# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound2 _database_code_depnum_ccdc_archive 'CCDC 888500' #TrackingRef 'Compound 2.cif (revised).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H85 Ag6 Cl3 F36 N12 O24 P6' _chemical_formula_weight 3378.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, y+1/2, -z+1' '-x, -y, -z' 'x, y, -z' '-x, y, z-1/2' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 32.769(9) _cell_length_b 44.126(12) _cell_length_c 24.110(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 34861(16) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 42996 _cell_measurement_theta_min 2.0435 _cell_measurement_theta_max 27.3584 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13328 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8484 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 135648 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.36 _reflns_number_total 20126 _reflns_number_gt 13715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1671P)^2^+200.0000P] 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 20126 _refine_ls_number_parameters 833 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.1053 _refine_ls_wR_factor_ref 0.3247 _refine_ls_wR_factor_gt 0.2883 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.83178(5) -0.11551(4) 0.0000 0.0947(4) Uani 1 2 d S . . Ag2 Ag 0.76377(3) -0.19382(2) 0.0000 0.0545(2) Uani 1 2 d S . . Ag3 Ag 0.33871(3) 0.20055(2) 0.0000 0.0537(2) Uani 1 2 d S . . Ag4 Ag 0.39589(3) 0.27671(2) 0.0000 0.0508(2) Uani 1 2 d S . . Ag5 Ag 0.56933(2) 0.035367(15) 0.36063(4) 0.0695(2) Uani 1 1 d . . . P1 P 0.32582(8) 0.08232(6) 0.16819(12) 0.0698(7) Uani 1 1 d . . . P2 P 0.27691(13) 0.28463(8) 0.0000 0.0625(8) Uani 1 2 d S . . P3 P 0.12127(11) 0.19687(9) 0.0000 0.0664(9) Uani 1 2 d SU . . P4 P 0.54303(9) 0.18617(7) 0.5000 0.0505(7) Uani 1 2 d S . . P5 P 0.5000 0.0000 0.5000 0.0564(10) Uani 1 4 d S . . P6 P 0.5000 0.0000 0.2500 0.0561(10) Uani 1 4 d S . . F1 F 0.35546(19) 0.05933(15) 0.1982(3) 0.094(2) Uani 1 1 d . . . F2 F 0.3118(9) 0.0594(3) 0.1330(9) 0.39(2) Uani 1 1 d . . . F3 F 0.3601(3) 0.0969(3) 0.1330(4) 0.142(4) Uani 1 1 d . . . F4 F 0.2977(3) 0.1059(4) 0.1426(8) 0.287(12) Uani 1 1 d . . . F5 F 0.2951(3) 0.0752(4) 0.2147(5) 0.188(6) Uani 1 1 d . . . F6 F 0.3448(5) 0.1054(3) 0.2145(6) 0.202(6) Uani 1 1 d . . . F7 F 0.2683(5) 0.2849(3) 0.0620(4) 0.184(5) Uani 1 1 d . . . F8 F 0.3059(5) 0.2572(3) 0.0000 0.133(5) Uani 1 2 d S . . F9 F 0.2389(7) 0.2605(3) 0.0000 0.211(9) Uani 1 2 d S . . F10 F 0.2420(5) 0.3096(4) 0.0000 0.161(6) Uani 1 2 d S . . F11 F 0.3098(5) 0.3092(3) 0.0000 0.176(7) Uani 1 2 d S . . F12 F 0.1093(8) 0.2010(4) 0.0557(5) 0.299(12) Uani 1 1 d . . . F13 F 0.1558(3) 0.1745(2) 0.0000 0.109(3) Uani 1 2 d S . . F14 F 0.0934(6) 0.1687(5) 0.0000 0.249(12) Uani 1 2 d S . . F15 F 0.0840(10) 0.2219(7) 0.0000 0.272(12) Uani 1 2 d SU . . F16 F 0.1461(6) 0.2279(4) 0.0000 0.251(13) Uani 1 2 d S . . F17 F 0.5456(2) 0.18522(16) 0.5661(2) 0.0876(19) Uani 1 1 d . . . F18 F 0.57534(18) 0.21381(14) 0.5000 0.0473(13) Uani 1 2 d S . . F19 F 0.5818(3) 0.16217(18) 0.5000 0.091(3) Uani 1 2 d S . . F20 F 0.5103(3) 0.1588(3) 0.5000 0.113(4) Uani 1 2 d S . . F21 F 0.5078(3) 0.2094(3) 0.5000 0.131(4) Uani 1 2 d S . . F22 F 0.4527(3) 0.0081(2) 0.5000 0.092(3) Uani 1 2 d S . . F23 F 0.4913(2) -0.0244(2) 0.4524(3) 0.113(2) Uani 1 1 d . . . F24 F 0.5000 0.0000 0.3169(3) 0.0646(17) Uani 1 2 d S . . F25 F 0.5000 0.0340(3) 0.2500 0.234(14) Uani 1 2 d S . . F26 F 0.4564(4) 0.0146(4) 0.2467(5) 0.097(5) Uani 0.50 1 d P . . O1 O 0.8422(2) -0.13010(15) 0.2965(3) 0.0663(16) Uani 1 1 d . . . O2 O 0.78339(17) -0.10360(12) 0.2854(2) 0.0503(12) Uani 1 1 d . . . O3 O 0.6243(3) -0.1192(2) 0.3260(8) 0.177(7) Uani 1 1 d . . . O4 O 0.68563(18) -0.09938(11) 0.3399(2) 0.0529(13) Uani 1 1 d . . . O5 O 0.78320(18) -0.21521(11) 0.2943(2) 0.0519(13) Uani 1 1 d . . . O6 O 0.76205(17) -0.16665(11) 0.2866(2) 0.0475(12) Uani 1 1 d . . . O7 O 0.32122(16) 0.21166(12) 0.2951(2) 0.0499(12) Uani 1 1 d . . . O8 O 0.38313(14) 0.18869(10) 0.28700(18) 0.0386(10) Uani 1 1 d . . . O9 O 0.53180(15) 0.19066(11) 0.29837(19) 0.0437(11) Uani 1 1 d . . . O10 O 0.47439(14) 0.18001(9) 0.34702(18) 0.0352(9) Uani 1 1 d . . . O11 O 0.3847(2) 0.29942(12) 0.2948(2) 0.0609(16) Uani 1 1 d . . . O12 O 0.40470(15) 0.25057(10) 0.28771(18) 0.0406(10) Uani 1 1 d . . . N1 N 0.8286(2) -0.11453(16) 0.0892(3) 0.0572(17) Uani 1 1 d . . . N2 N 0.76458(18) -0.19444(15) 0.0884(2) 0.0446(13) Uani 1 1 d . . . N3 N 0.34170(18) 0.19970(14) 0.0894(2) 0.0422(13) Uani 1 1 d . . . N4 N 0.39827(18) 0.27747(14) 0.0881(2) 0.0436(13) Uani 1 1 d . . . N5 N 0.54430(19) 0.07993(14) 0.3477(3) 0.0500(15) Uani 1 1 d . . . N6 N 0.5968(2) -0.00870(17) 0.3619(3) 0.0640(19) Uani 1 1 d . . . C1 C 0.8018(3) -0.0963(2) 0.1174(4) 0.064(2) Uani 1 1 d . . . H1 H 0.7850 -0.0832 0.0961 0.077 Uiso 1 1 calc R . . C2 C 0.7975(3) -0.09550(18) 0.1736(4) 0.0547(19) Uani 1 1 d . . . H2 H 0.7784 -0.0823 0.1907 0.066 Uiso 1 1 calc R . . C3 C 0.8222(3) -0.11487(17) 0.2053(3) 0.0517(18) Uani 1 1 d . . . C4 C 0.8494(3) -0.13323(19) 0.1792(4) 0.0558(19) Uani 1 1 d . . . H4 H 0.8665 -0.1464 0.1999 0.067 Uiso 1 1 calc R . . C5 C 0.8516(3) -0.1325(2) 0.1222(3) 0.0538(19) Uani 1 1 d . . . H5 H 0.8707 -0.1455 0.1047 0.065 Uiso 1 1 calc R . . C6 C 0.8183(2) -0.11726(16) 0.2666(3) 0.0496(17) Uani 1 1 d . . . C7 C 0.7741(3) -0.1057(2) 0.3451(3) 0.059(2) Uani 1 1 d . . . H7A H 0.7622 -0.0863 0.3577 0.070 Uiso 1 1 calc R . . H7B H 0.7998 -0.1090 0.3658 0.070 Uiso 1 1 calc R . . C8 C 0.7447(3) -0.1310(2) 0.3587(3) 0.056(2) Uani 1 1 d . . . C9 C 0.7378(4) -0.1285(3) 0.4226(4) 0.081(3) Uani 1 1 d . . . H9A H 0.7626 -0.1347 0.4421 0.121 Uiso 1 1 calc R . . H9B H 0.7151 -0.1417 0.4335 0.121 Uiso 1 1 calc R . . H9C H 0.7312 -0.1075 0.4322 0.121 Uiso 1 1 calc R . . C10 C 0.7041(3) -0.12802(17) 0.3266(3) 0.0541(19) Uani 1 1 d . . . H10A H 0.7093 -0.1293 0.2862 0.065 Uiso 1 1 calc R . . H10B H 0.6855 -0.1448 0.3370 0.065 Uiso 1 1 calc R . . C11 C 0.6458(3) -0.09776(18) 0.3374(5) 0.070(3) Uani 1 1 d . . . C12 C 0.6298(3) -0.06579(18) 0.3455(3) 0.0545(19) Uani 1 1 d . . . C13 C 0.6540(3) -0.0413(2) 0.3393(6) 0.079(3) Uani 1 1 d . . . H13 H 0.6822 -0.0433 0.3312 0.095 Uiso 1 1 calc R . . C14 C 0.6360(3) -0.0128(2) 0.3454(6) 0.090(4) Uani 1 1 d . . . H14 H 0.6520 0.0046 0.3375 0.108 Uiso 1 1 calc R . . C15 C 0.5733(3) -0.0337(2) 0.3665(4) 0.071(3) Uani 1 1 d . . . H15 H 0.5451 -0.0315 0.3749 0.085 Uiso 1 1 calc R . . C16 C 0.5892(3) -0.0624(2) 0.3591(5) 0.075(3) Uani 1 1 d . . . H16 H 0.5723 -0.0797 0.3635 0.090 Uiso 1 1 calc R . . C17 C 0.7615(3) -0.1631(2) 0.3473(3) 0.059(2) Uani 1 1 d . . . H17A H 0.7894 -0.1653 0.3626 0.071 Uiso 1 1 calc R . . H17B H 0.7438 -0.1787 0.3645 0.071 Uiso 1 1 calc R . . C18 C 0.7731(2) -0.19403(17) 0.2662(3) 0.0436(15) Uani 1 1 d . . . C19 C 0.76917(19) -0.19356(16) 0.2039(3) 0.0417(15) Uani 1 1 d . . . C20 C 0.7531(2) -0.16923(16) 0.1756(3) 0.0459(16) Uani 1 1 d . . . H20 H 0.7434 -0.1520 0.1951 0.055 Uiso 1 1 calc R . . C21 C 0.7511(2) -0.17020(16) 0.1184(3) 0.0442(15) Uani 1 1 d . . . H21 H 0.7399 -0.1533 0.0992 0.053 Uiso 1 1 calc R . . C22 C 0.7799(2) -0.21865(18) 0.1174(3) 0.0492(17) Uani 1 1 d . . . H22 H 0.7884 -0.2360 0.0971 0.059 Uiso 1 1 calc R . . C23 C 0.7838(2) -0.21920(16) 0.1740(3) 0.0435(15) Uani 1 1 d . . . H23 H 0.7957 -0.2360 0.1926 0.052 Uiso 1 1 calc R . . C24 C 0.3617(2) 0.17737(17) 0.1162(3) 0.0425(15) Uani 1 1 d . . . H24 H 0.3740 0.1616 0.0950 0.051 Uiso 1 1 calc R . . C25 C 0.3652(2) 0.17652(16) 0.1742(3) 0.0407(14) Uani 1 1 d . . . H25 H 0.3802 0.1609 0.1920 0.049 Uiso 1 1 calc R . . C26 C 0.3463(2) 0.19882(15) 0.2047(3) 0.0378(14) Uani 1 1 d . . . C27 C 0.3246(2) 0.22209(15) 0.1772(3) 0.0397(14) Uani 1 1 d . . . H27 H 0.3113 0.2376 0.1975 0.048 Uiso 1 1 calc R . . C28 C 0.3235(2) 0.22151(16) 0.1199(3) 0.0411(14) Uani 1 1 d . . . H28 H 0.3092 0.2372 0.1012 0.049 Uiso 1 1 calc R . . C29 C 0.3484(2) 0.20092(16) 0.2666(3) 0.0405(14) Uani 1 1 d . . . C30 C 0.3891(2) 0.19047(15) 0.3463(3) 0.0377(13) Uani 1 1 d . . . H30A H 0.3997 0.1708 0.3599 0.045 Uiso 1 1 calc R . . H30B H 0.3624 0.1941 0.3645 0.045 Uiso 1 1 calc R . . C31 C 0.4191(2) 0.21596(14) 0.3630(2) 0.0341(12) Uani 1 1 d . . . C32 C 0.4227(3) 0.21391(18) 0.4277(3) 0.0486(17) Uani 1 1 d . . . H32A H 0.4452 0.2268 0.4404 0.073 Uiso 1 1 calc R . . H32B H 0.4281 0.1929 0.4385 0.073 Uiso 1 1 calc R . . H32C H 0.3971 0.2207 0.4447 0.073 Uiso 1 1 calc R . . C33 C 0.4042(2) 0.24767(15) 0.3487(3) 0.0415(15) Uani 1 1 d . . . H33A H 0.3762 0.2508 0.3631 0.050 Uiso 1 1 calc R . . H33B H 0.4224 0.2630 0.3657 0.050 Uiso 1 1 calc R . . C34 C 0.3952(2) 0.27777(16) 0.2658(3) 0.0423(15) Uani 1 1 d . . . C35 C 0.3981(2) 0.27768(14) 0.2049(3) 0.0353(13) Uani 1 1 d . . . C36 C 0.4168(2) 0.25458(14) 0.1755(3) 0.0366(13) Uani 1 1 d . . . H36 H 0.4294 0.2383 0.1946 0.044 Uiso 1 1 calc R . . C37 C 0.4168(2) 0.25529(17) 0.1175(3) 0.0441(15) Uani 1 1 d . . . H37 H 0.4305 0.2396 0.0980 0.053 Uiso 1 1 calc R . . C38 C 0.3793(3) 0.30015(19) 0.1181(3) 0.0518(18) Uani 1 1 d . . . H38 H 0.3658 0.3158 0.0983 0.062 Uiso 1 1 calc R . . C39 C 0.3790(2) 0.30125(16) 0.1756(3) 0.0461(16) Uani 1 1 d . . . H39 H 0.3662 0.3175 0.1946 0.055 Uiso 1 1 calc R . . C40 C 0.4609(2) 0.21140(16) 0.3368(3) 0.0404(14) Uani 1 1 d . . . H40A H 0.4594 0.2153 0.2964 0.049 Uiso 1 1 calc R . . H40B H 0.4807 0.2258 0.3532 0.049 Uiso 1 1 calc R . . C41 C 0.51033(19) 0.17292(15) 0.3238(3) 0.0362(13) Uani 1 1 d . . . C42 C 0.52089(19) 0.14004(16) 0.3321(3) 0.0396(14) Uani 1 1 d . . . C43 C 0.5070(2) 0.12379(15) 0.3772(3) 0.0425(15) Uani 1 1 d . . . H43 H 0.4891 0.1331 0.4030 0.051 Uiso 1 1 calc R . . C44 C 0.5190(3) 0.09406(19) 0.3852(4) 0.0551(19) Uani 1 1 d . . . H44 H 0.5096 0.0833 0.4168 0.066 Uiso 1 1 calc R . . C45 C 0.5556(2) 0.09544(19) 0.3040(3) 0.0507(18) Uani 1 1 d . . . H45 H 0.5722 0.0856 0.2772 0.061 Uiso 1 1 calc R . . C46 C 0.5447(2) 0.12520(18) 0.2946(3) 0.0463(16) Uani 1 1 d . . . H46 H 0.5538 0.1353 0.2621 0.056 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 0.1009(10) 0.1216(11) 0.0616(7) 0.000 0.000 0.0294(8) Ag2 0.0552(5) 0.0661(5) 0.0421(4) 0.000 0.000 0.0103(4) Ag3 0.0458(4) 0.0788(6) 0.0364(4) 0.000 0.000 0.0047(4) Ag4 0.0576(5) 0.0592(5) 0.0356(4) 0.000 0.000 0.0083(4) Ag5 0.0554(4) 0.0497(4) 0.1035(6) -0.0130(3) -0.0077(4) 0.0106(3) P1 0.0597(14) 0.0708(15) 0.0789(17) 0.0069(13) 0.0092(12) 0.0195(12) P2 0.088(2) 0.0573(17) 0.0419(15) 0.000 0.000 0.0122(17) P3 0.0574(17) 0.0692(19) 0.073(2) 0.000 0.000 0.0093(15) P4 0.0511(15) 0.0667(17) 0.0337(13) 0.000 0.000 -0.0156(14) P5 0.054(2) 0.060(2) 0.055(2) 0.000 0.000 0.009(2) P6 0.050(2) 0.066(3) 0.053(2) 0.000 0.000 0.000 F1 0.067(4) 0.085(4) 0.130(6) 0.023(4) -0.018(4) 0.002(3) F2 0.68(4) 0.138(10) 0.35(2) -0.113(13) -0.38(3) 0.102(17) F3 0.087(5) 0.212(11) 0.129(7) 0.076(7) 0.007(5) 0.022(6) F4 0.085(6) 0.325(19) 0.45(3) 0.30(2) 0.070(10) 0.081(9) F5 0.086(6) 0.341(18) 0.137(8) 0.040(10) 0.013(5) 0.044(9) F6 0.265(16) 0.159(10) 0.182(12) -0.048(9) 0.057(11) -0.045(11) F7 0.308(16) 0.146(9) 0.098(6) -0.033(6) 0.051(8) 0.043(10) F8 0.174(12) 0.122(9) 0.104(8) 0.000 0.000 0.083(9) F9 0.25(2) 0.093(10) 0.29(2) 0.000 0.000 -0.031(12) F10 0.165(14) 0.131(11) 0.186(15) 0.000 0.000 0.044(10) F11 0.143(13) 0.100(9) 0.28(2) 0.000 0.000 -0.012(9) F12 0.53(4) 0.253(18) 0.109(9) -0.060(10) 0.078(14) 0.02(2) F13 0.099(7) 0.082(6) 0.145(10) 0.000 0.000 -0.001(6) F14 0.155(16) 0.140(14) 0.45(4) 0.000 0.000 -0.035(12) F15 0.271(13) 0.271(13) 0.275(13) 0.000 0.000 0.001(5) F16 0.137(13) 0.101(10) 0.52(4) 0.000 0.000 -0.040(10) F17 0.093(4) 0.120(5) 0.050(3) -0.009(3) 0.008(3) -0.045(4) F18 0.048(3) 0.055(3) 0.038(3) 0.000 0.000 -0.005(3) F19 0.110(7) 0.054(4) 0.108(7) 0.000 0.000 -0.001(5) F20 0.126(8) 0.149(9) 0.062(5) 0.000 0.000 -0.082(8) F21 0.063(6) 0.145(10) 0.184(13) 0.000 0.000 0.012(6) F22 0.059(5) 0.122(8) 0.094(6) 0.000 0.000 0.006(5) F23 0.106(6) 0.137(6) 0.097(5) -0.035(5) 0.009(4) 0.005(5) F24 0.063(4) 0.073(4) 0.057(4) 0.000 0.000 0.000(4) F25 0.52(4) 0.099(10) 0.082(8) 0.000 -0.065(16) 0.000 F26 0.080(7) 0.150(14) 0.061(7) 0.011(10) 0.016(6) 0.047(8) O1 0.072(4) 0.071(4) 0.056(3) -0.005(3) -0.008(3) 0.016(3) O2 0.058(3) 0.047(3) 0.046(3) -0.004(2) 0.000(2) 0.016(2) O3 0.075(6) 0.072(6) 0.38(2) -0.016(9) 0.038(9) 0.013(5) O4 0.060(3) 0.041(3) 0.058(3) 0.000(2) 0.000(3) 0.011(2) O5 0.070(4) 0.040(3) 0.046(3) 0.001(2) -0.009(3) 0.017(2) O6 0.063(3) 0.040(2) 0.040(3) -0.006(2) -0.002(2) 0.014(2) O7 0.052(3) 0.059(3) 0.039(3) -0.001(2) 0.006(2) 0.016(2) O8 0.041(2) 0.041(2) 0.034(2) -0.0001(19) -0.0015(19) 0.008(2) O9 0.045(3) 0.048(3) 0.039(2) 0.006(2) 0.005(2) -0.003(2) O10 0.039(2) 0.033(2) 0.033(2) 0.0036(17) 0.0016(18) -0.0007(18) O11 0.096(5) 0.049(3) 0.037(3) -0.005(2) 0.005(3) 0.027(3) O12 0.053(3) 0.036(2) 0.033(2) 0.0021(18) -0.002(2) 0.011(2) N1 0.057(4) 0.062(4) 0.052(4) 0.002(3) -0.004(3) 0.013(3) N2 0.039(3) 0.056(3) 0.040(3) 0.001(3) 0.003(2) 0.004(3) N3 0.041(3) 0.052(3) 0.033(3) -0.002(2) 0.004(2) -0.004(3) N4 0.047(3) 0.051(3) 0.033(3) -0.004(2) 0.003(2) 0.010(3) N5 0.042(3) 0.039(3) 0.068(4) -0.012(3) -0.008(3) -0.003(3) N6 0.047(4) 0.058(4) 0.087(5) -0.013(4) -0.007(4) 0.010(3) C1 0.070(6) 0.065(5) 0.057(5) -0.002(4) -0.005(4) 0.010(5) C2 0.052(4) 0.049(4) 0.063(5) 0.001(4) -0.005(4) 0.013(3) C3 0.062(5) 0.042(4) 0.051(4) 0.003(3) -0.004(4) -0.001(3) C4 0.053(4) 0.053(4) 0.062(5) -0.001(4) -0.001(4) 0.017(4) C5 0.050(4) 0.062(5) 0.050(4) -0.011(4) -0.004(3) 0.015(4) C6 0.054(4) 0.039(3) 0.056(4) -0.009(3) -0.004(4) 0.012(3) C7 0.066(5) 0.059(5) 0.051(4) -0.008(4) -0.011(4) 0.020(4) C8 0.064(5) 0.057(5) 0.047(4) 0.000(4) 0.006(4) 0.023(4) C9 0.115(9) 0.081(7) 0.047(5) -0.003(5) 0.014(5) 0.039(6) C10 0.069(5) 0.044(4) 0.049(4) -0.004(3) 0.005(4) 0.017(4) C11 0.056(5) 0.035(4) 0.120(8) 0.013(4) 0.026(5) 0.004(4) C12 0.059(5) 0.050(4) 0.054(4) 0.003(4) 0.005(4) 0.014(4) C13 0.055(5) 0.044(4) 0.137(10) 0.008(5) 0.008(6) -0.001(4) C14 0.054(5) 0.049(5) 0.167(12) -0.003(6) 0.009(6) 0.004(4) C15 0.063(6) 0.068(6) 0.081(7) 0.010(5) 0.023(5) 0.018(5) C16 0.062(5) 0.050(5) 0.113(8) 0.021(5) 0.025(5) 0.017(4) C17 0.078(6) 0.060(5) 0.039(4) 0.001(3) 0.000(4) 0.018(4) C18 0.040(3) 0.047(4) 0.043(4) -0.004(3) 0.006(3) 0.005(3) C19 0.029(3) 0.050(4) 0.046(4) -0.002(3) 0.000(3) 0.003(3) C20 0.042(4) 0.043(4) 0.053(4) -0.007(3) 0.002(3) 0.005(3) C21 0.041(4) 0.039(3) 0.053(4) -0.002(3) 0.006(3) -0.001(3) C22 0.040(4) 0.054(4) 0.053(4) -0.001(3) -0.001(3) 0.011(3) C23 0.036(3) 0.042(3) 0.052(4) -0.003(3) -0.004(3) 0.006(3) C24 0.043(4) 0.051(4) 0.034(3) -0.001(3) 0.000(3) 0.006(3) C25 0.033(3) 0.049(4) 0.039(3) -0.009(3) -0.002(3) 0.011(3) C26 0.036(3) 0.042(3) 0.036(3) -0.005(3) 0.001(3) 0.007(3) C27 0.035(3) 0.043(3) 0.041(3) -0.002(3) 0.005(3) 0.001(3) C28 0.038(3) 0.044(3) 0.042(4) 0.004(3) 0.000(3) -0.001(3) C29 0.041(3) 0.047(4) 0.033(3) 0.003(3) 0.003(3) 0.010(3) C30 0.037(3) 0.044(3) 0.033(3) 0.001(3) 0.001(3) 0.000(3) C31 0.037(3) 0.035(3) 0.030(3) 0.003(2) 0.000(2) -0.001(3) C32 0.060(4) 0.054(4) 0.031(3) 0.003(3) 0.000(3) 0.003(4) C33 0.052(4) 0.040(3) 0.032(3) -0.002(3) 0.000(3) 0.010(3) C34 0.045(4) 0.043(4) 0.039(4) 0.002(3) 0.002(3) 0.009(3) C35 0.040(3) 0.034(3) 0.032(3) 0.002(2) 0.005(2) 0.008(3) C36 0.039(3) 0.036(3) 0.035(3) 0.001(3) 0.002(3) 0.005(3) C37 0.048(4) 0.046(4) 0.038(3) -0.003(3) 0.003(3) 0.007(3) C38 0.059(5) 0.055(4) 0.041(4) 0.001(3) -0.003(3) 0.011(4) C39 0.050(4) 0.039(3) 0.049(4) -0.004(3) 0.002(3) 0.007(3) C40 0.036(3) 0.050(4) 0.036(3) 0.005(3) -0.002(3) 0.002(3) C41 0.033(3) 0.044(3) 0.032(3) -0.001(3) 0.003(2) 0.001(3) C42 0.031(3) 0.054(4) 0.034(3) -0.005(3) -0.004(3) 0.000(3) C43 0.048(4) 0.039(3) 0.041(3) -0.006(3) 0.007(3) 0.002(3) C44 0.046(4) 0.057(4) 0.062(5) 0.003(4) 0.002(4) 0.004(4) C45 0.040(4) 0.060(4) 0.052(4) -0.021(4) 0.002(3) 0.005(3) C46 0.043(4) 0.056(4) 0.040(4) 0.000(3) -0.003(3) 0.008(3) _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 2.153(7) 10 ? Ag1 N1 2.153(7) . ? Ag2 N2 2.132(6) . ? Ag2 N2 2.132(6) 10 ? Ag2 Ag3 3.3713(15) 9_655 ? Ag3 N3 2.157(6) . ? Ag3 N3 2.157(6) 10 ? Ag3 Ag2 3.3713(15) 9_655 ? Ag4 N4 2.125(6) 10 ? Ag4 N4 2.125(6) . ? Ag5 N6 2.143(7) . ? Ag5 N5 2.153(6) . ? P1 F2 1.398(11) . ? P1 F4 1.522(9) . ? P1 F5 1.539(10) . ? P1 F3 1.546(9) . ? P1 F1 1.579(6) . ? P1 F6 1.633(13) . ? P2 F7 1.522(9) 10 ? P2 F7 1.522(9) . ? P2 F11 1.527(15) . ? P2 F8 1.537(11) . ? P2 F10 1.590(15) . ? P2 F9 1.638(19) . ? P3 F12 1.411(12) 10 ? P3 F12 1.411(12) . ? P3 F13 1.503(11) . ? P3 F14 1.544(19) . ? P3 F16 1.593(15) . ? P3 F15 1.65(3) . ? P4 F21 1.543(12) . ? P4 F17 1.597(5) . ? P4 F17 1.597(5) 10_556 ? P4 F18 1.615(7) . ? P4 F20 1.616(9) . ? P4 F19 1.655(10) . ? P5 F22 1.592(8) 9_656 ? P5 F22 1.592(8) . ? P5 F23 1.600(7) 9_656 ? P5 F23 1.600(7) 2_655 ? P5 F23 1.600(7) . ? P5 F23 1.600(7) 10_556 ? P6 F25 1.502(14) . ? P6 F25 1.502(14) 2_655 ? P6 F26 1.571(11) 4_655 ? P6 F26 1.571(11) . ? P6 F26 1.571(11) 2_655 ? P6 F26 1.571(11) 3 ? P6 F24 1.614(7) 3 ? P6 F24 1.614(7) . ? F25 F26 1.670(16) . ? F25 F26 1.670(16) 4_655 ? F26 F26 1.30(3) 3 ? O1 C6 1.205(10) . ? O2 C6 1.371(9) . ? O2 C7 1.476(10) . ? O3 C11 1.210(14) . ? O4 C11 1.309(11) . ? O4 C10 1.437(9) . ? O5 C18 1.201(9) . ? O6 C18 1.354(8) . ? O6 C17 1.472(9) . ? O7 C29 1.221(8) . ? O8 C29 1.352(8) . ? O8 C30 1.445(8) . ? O9 C41 1.218(8) . ? O10 C41 1.341(8) . ? O10 C40 1.474(8) . ? O11 C34 1.232(9) . ? O12 C34 1.348(8) . ? O12 C33 1.477(8) . ? N1 C5 1.352(10) . ? N1 C1 1.371(12) . ? N2 C21 1.365(9) . ? N2 C22 1.373(10) . ? N3 C24 1.349(9) . ? N3 C28 1.351(9) . ? N4 C37 1.353(9) . ? N4 C38 1.383(10) . ? N5 C45 1.310(11) . ? N5 C44 1.376(11) . ? N6 C15 1.351(13) . ? N6 C14 1.357(13) . ? C1 C2 1.364(13) . ? C1 H1 0.9500 . ? C2 C3 1.404(11) . ? C2 H2 0.9500 . ? C3 C4 1.358(11) . ? C3 C6 1.487(11) . ? C4 C5 1.377(12) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.507(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.548(12) . ? C8 C17 1.547(11) . ? C8 C9 1.559(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.518(11) . ? C12 C13 1.348(13) . ? C12 C16 1.379(12) . ? C13 C14 1.395(13) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.381(13) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.507(10) . ? C19 C20 1.377(10) . ? C19 C23 1.424(10) . ? C20 C21 1.380(11) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.370(11) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.404(10) . ? C24 H24 0.9500 . ? C25 C26 1.375(9) . ? C25 H25 0.9500 . ? C26 C27 1.414(9) . ? C26 C29 1.495(9) . ? C27 C28 1.381(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 C31 1.547(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C33 1.520(9) . ? C31 C40 1.522(9) . ? C31 C32 1.568(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.471(9) . ? C35 C36 1.384(9) . ? C35 C39 1.406(9) . ? C36 C37 1.398(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.386(11) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.505(10) . ? C42 C46 1.362(10) . ? C42 C43 1.380(10) . ? C43 C44 1.383(11) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.379(11) . ? C45 H45 0.9500 . ? C46 H46 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 N1 Ag1 N1 174.0(4) 10 . ? N2 Ag2 N2 177.9(3) . 10 ? N2 Ag2 Ag3 90.65(16) . 9_655 ? N2 Ag2 Ag3 90.65(16) 10 9_655 ? N3 Ag3 N3 174.4(3) . 10 ? N3 Ag3 Ag2 92.51(15) . 9_655 ? N3 Ag3 Ag2 92.51(15) 10 9_655 ? N4 Ag4 N4 175.4(3) 10 . ? N6 Ag5 N5 172.2(3) . . ? F2 P1 F4 92.9(11) . . ? F2 P1 F5 94.6(15) . . ? F4 P1 F5 92.2(6) . . ? F2 P1 F3 101.9(15) . . ? F4 P1 F3 86.2(5) . . ? F5 P1 F3 163.5(8) . . ? F2 P1 F1 90.8(7) . . ? F4 P1 F1 176.1(10) . . ? F5 P1 F1 86.5(5) . . ? F3 P1 F1 94.1(4) . . ? F2 P1 F6 172.1(9) . . ? F4 P1 F6 94.7(11) . . ? F5 P1 F6 83.0(7) . . ? F3 P1 F6 80.8(7) . . ? F1 P1 F6 81.5(7) . . ? F7 P2 F7 158.6(13) 10 . ? F7 P2 F11 97.1(6) 10 . ? F7 P2 F11 97.1(6) . . ? F7 P2 F8 97.0(5) 10 . ? F7 P2 F8 97.0(5) . . ? F11 P2 F8 97.1(9) . . ? F7 P2 F10 82.0(5) 10 . ? F7 P2 F10 82.0(5) . . ? F11 P2 F10 90.9(9) . . ? F8 P2 F10 172.1(9) . . ? F7 P2 F9 82.2(6) 10 . ? F7 P2 F9 82.2(6) . . ? F11 P2 F9 175.3(10) . . ? F8 P2 F9 87.7(10) . . ? F10 P2 F9 84.4(10) . . ? F12 P3 F12 144(2) 10 . ? F12 P3 F13 107.2(10) 10 . ? F12 P3 F13 107.2(10) . . ? F12 P3 F14 86.6(10) 10 . ? F12 P3 F14 86.6(10) . . ? F13 P3 F14 85.2(10) . . ? F12 P3 F16 91.7(9) 10 . ? F12 P3 F16 91.7(9) . . ? F13 P3 F16 100.4(8) . . ? F14 P3 F16 174.4(11) . . ? F12 P3 F15 72.9(10) 10 . ? F12 P3 F15 72.9(10) . . ? F13 P3 F15 179.0(12) . . ? F14 P3 F15 95.8(14) . . ? F16 P3 F15 78.6(13) . . ? F21 P4 F17 93.2(3) . . ? F21 P4 F17 93.2(3) . 10_556 ? F17 P4 F17 173.3(6) . 10_556 ? F21 P4 F18 89.4(6) . . ? F17 P4 F18 89.2(2) . . ? F17 P4 F18 89.2(2) 10_556 . ? F21 P4 F20 90.0(7) . . ? F17 P4 F20 90.8(2) . . ? F17 P4 F20 90.8(2) 10_556 . ? F18 P4 F20 179.4(6) . . ? F21 P4 F19 178.2(6) . . ? F17 P4 F19 86.7(3) . . ? F17 P4 F19 86.7(3) 10_556 . ? F18 P4 F19 88.8(4) . . ? F20 P4 F19 91.8(6) . . ? F22 P5 F22 180.0 9_656 . ? F22 P5 F23 88.8(4) 9_656 9_656 ? F22 P5 F23 91.2(4) . 9_656 ? F22 P5 F23 88.8(4) 9_656 2_655 ? F22 P5 F23 91.2(4) . 2_655 ? F23 P5 F23 91.6(7) 9_656 2_655 ? F22 P5 F23 91.2(4) 9_656 . ? F22 P5 F23 88.8(4) . . ? F23 P5 F23 180.0 9_656 . ? F23 P5 F23 88.4(7) 2_655 . ? F22 P5 F23 91.2(4) 9_656 10_556 ? F22 P5 F23 88.8(4) . 10_556 ? F23 P5 F23 88.4(7) 9_656 10_556 ? F23 P5 F23 180.0 2_655 10_556 ? F23 P5 F23 91.6(7) . 10_556 ? F25 P6 F25 180.0 . 2_655 ? F25 P6 F26 65.8(6) . 4_655 ? F25 P6 F26 114.2(6) 2_655 4_655 ? F25 P6 F26 65.8(6) . . ? F25 P6 F26 114.2(6) 2_655 . ? F26 P6 F26 131.6(12) 4_655 . ? F25 P6 F26 114.2(6) . 2_655 ? F25 P6 F26 65.8(6) 2_655 2_655 ? F26 P6 F26 48.8(12) 4_655 2_655 ? F26 P6 F26 174.2(9) . 2_655 ? F25 P6 F26 114.2(6) . 3 ? F25 P6 F26 65.8(6) 2_655 3 ? F26 P6 F26 174.2(9) 4_655 3 ? F26 P6 F26 48.8(12) . 3 ? F26 P6 F26 131.6(12) 2_655 3 ? F25 P6 F24 90.0 . 3 ? F25 P6 F24 90.0 2_655 3 ? F26 P6 F24 92.9(5) 4_655 3 ? F26 P6 F24 87.1(5) . 3 ? F26 P6 F24 87.1(5) 2_655 3 ? F26 P6 F24 92.9(5) 3 3 ? F25 P6 F24 90.0 . . ? F25 P6 F24 90.0 2_655 . ? F26 P6 F24 87.1(5) 4_655 . ? F26 P6 F24 92.9(5) . . ? F26 P6 F24 92.9(5) 2_655 . ? F26 P6 F24 87.1(5) 3 . ? F24 P6 F24 180.0 3 . ? P6 F25 F26 59.1(6) . . ? P6 F25 F26 59.1(6) . 4_655 ? F26 F25 F26 118.2(12) . 4_655 ? F26 F26 P6 65.6(6) 3 . ? F26 F26 F25 120.3(6) 3 . ? P6 F26 F25 55.1(6) . . ? C6 O2 C7 117.9(6) . . ? C11 O4 C10 117.2(7) . . ? C18 O6 C17 117.3(6) . . ? C29 O8 C30 116.9(5) . . ? C41 O10 C40 114.4(5) . . ? C34 O12 C33 117.7(5) . . ? C5 N1 C1 114.1(7) . . ? C5 N1 Ag1 123.3(6) . . ? C1 N1 Ag1 122.5(6) . . ? C21 N2 C22 117.3(6) . . ? C21 N2 Ag2 121.0(5) . . ? C22 N2 Ag2 121.6(5) . . ? C24 N3 C28 118.3(6) . . ? C24 N3 Ag3 120.9(5) . . ? C28 N3 Ag3 120.8(5) . . ? C37 N4 C38 116.8(6) . . ? C37 N4 Ag4 121.9(5) . . ? C38 N4 Ag4 121.2(5) . . ? C45 N5 C44 117.5(7) . . ? C45 N5 Ag5 119.1(5) . . ? C44 N5 Ag5 123.3(6) . . ? C15 N6 C14 117.0(8) . . ? C15 N6 Ag5 120.2(6) . . ? C14 N6 Ag5 121.0(7) . . ? C2 C1 N1 125.1(8) . . ? C2 C1 H1 117.4 . . ? N1 C1 H1 117.4 . . ? C1 C2 C3 117.7(8) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C4 C3 C2 119.3(8) . . ? C4 C3 C6 118.2(7) . . ? C2 C3 C6 122.3(7) . . ? C3 C4 C5 118.9(8) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 124.9(7) . . ? N1 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? O1 C6 O2 123.4(7) . . ? O1 C6 C3 125.0(7) . . ? O2 C6 C3 111.6(7) . . ? O2 C7 C8 113.1(7) . . ? O2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? O2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C10 112.2(7) . . ? C7 C8 C17 114.4(7) . . ? C10 C8 C17 107.1(7) . . ? C7 C8 C9 104.8(8) . . ? C10 C8 C9 111.3(7) . . ? C17 C8 C9 107.0(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C8 108.9(6) . . ? O4 C10 H10A 109.9 . . ? C8 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C8 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O3 C11 O4 123.3(8) . . ? O3 C11 C12 123.7(9) . . ? O4 C11 C12 112.9(8) . . ? C13 C12 C16 120.4(8) . . ? C13 C12 C11 121.9(8) . . ? C16 C12 C11 117.6(8) . . ? C12 C13 C14 117.6(9) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? N6 C14 C13 123.4(9) . . ? N6 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? N6 C15 C16 121.6(9) . . ? N6 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C12 119.6(9) . . ? C15 C16 H16 120.2 . . ? C12 C16 H16 120.2 . . ? O6 C17 C8 106.1(6) . . ? O6 C17 H17A 110.5 . . ? C8 C17 H17A 110.5 . . ? O6 C17 H17B 110.5 . . ? C8 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? O5 C18 O6 124.2(7) . . ? O5 C18 C19 126.6(7) . . ? O6 C18 C19 109.1(6) . . ? C20 C19 C23 119.8(7) . . ? C20 C19 C18 122.5(6) . . ? C23 C19 C18 117.7(6) . . ? C19 C20 C21 119.3(7) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N2 C21 C20 122.5(7) . . ? N2 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C23 C22 N2 123.7(7) . . ? C23 C22 H22 118.2 . . ? N2 C22 H22 118.2 . . ? C22 C23 C19 117.3(7) . . ? C22 C23 H23 121.3 . . ? C19 C23 H23 121.3 . . ? N3 C24 C25 122.4(6) . . ? N3 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C26 C25 C24 118.6(6) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 119.6(6) . . ? C25 C26 C29 123.9(6) . . ? C27 C26 C29 116.5(6) . . ? C28 C27 C26 118.0(6) . . ? C28 C27 H27 121.0 . . ? C26 C27 H27 121.0 . . ? N3 C28 C27 123.1(6) . . ? N3 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? O7 C29 O8 124.3(6) . . ? O7 C29 C26 123.5(6) . . ? O8 C29 C26 112.1(5) . . ? O8 C30 C31 112.5(5) . . ? O8 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? O8 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C33 C31 C40 108.4(5) . . ? C33 C31 C30 114.0(6) . . ? C40 C31 C30 111.6(5) . . ? C33 C31 C32 107.6(5) . . ? C40 C31 C32 109.7(6) . . ? C30 C31 C32 105.3(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C33 C31 107.5(5) . . ? O12 C33 H33A 110.2 . . ? C31 C33 H33A 110.2 . . ? O12 C33 H33B 110.2 . . ? C31 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? O11 C34 O12 122.1(6) . . ? O11 C34 C35 125.9(6) . . ? O12 C34 C35 112.0(6) . . ? C36 C35 C39 118.9(6) . . ? C36 C35 C34 122.9(6) . . ? C39 C35 C34 118.1(6) . . ? C35 C36 C37 119.8(6) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? N4 C37 C36 122.6(6) . . ? N4 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? N4 C38 C39 123.5(7) . . ? N4 C38 H38 118.2 . . ? C39 C38 H38 118.2 . . ? C38 C39 C35 118.2(7) . . ? C38 C39 H39 120.9 . . ? C35 C39 H39 120.9 . . ? O10 C40 C31 109.0(5) . . ? O10 C40 H40A 109.9 . . ? C31 C40 H40A 109.9 . . ? O10 C40 H40B 109.9 . . ? C31 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O9 C41 O10 124.6(6) . . ? O9 C41 C42 123.6(6) . . ? O10 C41 C42 111.8(5) . . ? C46 C42 C43 117.5(7) . . ? C46 C42 C41 120.5(6) . . ? C43 C42 C41 122.0(6) . . ? C44 C43 C42 120.6(7) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? N5 C44 C43 120.6(8) . . ? N5 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? N5 C45 C46 123.9(7) . . ? N5 C45 H45 118.0 . . ? C46 C45 H45 118.1 . . ? C42 C46 C45 119.7(7) . . ? C42 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? 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 F26 P6 F25 F26 180.0 4_655 . . . ? F26 P6 F25 F26 173.7(10) 2_655 . . . ? F26 P6 F25 F26 -6.3(10) 3 . . . ? F24 P6 F25 F26 86.8(5) 3 . . . ? F24 P6 F25 F26 -93.2(5) . . . . ? F26 P6 F25 F26 180.0 . . . 4_655 ? F26 P6 F25 F26 -6.3(10) 2_655 . . 4_655 ? F26 P6 F25 F26 173.7(10) 3 . . 4_655 ? F24 P6 F25 F26 -93.2(5) 3 . . 4_655 ? F24 P6 F25 F26 86.8(5) . . . 4_655 ? F25 P6 F26 F26 -172.3(13) . . . 3 ? F25 P6 F26 F26 7.7(12) 2_655 . . 3 ? F26 P6 F26 F26 -172.3(12) 4_655 . . 3 ? F24 P6 F26 F26 96.4(11) 3 . . 3 ? F24 P6 F26 F26 -83.6(11) . . . 3 ? F25 P6 F26 F25 180.0 2_655 . . . ? F26 P6 F26 F25 0.0 4_655 . . . ? F26 P6 F26 F25 172.3(13) 3 . . . ? F24 P6 F26 F25 -91.3(2) 3 . . . ? F24 P6 F26 F25 88.7(2) . . . . ? P6 F25 F26 F26 8.1(13) . . . 3 ? F26 F25 F26 F26 8.1(13) 4_655 . . 3 ? F26 F25 F26 P6 0.0 4_655 . . . ? Ag3 Ag2 N2 C21 -72.3(5) 9_655 . . . ? Ag3 Ag2 N2 C22 110.0(6) 9_655 . . . ? Ag2 Ag3 N3 C24 117.7(5) 9_655 . . . ? Ag2 Ag3 N3 C28 -62.2(5) 9_655 . . . ? C5 N1 C1 C2 -0.2(14) . . . . ? Ag1 N1 C1 C2 177.5(7) . . . . ? N1 C1 C2 C3 -0.1(14) . . . . ? C1 C2 C3 C4 0.5(13) . . . . ? C1 C2 C3 C6 -176.3(8) . . . . ? C2 C3 C4 C5 -0.5(13) . . . . ? C6 C3 C4 C5 176.4(8) . . . . ? C1 N1 C5 C4 0.2(13) . . . . ? Ag1 N1 C5 C4 -177.6(7) . . . . ? C3 C4 C5 N1 0.2(14) . . . . ? C7 O2 C6 O1 -2.1(11) . . . . ? C7 O2 C6 C3 176.4(7) . . . . ? C4 C3 C6 O1 14.1(13) . . . . ? C2 C3 C6 O1 -169.0(8) . . . . ? C4 C3 C6 O2 -164.3(7) . . . . ? C2 C3 C6 O2 12.5(11) . . . . ? C6 O2 C7 C8 -96.8(8) . . . . ? O2 C7 C8 C10 -57.0(9) . . . . ? O2 C7 C8 C17 65.2(9) . . . . ? O2 C7 C8 C9 -177.9(7) . . . . ? C11 O4 C10 C8 -151.4(8) . . . . ? C7 C8 C10 O4 -58.6(8) . . . . ? C17 C8 C10 O4 175.1(7) . . . . ? C9 C8 C10 O4 58.4(9) . . . . ? C10 O4 C11 O3 2.1(18) . . . . ? C10 O4 C11 C12 -173.2(7) . . . . ? O3 C11 C12 C13 -157.0(15) . . . . ? O4 C11 C12 C13 18.2(15) . . . . ? O3 C11 C12 C16 22.6(19) . . . . ? O4 C11 C12 C16 -162.2(9) . . . . ? C16 C12 C13 C14 -2.3(17) . . . . ? C11 C12 C13 C14 177.3(11) . . . . ? C15 N6 C14 C13 -7.7(19) . . . . ? Ag5 N6 C14 C13 -172.5(10) . . . . ? C12 C13 C14 N6 6(2) . . . . ? C14 N6 C15 C16 5.3(16) . . . . ? Ag5 N6 C15 C16 170.2(8) . . . . ? N6 C15 C16 C12 -1.7(17) . . . . ? C13 C12 C16 C15 0.1(16) . . . . ? C11 C12 C16 C15 -179.5(10) . . . . ? C18 O6 C17 C8 -175.6(7) . . . . ? C7 C8 C17 O6 -72.7(9) . . . . ? C10 C8 C17 O6 52.3(9) . . . . ? C9 C8 C17 O6 171.7(8) . . . . ? C17 O6 C18 O5 -1.6(11) . . . . ? C17 O6 C18 C19 176.5(7) . . . . ? O5 C18 C19 C20 172.7(8) . . . . ? O6 C18 C19 C20 -5.4(9) . . . . ? O5 C18 C19 C23 -8.8(11) . . . . ? O6 C18 C19 C23 173.1(6) . . . . ? C23 C19 C20 C21 0.4(10) . . . . ? C18 C19 C20 C21 178.9(7) . . . . ? C22 N2 C21 C20 1.1(10) . . . . ? Ag2 N2 C21 C20 -176.7(5) . . . . ? C19 C20 C21 N2 -0.1(11) . . . . ? C21 N2 C22 C23 -2.6(11) . . . . ? Ag2 N2 C22 C23 175.2(6) . . . . ? N2 C22 C23 C19 2.9(11) . . . . ? C20 C19 C23 C22 -1.7(10) . . . . ? C18 C19 C23 C22 179.7(7) . . . . ? C28 N3 C24 C25 -1.7(10) . . . . ? Ag3 N3 C24 C25 178.4(5) . . . . ? N3 C24 C25 C26 2.0(11) . . . . ? C24 C25 C26 C27 -0.8(10) . . . . ? C24 C25 C26 C29 -178.6(7) . . . . ? C25 C26 C27 C28 -0.4(10) . . . . ? C29 C26 C27 C28 177.5(6) . . . . ? C24 N3 C28 C27 0.4(10) . . . . ? Ag3 N3 C28 C27 -179.7(5) . . . . ? C26 C27 C28 N3 0.7(10) . . . . ? C30 O8 C29 O7 -4.3(10) . . . . ? C30 O8 C29 C26 177.8(5) . . . . ? C25 C26 C29 O7 -149.9(8) . . . . ? C27 C26 C29 O7 32.4(10) . . . . ? C25 C26 C29 O8 28.1(10) . . . . ? C27 C26 C29 O8 -149.7(6) . . . . ? C29 O8 C30 C31 -101.6(7) . . . . ? O8 C30 C31 C33 63.9(7) . . . . ? O8 C30 C31 C40 -59.5(7) . . . . ? O8 C30 C31 C32 -178.4(5) . . . . ? C34 O12 C33 C31 -175.6(6) . . . . ? C40 C31 C33 O12 56.0(7) . . . . ? C30 C31 C33 O12 -69.0(7) . . . . ? C32 C31 C33 O12 174.6(6) . . . . ? C33 O12 C34 O11 -3.1(10) . . . . ? C33 O12 C34 C35 178.2(6) . . . . ? O11 C34 C35 C36 168.4(8) . . . . ? O12 C34 C35 C36 -13.0(10) . . . . ? O11 C34 C35 C39 -15.5(12) . . . . ? O12 C34 C35 C39 163.1(6) . . . . ? C39 C35 C36 C37 1.1(10) . . . . ? C34 C35 C36 C37 177.2(7) . . . . ? C38 N4 C37 C36 0.9(11) . . . . ? Ag4 N4 C37 C36 -176.4(5) . . . . ? C35 C36 C37 N4 -1.9(11) . . . . ? C37 N4 C38 C39 0.8(12) . . . . ? Ag4 N4 C38 C39 178.2(6) . . . . ? N4 C38 C39 C35 -1.6(12) . . . . ? C36 C35 C39 C38 0.5(11) . . . . ? C34 C35 C39 C38 -175.7(7) . . . . ? C41 O10 C40 C31 177.3(5) . . . . ? C33 C31 C40 O10 -176.1(5) . . . . ? C30 C31 C40 O10 -49.7(7) . . . . ? C32 C31 C40 O10 66.7(7) . . . . ? C40 O10 C41 O9 3.4(9) . . . . ? C40 O10 C41 C42 -175.8(5) . . . . ? O9 C41 C42 C46 -27.5(10) . . . . ? O10 C41 C42 C46 151.7(6) . . . . ? O9 C41 C42 C43 152.7(7) . . . . ? O10 C41 C42 C43 -28.2(9) . . . . ? C46 C42 C43 C44 3.6(11) . . . . ? C41 C42 C43 C44 -176.6(7) . . . . ? C45 N5 C44 C43 -1.7(11) . . . . ? Ag5 N5 C44 C43 173.7(6) . . . . ? C42 C43 C44 N5 -1.3(12) . . . . ? C44 N5 C45 C46 2.4(11) . . . . ? Ag5 N5 C45 C46 -173.3(6) . . . . ? C43 C42 C46 C45 -3.0(10) . . . . ? C41 C42 C46 C45 177.2(6) . . . . ? N5 C45 C46 C42 0.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.876 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.158 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.021 7098.3 944.7 2 0.500 0.500 -0.024 7098.5 944.7 _platon_squeeze_details ; 1 CHCl3 molecule was removed by the SQUEEZE process ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 888501' #TrackingRef 'Compound1.cif (revised).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46.50 H42.50 Ag3 Cl4.50 N6 O24' _chemical_formula_weight 1552.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P42/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 23.153(4) _cell_length_b 23.153(4) _cell_length_c 23.880(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12801(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 32885 _cell_measurement_theta_min 2.1111 _cell_measurement_theta_max 27.6923 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6184 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7991 _exptl_absorpt_correction_T_max 0.7991 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98593 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.66 _reflns_number_total 7644 _reflns_number_gt 6958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1163P)^2^+30.0000P] 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 7644 _refine_ls_number_parameters 402 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2456 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.006 _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 0.05506(3) 0.12279(3) 0.0000 0.0703(2) Uani 1 2 d S . . Ag2 Ag 0.20108(5) 0.07381(4) 0.0000 0.0981(4) Uani 1 2 d S . . Ag3 Ag 0.0000 0.5000 0.33087(5) 0.1027(4) Uani 1 2 d S . . Cl1 Cl -0.09391(10) 0.04759(9) 0.0000 0.0648(5) Uani 1 2 d S . . Cl2 Cl 0.19035(12) 0.23763(12) 0.0000 0.0801(7) Uani 1 2 d S . . Cl3 Cl 0.10084(11) 0.60084(11) 0.2500 0.1390(18) Uani 1 2 d SD . . O1 O 0.2493(2) 0.00582(16) 0.28557(18) 0.0723(12) Uani 1 1 d . . . O2 O 0.22990(19) 0.09959(16) 0.28645(15) 0.0621(10) Uani 1 1 d . . . O3 O 0.0947(3) 0.0544(2) 0.2856(2) 0.114(2) Uani 1 1 d . . . O4 O 0.11614(17) 0.14694(15) 0.28922(15) 0.0542(8) Uani 1 1 d . . . O5 O 0.24022(19) 0.31341(18) 0.3065(2) 0.0802(14) Uani 1 1 d . . . O6 O 0.17587(14) 0.25361(14) 0.34496(15) 0.0491(8) Uani 1 1 d . . . O7 O -0.0924(6) -0.0139(4) 0.0000 0.146(4) Uani 1 2 d S . . O8 O -0.1537(4) 0.0620(4) 0.0000 0.117(3) Uani 1 2 d S . . O9 O -0.0686(4) 0.0697(5) -0.0458(4) 0.182(5) Uani 1 1 d . . . O10 O 0.2432(7) 0.2063(8) 0.0000 0.213(8) Uani 1 2 d S . . O11 O 0.1459(7) 0.1988(8) 0.0000 0.207(8) Uani 1 2 d S . . O12 O 0.1920(6) 0.2650(6) 0.0485(5) 0.225(6) Uani 1 1 d . . . O13 O 0.1345(12) 0.6309(12) 0.2091(11) 0.43(3) Uani 0.50 1 d PDU . . O14 O 0.0747(7) 0.5495(6) 0.2305(8) 0.172(7) Uani 0.50 1 d PDU . . O15 O 0.0562(5) 0.6396(6) 0.2711(7) 0.136(5) Uani 0.50 1 d PDU . . O16 O 0.1384(9) 0.5904(10) 0.2969(8) 0.231(11) Uani 0.50 1 d PDU . . N1 N 0.0619(2) 0.1208(2) 0.09019(19) 0.0559(10) Uani 1 1 d . . . N2 N 0.2134(3) 0.0673(2) 0.0878(2) 0.0702(13) Uani 1 1 d . . . N3 N 0.0657(3) 0.4353(2) 0.3363(3) 0.090(2) Uani 1 1 d . . . C1 C 0.2107(4) 0.0168(3) 0.1138(3) 0.083(2) Uani 1 1 d . . . H1 H 0.2017 -0.0157 0.0926 0.099 Uiso 1 1 calc R . . C2 C 0.2202(4) 0.0097(3) 0.1685(3) 0.0741(18) Uani 1 1 d . . . H2 H 0.2178 -0.0268 0.1847 0.089 Uiso 1 1 calc R . . C3 C 0.2335(2) 0.0572(2) 0.2007(2) 0.0493(11) Uani 1 1 d . . . C4 C 0.2359(3) 0.1092(3) 0.1746(3) 0.0718(17) Uani 1 1 d . . . H4 H 0.2439 0.1424 0.1950 0.086 Uiso 1 1 calc R . . C5 C 0.2266(3) 0.1124(3) 0.1188(3) 0.0740(18) Uani 1 1 d . . . H5 H 0.2297 0.1483 0.1014 0.089 Uiso 1 1 calc R . . C6 C 0.2398(2) 0.0499(2) 0.2619(2) 0.0508(11) Uani 1 1 d . . . C7 C 0.2290(3) 0.1020(2) 0.3467(2) 0.0608(14) Uani 1 1 d . . . H7A H 0.2679 0.1068 0.3612 0.073 Uiso 1 1 calc R . . H7B H 0.2130 0.0666 0.3619 0.073 Uiso 1 1 calc R . . C8 C 0.1919(2) 0.1531(2) 0.3631(2) 0.0487(11) Uani 1 1 d . . . C9 C 0.1947(3) 0.1583(3) 0.4268(2) 0.0611(13) Uani 1 1 d . . . H9A H 0.1689 0.1882 0.4391 0.092 Uiso 1 1 calc R . . H9B H 0.2334 0.1678 0.4380 0.092 Uiso 1 1 calc R . . H9C H 0.1836 0.1223 0.4435 0.092 Uiso 1 1 calc R . . C10 C 0.1289(2) 0.1432(2) 0.3486(2) 0.0542(12) Uani 1 1 d . . . H10A H 0.1176 0.1052 0.3620 0.065 Uiso 1 1 calc R . . H10B H 0.1056 0.1714 0.3683 0.065 Uiso 1 1 calc R . . C11 C 0.0978(3) 0.1007(2) 0.2635(2) 0.0554(12) Uani 1 1 d . . . C12 C 0.08535(19) 0.1096(2) 0.2034(2) 0.0440(10) Uani 1 1 d . . . C13 C 0.0644(2) 0.0637(2) 0.1724(2) 0.0567(13) Uani 1 1 d . . . H13 H 0.0583 0.0279 0.1891 0.068 Uiso 1 1 calc R . . C14 C 0.0529(3) 0.0716(3) 0.1172(2) 0.0594(13) Uani 1 1 d . . . H14 H 0.0379 0.0407 0.0971 0.071 Uiso 1 1 calc R . . C15 C 0.0812(3) 0.1649(3) 0.1207(2) 0.0631(14) Uani 1 1 d . . . H15 H 0.0876 0.2001 0.1029 0.076 Uiso 1 1 calc R . . C16 C 0.0922(3) 0.1611(2) 0.1767(2) 0.0617(14) Uani 1 1 d . . . H16 H 0.1042 0.1935 0.1965 0.074 Uiso 1 1 calc R . . C17 C 0.2151(2) 0.2068(2) 0.3343(2) 0.0489(11) Uani 1 1 d . . . H17A H 0.2531 0.2162 0.3487 0.059 Uiso 1 1 calc R . . H17B H 0.2183 0.2002 0.2943 0.059 Uiso 1 1 calc R . . C18 C 0.1940(2) 0.3050(2) 0.3275(2) 0.0557(12) Uani 1 1 d . . . C19 C 0.1493(2) 0.3502(2) 0.3332(3) 0.0570(12) Uani 1 1 d . . . C20 C 0.0948(3) 0.3386(3) 0.3552(4) 0.089(2) Uani 1 1 d . . . H20 H 0.0859 0.3024 0.3697 0.107 Uiso 1 1 calc R . . C21 C 0.0546(3) 0.3823(4) 0.3548(5) 0.112(4) Uani 1 1 d . . . H21 H 0.0177 0.3744 0.3682 0.135 Uiso 1 1 calc R . . C22 C 0.1186(3) 0.4449(3) 0.3168(4) 0.089(2) Uani 1 1 d . . . H22 H 0.1272 0.4818 0.3039 0.107 Uiso 1 1 calc R . . C23 C 0.1605(3) 0.4043(2) 0.3143(3) 0.0750(19) Uani 1 1 d . . . H23 H 0.1967 0.4134 0.2999 0.090 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 0.0826(5) 0.0863(5) 0.0422(3) 0.000 0.000 -0.0021(4) Ag2 0.1427(9) 0.1056(7) 0.0462(4) 0.000 0.000 -0.0139(6) Ag3 0.0897(6) 0.0691(5) 0.1493(10) 0.000 0.000 0.0295(4) Cl1 0.0862(14) 0.0614(11) 0.0469(9) 0.000 0.000 0.0124(10) Cl2 0.0871(16) 0.0889(16) 0.0644(13) 0.000 0.000 -0.0261(13) Cl3 0.0750(11) 0.0750(11) 0.267(6) 0.0298(17) -0.0298(17) 0.0092(14) O1 0.109(3) 0.0423(19) 0.066(2) 0.0080(18) -0.005(2) 0.014(2) O2 0.093(3) 0.0466(19) 0.0462(19) 0.0012(15) 0.0038(19) 0.0191(18) O3 0.198(7) 0.066(3) 0.077(3) 0.021(2) -0.041(4) -0.054(4) O4 0.066(2) 0.0517(19) 0.0449(18) 0.0047(15) -0.0050(16) -0.0131(16) O5 0.060(2) 0.057(2) 0.124(4) 0.011(2) 0.022(3) -0.0062(18) O6 0.0471(17) 0.0407(16) 0.060(2) 0.0005(15) 0.0048(15) 0.0021(13) O7 0.191(12) 0.082(6) 0.166(11) 0.000 0.000 0.024(7) O8 0.080(5) 0.119(7) 0.151(9) 0.000 0.000 0.003(5) O9 0.155(7) 0.224(10) 0.167(8) 0.123(7) 0.075(6) 0.061(7) O10 0.144(12) 0.190(15) 0.31(2) 0.000 0.000 0.026(11) O11 0.185(13) 0.262(18) 0.175(13) 0.000 0.000 -0.140(14) O12 0.234(12) 0.265(13) 0.177(9) -0.157(9) -0.021(8) -0.029(10) O13 0.43(3) 0.43(3) 0.43(3) 0.004(5) 0.001(5) -0.002(5) O14 0.177(8) 0.165(8) 0.175(8) 0.000(5) -0.014(5) 0.001(5) O15 0.131(6) 0.132(6) 0.144(6) -0.010(5) -0.009(5) 0.010(5) O16 0.229(12) 0.227(12) 0.236(12) -0.005(5) -0.015(5) 0.000(5) N1 0.061(3) 0.066(3) 0.041(2) -0.0014(19) 0.0006(18) -0.002(2) N2 0.089(4) 0.072(3) 0.050(3) -0.002(2) -0.002(3) -0.002(3) N3 0.071(4) 0.054(3) 0.144(6) 0.013(3) 0.003(4) 0.011(2) C1 0.129(6) 0.061(4) 0.059(3) -0.009(3) -0.011(4) -0.016(4) C2 0.108(5) 0.053(3) 0.062(3) -0.004(3) -0.001(3) -0.004(3) C3 0.048(2) 0.046(2) 0.053(3) -0.005(2) 0.006(2) 0.0080(19) C4 0.113(5) 0.047(3) 0.056(3) -0.001(2) 0.000(3) -0.005(3) C5 0.116(5) 0.056(3) 0.050(3) 0.004(3) 0.000(3) -0.004(3) C6 0.053(3) 0.044(2) 0.056(3) -0.005(2) 0.002(2) 0.011(2) C7 0.089(4) 0.053(3) 0.041(2) 0.004(2) 0.008(3) 0.017(3) C8 0.059(3) 0.047(2) 0.040(2) 0.0048(19) -0.001(2) -0.001(2) C9 0.077(4) 0.064(3) 0.042(3) 0.000(2) -0.002(2) 0.000(3) C10 0.067(3) 0.056(3) 0.040(2) 0.008(2) 0.001(2) -0.012(2) C11 0.068(3) 0.051(3) 0.047(3) 0.007(2) -0.002(2) -0.011(2) C12 0.039(2) 0.044(2) 0.050(2) 0.0029(19) 0.0038(19) -0.0060(17) C13 0.066(3) 0.052(3) 0.052(3) 0.001(2) -0.002(2) -0.013(2) C14 0.065(3) 0.063(3) 0.050(3) -0.010(2) -0.001(2) -0.010(3) C15 0.085(4) 0.057(3) 0.048(3) 0.006(2) -0.003(3) -0.012(3) C16 0.080(4) 0.052(3) 0.052(3) -0.002(2) -0.007(3) -0.008(3) C17 0.052(3) 0.039(2) 0.055(3) 0.000(2) 0.005(2) 0.0014(19) C18 0.060(3) 0.042(2) 0.065(3) -0.005(2) 0.006(3) -0.010(2) C19 0.055(3) 0.047(3) 0.068(3) 0.003(2) 0.000(2) -0.005(2) C20 0.068(4) 0.056(3) 0.143(7) 0.022(4) 0.026(4) 0.004(3) C21 0.066(4) 0.078(5) 0.193(11) 0.033(6) 0.037(5) 0.013(3) C22 0.077(4) 0.043(3) 0.148(8) 0.017(4) -0.009(5) -0.005(3) C23 0.059(3) 0.044(3) 0.121(6) 0.012(3) 0.007(4) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.160(5) . ? Ag1 N1 2.160(5) 11 ? Ag2 N2 2.123(5) . ? Ag2 N2 2.123(5) 11 ? Ag3 N3 2.139(5) . ? Ag3 N3 2.139(5) 3_565 ? Ag3 O14 2.539(13) 8 ? Ag3 O14 2.539(13) 7_455 ? Cl1 O9 1.342(7) . ? Cl1 O9 1.342(7) 11 ? Cl1 O7 1.424(10) . ? Cl1 O8 1.423(9) . ? Cl2 O12 1.320(8) . ? Cl2 O12 1.320(8) 11 ? Cl2 O11 1.367(12) . ? Cl2 O10 1.423(16) . ? Cl3 O14 1.413(8) 7_455 ? Cl3 O14 1.413(8) . ? Cl3 O13 1.430(9) 7_455 ? Cl3 O13 1.430(9) . ? Cl3 O16 1.439(9) . ? Cl3 O16 1.439(9) 7_455 ? Cl3 O15 1.459(8) 7_455 ? Cl3 O15 1.459(8) . ? O1 C6 1.188(6) . ? O2 C6 1.311(6) . ? O2 C7 1.441(6) . ? O3 C11 1.197(7) . ? O4 C11 1.306(6) . ? O4 C10 1.451(6) . ? O5 C18 1.198(7) . ? O6 C18 1.329(6) . ? O6 C17 1.436(6) . ? O13 O16 1.05(4) 7_455 ? O14 O14 1.24(3) 7_455 ? O14 O15 1.51(2) 7_455 ? O14 Ag3 2.539(13) 7_455 ? O15 O14 1.51(2) 7_455 ? O15 O16 1.81(2) 7_455 ? O16 O13 1.05(4) 7_455 ? O16 O15 1.81(2) 7_455 ? N1 C14 1.324(7) . ? N1 C15 1.332(7) . ? N2 C5 1.317(8) . ? N2 C1 1.324(9) . ? N3 C21 1.329(10) . ? N3 C22 1.329(10) . ? C1 C2 1.336(9) . ? C1 H1 0.9300 . ? C2 C3 1.376(8) . ? C2 H2 0.9300 . ? C3 C4 1.357(8) . ? C3 C6 1.477(7) . ? C4 C5 1.353(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.514(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.518(7) . ? C8 C17 1.520(7) . ? C8 C9 1.528(7) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.479(7) . ? C12 C16 1.361(7) . ? C12 C13 1.383(7) . ? C13 C14 1.358(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.363(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.478(8) . ? C19 C23 1.356(8) . ? C19 C20 1.393(9) . ? C20 C21 1.376(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.353(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 171.2(3) . 11 ? N2 Ag2 N2 162.5(3) . 11 ? N3 Ag3 N3 173.0(4) . 3_565 ? N3 Ag3 O14 83.1(4) . 8 ? N3 Ag3 O14 101.0(4) . 7_455 ? O14 Ag3 O14 109.6(9) 8 7_455 ? O9 Cl1 O9 109.1(11) . 11 ? O9 Cl1 O7 111.8(6) . . ? O9 Cl1 O7 111.8(6) 11 . ? O9 Cl1 O8 109.6(4) . . ? O9 Cl1 O8 109.6(4) 11 . ? O7 Cl1 O8 104.9(7) . . ? O12 Cl2 O12 122.5(14) . 11 ? O12 Cl2 O11 109.8(7) . . ? O12 Cl2 O11 109.8(7) 11 . ? O12 Cl2 O10 102.7(7) . . ? O12 Cl2 O10 102.7(7) 11 . ? O11 Cl2 O10 108.1(12) . . ? O14 Cl3 O14 52.3(14) 7_455 . ? O14 Cl3 O13 114.6(13) 7_455 7_455 ? O14 Cl3 O13 153.2(17) . 7_455 ? O14 Cl3 O13 153.2(17) 7_455 . ? O14 Cl3 O13 114.6(13) . . ? O13 Cl3 O13 86(3) 7_455 . ? O14 Cl3 O16 100.3(15) 7_455 . ? O14 Cl3 O16 112.0(11) . . ? O13 Cl3 O16 106.5(12) . . ? O14 Cl3 O16 112.0(11) 7_455 7_455 ? O14 Cl3 O16 100.3(15) . 7_455 ? O13 Cl3 O16 106.5(12) 7_455 7_455 ? O16 Cl3 O16 144(2) . 7_455 ? O14 Cl3 O15 109.1(9) 7_455 7_455 ? O14 Cl3 O15 63.4(9) . 7_455 ? O13 Cl3 O15 108.9(12) 7_455 7_455 ? O13 Cl3 O15 76.9(13) . 7_455 ? O16 Cl3 O15 77.2(10) . 7_455 ? O16 Cl3 O15 105.2(10) 7_455 7_455 ? O14 Cl3 O15 63.4(9) 7_455 . ? O14 Cl3 O15 109.1(9) . . ? O13 Cl3 O15 76.9(13) 7_455 . ? O13 Cl3 O15 108.9(12) . . ? O16 Cl3 O15 105.2(10) . . ? O16 Cl3 O15 77.2(10) 7_455 . ? O15 Cl3 O15 172.3(12) 7_455 . ? C6 O2 C7 118.9(4) . . ? C11 O4 C10 118.4(4) . . ? C18 O6 C17 114.9(4) . . ? O16 O13 Cl3 69.1(10) 7_455 . ? O14 O14 Cl3 63.9(7) 7_455 . ? O14 O14 O15 115.9(14) 7_455 7_455 ? Cl3 O14 O15 59.8(6) . 7_455 ? O14 O14 Ag3 109.0(11) 7_455 7_455 ? Cl3 O14 Ag3 149.6(12) . 7_455 ? O15 O14 Ag3 135.1(11) 7_455 7_455 ? Cl3 O15 O14 56.8(6) . 7_455 ? Cl3 O15 O16 50.9(6) . 7_455 ? O14 O15 O16 90.4(10) 7_455 7_455 ? O13 O16 Cl3 68.2(12) 7_455 . ? O13 O16 O15 108(2) 7_455 7_455 ? Cl3 O16 O15 51.9(6) . 7_455 ? C14 N1 C15 116.5(5) . . ? C14 N1 Ag1 119.4(4) . . ? C15 N1 Ag1 123.6(4) . . ? C5 N2 C1 116.8(5) . . ? C5 N2 Ag2 121.9(4) . . ? C1 N2 Ag2 121.3(4) . . ? C21 N3 C22 116.7(6) . . ? C21 N3 Ag3 121.9(5) . . ? C22 N3 Ag3 121.1(5) . . ? N2 C1 C2 123.9(6) . . ? N2 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 117.4(5) . . ? C4 C3 C6 123.5(5) . . ? C2 C3 C6 118.9(5) . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N2 C5 C4 123.0(6) . . ? N2 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O1 C6 O2 125.0(5) . . ? O1 C6 C3 125.9(5) . . ? O2 C6 C3 109.0(4) . . ? O2 C7 C8 107.3(4) . . ? O2 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O2 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C7 C8 C10 111.6(5) . . ? C7 C8 C17 108.7(4) . . ? C10 C8 C17 111.2(4) . . ? C7 C8 C9 107.2(4) . . ? C10 C8 C9 106.3(4) . . ? C17 C8 C9 111.8(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C8 114.1(4) . . ? O4 C10 H10A 108.7 . . ? C8 C10 H10A 108.7 . . ? O4 C10 H10B 108.7 . . ? C8 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O3 C11 O4 123.1(5) . . ? O3 C11 C12 122.8(5) . . ? O4 C11 C12 113.9(4) . . ? C16 C12 C13 117.6(5) . . ? C16 C12 C11 123.7(5) . . ? C13 C12 C11 118.7(4) . . ? C14 C13 C12 119.0(5) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? N1 C14 C13 123.9(5) . . ? N1 C14 H14 118.0 . . ? C13 C14 H14 118.0 . . ? N1 C15 C16 123.3(5) . . ? N1 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C12 C16 C15 119.7(5) . . ? C12 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? O6 C17 C8 108.2(4) . . ? O6 C17 H17A 110.1 . . ? C8 C17 H17A 110.1 . . ? O6 C17 H17B 110.1 . . ? C8 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? O5 C18 O6 123.9(5) . . ? O5 C18 C19 123.3(5) . . ? O6 C18 C19 112.7(5) . . ? C23 C19 C20 118.6(6) . . ? C23 C19 C18 119.3(5) . . ? C20 C19 C18 122.0(5) . . ? C21 C20 C19 117.9(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? N3 C21 C20 123.3(7) . . ? N3 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N3 C22 C23 124.1(6) . . ? N3 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? C22 C23 C19 119.2(6) . . ? C22 C23 H23 120.4 . . ? C19 C23 H23 120.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.846 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 696.2 84.0 2 0.000 0.500 0.500 696.2 86.8 3 0.500 0.000 0.500 696.2 87.3 4 0.500 1.000 0.000 696.2 82.7 _platon_squeeze_details ; 0.5 CHCl3 molecule was removed by the SQUEEZE process ;