C52" 118.0(6) . . ? C53" C54" C55" 119.4(6) . . ? C56" C55" C54" 118.3(7) . . ? N51" C56" C55" 123.6(6) . . ? F6 P1 F1 90.5(2) . . ? F6 P1 F4 89.2(2) . . ? F1 P1 F4 179.4(3) . . ? F6 P1 F5 90.1(3) . . ? F1 P1 F5 90.1(2) . . ? F4 P1 F5 90.4(2) . . ? F6 P1 F2 179.3(3) . . ? F1 P1 F2 89.5(2) . . ? F4 P1 F2 90.8(2) . . ? F5 P1 F2 89.2(2) . . ? F6 P1 F3 90.2(3) . . ? F1 P1 F3 89.6(2) . . ? F4 P1 F3 89.9(2) . . ? F5 P1 F3 179.6(2) . . ? F2 P1 F3 90.5(2) . . ? F11 P2 F9 179.5(2) . . ? F11 P2 F7 90.7(2) . . ? F9 P2 F7 89.76(18) . . ? F11 P2 F12 90.5(2) . . ? F9 P2 F12 89.6(2) . . ? F7 P2 F12 89.6(2) . . ? F11 P2 F8 89.5(2) . . ? F9 P2 F8 90.4(2) . . ? F7 P2 F8 89.8(2) . . ? F12 P2 F8 179.4(2) . . ? F11 P2 F10 89.9(2) . . ? F9 P2 F10 89.6(2) . . ? F7 P2 F10 179.4(2) . . ? F12 P2 F10 90.3(2) . . ? F8 P2 F10 90.4(2) . . ? F15 P3 F17 91.7(5) . . ? F15 P3 F13 92.4(5) . . ? F17 P3 F13 175.6(5) . . ? F15 P3 F14 90.6(4) . . ? F17 P3 F14 92.8(4) . . ? F13 P3 F14 85.7(3) . . ? F15 P3 F16 89.4(4) . . ? F17 P3 F16 87.7(4) . . ? F13 P3 F16 93.8(3) . . ? F14 P3 F16 179.5(4) . . ? F15 P3 F18 177.6(5) . . ? F17 P3 F18 89.7(6) . . ? F13 P3 F18 86.2(4) . . ? F14 P3 F18 91.3(4) . . ? F16 P3 F18 88.6(4) . . ? Cl61 C60 Cl61 60.7(11) . . ? Cl61 C60 Cl62 104.2(11) . . ? Cl61 C60 Cl62 114.2(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 C6 C1 C2 C3 -0.9(8) . . . . ? C11 C1 C2 C3 -176.6(5) . . . . ? C6 C1 C2 C12 -179.4(5) . . . . ? C11 C1 C2 C12 4.8(8) . . . . ? C1 C2 C3 C4 2.4(8) . . . . ? C12 C2 C3 C4 -179.0(5) . . . . ? C2 C3 C4 C5 -2.1(9) . . . . ? C3 C4 C5 C6 0.2(9) . . . . ? C4 C5 C6 C1 1.4(9) . . . . ? C2 C1 C6 C5 -1.0(8) . . . . ? C11 C1 C6 C5 174.7(5) . . . . ? C32 N11 C11 C1 73.9(6) . . . . ? C22 N11 C11 C1 -109.7(5) . . . . ? C6 C1 C11 N11 27.1(8) . . . . ? C2 C1 C11 N11 -157.3(5) . . . . ? C1 C2 C12 N12 -170.9(5) . . . . ? C3 C2 C12 N12 10.6(7) . . . . ? C2 C12 N12 C42 87.7(6) . . . . ? C2 C12 N12 C52 -90.7(6) . . . . ? N41 Ag1 N21 C26 -150.0(4) 2_846 . . . ? N41 Ag1 N21 C22 18.0(5) 2_846 . . . ? C26 N21 C22 C23 -1.7(8) . . . . ? Ag1 N21 C22 C23 -170.0(4) . . . . ? C26 N21 C22 N11 175.4(5) . . . . ? Ag1 N21 C22 N11 7.1(6) . . . . ? C32 N11 C22 N21 39.5(7) . . . . ? C11 N11 C22 N21 -136.5(5) . . . . ? C32 N11 C22 C23 -143.3(5) . . . . ? C11 N11 C22 C23 40.6(7) . . . . ? N21 C22 C23 C24 2.7(9) . . . . ? N11 C22 C23 C24 -174.4(5) . . . . ? C22 C23 C24 C25 -0.7(9) . . . . ? C23 C24 C25 C26 -2.1(9) . . . . ? C22 N21 C26 C25 -1.3(8) . . . . ? Ag1 N21 C26 C25 167.4(5) . . . . ? C24 C25 C26 N21 3.2(9) . . . . ? C36 N31 C32 C33 -3.0(7) . . . . ? C36 N31 C32 N11 179.9(4) . . . . ? C22 N11 C32 N31 -161.8(5) . . . . ? C11 N11 C32 N31 14.3(6) . . . . ? C22 N11 C32 C33 21.0(7) . . . . ? C11 N11 C32 C33 -162.9(4) . . . . ? N31 C32 C33 C34 1.7(7) . . . . ? N11 C32 C33 C34 178.7(4) . . . . ? C32 C33 C34 C35 -0.1(8) . . . . ? C33 C34 C35 C36 -0.2(8) . . . . ? C32 N31 C36 C35 2.7(8) . . . . ? C34 C35 C36 N31 -1.1(8) . . . . ? C46 N41 C42 C43 -1.4(7) . . . . ? Ag1 N41 C42 C43 165.2(4) 2_846 . . . ? C46 N41 C42 N12 -179.2(4) . . . . ? Ag1 N41 C42 N12 -12.6(5) 2_846 . . . ? C52 N12 C42 N41 -27.6(7) . . . . ? C12 N12 C42 N41 154.1(4) . . . . ? C52 N12 C42 C43 154.6(5) . . . . ? C12 N12 C42 C43 -23.7(7) . . . . ? N41 C42 C43 C44 0.9(7) . . . . ? N12 C42 C43 C44 178.6(4) . . . . ? C42 C43 C44 C45 0.5(8) . . . . ? C43 C44 C45 C46 -1.3(8) . . . . ? C42 N41 C46 C45 0.6(7) . . . . ? Ag1 N41 C46 C45 -166.7(4) 2_846 . . . ? C44 C45 C46 N41 0.8(8) . . . . ? C56 N51 C52 C53 2.8(8) . . . . ? C56 N51 C52 N12 179.9(5) . . . . ? C42 N12 C52 N51 150.0(5) . . . . ? C12 N12 C52 N51 -31.7(7) . . . . ? C42 N12 C52 C53 -32.9(8) . . . . ? C12 N12 C52 C53 145.4(5) . . . . ? N51 C52 C53 C54 -3.3(8) . . . . ? N12 C52 C53 C54 179.8(5) . . . . ? C52 C53 C54 C55 0.7(9) . . . . ? C53 C54 C55 C56 2.1(9) . . . . ? C52 N51 C56 C55 0.2(9) . . . . ? C54 C55 C56 N51 -2.7(9) . . . . ? C6' C1' C2' C3' -1.3(8) . . . . ? C11' C1' C2' C3' 178.6(5) . . . . ? C6' C1' C2' C12' 177.4(5) . . . . ? C11' C1' C2' C12' -2.8(7) . . . . ? C1' C2' C3' C4' -0.2(8) . . . . ? C12' C2' C3' C4' -178.8(5) . . . . ? C2' C3' C4' C5' 1.7(8) . . . . ? C3' C4' C5' C6' -1.7(8) . . . . ? C4' C5' C6' C1' 0.2(8) . . . . ? C2' C1' C6' C5' 1.3(8) . . . . ? C11' C1' C6' C5' -178.5(5) . . . . ? C32' N11' C11' C1' -80.6(6) . . . . ? C22' N11' C11' C1' 99.2(5) . . . . ? C2' C1' C11' N11' 170.7(5) . . . . ? C6' C1' C11' N11' -9.5(7) . . . . ? C42' N12' C12' C2' -97.8(6) . . . . ? C52' N12' C12' C2' 86.4(6) . . . . ? C3' C2' C12' N12' 3.2(8) . . . . ? C1' C2' C12' N12' -175.5(5) . . . . ? N41' Ag2 N21' C22' -13.2(5) 2_747 . . . ? N41' Ag2 N21' C26' 151.7(3) 2_747 . . . ? C26' N21' C22' C23' -1.8(7) . . . . ? Ag2 N21' C22' C23' 163.3(4) . . . . ? C26' N21' C22' N11' -177.9(4) . . . . ? Ag2 N21' C22' N11' -12.8(6) . . . . ? C32' N11' C22' N21' -32.7(7) . . . . ? C11' N11' C22' N21' 147.5(4) . . . . ? C32' N11' C22' C23' 151.1(5) . . . . ? C11' N11' C22' C23' -28.7(7) . . . . ? N21' C22' C23' C24' 0.7(8) . . . . ? N11' C22' C23' C24' 176.7(5) . . . . ? C22' C23' C24' C25' 0.2(8) . . . . ? C23' C24' C25' C26' 0.1(9) . . . . ? C24' C25' C26' N21' -1.3(9) . . . . ? C22' N21' C26' C25' 2.1(8) . . . . ? Ag2 N21' C26' C25' -163.9(5) . . . . ? C36' N31' C32' N11' -179.7(4) . . . . ? C36' N31' C32' C33' 1.5(8) . . . . ? C22' N11' C32' N31' 158.8(5) . . . . ? C11' N11' C32' N31' -21.4(6) . . . . ? C22' N11' C32' C33' -22.5(8) . . . . ? C11' N11' C32' C33' 157.4(5) . . . . ? N31' C32' C33' C34' -1.3(8) . . . . ? N11' C32' C33' C34' 180.0(5) . . . . ? C32' C33' C34' C35' -0.6(8) . . . . ? C33' C34' C35' C36' 2.1(8) . . . . ? C32' N31' C36' C35' 0.2(8) . . . . ? C34' C35' C36' N31' -2.0(8) . . . . ? C46' N41' C42' N12' 178.1(4) . . . . ? Ag2 N41' C42' N12' 12.0(6) 2_747 . . . ? C46' N41' C42' C43' 0.8(7) . . . . ? Ag2 N41' C42' C43' -165.3(4) 2_747 . . . ? C52' N12' C42' N41' 29.3(7) . . . . ? C12' N12' C42' N41' -146.2(5) . . . . ? C52' N12' C42' C43' -153.3(5) . . . . ? C12' N12' C42' C43' 31.2(7) . . . . ? N41' C42' C43' C44' 0.0(8) . . . . ? N12' C42' C43' C44' -177.3(5) . . . . ? C42' C43' C44' C45' -0.9(8) . . . . ? C43' C44' C45' C46' 1.1(9) . . . . ? C42' N41' C46' C45' -0.6(8) . . . . ? Ag2 N41' C46' C45' 165.7(5) 2_747 . . . ? C44' C45' C46' N41' -0.3(9) . . . . ? C56' N51' C52' N12' 179.7(4) . . . . ? C56' N51' C52' C53' -2.3(7) . . . . ? C42' N12' C52' N51' -149.0(5) . . . . ? C12' N12' C52' N51' 26.6(6) . . . . ? C42' N12' C52' C53' 32.9(7) . . . . ? C12' N12' C52' C53' -151.5(5) . . . . ? N51' C52' C53' C54' 3.1(8) . . . . ? N12' C52' C53' C54' -178.9(5) . . . . ? C52' C53' C54' C55' -1.7(8) . . . . ? C53' C54' C55' C56' -0.4(8) . . . . ? C52' N51' C56' C55' 0.0(7) . . . . ? C54' C55' C56' N51' 1.4(8) . . . . ? C6" C1" C2" C3" -1.2(9) . . . . ? C11" C1" C2" C3" 178.1(6) . . . . ? C6" C1" C2" C12" 177.7(5) . . . . ? C11" C1" C2" C12" -2.9(8) . . . . ? C1" C2" C3" C4" 2.2(9) . . . . ? C12" C2" C3" C4" -176.6(6) . . . . ? C2" C3" C4" C5" -1.2(9) . . . . ? C3" C4" C5" C6" -0.9(9) . . . . ? C2" C1" C6" C5" -0.8(9) . . . . ? C11" C1" C6" C5" 179.9(6) . . . . ? C4" C5" C6" C1" 1.9(9) . . . . ? C32" N11" C11" C1" 87.1(6) . . . . ? C22" N11" C11" C1" -94.7(6) . . . . ? C6" C1" C11" N11" 0.7(8) . . . . ? C2" C1" C11" N11" -178.6(5) . . . . ? C42" N12" C12" C2" 100.6(6) . . . . ? C52" N12" C12" C2" -80.0(6) . . . . ? C3" C2" C12" N12" -17.2(9) . . . . ? C1" C2" C12" N12" 163.9(5) . . . . ? N41" Ag3 N21" C26" -145.1(4) 2_657 . . . ? N41" Ag3 N21" C22" 17.0(6) 2_657 . . . ? C26" N21" C22" N11" 176.3(4) . . . . ? Ag3 N21" C22" N11" 14.0(6) . . . . ? C26" N21" C22" C23" 0.5(6) . . . . ? Ag3 N21" C22" C23" -161.8(3) . . . . ? C32" N11" C22" N21" 33.7(7) . . . . ? C11" N11" C22" N21" -144.3(4) . . . . ? C32" N11" C22" C23" -150.4(5) . . . . ? C11" N11" C22" C23" 31.5(6) . . . . ? N21" C22" C23" C24" 0.9(7) . . . . ? N11" C22" C23" C24" -174.8(4) . . . . ? C22" C23" C24" C25" -1.1(7) . . . . ? C23" C24" C25" C26" -0.1(7) . . . . ? C22" N21" C26" C25" -1.8(7) . . . . ? Ag3 N21" C26" C25" 161.4(4) . . . . ? C24" C25" C26" N21" 1.6(8) . . . . ? C36" N31" C32" N11" -179.0(5) . . . . ? C36" N31" C32" C33" -1.2(8) . . . . ? C22" N11" C32" N31" -156.9(5) . . . . ? C11" N11" C32" N31" 21.2(7) . . . . ? C22" N11" C32" C33" 25.4(8) . . . . ? C11" N11" C32" C33" -156.6(5) . . . . ? N31" C32" C33" C34" 0.1(8) . . . . ? N11" C32" C33" C34" 177.8(5) . . . . ? C32" C33" C34" C35" 1.1(8) . . . . ? C33" C34" C35" C36" -1.1(9) . . . . ? C32" N31" C36" C35" 1.3(9) . . . . ? C34" C35" C36" N31" -0.1(9) . . . . ? C46" N41" C42" C43" -3.1(7) . . . . ? Ag3 N41" C42" C43" 170.5(4) 2_657 . . . ? C46" N41" C42" N12" 178.4(5) . . . . ? Ag3 N41" C42" N12" -8.0(6) 2_657 . . . ? C52" N12" C42" N41" -33.6(7) . . . . ? C12" N12" C42" N41" 145.7(5) . . . . ? C52" N12" C42" C43" 147.9(5) . . . . ? C12" N12" C42" C43" -32.9(7) . . . . ? N41" C42" C43" C44" 3.4(8) . . . . ? N12" C42" C43" C44" -178.1(5) . . . . ? C42" C43" C44" C45" -1.5(9) . . . . ? C43" C44" C45" C46" -0.6(10) . . . . ? C42" N41" C46" C45" 0.9(8) . . . . ? Ag3 N41" C46" C45" -172.7(5) 2_657 . . . ? C44" C45" C46" N41" 0.9(10) . . . . ? C56" N51" C52" N12" -179.7(4) . . . . ? C56" N51" C52" C53" 1.0(7) . . . . ? C42" N12" C52" N51" 152.9(5) . . . . ? C12" N12" C52" N51" -26.4(6) . . . . ? C42" N12" C52" C53" -27.8(7) . . . . ? C12" N12" C52" C53" 153.0(4) . . . . ? N51" C52" C53" C54" -1.1(7) . . . . ? N12" C52" C53" C54" 179.6(4) . . . . ? C52" C53" C54" C55" 0.2(7) . . . . ? C53" C54" C55" C56" 0.9(7) . . . . ? C52" N51" C56" C55" 0.2(8) . . . . ? C54" C55" C56" N51" -1.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.045 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.115 #END data_3csbo _database_code_depnum_ccdc_archive 'CCDC 614168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 N6' _chemical_formula_weight 444.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.483(2) _cell_length_b 16.999(4) _cell_length_c 8.759(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.643(3) _cell_angle_gamma 90.00 _cell_volume 1138.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 4952 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.767164 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 14413 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0084 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.40 _reflns_number_total 2292 _reflns_number_gt 2102 _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^)+(0.0481P)^2^+0.3332P] 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 2292 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 C1 C 0.39404(15) 0.06796(7) 0.43973(14) 0.0294(3) Uani 1 1 d . . . C2 C 0.55500(16) 0.07137(7) 0.58273(15) 0.0323(3) Uani 1 1 d . . . H2A H 0.5942 0.1200 0.6401 0.039 Uiso 1 1 calc R . . C6 C 0.34120(16) -0.00439(7) 0.35761(15) 0.0335(3) Uani 1 1 d . . . H6A H 0.2329 -0.0080 0.2596 0.040 Uiso 1 1 calc R . . N11 N 0.13881(13) 0.13756(6) 0.21237(12) 0.0327(3) Uani 1 1 d . . . C11 C 0.28365(17) 0.14242(8) 0.38243(15) 0.0353(3) Uani 1 1 d . . . H11A H 0.2353 0.1544 0.4644 0.042 Uiso 1 1 calc R . . H11B H 0.3605 0.1868 0.3850 0.042 Uiso 1 1 calc R . . N21 N -0.03075(16) 0.07585(6) 0.32491(14) 0.0381(3) Uani 1 1 d . . . C22 C -0.02595(16) 0.11234(7) 0.19082(15) 0.0302(3) Uani 1 1 d . . . C23 C -0.17836(17) 0.12654(7) 0.04012(16) 0.0345(3) Uani 1 1 d . . . H23A H -0.1719 0.1526 -0.0529 0.041 Uiso 1 1 calc R . . C24 C -0.33708(18) 0.10156(9) 0.03137(19) 0.0433(3) Uani 1 1 d . . . H24A H -0.4415 0.1102 -0.0687 0.052 Uiso 1 1 calc R . . C25 C -0.3437(2) 0.06382(9) 0.1692(2) 0.0492(4) Uani 1 1 d . . . H25A H -0.4516 0.0463 0.1657 0.059 Uiso 1 1 calc R . . C26 C -0.1889(2) 0.05271(8) 0.3107(2) 0.0454(4) Uani 1 1 d . . . H26A H -0.1933 0.0270 0.4051 0.054 Uiso 1 1 calc R . . N31 N 0.24851(16) 0.23394(7) 0.09458(15) 0.0443(3) Uani 1 1 d . . . C32 C 0.17067(15) 0.16360(7) 0.07473(15) 0.0297(3) Uani 1 1 d . . . C33 C 0.12719(18) 0.11693(8) -0.06837(16) 0.0369(3) Uani 1 1 d . . . H33A H 0.0764 0.0664 -0.0759 0.044 Uiso 1 1 calc R . . C34 C 0.1599(2) 0.14602(9) -0.19968(18) 0.0447(3) Uani 1 1 d . . . H34A H 0.1295 0.1163 -0.3004 0.054 Uiso 1 1 calc R . . C35 C 0.2379(2) 0.21927(10) -0.1815(2) 0.0517(4) Uani 1 1 d . . . H35A H 0.2604 0.2411 -0.2700 0.062 Uiso 1 1 calc R . . C36 C 0.2817(2) 0.25959(10) -0.0331(2) 0.0560(4) Uani 1 1 d . . . H36A H 0.3392 0.3088 -0.0200 0.067 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 C1 0.0308(6) 0.0347(6) 0.0255(6) 0.0010(4) 0.0148(5) -0.0036(5) C2 0.0343(6) 0.0332(6) 0.0289(6) -0.0044(5) 0.0131(5) -0.0063(5) C6 0.0311(6) 0.0392(7) 0.0263(6) -0.0020(5) 0.0088(5) -0.0035(5) N11 0.0318(5) 0.0379(6) 0.0276(5) 0.0032(4) 0.0121(4) -0.0011(4) C11 0.0378(7) 0.0357(7) 0.0285(6) -0.0015(5) 0.0109(5) -0.0010(5) N21 0.0512(7) 0.0336(6) 0.0386(6) 0.0017(4) 0.0280(5) 0.0010(5) C22 0.0360(6) 0.0251(6) 0.0337(6) -0.0019(5) 0.0190(5) 0.0010(5) C23 0.0353(7) 0.0337(6) 0.0359(6) -0.0022(5) 0.0168(5) 0.0003(5) C24 0.0343(7) 0.0458(8) 0.0506(8) -0.0124(6) 0.0192(6) -0.0030(6) C25 0.0491(8) 0.0481(8) 0.0673(10) -0.0171(7) 0.0412(8) -0.0136(6) C26 0.0647(9) 0.0366(7) 0.0541(9) -0.0054(6) 0.0438(8) -0.0065(6) N31 0.0527(7) 0.0338(6) 0.0434(6) 0.0039(5) 0.0180(5) -0.0079(5) C32 0.0276(6) 0.0290(6) 0.0321(6) 0.0062(5) 0.0126(5) 0.0030(4) C33 0.0439(7) 0.0315(6) 0.0373(7) 0.0022(5) 0.0194(6) 0.0001(5) C34 0.0542(8) 0.0472(8) 0.0389(7) 0.0060(6) 0.0259(7) 0.0087(6) C35 0.0574(9) 0.0567(9) 0.0498(9) 0.0195(7) 0.0313(7) 0.0030(7) C36 0.0656(10) 0.0459(8) 0.0559(9) 0.0127(7) 0.0258(8) -0.0158(7) _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 C1 C6 1.3970(17) . ? C1 C2 1.3986(17) . ? C1 C11 1.5245(18) . ? C2 C6 1.3952(18) 3_656 ? C6 C2 1.3952(18) 3_656 ? N11 C22 1.3944(16) . ? N11 C32 1.4157(15) . ? N11 C11 1.4666(15) . ? N21 C22 1.3443(16) . ? N21 C26 1.3510(19) . ? C22 C23 1.4124(18) . ? C23 C24 1.3819(19) . ? C24 C25 1.390(2) . ? C25 C26 1.374(2) . ? N31 C36 1.3386(19) . ? N31 C32 1.3403(17) . ? C32 C33 1.3915(18) . ? C33 C34 1.3859(19) . ? C34 C35 1.386(2) . ? C35 C36 1.371(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.97(11) . . ? C6 C1 C11 123.15(11) . . ? C2 C1 C11 118.87(11) . . ? C6 C2 C1 120.98(11) 3_656 . ? C2 C6 C1 121.05(11) 3_656 . ? C22 N11 C32 122.03(10) . . ? C22 N11 C11 120.32(10) . . ? C32 N11 C11 117.55(10) . . ? N11 C11 C1 114.39(10) . . ? C22 N21 C26 117.27(12) . . ? N21 C22 N11 115.54(11) . . ? N21 C22 C23 122.26(12) . . ? N11 C22 C23 122.17(11) . . ? C24 C23 C22 118.37(12) . . ? C23 C24 C25 119.90(14) . . ? C26 C25 C24 117.69(13) . . ? N21 C26 C25 124.50(13) . . ? C36 N31 C32 116.88(12) . . ? N31 C32 C33 123.30(12) . . ? N31 C32 N11 115.68(11) . . ? C33 C32 N11 121.00(11) . . ? C34 C33 C32 118.28(12) . . ? C33 C34 C35 118.82(14) . . ? C36 C35 C34 118.56(13) . . ? N31 C36 C35 124.08(14) . . ? 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 C6 C1 C2 C6 -0.57(19) . . . 3_656 ? C11 C1 C2 C6 178.50(11) . . . 3_656 ? C2 C1 C6 C2 0.57(19) . . . 3_656 ? C11 C1 C6 C2 -178.45(11) . . . 3_656 ? C22 N11 C11 C1 91.29(14) . . . . ? C32 N11 C11 C1 -92.30(13) . . . . ? C6 C1 C11 N11 -14.17(17) . . . . ? C2 C1 C11 N11 166.81(11) . . . . ? C26 N21 C22 N11 178.01(11) . . . . ? C26 N21 C22 C23 0.04(18) . . . . ? C32 N11 C22 N21 168.16(11) . . . . ? C11 N11 C22 N21 -15.60(16) . . . . ? C32 N11 C22 C23 -13.86(18) . . . . ? C11 N11 C22 C23 162.38(11) . . . . ? N21 C22 C23 C24 -0.24(18) . . . . ? N11 C22 C23 C24 -178.08(11) . . . . ? C22 C23 C24 C25 0.28(19) . . . . ? C23 C24 C25 C26 -0.1(2) . . . . ? C22 N21 C26 C25 0.1(2) . . . . ? C24 C25 C26 N21 -0.1(2) . . . . ? C36 N31 C32 C33 1.2(2) . . . . ? C36 N31 C32 N11 179.36(13) . . . . ? C22 N11 C32 N31 128.03(12) . . . . ? C11 N11 C32 N31 -48.31(15) . . . . ? C22 N11 C32 C33 -53.75(17) . . . . ? C11 N11 C32 C33 129.92(13) . . . . ? N31 C32 C33 C34 -2.6(2) . . . . ? N11 C32 C33 C34 179.33(12) . . . . ? C32 C33 C34 C35 1.4(2) . . . . ? C33 C34 C35 C36 0.9(2) . . . . ? C32 N31 C36 C35 1.4(2) . . . . ? C34 C35 C36 N31 -2.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.147 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.034 #END data_3csbp _database_code_depnum_ccdc_archive 'CCDC 614169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag N7 O3' _chemical_formula_weight 614.41 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8253(18) _cell_length_b 10.437(2) _cell_length_c 14.732(3) _cell_angle_alpha 85.759(2) _cell_angle_beta 84.787(2) _cell_angle_gamma 70.861(2) _cell_volume 1275.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6981 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.636725 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 16279 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5067 _reflns_number_gt 4815 _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^)+(0.0398P)^2^+0.6586P] 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 5067 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.049548(15) 0.320594(12) 0.230839(9) 0.02608(6) Uani 1 1 d . . . C1 C 0.3834(2) -0.11145(17) 0.26616(11) 0.0221(3) Uani 1 1 d . . . C2 C 0.2166(2) -0.05138(17) 0.26445(11) 0.0232(3) Uani 1 1 d . . . H2A H 0.1717 0.0448 0.2598 0.028 Uiso 1 1 calc R . . C3 C 0.1155(2) -0.13013(18) 0.26950(11) 0.0229(3) Uani 1 1 d . . . C4 C 0.1827(2) -0.27162(18) 0.27581(12) 0.0280(4) Uani 1 1 d . . . H4A H 0.1151 -0.3266 0.2790 0.034 Uiso 1 1 calc R . . C5 C 0.3480(2) -0.33176(18) 0.27744(13) 0.0319(4) Uani 1 1 d . . . H5A H 0.3928 -0.4279 0.2818 0.038 Uiso 1 1 calc R . . C6 C 0.4495(2) -0.25266(18) 0.27274(12) 0.0271(4) Uani 1 1 d . . . H6A H 0.5624 -0.2947 0.2740 0.033 Uiso 1 1 calc R . . N11 N 0.41954(17) 0.11941(14) 0.25877(10) 0.0235(3) Uani 1 1 d . . . C11 C 0.4977(2) -0.02865(17) 0.25901(13) 0.0269(4) Uani 1 1 d . . . H11A H 0.5672 -0.0567 0.3109 0.032 Uiso 1 1 calc R . . H11B H 0.5681 -0.0510 0.2022 0.032 Uiso 1 1 calc R . . N13 N -0.12693(17) 0.07909(15) 0.24977(10) 0.0238(3) Uani 1 1 d . . . C13 C -0.0669(2) -0.06789(18) 0.26956(13) 0.0289(4) Uani 1 1 d . . . H13A H -0.1050 -0.1129 0.2238 0.035 Uiso 1 1 calc R . . H13B H -0.1148 -0.0879 0.3301 0.035 Uiso 1 1 calc R . . N21 N 0.21398(18) 0.27739(16) 0.34549(10) 0.0263(3) Uani 1 1 d . . . C22 C 0.3619(2) 0.18239(17) 0.34188(12) 0.0234(3) Uani 1 1 d . . . C23 C 0.4540(2) 0.1483(2) 0.41864(13) 0.0316(4) Uani 1 1 d . . . H23A H 0.5576 0.0816 0.4153 0.038 Uiso 1 1 calc R . . C24 C 0.3920(3) 0.2129(2) 0.49899(14) 0.0397(5) Uani 1 1 d . . . H24A H 0.4529 0.1906 0.5512 0.048 Uiso 1 1 calc R . . C25 C 0.2399(3) 0.3110(2) 0.50316(14) 0.0419(5) Uani 1 1 d . . . H25A H 0.1949 0.3560 0.5578 0.050 Uiso 1 1 calc R . . C26 C 0.1566(3) 0.3405(2) 0.42466(14) 0.0365(4) Uani 1 1 d . . . H26A H 0.0539 0.4086 0.4265 0.044 Uiso 1 1 calc R . . N31 N 0.3994(2) 0.12407(17) 0.09996(11) 0.0321(3) Uani 1 1 d . . . C32 C 0.39950(19) 0.19358(17) 0.17372(11) 0.0224(3) Uani 1 1 d . . . C33 C 0.3893(2) 0.32986(18) 0.16830(13) 0.0281(4) Uani 1 1 d . . . H33A H 0.3917 0.3757 0.2212 0.034 Uiso 1 1 calc R . . C34 C 0.3754(3) 0.3966(2) 0.08246(15) 0.0389(5) Uani 1 1 d . . . H34A H 0.3666 0.4900 0.0765 0.047 Uiso 1 1 calc R . . C35 C 0.3744(3) 0.3280(3) 0.00588(14) 0.0432(5) Uani 1 1 d . . . H35A H 0.3644 0.3728 -0.0529 0.052 Uiso 1 1 calc R . . C36 C 0.3882(3) 0.1926(2) 0.01747(13) 0.0388(5) Uani 1 1 d . . . H36A H 0.3900 0.1445 -0.0351 0.047 Uiso 1 1 calc R . . N41 N -0.06922(17) 0.23085(15) 0.13412(10) 0.0244(3) Uani 1 1 d . . . C42 C -0.12939(19) 0.12859(18) 0.15683(12) 0.0231(3) Uani 1 1 d . . . C43 C -0.1900(2) 0.0710(2) 0.09170(13) 0.0299(4) Uani 1 1 d . . . H43A H -0.2300 -0.0021 0.1089 0.036 Uiso 1 1 calc R . . C44 C -0.1912(2) 0.1216(2) 0.00157(13) 0.0342(4) Uani 1 1 d . . . H44A H -0.2320 0.0834 -0.0434 0.041 Uiso 1 1 calc R . . C45 C -0.1321(2) 0.2284(2) -0.02181(12) 0.0328(4) Uani 1 1 d . . . H45A H -0.1326 0.2654 -0.0827 0.039 Uiso 1 1 calc R . . C46 C -0.0725(2) 0.2796(2) 0.04572(12) 0.0295(4) Uani 1 1 d . . . H46A H -0.0316 0.3525 0.0296 0.035 Uiso 1 1 calc R . . N51 N -0.1167(2) 0.10643(18) 0.40424(11) 0.0327(4) Uani 1 1 d . . . C52 C -0.1678(2) 0.16569(18) 0.32307(12) 0.0242(3) Uani 1 1 d . . . C53 C -0.2630(2) 0.30290(19) 0.31324(12) 0.0272(4) Uani 1 1 d . . . H53A H -0.2993 0.3419 0.2556 0.033 Uiso 1 1 calc R . . C54 C -0.3023(2) 0.3796(2) 0.39010(13) 0.0334(4) Uani 1 1 d . . . H54A H -0.3655 0.4727 0.3854 0.040 Uiso 1 1 calc R . . C55 C -0.2488(3) 0.3197(2) 0.47470(14) 0.0395(5) Uani 1 1 d . . . H55A H -0.2739 0.3708 0.5280 0.047 Uiso 1 1 calc R . . C56 C -0.1583(3) 0.1834(2) 0.47789(13) 0.0399(5) Uani 1 1 d . . . H56A H -0.1234 0.1417 0.5352 0.048 Uiso 1 1 calc R . . N60 N -0.11252(18) 0.61357(15) 0.19107(10) 0.0259(3) Uani 1 1 d . . . O61 O -0.0151(2) 0.53541(14) 0.13540(10) 0.0416(4) Uani 1 1 d . . . O62 O -0.12825(19) 0.57092(16) 0.27259(10) 0.0415(3) Uani 1 1 d . . . O63 O -0.19038(18) 0.73126(13) 0.16535(11) 0.0383(3) 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 0.02489(8) 0.02486(8) 0.02914(9) 0.00156(5) -0.00777(5) -0.00797(6) C1 0.0235(8) 0.0237(8) 0.0185(7) 0.0002(6) -0.0002(6) -0.0074(7) C2 0.0248(8) 0.0218(8) 0.0222(8) 0.0019(6) -0.0022(6) -0.0069(7) C3 0.0262(8) 0.0265(8) 0.0178(7) 0.0020(6) -0.0045(6) -0.0106(7) C4 0.0362(10) 0.0259(9) 0.0266(9) 0.0015(7) -0.0102(7) -0.0149(8) C5 0.0392(10) 0.0200(8) 0.0359(10) -0.0016(7) -0.0096(8) -0.0069(8) C6 0.0253(9) 0.0243(9) 0.0285(9) -0.0016(7) -0.0033(7) -0.0032(7) N11 0.0223(7) 0.0222(7) 0.0257(7) 0.0028(6) -0.0014(5) -0.0075(6) C11 0.0200(8) 0.0234(8) 0.0344(9) 0.0038(7) -0.0002(7) -0.0044(7) N13 0.0218(7) 0.0261(7) 0.0239(7) 0.0040(6) -0.0039(5) -0.0090(6) C13 0.0272(9) 0.0260(9) 0.0372(10) 0.0059(7) -0.0071(7) -0.0138(7) N21 0.0258(7) 0.0293(8) 0.0256(7) -0.0032(6) -0.0027(6) -0.0107(6) C22 0.0234(8) 0.0264(8) 0.0239(8) 0.0037(6) -0.0025(6) -0.0135(7) C23 0.0323(10) 0.0360(10) 0.0297(9) 0.0090(8) -0.0093(8) -0.0161(8) C24 0.0572(13) 0.0479(12) 0.0245(9) 0.0072(8) -0.0141(9) -0.0303(11) C25 0.0597(14) 0.0465(12) 0.0254(9) -0.0077(8) 0.0008(9) -0.0252(11) C26 0.0369(11) 0.0398(11) 0.0334(10) -0.0098(8) 0.0016(8) -0.0126(9) N31 0.0329(8) 0.0378(9) 0.0288(8) -0.0057(7) -0.0007(6) -0.0153(7) C32 0.0173(7) 0.0264(8) 0.0241(8) 0.0012(6) -0.0012(6) -0.0083(6) C33 0.0315(9) 0.0255(9) 0.0285(9) -0.0002(7) 0.0003(7) -0.0118(7) C34 0.0393(11) 0.0287(10) 0.0467(12) 0.0087(9) 0.0006(9) -0.0113(8) C35 0.0415(12) 0.0554(14) 0.0282(10) 0.0142(9) -0.0062(8) -0.0121(10) C36 0.0416(11) 0.0537(13) 0.0243(9) -0.0056(9) -0.0033(8) -0.0189(10) N41 0.0241(7) 0.0269(7) 0.0230(7) 0.0018(6) -0.0031(5) -0.0096(6) C42 0.0173(7) 0.0286(8) 0.0227(8) 0.0004(6) -0.0016(6) -0.0067(6) C43 0.0249(9) 0.0386(10) 0.0311(9) -0.0052(8) -0.0005(7) -0.0165(8) C44 0.0309(10) 0.0469(11) 0.0270(9) -0.0099(8) -0.0017(7) -0.0139(8) C45 0.0347(10) 0.0409(11) 0.0203(8) -0.0003(7) -0.0018(7) -0.0092(8) C46 0.0318(9) 0.0322(9) 0.0244(9) 0.0035(7) -0.0019(7) -0.0113(8) N51 0.0311(8) 0.0403(9) 0.0254(8) 0.0096(7) -0.0048(6) -0.0112(7) C52 0.0189(8) 0.0327(9) 0.0225(8) 0.0059(7) -0.0020(6) -0.0117(7) C53 0.0244(8) 0.0338(9) 0.0225(8) 0.0055(7) -0.0022(7) -0.0096(7) C54 0.0326(10) 0.0346(10) 0.0315(10) -0.0011(8) 0.0029(8) -0.0102(8) C55 0.0468(12) 0.0500(12) 0.0232(9) -0.0040(8) 0.0030(8) -0.0189(10) C56 0.0453(12) 0.0541(13) 0.0211(9) 0.0077(8) -0.0045(8) -0.0188(10) N60 0.0249(7) 0.0242(7) 0.0316(8) -0.0019(6) -0.0045(6) -0.0114(6) O61 0.0549(9) 0.0273(7) 0.0345(8) -0.0026(6) 0.0071(7) -0.0047(6) O62 0.0469(9) 0.0438(8) 0.0315(7) 0.0027(6) 0.0049(6) -0.0144(7) O63 0.0380(8) 0.0211(6) 0.0550(9) 0.0003(6) -0.0117(7) -0.0067(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 N21 2.2507(15) . ? Ag1 N41 2.2625(15) . ? Ag1 O61 2.4839(15) . ? C1 C6 1.395(2) . ? C1 C2 1.400(2) . ? C1 C11 1.521(2) . ? C2 C3 1.392(2) . ? C3 C4 1.399(3) . ? C3 C13 1.525(2) . ? C4 C5 1.388(3) . ? C5 C6 1.397(3) . ? N11 C22 1.406(2) . ? N11 C32 1.417(2) . ? N11 C11 1.471(2) . ? N13 C52 1.405(2) . ? N13 C42 1.427(2) . ? N13 C13 1.466(2) . ? N21 C22 1.355(2) . ? N21 C26 1.356(2) . ? C22 C23 1.409(2) . ? C23 C24 1.384(3) . ? C24 C25 1.395(3) . ? C25 C26 1.388(3) . ? N31 C32 1.351(2) . ? N31 C36 1.358(3) . ? C32 C33 1.392(2) . ? C33 C34 1.393(3) . ? C34 C35 1.383(3) . ? C35 C36 1.377(3) . ? N41 C42 1.349(2) . ? N41 C46 1.362(2) . ? C42 C43 1.399(3) . ? C43 C44 1.392(3) . ? C44 C45 1.388(3) . ? C45 C46 1.382(3) . ? N51 C56 1.349(3) . ? N51 C52 1.350(2) . ? C52 C53 1.407(3) . ? C53 C54 1.387(3) . ? C54 C55 1.402(3) . ? C55 C56 1.384(3) . ? N60 O63 1.245(2) . ? N60 O61 1.260(2) . ? N60 O62 1.261(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Ag1 N41 145.85(5) . . ? N21 Ag1 O61 122.55(6) . . ? N41 Ag1 O61 90.26(6) . . ? C6 C1 C2 119.47(16) . . ? C6 C1 C11 118.00(15) . . ? C2 C1 C11 122.52(15) . . ? C3 C2 C1 121.10(16) . . ? C2 C3 C4 119.10(16) . . ? C2 C3 C13 122.43(16) . . ? C4 C3 C13 118.47(15) . . ? C5 C4 C3 120.05(17) . . ? C4 C5 C6 120.85(16) . . ? C1 C6 C5 119.44(16) . . ? C22 N11 C32 121.98(14) . . ? C22 N11 C11 119.52(14) . . ? C32 N11 C11 118.46(14) . . ? N11 C11 C1 115.10(14) . . ? C52 N13 C42 122.57(14) . . ? C52 N13 C13 118.59(14) . . ? C42 N13 C13 118.65(15) . . ? N13 C13 C3 115.30(14) . . ? C22 N21 C26 118.53(16) . . ? C22 N21 Ag1 122.94(12) . . ? C26 N21 Ag1 118.26(13) . . ? N21 C22 N11 117.47(15) . . ? N21 C22 C23 121.11(17) . . ? N11 C22 C23 121.42(16) . . ? C24 C23 C22 119.29(19) . . ? C23 C24 C25 119.92(18) . . ? C26 C25 C24 117.69(19) . . ? N21 C26 C25 123.5(2) . . ? C32 N31 C36 117.33(17) . . ? N31 C32 C33 123.03(16) . . ? N31 C32 N11 116.85(15) . . ? C33 C32 N11 120.03(16) . . ? C32 C33 C34 117.64(18) . . ? C35 C34 C33 120.47(19) . . ? C36 C35 C34 117.89(19) . . ? N31 C36 C35 123.61(19) . . ? C42 N41 C46 118.07(15) . . ? C42 N41 Ag1 124.66(11) . . ? C46 N41 Ag1 117.19(12) . . ? N41 C42 C43 121.53(16) . . ? N41 C42 N13 117.69(15) . . ? C43 C42 N13 120.77(16) . . ? C44 C43 C42 119.52(18) . . ? C45 C44 C43 119.15(17) . . ? C46 C45 C44 118.33(17) . . ? N41 C46 C45 123.37(18) . . ? C56 N51 C52 117.97(17) . . ? N51 C52 N13 115.36(16) . . ? N51 C52 C53 122.47(17) . . ? N13 C52 C53 122.08(15) . . ? C54 C53 C52 118.11(17) . . ? C53 C54 C55 120.03(19) . . ? C56 C55 C54 117.65(19) . . ? N51 C56 C55 123.75(18) . . ? O63 N60 O61 119.90(16) . . ? O63 N60 O62 121.09(16) . . ? O61 N60 O62 119.01(15) . . ? N60 O61 Ag1 99.19(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 C6 C1 C2 C3 0.2(3) . . . . ? C11 C1 C2 C3 178.84(15) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C1 C2 C3 C13 178.86(16) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C13 C3 C4 C5 -178.96(17) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C2 C1 C6 C5 0.1(3) . . . . ? C11 C1 C6 C5 -178.64(16) . . . . ? C4 C5 C6 C1 -0.1(3) . . . . ? C22 N11 C11 C1 81.2(2) . . . . ? C32 N11 C11 C1 -96.47(18) . . . . ? C6 C1 C11 N11 -175.90(15) . . . . ? C2 C1 C11 N11 5.4(2) . . . . ? C52 N13 C13 C3 -92.39(19) . . . . ? C42 N13 C13 C3 82.69(19) . . . . ? C2 C3 C13 N13 9.1(2) . . . . ? C4 C3 C13 N13 -171.67(16) . . . . ? N41 Ag1 N21 C22 51.47(18) . . . . ? O61 Ag1 N21 C22 -110.47(13) . . . . ? N41 Ag1 N21 C26 -122.38(15) . . . . ? O61 Ag1 N21 C26 75.68(15) . . . . ? C26 N21 C22 N11 -179.32(16) . . . . ? Ag1 N21 C22 N11 6.8(2) . . . . ? C26 N21 C22 C23 0.7(3) . . . . ? Ag1 N21 C22 C23 -173.13(13) . . . . ? C32 N11 C22 N21 42.2(2) . . . . ? C11 N11 C22 N21 -135.43(16) . . . . ? C32 N11 C22 C23 -137.86(17) . . . . ? C11 N11 C22 C23 44.5(2) . . . . ? N21 C22 C23 C24 0.1(3) . . . . ? N11 C22 C23 C24 -179.90(17) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C22 N21 C26 C25 -1.5(3) . . . . ? Ag1 N21 C26 C25 172.67(16) . . . . ? C24 C25 C26 N21 1.4(3) . . . . ? C36 N31 C32 C33 -0.2(3) . . . . ? C36 N31 C32 N11 -176.85(16) . . . . ? C22 N11 C32 N31 -154.79(16) . . . . ? C11 N11 C32 N31 22.8(2) . . . . ? C22 N11 C32 C33 28.5(2) . . . . ? C11 N11 C32 C33 -153.92(16) . . . . ? N31 C32 C33 C34 1.2(3) . . . . ? N11 C32 C33 C34 177.74(16) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C32 N31 C36 C35 -1.1(3) . . . . ? C34 C35 C36 N31 1.4(3) . . . . ? N21 Ag1 N41 C42 38.73(18) . . . . ? O61 Ag1 N41 C42 -156.41(14) . . . . ? N21 Ag1 N41 C46 -137.83(13) . . . . ? O61 Ag1 N41 C46 27.02(13) . . . . ? C46 N41 C42 C43 1.6(3) . . . . ? Ag1 N41 C42 C43 -174.95(13) . . . . ? C46 N41 C42 N13 -179.41(15) . . . . ? Ag1 N41 C42 N13 4.1(2) . . . . ? C52 N13 C42 N41 42.5(2) . . . . ? C13 N13 C42 N41 -132.39(16) . . . . ? C52 N13 C42 C43 -138.50(17) . . . . ? C13 N13 C42 C43 46.6(2) . . . . ? N41 C42 C43 C44 -1.2(3) . . . . ? N13 C42 C43 C44 179.87(16) . . . . ? C42 C43 C44 C45 0.0(3) . . . . ? C43 C44 C45 C46 0.7(3) . . . . ? C42 N41 C46 C45 -0.9(3) . . . . ? Ag1 N41 C46 C45 175.90(15) . . . . ? C44 C45 C46 N41 -0.2(3) . . . . ? C56 N51 C52 N13 -177.24(16) . . . . ? C56 N51 C52 C53 -0.6(3) . . . . ? C42 N13 C52 N51 -161.65(15) . . . . ? C13 N13 C52 N51 13.2(2) . . . . ? C42 N13 C52 C53 21.7(2) . . . . ? C13 N13 C52 C53 -163.45(16) . . . . ? N51 C52 C53 C54 1.2(3) . . . . ? N13 C52 C53 C54 177.66(16) . . . . ? C52 C53 C54 C55 -0.6(3) . . . . ? C53 C54 C55 C56 -0.5(3) . . . . ? C52 N51 C56 C55 -0.7(3) . . . . ? C54 C55 C56 N51 1.2(3) . . . . ? O63 N60 O61 Ag1 -171.15(13) . . . . ? O62 N60 O61 Ag1 9.46(18) . . . . ? N21 Ag1 O61 N60 -75.80(13) . . . . ? N41 Ag1 O61 N60 114.22(12) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.284 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.068 #END data_3csbq _database_code_depnum_ccdc_archive 'CCDC 614170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag B F4 N6' _chemical_formula_weight 639.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.618(4) _cell_length_b 12.798(4) _cell_length_c 17.110(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.394(4) _cell_angle_gamma 90.00 _cell_volume 2650.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 7248 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.799825 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 32363 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.35 _reflns_number_total 5348 _reflns_number_gt 4246 _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^)+(0.0332P)^2^+1.5060P] 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 5348 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.158939(15) 0.269702(15) 0.385990(11) 0.03002(7) Uani 1 1 d . . . C1 C 0.69788(18) 0.10967(18) 0.44089(13) 0.0256(5) Uani 1 1 d . . . C2 C 0.61204(18) 0.18223(18) 0.41393(13) 0.0244(5) Uani 1 1 d . . . C3 C 0.6371(2) 0.28394(19) 0.39598(14) 0.0295(5) Uani 1 1 d . . . H3A H 0.5793 0.3337 0.3790 0.035 Uiso 1 1 calc R . . C4 C 0.7453(2) 0.3137(2) 0.40256(15) 0.0335(6) Uani 1 1 d . . . H4A H 0.7613 0.3831 0.3896 0.040 Uiso 1 1 calc R . . C5 C 0.8292(2) 0.2418(2) 0.42795(16) 0.0362(6) Uani 1 1 d . . . H5A H 0.9032 0.2612 0.4321 0.043 Uiso 1 1 calc R . . C6 C 0.8056(2) 0.1414(2) 0.44742(15) 0.0340(6) Uani 1 1 d . . . H6A H 0.8643 0.0927 0.4657 0.041 Uiso 1 1 calc R . . C11 C 0.67164(19) -0.00097(19) 0.46173(15) 0.0310(5) Uani 1 1 d . . . H11A H 0.6245 0.0024 0.4991 0.037 Uiso 1 1 calc R . . H11B H 0.6287 -0.0362 0.4112 0.037 Uiso 1 1 calc R . . N11 N 0.76960(16) -0.06427(15) 0.49983(12) 0.0292(4) Uani 1 1 d . . . N12 N 0.41245(15) 0.23196(16) 0.38386(11) 0.0280(4) Uani 1 1 d . . . C12 C 0.49442(18) 0.14785(18) 0.40566(15) 0.0293(5) Uani 1 1 d . . . H12A H 0.4742 0.0926 0.3635 0.035 Uiso 1 1 calc R . . H12B H 0.4913 0.1167 0.4579 0.035 Uiso 1 1 calc R . . N21 N 0.85406(16) -0.22617(16) 0.49129(12) 0.0297(4) Uani 1 1 d . . . C22 C 0.80582(19) -0.13884(19) 0.45349(14) 0.0296(5) Uani 1 1 d . . . C23 C 0.7878(2) -0.1244(2) 0.36957(16) 0.0442(7) Uani 1 1 d . . . H23A H 0.7546 -0.0620 0.3439 0.053 Uiso 1 1 calc R . . C24 C 0.8188(3) -0.2017(3) 0.32520(18) 0.0560(9) Uani 1 1 d . . . H24A H 0.8059 -0.1935 0.2681 0.067 Uiso 1 1 calc R . . C25 C 0.8687(3) -0.2916(3) 0.36292(18) 0.0518(8) Uani 1 1 d . . . H25A H 0.8904 -0.3457 0.3327 0.062 Uiso 1 1 calc R . . C26 C 0.8858(2) -0.3002(2) 0.44601(17) 0.0399(6) Uani 1 1 d . . . H26A H 0.9217 -0.3610 0.4727 0.048 Uiso 1 1 calc R . . N31 N 0.75366(17) -0.02305(15) 0.62897(12) 0.0304(5) Uani 1 1 d . . . C32 C 0.82008(19) -0.04973(17) 0.58357(14) 0.0268(5) Uani 1 1 d . . . C33 C 0.9342(2) -0.0606(2) 0.61622(16) 0.0361(6) Uani 1 1 d . . . H33A H 0.9796 -0.0776 0.5822 0.043 Uiso 1 1 calc R . . C34 C 0.9794(2) -0.0461(2) 0.69869(17) 0.0435(7) Uani 1 1 d . . . H34A H 1.0568 -0.0534 0.7224 0.052 Uiso 1 1 calc R . . C35 C 0.9110(2) -0.0205(2) 0.74715(17) 0.0427(7) Uani 1 1 d . . . H35A H 0.9401 -0.0112 0.8043 0.051 Uiso 1 1 calc R . . C36 C 0.8002(2) -0.00919(19) 0.70950(15) 0.0358(6) Uani 1 1 d . . . H36A H 0.7534 0.0095 0.7421 0.043 Uiso 1 1 calc R . . N41 N 0.24266(16) 0.26784(15) 0.28714(11) 0.0263(4) Uani 1 1 d . . . C42 C 0.34872(19) 0.23971(17) 0.30237(14) 0.0265(5) Uani 1 1 d . . . C43 C 0.3950(2) 0.2153(2) 0.23940(16) 0.0377(6) Uani 1 1 d . . . H43A H 0.4707 0.1960 0.2513 0.045 Uiso 1 1 calc R . . C44 C 0.3299(2) 0.2193(2) 0.15987(16) 0.0458(7) Uani 1 1 d . . . H44A H 0.3597 0.2011 0.1166 0.055 Uiso 1 1 calc R . . C45 C 0.2206(2) 0.2501(2) 0.14357(16) 0.0410(7) Uani 1 1 d . . . H45A H 0.1744 0.2547 0.0892 0.049 Uiso 1 1 calc R . . C46 C 0.1811(2) 0.2737(2) 0.20825(14) 0.0326(5) Uani 1 1 d . . . H46A H 0.1063 0.2955 0.1972 0.039 Uiso 1 1 calc R . . N51 N 0.42724(17) 0.25688(16) 0.52238(12) 0.0334(5) Uani 1 1 d . . . C52 C 0.39631(18) 0.29628(18) 0.44646(14) 0.0267(5) Uani 1 1 d . . . C53 C 0.3523(2) 0.39673(19) 0.43013(15) 0.0331(6) Uani 1 1 d . . . H53A H 0.3337 0.4240 0.3763 0.040 Uiso 1 1 calc R . . C54 C 0.3363(2) 0.4556(2) 0.49315(16) 0.0412(7) Uani 1 1 d . . . H54A H 0.3059 0.5238 0.4831 0.049 Uiso 1 1 calc R . . C55 C 0.3648(2) 0.4149(2) 0.57149(16) 0.0417(7) Uani 1 1 d . . . H55A H 0.3534 0.4537 0.6158 0.050 Uiso 1 1 calc R . . C56 C 0.4100(2) 0.3164(2) 0.58279(15) 0.0375(6) Uani 1 1 d . . . H56A H 0.4304 0.2885 0.6364 0.045 Uiso 1 1 calc R . . B1 B -0.0257(3) 0.4327(3) 0.2999(2) 0.0470(8) Uani 1 1 d . . . F1 F -0.03563(15) 0.32667(13) 0.28326(12) 0.0604(5) Uani 1 1 d . A . F2 F -0.1330(2) 0.4689(2) 0.2966(2) 0.0684(13) Uani 0.676(6) 1 d P A 1 F3 F 0.0047(4) 0.4738(3) 0.2382(2) 0.0929(17) Uani 0.676(6) 1 d P A 1 F4 F 0.0431(4) 0.4477(3) 0.3724(3) 0.0873(17) Uani 0.676(6) 1 d P A 1 F2' F -0.0763(7) 0.5077(4) 0.2492(4) 0.063(3) Uani 0.324(6) 1 d P A 2 F3' F 0.0949(6) 0.4648(5) 0.3158(8) 0.112(5) Uani 0.324(6) 1 d P A 2 F4' F -0.0346(12) 0.4548(7) 0.3780(5) 0.113(5) Uani 0.324(6) 1 d P 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 0.02886(10) 0.03355(10) 0.02730(10) 0.00638(8) 0.00735(7) 0.00610(8) C1 0.0244(12) 0.0324(13) 0.0196(11) 0.0022(9) 0.0056(10) 0.0017(10) C2 0.0234(12) 0.0322(13) 0.0167(11) -0.0016(9) 0.0042(9) 0.0016(10) C3 0.0302(13) 0.0293(14) 0.0285(13) 0.0012(10) 0.0076(10) 0.0046(10) C4 0.0372(14) 0.0325(13) 0.0315(13) -0.0003(11) 0.0109(11) -0.0034(11) C5 0.0240(13) 0.0476(17) 0.0380(14) 0.0009(12) 0.0103(11) -0.0047(11) C6 0.0248(13) 0.0412(15) 0.0361(14) 0.0063(11) 0.0090(11) 0.0069(11) C11 0.0243(12) 0.0365(14) 0.0298(13) 0.0094(11) 0.0036(10) 0.0079(10) N11 0.0285(11) 0.0321(11) 0.0260(11) 0.0052(8) 0.0060(9) 0.0075(9) N12 0.0236(10) 0.0336(10) 0.0247(10) -0.0007(8) 0.0035(8) 0.0053(9) C12 0.0240(12) 0.0291(13) 0.0332(13) 0.0029(10) 0.0057(10) 0.0046(10) N21 0.0262(10) 0.0348(11) 0.0285(10) -0.0006(9) 0.0085(8) 0.0054(9) C22 0.0250(12) 0.0384(14) 0.0255(12) 0.0019(10) 0.0077(10) 0.0002(10) C23 0.0503(18) 0.0537(18) 0.0286(14) 0.0060(12) 0.0111(13) 0.0001(14) C24 0.068(2) 0.076(2) 0.0290(15) -0.0061(15) 0.0216(15) -0.0069(18) C25 0.0568(19) 0.062(2) 0.0453(17) -0.0184(15) 0.0286(15) -0.0034(15) C26 0.0340(14) 0.0425(16) 0.0470(16) -0.0078(12) 0.0180(13) 0.0023(12) N31 0.0325(11) 0.0274(11) 0.0323(12) -0.0011(9) 0.0106(9) 0.0052(9) C32 0.0310(13) 0.0209(12) 0.0284(12) 0.0030(9) 0.0083(10) 0.0037(9) C33 0.0292(14) 0.0427(15) 0.0366(15) -0.0016(12) 0.0095(12) 0.0019(11) C34 0.0324(15) 0.0510(18) 0.0413(16) -0.0034(13) 0.0010(13) 0.0035(13) C35 0.0504(18) 0.0412(16) 0.0304(14) -0.0055(12) 0.0018(13) 0.0069(13) C36 0.0449(16) 0.0306(14) 0.0336(14) -0.0042(11) 0.0140(12) 0.0053(11) N41 0.0253(10) 0.0264(9) 0.0251(10) 0.0027(8) 0.0034(8) 0.0010(8) C42 0.0267(12) 0.0250(12) 0.0265(12) -0.0007(9) 0.0055(10) -0.0008(9) C43 0.0331(14) 0.0482(17) 0.0331(14) -0.0061(12) 0.0114(11) 0.0026(12) C44 0.0506(17) 0.0597(19) 0.0297(14) -0.0080(13) 0.0155(13) -0.0008(15) C45 0.0480(17) 0.0470(18) 0.0228(13) 0.0016(11) 0.0017(12) -0.0050(12) C46 0.0313(13) 0.0341(13) 0.0276(12) 0.0058(11) 0.0005(10) -0.0021(11) N51 0.0278(11) 0.0426(13) 0.0253(11) 0.0013(9) 0.0004(8) 0.0066(9) C52 0.0197(11) 0.0334(14) 0.0242(12) -0.0014(9) 0.0015(9) -0.0005(9) C53 0.0377(14) 0.0293(13) 0.0281(13) 0.0041(10) 0.0026(11) -0.0017(11) C54 0.0485(17) 0.0318(14) 0.0373(16) -0.0050(12) 0.0024(13) 0.0033(12) C55 0.0402(16) 0.0477(17) 0.0318(15) -0.0142(12) 0.0016(12) 0.0052(13) C56 0.0331(14) 0.0530(16) 0.0203(12) -0.0031(11) -0.0023(10) 0.0046(12) B1 0.049(2) 0.043(2) 0.048(2) 0.0163(15) 0.0117(17) 0.0130(16) F1 0.0558(11) 0.0468(11) 0.0776(13) 0.0035(9) 0.0173(10) 0.0132(8) F2 0.0483(18) 0.0514(19) 0.095(3) -0.0096(17) 0.0037(17) 0.0178(13) F3 0.128(4) 0.075(3) 0.088(3) 0.035(2) 0.049(3) -0.014(3) F4 0.077(3) 0.107(3) 0.055(3) -0.017(2) -0.020(2) 0.038(3) F2' 0.086(6) 0.036(3) 0.042(4) 0.000(2) -0.024(4) 0.024(3) F3' 0.042(4) 0.038(4) 0.254(14) -0.001(5) 0.037(6) 0.001(3) F4' 0.217(15) 0.083(6) 0.070(6) 0.006(4) 0.087(9) -0.022(7) _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 N21 2.223(2) 3_656 ? Ag1 N41 2.233(2) . ? C1 C6 1.392(3) . ? C1 C2 1.402(3) . ? C1 C11 1.519(3) . ? C2 C3 1.394(3) . ? C2 C12 1.516(3) . ? C3 C4 1.392(3) . ? C4 C5 1.377(4) . ? C5 C6 1.381(4) . ? C11 N11 1.468(3) . ? N11 C22 1.397(3) . ? N11 C32 1.406(3) . ? N12 C42 1.403(3) . ? N12 C52 1.411(3) . ? N12 C12 1.466(3) . ? N21 C22 1.347(3) . ? N21 C26 1.354(3) . ? N21 Ag1 2.223(2) 3_656 ? C22 C23 1.401(3) . ? C23 C24 1.370(4) . ? C24 C25 1.380(5) . ? C25 C26 1.381(4) . ? N31 C32 1.338(3) . ? N31 C36 1.348(3) . ? C32 C33 1.396(3) . ? C33 C34 1.377(4) . ? C34 C35 1.394(4) . ? C35 C36 1.372(4) . ? N41 C42 1.338(3) . ? N41 C46 1.356(3) . ? C42 C43 1.399(3) . ? C43 C44 1.378(4) . ? C44 C45 1.385(4) . ? C45 C46 1.370(4) . ? N51 C52 1.345(3) . ? N51 C56 1.350(3) . ? C52 C53 1.397(3) . ? C53 C54 1.376(4) . ? C54 C55 1.387(4) . ? C55 C56 1.374(4) . ? B1 F4 1.311(5) . ? B1 F2' 1.330(6) . ? B1 F3 1.330(4) . ? B1 F1 1.386(4) . ? B1 F4' 1.400(8) . ? B1 F2 1.416(4) . ? B1 F3' 1.525(7) . ? 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 N21 Ag1 N41 152.84(7) 3_656 . ? C6 C1 C2 118.6(2) . . ? C6 C1 C11 121.7(2) . . ? C2 C1 C11 119.7(2) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 C12 121.8(2) . . ? C1 C2 C12 118.9(2) . . ? C4 C3 C2 121.1(2) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 120.0(2) . . ? C5 C6 C1 121.6(2) . . ? N11 C11 C1 114.0(2) . . ? C22 N11 C32 122.80(19) . . ? C22 N11 C11 119.6(2) . . ? C32 N11 C11 117.51(19) . . ? C42 N12 C52 123.26(19) . . ? C42 N12 C12 118.05(19) . . ? C52 N12 C12 118.54(19) . . ? N12 C12 C2 114.35(19) . . ? C22 N21 C26 118.2(2) . . ? C22 N21 Ag1 121.17(15) . 3_656 ? C26 N21 Ag1 118.54(18) . 3_656 ? N21 C22 N11 118.0(2) . . ? N21 C22 C23 121.5(2) . . ? N11 C22 C23 120.5(2) . . ? C24 C23 C22 118.9(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C26 117.8(3) . . ? N21 C26 C25 123.2(3) . . ? C32 N31 C36 117.6(2) . . ? N31 C32 C33 122.5(2) . . ? N31 C32 N11 116.6(2) . . ? C33 C32 N11 120.9(2) . . ? C34 C33 C32 118.6(2) . . ? C33 C34 C35 119.6(3) . . ? C36 C35 C34 117.8(2) . . ? N31 C36 C35 123.9(2) . . ? C42 N41 C46 118.0(2) . . ? C42 N41 Ag1 121.07(15) . . ? C46 N41 Ag1 119.52(16) . . ? N41 C42 C43 121.5(2) . . ? N41 C42 N12 118.3(2) . . ? C43 C42 N12 120.2(2) . . ? C44 C43 C42 119.3(2) . . ? C43 C44 C45 119.5(2) . . ? C46 C45 C44 118.0(2) . . ? N41 C46 C45 123.7(2) . . ? C52 N51 C56 117.5(2) . . ? N51 C52 C53 121.9(2) . . ? N51 C52 N12 116.8(2) . . ? C53 C52 N12 121.3(2) . . ? C54 C53 C52 119.0(2) . . ? C53 C54 C55 119.8(2) . . ? C56 C55 C54 117.7(2) . . ? N51 C56 C55 124.1(2) . . ? F4 B1 F2' 125.5(4) . . ? F4 B1 F3 115.5(4) . . ? F2' B1 F3 52.4(4) . . ? F4 B1 F1 109.5(3) . . ? F2' B1 F1 125.0(4) . . ? F3 B1 F1 104.7(3) . . ? F4 B1 F4' 43.8(5) . . ? F2' B1 F4' 108.9(6) . . ? F3 B1 F4' 142.8(5) . . ? F1 B1 F4' 111.5(4) . . ? F4 B1 F2 111.1(4) . . ? F2' B1 F2 57.4(4) . . ? F3 B1 F2 109.1(3) . . ? F1 B1 F2 106.4(3) . . ? F4' B1 F2 68.9(6) . . ? F4 B1 F3' 55.4(5) . . ? F2' B1 F3' 101.1(5) . . ? F3 B1 F3' 62.4(5) . . ? F1 B1 F3' 109.1(3) . . ? F4' B1 F3' 96.9(7) . . ? F2 B1 F3' 144.5(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 C6 C1 C2 C3 -1.2(3) . . . . ? C11 C1 C2 C3 179.2(2) . . . . ? C6 C1 C2 C12 179.2(2) . . . . ? C11 C1 C2 C12 -0.4(3) . . . . ? C1 C2 C3 C4 1.5(3) . . . . ? C12 C2 C3 C4 -178.9(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? C11 C1 C6 C5 179.6(2) . . . . ? C6 C1 C11 N11 8.5(3) . . . . ? C2 C1 C11 N11 -171.9(2) . . . . ? C1 C11 N11 C22 -102.7(2) . . . . ? C1 C11 N11 C32 80.2(3) . . . . ? C42 N12 C12 C2 100.7(2) . . . . ? C52 N12 C12 C2 -83.5(3) . . . . ? C3 C2 C12 N12 -4.6(3) . . . . ? C1 C2 C12 N12 175.00(19) . . . . ? C26 N21 C22 N11 177.8(2) . . . . ? Ag1 N21 C22 N11 14.5(3) 3_656 . . . ? C26 N21 C22 C23 0.5(4) . . . . ? Ag1 N21 C22 C23 -162.76(19) 3_656 . . . ? C32 N11 C22 N21 29.3(3) . . . . ? C11 N11 C22 N21 -147.7(2) . . . . ? C32 N11 C22 C23 -153.4(2) . . . . ? C11 N11 C22 C23 29.7(3) . . . . ? N21 C22 C23 C24 0.9(4) . . . . ? N11 C22 C23 C24 -176.4(3) . . . . ? C22 C23 C24 C25 -1.1(5) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C22 N21 C26 C25 -1.7(4) . . . . ? Ag1 N21 C26 C25 162.0(2) 3_656 . . . ? C24 C25 C26 N21 1.5(4) . . . . ? C36 N31 C32 C33 -1.8(3) . . . . ? C36 N31 C32 N11 179.7(2) . . . . ? C22 N11 C32 N31 -145.6(2) . . . . ? C11 N11 C32 N31 31.4(3) . . . . ? C22 N11 C32 C33 35.9(3) . . . . ? C11 N11 C32 C33 -147.1(2) . . . . ? N31 C32 C33 C34 1.9(4) . . . . ? N11 C32 C33 C34 -179.6(2) . . . . ? C32 C33 C34 C35 -0.4(4) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? C32 N31 C36 C35 0.2(4) . . . . ? C34 C35 C36 N31 1.2(4) . . . . ? N21 Ag1 N41 C42 -16.8(3) 3_656 . . . ? N21 Ag1 N41 C46 149.28(18) 3_656 . . . ? C46 N41 C42 C43 -1.1(3) . . . . ? Ag1 N41 C42 C43 165.24(18) . . . . ? C46 N41 C42 N12 -179.1(2) . . . . ? Ag1 N41 C42 N12 -12.8(3) . . . . ? C52 N12 C42 N41 -32.7(3) . . . . ? C12 N12 C42 N41 142.8(2) . . . . ? C52 N12 C42 C43 149.3(2) . . . . ? C12 N12 C42 C43 -35.3(3) . . . . ? N41 C42 C43 C44 -0.6(4) . . . . ? N12 C42 C43 C44 177.4(2) . . . . ? C42 C43 C44 C45 1.7(4) . . . . ? C43 C44 C45 C46 -1.1(4) . . . . ? C42 N41 C46 C45 1.7(4) . . . . ? Ag1 N41 C46 C45 -164.9(2) . . . . ? C44 C45 C46 N41 -0.6(4) . . . . ? C56 N51 C52 C53 2.7(3) . . . . ? C56 N51 C52 N12 -178.5(2) . . . . ? C42 N12 C52 N51 153.6(2) . . . . ? C12 N12 C52 N51 -21.9(3) . . . . ? C42 N12 C52 C53 -27.7(3) . . . . ? C12 N12 C52 C53 156.9(2) . . . . ? N51 C52 C53 C54 -2.5(4) . . . . ? N12 C52 C53 C54 178.8(2) . . . . ? C52 C53 C54 C55 0.5(4) . . . . ? C53 C54 C55 C56 1.0(4) . . . . ? C52 N51 C56 C55 -1.2(4) . . . . ? C54 C55 C56 N51 -0.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.466 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.058 #END data_3csbs _database_code_depnum_ccdc_archive 'CCDC 614171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag N7 O3' _chemical_formula_weight 614.41 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.659(5) _cell_length_b 12.417(5) _cell_length_c 17.195(5) _cell_angle_alpha 90.0 _cell_angle_beta 106.291(5) _cell_angle_gamma 90.0 _cell_volume 2594.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 8085 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.855763 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 31748 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0099 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.36 _reflns_number_total 5275 _reflns_number_gt 4891 _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^)+(0.0256P)^2^+1.8526P] 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 5275 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.006 _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 0.147794(11) 0.280184(12) 0.370690(8) 0.03082(5) Uani 1 1 d . . . C1 C 0.61470(14) 0.17825(15) 0.40978(10) 0.0246(3) Uani 1 1 d . . . C2 C 0.70266(14) 0.10643(15) 0.43979(10) 0.0257(3) Uani 1 1 d . . . C3 C 0.80939(15) 0.14145(17) 0.44654(12) 0.0343(4) Uani 1 1 d . . . H3A H 0.8693 0.0938 0.4679 0.041 Uiso 1 1 calc R . . C4 C 0.83038(16) 0.24466(18) 0.42277(13) 0.0371(4) Uani 1 1 d . . . H4A H 0.9036 0.2664 0.4266 0.045 Uiso 1 1 calc R . . C5 C 0.74397(16) 0.31512(16) 0.39354(12) 0.0341(4) Uani 1 1 d . . . H5A H 0.7575 0.3859 0.3777 0.041 Uiso 1 1 calc R . . C6 C 0.63660(15) 0.28181(15) 0.38741(12) 0.0297(4) Uani 1 1 d . . . H6A H 0.5774 0.3307 0.3676 0.036 Uiso 1 1 calc R . . N11 N 0.41389(12) 0.22358(12) 0.37850(9) 0.0269(3) Uani 1 1 d . . . C11 C 0.49863(14) 0.13953(15) 0.40245(11) 0.0284(4) Uani 1 1 d . . . H11A H 0.4805 0.0807 0.3620 0.034 Uiso 1 1 calc R . . H11B H 0.4964 0.1092 0.4552 0.034 Uiso 1 1 calc R . . C12 C 0.67866(14) -0.00678(15) 0.46376(11) 0.0299(4) Uani 1 1 d . . . H12A H 0.6315 -0.0019 0.5008 0.036 Uiso 1 1 calc R . . H12B H 0.6366 -0.0457 0.4146 0.036 Uiso 1 1 calc R . . N12 N 0.77711(13) -0.06990(13) 0.50347(9) 0.0297(3) Uani 1 1 d . . . N21 N 0.24764(12) 0.26144(12) 0.27849(9) 0.0265(3) Uani 1 1 d . . . C22 C 0.35301(15) 0.22870(14) 0.29664(11) 0.0269(4) Uani 1 1 d . . . C23 C 0.40155(17) 0.19672(17) 0.23625(12) 0.0365(4) Uani 1 1 d . . . H23A H 0.4762 0.1740 0.2503 0.044 Uiso 1 1 calc R . . C24 C 0.33943(19) 0.19879(19) 0.15606(13) 0.0419(5) Uani 1 1 d . . . H24A H 0.3707 0.1764 0.1145 0.050 Uiso 1 1 calc R . . C25 C 0.23140(19) 0.23371(17) 0.13676(12) 0.0392(5) Uani 1 1 d . . . H25A H 0.1874 0.2364 0.0821 0.047 Uiso 1 1 calc R . . C26 C 0.18935(16) 0.26461(16) 0.19932(12) 0.0318(4) Uani 1 1 d . . . H26A H 0.1155 0.2895 0.1861 0.038 Uiso 1 1 calc R . . N31 N 0.42783(13) 0.25136(14) 0.51581(10) 0.0317(3) Uani 1 1 d . . . C32 C 0.39536(14) 0.29031(14) 0.43987(11) 0.0261(4) Uani 1 1 d . . . C33 C 0.34989(15) 0.39377(15) 0.42290(11) 0.0312(4) Uani 1 1 d . . . H33A H 0.3291 0.4207 0.3690 0.037 Uiso 1 1 calc R . . C34 C 0.33600(17) 0.45566(17) 0.48620(13) 0.0387(5) Uani 1 1 d . . . H34A H 0.3056 0.5259 0.4760 0.046 Uiso 1 1 calc R . . C35 C 0.36643(17) 0.41515(17) 0.56443(12) 0.0387(5) Uani 1 1 d . . . H35A H 0.3562 0.4559 0.6085 0.046 Uiso 1 1 calc R . . C36 C 0.41213(16) 0.31345(18) 0.57587(11) 0.0359(4) Uani 1 1 d . . . H36A H 0.4339 0.2855 0.6294 0.043 Uiso 1 1 calc R . . N41 N 0.85895(12) -0.23984(13) 0.50163(9) 0.0287(3) Uani 1 1 d . . . C42 C 0.81222(15) -0.15192(16) 0.46037(11) 0.0299(4) Uani 1 1 d . . . C43 C 0.79524(18) -0.1430(2) 0.37637(12) 0.0434(5) Uani 1 1 d . . . H43A H 0.7625 -0.0802 0.3481 0.052 Uiso 1 1 calc R . . C44 C 0.8270(2) -0.2271(2) 0.33559(14) 0.0519(6) Uani 1 1 d . . . H44A H 0.8149 -0.2231 0.2786 0.062 Uiso 1 1 calc R . . C45 C 0.87654(19) -0.3173(2) 0.37756(14) 0.0469(5) Uani 1 1 d . . . H45A H 0.8999 -0.3754 0.3504 0.056 Uiso 1 1 calc R . . C46 C 0.89090(16) -0.32030(18) 0.46006(13) 0.0368(4) Uani 1 1 d . . . H46A H 0.9250 -0.3820 0.4892 0.044 Uiso 1 1 calc R . . N51 N 0.75994(13) -0.02028(12) 0.63064(10) 0.0301(3) Uani 1 1 d . . . C52 C 0.82637(15) -0.05234(14) 0.58678(11) 0.0281(4) Uani 1 1 d . . . C53 C 0.93997(16) -0.06570(17) 0.62001(12) 0.0366(4) Uani 1 1 d . . . H53A H 0.9852 -0.0866 0.5869 0.044 Uiso 1 1 calc R . . C54 C 0.98484(17) -0.04779(19) 0.70210(13) 0.0431(5) Uani 1 1 d . . . H54A H 1.0616 -0.0564 0.7264 0.052 Uiso 1 1 calc R . . C55 C 0.91618(18) -0.01708(17) 0.74863(13) 0.0411(5) Uani 1 1 d . . . H55A H 0.9445 -0.0053 0.8053 0.049 Uiso 1 1 calc R . . C56 C 0.80560(17) -0.00417(16) 0.71007(12) 0.0353(4) Uani 1 1 d . . . H56A H 0.7589 0.0175 0.7418 0.042 Uiso 1 1 calc R . . N60 N -0.02915(14) 0.42988(14) 0.28708(10) 0.0357(4) Uani 1 1 d . . . O61 O 0.02664(17) 0.44870(16) 0.35733(10) 0.0682(6) Uani 1 1 d . . . O62 O -0.01858(16) 0.33936(16) 0.25886(12) 0.0688(6) Uani 1 1 d . . . O63 O -0.09615(14) 0.49632(13) 0.24729(9) 0.0511(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 0.02713(8) 0.03519(9) 0.02935(8) 0.00364(6) 0.00661(6) 0.00806(6) C1 0.0221(8) 0.0304(9) 0.0207(8) -0.0022(7) 0.0048(6) 0.0021(7) C2 0.0229(8) 0.0320(9) 0.0221(8) 0.0012(7) 0.0061(6) 0.0036(7) C3 0.0218(9) 0.0414(11) 0.0396(10) 0.0066(9) 0.0083(8) 0.0058(8) C4 0.0227(9) 0.0440(11) 0.0448(11) 0.0009(9) 0.0098(8) -0.0030(8) C5 0.0323(10) 0.0303(9) 0.0407(11) -0.0005(8) 0.0118(8) -0.0027(8) C6 0.0256(9) 0.0290(9) 0.0330(9) -0.0001(7) 0.0056(7) 0.0045(7) N11 0.0199(7) 0.0314(8) 0.0276(8) 0.0013(6) 0.0037(6) 0.0056(6) C11 0.0213(8) 0.0284(9) 0.0343(9) 0.0022(7) 0.0057(7) 0.0049(7) C12 0.0214(8) 0.0338(10) 0.0329(9) 0.0088(8) 0.0047(7) 0.0063(7) N12 0.0268(8) 0.0329(8) 0.0278(8) 0.0052(6) 0.0049(6) 0.0100(6) N21 0.0237(7) 0.0280(7) 0.0259(7) 0.0036(6) 0.0038(6) 0.0008(6) C22 0.0246(9) 0.0266(9) 0.0281(9) 0.0001(7) 0.0053(7) -0.0017(7) C23 0.0290(10) 0.0450(11) 0.0361(10) -0.0053(9) 0.0103(8) 0.0004(8) C24 0.0434(12) 0.0526(13) 0.0320(10) -0.0090(9) 0.0145(9) -0.0043(10) C25 0.0456(12) 0.0426(11) 0.0249(9) -0.0014(8) 0.0027(8) -0.0058(9) C26 0.0286(9) 0.0331(10) 0.0291(9) 0.0040(8) 0.0005(7) -0.0013(8) N31 0.0283(8) 0.0357(8) 0.0269(8) 0.0027(7) 0.0010(6) 0.0056(7) C32 0.0187(8) 0.0303(9) 0.0260(8) 0.0012(7) 0.0010(6) -0.0004(7) C33 0.0293(9) 0.0300(9) 0.0301(9) 0.0056(8) 0.0014(7) -0.0006(8) C34 0.0389(11) 0.0291(10) 0.0421(11) -0.0002(8) 0.0016(9) 0.0033(8) C35 0.0351(10) 0.0424(11) 0.0331(10) -0.0109(9) 0.0008(8) 0.0038(9) C36 0.0323(10) 0.0466(11) 0.0232(9) 0.0000(8) -0.0013(7) 0.0058(9) N41 0.0229(7) 0.0348(8) 0.0277(8) -0.0024(6) 0.0059(6) 0.0050(6) C42 0.0233(8) 0.0393(10) 0.0272(9) 0.0022(8) 0.0073(7) 0.0041(8) C43 0.0434(12) 0.0583(14) 0.0291(10) 0.0074(9) 0.0109(9) 0.0085(10) C44 0.0521(14) 0.0782(18) 0.0279(11) -0.0032(11) 0.0153(10) 0.0050(12) C45 0.0412(12) 0.0602(14) 0.0430(12) -0.0158(11) 0.0178(10) 0.0034(11) C46 0.0282(9) 0.0426(11) 0.0403(11) -0.0069(9) 0.0111(8) 0.0069(8) N51 0.0296(8) 0.0279(8) 0.0327(8) 0.0005(6) 0.0087(6) 0.0057(6) C52 0.0283(9) 0.0244(8) 0.0309(9) 0.0039(7) 0.0074(7) 0.0040(7) C53 0.0277(9) 0.0430(11) 0.0383(11) -0.0024(9) 0.0081(8) 0.0051(8) C54 0.0300(10) 0.0494(13) 0.0433(12) -0.0064(10) -0.0006(9) 0.0037(9) C55 0.0446(12) 0.0391(11) 0.0331(10) -0.0073(9) 0.0006(9) 0.0044(9) C56 0.0420(11) 0.0293(9) 0.0354(10) -0.0037(8) 0.0121(9) 0.0039(8) N60 0.0333(9) 0.0351(9) 0.0345(9) -0.0001(7) 0.0023(7) 0.0075(7) O61 0.0839(14) 0.0581(11) 0.0402(9) -0.0048(8) -0.0196(9) 0.0293(10) O62 0.0636(12) 0.0610(12) 0.0674(12) -0.0240(10) -0.0051(9) 0.0306(10) O63 0.0558(10) 0.0423(9) 0.0408(8) 0.0004(7) -0.0101(7) 0.0188(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 N41 2.2767(17) 3_656 ? Ag1 N21 2.2999(16) . ? Ag1 O62 2.5301(19) . ? Ag1 O61 2.5662(19) . ? C1 C6 1.392(3) . ? C1 C2 1.407(2) . ? C1 C11 1.517(2) . ? C2 C3 1.393(3) . ? C2 C12 1.519(3) . ? C3 C4 1.393(3) . ? C4 C5 1.381(3) . ? C5 C6 1.396(3) . ? N11 C22 1.404(2) . ? N11 C32 1.412(2) . ? N11 C11 1.470(2) . ? C12 N12 1.468(2) . ? N12 C42 1.403(2) . ? N12 C52 1.410(2) . ? N21 C22 1.345(2) . ? N21 C26 1.355(2) . ? C22 C23 1.404(3) . ? C23 C24 1.383(3) . ? C24 C25 1.383(3) . ? C25 C26 1.382(3) . ? N31 C32 1.344(2) . ? N31 C36 1.347(3) . ? C32 C33 1.404(3) . ? C33 C34 1.383(3) . ? C34 C35 1.386(3) . ? C35 C36 1.380(3) . ? N41 C42 1.345(2) . ? N41 C46 1.355(3) . ? N41 Ag1 2.2767(17) 3_656 ? C42 C43 1.404(3) . ? C43 C44 1.379(3) . ? C44 C45 1.384(4) . ? C45 C46 1.379(3) . ? N51 C52 1.338(2) . ? N51 C56 1.340(3) . ? C52 C53 1.400(3) . ? C53 C54 1.384(3) . ? C54 C55 1.390(3) . ? C55 C56 1.380(3) . ? N60 O61 1.239(2) . ? N60 O63 1.242(2) . ? N60 O62 1.246(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Ag1 N21 144.98(5) 3_656 . ? N41 Ag1 O62 123.26(7) 3_656 . ? N21 Ag1 O62 90.39(7) . . ? N41 Ag1 O61 94.74(6) 3_656 . ? N21 Ag1 O61 116.81(6) . . ? O62 Ag1 O61 49.16(5) . . ? C6 C1 C2 119.24(16) . . ? C6 C1 C11 122.21(15) . . ? C2 C1 C11 118.56(16) . . ? C3 C2 C1 118.82(17) . . ? C3 C2 C12 121.96(16) . . ? C1 C2 C12 119.22(16) . . ? C2 C3 C4 121.54(17) . . ? C5 C4 C3 119.52(18) . . ? C4 C5 C6 119.67(19) . . ? C1 C6 C5 121.18(17) . . ? C22 N11 C32 124.28(15) . . ? C22 N11 C11 117.72(15) . . ? C32 N11 C11 117.93(14) . . ? N11 C11 C1 114.32(15) . . ? N12 C12 C2 114.32(15) . . ? C42 N12 C52 122.25(15) . . ? C42 N12 C12 119.67(15) . . ? C52 N12 C12 117.76(15) . . ? C22 N21 C26 117.85(16) . . ? C22 N21 Ag1 124.88(12) . . ? C26 N21 Ag1 116.10(13) . . ? N21 C22 N11 118.44(16) . . ? N21 C22 C23 121.69(17) . . ? N11 C22 C23 119.85(17) . . ? C24 C23 C22 119.19(19) . . ? C25 C24 C23 119.50(19) . . ? C26 C25 C24 118.11(19) . . ? N21 C26 C25 123.64(19) . . ? C32 N31 C36 117.91(17) . . ? N31 C32 C33 121.78(17) . . ? N31 C32 N11 116.44(16) . . ? C33 C32 N11 121.72(16) . . ? C34 C33 C32 118.68(17) . . ? C33 C34 C35 120.00(19) . . ? C36 C35 C34 117.51(19) . . ? N31 C36 C35 124.08(18) . . ? C42 N41 C46 118.19(17) . . ? C42 N41 Ag1 123.87(12) . 3_656 ? C46 N41 Ag1 116.36(14) . 3_656 ? N41 C42 N12 117.90(16) . . ? N41 C42 C43 121.63(18) . . ? N12 C42 C43 120.44(18) . . ? C44 C43 C42 118.8(2) . . ? C43 C44 C45 120.1(2) . . ? C46 C45 C44 117.9(2) . . ? N41 C46 C45 123.4(2) . . ? C52 N51 C56 117.33(17) . . ? N51 C52 C53 122.76(17) . . ? N51 C52 N12 116.74(16) . . ? C53 C52 N12 120.47(17) . . ? C54 C53 C52 118.54(19) . . ? C53 C54 C55 119.17(19) . . ? C56 C55 C54 117.99(19) . . ? N51 C56 C55 124.17(19) . . ? O61 N60 O63 121.76(18) . . ? O61 N60 O62 117.12(18) . . ? O63 N60 O62 121.06(18) . . ? N60 O61 Ag1 95.53(13) . . ? N60 O62 Ag1 97.09(12) . . ? 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 C6 C1 C2 C3 0.3(3) . . . . ? C11 C1 C2 C3 179.90(16) . . . . ? C6 C1 C2 C12 -179.67(16) . . . . ? C11 C1 C2 C12 0.0(2) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C12 C2 C3 C4 178.59(19) . . . . ? C2 C3 C4 C5 1.5(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C2 C1 C6 C5 0.6(3) . . . . ? C11 C1 C6 C5 -179.01(17) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? C22 N11 C11 C1 98.83(19) . . . . ? C32 N11 C11 C1 -84.2(2) . . . . ? C6 C1 C11 N11 -6.3(2) . . . . ? C2 C1 C11 N11 174.04(15) . . . . ? C3 C2 C12 N12 7.3(3) . . . . ? C1 C2 C12 N12 -172.82(15) . . . . ? C2 C12 N12 C42 -105.2(2) . . . . ? C2 C12 N12 C52 81.1(2) . . . . ? N41 Ag1 N21 C22 -14.6(2) 3_656 . . . ? O62 Ag1 N21 C22 -179.50(15) . . . . ? O61 Ag1 N21 C22 137.33(14) . . . . ? N41 Ag1 N21 C26 152.68(13) 3_656 . . . ? O62 Ag1 N21 C26 -12.21(14) . . . . ? O61 Ag1 N21 C26 -55.38(15) . . . . ? C26 N21 C22 N11 -179.11(16) . . . . ? Ag1 N21 C22 N11 -12.0(2) . . . . ? C26 N21 C22 C23 -1.1(3) . . . . ? Ag1 N21 C22 C23 165.95(14) . . . . ? C32 N11 C22 N21 -29.2(3) . . . . ? C11 N11 C22 N21 147.48(16) . . . . ? C32 N11 C22 C23 152.75(18) . . . . ? C11 N11 C22 C23 -30.5(2) . . . . ? N21 C22 C23 C24 -0.1(3) . . . . ? N11 C22 C23 C24 177.85(19) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C22 N21 C26 C25 1.6(3) . . . . ? Ag1 N21 C26 C25 -166.62(16) . . . . ? C24 C25 C26 N21 -0.8(3) . . . . ? C36 N31 C32 C33 2.2(3) . . . . ? C36 N31 C32 N11 179.47(17) . . . . ? C22 N11 C32 N31 155.24(17) . . . . ? C11 N11 C32 N31 -21.5(2) . . . . ? C22 N11 C32 C33 -27.5(3) . . . . ? C11 N11 C32 C33 155.80(16) . . . . ? N31 C32 C33 C34 -1.6(3) . . . . ? N11 C32 C33 C34 -178.73(17) . . . . ? C32 C33 C34 C35 -0.2(3) . . . . ? C33 C34 C35 C36 1.2(3) . . . . ? C32 N31 C36 C35 -1.1(3) . . . . ? C34 C35 C36 N31 -0.6(3) . . . . ? C46 N41 C42 N12 178.62(17) . . . . ? Ag1 N41 C42 N12 13.5(2) 3_656 . . . ? C46 N41 C42 C43 0.7(3) . . . . ? Ag1 N41 C42 C43 -164.41(15) 3_656 . . . ? C52 N12 C42 N41 27.3(3) . . . . ? C12 N12 C42 N41 -146.06(17) . . . . ? C52 N12 C42 C43 -154.75(19) . . . . ? C12 N12 C42 C43 31.9(3) . . . . ? N41 C42 C43 C44 0.3(3) . . . . ? N12 C42 C43 C44 -177.5(2) . . . . ? C42 C43 C44 C45 -1.2(4) . . . . ? C43 C44 C45 C46 1.0(4) . . . . ? C42 N41 C46 C45 -1.0(3) . . . . ? Ag1 N41 C46 C45 165.29(17) 3_656 . . . ? C44 C45 C46 N41 0.1(3) . . . . ? C56 N51 C52 C53 -2.2(3) . . . . ? C56 N51 C52 N12 179.46(16) . . . . ? C42 N12 C52 N51 -144.63(18) . . . . ? C12 N12 C52 N51 28.9(2) . . . . ? C42 N12 C52 C53 37.0(3) . . . . ? C12 N12 C52 C53 -149.51(18) . . . . ? N51 C52 C53 C54 1.8(3) . . . . ? N12 C52 C53 C54 -179.89(19) . . . . ? C52 C53 C54 C55 -0.1(3) . . . . ? C53 C54 C55 C56 -1.0(3) . . . . ? C52 N51 C56 C55 1.0(3) . . . . ? C54 C55 C56 N51 0.6(3) . . . . ? O63 N60 O61 Ag1 -172.39(18) . . . . ? O62 N60 O61 Ag1 10.5(2) . . . . ? N41 Ag1 O61 N60 -137.02(15) 3_656 . . . ? N21 Ag1 O61 N60 58.69(17) . . . . ? O62 Ag1 O61 N60 -6.04(13) . . . . ? O61 N60 O62 Ag1 -10.6(2) . . . . ? O63 N60 O62 Ag1 172.18(17) . . . . ? N41 Ag1 O62 N60 70.15(17) 3_656 . . . ? N21 Ag1 O62 N60 -120.16(15) . . . . ? O61 Ag1 O62 N60 6.02(13) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.574 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.049 #END data_c:\docume~1\chriss\mydocu~1\papers\cs10\3csbu\work\3csbu _database_code_depnum_ccdc_archive 'CCDC 614172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Ag F6 N6 O P' _chemical_formula_weight 729.41 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' 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 8.623(3) _cell_length_b 25.164(9) _cell_length_c 14.262(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.626(4) _cell_angle_gamma 90.00 _cell_volume 3084.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 5109 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.99 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830675 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 17476 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3121 _reflns_number_gt 2833 _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^)+(0.0449P)^2^+17.7216P] 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 3121 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _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 0.0000 0.15052(2) 0.7500 0.04154(19) Uani 1 2 d S . . C1 C 0.3620(5) -0.04418(18) 0.7617(3) 0.0303(9) Uani 1 1 d . . . C2 C 0.5000 -0.0168(2) 0.7500 0.0251(11) Uani 1 2 d S . . H2A H 0.5000 0.0209 0.7500 0.030 Uiso 1 2 calc SR . . C5 C 0.5000 -0.1267(3) 0.7500 0.0461(17) Uani 1 2 d S . . H5A H 0.5000 -0.1644 0.7500 0.055 Uiso 1 2 calc SR . . C6 C 0.3635(6) -0.09983(19) 0.7621(3) 0.0401(11) Uani 1 1 d . . . H6A H 0.2709 -0.1190 0.7707 0.048 Uiso 1 1 calc R . . N11 N 0.2185(4) 0.04302(15) 0.7682(2) 0.0307(8) Uani 1 1 d . . . C11 C 0.2091(5) -0.01508(18) 0.7728(3) 0.0341(10) Uani 1 1 d . . . H11A H 0.1310 -0.0274 0.7229 0.041 Uiso 1 1 calc R . . H11B H 0.1712 -0.0251 0.8341 0.041 Uiso 1 1 calc R . . N21 N 0.1897(5) 0.12199(18) 0.8539(3) 0.0455(10) Uani 1 1 d . . . C22 C 0.2465(5) 0.0717(2) 0.8515(3) 0.0372(10) Uani 1 1 d . . . C23 C 0.3279(6) 0.0489(3) 0.9300(4) 0.0495(13) Uani 1 1 d . . . H23A H 0.3679 0.0138 0.9271 0.059 Uiso 1 1 calc R . . C24 C 0.3494(7) 0.0780(3) 1.0119(4) 0.068(2) Uani 1 1 d . . . H24A H 0.4025 0.0629 1.0664 0.082 Uiso 1 1 calc R . . C25 C 0.2933(9) 0.1294(4) 1.0141(5) 0.084(2) Uani 1 1 d . . . H25A H 0.3081 0.1504 1.0695 0.100 Uiso 1 1 calc R . . C26 C 0.2150(8) 0.1492(3) 0.9335(5) 0.0717(19) Uani 1 1 d . . . H26A H 0.1767 0.1846 0.9349 0.086 Uiso 1 1 calc R . . N31 N 0.1185(5) 0.04160(16) 0.6118(3) 0.0380(9) Uani 1 1 d . . . C32 C 0.2063(5) 0.06730(18) 0.6785(3) 0.0320(9) Uani 1 1 d . . . C33 C 0.2883(6) 0.1139(2) 0.6615(4) 0.0453(12) Uani 1 1 d . . . H33A H 0.3535 0.1303 0.7100 0.054 Uiso 1 1 calc R . . C34 C 0.2714(7) 0.1352(2) 0.5723(4) 0.0553(14) Uani 1 1 d . . . H34A H 0.3248 0.1669 0.5583 0.066 Uiso 1 1 calc R . . C35 C 0.1764(8) 0.1102(3) 0.5037(4) 0.0583(15) Uani 1 1 d . . . H35A H 0.1608 0.1247 0.4422 0.070 Uiso 1 1 calc R . . C36 C 0.1044(7) 0.0635(2) 0.5264(3) 0.0496(13) Uani 1 1 d . . . H36A H 0.0411 0.0459 0.4784 0.059 Uiso 1 1 calc R . . O40 O 0.0653(8) 0.2382(3) 0.6666(6) 0.0522(19) Uani 0.50 1 d P . . H40 H -0.0317 0.2463 0.6889 0.078 Uiso 0.50 1 d PR . . C41 C 0.0565(16) 0.2597(5) 0.5840(12) 0.083(5) Uani 0.50 1 d P . . H41A H 0.0401 0.2319 0.5360 0.124 Uiso 0.50 1 calc PR . . H41B H 0.1535 0.2786 0.5750 0.124 Uiso 0.50 1 calc PR . . H41C H -0.0308 0.2847 0.5782 0.124 Uiso 0.50 1 calc PR . . P1 P 0.5000 0.27521(10) 0.7500 0.0910(11) Uani 1 2 d S . . F1 F 0.5000 0.3365(3) 0.7500 0.224(8) Uani 1 2 d S . . F2 F 0.3375(8) 0.2778(3) 0.7949(8) 0.197(4) Uani 1 1 d . . . F3 F 0.3985(10) 0.2784(4) 0.6568(6) 0.213(4) Uani 1 1 d . . . F4 F 0.5000 0.2169(3) 0.7500 0.267(10) Uani 1 2 d S . . 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 0.0358(3) 0.0360(3) 0.0518(3) 0.000 -0.0029(2) 0.000 C1 0.028(2) 0.037(2) 0.026(2) 0.0003(17) 0.0022(16) -0.0037(18) C2 0.025(3) 0.025(3) 0.025(3) 0.000 0.001(2) 0.000 C5 0.063(5) 0.027(3) 0.048(4) 0.000 0.010(3) 0.000 C6 0.046(3) 0.035(2) 0.041(3) 0.000(2) 0.012(2) -0.013(2) N11 0.0215(16) 0.043(2) 0.0274(18) 0.0001(15) 0.0025(13) 0.0039(15) C11 0.023(2) 0.043(3) 0.037(2) 0.0056(19) 0.0047(17) -0.0044(18) N21 0.037(2) 0.054(3) 0.044(2) -0.015(2) -0.0077(18) 0.0011(19) C22 0.022(2) 0.057(3) 0.032(2) -0.003(2) 0.0000(17) 0.0025(19) C23 0.033(2) 0.078(4) 0.037(3) 0.002(3) 0.001(2) 0.013(3) C24 0.049(3) 0.121(6) 0.034(3) -0.011(3) -0.010(2) 0.017(4) C25 0.073(4) 0.118(6) 0.055(4) -0.042(4) -0.022(3) 0.014(4) C26 0.070(4) 0.079(4) 0.063(4) -0.035(4) -0.019(3) 0.013(4) N31 0.041(2) 0.043(2) 0.030(2) -0.0048(16) 0.0027(16) 0.0041(17) C32 0.024(2) 0.040(2) 0.032(2) -0.0023(18) 0.0066(16) 0.0053(17) C33 0.036(2) 0.047(3) 0.053(3) 0.005(2) 0.004(2) -0.003(2) C34 0.059(3) 0.048(3) 0.061(4) 0.014(3) 0.017(3) -0.001(3) C35 0.078(4) 0.061(4) 0.037(3) 0.012(3) 0.012(3) 0.010(3) C36 0.066(3) 0.054(3) 0.028(3) -0.005(2) 0.003(2) 0.007(3) O40 0.044(4) 0.026(3) 0.088(6) 0.010(4) 0.015(4) -0.002(3) C41 0.072(9) 0.040(6) 0.128(13) 0.024(8) -0.046(9) -0.014(6) P1 0.0745(18) 0.0440(13) 0.143(3) 0.000 -0.0603(19) 0.000 F1 0.079(5) 0.067(5) 0.52(3) 0.000 0.001(9) 0.000 F2 0.098(5) 0.162(7) 0.333(13) 0.053(7) 0.038(6) -0.007(4) F3 0.187(8) 0.281(12) 0.154(7) 0.041(7) -0.090(6) 0.003(8) F4 0.193(11) 0.045(4) 0.53(3) 0.000 -0.141(14) 0.000 _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 N21 2.235(4) 2_556 ? Ag1 N21 2.235(4) . ? Ag1 O40 2.591(7) . ? Ag1 O40 2.591(7) 2_556 ? C1 C2 1.397(5) . ? C1 C6 1.400(6) . ? C1 C11 1.528(6) . ? C2 C1 1.397(5) 2_656 ? C5 C6 1.380(6) . ? C5 C6 1.380(6) 2_656 ? N11 C22 1.394(6) . ? N11 C32 1.414(6) . ? N11 C11 1.466(6) . ? N21 C26 1.329(7) . ? N21 C22 1.359(7) . ? C22 C23 1.395(7) . ? C23 C24 1.378(8) . ? C24 C25 1.382(11) . ? C25 C26 1.379(10) . ? N31 C36 1.333(6) . ? N31 C32 1.334(6) . ? C32 C33 1.401(7) . ? C33 C34 1.377(8) . ? C34 C35 1.378(9) . ? C35 C36 1.379(8) . ? O40 C41 1.292(17) . ? P1 F4 1.467(8) . ? P1 F3 1.533(7) 2_656 ? P1 F3 1.533(7) . ? P1 F1 1.543(8) . ? P1 F2 1.589(8) 2_656 ? P1 F2 1.589(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 N21 Ag1 N21 142.5(2) 2_556 . ? N21 Ag1 O40 98.3(2) 2_556 . ? N21 Ag1 O40 113.8(2) . . ? N21 Ag1 O40 113.8(2) 2_556 2_556 ? N21 Ag1 O40 98.3(2) . 2_556 ? O40 Ag1 O40 63.2(4) . 2_556 ? C2 C1 C6 119.0(4) . . ? C2 C1 C11 121.8(4) . . ? C6 C1 C11 119.2(4) . . ? C1 C2 C1 120.9(5) 2_656 . ? C6 C5 C6 121.3(6) . 2_656 ? C5 C6 C1 119.8(5) . . ? C22 N11 C32 122.8(4) . . ? C22 N11 C11 119.0(4) . . ? C32 N11 C11 118.1(4) . . ? N11 C11 C1 115.0(3) . . ? C26 N21 C22 117.8(5) . . ? C26 N21 Ag1 117.5(4) . . ? C22 N21 Ag1 121.9(3) . . ? N21 C22 N11 117.7(4) . . ? N21 C22 C23 121.4(5) . . ? N11 C22 C23 120.8(5) . . ? C24 C23 C22 119.1(6) . . ? C23 C24 C25 119.6(6) . . ? C26 C25 C24 117.9(6) . . ? N21 C26 C25 124.2(7) . . ? C36 N31 C32 117.1(4) . . ? N31 C32 C33 123.2(4) . . ? N31 C32 N11 115.6(4) . . ? C33 C32 N11 121.1(4) . . ? C34 C33 C32 118.0(5) . . ? C33 C34 C35 119.3(5) . . ? C34 C35 C36 118.4(5) . . ? N31 C36 C35 123.8(5) . . ? C41 O40 Ag1 140.8(8) . . ? F4 P1 F3 93.0(4) . 2_656 ? F4 P1 F3 93.0(4) . . ? F3 P1 F3 174.1(9) 2_656 . ? F4 P1 F1 180.000(2) . . ? F3 P1 F1 87.0(4) 2_656 . ? F3 P1 F1 87.0(4) . . ? F4 P1 F2 92.4(3) . 2_656 ? F3 P1 F2 83.5(5) 2_656 2_656 ? F3 P1 F2 96.3(5) . 2_656 ? F1 P1 F2 87.6(3) . 2_656 ? F4 P1 F2 92.4(3) . . ? F3 P1 F2 96.3(5) 2_656 . ? F3 P1 F2 83.5(5) . . ? F1 P1 F2 87.6(3) . . ? F2 P1 F2 175.2(6) 2_656 . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.720 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.089 #END data_c:\chris'~1\canter~2\papers\cs10\3csce\3csce2\3csce2 _database_code_depnum_ccdc_archive 'CCDC 614173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H52 Ag3 F18 N12 O2 P3' _chemical_formula_weight 1683.62 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' 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 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 14.7918(9) _cell_length_b 14.7643(9) _cell_length_c 29.0604(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.8810(10) _cell_angle_gamma 90.00 _cell_volume 6323.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6948 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.31 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790843 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 47897 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.39 _reflns_number_total 12819 _reflns_number_gt 9727 _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^)+(0.0702P)^2^+19.7685P] 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 12819 _refine_ls_number_parameters 915 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.004 _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 0.27686(2) 0.54341(2) 0.297845(13) 0.02965(11) Uani 1 1 d . . . Ag2 Ag 0.28908(3) 0.72141(3) 0.034514(13) 0.03001(11) Uani 1 1 d . . . Ag3 Ag 0.23646(3) 0.33322(3) 0.220748(16) 0.04481(13) Uani 1 1 d . . . C1' C 0.1139(3) 0.4411(3) 0.16343(15) 0.0274(10) Uani 1 1 d . . . C1 C 0.4233(3) 0.5989(3) 0.23351(16) 0.0270(10) Uani 1 1 d . . . C2 C 0.4026(3) 0.6713(3) 0.26167(15) 0.0280(10) Uani 1 1 d . . . H2A H 0.4213 0.6695 0.2938 0.034 Uiso 1 1 calc R . . C2' C 0.1665(4) 0.5125(4) 0.15068(18) 0.0354(12) Uani 1 1 d . . . H2'A H 0.1651 0.5685 0.1667 0.042 Uiso 1 1 calc R . . C3 C 0.3553(3) 0.7459(3) 0.24345(16) 0.0274(10) Uani 1 1 d . . . H3A H 0.3420 0.7945 0.2632 0.033 Uiso 1 1 calc R . . C3' C 0.2209(4) 0.5031(4) 0.11489(17) 0.0335(11) Uani 1 1 d . . . H3'A H 0.2554 0.5536 0.1062 0.040 Uiso 1 1 calc R . . C4 C 0.3267(3) 0.7504(3) 0.19633(16) 0.0266(10) Uani 1 1 d . . . C4' C 0.2271(3) 0.4222(3) 0.09111(16) 0.0280(10) Uani 1 1 d . . . C5' C 0.1743(4) 0.3496(3) 0.10359(17) 0.0324(11) Uani 1 1 d . . . H5'A H 0.1766 0.2936 0.0877 0.039 Uiso 1 1 calc R . . C5 C 0.3489(3) 0.6788(3) 0.16839(16) 0.0306(11) Uani 1 1 d . . . H5A H 0.3309 0.6811 0.1362 0.037 Uiso 1 1 calc R . . C6' C 0.1183(3) 0.3590(3) 0.13913(16) 0.0299(11) Uani 1 1 d . . . H6'A H 0.0823 0.3091 0.1473 0.036 Uiso 1 1 calc R . . C6 C 0.3965(3) 0.6043(3) 0.18624(16) 0.0301(11) Uani 1 1 d . . . H6A H 0.4111 0.5564 0.1663 0.036 Uiso 1 1 calc R . . N11' N 0.0872(3) 0.4939(3) 0.24336(13) 0.0287(9) Uani 1 1 d . . . C11 C 0.4773(3) 0.5190(3) 0.25367(17) 0.0305(11) Uani 1 1 d . . . H11A H 0.5358 0.5164 0.2396 0.037 Uiso 1 1 calc R . . H11B H 0.4909 0.5290 0.2872 0.037 Uiso 1 1 calc R . . C11' C 0.0485(3) 0.4505(4) 0.20081(17) 0.0327(11) Uani 1 1 d . . . H11C H -0.0047 0.4861 0.1883 0.039 Uiso 1 1 calc R . . H11D H 0.0266 0.3894 0.2085 0.039 Uiso 1 1 calc R . . N11 N 0.4309(3) 0.4304(3) 0.24669(13) 0.0288(9) Uani 1 1 d . . . N14 N 0.2615(3) 0.8403(3) 0.12799(13) 0.0294(9) Uani 1 1 d . . . N14' N 0.3013(3) 0.4961(3) 0.02723(13) 0.0274(9) Uani 1 1 d . . . C14' C 0.2916(4) 0.4122(3) 0.05404(17) 0.0320(11) Uani 1 1 d . . . H14A H 0.3519 0.3942 0.0685 0.038 Uiso 1 1 calc R . . H14B H 0.2697 0.3631 0.0327 0.038 Uiso 1 1 calc R . . C14 C 0.2707(4) 0.8307(3) 0.17856(16) 0.0313(11) Uani 1 1 d . . . H14C H 0.2094 0.8253 0.1895 0.038 Uiso 1 1 calc R . . H14D H 0.2986 0.8865 0.1922 0.038 Uiso 1 1 calc R . . N21 N 0.3698(3) 0.3251(3) 0.19307(15) 0.0344(10) Uani 1 1 d . . . N21' N 0.1526(3) 0.3634(3) 0.27793(14) 0.0322(9) Uani 1 1 d . . . C22' C 0.1034(3) 0.4390(3) 0.28260(16) 0.0298(11) Uani 1 1 d . . . C22 C 0.4384(3) 0.3807(3) 0.20585(16) 0.0278(10) Uani 1 1 d . . . C23' C 0.0675(4) 0.4610(4) 0.32416(18) 0.0403(13) Uani 1 1 d . . . H23A H 0.0321 0.5141 0.3268 0.048 Uiso 1 1 calc R . . C23 C 0.5135(4) 0.3890(4) 0.17989(17) 0.0340(11) Uani 1 1 d . . . H23B H 0.5607 0.4307 0.1888 0.041 Uiso 1 1 calc R . . C24 C 0.5177(4) 0.3358(4) 0.14129(18) 0.0408(13) Uani 1 1 d . . . H24A H 0.5678 0.3408 0.1231 0.049 Uiso 1 1 calc R . . C24' C 0.0850(5) 0.4029(4) 0.36154(19) 0.0482(16) Uani 1 1 d . . . H24B H 0.0622 0.4169 0.3903 0.058 Uiso 1 1 calc R . . C25' C 0.1342(4) 0.3265(4) 0.35718(19) 0.0454(15) Uani 1 1 d . . . H25A H 0.1463 0.2866 0.3826 0.054 Uiso 1 1 calc R . . C25 C 0.4483(4) 0.2746(4) 0.12904(19) 0.0422(14) Uani 1 1 d . . . H25B H 0.4508 0.2360 0.1030 0.051 Uiso 1 1 calc R . . C26 C 0.3763(4) 0.2718(4) 0.15572(18) 0.0386(12) Uani 1 1 d . . . H26A H 0.3285 0.2304 0.1475 0.046 Uiso 1 1 calc R . . C26' C 0.1666(4) 0.3079(4) 0.3148(2) 0.0426(14) Uani 1 1 d . . . H26B H 0.2001 0.2537 0.3116 0.051 Uiso 1 1 calc R . . N31 N 0.3695(3) 0.4351(3) 0.31836(13) 0.0263(8) Uani 1 1 d . . . N31' N 0.1573(3) 0.6212(3) 0.27737(13) 0.0258(8) Uani 1 1 d . . . C32' C 0.0906(3) 0.5884(3) 0.24774(16) 0.0272(10) Uani 1 1 d . . . C32 C 0.4091(3) 0.3845(3) 0.28716(16) 0.0272(10) Uani 1 1 d . . . C33 C 0.4311(3) 0.2943(4) 0.29543(18) 0.0329(11) Uani 1 1 d . . . H33A H 0.4565 0.2590 0.2725 0.040 Uiso 1 1 calc R . . C33' C 0.0313(3) 0.6464(4) 0.22182(18) 0.0356(12) Uani 1 1 d . . . H33B H -0.0158 0.6227 0.2010 0.043 Uiso 1 1 calc R . . C34 C 0.4155(4) 0.2567(4) 0.33737(18) 0.0362(12) Uani 1 1 d . . . H34A H 0.4297 0.1949 0.3434 0.043 Uiso 1 1 calc R . . C34' C 0.0427(4) 0.7384(4) 0.2272(2) 0.0433(14) Uani 1 1 d . . . H34B H 0.0058 0.7788 0.2084 0.052 Uiso 1 1 calc R . . C35' C 0.1073(3) 0.7724(4) 0.25971(18) 0.0341(11) Uani 1 1 d . . . H35A H 0.1136 0.8357 0.2647 0.041 Uiso 1 1 calc R . . C35 C 0.3793(4) 0.3093(4) 0.37064(17) 0.0342(12) Uani 1 1 d . . . H35B H 0.3708 0.2851 0.4002 0.041 Uiso 1 1 calc R . . C36 C 0.3559(3) 0.3977(4) 0.35982(16) 0.0302(11) Uani 1 1 d . . . H36A H 0.3293 0.4336 0.3822 0.036 Uiso 1 1 calc R . . C36' C 0.1622(3) 0.7121(3) 0.28451(17) 0.0306(11) Uani 1 1 d . . . H36B H 0.2055 0.7347 0.3077 0.037 Uiso 1 1 calc R . . N41' N 0.2100(3) 0.6164(3) -0.00313(13) 0.0283(9) Uani 1 1 d . . . N41 N 0.3563(3) 0.8378(3) 0.06705(13) 0.0287(9) Uani 1 1 d . . . C42 C 0.3321(3) 0.8794(3) 0.10573(16) 0.0291(10) Uani 1 1 d . . . C42' C 0.2254(4) 0.5269(3) 0.00024(16) 0.0316(11) Uani 1 1 d . . . C43 C 0.3759(4) 0.9562(4) 0.12264(18) 0.0366(12) Uani 1 1 d . . . H43A H 0.3579 0.9846 0.1497 0.044 Uiso 1 1 calc R . . C43' C 0.1634(5) 0.4656(4) -0.0210(2) 0.062(2) Uani 1 1 d . . . H43B H 0.1737 0.4022 -0.0184 0.074 Uiso 1 1 calc R . . C44 C 0.4466(4) 0.9919(4) 0.0998(2) 0.0417(13) Uani 1 1 d . . . H44A H 0.4776 1.0446 0.1114 0.050 Uiso 1 1 calc R . . C44' C 0.0866(6) 0.4983(5) -0.0461(3) 0.079(3) Uani 1 1 d . . . H44B H 0.0429 0.4573 -0.0600 0.095 Uiso 1 1 calc R . . C45 C 0.4714(4) 0.9510(4) 0.06064(19) 0.0392(13) Uani 1 1 d . . . H45A H 0.5194 0.9747 0.0445 0.047 Uiso 1 1 calc R . . C45' C 0.0736(5) 0.5894(5) -0.0509(2) 0.0611(19) Uani 1 1 d . . . H45B H 0.0221 0.6129 -0.0687 0.073 Uiso 1 1 calc R . . C46 C 0.4249(3) 0.8744(4) 0.04519(18) 0.0351(12) Uani 1 1 d . . . H46A H 0.4418 0.8459 0.0179 0.042 Uiso 1 1 calc R . . C46' C 0.1370(4) 0.6455(4) -0.02926(18) 0.0391(12) Uani 1 1 d . . . H46B H 0.1288 0.7090 -0.0330 0.047 Uiso 1 1 calc R . . N51' N 0.4336(3) 0.5312(3) 0.07238(14) 0.0336(10) Uani 1 1 d . . . N51 N 0.1370(3) 0.7427(3) 0.12304(15) 0.0349(10) Uani 1 1 d . . . C52' C 0.3838(3) 0.5438(3) 0.03247(16) 0.0275(10) Uani 1 1 d . . . C52 C 0.1810(3) 0.8095(3) 0.10334(17) 0.0302(11) Uani 1 1 d . . . C53' C 0.4129(3) 0.5974(3) -0.00326(17) 0.0301(11) Uani 1 1 d . . . H53A H 0.3760 0.6050 -0.0314 0.036 Uiso 1 1 calc R . . C53 C 0.1476(4) 0.8509(4) 0.06190(18) 0.0350(12) Uani 1 1 d . . . H53B H 0.1797 0.8989 0.0488 0.042 Uiso 1 1 calc R . . C54' C 0.4969(4) 0.6390(4) 0.0035(2) 0.0379(12) Uani 1 1 d . . . H54A H 0.5180 0.6770 -0.0197 0.045 Uiso 1 1 calc R . . C54 C 0.0660(4) 0.8192(4) 0.04064(19) 0.0426(14) Uani 1 1 d . . . H54B H 0.0414 0.8454 0.0125 0.051 Uiso 1 1 calc R . . C55 C 0.0209(4) 0.7497(4) 0.0605(2) 0.0430(14) Uani 1 1 d . . . H55A H -0.0345 0.7265 0.0462 0.052 Uiso 1 1 calc R . . C55' C 0.5499(4) 0.6246(4) 0.0446(2) 0.0418(14) Uani 1 1 d . . . H55B H 0.6080 0.6518 0.0499 0.050 Uiso 1 1 calc R . . C56' C 0.5160(4) 0.5699(4) 0.07718(19) 0.0405(13) Uani 1 1 d . . . H56A H 0.5532 0.5588 0.1049 0.049 Uiso 1 1 calc R . . C56 C 0.0587(4) 0.7150(4) 0.10153(19) 0.0410(13) Uani 1 1 d . . . H56B H 0.0269 0.6680 0.1156 0.049 Uiso 1 1 calc R . . P1 P 0.23356(14) 0.01858(16) 0.30919(14) 0.1069(12) Uani 1 1 d . . . F1 F 0.2844(5) -0.0401(7) 0.2761(4) 0.251(7) Uani 1 1 d . A . F2 F 0.1537(3) 0.0178(4) 0.2661(2) 0.113(2) Uani 1 1 d . A 1 F3 F 0.2692(8) 0.1081(7) 0.2831(4) 0.228(6) Uani 1 1 d . A 1 F4 F 0.3130(5) 0.0207(7) 0.3454(5) 0.278(8) Uani 1 1 d . A . F5 F 0.1772(5) 0.0811(5) 0.3371(3) 0.152(3) Uani 1 1 d . A . F6 F 0.1851(8) -0.0606(6) 0.3308(3) 0.243(7) Uani 1 1 d . A . P2 P 0.70064(11) 0.16179(10) 0.08642(5) 0.0389(3) Uani 1 1 d . . . F7 F 0.7513(3) 0.1586(3) 0.04032(11) 0.0569(10) Uani 1 1 d . B . F8 F 0.6516(3) 0.1651(3) 0.13332(13) 0.0778(14) Uani 1 1 d . B . F9 F 0.6413(3) 0.0794(3) 0.06778(16) 0.0711(16) Uani 0.904(8) 1 d P B 1 F10 F 0.7707(3) 0.0899(4) 0.11024(13) 0.0649(16) Uani 0.904(8) 1 d P B 1 F11 F 0.6279(5) 0.2278(4) 0.06182(15) 0.098(3) Uani 0.904(8) 1 d P B 1 F12 F 0.7641(6) 0.2396(5) 0.10498(17) 0.138(4) Uani 0.904(8) 1 d P B 1 F9' F 0.700(3) 0.071(3) 0.0937(16) 0.064(13) Uiso 0.096(8) 1 d P B 2 F10' F 0.797(2) 0.160(3) 0.1110(13) 0.046(11) Uiso 0.096(8) 1 d P B 2 F11' F 0.599(3) 0.154(3) 0.0693(13) 0.053(12) Uiso 0.096(8) 1 d P B 2 F12' F 0.689(2) 0.271(2) 0.0827(14) 0.041(10) Uiso 0.096(8) 1 d P B 2 P3 P 0.74598(11) -0.14160(10) -0.00304(5) 0.0425(4) Uani 1 1 d . . . F13 F 0.7760(5) -0.1042(4) 0.04506(16) 0.123(2) Uani 1 1 d . C . F14 F 0.7123(6) -0.1825(5) -0.0516(2) 0.144(3) Uani 1 1 d D C . F15 F 0.7552(10) -0.0570(8) -0.0310(4) 0.076(4) Uani 0.554(17) 1 d P C 1 F16 F 0.7265(13) -0.2366(8) 0.0234(4) 0.107(7) Uani 0.554(17) 1 d P C 1 F17 F 0.8352(7) -0.1833(10) -0.0163(3) 0.084(4) Uani 0.554(17) 1 d P C 1 F18 F 0.6505(12) -0.1098(11) 0.0087(7) 0.137(7) Uani 0.554(17) 1 d P C 1 F15' F 0.8481(8) -0.0990(16) -0.0055(6) 0.129(8) Uani 0.446(17) 1 d P C 2 F16' F 0.6485(11) -0.1674(18) 0.0020(6) 0.151(11) Uani 0.446(17) 1 d PD C 2 F17' F 0.7937(19) -0.2315(9) 0.0088(9) 0.158(15) Uani 0.446(17) 1 d P C 2 F18' F 0.7150(17) -0.0401(10) -0.0157(7) 0.113(9) Uani 0.446(17) 1 d P C 2 O60 O 0.1865(9) 0.1720(5) 0.1961(3) 0.073(3) Uani 0.50 1 d P . . O70 O 0.1129(9) 0.1008(7) 0.1144(4) 0.089(4) Uani 0.50 1 d P . . O80 O 0.9312(7) 0.0432(7) 0.0506(4) 0.072(3) Uiso 0.50 1 d P . . O90 O 0.9728(11) 0.1562(13) 0.0949(6) 0.143(6) 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 0.02868(19) 0.0261(2) 0.0329(2) -0.00011(15) -0.00486(15) 0.00437(15) Ag2 0.0363(2) 0.0247(2) 0.02886(19) -0.00245(15) 0.00176(15) -0.00029(15) Ag3 0.0372(2) 0.0509(3) 0.0481(3) 0.0027(2) 0.01334(19) 0.0010(2) C1' 0.029(2) 0.034(3) 0.019(2) -0.0023(19) 0.0020(18) -0.007(2) C1 0.026(2) 0.028(3) 0.026(2) 0.005(2) 0.0013(19) -0.006(2) C2 0.029(2) 0.036(3) 0.019(2) -0.001(2) 0.0028(19) -0.010(2) C2' 0.044(3) 0.027(3) 0.037(3) -0.008(2) 0.012(2) -0.007(2) C3 0.030(2) 0.028(2) 0.024(2) -0.0035(19) 0.0016(19) -0.007(2) C3' 0.043(3) 0.028(3) 0.031(3) -0.005(2) 0.014(2) -0.009(2) C4 0.032(2) 0.026(2) 0.023(2) -0.0006(19) 0.0031(19) -0.007(2) C4' 0.031(2) 0.031(3) 0.022(2) 0.002(2) 0.0026(19) 0.000(2) C5' 0.042(3) 0.025(3) 0.029(2) -0.002(2) 0.002(2) -0.003(2) C5 0.041(3) 0.031(3) 0.019(2) 0.0005(19) 0.002(2) -0.002(2) C6' 0.032(3) 0.031(3) 0.026(2) 0.000(2) 0.003(2) -0.010(2) C6 0.038(3) 0.029(3) 0.024(2) -0.003(2) 0.004(2) -0.001(2) N11' 0.031(2) 0.034(2) 0.0215(19) -0.0019(17) 0.0054(16) -0.0074(18) C11 0.027(2) 0.033(3) 0.031(2) 0.004(2) -0.001(2) -0.006(2) C11' 0.030(2) 0.039(3) 0.029(2) -0.005(2) 0.004(2) -0.010(2) N11 0.035(2) 0.028(2) 0.0239(19) 0.0049(17) 0.0040(17) 0.0004(18) N14 0.035(2) 0.028(2) 0.024(2) -0.0019(17) -0.0004(17) 0.0015(18) N14' 0.035(2) 0.024(2) 0.0238(19) 0.0012(16) 0.0070(17) 0.0004(17) C14' 0.046(3) 0.019(2) 0.032(2) -0.001(2) 0.009(2) 0.003(2) C14 0.038(3) 0.030(3) 0.025(2) -0.005(2) 0.001(2) -0.001(2) N21 0.036(2) 0.035(2) 0.032(2) 0.0004(19) 0.0042(19) 0.0049(19) N21' 0.028(2) 0.037(2) 0.032(2) 0.0019(19) 0.0038(17) -0.0094(19) C22' 0.029(2) 0.034(3) 0.027(2) -0.001(2) 0.005(2) -0.011(2) C22 0.030(2) 0.028(3) 0.025(2) 0.0045(19) 0.0016(19) 0.006(2) C23' 0.055(3) 0.036(3) 0.032(3) -0.006(2) 0.018(3) -0.013(3) C23 0.038(3) 0.033(3) 0.032(3) 0.008(2) 0.006(2) 0.006(2) C24 0.047(3) 0.046(3) 0.031(3) 0.012(2) 0.014(2) 0.016(3) C24' 0.071(4) 0.048(4) 0.028(3) -0.005(3) 0.014(3) -0.025(3) C25' 0.046(3) 0.054(4) 0.035(3) 0.010(3) -0.004(3) -0.023(3) C25 0.056(4) 0.037(3) 0.033(3) 0.002(2) 0.004(3) 0.017(3) C26 0.045(3) 0.035(3) 0.035(3) -0.002(2) -0.002(2) 0.005(2) C26' 0.031(3) 0.045(3) 0.051(3) 0.009(3) -0.004(2) -0.011(2) N31 0.029(2) 0.025(2) 0.0242(19) 0.0034(16) -0.0018(16) 0.0035(16) N31' 0.0245(19) 0.028(2) 0.0249(19) 0.0023(16) 0.0047(16) 0.0014(16) C32' 0.022(2) 0.037(3) 0.024(2) -0.003(2) 0.0080(18) -0.001(2) C32 0.023(2) 0.029(3) 0.029(2) 0.006(2) -0.0008(19) 0.0013(19) C33 0.032(3) 0.031(3) 0.038(3) 0.005(2) 0.010(2) 0.010(2) C33' 0.024(2) 0.046(3) 0.035(3) -0.003(2) -0.003(2) 0.007(2) C34 0.041(3) 0.029(3) 0.041(3) 0.012(2) 0.009(2) 0.008(2) C34' 0.037(3) 0.050(4) 0.043(3) 0.002(3) -0.001(2) 0.019(3) C35' 0.030(3) 0.031(3) 0.042(3) -0.004(2) 0.007(2) 0.011(2) C35 0.037(3) 0.038(3) 0.027(2) 0.011(2) 0.003(2) 0.002(2) C36 0.033(3) 0.035(3) 0.023(2) 0.002(2) -0.001(2) 0.003(2) C36' 0.026(2) 0.033(3) 0.033(3) -0.005(2) 0.006(2) 0.001(2) N41' 0.031(2) 0.030(2) 0.0242(19) 0.0007(17) 0.0022(16) -0.0017(17) N41 0.029(2) 0.029(2) 0.027(2) 0.0021(17) -0.0025(17) 0.0012(17) C42 0.032(2) 0.026(3) 0.028(2) 0.005(2) -0.005(2) 0.006(2) C42' 0.043(3) 0.027(3) 0.025(2) 0.000(2) 0.005(2) -0.005(2) C43 0.046(3) 0.033(3) 0.030(3) -0.004(2) -0.002(2) 0.000(2) C43' 0.079(5) 0.033(3) 0.068(4) -0.004(3) -0.026(4) -0.009(3) C44 0.045(3) 0.033(3) 0.045(3) 0.006(3) -0.007(3) -0.010(2) C44' 0.083(6) 0.050(4) 0.094(6) 0.002(4) -0.045(5) -0.021(4) C45 0.036(3) 0.044(3) 0.037(3) 0.011(2) -0.004(2) -0.008(2) C45' 0.051(4) 0.058(4) 0.069(4) 0.007(3) -0.029(3) -0.004(3) C46 0.033(3) 0.039(3) 0.033(3) 0.006(2) 0.000(2) 0.000(2) C46' 0.039(3) 0.042(3) 0.036(3) 0.004(2) 0.000(2) 0.000(2) N51' 0.042(2) 0.033(2) 0.026(2) -0.0053(18) 0.0025(18) 0.0067(19) N51 0.038(2) 0.030(2) 0.037(2) -0.0031(19) 0.0058(19) -0.0024(19) C52' 0.039(3) 0.020(2) 0.024(2) -0.0033(18) 0.007(2) 0.004(2) C52 0.032(3) 0.027(3) 0.032(3) -0.004(2) 0.002(2) 0.006(2) C53' 0.035(3) 0.029(3) 0.028(2) -0.002(2) 0.010(2) 0.005(2) C53 0.034(3) 0.034(3) 0.036(3) 0.002(2) 0.003(2) 0.004(2) C54' 0.037(3) 0.034(3) 0.046(3) -0.003(2) 0.018(2) 0.002(2) C54 0.035(3) 0.056(4) 0.035(3) -0.005(3) -0.002(2) 0.011(3) C55 0.030(3) 0.057(4) 0.042(3) -0.011(3) 0.004(2) -0.002(3) C55' 0.036(3) 0.035(3) 0.055(3) -0.021(3) 0.007(3) 0.002(2) C56' 0.044(3) 0.043(3) 0.034(3) -0.013(2) 0.000(2) 0.008(3) C56 0.038(3) 0.044(3) 0.042(3) -0.006(3) 0.009(2) -0.007(3) P1 0.0414(11) 0.0558(13) 0.221(4) -0.0468(18) -0.0055(15) 0.0045(10) F1 0.109(5) 0.282(11) 0.342(13) -0.260(11) -0.103(7) 0.110(7) F2 0.054(3) 0.119(5) 0.168(6) 0.045(4) 0.022(3) 0.021(3) F3 0.293(14) 0.163(8) 0.248(11) -0.093(8) 0.133(11) -0.128(9) F4 0.090(5) 0.271(11) 0.443(17) -0.285(12) -0.143(7) 0.090(6) F5 0.110(5) 0.134(6) 0.213(8) 0.001(6) 0.028(5) 0.052(5) F6 0.348(14) 0.122(6) 0.220(9) 0.092(6) -0.193(10) -0.123(8) P2 0.0579(9) 0.0339(8) 0.0249(6) 0.0067(6) 0.0041(6) -0.0036(7) F7 0.073(2) 0.067(3) 0.0322(17) 0.0084(16) 0.0139(17) -0.007(2) F8 0.106(3) 0.091(3) 0.041(2) 0.031(2) 0.036(2) 0.054(3) F9 0.079(3) 0.066(3) 0.067(3) 0.004(2) 0.003(3) -0.036(3) F10 0.061(3) 0.095(4) 0.039(2) 0.023(2) 0.009(2) 0.025(3) F11 0.170(6) 0.090(5) 0.038(2) 0.026(3) 0.027(3) 0.088(5) F12 0.259(10) 0.108(5) 0.047(3) -0.016(3) 0.008(4) -0.131(6) P3 0.0587(9) 0.0350(8) 0.0342(7) -0.0019(6) 0.0064(7) 0.0088(7) F13 0.222(7) 0.078(4) 0.058(3) -0.019(3) -0.046(4) 0.013(4) F14 0.219(8) 0.120(5) 0.080(4) -0.050(4) -0.060(4) 0.087(5) F15 0.128(11) 0.039(6) 0.060(6) 0.019(5) -0.003(6) -0.031(6) F16 0.211(18) 0.048(6) 0.070(6) 0.013(4) 0.065(10) -0.013(8) F17 0.062(6) 0.104(11) 0.085(7) -0.002(6) 0.004(5) 0.037(6) F18 0.125(12) 0.116(12) 0.187(14) 0.005(11) 0.106(11) 0.041(10) F15' 0.060(8) 0.17(2) 0.157(15) -0.007(13) 0.023(8) -0.029(9) F16' 0.080(11) 0.21(3) 0.162(18) 0.072(18) -0.030(11) -0.081(14) F17' 0.22(3) 0.030(8) 0.19(3) -0.029(11) -0.15(2) 0.047(12) F18' 0.18(2) 0.058(8) 0.085(13) -0.007(8) -0.052(12) 0.063(11) O60 0.142(10) 0.021(4) 0.063(6) -0.008(4) 0.043(6) -0.032(5) O70 0.162(12) 0.054(6) 0.063(6) -0.008(5) 0.085(7) -0.024(7) O90 0.117(13) 0.171(17) 0.145(15) 0.016(13) 0.031(11) -0.039(12) _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 N31' 2.150(4) . ? Ag1 N31 2.157(4) . ? Ag2 N41 2.162(4) . ? Ag2 N41' 2.179(4) . ? Ag3 N21 2.195(4) . ? Ag3 N21' 2.202(4) . ? Ag3 O60 2.576(8) . ? C1' C2' 1.379(7) . ? C1' C6' 1.408(7) . ? C1' C11' 1.521(7) . ? C1 C6 1.399(6) . ? C1 C2 1.397(7) . ? C1 C11 1.514(7) . ? C2 C3 1.386(7) . ? C2' C3' 1.376(7) . ? C3 C4 1.400(6) . ? C3' C4' 1.387(7) . ? C4 C5 1.389(7) . ? C4 C14 1.511(7) . ? C4' C5' 1.392(7) . ? C4' C14' 1.506(7) . ? C5' C6' 1.384(7) . ? C5 C6 1.384(7) . ? N11' C32' 1.402(7) . ? N11' C22' 1.402(6) . ? N11' C11' 1.465(6) . ? C11 N11 1.483(6) . ? N11 C22 1.408(6) . ? N11 C32 1.417(6) . ? N14 C42 1.399(7) . ? N14 C52 1.412(6) . ? N14 C14 1.471(6) . ? N14' C42' 1.390(6) . ? N14' C52' 1.406(6) . ? N14' C14' 1.477(6) . ? N21 C22 1.333(7) . ? N21 C26 1.350(7) . ? N21' C22' 1.347(7) . ? N21' C26' 1.351(7) . ? C22' C23' 1.397(7) . ? C22 C23 1.400(7) . ? C23' C24' 1.390(8) . ? C23 C24 1.375(8) . ? C24 C25 1.390(9) . ? C24' C25' 1.354(9) . ? C25' C26' 1.386(9) . ? C25 C26 1.372(8) . ? N31 C32 1.347(6) . ? N31 C36 1.355(6) . ? N31' C32' 1.343(6) . ? N31' C36' 1.359(6) . ? C32' C33' 1.399(7) . ? C32 C33 1.387(7) . ? C33 C34 1.376(7) . ? C33' C34' 1.377(8) . ? C34 C35 1.383(8) . ? C34' C35' 1.379(8) . ? C35' C36' 1.367(7) . ? C35 C36 1.380(7) . ? N41' C46' 1.337(7) . ? N41' C42' 1.343(6) . ? N41 C46 1.355(7) . ? N41 C42 1.355(6) . ? C42 C43 1.377(7) . ? C42' C43' 1.396(8) . ? C43 C44 1.390(8) . ? C43' C44' 1.382(10) . ? C44 C45 1.366(8) . ? C44' C45' 1.364(10) . ? C45 C46 1.379(8) . ? C45' C46' 1.364(8) . ? N51' C52' 1.333(6) . ? N51' C56' 1.343(7) . ? N51 C56 1.332(7) . ? N51 C52 1.337(7) . ? C52' C53' 1.402(7) . ? C52 C53 1.402(7) . ? C53' C54' 1.385(7) . ? C53 C54 1.390(8) . ? C54' C55' 1.387(8) . ? C54 C55 1.377(9) . ? C55 C56 1.373(8) . ? C55' C56' 1.372(9) . ? P1 F4 1.509(8) . ? P1 F5 1.523(7) . ? P1 F6 1.534(9) . ? P1 F1 1.538(8) . ? P1 F3 1.633(10) . ? P1 F2 1.646(7) . ? P2 F9' 1.36(5) . ? P2 F10' 1.54(4) . ? P2 F11' 1.54(4) . ? P2 F12 1.550(5) . ? P2 F9 1.570(5) . ? P2 F11 1.577(5) . ? P2 F7 1.590(4) . ? P2 F8 1.598(4) . ? P2 F10 1.599(4) . ? P2 F12' 1.62(4) . ? P3 F15 1.502(10) . ? P3 F16' 1.511(14) . ? P3 F17' 1.529(12) . ? P3 F13 1.533(5) . ? P3 F17 1.534(9) . ? P3 F18 1.554(12) . ? P3 F14 1.575(5) . ? P3 F18' 1.601(14) . ? P3 F16 1.636(10) . ? P3 F15' 1.643(13) . ? 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 N31' Ag1 N31 163.93(15) . . ? N41 Ag2 N41' 172.70(15) . . ? N21 Ag3 N21' 150.30(15) . . ? N21 Ag3 O60 95.4(3) . . ? N21' Ag3 O60 103.3(2) . . ? C2' C1' C6' 118.2(4) . . ? C2' C1' C11' 122.0(5) . . ? C6' C1' C11' 119.7(4) . . ? C6 C1 C2 118.3(4) . . ? C6 C1 C11 121.4(4) . . ? C2 C1 C11 120.3(4) . . ? C3 C2 C1 120.9(4) . . ? C3' C2' C1' 120.4(5) . . ? C2 C3 C4 120.8(5) . . ? C2' C3' C4' 122.1(5) . . ? C5 C4 C3 118.0(5) . . ? C5 C4 C14 123.1(4) . . ? C3 C4 C14 118.9(4) . . ? C3' C4' C5' 118.1(4) . . ? C3' C4' C14' 120.9(4) . . ? C5' C4' C14' 121.0(4) . . ? C6' C5' C4' 120.1(5) . . ? C6 C5 C4 121.6(4) . . ? C5' C6' C1' 121.1(5) . . ? C5 C6 C1 120.4(5) . . ? C32' N11' C22' 119.9(4) . . ? C32' N11' C11' 121.4(4) . . ? C22' N11' C11' 117.5(4) . . ? N11 C11 C1 114.3(4) . . ? N11' C11' C1' 114.6(4) . . ? C22 N11 C32 119.3(4) . . ? C22 N11 C11 120.4(4) . . ? C32 N11 C11 116.3(4) . . ? C42 N14 C52 121.9(4) . . ? C42 N14 C14 119.5(4) . . ? C52 N14 C14 118.6(4) . . ? C42' N14' C52' 123.3(4) . . ? C42' N14' C14' 117.5(4) . . ? C52' N14' C14' 119.1(4) . . ? N14' C14' C4' 113.0(4) . . ? N14 C14 C4 114.8(4) . . ? C22 N21 C26 118.6(5) . . ? C22 N21 Ag3 123.4(3) . . ? C26 N21 Ag3 117.0(4) . . ? C22' N21' C26' 118.1(5) . . ? C22' N21' Ag3 126.0(3) . . ? C26' N21' Ag3 114.7(4) . . ? N21' C22' C23' 121.8(5) . . ? N21' C22' N11' 116.9(4) . . ? C23' C22' N11' 121.2(5) . . ? N21 C22 C23 121.6(5) . . ? N21 C22 N11 116.3(4) . . ? C23 C22 N11 122.1(5) . . ? C24' C23' C22' 118.2(6) . . ? C24 C23 C22 118.8(5) . . ? C23 C24 C25 119.8(5) . . ? C25' C24' C23' 120.4(5) . . ? C24' C25' C26' 118.5(5) . . ? C26 C25 C24 117.8(5) . . ? N21 C26 C25 123.3(5) . . ? N21' C26' C25' 122.9(6) . . ? C32 N31 C36 118.6(4) . . ? C32 N31 Ag1 121.8(3) . . ? C36 N31 Ag1 114.1(3) . . ? C32' N31' C36' 118.7(4) . . ? C32' N31' Ag1 121.8(3) . . ? C36' N31' Ag1 117.0(3) . . ? N31' C32' C33' 121.1(5) . . ? N31' C32' N11' 115.9(4) . . ? C33' C32' N11' 123.0(4) . . ? N31 C32 C33 121.6(4) . . ? N31 C32 N11 115.9(4) . . ? C33 C32 N11 122.4(5) . . ? C34 C33 C32 119.1(5) . . ? C34' C33' C32' 118.5(5) . . ? C33 C34 C35 119.7(5) . . ? C33' C34' C35' 120.5(5) . . ? C36' C35' C34' 118.0(5) . . ? C36 C35 C34 118.5(5) . . ? N31 C36 C35 122.3(5) . . ? N31' C36' C35' 122.7(5) . . ? C46' N41' C42' 118.8(5) . . ? C46' N41' Ag2 115.4(4) . . ? C42' N41' Ag2 125.7(3) . . ? C46 N41 C42 118.0(4) . . ? C46 N41 Ag2 116.5(3) . . ? C42 N41 Ag2 125.3(3) . . ? N41 C42 C43 121.3(5) . . ? N41 C42 N14 117.2(4) . . ? C43 C42 N14 121.5(5) . . ? N41' C42' N14' 119.1(4) . . ? N41' C42' C43' 120.3(5) . . ? N14' C42' C43' 120.5(5) . . ? C42 C43 C44 119.6(5) . . ? C44' C43' C42' 119.1(6) . . ? C45 C44 C43 119.7(5) . . ? C45' C44' C43' 120.0(6) . . ? C44 C45 C46 118.2(5) . . ? C44' C45' C46' 117.9(6) . . ? N41 C46 C45 123.2(5) . . ? N41' C46' C45' 123.8(6) . . ? C52' N51' C56' 117.4(5) . . ? C56 N51 C52 117.4(5) . . ? N51' C52' C53' 122.8(5) . . ? N51' C52' N14' 115.8(4) . . ? C53' C52' N14' 121.4(4) . . ? N51 C52 C53 122.8(5) . . ? N51 C52 N14 116.2(4) . . ? C53 C52 N14 121.0(5) . . ? C54' C53' C52' 118.3(5) . . ? C54 C53 C52 117.6(5) . . ? C53' C54' C55' 119.2(5) . . ? C55 C54 C53 119.9(5) . . ? C56 C55 C54 117.7(5) . . ? C56' C55' C54' 118.2(5) . . ? N51' C56' C55' 124.1(5) . . ? N51 C56 C55 124.6(5) . . ? F4 P1 F5 92.7(5) . . ? F4 P1 F6 95.4(7) . . ? F5 P1 F6 87.0(7) . . ? F4 P1 F1 93.1(4) . . ? F5 P1 F1 173.5(6) . . ? F6 P1 F1 95.6(7) . . ? F4 P1 F3 92.5(7) . . ? F5 P1 F3 88.3(5) . . ? F6 P1 F3 171.0(7) . . ? F1 P1 F3 88.4(7) . . ? F4 P1 F2 174.6(7) . . ? F5 P1 F2 91.1(4) . . ? F6 P1 F2 88.6(3) . . ? F1 P1 F2 83.0(4) . . ? F3 P1 F2 83.8(5) . . ? F9' P2 F10' 86(3) . . ? F9' P2 F11' 88(3) . . ? F10' P2 F11' 170(2) . . ? F9' P2 F12 133(2) . . ? F10' P2 F12 48.7(16) . . ? F11' P2 F12 135.2(17) . . ? F9' P2 F9 44(2) . . ? F10' P2 F9 128.2(17) . . ? F11' P2 F9 48.1(16) . . ? F12 P2 F9 176.7(5) . . ? F9' P2 F11 132(2) . . ? F10' P2 F11 142.0(18) . . ? F11' P2 F11 45.0(16) . . ? F12 P2 F11 94.0(4) . . ? F9 P2 F11 89.0(3) . . ? F9' P2 F7 96.3(19) . . ? F10' P2 F7 84.6(14) . . ? F11' P2 F7 103.9(15) . . ? F12 P2 F7 90.0(3) . . ? F9 P2 F7 88.6(2) . . ? F11 P2 F7 89.3(2) . . ? F9' P2 F8 83.7(19) . . ? F10' P2 F8 94.2(14) . . ? F11' P2 F8 77.2(15) . . ? F12 P2 F8 89.2(3) . . ? F9 P2 F8 92.1(3) . . ? F11 P2 F8 91.5(2) . . ? F7 P2 F8 178.9(3) . . ? F9' P2 F10 45(2) . . ? F10' P2 F10 41.4(17) . . ? F11' P2 F10 131.8(17) . . ? F12 P2 F10 89.5(4) . . ? F9 P2 F10 87.6(3) . . ? F11 P2 F10 176.6(4) . . ? F7 P2 F10 90.6(2) . . ? F8 P2 F10 88.6(2) . . ? F9' P2 F12' 172(2) . . ? F10' P2 F12' 97(2) . . ? F11' P2 F12' 88(2) . . ? F12 P2 F12' 48.9(13) . . ? F9 P2 F12' 134.1(14) . . ? F11 P2 F12' 45.1(13) . . ? F7 P2 F12' 91.5(13) . . ? F8 P2 F12' 88.6(13) . . ? F10 P2 F12' 138.3(14) . . ? F15 P3 F16' 113.2(10) . . ? F15 P3 F17' 141.5(15) . . ? F16' P3 F17' 100.6(14) . . ? F15 P3 F13 99.3(5) . . ? F16' P3 F13 101.9(8) . . ? F17' P3 F13 90.8(7) . . ? F15 P3 F17 94.5(8) . . ? F16' P3 F17 140.5(11) . . ? F17' P3 F17 47.0(12) . . ? F13 P3 F17 100.6(5) . . ? F15 P3 F18 89.6(8) . . ? F16' P3 F18 33.0(9) . . ? F17' P3 F18 128.5(14) . . ? F13 P3 F18 83.6(9) . . ? F17 P3 F18 173.5(9) . . ? F15 P3 F14 82.6(5) . . ? F16' P3 F14 76.0(7) . . ? F17' P3 F14 88.5(7) . . ? F13 P3 F14 177.7(5) . . ? F17 P3 F14 80.5(5) . . ? F18 P3 F14 95.0(8) . . ? F15 P3 F18' 30.1(8) . . ? F16' P3 F18' 90.1(12) . . ? F17' P3 F18' 169.2(14) . . ? F13 P3 F18' 85.8(7) . . ? F17 P3 F18' 123.6(11) . . ? F18 P3 F18' 61.3(10) . . ? F14 P3 F18' 95.2(7) . . ? F15 P3 F16 173.7(8) . . ? F16' P3 F16 62.0(10) . . ? F17' P3 F16 41.1(12) . . ? F13 P3 F16 85.9(6) . . ? F17 P3 F16 88.0(7) . . ? F18 P3 F16 87.4(8) . . ? F14 P3 F16 92.1(6) . . ? F18' P3 F16 148.4(11) . . ? F15 P3 F15' 62.1(8) . . ? F16' P3 F15' 171.6(11) . . ? F17' P3 F15' 86.2(12) . . ? F13 P3 F15' 72.9(7) . . ? F17 P3 F15' 47.9(7) . . ? F18 P3 F15' 138.6(10) . . ? F14 P3 F15' 109.2(7) . . ? F18' P3 F15' 82.9(11) . . ? F16 P3 F15' 123.2(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.604 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.115 #END data_ab5 _database_code_depnum_ccdc_archive 'CCDC 614174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Ag Cl N8 O4' _chemical_formula_weight 733.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 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 8.522(1) _cell_length_b 22.118(1) _cell_length_c 17.633(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.41(1) _cell_angle_gamma 90.00 _cell_volume 3233.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 285 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 21.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7885 _exptl_absorpt_correction_T_max 0.9282 _exptl_absorpt_process_details 'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73465 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7770 _reflns_number_gt 6170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal-99 (E.Keller 1999)' _computing_publication_material 'XCIF 6.12 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+1.7272P] 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 7770 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.042 _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 0.975316(16) 0.761827(6) 0.053760(8) 0.02951(5) Uani 1 1 d . . . N1 N 1.19141(17) 0.75460(6) 0.15310(9) 0.0248(3) Uani 1 1 d . . . C2 C 1.2244(2) 0.69995(9) 0.18677(11) 0.0319(4) Uani 1 1 d . . . H2 H 1.1714 0.6655 0.1604 0.038 Uiso 1 1 calc R . . C3 C 1.3313(3) 0.69157(9) 0.25758(12) 0.0378(5) Uani 1 1 d . . . H3 H 1.3512 0.6524 0.2798 0.045 Uiso 1 1 calc R . . C4 C 1.4088(3) 0.74172(10) 0.29551(12) 0.0389(5) Uani 1 1 d . . . H4 H 1.4823 0.7374 0.3447 0.047 Uiso 1 1 calc R . . C5 C 1.3790(2) 0.79797(9) 0.26163(11) 0.0326(4) Uani 1 1 d . . . H5 H 1.4323 0.8327 0.2870 0.039 Uiso 1 1 calc R . . C6 C 1.2691(2) 0.80321(8) 0.18926(10) 0.0235(3) Uani 1 1 d . . . N7 N 1.23285(16) 0.85963(6) 0.15456(8) 0.0223(3) Uani 1 1 d . . . C8 C 1.2009(2) 0.86872(8) 0.07320(10) 0.0233(3) Uani 1 1 d . . . N9 N 1.12204(18) 0.91951(7) 0.04679(9) 0.0285(3) Uani 1 1 d . . . C10 C 1.0915(2) 0.93007(9) -0.03004(11) 0.0356(4) Uani 1 1 d . . . H10 H 1.0351 0.9661 -0.0491 0.043 Uiso 1 1 calc R . . C11 C 1.1366(3) 0.89221(10) -0.08304(11) 0.0414(5) Uani 1 1 d . . . H11 H 1.1106 0.9013 -0.1372 0.050 Uiso 1 1 calc R . . C12 C 1.2211(3) 0.84030(10) -0.05487(12) 0.0407(5) Uani 1 1 d . . . H12 H 1.2553 0.8133 -0.0897 0.049 Uiso 1 1 calc R . . C13 C 1.2556(2) 0.82797(9) 0.02422(11) 0.0309(4) Uani 1 1 d . . . H13 H 1.3147 0.7929 0.0447 0.037 Uiso 1 1 calc R . . C14 C 1.2446(2) 0.91299(8) 0.20467(10) 0.0246(4) Uani 1 1 d . . . H14A H 1.2237 0.9006 0.2554 0.030 Uiso 1 1 calc R . . H14B H 1.1591 0.9419 0.1804 0.030 Uiso 1 1 calc R . . C15 C 1.40605(19) 0.94507(7) 0.21957(9) 0.0206(3) Uani 1 1 d . . . C16 C 1.53214(19) 0.92484(7) 0.18806(9) 0.0198(3) Uani 1 1 d . . . H16 H 1.5191 0.8889 0.1578 0.024 Uiso 1 1 calc R . . C17 C 1.67672(19) 0.95647(7) 0.20024(9) 0.0197(3) Uani 1 1 d . . . C18 C 1.6945(2) 1.00952(8) 0.24411(10) 0.0241(3) Uani 1 1 d . . . H18 H 1.7916 1.0322 0.2516 0.029 Uiso 1 1 calc R . . C19 C 1.5707(2) 1.02916(8) 0.27674(10) 0.0275(4) Uani 1 1 d . . . H19 H 1.5842 1.0648 0.3076 0.033 Uiso 1 1 calc R . . C20 C 1.4272(2) 0.99723(8) 0.26468(10) 0.0262(4) Uani 1 1 d . . . H20 H 1.3429 1.0111 0.2873 0.031 Uiso 1 1 calc R . . N21 N 0.79111(17) 0.83561(7) 0.00377(8) 0.0248(3) Uani 1 1 d . . . C22 C 0.7530(2) 0.83908(9) -0.07458(11) 0.0323(4) Uani 1 1 d . . . H22 H 0.7821 0.8062 -0.1033 0.039 Uiso 1 1 calc R . . C23 C 0.6747(2) 0.88734(10) -0.11525(11) 0.0378(5) Uani 1 1 d . . . H23 H 0.6524 0.8885 -0.1706 0.045 Uiso 1 1 calc R . . C24 C 0.6292(2) 0.93445(10) -0.07318(12) 0.0374(5) Uani 1 1 d . . . H24 H 0.5750 0.9687 -0.0994 0.045 Uiso 1 1 calc R . . C25 C 0.6629(2) 0.93122(9) 0.00673(11) 0.0320(4) Uani 1 1 d . . . H25 H 0.6302 0.9628 0.0362 0.038 Uiso 1 1 calc R . . C26 C 0.74587(19) 0.88098(8) 0.04434(10) 0.0230(3) Uani 1 1 d . . . N27 N 0.78952(17) 0.87795(6) 0.12551(8) 0.0226(3) Uani 1 1 d . . . C28 C 0.8112(2) 0.82257(8) 0.16687(10) 0.0251(4) Uani 1 1 d . . . N29 N 0.9114(2) 0.82450(7) 0.23703(9) 0.0332(4) Uani 1 1 d . . . C30 C 0.9380(3) 0.77249(10) 0.27739(12) 0.0428(5) Uani 1 1 d . . . H30 H 1.0087 0.7733 0.3277 0.051 Uiso 1 1 calc R . . C31 C 0.8691(3) 0.71834(10) 0.25026(13) 0.0466(6) Uani 1 1 d . . . H31 H 0.8953 0.6824 0.2799 0.056 Uiso 1 1 calc R . . C32 C 0.7606(3) 0.71736(10) 0.17878(13) 0.0418(5) Uani 1 1 d . . . H32 H 0.7084 0.6807 0.1591 0.050 Uiso 1 1 calc R . . C33 C 0.7286(2) 0.77019(8) 0.13606(12) 0.0321(4) Uani 1 1 d . . . H33 H 0.6526 0.7709 0.0872 0.039 Uiso 1 1 calc R . . C34 C 0.8188(2) 0.93415(8) 0.16991(10) 0.0241(3) Uani 1 1 d . . . H34A H 0.8489 0.9659 0.1363 0.029 Uiso 1 1 calc R . . H34B H 0.9118 0.9281 0.2147 0.029 Uiso 1 1 calc R . . N35 N 0.9021(3) 0.68606(9) -0.03056(11) 0.0530(5) Uani 1 1 d . . . C36 C 0.8517(3) 0.64190(10) -0.05783(11) 0.0387(5) Uani 1 1 d . . . C37 C 0.7880(3) 0.58549(10) -0.09375(14) 0.0522(6) Uani 1 1 d . . . H37A H 0.7144 0.5937 -0.1443 0.078 Uiso 1 1 calc R . . H37B H 0.7293 0.5645 -0.0598 0.078 Uiso 1 1 calc R . . H37C H 0.8770 0.5600 -0.1015 0.078 Uiso 1 1 calc R . . Cl1 Cl 1.09854(5) 0.45042(2) -0.13452(3) 0.03319(10) Uani 1 1 d . . . O1 O 1.0930(2) 0.51425(7) -0.14834(10) 0.0493(4) Uani 1 1 d . . . O2 O 0.9766(2) 0.43403(9) -0.09493(11) 0.0618(5) Uani 1 1 d . . . O3 O 1.0690(2) 0.42050(8) -0.20864(10) 0.0597(5) Uani 1 1 d . . . O4 O 1.25517(18) 0.43383(9) -0.08967(10) 0.0567(5) Uani 1 1 d . . . N38 N 1.4350(5) 0.69583(15) -0.0188(2) 0.1046(10) Uani 1 1 d . . . C39 C 1.3929(4) 0.64789(15) -0.01080(17) 0.0656(7) Uani 1 1 d . . . C40 C 1.3451(4) 0.58623(15) 0.00169(19) 0.0756(9) Uani 1 1 d . . . H40A H 1.4364 0.5647 0.0346 0.113 Uiso 1 1 calc R . . H40B H 1.3117 0.5655 -0.0486 0.113 Uiso 1 1 calc R . . H40C H 1.2549 0.5869 0.0275 0.113 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 0.02801(7) 0.02571(7) 0.03163(8) -0.00543(6) 0.00044(5) 0.00253(6) N1 0.0229(7) 0.0238(8) 0.0283(7) 0.0003(6) 0.0072(6) 0.0006(6) C2 0.0353(10) 0.0244(9) 0.0372(10) 0.0011(8) 0.0109(8) 0.0019(8) C3 0.0448(12) 0.0307(10) 0.0373(10) 0.0102(9) 0.0086(9) 0.0082(9) C4 0.0377(10) 0.0454(12) 0.0305(10) 0.0094(9) 0.0014(8) 0.0050(9) C5 0.0307(10) 0.0354(11) 0.0290(9) 0.0027(8) 0.0016(8) -0.0050(8) C6 0.0197(8) 0.0274(9) 0.0251(8) 0.0005(7) 0.0085(7) -0.0011(7) N7 0.0202(7) 0.0231(7) 0.0233(7) 0.0003(6) 0.0046(6) -0.0024(6) C8 0.0186(8) 0.0262(9) 0.0254(8) 0.0010(7) 0.0057(6) -0.0066(7) N9 0.0287(8) 0.0245(8) 0.0312(8) 0.0037(6) 0.0049(6) -0.0038(6) C10 0.0380(11) 0.0306(10) 0.0357(10) 0.0098(8) 0.0037(8) -0.0060(8) C11 0.0528(13) 0.0443(13) 0.0261(9) 0.0075(9) 0.0068(9) -0.0102(10) C12 0.0517(13) 0.0435(12) 0.0317(10) -0.0032(9) 0.0199(9) -0.0039(10) C13 0.0310(9) 0.0332(10) 0.0315(9) 0.0017(8) 0.0131(8) 0.0000(8) C14 0.0192(8) 0.0282(9) 0.0281(8) -0.0041(7) 0.0088(7) -0.0006(7) C15 0.0196(8) 0.0216(8) 0.0206(7) 0.0022(6) 0.0050(6) 0.0005(6) C16 0.0202(8) 0.0175(8) 0.0214(8) -0.0015(6) 0.0042(6) 0.0000(6) C17 0.0187(8) 0.0201(8) 0.0192(7) 0.0034(6) 0.0022(6) 0.0013(6) C18 0.0251(8) 0.0218(8) 0.0230(8) 0.0002(7) 0.0007(7) -0.0048(7) C19 0.0346(10) 0.0224(9) 0.0244(8) -0.0067(7) 0.0047(7) -0.0022(7) C20 0.0271(9) 0.0280(9) 0.0257(8) -0.0023(7) 0.0107(7) 0.0029(7) N21 0.0220(7) 0.0242(8) 0.0272(7) -0.0003(6) 0.0039(6) 0.0013(6) C22 0.0327(10) 0.0341(10) 0.0279(9) -0.0050(8) 0.0026(8) 0.0020(8) C23 0.0401(11) 0.0430(12) 0.0264(9) 0.0040(9) -0.0005(8) 0.0042(9) C24 0.0359(10) 0.0371(11) 0.0370(10) 0.0119(9) 0.0038(8) 0.0110(9) C25 0.0295(9) 0.0306(10) 0.0368(10) 0.0045(8) 0.0092(8) 0.0082(8) C26 0.0173(8) 0.0233(8) 0.0289(8) 0.0024(7) 0.0066(7) -0.0002(6) N27 0.0229(7) 0.0211(7) 0.0252(7) 0.0012(6) 0.0081(6) 0.0034(6) C28 0.0255(8) 0.0254(9) 0.0287(9) 0.0038(7) 0.0156(7) 0.0058(7) N29 0.0413(9) 0.0347(9) 0.0255(8) 0.0027(7) 0.0114(7) 0.0113(7) C30 0.0610(14) 0.0430(13) 0.0285(10) 0.0081(9) 0.0187(10) 0.0181(10) C31 0.0734(16) 0.0338(11) 0.0416(12) 0.0151(10) 0.0318(12) 0.0187(11) C32 0.0538(13) 0.0260(10) 0.0537(13) 0.0051(9) 0.0291(11) 0.0000(9) C33 0.0317(10) 0.0301(10) 0.0385(10) 0.0029(8) 0.0164(8) -0.0005(8) C34 0.0197(8) 0.0229(9) 0.0302(9) -0.0004(7) 0.0070(7) -0.0013(7) N35 0.0804(15) 0.0362(11) 0.0405(10) -0.0104(9) 0.0100(10) -0.0076(10) C36 0.0540(13) 0.0335(11) 0.0277(9) -0.0047(9) 0.0079(9) 0.0019(10) C37 0.0702(16) 0.0380(13) 0.0445(13) -0.0154(10) 0.0054(12) -0.0064(11) Cl1 0.0263(2) 0.0361(2) 0.0360(2) 0.00660(19) 0.00497(18) -0.00105(18) O1 0.0514(9) 0.0336(8) 0.0635(10) 0.0032(7) 0.0144(8) -0.0033(7) O2 0.0411(9) 0.0812(13) 0.0676(11) 0.0289(10) 0.0217(8) -0.0038(9) O3 0.0572(10) 0.0608(11) 0.0548(10) -0.0217(9) 0.0001(8) 0.0121(9) O4 0.0309(8) 0.0765(12) 0.0565(10) 0.0208(9) -0.0026(7) 0.0050(8) N38 0.128(3) 0.065(2) 0.115(3) 0.0016(18) 0.017(2) 0.0034(19) C39 0.0680(18) 0.0615(19) 0.0632(17) -0.0078(14) 0.0071(14) 0.0035(15) C40 0.0687(19) 0.078(2) 0.075(2) -0.0018(16) 0.0064(16) -0.0161(16) _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 N35 2.2311(19) . ? Ag1 N1 2.2336(15) . ? Ag1 N21 2.2941(14) . ? N1 C6 1.343(2) . ? N1 C2 1.347(2) . ? C2 C3 1.377(3) . ? C3 C4 1.382(3) . ? C4 C5 1.378(3) . ? C5 C6 1.402(2) . ? C6 N7 1.393(2) . ? N7 C8 1.411(2) . ? N7 C14 1.464(2) . ? C8 N9 1.336(2) . ? C8 C13 1.401(3) . ? N9 C10 1.339(2) . ? C10 C11 1.374(3) . ? C11 C12 1.385(3) . ? C12 C13 1.384(3) . ? C14 C15 1.516(2) . ? C15 C20 1.389(2) . ? C15 C16 1.393(2) . ? C16 C17 1.390(2) . ? C17 C18 1.394(2) . ? C17 C34 1.515(2) 1_655 ? C18 C19 1.383(2) . ? C19 C20 1.385(3) . ? N21 C26 1.340(2) . ? N21 C22 1.346(2) . ? C22 C23 1.370(3) . ? C23 C24 1.386(3) . ? C24 C25 1.373(3) . ? C25 C26 1.399(2) . ? C26 N27 1.394(2) . ? N27 C28 1.416(2) . ? N27 C34 1.460(2) . ? C28 N29 1.331(2) . ? C28 C33 1.398(3) . ? N29 C30 1.344(3) . ? C30 C31 1.370(3) . ? C31 C32 1.380(3) . ? C32 C33 1.383(3) . ? C34 C17 1.515(2) 1_455 ? N35 C36 1.129(3) . ? C36 C37 1.447(3) . ? Cl1 O2 1.4266(16) . ? Cl1 O1 1.4315(16) . ? Cl1 O4 1.4326(15) . ? Cl1 O3 1.4342(17) . ? N38 C39 1.139(4) . ? C39 C40 1.455(4) . ? 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 N35 Ag1 N1 121.40(7) . . ? N35 Ag1 N21 102.57(7) . . ? N1 Ag1 N21 135.93(5) . . ? C6 N1 C2 118.64(16) . . ? C6 N1 Ag1 122.74(11) . . ? C2 N1 Ag1 117.37(12) . . ? N1 C2 C3 123.17(18) . . ? C2 C3 C4 118.18(19) . . ? C5 C4 C3 119.71(19) . . ? C4 C5 C6 119.09(18) . . ? N1 C6 N7 118.30(15) . . ? N1 C6 C5 121.17(16) . . ? N7 C6 C5 120.48(16) . . ? C6 N7 C8 123.04(14) . . ? C6 N7 C14 118.69(14) . . ? C8 N7 C14 117.96(14) . . ? N9 C8 C13 122.59(16) . . ? N9 C8 N7 115.90(15) . . ? C13 C8 N7 121.46(16) . . ? C8 N9 C10 117.58(17) . . ? N9 C10 C11 124.22(19) . . ? C10 C11 C12 117.73(18) . . ? C13 C12 C11 119.74(19) . . ? C12 C13 C8 118.10(18) . . ? N7 C14 C15 114.49(13) . . ? C20 C15 C16 119.06(15) . . ? C20 C15 C14 118.67(14) . . ? C16 C15 C14 122.25(15) . . ? C17 C16 C15 121.00(15) . . ? C16 C17 C18 119.19(15) . . ? C16 C17 C34 122.27(15) . 1_655 ? C18 C17 C34 118.51(15) . 1_655 ? C19 C18 C17 120.00(16) . . ? C18 C19 C20 120.48(16) . . ? C19 C20 C15 120.25(16) . . ? C26 N21 C22 118.34(15) . . ? C26 N21 Ag1 125.71(11) . . ? C22 N21 Ag1 114.55(12) . . ? N21 C22 C23 123.63(18) . . ? C22 C23 C24 117.94(18) . . ? C25 C24 C23 119.50(18) . . ? C24 C25 C26 119.35(18) . . ? N21 C26 N27 118.08(15) . . ? N21 C26 C25 121.21(16) . . ? N27 C26 C25 120.67(16) . . ? C26 N27 C28 122.84(14) . . ? C26 N27 C34 118.77(14) . . ? C28 N27 C34 118.36(14) . . ? N29 C28 C33 122.99(17) . . ? N29 C28 N27 115.47(16) . . ? C33 C28 N27 121.52(16) . . ? C28 N29 C30 117.23(18) . . ? N29 C30 C31 123.9(2) . . ? C30 C31 C32 118.3(2) . . ? C31 C32 C33 119.3(2) . . ? C32 C33 C28 118.1(2) . . ? N27 C34 C17 114.57(14) . 1_455 ? C36 N35 Ag1 162.51(19) . . ? N35 C36 C37 179.2(2) . . ? O2 Cl1 O1 109.59(11) . . ? O2 Cl1 O4 110.86(10) . . ? O1 Cl1 O4 109.64(10) . . ? O2 Cl1 O3 109.56(12) . . ? O1 Cl1 O3 107.93(11) . . ? O4 Cl1 O3 109.21(11) . . ? N38 C39 C40 177.7(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 N35 Ag1 N1 C6 158.16(13) . . . . ? N21 Ag1 N1 C6 -17.63(16) . . . . ? N35 Ag1 N1 C2 -34.83(15) . . . . ? N21 Ag1 N1 C2 149.39(12) . . . . ? C6 N1 C2 C3 1.6(3) . . . . ? Ag1 N1 C2 C3 -165.93(15) . . . . ? N1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 -0.7(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C2 N1 C6 N7 -179.23(15) . . . . ? Ag1 N1 C6 N7 -12.4(2) . . . . ? C2 N1 C6 C5 -1.8(2) . . . . ? Ag1 N1 C6 C5 165.04(13) . . . . ? C4 C5 C6 N1 0.8(3) . . . . ? C4 C5 C6 N7 178.13(17) . . . . ? N1 C6 N7 C8 -37.7(2) . . . . ? C5 C6 N7 C8 144.91(17) . . . . ? N1 C6 N7 C14 148.92(15) . . . . ? C5 C6 N7 C14 -28.5(2) . . . . ? C6 N7 C8 N9 160.44(15) . . . . ? C14 N7 C8 N9 -26.1(2) . . . . ? C6 N7 C8 C13 -22.3(2) . . . . ? C14 N7 C8 C13 151.21(16) . . . . ? C13 C8 N9 C10 1.9(3) . . . . ? N7 C8 N9 C10 179.12(15) . . . . ? C8 N9 C10 C11 -0.2(3) . . . . ? N9 C10 C11 C12 -1.1(3) . . . . ? C10 C11 C12 C13 0.7(3) . . . . ? C11 C12 C13 C8 0.8(3) . . . . ? N9 C8 C13 C12 -2.2(3) . . . . ? N7 C8 C13 C12 -179.29(17) . . . . ? C6 N7 C14 C15 93.20(18) . . . . ? C8 N7 C14 C15 -80.57(18) . . . . ? N7 C14 C15 C20 178.18(15) . . . . ? N7 C14 C15 C16 -0.2(2) . . . . ? C20 C15 C16 C17 -0.9(2) . . . . ? C14 C15 C16 C17 177.50(15) . . . . ? C15 C16 C17 C18 -0.6(2) . . . . ? C15 C16 C17 C34 177.13(15) . . . 1_655 ? C16 C17 C18 C19 1.8(2) . . . . ? C34 C17 C18 C19 -176.01(15) 1_655 . . . ? C17 C18 C19 C20 -1.5(3) . . . . ? C18 C19 C20 C15 0.0(3) . . . . ? C16 C15 C20 C19 1.2(3) . . . . ? C14 C15 C20 C19 -177.23(16) . . . . ? N35 Ag1 N21 C26 155.42(14) . . . . ? N1 Ag1 N21 C26 -28.26(17) . . . . ? N35 Ag1 N21 C22 -38.45(14) . . . . ? N1 Ag1 N21 C22 137.86(12) . . . . ? C26 N21 C22 C23 2.1(3) . . . . ? Ag1 N21 C22 C23 -165.16(16) . . . . ? N21 C22 C23 C24 -1.5(3) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C23 C24 C25 C26 1.4(3) . . . . ? C22 N21 C26 N27 -178.26(15) . . . . ? Ag1 N21 C26 N27 -12.6(2) . . . . ? C22 N21 C26 C25 -0.8(2) . . . . ? Ag1 N21 C26 C25 164.86(13) . . . . ? C24 C25 C26 N21 -0.9(3) . . . . ? C24 C25 C26 N27 176.50(17) . . . . ? N21 C26 N27 C28 -29.1(2) . . . . ? C25 C26 N27 C28 153.40(16) . . . . ? N21 C26 N27 C34 149.05(15) . . . . ? C25 C26 N27 C34 -28.4(2) . . . . ? C26 N27 C28 N29 153.74(15) . . . . ? C34 N27 C28 N29 -24.4(2) . . . . ? C26 N27 C28 C33 -27.9(2) . . . . ? C34 N27 C28 C33 153.90(16) . . . . ? C33 C28 N29 C30 3.2(3) . . . . ? N27 C28 N29 C30 -178.53(16) . . . . ? C28 N29 C30 C31 0.4(3) . . . . ? N29 C30 C31 C32 -2.9(3) . . . . ? C30 C31 C32 C33 1.9(3) . . . . ? C31 C32 C33 C28 1.4(3) . . . . ? N29 C28 C33 C32 -4.1(3) . . . . ? N27 C28 C33 C32 177.73(16) . . . . ? C26 N27 C34 C17 97.33(17) . . . 1_455 ? C28 N27 C34 C17 -84.42(18) . . . 1_455 ? N1 Ag1 N35 C36 76.1(7) . . . . ? N21 Ag1 N35 C36 -106.9(7) . . . . ? Ag1 N35 C36 C37 -174(100) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.363 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.056 #END data_ab7j _database_code_depnum_ccdc_archive 'CCDC 614175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H52 Ag2 Cl2 N12 O10' _chemical_formula_weight 1339.74 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 20.973(1) _cell_length_b 29.544(1) _cell_length_c 17.798(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11028.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 178 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 16.24 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5440 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7785 _exptl_absorpt_correction_T_max 0.9574 _exptl_absorpt_process_details 'SADABS 2.03(Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44563 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.40 _reflns_number_total 9832 _reflns_number_gt 6090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal-99 (E.Keller 1999)' _computing_publication_material 'XCIF 6.12 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+83.5937P] 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 9832 _refine_ls_number_parameters 723 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.061 _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 1.21926(3) 0.101067(19) 0.03132(3) 0.03832(17) Uani 1 1 d . . . Ag2 Ag 0.78878(2) 0.141889(17) 0.38348(3) 0.03155(16) Uani 1 1 d . . . N1 N 1.2305(3) 0.06549(19) 0.1428(3) 0.0321(14) Uani 1 1 d . . . C2 C 1.2892(3) 0.0660(2) 0.1742(4) 0.0369(17) Uani 1 1 d . . . H2 H 1.3250 0.0727 0.1435 0.044 Uiso 1 1 calc R A . C3 C 1.2985(4) 0.0569(3) 0.2495(4) 0.044(2) Uani 1 1 d . . . H3 H 1.3403 0.0567 0.2701 0.052 Uiso 1 1 calc R . . C4 C 1.2465(4) 0.0484(2) 0.2944(4) 0.0411(18) Uani 1 1 d . . . H4 H 1.2516 0.0434 0.3468 0.049 Uiso 1 1 calc R A . C5 C 1.1876(3) 0.0471(2) 0.2624(4) 0.0353(17) Uani 1 1 d . . . H5 H 1.1512 0.0406 0.2925 0.042 Uiso 1 1 calc R . . C6 C 1.1804(3) 0.0552(2) 0.1861(4) 0.0292(16) Uani 1 1 d . . . N7 N 1.1204(2) 0.05488(19) 0.1524(3) 0.0281(13) Uani 1 1 d . . . C8 C 1.1088(3) 0.0454(2) 0.0752(4) 0.0285(15) Uani 1 1 d . . . N9 N 1.0560(3) 0.06336(19) 0.0472(3) 0.0359(14) Uani 1 1 d . . . C10 C 1.0415(4) 0.0540(3) -0.0256(4) 0.0431(19) Uani 1 1 d . . . H10 H 1.0036 0.0665 -0.0462 0.052 Uiso 1 1 calc R A . C11 C 1.0790(4) 0.0273(3) -0.0709(4) 0.0442(19) Uani 1 1 d . . . H11 H 1.0676 0.0218 -0.1218 0.053 Uiso 1 1 calc R . . C12 C 1.1334(4) 0.0089(3) -0.0405(4) 0.047(2) Uani 1 1 d . . . H12 H 1.1600 -0.0100 -0.0703 0.056 Uiso 1 1 calc R A . C13 C 1.1492(3) 0.0178(2) 0.0333(4) 0.0359(17) Uani 1 1 d . . . H13 H 1.1867 0.0055 0.0550 0.043 Uiso 1 1 calc R . . C14 C 1.0648(3) 0.0613(2) 0.2008(4) 0.0280(15) Uani 1 1 d . . . H14A H 1.0321 0.0785 0.1726 0.034 Uiso 1 1 calc R A . H14B H 1.0776 0.0799 0.2445 0.034 Uiso 1 1 calc R . . C15 C 1.0350(3) 0.0181(2) 0.2294(4) 0.0252(14) Uani 1 1 d . . . C16 C 1.0537(3) -0.0244(2) 0.2050(4) 0.0297(16) Uani 1 1 d . . . H16 H 1.0877 -0.0269 0.1700 0.036 Uiso 1 1 calc R A . C17 C 1.0238(3) -0.0633(2) 0.2309(4) 0.0315(16) Uani 1 1 d . . . H17 H 1.0373 -0.0921 0.2134 0.038 Uiso 1 1 calc R . . C18 C 0.9751(3) -0.0601(2) 0.2812(4) 0.0315(16) Uani 1 1 d . . . H18 H 0.9547 -0.0867 0.2991 0.038 Uiso 1 1 calc R A . C19 C 0.9555(3) -0.0179(2) 0.3063(4) 0.0274(15) Uani 1 1 d . . . H19 H 0.9215 -0.0158 0.3414 0.033 Uiso 1 1 calc R . . C20 C 0.9845(3) 0.0213(2) 0.2811(4) 0.0235(14) Uani 1 1 d . . . C21 C 0.9644(3) 0.0674(2) 0.3073(4) 0.0336(17) Uani 1 1 d . . . H21A H 0.9972 0.0793 0.3420 0.040 Uiso 1 1 calc R . . H21B H 0.9627 0.0879 0.2633 0.040 Uiso 1 1 calc R . . N22 N 0.9021(2) 0.06867(18) 0.3455(3) 0.0284(13) Uani 1 1 d . . . C23 C 0.9005(3) 0.0745(2) 0.4227(4) 0.0290(15) Uani 1 1 d . . . N24 N 0.8524(3) 0.09810(18) 0.4532(3) 0.0294(13) Uani 1 1 d . . . C25 C 0.8513(4) 0.1031(3) 0.5290(4) 0.0382(18) Uani 1 1 d . . . H25 H 0.8159 0.1184 0.5507 0.046 Uiso 1 1 calc R . . C26 C 0.8973(4) 0.0876(3) 0.5756(4) 0.045(2) Uani 1 1 d . . . H26 H 0.8952 0.0925 0.6283 0.054 Uiso 1 1 calc R A . C27 C 0.9476(4) 0.0641(3) 0.5435(5) 0.053(2) Uani 1 1 d . . . H27 H 0.9808 0.0528 0.5745 0.064 Uiso 1 1 calc R . . C28 C 0.9499(4) 0.0571(3) 0.4670(4) 0.0434(19) Uani 1 1 d . . . H28 H 0.9842 0.0408 0.4449 0.052 Uiso 1 1 calc R A . C29 C 0.8477(3) 0.0675(2) 0.2998(4) 0.0303(16) Uani 1 1 d . . . C30 C 0.7879(3) 0.0555(2) 0.3275(4) 0.0349(16) Uani 1 1 d . . . H30 H 0.7824 0.0470 0.3785 0.042 Uiso 1 1 calc R A . C31 C 0.7370(4) 0.0564(2) 0.2786(5) 0.046(2) Uani 1 1 d . . . H31 H 0.6957 0.0487 0.2962 0.055 Uiso 1 1 calc R . . C32 C 0.7456(5) 0.0682(3) 0.2046(6) 0.058(3) Uani 1 1 d . . . H32 H 0.7107 0.0694 0.1706 0.069 Uiso 1 1 calc R A . C33 C 0.8062(5) 0.0781(3) 0.1820(5) 0.052(2) Uani 1 1 d . . . H33 H 0.8128 0.0852 0.1306 0.063 Uiso 1 1 calc R . . N34 N 0.8571(3) 0.07838(19) 0.2275(3) 0.0401(15) Uani 1 1 d . . . N35 N 0.7744(2) 0.17978(17) 0.2744(3) 0.0250(12) Uani 1 1 d . . . C36 C 0.7160(3) 0.1781(2) 0.2436(4) 0.0317(16) Uani 1 1 d . . . H36 H 0.6806 0.1719 0.2753 0.038 Uiso 1 1 calc R . . C37 C 0.7050(3) 0.1849(2) 0.1686(4) 0.0346(17) Uani 1 1 d . . . H37 H 0.6631 0.1834 0.1485 0.041 Uiso 1 1 calc R A . C38 C 0.7568(4) 0.1939(2) 0.1234(4) 0.0357(17) Uani 1 1 d . . . H38 H 0.7508 0.1980 0.0709 0.043 Uiso 1 1 calc R . . C39 C 0.8168(3) 0.1971(2) 0.1533(4) 0.0297(16) Uani 1 1 d . . . H39 H 0.8524 0.2039 0.1223 0.036 Uiso 1 1 calc R A . C40 C 0.8245(3) 0.1900(2) 0.2306(4) 0.0258(15) Uani 1 1 d . . . N41 N 0.8843(2) 0.19204(18) 0.2633(3) 0.0266(12) Uani 1 1 d . . . C42 C 0.8933(3) 0.2001(2) 0.3413(4) 0.0290(15) Uani 1 1 d . . . N43 N 0.9443(3) 0.1799(2) 0.3721(3) 0.0376(15) Uani 1 1 d . . . C44 C 0.9552(4) 0.1870(3) 0.4450(4) 0.046(2) Uani 1 1 d . . . H44 H 0.9910 0.1725 0.4671 0.055 Uiso 1 1 calc R . . C45 C 0.9185(4) 0.2138(3) 0.4899(4) 0.043(2) Uani 1 1 d . . . H45 H 0.9279 0.2172 0.5418 0.052 Uiso 1 1 calc R A . C46 C 0.8673(4) 0.2357(2) 0.4575(4) 0.0391(18) Uani 1 1 d . . . H46 H 0.8415 0.2552 0.4870 0.047 Uiso 1 1 calc R . . C47 C 0.8535(3) 0.2294(2) 0.3820(4) 0.0312(16) Uani 1 1 d . . . H47 H 0.8185 0.2443 0.3587 0.037 Uiso 1 1 calc R A . C48 C 0.9406(3) 0.1837(2) 0.2172(4) 0.0282(15) Uani 1 1 d . . . H48A H 0.9280 0.1648 0.1737 0.034 Uiso 1 1 calc R . . H48B H 0.9718 0.1662 0.2471 0.034 Uiso 1 1 calc R . . C49 C 0.9730(3) 0.2259(2) 0.1880(3) 0.0239(14) Uani 1 1 d . . . C50 C 0.9540(3) 0.2691(2) 0.2094(4) 0.0270(15) Uani 1 1 d . . . H50 H 0.9187 0.2724 0.2425 0.032 Uiso 1 1 calc R . . C51 C 0.9852(3) 0.3072(2) 0.1837(4) 0.0322(16) Uani 1 1 d . . . H51 H 0.9720 0.3364 0.2000 0.039 Uiso 1 1 calc R A . C52 C 1.0355(3) 0.3028(2) 0.1342(4) 0.0361(18) Uani 1 1 d . . . H52 H 1.0559 0.3290 0.1143 0.043 Uiso 1 1 calc R . . C53 C 1.0562(3) 0.2599(2) 0.1137(4) 0.0304(16) Uani 1 1 d . . . H53 H 1.0919 0.2568 0.0812 0.036 Uiso 1 1 calc R A . C54 C 1.0256(3) 0.2216(2) 0.1397(4) 0.0251(15) Uani 1 1 d . . . C55 C 1.0478(3) 0.1741(2) 0.1184(4) 0.0281(15) Uani 1 1 d . . . H55A H 1.0541 0.1564 0.1650 0.034 Uiso 1 1 calc R A . H55B H 1.0136 0.1592 0.0891 0.034 Uiso 1 1 calc R . . N56 N 1.1065(2) 0.17282(19) 0.0747(3) 0.0283(13) Uani 1 1 d . . . C57 C 1.1023(3) 0.1660(2) -0.0029(4) 0.0294(16) Uani 1 1 d . . . N58 N 1.1499(3) 0.14367(18) -0.0363(3) 0.0295(13) Uani 1 1 d . . . C59 C 1.1469(4) 0.1378(3) -0.1115(4) 0.0435(19) Uani 1 1 d . . . H59 H 1.1818 0.1234 -0.1359 0.052 Uiso 1 1 calc R A . C60 C 1.0966(4) 0.1512(3) -0.1539(5) 0.052(2) Uani 1 1 d . . . H60 H 1.0961 0.1460 -0.2066 0.063 Uiso 1 1 calc R . . C61 C 1.0455(4) 0.1730(3) -0.1182(5) 0.053(2) Uani 1 1 d . . . H61 H 1.0090 0.1820 -0.1461 0.063 Uiso 1 1 calc R A . C62 C 1.0490(4) 0.1810(3) -0.0423(4) 0.0418(19) Uani 1 1 d . . . H62 H 1.0156 0.1966 -0.0171 0.050 Uiso 1 1 calc R . . C63 C 1.1655(3) 0.1769(2) 0.1137(4) 0.0355(17) Uani 1 1 d . . . C64 C 1.2207(3) 0.1909(2) 0.0779(5) 0.045(2) Uani 1 1 d . . . H64 H 1.2206 0.1979 0.0258 0.053 Uiso 1 1 calc R . . C65 C 1.2749(4) 0.1943(3) 0.1193(7) 0.064(3) Uani 1 1 d . . . H65 H 1.3134 0.2041 0.0962 0.077 Uiso 1 1 calc R A . C66 C 1.2744(6) 0.1836(4) 0.1942(8) 0.083(4) Uani 1 1 d . . . H66 H 1.3124 0.1847 0.2232 0.099 Uiso 1 1 calc R . . C67 C 1.2175(6) 0.1713(4) 0.2262(6) 0.080(4) Uani 1 1 d . . . H67 H 1.2166 0.1655 0.2786 0.096 Uiso 1 1 calc R A . N68 N 1.1625(3) 0.1671(3) 0.1869(4) 0.054(2) Uani 1 1 d . . . Cl1 Cl 0.64226(9) 0.13420(7) 0.45369(12) 0.0482(5) Uani 1 1 d . . . O4 O 0.6004(3) 0.1488(2) 0.5117(3) 0.0683(19) Uani 1 1 d . . . O3 O 0.6942(3) 0.1651(2) 0.4474(4) 0.071(2) Uani 1 1 d . . . O2 O 0.6121(4) 0.1366(5) 0.3854(5) 0.175(6) Uani 1 1 d . . . O1 O 0.6690(7) 0.0922(3) 0.4686(8) 0.215(8) Uani 1 1 d . . . O5 O 1.3971(7) 0.0447(5) -0.0826(7) 0.0727(8) Uiso 0.40 1 d PD A 4 Cl2 Cl 1.3600(4) 0.0562(2) -0.0195(5) 0.0727(8) Uiso 0.40 1 d PD A 4 O6 O 1.3265(7) 0.0134(4) 0.0064(9) 0.0727(8) Uiso 0.40 1 d PD A 4 O7 O 1.3951(7) 0.0705(5) 0.0391(7) 0.0727(8) Uiso 0.40 1 d PD A 4 O8 O 1.3058(6) 0.0804(5) -0.0438(9) 0.0727(8) Uiso 0.40 1 d PD A 4 O9 O 1.4086(5) 0.1048(4) -0.0984(6) 0.0727(8) Uiso 0.60 1 d PD A 1 Cl3 Cl 1.3687(2) 0.09040(16) -0.0372(3) 0.0727(8) Uiso 0.60 1 d PD A 1 O10 O 1.3076(5) 0.1051(4) -0.0543(7) 0.0727(8) Uiso 0.60 1 d PD A 1 O11 O 1.3508(7) 0.0420(4) -0.0277(8) 0.0727(8) Uiso 0.60 1 d PD A 1 O12 O 1.3894(5) 0.1072(4) 0.0312(6) 0.0727(8) Uiso 0.60 1 d PD A 1 O13 O 1.1753(8) 0.2380(5) 0.3997(9) 0.084(2) Uiso 0.50 1 d P B 3 O18 O 1.0956(7) 0.2182(5) 0.3337(9) 0.084(2) Uiso 0.50 1 d P C 4 O14 O 1.3917(7) 0.1566(5) -0.1270(8) 0.084(2) Uiso 0.50 1 d P D 5 O15 O 1.1636(15) 0.2272(10) 0.4508(19) 0.084(2) Uiso 0.25 1 d P E 6 O16 O 1.1352(16) 0.2198(11) 0.4001(19) 0.084(2) Uiso 0.25 1 d P F 7 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 0.0313(3) 0.0400(3) 0.0436(4) 0.0014(3) 0.0102(3) 0.0066(2) Ag2 0.0310(3) 0.0330(3) 0.0307(3) 0.0048(2) 0.0048(2) 0.0065(2) N1 0.027(3) 0.032(3) 0.038(4) -0.007(3) 0.004(3) -0.002(2) C2 0.022(4) 0.040(4) 0.049(5) -0.009(3) 0.003(3) 0.003(3) C3 0.034(4) 0.048(5) 0.049(5) -0.016(4) -0.017(4) 0.004(4) C4 0.043(5) 0.040(4) 0.041(5) -0.010(4) -0.003(4) -0.001(4) C5 0.035(4) 0.036(4) 0.035(4) -0.006(3) -0.004(3) -0.003(3) C6 0.033(4) 0.021(3) 0.034(4) -0.009(3) 0.005(3) 0.000(3) N7 0.023(3) 0.038(3) 0.024(3) -0.005(3) 0.007(2) -0.006(2) C8 0.028(4) 0.026(3) 0.031(4) 0.000(3) 0.002(3) -0.003(3) N9 0.033(3) 0.036(3) 0.039(4) -0.002(3) -0.001(3) -0.003(3) C10 0.041(5) 0.053(5) 0.035(5) 0.007(4) -0.008(4) -0.011(4) C11 0.049(5) 0.052(5) 0.032(5) -0.004(4) -0.008(4) -0.008(4) C12 0.058(5) 0.045(5) 0.037(5) -0.006(4) 0.008(4) -0.006(4) C13 0.041(4) 0.032(4) 0.035(4) -0.001(3) 0.001(3) 0.003(3) C14 0.030(4) 0.022(3) 0.031(4) -0.007(3) 0.005(3) 0.002(3) C15 0.020(3) 0.025(3) 0.030(4) -0.001(3) -0.002(3) 0.003(3) C16 0.018(3) 0.036(4) 0.035(4) -0.005(3) 0.003(3) 0.005(3) C17 0.027(4) 0.026(4) 0.041(4) -0.005(3) -0.006(3) 0.006(3) C18 0.030(4) 0.029(4) 0.036(4) 0.002(3) -0.004(3) -0.002(3) C19 0.026(4) 0.032(4) 0.025(4) -0.001(3) 0.005(3) 0.002(3) C20 0.022(3) 0.026(3) 0.022(4) -0.001(3) -0.002(3) 0.003(3) C21 0.027(4) 0.030(4) 0.044(5) -0.003(3) 0.011(3) 0.006(3) N22 0.025(3) 0.032(3) 0.028(3) -0.005(2) 0.002(2) 0.007(2) C23 0.031(4) 0.028(4) 0.028(4) -0.004(3) -0.001(3) 0.004(3) N24 0.034(3) 0.031(3) 0.023(3) 0.001(2) 0.005(2) 0.005(3) C25 0.044(4) 0.047(4) 0.023(4) -0.002(3) 0.010(3) 0.001(4) C26 0.053(5) 0.054(5) 0.028(4) -0.002(4) -0.009(4) 0.003(4) C27 0.059(5) 0.056(5) 0.044(5) 0.004(4) -0.022(4) 0.020(4) C28 0.040(4) 0.046(5) 0.044(5) -0.006(4) -0.006(4) 0.021(4) C29 0.036(4) 0.024(3) 0.031(4) -0.005(3) 0.006(3) 0.012(3) C30 0.040(4) 0.028(4) 0.037(4) -0.001(3) 0.000(3) 0.001(3) C31 0.037(5) 0.034(4) 0.067(6) -0.009(4) -0.019(4) 0.004(3) C32 0.069(6) 0.035(4) 0.069(7) -0.012(4) -0.034(5) 0.015(5) C33 0.094(7) 0.030(4) 0.032(5) -0.003(3) -0.021(5) 0.020(4) N34 0.064(4) 0.030(3) 0.026(4) -0.001(3) 0.001(3) 0.015(3) N35 0.026(3) 0.023(3) 0.026(3) -0.001(2) 0.002(2) 0.004(2) C36 0.027(4) 0.030(4) 0.038(4) -0.002(3) 0.004(3) 0.003(3) C37 0.037(4) 0.030(4) 0.037(4) -0.004(3) -0.005(3) 0.005(3) C38 0.055(5) 0.028(4) 0.025(4) -0.003(3) -0.004(4) 0.003(3) C39 0.036(4) 0.023(3) 0.030(4) 0.000(3) 0.000(3) -0.002(3) C40 0.033(4) 0.015(3) 0.030(4) -0.001(3) -0.001(3) 0.005(3) N41 0.023(3) 0.031(3) 0.026(3) 0.001(2) 0.005(2) 0.000(2) C42 0.029(4) 0.035(4) 0.024(4) 0.006(3) 0.003(3) -0.003(3) N43 0.029(3) 0.050(4) 0.034(4) 0.001(3) -0.001(3) -0.001(3) C44 0.041(5) 0.059(5) 0.037(5) 0.004(4) -0.007(4) 0.001(4) C45 0.048(5) 0.055(5) 0.026(4) -0.001(4) -0.004(4) -0.016(4) C46 0.048(5) 0.037(4) 0.032(4) -0.006(3) 0.003(4) -0.003(4) C47 0.034(4) 0.029(4) 0.031(4) 0.001(3) 0.002(3) -0.001(3) C48 0.029(4) 0.028(4) 0.028(4) -0.002(3) 0.004(3) 0.001(3) C49 0.024(3) 0.028(3) 0.020(4) -0.001(3) -0.002(3) 0.002(3) C50 0.030(4) 0.028(3) 0.024(4) -0.005(3) 0.001(3) 0.003(3) C51 0.034(4) 0.025(4) 0.037(4) -0.004(3) -0.006(3) 0.002(3) C52 0.035(4) 0.030(4) 0.044(5) 0.003(3) -0.004(3) -0.005(3) C53 0.021(3) 0.037(4) 0.032(4) 0.005(3) 0.000(3) 0.000(3) C54 0.020(3) 0.026(3) 0.029(4) -0.002(3) -0.004(3) 0.002(3) C55 0.025(4) 0.028(3) 0.031(4) 0.000(3) 0.008(3) 0.001(3) N56 0.022(3) 0.039(3) 0.024(3) -0.006(3) 0.001(2) 0.007(2) C57 0.019(3) 0.034(4) 0.035(4) -0.002(3) 0.002(3) -0.004(3) N58 0.029(3) 0.029(3) 0.031(3) -0.005(3) 0.011(2) 0.000(2) C59 0.052(5) 0.039(4) 0.039(5) -0.007(4) 0.013(4) -0.009(4) C60 0.071(6) 0.058(5) 0.027(5) -0.005(4) 0.004(4) -0.003(5) C61 0.045(5) 0.066(6) 0.047(5) 0.001(4) -0.018(4) -0.008(4) C62 0.035(4) 0.054(5) 0.037(5) 0.003(4) 0.001(3) 0.001(4) C63 0.033(4) 0.033(4) 0.041(5) -0.013(3) -0.012(3) 0.010(3) C64 0.030(4) 0.034(4) 0.070(6) -0.004(4) -0.002(4) -0.002(3) C65 0.033(5) 0.036(5) 0.123(10) -0.006(5) -0.025(6) -0.003(4) C66 0.068(8) 0.067(7) 0.113(10) -0.035(7) -0.053(8) 0.018(6) C67 0.088(8) 0.093(8) 0.057(6) -0.039(6) -0.038(6) 0.043(7) N68 0.054(4) 0.078(5) 0.031(4) -0.020(4) -0.015(3) 0.032(4) Cl1 0.0443(11) 0.0533(12) 0.0469(13) -0.0134(9) 0.0138(9) -0.0115(9) O4 0.053(4) 0.096(5) 0.056(4) -0.019(4) 0.023(3) -0.012(4) O3 0.037(3) 0.071(4) 0.105(5) -0.037(4) 0.035(3) -0.008(3) O2 0.077(6) 0.385(19) 0.063(6) -0.084(9) 0.005(5) -0.040(9) O1 0.291(16) 0.061(6) 0.293(17) 0.051(8) 0.201(14) 0.051(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 N1 2.257(6) . ? Ag1 N58 2.269(6) . ? Ag1 O8 2.336(15) . ? Ag1 O10 2.403(11) . ? Ag2 N24 2.235(5) . ? Ag2 N35 2.261(5) . ? Ag2 O3 2.387(5) . ? N1 C6 1.338(8) . ? N1 C2 1.351(9) . ? C2 C3 1.382(11) . ? C2 H2 0.9500 . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.361(10) . ? C4 H4 0.9500 . ? C5 C6 1.388(10) . ? C5 H5 0.9500 . ? C6 N7 1.395(8) . ? N7 C8 1.424(9) . ? N7 C14 1.463(8) . ? C8 N9 1.324(9) . ? C8 C13 1.392(9) . ? N9 C10 1.361(9) . ? C10 C11 1.374(11) . ? C10 H10 0.9500 . ? C11 C12 1.375(11) . ? C11 H11 0.9500 . ? C12 C13 1.381(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.509(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.385(9) . ? C15 C20 1.406(9) . ? C16 C17 1.387(9) . ? C16 H16 0.9500 . ? C17 C18 1.363(9) . ? C17 H17 0.9500 . ? C18 C19 1.388(9) . ? C18 H18 0.9500 . ? C19 C20 1.382(9) . ? C19 H19 0.9500 . ? C20 C21 1.500(9) . ? C21 N22 1.472(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N22 C23 1.385(8) . ? N22 C29 1.402(9) . ? C23 N24 1.341(8) . ? C23 C28 1.402(10) . ? N24 C25 1.357(9) . ? C25 C26 1.353(10) . ? C25 H25 0.9500 . ? C26 C27 1.386(11) . ? C26 H26 0.9500 . ? C27 C28 1.378(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N34 1.340(9) . ? C29 C30 1.394(9) . ? C30 C31 1.376(10) . ? C30 H30 0.9500 . ? C31 C32 1.375(12) . ? C31 H31 0.9500 . ? C32 C33 1.366(13) . ? C32 H32 0.9500 . ? C33 N34 1.339(10) . ? C33 H33 0.9500 . ? N35 C36 1.343(8) . ? N35 C40 1.343(8) . ? C36 C37 1.369(10) . ? C36 H36 0.9500 . ? C37 C38 1.377(10) . ? C37 H37 0.9500 . ? C38 C39 1.370(10) . ? C38 H38 0.9500 . ? C39 C40 1.402(9) . ? C39 H39 0.9500 . ? C40 N41 1.384(8) . ? N41 C42 1.421(8) . ? N41 C48 1.458(8) . ? C42 N43 1.343(9) . ? C42 C47 1.404(9) . ? N43 C44 1.335(9) . ? C44 C45 1.362(11) . ? C44 H44 0.9500 . ? C45 C46 1.380(11) . ? C45 H45 0.9500 . ? C46 C47 1.388(10) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.512(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.388(8) . ? C49 C54 1.404(9) . ? C50 C51 1.383(9) . ? C50 H50 0.9500 . ? C51 C52 1.381(10) . ? C51 H51 0.9500 . ? C52 C53 1.390(9) . ? C52 H52 0.9500 . ? C53 C54 1.380(9) . ? C53 H53 0.9500 . ? C54 C55 1.525(9) . ? C55 N56 1.457(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? N56 C57 1.399(8) . ? N56 C63 1.423(8) . ? C57 N58 1.337(8) . ? C57 C62 1.392(10) . ? N58 C59 1.351(9) . ? C59 C60 1.356(11) . ? C59 H59 0.9500 . ? C60 C61 1.404(12) . ? C60 H60 0.9500 . ? C61 C62 1.374(11) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 N68 1.335(10) . ? C63 C64 1.385(11) . ? C64 C65 1.359(11) . ? C64 H64 0.9500 . ? C65 C66 1.370(15) . ? C65 H65 0.9500 . ? C66 C67 1.371(16) . ? C66 H66 0.9500 . ? C67 N68 1.355(12) . ? C67 H67 0.9500 . ? Cl1 O2 1.372(9) . ? Cl1 O1 1.388(10) . ? Cl1 O4 1.423(6) . ? Cl1 O3 1.426(6) . ? O5 Cl2 1.409(12) . ? Cl2 O7 1.346(11) . ? Cl2 O8 1.411(12) . ? Cl2 O6 1.517(12) . ? O9 Cl3 1.438(10) . ? Cl3 O12 1.385(10) . ? Cl3 O10 1.387(10) . ? Cl3 O11 1.487(11) . ? 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 N58 142.32(19) . . ? N1 Ag1 O8 107.5(4) . . ? N58 Ag1 O8 109.8(4) . . ? N1 Ag1 O10 120.0(3) . . ? N58 Ag1 O10 97.5(3) . . ? O8 Ag1 O10 18.3(4) . . ? N24 Ag2 N35 147.49(19) . . ? N24 Ag2 O3 113.4(2) . . ? N35 Ag2 O3 98.9(2) . . ? C6 N1 C2 118.6(6) . . ? C6 N1 Ag1 122.0(5) . . ? C2 N1 Ag1 117.0(5) . . ? N1 C2 C3 121.9(7) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 119.1(7) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 118.9(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 120.1(7) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 121.2(6) . . ? N1 C6 N7 117.5(6) . . ? C5 C6 N7 121.2(6) . . ? C6 N7 C8 124.8(5) . . ? C6 N7 C14 117.7(5) . . ? C8 N7 C14 117.3(5) . . ? N9 C8 C13 122.9(7) . . ? N9 C8 N7 115.2(6) . . ? C13 C8 N7 121.9(6) . . ? C8 N9 C10 117.6(6) . . ? N9 C10 C11 123.3(7) . . ? N9 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 118.1(7) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? C11 C12 C13 119.8(8) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C8 118.4(7) . . ? C12 C13 H13 120.8 . . ? C8 C13 H13 120.8 . . ? N7 C14 C15 114.8(5) . . ? N7 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N7 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C20 118.7(6) . . ? C16 C15 C14 122.9(6) . . ? C20 C15 C14 118.4(5) . . ? C15 C16 C17 121.2(6) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.7(6) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 121.2(6) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C15 119.1(6) . . ? C19 C20 C21 122.4(6) . . ? C15 C20 C21 118.4(6) . . ? N22 C21 C20 114.5(5) . . ? N22 C21 H21A 108.6 . . ? C20 C21 H21A 108.6 . . ? N22 C21 H21B 108.6 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 N22 C29 123.9(5) . . ? C23 N22 C21 118.9(6) . . ? C29 N22 C21 116.9(5) . . ? N24 C23 N22 119.1(6) . . ? N24 C23 C28 121.3(6) . . ? N22 C23 C28 119.6(6) . . ? C23 N24 C25 118.2(6) . . ? C23 N24 Ag2 121.6(4) . . ? C25 N24 Ag2 118.6(5) . . ? C26 C25 N24 124.1(7) . . ? C26 C25 H25 118.0 . . ? N24 C25 H25 118.0 . . ? C25 C26 C27 117.3(7) . . ? C25 C26 H26 121.3 . . ? C27 C26 H26 121.3 . . ? C28 C27 C26 120.7(7) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C23 118.3(7) . . ? C27 C28 H28 120.8 . . ? C23 C28 H28 120.8 . . ? N34 C29 C30 122.2(7) . . ? N34 C29 N22 115.5(6) . . ? C30 C29 N22 122.3(6) . . ? C31 C30 C29 118.0(7) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C32 C31 C30 120.6(8) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 117.2(8) . . ? C33 C32 H32 121.4 . . ? C31 C32 H32 121.4 . . ? N34 C33 C32 124.5(8) . . ? N34 C33 H33 117.8 . . ? C32 C33 H33 117.8 . . ? C33 N34 C29 117.5(7) . . ? C36 N35 C40 119.0(6) . . ? C36 N35 Ag2 117.0(4) . . ? C40 N35 Ag2 120.3(4) . . ? N35 C36 C37 123.1(7) . . ? N35 C36 H36 118.4 . . ? C37 C36 H36 118.4 . . ? C36 C37 C38 117.7(7) . . ? C36 C37 H37 121.1 . . ? C38 C37 H37 121.1 . . ? C39 C38 C37 120.7(7) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 118.5(7) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N35 C40 N41 118.4(6) . . ? N35 C40 C39 120.9(6) . . ? N41 C40 C39 120.7(6) . . ? C40 N41 C42 122.6(5) . . ? C40 N41 C48 119.3(5) . . ? C42 N41 C48 118.1(5) . . ? N43 C42 C47 122.5(6) . . ? N43 C42 N41 115.5(6) . . ? C47 C42 N41 121.9(6) . . ? C44 N43 C42 117.5(6) . . ? N43 C44 C45 124.5(7) . . ? N43 C44 H44 117.8 . . ? C45 C44 H44 117.8 . . ? C44 C45 C46 117.8(7) . . ? C44 C45 H45 121.1 . . ? C46 C45 H45 121.1 . . ? C45 C46 C47 120.3(7) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C42 117.3(7) . . ? C46 C47 H47 121.3 . . ? C42 C47 H47 121.3 . . ? N41 C48 C49 114.8(5) . . ? N41 C48 H48A 108.6 . . ? C49 C48 H48A 108.6 . . ? N41 C48 H48B 108.6 . . ? C49 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? C50 C49 C54 118.6(6) . . ? C50 C49 C48 122.2(6) . . ? C54 C49 C48 119.2(5) . . ? C51 C50 C49 121.4(6) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C52 C51 C50 119.8(6) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C53 119.4(6) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 121.1(6) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C49 119.7(6) . . ? C53 C54 C55 121.9(6) . . ? C49 C54 C55 118.4(6) . . ? N56 C55 C54 114.5(5) . . ? N56 C55 H55A 108.6 . . ? C54 C55 H55A 108.6 . . ? N56 C55 H55B 108.6 . . ? C54 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C57 N56 C63 123.3(6) . . ? C57 N56 C55 118.5(5) . . ? C63 N56 C55 118.2(6) . . ? N58 C57 C62 122.2(7) . . ? N58 C57 N56 117.6(6) . . ? C62 C57 N56 120.2(6) . . ? C57 N58 C59 118.0(6) . . ? C57 N58 Ag1 121.1(5) . . ? C59 N58 Ag1 118.9(5) . . ? N58 C59 C60 123.4(7) . . ? N58 C59 H59 118.3 . . ? C60 C59 H59 118.3 . . ? C59 C60 C61 118.5(8) . . ? C59 C60 H60 120.8 . . ? C61 C60 H60 120.8 . . ? C62 C61 C60 118.9(8) . . ? C62 C61 H61 120.6 . . ? C60 C61 H61 120.6 . . ? C61 C62 C57 119.0(7) . . ? C61 C62 H62 120.5 . . ? C57 C62 H62 120.5 . . ? N68 C63 C64 123.6(7) . . ? N68 C63 N56 114.6(7) . . ? C64 C63 N56 121.8(7) . . ? C65 C64 C63 118.2(9) . . ? C65 C64 H64 120.9 . . ? C63 C64 H64 120.9 . . ? C64 C65 C66 120.2(10) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C65 C66 C67 118.2(9) . . ? C65 C66 H66 120.9 . . ? C67 C66 H66 120.9 . . ? N68 C67 C66 123.5(10) . . ? N68 C67 H67 118.3 . . ? C66 C67 H67 118.3 . . ? C63 N68 C67 116.3(9) . . ? O2 Cl1 O1 113.8(9) . . ? O2 Cl1 O4 110.1(5) . . ? O1 Cl1 O4 112.4(6) . . ? O2 Cl1 O3 104.4(6) . . ? O1 Cl1 O3 106.2(7) . . ? O4 Cl1 O3 109.6(4) . . ? Cl1 O3 Ag2 119.2(3) . . ? O7 Cl2 O5 113.0(10) . . ? O7 Cl2 O8 121.3(10) . . ? O5 Cl2 O8 108.8(10) . . ? O7 Cl2 O6 106.3(10) . . ? O5 Cl2 O6 107.2(9) . . ? O8 Cl2 O6 98.2(9) . . ? Cl2 O8 Ag1 125.6(10) . . ? O12 Cl3 O10 111.7(8) . . ? O12 Cl3 O9 112.2(7) . . ? O10 Cl3 O9 106.1(7) . . ? O12 Cl3 O11 108.8(8) . . ? O10 Cl3 O11 95.4(8) . . ? O9 Cl3 O11 121.2(8) . . ? Cl3 O10 Ag1 123.9(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 N58 Ag1 N1 C6 18.6(7) . . . . ? O8 Ag1 N1 C6 -153.2(6) . . . . ? O10 Ag1 N1 C6 -167.7(5) . . . . ? N58 Ag1 N1 C2 -143.6(4) . . . . ? O8 Ag1 N1 C2 44.7(6) . . . . ? O10 Ag1 N1 C2 30.1(6) . . . . ? C6 N1 C2 C3 -1.2(10) . . . . ? Ag1 N1 C2 C3 161.6(6) . . . . ? N1 C2 C3 C4 -1.7(11) . . . . ? C2 C3 C4 C5 2.8(11) . . . . ? C3 C4 C5 C6 -1.3(11) . . . . ? C2 N1 C6 C5 2.7(9) . . . . ? Ag1 N1 C6 C5 -159.1(5) . . . . ? C2 N1 C6 N7 -179.8(6) . . . . ? Ag1 N1 C6 N7 18.3(8) . . . . ? C4 C5 C6 N1 -1.5(10) . . . . ? C4 C5 C6 N7 -178.9(6) . . . . ? N1 C6 N7 C8 28.2(9) . . . . ? C5 C6 N7 C8 -154.4(6) . . . . ? N1 C6 N7 C14 -156.8(6) . . . . ? C5 C6 N7 C14 20.6(9) . . . . ? C6 N7 C8 N9 -154.3(6) . . . . ? C14 N7 C8 N9 30.6(8) . . . . ? C6 N7 C8 C13 27.8(10) . . . . ? C14 N7 C8 C13 -147.3(6) . . . . ? C13 C8 N9 C10 0.1(10) . . . . ? N7 C8 N9 C10 -177.7(6) . . . . ? C8 N9 C10 C11 -0.5(11) . . . . ? N9 C10 C11 C12 0.8(12) . . . . ? C10 C11 C12 C13 -0.7(11) . . . . ? C11 C12 C13 C8 0.4(11) . . . . ? N9 C8 C13 C12 -0.1(10) . . . . ? N7 C8 C13 C12 177.7(6) . . . . ? C6 N7 C14 C15 -92.9(7) . . . . ? C8 N7 C14 C15 82.5(7) . . . . ? N7 C14 C15 C16 -7.2(9) . . . . ? N7 C14 C15 C20 175.0(6) . . . . ? C20 C15 C16 C17 -0.1(10) . . . . ? C14 C15 C16 C17 -178.0(6) . . . . ? C15 C16 C17 C18 -0.1(10) . . . . ? C16 C17 C18 C19 0.2(10) . . . . ? C17 C18 C19 C20 0.0(10) . . . . ? C18 C19 C20 C15 -0.2(10) . . . . ? C18 C19 C20 C21 -180.0(6) . . . . ? C16 C15 C20 C19 0.3(9) . . . . ? C14 C15 C20 C19 178.2(6) . . . . ? C16 C15 C20 C21 -179.9(6) . . . . ? C14 C15 C20 C21 -2.0(9) . . . . ? C19 C20 C21 N22 -14.9(10) . . . . ? C15 C20 C21 N22 165.3(6) . . . . ? C20 C21 N22 C23 106.5(7) . . . . ? C20 C21 N22 C29 -78.6(8) . . . . ? C29 N22 C23 N24 -28.8(10) . . . . ? C21 N22 C23 N24 145.7(6) . . . . ? C29 N22 C23 C28 153.3(7) . . . . ? C21 N22 C23 C28 -32.2(9) . . . . ? N22 C23 N24 C25 179.3(6) . . . . ? C28 C23 N24 C25 -2.8(10) . . . . ? N22 C23 N24 Ag2 -15.1(8) . . . . ? C28 C23 N24 Ag2 162.8(5) . . . . ? N35 Ag2 N24 C23 -19.0(7) . . . . ? O3 Ag2 N24 C23 166.2(5) . . . . ? N35 Ag2 N24 C25 146.5(5) . . . . ? O3 Ag2 N24 C25 -28.2(6) . . . . ? C23 N24 C25 C26 3.3(11) . . . . ? Ag2 N24 C25 C26 -162.7(6) . . . . ? N24 C25 C26 C27 -1.8(12) . . . . ? C25 C26 C27 C28 -0.1(13) . . . . ? C26 C27 C28 C23 0.5(13) . . . . ? N24 C23 C28 C27 1.0(11) . . . . ? N22 C23 C28 C27 178.8(7) . . . . ? C23 N22 C29 N34 156.2(6) . . . . ? C21 N22 C29 N34 -18.4(8) . . . . ? C23 N22 C29 C30 -24.3(10) . . . . ? C21 N22 C29 C30 161.1(6) . . . . ? N34 C29 C30 C31 -1.9(10) . . . . ? N22 C29 C30 C31 178.6(6) . . . . ? C29 C30 C31 C32 0.7(11) . . . . ? C30 C31 C32 C33 1.2(11) . . . . ? C31 C32 C33 N34 -2.2(12) . . . . ? C32 C33 N34 C29 1.1(11) . . . . ? C30 C29 N34 C33 1.0(10) . . . . ? N22 C29 N34 C33 -179.4(6) . . . . ? N24 Ag2 N35 C36 140.0(5) . . . . ? O3 Ag2 N35 C36 -44.9(5) . . . . ? N24 Ag2 N35 C40 -18.3(7) . . . . ? O3 Ag2 N35 C40 156.8(5) . . . . ? C40 N35 C36 C37 2.2(9) . . . . ? Ag2 N35 C36 C37 -156.4(5) . . . . ? N35 C36 C37 C38 -0.1(10) . . . . ? C36 C37 C38 C39 -1.7(10) . . . . ? C37 C38 C39 C40 1.3(10) . . . . ? C36 N35 C40 N41 179.4(6) . . . . ? Ag2 N35 C40 N41 -22.7(7) . . . . ? C36 N35 C40 C39 -2.5(9) . . . . ? Ag2 N35 C40 C39 155.3(5) . . . . ? C38 C39 C40 N35 0.8(9) . . . . ? C38 C39 C40 N41 178.8(6) . . . . ? N35 C40 N41 C42 -23.2(9) . . . . ? C39 C40 N41 C42 158.7(6) . . . . ? N35 C40 N41 C48 154.0(6) . . . . ? C39 C40 N41 C48 -24.1(9) . . . . ? C40 N41 C42 N43 147.7(6) . . . . ? C48 N41 C42 N43 -29.5(8) . . . . ? C40 N41 C42 C47 -36.0(9) . . . . ? C48 N41 C42 C47 146.7(6) . . . . ? C47 C42 N43 C44 2.7(10) . . . . ? N41 C42 N43 C44 178.9(6) . . . . ? C42 N43 C44 C45 -0.7(11) . . . . ? N43 C44 C45 C46 -1.4(12) . . . . ? C44 C45 C46 C47 1.6(11) . . . . ? C45 C46 C47 C42 0.2(10) . . . . ? N43 C42 C47 C46 -2.4(10) . . . . ? N41 C42 C47 C46 -178.4(6) . . . . ? C40 N41 C48 C49 96.9(7) . . . . ? C42 N41 C48 C49 -85.8(7) . . . . ? N41 C48 C49 C50 5.6(9) . . . . ? N41 C48 C49 C54 -176.5(6) . . . . ? C54 C49 C50 C51 0.6(10) . . . . ? C48 C49 C50 C51 178.4(6) . . . . ? C49 C50 C51 C52 1.5(10) . . . . ? C50 C51 C52 C53 -3.1(10) . . . . ? C51 C52 C53 C54 2.5(10) . . . . ? C52 C53 C54 C49 -0.4(10) . . . . ? C52 C53 C54 C55 -179.5(6) . . . . ? C50 C49 C54 C53 -1.1(9) . . . . ? C48 C49 C54 C53 -179.0(6) . . . . ? C50 C49 C54 C55 177.9(6) . . . . ? C48 C49 C54 C55 0.1(9) . . . . ? C53 C54 C55 N56 5.3(9) . . . . ? C49 C54 C55 N56 -173.7(6) . . . . ? C54 C55 N56 C57 -101.6(7) . . . . ? C54 C55 N56 C63 80.7(7) . . . . ? C63 N56 C57 N58 29.4(9) . . . . ? C55 N56 C57 N58 -148.1(6) . . . . ? C63 N56 C57 C62 -152.4(7) . . . . ? C55 N56 C57 C62 30.0(9) . . . . ? C62 C57 N58 C59 3.3(10) . . . . ? N56 C57 N58 C59 -178.6(6) . . . . ? C62 C57 N58 Ag1 -160.6(5) . . . . ? N56 C57 N58 Ag1 17.5(8) . . . . ? N1 Ag1 N58 C57 19.9(6) . . . . ? O8 Ag1 N58 C57 -168.5(6) . . . . ? O10 Ag1 N58 C57 -154.6(5) . . . . ? N1 Ag1 N58 C59 -143.9(5) . . . . ? O8 Ag1 N58 C59 27.7(7) . . . . ? O10 Ag1 N58 C59 41.6(6) . . . . ? C57 N58 C59 C60 -3.5(11) . . . . ? Ag1 N58 C59 C60 160.8(6) . . . . ? N58 C59 C60 C61 0.9(12) . . . . ? C59 C60 C61 C62 1.9(12) . . . . ? C60 C61 C62 C57 -2.0(12) . . . . ? N58 C57 C62 C61 -0.6(11) . . . . ? N56 C57 C62 C61 -178.6(7) . . . . ? C57 N56 C63 N68 -157.2(6) . . . . ? C55 N56 C63 N68 20.4(9) . . . . ? C57 N56 C63 C64 24.3(10) . . . . ? C55 N56 C63 C64 -158.2(6) . . . . ? N68 C63 C64 C65 1.0(11) . . . . ? N56 C63 C64 C65 179.4(7) . . . . ? C63 C64 C65 C66 0.6(13) . . . . ? C64 C65 C66 C67 -2.6(14) . . . . ? C65 C66 C67 N68 3.2(16) . . . . ? C64 C63 N68 C67 -0.5(11) . . . . ? N56 C63 N68 C67 -179.0(7) . . . . ? C66 C67 N68 C63 -1.7(14) . . . . ? O2 Cl1 O3 Ag2 -80.1(7) . . . . ? O1 Cl1 O3 Ag2 40.4(8) . . . . ? O4 Cl1 O3 Ag2 162.0(4) . . . . ? N24 Ag2 O3 Cl1 -79.0(5) . . . . ? N35 Ag2 O3 Cl1 103.9(5) . . . . ? O7 Cl2 O8 Ag1 -54.5(16) . . . . ? O5 Cl2 O8 Ag1 171.8(10) . . . . ? O6 Cl2 O8 Ag1 60.3(12) . . . . ? N1 Ag1 O8 Cl2 -9.4(13) . . . . ? N58 Ag1 O8 Cl2 176.0(10) . . . . ? O10 Ag1 O8 Cl2 127(2) . . . . ? O12 Cl3 O10 Ag1 -49.1(10) . . . . ? O9 Cl3 O10 Ag1 -171.7(7) . . . . ? O11 Cl3 O10 Ag1 63.6(9) . . . . ? N1 Ag1 O10 Cl3 -6.3(10) . . . . ? N58 Ag1 O10 Cl3 169.8(8) . . . . ? O8 Ag1 O10 Cl3 -56.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.392 _refine_diff_density_min -1.496 _refine_diff_density_rms 0.127 #END data_ab8 _database_code_depnum_ccdc_archive 'CCDC 614176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 N6' _chemical_formula_weight 444.53 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' _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 9.218(1) _cell_length_b 11.011(1) _cell_length_c 12.294(1) _cell_angle_alpha 104.89(1) _cell_angle_beta 95.32(1) _cell_angle_gamma 108.07(1) _cell_volume 1126.08(18) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 103 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 21.39 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.83 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9360 _exptl_absorpt_correction_T_max 0.9809 _exptl_absorpt_process_details 'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35395 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.40 _reflns_number_total 5013 _reflns_number_gt 3900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal-99 (E.Keller 1999)' _computing_publication_material 'XCIF 6.12 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.2205P] 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 5013 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 N1 N 1.44408(12) 0.52885(10) 0.76114(9) 0.0317(2) Uani 1 1 d . . . C2 C 1.57951(15) 0.51248(13) 0.78936(12) 0.0359(3) Uani 1 1 d . . . H2 H 1.6129 0.4564 0.7324 0.043 Uiso 1 1 calc R . . C3 C 1.67255(15) 0.57242(13) 0.89610(12) 0.0366(3) Uani 1 1 d . . . H3 H 1.7691 0.5605 0.9122 0.044 Uiso 1 1 calc R . . C4 C 1.62051(15) 0.65097(13) 0.97947(11) 0.0356(3) Uani 1 1 d . . . H4 H 1.6804 0.6920 1.0548 0.043 Uiso 1 1 calc R . . C5 C 1.48198(14) 0.66955(12) 0.95309(10) 0.0304(3) Uani 1 1 d . . . H5 H 1.4444 0.7223 1.0096 0.036 Uiso 1 1 calc R . . C6 C 1.39797(13) 0.60849(10) 0.84059(10) 0.0243(2) Uani 1 1 d . . . N7 N 1.25459(11) 0.62212(9) 0.80507(8) 0.0253(2) Uani 1 1 d . . . C8 C 1.21649(13) 0.73591(11) 0.84989(9) 0.0235(2) Uani 1 1 d . . . N9 N 1.33114(11) 0.84730(10) 0.91469(9) 0.0298(2) Uani 1 1 d . . . C10 C 1.29693(15) 0.95872(12) 0.95272(11) 0.0353(3) Uani 1 1 d . . . H10 H 1.3780 1.0376 0.9992 0.042 Uiso 1 1 calc R . . C11 C 1.15211(16) 0.96604(13) 0.92875(12) 0.0388(3) Uani 1 1 d . . . H11 H 1.1338 1.0480 0.9554 0.047 Uiso 1 1 calc R . . C12 C 1.03361(16) 0.84934(14) 0.86411(12) 0.0384(3) Uani 1 1 d . . . H12 H 0.9312 0.8499 0.8470 0.046 Uiso 1 1 calc R . . C13 C 1.06388(14) 0.73311(12) 0.82485(10) 0.0293(3) Uani 1 1 d . . . H13 H 0.9830 0.6523 0.7815 0.035 Uiso 1 1 calc R . . C14 C 1.14537(13) 0.51664(11) 0.70685(9) 0.0255(2) Uani 1 1 d . . . H14A H 1.2040 0.4693 0.6595 0.031 Uiso 1 1 calc R . . H14B H 1.0968 0.5588 0.6592 0.031 Uiso 1 1 calc R . . C15 C 1.01796(12) 0.41457(10) 0.73966(9) 0.0220(2) Uani 1 1 d . . . C16 C 1.02924(14) 0.40473(11) 0.85056(10) 0.0290(3) Uani 1 1 d . . . H16 H 1.1154 0.4661 0.9078 0.035 Uiso 1 1 calc R . . C17 C 0.91691(16) 0.30697(13) 0.87883(11) 0.0357(3) Uani 1 1 d . . . H17 H 0.9267 0.3011 0.9548 0.043 Uiso 1 1 calc R . . C18 C 0.79036(16) 0.21787(13) 0.79608(11) 0.0368(3) Uani 1 1 d . . . H18 H 0.7129 0.1506 0.8149 0.044 Uiso 1 1 calc R . . C19 C 0.77740(14) 0.22735(12) 0.68550(10) 0.0310(3) Uani 1 1 d . . . H19 H 0.6903 0.1661 0.6290 0.037 Uiso 1 1 calc R . . C20 C 0.88912(12) 0.32453(10) 0.65579(9) 0.0221(2) Uani 1 1 d . . . C21 C 0.87437(13) 0.33666(11) 0.53538(9) 0.0250(2) Uani 1 1 d . . . H21A H 0.8536 0.4201 0.5375 0.030 Uiso 1 1 calc R . . H21B H 0.9750 0.3450 0.5102 0.030 Uiso 1 1 calc R . . N22 N 0.75231(11) 0.22433(9) 0.45034(8) 0.0250(2) Uani 1 1 d . . . C23 C 0.78227(13) 0.10465(11) 0.40778(9) 0.0246(2) Uani 1 1 d . . . N24 N 0.93031(12) 0.11845(11) 0.40408(10) 0.0348(2) Uani 1 1 d . . . C25 C 0.96297(18) 0.00630(15) 0.36491(13) 0.0449(3) Uani 1 1 d . . . H25 H 1.0685 0.0152 0.3632 0.054 Uiso 1 1 calc R . . C26 C 0.85424(19) -0.12003(14) 0.32721(13) 0.0466(4) Uani 1 1 d . . . H26 H 0.8827 -0.1961 0.2971 0.056 Uiso 1 1 calc R . . C27 C 0.70165(18) -0.13335(13) 0.33433(13) 0.0454(4) Uani 1 1 d . . . H27 H 0.6232 -0.2196 0.3106 0.054 Uiso 1 1 calc R . . C28 C 0.66439(15) -0.02038(12) 0.37614(12) 0.0364(3) Uani 1 1 d . . . H28 H 0.5606 -0.0275 0.3833 0.044 Uiso 1 1 calc R . . C29 C 0.60556(13) 0.23476(11) 0.42554(9) 0.0235(2) Uani 1 1 d . . . N30 N 0.56990(12) 0.32172(10) 0.50611(8) 0.0308(2) Uani 1 1 d . . . C31 C 0.43072(15) 0.33480(13) 0.48443(11) 0.0359(3) Uani 1 1 d . . . H31 H 0.4047 0.3970 0.5414 0.043 Uiso 1 1 calc R . . C32 C 0.32373(15) 0.26351(14) 0.38474(12) 0.0389(3) Uani 1 1 d . . . H32 H 0.2252 0.2736 0.3739 0.047 Uiso 1 1 calc R . . C33 C 0.36499(15) 0.17654(14) 0.30077(11) 0.0377(3) Uani 1 1 d . . . H33 H 0.2949 0.1269 0.2302 0.045 Uiso 1 1 calc R . . C34 C 0.50672(14) 0.16203(12) 0.31940(10) 0.0297(3) Uani 1 1 d . . . H34 H 0.5372 0.1041 0.2618 0.036 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 N1 0.0283(5) 0.0305(5) 0.0312(5) 0.0024(4) 0.0043(4) 0.0091(4) C2 0.0325(7) 0.0364(7) 0.0396(7) 0.0086(5) 0.0091(5) 0.0146(6) C3 0.0272(6) 0.0399(7) 0.0454(8) 0.0176(6) 0.0044(5) 0.0121(5) C4 0.0327(7) 0.0348(6) 0.0331(6) 0.0096(5) -0.0046(5) 0.0068(5) C5 0.0303(6) 0.0285(6) 0.0273(6) 0.0043(5) 0.0016(5) 0.0077(5) C6 0.0205(5) 0.0210(5) 0.0258(5) 0.0050(4) 0.0030(4) 0.0014(4) N7 0.0197(5) 0.0229(5) 0.0240(5) -0.0003(4) -0.0003(4) 0.0020(4) C8 0.0222(5) 0.0245(5) 0.0200(5) 0.0060(4) 0.0043(4) 0.0036(4) N9 0.0222(5) 0.0259(5) 0.0322(5) -0.0008(4) 0.0038(4) 0.0041(4) C10 0.0307(7) 0.0281(6) 0.0376(7) -0.0007(5) 0.0060(5) 0.0061(5) C11 0.0407(8) 0.0320(6) 0.0441(8) 0.0059(6) 0.0069(6) 0.0179(6) C12 0.0307(7) 0.0433(7) 0.0428(7) 0.0129(6) 0.0005(6) 0.0171(6) C13 0.0239(6) 0.0299(6) 0.0291(6) 0.0085(5) -0.0015(5) 0.0049(5) C14 0.0217(5) 0.0240(5) 0.0207(5) 0.0005(4) 0.0003(4) 0.0004(4) C15 0.0214(5) 0.0196(5) 0.0226(5) 0.0036(4) 0.0022(4) 0.0067(4) C16 0.0322(6) 0.0273(6) 0.0221(5) 0.0048(4) -0.0001(5) 0.0066(5) C17 0.0472(8) 0.0345(6) 0.0247(6) 0.0122(5) 0.0075(5) 0.0103(6) C18 0.0391(7) 0.0320(6) 0.0356(7) 0.0152(5) 0.0114(6) 0.0021(5) C19 0.0258(6) 0.0282(6) 0.0308(6) 0.0076(5) 0.0024(5) -0.0002(5) C20 0.0203(5) 0.0210(5) 0.0228(5) 0.0050(4) 0.0027(4) 0.0058(4) C21 0.0205(5) 0.0238(5) 0.0220(5) 0.0041(4) -0.0016(4) -0.0002(4) N22 0.0186(5) 0.0247(5) 0.0239(5) 0.0015(4) -0.0020(4) 0.0034(4) C23 0.0239(6) 0.0269(5) 0.0207(5) 0.0065(4) 0.0021(4) 0.0068(5) N24 0.0264(5) 0.0382(6) 0.0413(6) 0.0127(5) 0.0065(4) 0.0123(5) C25 0.0399(8) 0.0516(8) 0.0535(9) 0.0185(7) 0.0138(7) 0.0262(7) C26 0.0622(10) 0.0406(8) 0.0469(8) 0.0121(6) 0.0123(7) 0.0319(7) C27 0.0530(9) 0.0260(6) 0.0489(8) 0.0071(6) 0.0040(7) 0.0077(6) C28 0.0290(6) 0.0284(6) 0.0454(7) 0.0076(5) 0.0062(5) 0.0042(5) C29 0.0206(5) 0.0240(5) 0.0224(5) 0.0062(4) 0.0028(4) 0.0041(4) N30 0.0321(6) 0.0311(5) 0.0267(5) 0.0031(4) 0.0031(4) 0.0128(4) C31 0.0373(7) 0.0374(7) 0.0376(7) 0.0090(5) 0.0117(6) 0.0196(6) C32 0.0258(6) 0.0474(8) 0.0467(8) 0.0157(6) 0.0050(6) 0.0165(6) C33 0.0264(6) 0.0451(7) 0.0337(7) 0.0055(6) -0.0038(5) 0.0093(6) C34 0.0244(6) 0.0345(6) 0.0242(6) 0.0029(5) 0.0016(5) 0.0077(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 N1 C6 1.3311(15) . ? N1 C2 1.3427(17) . ? C2 C3 1.3741(19) . ? C3 C4 1.3862(19) . ? C4 C5 1.3773(18) . ? C5 C6 1.4018(16) . ? C6 N7 1.4177(15) . ? N7 C8 1.3967(14) . ? N7 C14 1.4659(13) . ? C8 N9 1.3392(14) . ? C8 C13 1.4009(16) . ? N9 C10 1.3401(16) . ? C10 C11 1.3716(19) . ? C11 C12 1.3854(19) . ? C12 C13 1.3703(18) . ? C14 C15 1.5190(15) . ? C15 C16 1.3921(16) . ? C15 C20 1.4049(15) . ? C16 C17 1.3854(18) . ? C17 C18 1.3840(18) . ? C18 C19 1.3871(17) . ? C19 C20 1.3878(16) . ? C20 C21 1.5176(15) . ? C21 N22 1.4638(13) . ? N22 C29 1.4050(14) . ? N22 C23 1.4089(14) . ? C23 N24 1.3319(15) . ? C23 C28 1.3948(16) . ? N24 C25 1.3414(17) . ? C25 C26 1.368(2) . ? C26 C27 1.382(2) . ? C27 C28 1.3779(19) . ? C29 N30 1.3320(15) . ? C29 C34 1.4014(15) . ? N30 C31 1.3449(16) . ? C31 C32 1.3755(19) . ? C32 C33 1.3850(19) . ? C33 C34 1.3702(18) . ? 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 C6 N1 C2 118.23(11) . . ? N1 C2 C3 123.63(12) . . ? C2 C3 C4 117.65(12) . . ? C5 C4 C3 120.02(12) . . ? C4 C5 C6 118.20(12) . . ? N1 C6 C5 122.16(11) . . ? N1 C6 N7 115.40(10) . . ? C5 C6 N7 122.37(10) . . ? C8 N7 C6 124.25(9) . . ? C8 N7 C14 117.23(9) . . ? C6 N7 C14 118.19(9) . . ? N9 C8 N7 117.69(10) . . ? N9 C8 C13 121.74(10) . . ? N7 C8 C13 120.55(10) . . ? C8 N9 C10 117.93(10) . . ? N9 C10 C11 124.10(11) . . ? C10 C11 C12 117.42(12) . . ? C13 C12 C11 120.09(12) . . ? C12 C13 C8 118.65(11) . . ? N7 C14 C15 113.97(9) . . ? C16 C15 C20 119.10(10) . . ? C16 C15 C14 121.22(10) . . ? C20 C15 C14 119.63(9) . . ? C17 C16 C15 121.13(11) . . ? C18 C17 C16 119.76(11) . . ? C17 C18 C19 119.59(12) . . ? C18 C19 C20 121.33(11) . . ? C19 C20 C15 119.08(10) . . ? C19 C20 C21 121.56(10) . . ? C15 C20 C21 119.35(10) . . ? N22 C21 C20 114.68(9) . . ? C29 N22 C23 122.85(9) . . ? C29 N22 C21 118.81(9) . . ? C23 N22 C21 117.88(9) . . ? N24 C23 C28 122.44(11) . . ? N24 C23 N22 115.83(10) . . ? C28 C23 N22 121.68(11) . . ? C23 N24 C25 117.33(11) . . ? N24 C25 C26 124.30(14) . . ? C25 C26 C27 117.82(13) . . ? C28 C27 C26 119.38(13) . . ? C27 C28 C23 118.64(13) . . ? N30 C29 C34 122.47(11) . . ? N30 C29 N22 116.21(10) . . ? C34 C29 N22 121.24(10) . . ? C29 N30 C31 117.60(10) . . ? N30 C31 C32 123.91(12) . . ? C31 C32 C33 117.53(12) . . ? C34 C33 C32 120.08(12) . . ? C33 C34 C29 118.32(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 C6 N1 C2 C3 0.63(19) . . . . ? N1 C2 C3 C4 1.8(2) . . . . ? C2 C3 C4 C5 -1.7(2) . . . . ? C3 C4 C5 C6 -0.70(19) . . . . ? C2 N1 C6 C5 -3.24(18) . . . . ? C2 N1 C6 N7 179.61(10) . . . . ? C4 C5 C6 N1 3.30(18) . . . . ? C4 C5 C6 N7 -179.76(11) . . . . ? N1 C6 N7 C8 -150.90(11) . . . . ? C5 C6 N7 C8 31.96(17) . . . . ? N1 C6 N7 C14 22.30(15) . . . . ? C5 C6 N7 C14 -154.84(11) . . . . ? C6 N7 C8 N9 12.62(16) . . . . ? C14 N7 C8 N9 -160.64(10) . . . . ? C6 N7 C8 C13 -168.94(11) . . . . ? C14 N7 C8 C13 17.80(15) . . . . ? N7 C8 N9 C10 176.43(11) . . . . ? C13 C8 N9 C10 -1.99(17) . . . . ? C8 N9 C10 C11 -0.5(2) . . . . ? N9 C10 C11 C12 2.1(2) . . . . ? C10 C11 C12 C13 -1.3(2) . . . . ? C11 C12 C13 C8 -1.0(2) . . . . ? N9 C8 C13 C12 2.76(18) . . . . ? N7 C8 C13 C12 -175.62(11) . . . . ? C8 N7 C14 C15 -88.09(12) . . . . ? C6 N7 C14 C15 98.23(12) . . . . ? N7 C14 C15 C16 -15.21(15) . . . . ? N7 C14 C15 C20 167.43(10) . . . . ? C20 C15 C16 C17 0.82(18) . . . . ? C14 C15 C16 C17 -176.56(11) . . . . ? C15 C16 C17 C18 -0.5(2) . . . . ? C16 C17 C18 C19 0.1(2) . . . . ? C17 C18 C19 C20 0.1(2) . . . . ? C18 C19 C20 C15 0.21(18) . . . . ? C18 C19 C20 C21 -179.10(12) . . . . ? C16 C15 C20 C19 -0.65(16) . . . . ? C14 C15 C20 C19 176.76(11) . . . . ? C16 C15 C20 C21 178.67(10) . . . . ? C14 C15 C20 C21 -3.91(15) . . . . ? C19 C20 C21 N22 -11.24(16) . . . . ? C15 C20 C21 N22 169.45(10) . . . . ? C20 C21 N22 C29 94.97(12) . . . . ? C20 C21 N22 C23 -77.37(13) . . . . ? C29 N22 C23 N24 157.92(10) . . . . ? C21 N22 C23 N24 -30.06(15) . . . . ? C29 N22 C23 C28 -24.62(17) . . . . ? C21 N22 C23 C28 147.39(12) . . . . ? C28 C23 N24 C25 2.00(19) . . . . ? N22 C23 N24 C25 179.43(11) . . . . ? C23 N24 C25 C26 1.1(2) . . . . ? N24 C25 C26 C27 -2.8(2) . . . . ? C25 C26 C27 C28 1.4(2) . . . . ? C26 C27 C28 C23 1.4(2) . . . . ? N24 C23 C28 C27 -3.2(2) . . . . ? N22 C23 C28 C27 179.51(12) . . . . ? C23 N22 C29 N30 149.19(11) . . . . ? C21 N22 C29 N30 -22.75(15) . . . . ? C23 N22 C29 C34 -33.85(16) . . . . ? C21 N22 C29 C34 154.21(11) . . . . ? C34 C29 N30 C31 2.51(18) . . . . ? N22 C29 N30 C31 179.43(11) . . . . ? C29 N30 C31 C32 0.3(2) . . . . ? N30 C31 C32 C33 -2.2(2) . . . . ? C31 C32 C33 C34 1.2(2) . . . . ? C32 C33 C34 C29 1.4(2) . . . . ? N30 C29 C34 C33 -3.36(18) . . . . ? N22 C29 C34 C33 179.87(11) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.218 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.043 #END data_lj64 _database_code_depnum_ccdc_archive 'CCDC 614177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 N6' _chemical_formula_sum 'C28 H24 N6' _chemical_formula_weight 444.53 _chemical_absolute_configuration unk 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 0.0000 '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 0.0000 '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 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.635(3) _cell_length_b 9.2483(19) _cell_length_c 16.571(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.094(3) _cell_angle_gamma 90.00 _cell_volume 2243.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10633 _cell_measurement_theta_min 2.458 _cell_measurement_theta_max 28.1135 _exptl_crystal_description multi-face _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Crystream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 105 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.44 _diffrn_reflns_number 10605 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2821 _reflns_number_gt 2684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0446P)^2^+0.4092P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_number_reflns 2821 _refine_ls_number_parameters 310 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 C1 C 0.5000 -0.1533(4) 0.5000 0.0308(10) Uani 1 2 d S . . H1 H 0.5000 -0.2560 0.5000 0.037 Uiso 1 2 calc SR . . C2 C 0.5098(2) -0.0801(3) 0.42831(19) 0.0280(6) Uani 1 1 d . . . H2 H 0.5167 -0.1323 0.3793 0.034 Uiso 1 1 calc R . . C3 C 0.50952(18) 0.0707(3) 0.42740(17) 0.0221(6) Uani 1 1 d . . . C4 C 0.5000 0.1446(5) 0.5000 0.0220(8) Uani 1 2 d S . . H4 H 0.5000 0.2473 0.5000 0.026 Uiso 1 2 calc SR . . C5 C 0.5159(2) 0.1486(3) 0.34771(16) 0.0266(6) Uani 1 1 d . . . H5A H 0.5706 0.1127 0.3189 0.032 Uiso 1 1 calc R . . H5B H 0.4618 0.1225 0.3149 0.032 Uiso 1 1 calc R . . C6 C 0.44415(19) 0.3886(3) 0.32723(16) 0.0236(6) Uani 1 1 d . . . C7 C 0.3630(2) 0.3782(5) 0.3689(2) 0.0421(9) Uani 1 1 d . . . H7 H 0.3579 0.3173 0.4148 0.050 Uiso 1 1 calc R . . C8 C 0.2887(2) 0.4593(5) 0.3421(2) 0.0475(9) Uani 1 1 d . . . H8 H 0.2320 0.4546 0.3699 0.057 Uiso 1 1 calc R . . C9 C 0.2977(2) 0.5453(4) 0.2759(2) 0.0359(8) Uani 1 1 d . . . H9 H 0.2480 0.6016 0.2565 0.043 Uiso 1 1 calc R . . C10 C 0.3812(2) 0.5475(4) 0.2384(2) 0.0395(8) Uani 1 1 d . . . H10 H 0.3878 0.6075 0.1923 0.047 Uiso 1 1 calc R . . C11 C 0.6013(2) 0.3720(3) 0.37816(16) 0.0267(6) Uani 1 1 d . . . C12 C 0.6070(2) 0.5219(3) 0.38858(18) 0.0301(7) Uani 1 1 d . . . H12 H 0.5574 0.5829 0.3742 0.036 Uiso 1 1 calc R . . C13 C 0.6865(2) 0.5787(4) 0.4202(2) 0.0398(8) Uani 1 1 d . . . H13 H 0.6913 0.6800 0.4289 0.048 Uiso 1 1 calc R . . C14 C 0.7591(2) 0.4895(5) 0.4395(2) 0.0412(8) Uani 1 1 d . . . H14 H 0.8137 0.5270 0.4623 0.049 Uiso 1 1 calc R . . C15 C 0.7487(2) 0.3430(4) 0.4240(2) 0.0382(8) Uani 1 1 d . . . H15 H 0.7990 0.2809 0.4349 0.046 Uiso 1 1 calc R . . C16 C 0.5000 0.5056(4) 0.0000 0.0314(10) Uani 1 2 d S . . H16 H 0.5000 0.4029 0.0000 0.038 Uiso 1 2 calc SR . . C17 C 0.5247(2) 0.5786(3) 0.06972(19) 0.0292(6) Uani 1 1 d . . . H17 H 0.5405 0.5264 0.1171 0.035 Uiso 1 1 calc R . . C18 C 0.52603(18) 0.7298(3) 0.06968(18) 0.0237(6) Uani 1 1 d . . . C19 C 0.5000 0.8032(4) 0.0000 0.0235(8) Uani 1 2 d S . . H19 H 0.5000 0.9059 0.0000 0.028 Uiso 1 2 calc SR . . C20 C 0.5574(2) 0.8086(3) 0.14503(17) 0.0270(6) Uani 1 1 d . . . H20A H 0.5259 0.7665 0.1923 0.032 Uiso 1 1 calc R . . H20B H 0.6238 0.7924 0.1522 0.032 Uiso 1 1 calc R . . C21 C 0.45063(19) 1.0128(3) 0.16070(16) 0.0243(6) Uani 1 1 d . . . C22 C 0.4130(2) 1.1354(4) 0.12551(18) 0.0307(7) Uani 1 1 d . . . H22 H 0.4454 1.1875 0.0853 0.037 Uiso 1 1 calc R . . C23 C 0.3273(2) 1.1802(4) 0.1503(2) 0.0370(7) Uani 1 1 d . . . H23 H 0.3007 1.2655 0.1285 0.044 Uiso 1 1 calc R . . C24 C 0.2806(2) 1.0993(4) 0.2071(2) 0.0377(8) Uani 1 1 d . . . H24 H 0.2229 1.1294 0.2270 0.045 Uiso 1 1 calc R . . C25 C 0.3206(2) 0.9747(4) 0.23348(18) 0.0351(7) Uani 1 1 d . . . H25 H 0.2869 0.9159 0.2699 0.042 Uiso 1 1 calc R . . C26 C 0.60933(19) 1.0569(3) 0.11625(17) 0.0240(6) Uani 1 1 d . . . C27 C 0.6120(2) 1.2038(3) 0.13512(18) 0.0274(6) Uani 1 1 d . . . H27 H 0.5657 1.2466 0.1673 0.033 Uiso 1 1 calc R . . C28 C 0.6837(2) 1.2853(3) 0.10587(19) 0.0312(7) Uani 1 1 d . . . H28 H 0.6860 1.3863 0.1162 0.037 Uiso 1 1 calc R . . C29 C 0.7522(2) 1.2201(4) 0.0617(2) 0.0368(8) Uani 1 1 d . . . H29 H 0.8020 1.2743 0.0409 0.044 Uiso 1 1 calc R . . C30 C 0.7453(2) 1.0732(4) 0.0489(2) 0.0352(8) Uani 1 1 d . . . H30 H 0.7931 1.0269 0.0201 0.042 Uiso 1 1 calc R . . N1 N 0.52137(16) 0.3057(3) 0.35190(14) 0.0248(5) Uani 1 1 d . . . N2 N 0.45381(17) 0.4711(3) 0.26243(15) 0.0334(6) Uani 1 1 d . . . N3 N 0.67148(17) 0.2834(3) 0.39446(16) 0.0320(6) Uani 1 1 d . . . N4 N 0.54000(16) 0.9648(3) 0.14329(14) 0.0242(5) Uani 1 1 d . . . N5 N 0.40408(17) 0.9292(3) 0.21171(16) 0.0301(6) Uani 1 1 d . . . N6 N 0.67571(17) 0.9919(3) 0.07440(16) 0.0304(5) 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 C1 0.034(2) 0.0168(19) 0.042(2) 0.000 0.0053(19) 0.000 C2 0.0284(15) 0.0264(15) 0.0294(15) -0.0054(12) 0.0027(13) 0.0031(12) C3 0.0170(12) 0.0245(14) 0.0247(13) 0.0003(11) -0.0002(11) 0.0001(11) C4 0.0198(19) 0.0208(18) 0.0255(18) 0.000 -0.0030(15) 0.000 C5 0.0312(15) 0.0275(14) 0.0211(13) -0.0033(12) -0.0008(11) 0.0025(13) C6 0.0223(13) 0.0271(13) 0.0215(13) -0.0042(12) -0.0032(11) -0.0006(12) C7 0.0341(17) 0.059(2) 0.0332(18) 0.0198(17) 0.0058(14) 0.0070(17) C8 0.0283(16) 0.072(3) 0.0421(19) 0.0095(19) 0.0060(15) 0.0150(17) C9 0.0280(16) 0.0398(18) 0.0398(18) -0.0010(15) -0.0066(14) 0.0067(14) C10 0.0362(17) 0.043(2) 0.0397(19) 0.0189(16) -0.0023(15) 0.0003(15) C11 0.0236(14) 0.0373(17) 0.0193(13) 0.0052(12) 0.0019(11) -0.0022(12) C12 0.0264(15) 0.0335(17) 0.0303(15) -0.0046(13) 0.0003(13) 0.0015(13) C13 0.0377(17) 0.0441(19) 0.0376(18) -0.0089(16) 0.0031(16) -0.0136(16) C14 0.0278(15) 0.066(2) 0.0293(16) 0.0032(17) -0.0020(13) -0.0120(18) C15 0.0244(15) 0.059(2) 0.0313(16) 0.0145(17) 0.0016(14) 0.0004(15) C16 0.035(2) 0.0126(18) 0.047(3) 0.000 0.010(2) 0.000 C17 0.0285(15) 0.0237(14) 0.0353(16) 0.0071(13) 0.0078(13) 0.0033(13) C18 0.0176(12) 0.0219(13) 0.0317(15) 0.0012(12) 0.0060(12) 0.0028(11) C19 0.0210(19) 0.0183(18) 0.031(2) 0.000 0.0063(16) 0.000 C20 0.0284(14) 0.0231(14) 0.0295(14) 0.0066(12) 0.0024(13) 0.0026(12) C21 0.0261(14) 0.0255(14) 0.0212(13) -0.0068(11) -0.0010(11) 0.0009(12) C22 0.0338(16) 0.0305(15) 0.0278(15) 0.0039(13) 0.0005(12) 0.0008(13) C23 0.0367(17) 0.0358(17) 0.0384(18) -0.0033(15) -0.0069(15) 0.0090(14) C24 0.0296(16) 0.045(2) 0.0386(18) -0.0099(15) 0.0020(14) 0.0031(14) C25 0.0311(15) 0.0463(19) 0.0280(15) -0.0017(15) 0.0047(12) -0.0053(16) C26 0.0230(13) 0.0291(15) 0.0199(14) -0.0007(12) -0.0028(11) 0.0002(12) C27 0.0267(15) 0.0292(16) 0.0263(15) 0.0031(12) -0.0012(12) 0.0017(12) C28 0.0308(15) 0.0262(15) 0.0366(17) 0.0046(13) -0.0071(13) -0.0038(13) C29 0.0277(16) 0.0427(19) 0.0401(18) 0.0090(16) -0.0017(14) -0.0095(15) C30 0.0254(15) 0.044(2) 0.0358(18) 0.0008(15) 0.0034(13) 0.0043(15) N1 0.0252(12) 0.0226(12) 0.0266(12) 0.0027(10) -0.0013(10) -0.0002(10) N2 0.0273(13) 0.0420(15) 0.0310(13) 0.0126(12) 0.0002(11) 0.0001(12) N3 0.0245(13) 0.0396(15) 0.0318(14) 0.0079(12) 0.0043(11) 0.0018(11) N4 0.0254(12) 0.0207(11) 0.0264(11) 0.0000(10) 0.0015(10) 0.0000(9) N5 0.0311(14) 0.0321(13) 0.0272(13) -0.0016(11) 0.0016(11) -0.0044(11) N6 0.0260(12) 0.0334(14) 0.0318(13) -0.0010(12) -0.0003(11) 0.0025(11) _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 C1 C2 1.375(4) 2_656 ? C1 C2 1.375(4) . ? C1 H1 0.9500 . ? C2 C3 1.395(4) . ? C2 H2 0.9500 . ? C3 C4 1.391(3) . ? C3 C5 1.508(4) . ? C4 C3 1.391(3) 2_656 ? C4 H4 0.9500 . ? C5 N1 1.456(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N2 1.325(4) . ? C6 C7 1.378(4) . ? C6 N1 1.425(4) . ? C7 C8 1.393(5) . ? C7 H7 0.9500 . ? C8 C9 1.361(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 N2 1.336(4) . ? C10 H10 0.9500 . ? C11 N3 1.340(4) . ? C11 N1 1.390(4) . ? C11 C12 1.399(5) . ? C12 C13 1.379(5) . ? C12 H12 0.9500 . ? C13 C14 1.382(5) . ? C13 H13 0.9500 . ? C14 C15 1.388(6) . ? C14 H14 0.9500 . ? C15 N3 1.348(4) . ? C15 H15 0.9500 . ? C16 C17 1.385(4) 2_655 ? C16 C17 1.385(4) . ? C16 H16 0.9500 . ? C17 C18 1.398(4) . ? C17 H17 0.9500 . ? C18 C19 1.392(4) . ? C18 C20 1.516(4) . ? C19 C18 1.392(4) 2_655 ? C19 H19 0.9500 . ? C20 N4 1.467(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N5 1.334(4) . ? C21 C22 1.389(4) . ? C21 N4 1.411(3) . ? C22 C23 1.384(5) . ? C22 H22 0.9500 . ? C23 C24 1.384(5) . ? C23 H23 0.9500 . ? C24 C25 1.364(5) . ? C24 H24 0.9500 . ? C25 N5 1.343(4) . ? C25 H25 0.9500 . ? C26 N6 1.338(4) . ? C26 C27 1.394(4) . ? C26 N4 1.399(4) . ? C27 C28 1.381(4) . ? C27 H27 0.9500 . ? C28 C29 1.380(5) . ? C28 H28 0.9500 . ? C29 C30 1.378(5) . ? C29 H29 0.9500 . ? C30 N6 1.335(4) . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C2 121.0(4) 2_656 . ? C2 C1 H1 119.5 2_656 . ? C2 C1 H1 119.5 . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 C5 122.0(2) . . ? C2 C3 C5 119.2(3) . . ? C3 C4 C3 121.1(4) . 2_656 ? C3 C4 H4 119.4 . . ? C3 C4 H4 119.4 2_656 . ? N1 C5 C3 116.0(2) . . ? N1 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? N1 C5 H5B 108.3 . . ? C3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N2 C6 C7 122.6(3) . . ? N2 C6 N1 117.2(3) . . ? C7 C6 N1 120.2(3) . . ? C6 C7 C8 118.5(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 117.5(3) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? N2 C10 C9 124.5(3) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N3 C11 N1 116.0(3) . . ? N3 C11 C12 122.3(3) . . ? N1 C11 C12 121.7(3) . . ? C13 C12 C11 118.3(3) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 117.2(3) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? N3 C15 C14 123.8(3) . . ? N3 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C17 C16 C17 121.7(4) 2_655 . ? C17 C16 H16 119.2 2_655 . ? C17 C16 H16 119.2 . . ? C16 C17 C18 119.4(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.0(3) . . ? C19 C18 C20 122.1(3) . . ? C17 C18 C20 119.0(3) . . ? C18 C19 C18 121.6(4) . 2_655 ? C18 C19 H19 119.2 . . ? C18 C19 H19 119.2 2_655 . ? N4 C20 C18 113.9(2) . . ? N4 C20 H20A 108.8 . . ? C18 C20 H20A 108.8 . . ? N4 C20 H20B 108.8 . . ? C18 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? N5 C21 C22 122.5(3) . . ? N5 C21 N4 114.9(2) . . ? C22 C21 N4 122.6(3) . . ? C23 C22 C21 118.6(3) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 117.6(3) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? N5 C25 C24 124.6(3) . . ? N5 C25 H25 117.7 . . ? C24 C25 H25 117.7 . . ? N6 C26 C27 122.3(3) . . ? N6 C26 N4 114.8(3) . . ? C27 C26 N4 122.8(3) . . ? C28 C27 C26 118.3(3) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 117.3(3) . . ? C28 C29 H29 121.3 . . ? C30 C29 H29 121.3 . . ? N6 C30 C29 124.2(3) . . ? N6 C30 H30 117.9 . . ? C29 C30 H30 117.9 . . ? C11 N1 C6 121.3(2) . . ? C11 N1 C5 120.1(2) . . ? C6 N1 C5 118.6(2) . . ? C6 N2 C10 117.4(3) . . ? C11 N3 C15 117.7(3) . . ? C26 N4 C21 123.2(2) . . ? C26 N4 C20 118.7(2) . . ? C21 N4 C20 117.8(2) . . ? C21 N5 C25 117.0(3) . . ? C30 N6 C26 117.7(3) . . ? 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 C1 C2 C3 -0.3(2) 2_656 . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C1 C2 C3 C5 -177.2(2) . . . . ? C2 C3 C4 C3 -0.3(2) . . . 2_656 ? C5 C3 C4 C3 177.4(3) . . . 2_656 ? C4 C3 C5 N1 6.3(4) . . . . ? C2 C3 C5 N1 -176.1(3) . . . . ? N2 C6 C7 C8 -0.7(6) . . . . ? N1 C6 C7 C8 -179.0(3) . . . . ? C6 C7 C8 C9 0.3(6) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C8 C9 C10 N2 0.1(6) . . . . ? N3 C11 C12 C13 -3.0(5) . . . . ? N1 C11 C12 C13 175.5(3) . . . . ? C11 C12 C13 C14 1.3(5) . . . . ? C12 C13 C14 C15 1.3(5) . . . . ? C13 C14 C15 N3 -2.5(5) . . . . ? C17 C16 C17 C18 -0.90(19) 2_655 . . . ? C16 C17 C18 C19 1.8(4) . . . . ? C16 C17 C18 C20 -177.2(2) . . . . ? C17 C18 C19 C18 -0.89(19) . . . 2_655 ? C20 C18 C19 C18 178.0(3) . . . 2_655 ? C19 C18 C20 N4 11.8(4) . . . . ? C17 C18 C20 N4 -169.3(2) . . . . ? N5 C21 C22 C23 6.4(4) . . . . ? N4 C21 C22 C23 -175.6(3) . . . . ? C21 C22 C23 C24 -2.1(5) . . . . ? C22 C23 C24 C25 -2.8(5) . . . . ? C23 C24 C25 N5 4.0(5) . . . . ? N6 C26 C27 C28 3.3(4) . . . . ? N4 C26 C27 C28 179.6(3) . . . . ? C26 C27 C28 C29 -2.4(5) . . . . ? C27 C28 C29 C30 -0.1(5) . . . . ? C28 C29 C30 N6 2.0(5) . . . . ? N3 C11 N1 C6 -175.5(2) . . . . ? C12 C11 N1 C6 5.9(4) . . . . ? N3 C11 N1 C5 3.3(4) . . . . ? C12 C11 N1 C5 -175.3(3) . . . . ? N2 C6 N1 C11 64.4(4) . . . . ? C7 C6 N1 C11 -117.3(3) . . . . ? N2 C6 N1 C5 -114.4(3) . . . . ? C7 C6 N1 C5 63.9(4) . . . . ? C3 C5 N1 C11 72.8(3) . . . . ? C3 C5 N1 C6 -108.3(3) . . . . ? C7 C6 N2 C10 0.8(5) . . . . ? N1 C6 N2 C10 179.1(3) . . . . ? C9 C10 N2 C6 -0.5(5) . . . . ? N1 C11 N3 C15 -176.7(3) . . . . ? C12 C11 N3 C15 1.9(4) . . . . ? C14 C15 N3 C11 0.9(5) . . . . ? N6 C26 N4 C21 -155.6(3) . . . . ? C27 C26 N4 C21 27.9(4) . . . . ? N6 C26 N4 C20 17.3(4) . . . . ? C27 C26 N4 C20 -159.3(3) . . . . ? N5 C21 N4 C26 -156.6(3) . . . . ? C22 C21 N4 C26 25.2(4) . . . . ? N5 C21 N4 C20 30.5(3) . . . . ? C22 C21 N4 C20 -147.7(3) . . . . ? C18 C20 N4 C26 -93.8(3) . . . . ? C18 C20 N4 C21 79.4(3) . . . . ? C22 C21 N5 C25 -5.4(4) . . . . ? N4 C21 N5 C25 176.5(2) . . . . ? C24 C25 N5 C21 0.1(4) . . . . ? C29 C30 N6 C26 -1.2(5) . . . . ? C27 C26 N6 C30 -1.5(4) . . . . ? N4 C26 N6 C30 -178.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.147 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.034 #END data_lj93sad _database_code_depnum_ccdc_archive 'CCDC 614178' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H33 Ag N10 O3' _chemical_formula_sum 'C39 H33 Ag N10 O3' _chemical_formula_weight 797.62 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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1320(15) _cell_length_b 12.801(2) _cell_length_c 15.264(3) _cell_angle_alpha 81.910(3) _cell_angle_beta 81.998(3) _cell_angle_gamma 71.440(3) _cell_volume 1666.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4789 _cell_measurement_theta_min 2.2695 _cell_measurement_theta_max 26.2365 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.138 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.096 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 105 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 16508 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.40 _reflns_number_total 7771 _reflns_number_gt 5892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0433P)^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 7771 _refine_ls_number_parameters 467 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.8035(3) 0.1224(3) 0.8336(2) 0.0360(7) Uani 1 1 d . . . H1 H 0.7736 0.2001 0.8368 0.043 Uiso 1 1 calc R . . C2 C 0.8542(4) 0.0531(3) 0.9077(2) 0.0456(9) Uani 1 1 d . . . H2 H 0.8563 0.0818 0.9615 0.055 Uiso 1 1 calc R . . C3 C 0.9020(4) -0.0597(3) 0.9017(2) 0.0463(9) Uani 1 1 d . . . H3 H 0.9372 -0.1099 0.9519 0.056 Uiso 1 1 calc R . . C4 C 0.8989(4) -0.0992(3) 0.8236(2) 0.0397(8) Uani 1 1 d . . . H4 H 0.9349 -0.1766 0.8185 0.048 Uiso 1 1 calc R . . C5 C 0.8414(3) -0.0235(2) 0.75069(19) 0.0273(6) Uani 1 1 d . . . C6 C 0.7961(3) 0.0071(2) 0.59152(18) 0.0237(6) Uani 1 1 d . . . C7 C 0.8677(3) 0.0891(2) 0.56221(18) 0.0261(6) Uani 1 1 d . . . H7 H 0.9359 0.1032 0.5975 0.031 Uiso 1 1 calc R . . C8 C 0.8368(3) 0.1493(2) 0.48053(19) 0.0307(6) Uani 1 1 d . . . H8 H 0.8830 0.2061 0.4591 0.037 Uiso 1 1 calc R . . C9 C 0.7377(4) 0.1259(3) 0.4302(2) 0.0361(7) Uani 1 1 d . . . H9 H 0.7141 0.1661 0.3741 0.043 Uiso 1 1 calc R . . C10 C 0.6748(4) 0.0427(3) 0.4645(2) 0.0371(7) Uani 1 1 d . . . H10 H 0.6083 0.0257 0.4298 0.045 Uiso 1 1 calc R . . C11 C 0.7974(3) -0.1690(2) 0.6795(2) 0.0303(6) Uani 1 1 d . . . H11A H 0.8801 -0.2257 0.7108 0.036 Uiso 1 1 calc R . . H11B H 0.8031 -0.1907 0.6190 0.036 Uiso 1 1 calc R . . C12 C 0.6414(3) -0.1687(2) 0.72860(18) 0.0242(6) Uani 1 1 d . . . C13 C 0.5226(3) -0.0704(2) 0.74088(18) 0.0238(6) Uani 1 1 d . . . H13 H 0.5408 -0.0017 0.7201 0.029 Uiso 1 1 calc R . . C14 C 0.3786(3) -0.0711(2) 0.78285(17) 0.0210(5) Uani 1 1 d . . . C15 C 0.3522(3) -0.1724(2) 0.81313(18) 0.0251(6) Uani 1 1 d . . . H15 H 0.2536 -0.1736 0.8421 0.030 Uiso 1 1 calc R . . C16 C 0.4696(3) -0.2717(2) 0.80111(18) 0.0257(6) Uani 1 1 d . . . C17 C 0.6133(3) -0.2687(2) 0.75899(19) 0.0280(6) Uani 1 1 d . . . H17 H 0.6938 -0.3362 0.7508 0.034 Uiso 1 1 calc R . . C18 C 0.2462(3) 0.0356(2) 0.79470(19) 0.0247(6) Uani 1 1 d . . . H18A H 0.1634 0.0376 0.7584 0.030 Uiso 1 1 calc R . . H18B H 0.2023 0.0341 0.8578 0.030 Uiso 1 1 calc R . . C19 C 0.2586(3) 0.1969(2) 0.68602(17) 0.0214(5) Uani 1 1 d . . . C20 C 0.1116(3) 0.2264(2) 0.65840(19) 0.0282(6) Uani 1 1 d . . . H20 H 0.0297 0.2087 0.6967 0.034 Uiso 1 1 calc R . . C21 C 0.0841(4) 0.2817(2) 0.5748(2) 0.0318(7) Uani 1 1 d . . . H21 H -0.0162 0.3020 0.5548 0.038 Uiso 1 1 calc R . . C22 C 0.2058(4) 0.3067(2) 0.52098(19) 0.0314(7) Uani 1 1 d . . . H22 H 0.1915 0.3427 0.4626 0.038 Uiso 1 1 calc R . . C23 C 0.3476(4) 0.2786(2) 0.55333(19) 0.0301(6) Uani 1 1 d . . . H23 H 0.4295 0.2989 0.5169 0.036 Uiso 1 1 calc R . . C24 C 0.3503(3) 0.1770(2) 0.83300(17) 0.0217(5) Uani 1 1 d . . . C25 C 0.3672(3) 0.2834(2) 0.82059(18) 0.0250(6) Uani 1 1 d . . . H25 H 0.3396 0.3309 0.7679 0.030 Uiso 1 1 calc R . . C26 C 0.4248(3) 0.3173(2) 0.88676(19) 0.0300(6) Uani 1 1 d . . . H26 H 0.4376 0.3889 0.8800 0.036 Uiso 1 1 calc R . . C27 C 0.4641(4) 0.2464(2) 0.9633(2) 0.0340(7) Uani 1 1 d . . . H27 H 0.5051 0.2677 1.0094 0.041 Uiso 1 1 calc R . . C28 C 0.4415(4) 0.1443(2) 0.97001(19) 0.0328(7) Uani 1 1 d . . . H28 H 0.4657 0.0962 1.0229 0.039 Uiso 1 1 calc R . . C29 C 0.4523(3) -0.3841(2) 0.83641(19) 0.0294(6) Uani 1 1 d D . . H29A H 0.5182 -0.4391 0.7963 0.035 Uiso 1 1 calc R . . H29B H 0.4920 -0.4056 0.8956 0.035 Uiso 1 1 calc RD . . C30 C 0.2049(3) -0.3814(2) 0.9292(2) 0.0294(6) Uani 1 1 d D . . C31 C 0.0390(9) -0.3754(6) 0.9399(5) 0.0417(6) Uiso 0.50 1 d P A 1 H31 H -0.0149 -0.3787 0.8919 0.050 Uiso 0.50 1 calc PR A 1 C32 C -0.0303(9) -0.3645(6) 1.0256(5) 0.0417(6) Uiso 0.50 1 d P A 1 H32 H -0.1370 -0.3599 1.0373 0.050 Uiso 0.50 1 calc PR A 1 C34 C 0.2085(9) -0.3716(6) 1.0742(5) 0.0417(6) Uiso 0.50 1 d P A 1 H34 H 0.2667 -0.3706 1.1209 0.050 Uiso 0.50 1 calc PR A 1 N7 N 0.2823(7) -0.3840(5) 0.9919(4) 0.0417(6) Uiso 0.50 1 d P A 1 N7A N 0.0552(7) -0.3346(5) 0.9385(4) 0.0417(6) Uiso 0.50 1 d PD A 2 C32A C -0.0251(9) -0.3238(6) 1.0201(5) 0.0417(6) Uiso 0.50 1 d PD A 2 H32A H -0.1345 -0.2904 1.0248 0.050 Uiso 0.50 1 calc PR A 2 C31A C 0.2840(9) -0.4200(6) 1.0095(4) 0.0417(6) Uiso 0.50 1 d PD A 2 H31A H 0.3934 -0.4531 1.0057 0.050 Uiso 0.50 1 calc PRD A 2 C34A C 0.2006(9) -0.4084(6) 1.0885(5) 0.0417(6) Uiso 0.50 1 d PD A 2 H34A H 0.2512 -0.4352 1.1411 0.050 Uiso 0.50 1 calc PR A 2 C33 C 0.0479(4) -0.3599(3) 1.0948(2) 0.0468(9) Uani 1 1 d D . . H33 H -0.0025 -0.3495 1.1531 0.056 Uiso 1 1 calc R A 1 C35 C 0.2396(4) -0.4086(2) 0.7685(2) 0.0329(7) Uani 1 1 d . . . C36 C 0.3300(4) -0.4032(3) 0.6892(2) 0.0402(8) Uani 1 1 d . A . H36 H 0.4215 -0.3821 0.6864 0.048 Uiso 1 1 calc R B 1 C37 C 0.2879(6) -0.4281(3) 0.6157(3) 0.0585(11) Uani 1 1 d . A 1 H37 H 0.3518 -0.4263 0.5611 0.070 Uiso 1 1 calc R A 1 C38 C 0.1542(5) -0.4562(3) 0.6180(3) 0.0578(11) Uani 1 1 d . A 1 H38 H 0.1234 -0.4723 0.5658 0.069 Uiso 1 1 calc R A 1 C39 C 0.0663(5) -0.4601(3) 0.6986(3) 0.0501(10) Uani 1 1 d . A 1 H39 H -0.0262 -0.4798 0.7015 0.060 Uiso 1 1 calc R A 1 N1 N 0.7940(3) 0.08602(19) 0.75642(15) 0.0276(5) Uani 1 1 d . . . N2 N 0.8275(3) -0.06179(18) 0.67174(15) 0.0260(5) Uani 1 1 d . . . N3 N 0.7013(3) -0.0159(2) 0.54359(16) 0.0308(6) Uani 1 1 d . . . N4 N 0.3766(3) 0.22363(18) 0.63428(15) 0.0242(5) Uani 1 1 d . . . N5 N 0.2894(3) 0.13751(18) 0.77013(14) 0.0221(5) Uani 1 1 d . . . N6 N 0.3873(3) 0.10848(19) 0.90647(15) 0.0278(5) Uani 1 1 d . . . N8 N 0.2912(3) -0.38997(19) 0.84497(15) 0.0288(5) Uani 1 1 d . A . N9 N 0.1067(3) -0.4368(2) 0.7740(2) 0.0462(7) Uani 1 1 d . A . N10 N 0.6990(3) 0.4148(2) 0.65184(17) 0.0332(6) Uani 1 1 d . . . O1 O 0.6743(3) 0.3669(2) 0.59290(15) 0.0560(7) Uani 1 1 d . . . O2 O 0.6836(4) 0.3737(2) 0.72883(16) 0.0683(8) Uani 1 1 d . . . O3 O 0.7366(3) 0.4998(2) 0.6341(2) 0.0638(8) Uani 1 1 d . . . Ag1 Ag 0.60997(3) 0.207788(19) 0.676155(15) 0.02949(8) 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 C1 0.0292(16) 0.049(2) 0.0332(17) -0.0118(15) 0.0001(13) -0.0145(15) C2 0.0349(18) 0.075(3) 0.0308(17) -0.0062(17) -0.0058(14) -0.0200(18) C3 0.0340(18) 0.065(3) 0.0384(19) 0.0115(17) -0.0129(15) -0.0161(18) C4 0.0323(17) 0.0413(19) 0.0447(19) 0.0094(15) -0.0099(15) -0.0136(15) C5 0.0180(13) 0.0303(16) 0.0336(16) 0.0011(12) -0.0019(12) -0.0094(12) C6 0.0192(13) 0.0245(14) 0.0267(14) -0.0073(11) 0.0032(11) -0.0059(11) C7 0.0248(14) 0.0247(15) 0.0302(15) -0.0076(12) 0.0028(12) -0.0097(12) C8 0.0344(16) 0.0265(15) 0.0308(16) -0.0049(12) 0.0051(13) -0.0114(13) C9 0.0460(19) 0.0349(17) 0.0262(15) -0.0043(13) -0.0014(14) -0.0111(15) C10 0.0363(18) 0.048(2) 0.0315(17) -0.0091(15) -0.0035(14) -0.0168(15) C11 0.0295(16) 0.0199(14) 0.0407(17) -0.0045(12) 0.0060(13) -0.0098(12) C12 0.0268(14) 0.0203(14) 0.0262(14) -0.0005(11) -0.0007(11) -0.0097(11) C13 0.0266(14) 0.0207(14) 0.0275(14) -0.0011(11) -0.0012(11) -0.0131(12) C14 0.0260(14) 0.0190(13) 0.0198(13) -0.0002(10) -0.0039(11) -0.0097(11) C15 0.0270(14) 0.0234(14) 0.0269(14) 0.0007(11) -0.0015(12) -0.0124(12) C16 0.0319(15) 0.0217(14) 0.0255(14) 0.0002(11) -0.0021(12) -0.0124(12) C17 0.0295(15) 0.0184(14) 0.0347(16) -0.0046(12) 0.0006(12) -0.0065(12) C18 0.0249(14) 0.0218(14) 0.0300(15) 0.0006(11) -0.0016(12) -0.0125(12) C19 0.0243(14) 0.0141(12) 0.0265(14) -0.0045(10) -0.0006(11) -0.0065(11) C20 0.0271(15) 0.0269(16) 0.0344(16) -0.0039(12) -0.0045(13) -0.0128(13) C21 0.0317(16) 0.0281(16) 0.0385(17) -0.0022(13) -0.0134(13) -0.0094(13) C22 0.0434(18) 0.0236(15) 0.0291(15) 0.0000(12) -0.0116(14) -0.0106(13) C23 0.0354(17) 0.0252(15) 0.0313(15) -0.0026(12) 0.0018(13) -0.0139(13) C24 0.0187(13) 0.0206(13) 0.0241(14) -0.0028(11) 0.0021(10) -0.0053(11) C25 0.0272(15) 0.0196(14) 0.0269(14) -0.0005(11) -0.0001(12) -0.0071(11) C26 0.0353(16) 0.0233(15) 0.0338(16) -0.0061(12) -0.0004(13) -0.0121(13) C27 0.0433(18) 0.0303(16) 0.0305(16) -0.0077(13) -0.0067(14) -0.0111(14) C28 0.0443(18) 0.0271(16) 0.0256(15) 0.0006(12) -0.0061(13) -0.0092(14) C29 0.0319(16) 0.0226(15) 0.0333(16) -0.0013(12) 0.0030(13) -0.0112(12) C30 0.0337(16) 0.0150(13) 0.0380(17) 0.0001(12) -0.0016(13) -0.0074(12) C33 0.050(2) 0.047(2) 0.0421(19) -0.0094(16) 0.0108(16) -0.0160(17) C35 0.0417(18) 0.0140(14) 0.0423(18) 0.0022(12) -0.0092(14) -0.0073(13) C36 0.055(2) 0.0270(17) 0.0413(19) 0.0027(14) -0.0056(16) -0.0179(15) C37 0.089(3) 0.040(2) 0.047(2) 0.0014(17) -0.009(2) -0.021(2) C38 0.091(3) 0.0299(19) 0.047(2) -0.0042(16) -0.033(2) 0.000(2) C39 0.055(2) 0.0292(18) 0.069(3) -0.0076(17) -0.032(2) -0.0049(16) N1 0.0239(12) 0.0298(13) 0.0289(13) -0.0039(10) -0.0017(10) -0.0083(10) N2 0.0231(12) 0.0223(12) 0.0323(13) -0.0005(10) 0.0009(10) -0.0088(10) N3 0.0315(14) 0.0323(14) 0.0322(13) -0.0071(11) 0.0005(11) -0.0149(11) N4 0.0257(12) 0.0203(12) 0.0262(12) -0.0007(9) -0.0014(10) -0.0075(10) N5 0.0243(12) 0.0181(11) 0.0253(12) -0.0003(9) -0.0020(9) -0.0093(9) N6 0.0359(14) 0.0207(12) 0.0260(12) 0.0012(10) -0.0034(10) -0.0090(10) N8 0.0347(14) 0.0231(12) 0.0296(13) -0.0019(10) 0.0040(11) -0.0135(11) N9 0.0437(17) 0.0342(15) 0.0631(19) -0.0074(14) -0.0163(15) -0.0098(13) N10 0.0372(15) 0.0327(14) 0.0322(14) -0.0058(12) 0.0022(11) -0.0154(12) O1 0.097(2) 0.0480(15) 0.0344(13) -0.0062(11) -0.0085(13) -0.0363(15) O2 0.127(3) 0.0530(17) 0.0331(14) 0.0006(12) -0.0123(15) -0.0397(18) O3 0.0743(19) 0.0386(15) 0.090(2) -0.0068(14) 0.0076(16) -0.0398(14) Ag1 0.02573(12) 0.02624(12) 0.03757(14) -0.00162(9) -0.00404(9) -0.00977(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.350(4) . ? C1 C2 1.373(5) . ? C1 H1 0.9500 . ? C2 C3 1.382(5) . ? C2 H2 0.9500 . ? C3 C4 1.366(5) . ? C3 H3 0.9500 . ? C4 C5 1.410(4) . ? C4 H4 0.9500 . ? C5 N1 1.341(4) . ? C5 N2 1.399(4) . ? C6 N3 1.331(3) . ? C6 C7 1.397(4) . ? C6 N2 1.412(3) . ? C7 C8 1.384(4) . ? C7 H7 0.9500 . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C10 1.373(4) . ? C9 H9 0.9500 . ? C10 N3 1.338(4) . ? C10 H10 0.9500 . ? C11 N2 1.470(3) . ? C11 C12 1.513(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.388(4) . ? C12 C13 1.392(4) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.397(4) . ? C14 C18 1.522(4) . ? C15 C16 1.394(4) . ? C15 H15 0.9500 . ? C16 C17 1.389(4) . ? C16 C29 1.513(4) . ? C17 H17 0.9500 . ? C18 N5 1.465(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N4 1.351(3) . ? C19 C20 1.383(4) . ? C19 N5 1.412(3) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.372(4) . ? C22 H22 0.9500 . ? C23 N4 1.349(4) . ? C23 H23 0.9500 . ? C24 N6 1.335(3) . ? C24 N5 1.397(3) . ? C24 C25 1.402(4) . ? C25 C26 1.379(4) . ? C25 H25 0.9500 . ? C26 C27 1.389(4) . ? C26 H26 0.9500 . ? C27 C28 1.375(4) . ? C27 H27 0.9500 . ? C28 N6 1.341(4) . ? C28 H28 0.9500 . ? C29 N8 1.483(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N7 1.257(7) . ? C30 N7A 1.303(7) . ? C30 N8 1.410(4) . ? C30 C31A 1.454(8) . ? C30 C31 1.480(8) . ? C31 C32 1.376(11) . ? C31 H31 0.9500 . ? C32 C33 1.373(8) . ? C32 H32 0.9500 . ? C34 N7 1.346(10) . ? C34 C33 1.420(9) . ? C34 H34 0.9500 . ? N7A C32A 1.356(10) . ? C32A C33 1.352(8) . ? C32A H32A 0.9500 . ? C31A C34A 1.334(10) . ? C31A H31A 0.9500 . ? C34A C33 1.329(9) . ? C34A H34A 0.9500 . ? C33 H33 0.9500 . ? C35 N9 1.361(4) . ? C35 C36 1.373(5) . ? C35 N8 1.395(4) . ? C36 C37 1.345(5) . ? C36 H36 0.9500 . ? C37 C38 1.373(6) . ? C37 H37 0.9500 . ? C38 C39 1.376(6) . ? C38 H38 0.9500 . ? C39 N9 1.354(4) . ? C39 H39 0.9500 . ? N1 Ag1 2.263(2) . ? N4 Ag1 2.249(2) . ? N10 O2 1.227(3) . ? N10 O3 1.228(3) . ? N10 O1 1.239(3) . ? O1 Ag1 2.436(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.4(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 117.9(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 N2 118.6(2) . . ? N1 C5 C4 121.0(3) . . ? N2 C5 C4 120.3(3) . . ? N3 C6 C7 122.6(3) . . ? N3 C6 N2 115.3(2) . . ? C7 C6 N2 121.9(2) . . ? C8 C7 C6 118.4(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 119.4(3) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 117.7(3) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? N3 C10 C9 124.1(3) . . ? N3 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N2 C11 C12 113.9(2) . . ? N2 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N2 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 118.9(2) . . ? C17 C12 C11 119.5(2) . . ? C13 C12 C11 121.5(2) . . ? C14 C13 C12 121.1(2) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.2(2) . . ? C13 C14 C18 121.8(2) . . ? C15 C14 C18 119.0(2) . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.1(2) . . ? C17 C16 C29 117.4(2) . . ? C15 C16 C29 123.4(2) . . ? C16 C17 C12 121.1(3) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? N5 C18 C14 114.9(2) . . ? N5 C18 H18A 108.5 . . ? C14 C18 H18A 108.5 . . ? N5 C18 H18B 108.5 . . ? C14 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? N4 C19 C20 121.6(2) . . ? N4 C19 N5 117.9(2) . . ? C20 C19 N5 120.5(2) . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 118.5(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C23 C22 C21 118.9(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? N4 C23 C22 123.3(3) . . ? N4 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? N6 C24 N5 115.8(2) . . ? N6 C24 C25 122.2(2) . . ? N5 C24 C25 121.9(2) . . ? C26 C25 C24 118.4(3) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 119.8(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 117.7(3) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? N6 C28 C27 124.0(3) . . ? N6 C28 H28 118.0 . . ? C27 C28 H28 118.0 . . ? N8 C29 C16 114.8(2) . . ? N8 C29 H29A 108.6 . . ? C16 C29 H29A 108.6 . . ? N8 C29 H29B 108.6 . . ? C16 C29 H29B 108.6 . . ? H29A C29 H29B 107.5 . . ? N7 C30 N7A 118.8(5) . . ? N7 C30 N8 114.4(4) . . ? N7A C30 N8 122.2(4) . . ? N7A C30 C31A 117.8(4) . . ? N8 C30 C31A 120.0(4) . . ? N7 C30 C31 124.7(5) . . ? N8 C30 C31 120.8(4) . . ? C31A C30 C31 115.2(4) . . ? C32 C31 C30 114.0(6) . . ? C32 C31 H31 123.0 . . ? C30 C31 H31 123.0 . . ? C33 C32 C31 122.9(7) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? N7 C34 C33 123.3(7) . . ? N7 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? C30 N7 C34 118.7(6) . . ? C30 N7A C32A 121.3(6) . . ? C33 C32A N7A 121.0(7) . . ? C33 C32A H32A 119.5 . . ? N7A C32A H32A 119.5 . . ? C34A C31A C30 119.0(7) . . ? C34A C31A H31A 120.5 . . ? C30 C31A H31A 120.5 . . ? C33 C34A C31A 121.2(7) . . ? C33 C34A H34A 119.4 . . ? C31A C34A H34A 119.4 . . ? C34A C33 C32A 119.6(5) . . ? C34A C33 C32 117.6(5) . . ? C32A C33 C34 109.5(5) . . ? C32 C33 C34 116.1(5) . . ? C34A C33 H33 116.4 . . ? C32A C33 H33 123.9 . . ? C32 C33 H33 121.9 . . ? C34 C33 H33 121.9 . . ? N9 C35 C36 121.4(3) . . ? N9 C35 N8 120.2(3) . . ? C36 C35 N8 118.3(3) . . ? C37 C36 C35 119.4(3) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 121.2(4) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C39 117.7(3) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? N9 C39 C38 122.5(4) . . ? N9 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C5 N1 C1 118.4(3) . . ? C5 N1 Ag1 123.42(18) . . ? C1 N1 Ag1 112.7(2) . . ? C5 N2 C6 123.6(2) . . ? C5 N2 C11 117.0(2) . . ? C6 N2 C11 116.8(2) . . ? C6 N3 C10 117.8(2) . . ? C23 N4 C19 117.8(2) . . ? C23 N4 Ag1 115.26(18) . . ? C19 N4 Ag1 126.33(18) . . ? C24 N5 C19 121.8(2) . . ? C24 N5 C18 118.8(2) . . ? C19 N5 C18 119.2(2) . . ? C24 N6 C28 117.9(2) . . ? C35 N8 C30 125.1(3) . . ? C35 N8 C29 116.4(2) . . ? C30 N8 C29 118.5(2) . . ? C39 N9 C35 117.9(3) . . ? O2 N10 O3 121.4(3) . . ? O2 N10 O1 117.1(3) . . ? O3 N10 O1 121.5(3) . . ? N10 O1 Ag1 103.01(17) . . ? N4 Ag1 N1 139.18(8) . . ? N4 Ag1 O1 103.35(9) . . ? N1 Ag1 O1 117.12(9) . . ? 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 C3 2.0(5) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C2 C3 C4 C5 -2.1(5) . . . . ? C3 C4 C5 N1 1.7(4) . . . . ? C3 C4 C5 N2 -175.9(3) . . . . ? N3 C6 C7 C8 0.8(4) . . . . ? N2 C6 C7 C8 176.6(2) . . . . ? C6 C7 C8 C9 -0.6(4) . . . . ? C7 C8 C9 C10 -0.2(4) . . . . ? C8 C9 C10 N3 1.0(5) . . . . ? N2 C11 C12 C17 -164.8(2) . . . . ? N2 C11 C12 C13 18.0(4) . . . . ? C17 C12 C13 C14 0.2(4) . . . . ? C11 C12 C13 C14 177.5(3) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C12 C13 C14 C18 -178.4(2) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C18 C14 C15 C16 178.2(2) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C14 C15 C16 C29 176.6(3) . . . . ? C15 C16 C17 C12 -0.2(4) . . . . ? C29 C16 C17 C12 -176.8(3) . . . . ? C13 C12 C17 C16 0.0(4) . . . . ? C11 C12 C17 C16 -177.4(3) . . . . ? C13 C14 C18 N5 -8.3(4) . . . . ? C15 C14 C18 N5 173.4(2) . . . . ? N4 C19 C20 C21 2.0(4) . . . . ? N5 C19 C20 C21 -178.1(2) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C20 C21 C22 C23 -1.8(4) . . . . ? C21 C22 C23 N4 2.6(4) . . . . ? N6 C24 C25 C26 0.3(4) . . . . ? N5 C24 C25 C26 178.5(2) . . . . ? C24 C25 C26 C27 -0.1(4) . . . . ? C25 C26 C27 C28 -0.8(4) . . . . ? C26 C27 C28 N6 1.5(5) . . . . ? C17 C16 C29 N8 -155.2(2) . . . . ? C15 C16 C29 N8 28.4(4) . . . . ? N7 C30 C31 C32 4.6(8) . . . . ? N7A C30 C31 C32 -78.0(12) . . . . ? N8 C30 C31 C32 -178.5(5) . . . . ? C31A C30 C31 C32 24.1(8) . . . . ? C30 C31 C32 C33 -0.1(10) . . . . ? N7A C30 N7 C34 20.6(8) . . . . ? N8 C30 N7 C34 177.2(5) . . . . ? C31A C30 N7 C34 -71.5(14) . . . . ? C31 C30 N7 C34 -5.7(8) . . . . ? C33 C34 N7 C30 2.6(10) . . . . ? N7 C30 N7A C32A -23.1(8) . . . . ? N8 C30 N7A C32A -177.8(5) . . . . ? C31A C30 N7A C32A -1.1(8) . . . . ? C31 C30 N7A C32A 88.4(13) . . . . ? C30 N7A C32A C33 1.0(9) . . . . ? N7 C30 C31A C34A 99.9(16) . . . . ? N7A C30 C31A C34A 1.4(8) . . . . ? N8 C30 C31A C34A 178.2(5) . . . . ? C31 C30 C31A C34A -24.2(8) . . . . ? C30 C31A C34A C33 -1.6(10) . . . . ? C31A C34A C33 C32A 1.5(9) . . . . ? C31A C34A C33 C32 27.0(9) . . . . ? C31A C34A C33 C34 -64.6(15) . . . . ? N7A C32A C33 C34A -1.1(8) . . . . ? N7A C32A C33 C32 -92.1(16) . . . . ? N7A C32A C33 C34 19.4(8) . . . . ? C31 C32 C33 C34A -26.2(9) . . . . ? C31 C32 C33 C32A 75.2(15) . . . . ? C31 C32 C33 C34 -2.5(9) . . . . ? N7 C34 C33 C34A 100.7(18) . . . . ? N7 C34 C33 C32A -21.9(8) . . . . ? N7 C34 C33 C32 1.5(9) . . . . ? N9 C35 C36 C37 -1.1(5) . . . . ? N8 C35 C36 C37 175.6(3) . . . . ? C35 C36 C37 C38 1.6(5) . . . . ? C36 C37 C38 C39 -1.3(5) . . . . ? C37 C38 C39 N9 0.4(5) . . . . ? N2 C5 N1 C1 178.1(2) . . . . ? C4 C5 N1 C1 0.4(4) . . . . ? N2 C5 N1 Ag1 26.0(3) . . . . ? C4 C5 N1 Ag1 -151.7(2) . . . . ? C2 C1 N1 C5 -2.3(4) . . . . ? C2 C1 N1 Ag1 152.6(3) . . . . ? N1 C5 N2 C6 13.2(4) . . . . ? C4 C5 N2 C6 -169.0(3) . . . . ? N1 C5 N2 C11 -147.8(2) . . . . ? C4 C5 N2 C11 29.9(4) . . . . ? N3 C6 N2 C5 -141.8(3) . . . . ? C7 C6 N2 C5 42.1(4) . . . . ? N3 C6 N2 C11 19.3(3) . . . . ? C7 C6 N2 C11 -156.8(2) . . . . ? C12 C11 N2 C5 65.4(3) . . . . ? C12 C11 N2 C6 -97.0(3) . . . . ? C7 C6 N3 C10 -0.1(4) . . . . ? N2 C6 N3 C10 -176.2(2) . . . . ? C9 C10 N3 C6 -0.8(4) . . . . ? C22 C23 N4 C19 -1.1(4) . . . . ? C22 C23 N4 Ag1 -172.7(2) . . . . ? C20 C19 N4 C23 -1.3(4) . . . . ? N5 C19 N4 C23 178.8(2) . . . . ? C20 C19 N4 Ag1 169.28(19) . . . . ? N5 C19 N4 Ag1 -10.6(3) . . . . ? N6 C24 N5 C19 -174.1(2) . . . . ? C25 C24 N5 C19 7.6(4) . . . . ? N6 C24 N5 C18 10.3(3) . . . . ? C25 C24 N5 C18 -167.9(2) . . . . ? N4 C19 N5 C24 56.2(3) . . . . ? C20 C19 N5 C24 -123.7(3) . . . . ? N4 C19 N5 C18 -128.2(3) . . . . ? C20 C19 N5 C18 51.9(3) . . . . ? C14 C18 N5 C24 -85.1(3) . . . . ? C14 C18 N5 C19 99.1(3) . . . . ? N5 C24 N6 C28 -177.9(2) . . . . ? C25 C24 N6 C28 0.4(4) . . . . ? C27 C28 N6 C24 -1.3(4) . . . . ? N9 C35 N8 C30 -10.0(4) . . . . ? C36 C35 N8 C30 173.2(3) . . . . ? N9 C35 N8 C29 167.0(2) . . . . ? C36 C35 N8 C29 -9.8(4) . . . . ? N7 C30 N8 C35 168.1(4) . . . . ? N7A C30 N8 C35 -36.2(5) . . . . ? C31A C30 N8 C35 147.1(4) . . . . ? C31 C30 N8 C35 -9.2(5) . . . . ? N7 C30 N8 C29 -8.9(4) . . . . ? N7A C30 N8 C29 146.8(4) . . . . ? C31A C30 N8 C29 -29.9(5) . . . . ? C31 C30 N8 C29 173.8(4) . . . . ? C16 C29 N8 C35 84.4(3) . . . . ? C16 C29 N8 C30 -98.4(3) . . . . ? C38 C39 N9 C35 0.0(5) . . . . ? C36 C35 N9 C39 0.3(4) . . . . ? N8 C35 N9 C39 -176.4(3) . . . . ? O2 N10 O1 Ag1 -1.0(3) . . . . ? O3 N10 O1 Ag1 179.4(2) . . . . ? C23 N4 Ag1 N1 -146.43(18) . . . . ? C19 N4 Ag1 N1 42.8(3) . . . . ? C23 N4 Ag1 O1 26.1(2) . . . . ? C19 N4 Ag1 O1 -144.7(2) . . . . ? C5 N1 Ag1 N4 43.4(3) . . . . ? C1 N1 Ag1 N4 -110.2(2) . . . . ? C5 N1 Ag1 O1 -128.5(2) . . . . ? C1 N1 Ag1 O1 78.0(2) . . . . ? N10 O1 Ag1 N4 124.7(2) . . . . ? N10 O1 Ag1 N1 -60.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.628 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.081 #END