# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Ag B F4 N3 O10 S3' _chemical_formula_weight 882.42 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.310 _cell_length_b 13.738 _cell_length_c 15.829 _cell_angle_alpha 67.25 _cell_angle_beta 81.91 _cell_angle_gamma 89.77 _cell_volume 2043.9 _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9127 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12104 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.14 _reflns_number_total 6346 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1500P)^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 goem _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6346 _refine_ls_number_parameters 506 _refine_ls_number_restraints 187 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.048 _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 0.51001(6) 0.70675(4) -1.38377(4) 0.0535(3) Uani 1 1 d . . . C1 C 0.8040(6) 0.9580(5) -1.9641(4) 0.0388(14) Uani 1 1 d . . . C2 C 0.7575(6) 1.0556(5) -2.0089(4) 0.0404(14) Uani 1 1 d . . . H2A H 0.6986 1.0857 -1.9771 0.049 Uiso 1 1 calc R . . C3 C 0.8009(6) 1.1073(5) -2.1022(4) 0.0398(14) Uani 1 1 d . . . C4 C 0.8884(7) 1.0645(5) -2.1511(4) 0.0425(15) Uani 1 1 d . . . H4A H 0.9166 1.1002 -2.2143 0.051 Uiso 1 1 calc R . . C5 C 0.9320(6) 0.9667(5) -2.1025(5) 0.0416(15) Uani 1 1 d . . . C6 C 0.8937(6) 0.9116(5) -2.0091(5) 0.0418(15) Uani 1 1 d . . . H6A H 0.9263 0.8463 -1.9775 0.050 Uiso 1 1 calc R . . C7 C 0.6444(7) 0.8694(6) -1.8330(5) 0.0482(17) Uani 1 1 d . . . C8 C 0.8194(8) 1.2922(5) -2.1646(6) 0.0523(18) Uani 1 1 d . . . C9 C 0.9979(8) 0.8651(6) -2.1899(5) 0.0533(18) Uani 1 1 d . . . C10 C 0.6191(7) 0.8312(5) -1.7302(5) 0.0445(16) Uani 1 1 d . . . C11 C 0.4906(7) 0.7965(6) -1.6854(5) 0.0516(17) Uani 1 1 d . . . H11A H 0.4232 0.7968 -1.7188 0.062 Uiso 1 1 calc R . . C12 C 0.4677(7) 0.7623(6) -1.5909(5) 0.0499(17) Uani 1 1 d . . . H12A H 0.3830 0.7385 -1.5605 0.060 Uiso 1 1 calc R . . C13 C 0.6838(7) 0.7951(5) -1.5843(5) 0.0477(16) Uani 1 1 d . . . H13A H 0.7488 0.7957 -1.5493 0.057 Uiso 1 1 calc R . . C14 C 0.7171(7) 0.8286(5) -1.6788(5) 0.0452(15) Uani 1 1 d . . . H14A H 0.8035 0.8490 -1.7071 0.054 Uiso 1 1 calc R . . C15 C 0.7439(7) 1.3883(5) -2.2058(5) 0.0488(17) Uani 1 1 d . . . C16 C 0.6132(7) 1.3809(6) -2.2114(5) 0.0514(18) Uani 1 1 d . . . H16A H 0.5675 1.3154 -2.1871 0.062 Uiso 1 1 calc R . . C17 C 0.5504(8) 1.4717(6) -2.2534(5) 0.0574(19) Uani 1 1 d . . . H17A H 0.4619 1.4665 -2.2577 0.069 Uiso 1 1 calc R . . C18 C 0.7395(8) 1.5744(6) -2.2799(6) 0.061(2) Uani 1 1 d . . . H18A H 0.7830 1.6406 -2.3016 0.073 Uiso 1 1 calc R . . C19 C 0.8072(8) 1.4883(6) -2.2409(6) 0.063(2) Uani 1 1 d . . . H19A H 0.8957 1.4957 -2.2375 0.076 Uiso 1 1 calc R . . C20 C 1.1161(7) 0.8328(5) -2.2356(5) 0.0496(17) Uani 1 1 d . . . C21 C 1.2413(7) 0.8639(6) -2.2329(5) 0.0530(18) Uani 1 1 d . . . H21A H 1.2549 0.9077 -2.2022 0.064 Uiso 1 1 calc R . . C22 C 1.3469(8) 0.8297(6) -2.2762(6) 0.059(2) Uani 1 1 d . . . H22A H 1.4316 0.8509 -2.2743 0.071 Uiso 1 1 calc R . . C23 C 1.2069(9) 0.7377(6) -2.3247(6) 0.061(2) Uani 1 1 d . . . H23A H 1.1951 0.6945 -2.3563 0.073 Uiso 1 1 calc R . . C24 C 1.0987(9) 0.7691(7) -2.2841(6) 0.061(2) Uani 1 1 d . . . H24A H 1.0150 0.7486 -2.2887 0.073 Uiso 1 1 calc R . . O1 O 0.7695(4) 0.9075(4) -1.8675(3) 0.0449(11) Uani 1 1 d . . . O2 O 0.7484(5) 1.2053(3) -2.1488(3) 0.0462(11) Uani 1 1 d . . . O3 O 1.0315(5) 0.9278(4) -2.1485(3) 0.0465(11) Uani 1 1 d . . . O4 O 0.5649(7) 0.8675(7) -1.8804(4) 0.092(2) Uani 1 1 d . . . O5 O 0.9273(7) 1.2932(4) -2.1470(6) 0.098(3) Uani 1 1 d . . . O6 O 0.8871(6) 0.8371(7) -2.1868(6) 0.088(2) Uani 1 1 d . . . B1 B 0.9501(10) 0.2302(7) 0.5667(7) 0.059(2) Uani 1 1 d . . . F1 F 1.0026(5) 0.1370(4) 0.6170(4) 0.0801(14) Uani 1 1 d U . . F2 F 0.8540(7) 0.2136(7) 0.5252(6) 0.125(3) Uani 1 1 d U . . F3 F 1.0372(7) 0.3031(6) 0.5054(6) 0.139(3) Uani 1 1 d U . . F4 F 0.8798(12) 0.2667(7) 0.6315(6) 0.157(4) Uani 1 1 d U . . N1 N 0.5611(6) 0.7614(4) -1.5405(4) 0.0481(14) Uani 1 1 d . . . N2 N 0.6141(7) 1.5695(4) -2.2890(4) 0.0554(16) Uani 1 1 d . . . N3 N 1.3293(6) 0.7660(5) -2.3214(4) 0.0532(16) Uani 1 1 d . . . O8 O 0.3430(6) 0.5588(5) -1.3965(4) 0.0702(16) Uani 1 1 d . . . O7 O 0.6790(8) 0.8246(5) -1.3510(6) 0.096(2) Uani 1 1 d U . . S1 S 0.7791(10) 0.9164(5) -1.3843(5) 0.0797(19) Uani 0.542(14) 1 d PU A 1 C26 C 0.695(2) 0.9965(14) -1.3294(16) 0.109(9) Uani 0.542(14) 1 d PD A 1 C25 C 0.756(3) 0.996(2) -1.4999(16) 0.115(6) Uani 0.542(14) 1 d PDU A 1 S1' S 0.7202(12) 0.9402(7) -1.3763(6) 0.088(2) Uani 0.458(14) 1 d PU A 2 C25' C 0.879(2) 0.947(2) -1.444(2) 0.097(7) Uani 0.458(14) 1 d PDU A 2 C26' C 0.636(3) 1.012(2) -1.471(2) 0.110(8) Uani 0.458(14) 1 d PDU A 2 S2 S 0.2857(2) 0.46467(14) -1.40332(14) 0.0593(5) Uani 1 1 d U . . C27 C 0.1167(12) 0.4621(10) -1.3641(8) 0.101(4) Uani 1 1 d DU . . H27A H 0.1029 0.4445 -1.2985 0.151 Uiso 1 1 calc R . . H27B H 0.0709 0.4102 -1.3773 0.151 Uiso 1 1 calc R . . H27C H 0.0841 0.5304 -1.3951 0.151 Uiso 1 1 calc R . . C28 C 0.2773(11) 0.4972(8) -1.5222(7) 0.083(3) Uani 1 1 d DU . . H28A H 0.3641 0.5015 -1.5552 0.125 Uiso 1 1 calc R . . H28B H 0.2385 0.5640 -1.5474 0.125 Uiso 1 1 calc R . . H28C H 0.2247 0.4435 -1.5285 0.125 Uiso 1 1 calc R . . S3 S 1.5057(6) 0.7289(5) -2.0355(4) 0.174(2) Uani 1 1 d U . . O9 O 1.3792(14) 0.7376(11) -2.0337(10) 0.163(4) Uani 1 1 d U . . C29 C 1.5708(11) 0.8840(15) -2.1137(12) 0.163(7) Uani 1 1 d DU . . H29A H 1.5395 0.9275 -2.0810 0.245 Uiso 1 1 calc R . . H29B H 1.5382 0.9076 -2.1719 0.245 Uiso 1 1 calc R . . H29C H 1.6650 0.8890 -2.1247 0.245 Uiso 1 1 calc R . . C30 C 1.585(2) 0.6845(15) -2.1140(14) 0.182(7) Uani 1 1 d DU . . H30A H 1.5662 0.6098 -2.0931 0.274 Uiso 1 1 calc R . . H30B H 1.6775 0.6988 -2.1208 0.274 Uiso 1 1 calc R . . H30C H 1.5550 0.7200 -2.1727 0.274 Uiso 1 1 calc R . . O1W O 1.005(4) 1.392(3) -2.009(2) 0.207(11) Uani 0.50 1 d PU . . O2W O 0.916(4) 1.433(3) -1.971(3) 0.218(12) Uani 0.50 1 d PU . . 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 0.0669(4) 0.0372(3) 0.0460(3) -0.0118(2) 0.0113(2) 0.0132(2) C1 0.039(4) 0.033(3) 0.040(3) -0.012(3) 0.006(3) -0.006(3) C2 0.034(4) 0.038(3) 0.046(3) -0.016(3) 0.007(3) 0.000(3) C3 0.036(4) 0.030(3) 0.050(4) -0.014(3) -0.001(3) 0.002(3) C4 0.041(4) 0.038(3) 0.045(3) -0.015(3) 0.002(3) -0.003(3) C5 0.033(4) 0.037(3) 0.055(4) -0.022(3) 0.004(3) 0.000(3) C6 0.036(4) 0.030(3) 0.055(4) -0.013(3) -0.001(3) 0.000(3) C7 0.039(4) 0.047(4) 0.047(4) -0.010(3) 0.004(3) -0.019(3) C8 0.039(4) 0.034(3) 0.073(5) -0.010(3) -0.004(3) -0.004(3) C9 0.047(5) 0.054(4) 0.064(4) -0.031(4) 0.003(3) -0.001(3) C10 0.038(4) 0.032(3) 0.051(4) -0.007(3) 0.009(3) -0.008(3) C11 0.042(4) 0.049(4) 0.054(4) -0.012(3) 0.001(3) -0.010(3) C12 0.037(4) 0.047(4) 0.056(4) -0.013(3) 0.006(3) -0.002(3) C13 0.049(4) 0.044(4) 0.043(3) -0.012(3) 0.002(3) 0.002(3) C14 0.034(4) 0.044(4) 0.051(4) -0.014(3) 0.000(3) -0.004(3) C15 0.045(4) 0.033(3) 0.056(4) -0.008(3) 0.004(3) 0.001(3) C16 0.049(5) 0.038(3) 0.053(4) -0.006(3) 0.002(3) 0.001(3) C17 0.052(5) 0.046(4) 0.055(4) -0.004(3) 0.007(3) 0.002(3) C18 0.052(5) 0.033(4) 0.083(5) -0.011(3) 0.000(4) -0.005(3) C19 0.048(5) 0.040(4) 0.094(6) -0.019(4) -0.009(4) -0.001(3) C20 0.051(5) 0.043(4) 0.057(4) -0.026(3) 0.007(3) 0.000(3) C21 0.049(5) 0.053(4) 0.066(4) -0.038(4) 0.004(3) 0.001(3) C22 0.050(5) 0.059(5) 0.070(5) -0.034(4) 0.009(4) 0.001(4) C23 0.071(6) 0.058(5) 0.069(5) -0.045(4) -0.003(4) 0.001(4) C24 0.059(5) 0.061(5) 0.076(5) -0.045(4) 0.000(4) -0.005(4) O1 0.039(3) 0.043(2) 0.042(2) -0.0093(19) 0.0053(19) -0.005(2) O2 0.042(3) 0.033(2) 0.056(3) -0.012(2) 0.000(2) 0.0036(19) O3 0.043(3) 0.045(2) 0.060(3) -0.034(2) 0.005(2) 0.001(2) O4 0.067(4) 0.129(6) 0.051(3) -0.008(3) 0.001(3) -0.048(4) O5 0.064(5) 0.034(3) 0.177(8) -0.011(4) -0.049(5) -0.003(3) O6 0.048(4) 0.125(6) 0.129(6) -0.096(5) 0.004(4) -0.008(4) B1 0.061(6) 0.046(5) 0.069(5) -0.020(4) -0.013(5) -0.011(4) F1 0.073(3) 0.069(3) 0.082(3) -0.013(3) -0.009(3) 0.004(3) F2 0.082(5) 0.121(6) 0.159(7) -0.030(5) -0.053(5) 0.003(4) F3 0.084(5) 0.099(5) 0.159(7) 0.024(5) 0.006(4) -0.016(4) F4 0.247(10) 0.104(5) 0.121(6) -0.054(5) -0.006(6) 0.045(6) N1 0.050(4) 0.036(3) 0.049(3) -0.013(2) 0.010(3) 0.003(2) N2 0.065(5) 0.034(3) 0.052(3) -0.005(2) 0.006(3) 0.001(3) N3 0.059(4) 0.043(3) 0.056(3) -0.024(3) 0.008(3) 0.003(3) O8 0.082(4) 0.052(3) 0.079(4) -0.026(3) -0.016(3) -0.007(3) O7 0.105(4) 0.051(3) 0.120(4) -0.020(3) -0.017(4) -0.009(3) S1 0.092(5) 0.043(2) 0.096(3) -0.016(2) -0.018(3) 0.000(3) C26 0.102(16) 0.051(10) 0.19(2) -0.085(14) 0.028(15) -0.002(10) C25 0.129(12) 0.099(11) 0.126(11) -0.052(9) -0.027(10) 0.020(10) S1' 0.095(5) 0.055(4) 0.096(3) -0.015(3) -0.002(4) -0.003(3) C25' 0.097(13) 0.083(11) 0.126(13) -0.062(10) 0.001(11) -0.004(10) C26' 0.119(14) 0.084(12) 0.121(14) -0.030(11) -0.029(12) 0.011(11) S2 0.0697(13) 0.0382(9) 0.0644(11) -0.0176(8) 0.0004(9) 0.0037(8) C27 0.093(8) 0.088(7) 0.104(8) -0.031(6) 0.021(6) -0.010(6) C28 0.106(8) 0.063(5) 0.080(6) -0.033(5) 0.002(5) -0.001(5) S3 0.178(4) 0.209(4) 0.127(3) -0.072(3) 0.018(3) 0.078(4) O9 0.175(10) 0.174(9) 0.165(8) -0.095(7) -0.027(8) 0.042(8) C29 0.056(7) 0.311(17) 0.189(12) -0.187(13) 0.038(7) -0.065(9) C30 0.179(12) 0.214(13) 0.135(10) -0.056(10) 0.000(9) 0.075(11) O1W 0.231(18) 0.209(17) 0.191(16) -0.086(13) -0.045(14) 0.044(14) O2W 0.219(18) 0.220(17) 0.194(16) -0.056(13) -0.040(14) 0.038(14) _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 2.278(6) . ? Ag1 N3 2.280(6) 1_456 ? Ag1 N2 2.282(6) 1_546 ? C1 C2 1.374(9) . ? C1 C6 1.389(9) . ? C1 O1 1.406(8) . ? C2 C3 1.376(9) . ? C2 H2A 0.9300 . ? C3 C4 1.382(9) . ? C3 O2 1.410(8) . ? C4 C5 1.376(10) . ? C4 H4A 0.9300 . ? C5 C6 1.373(10) . ? C5 O3 1.397(8) . ? C6 H6A 0.9300 . ? C7 O4 1.193(9) . ? C7 O1 1.350(8) . ? C7 C10 1.487(10) . ? C8 O5 1.186(10) . ? C8 O2 1.322(9) . ? C8 C15 1.497(10) . ? C9 O6 1.196(10) . ? C9 O3 1.339(9) . ? C9 C20 1.483(10) . ? C10 C14 1.377(10) . ? C10 C11 1.402(10) . ? C11 C12 1.368(11) . ? C11 H11A 0.9300 . ? C12 N1 1.332(10) . ? C12 H12A 0.9300 . ? C13 N1 1.343(9) . ? C13 C14 1.376(10) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.370(11) . ? C15 C19 1.392(10) . ? C16 C17 1.375(11) . ? C16 H16A 0.9300 . ? C17 N2 1.368(10) . ? C17 H17A 0.9300 . ? C18 N2 1.325(11) . ? C18 C19 1.348(12) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.373(11) . ? C20 C24 1.395(10) . ? C21 C22 1.382(10) . ? C21 H21A 0.9300 . ? C22 N3 1.354(10) . ? C22 H22A 0.9300 . ? C23 N3 1.336(11) . ? C23 C24 1.360(12) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? B1 F2 1.328(12) . ? B1 F3 1.328(11) . ? B1 F1 1.376(11) . ? B1 F4 1.420(13) . ? N2 Ag1 2.282(6) 1_564 ? N3 Ag1 2.280(6) 1_654 ? O8 S2 1.471(6) . ? O7 S1 1.509(10) . ? O7 S1' 1.526(11) . ? S1 C25 1.78(3) . ? S1 C26 1.801(17) . ? S1' C26' 1.79(3) . ? S1' C25' 1.81(3) . ? S2 C27 1.761(11) . ? S2 C28 1.773(10) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? S3 O9 1.307(14) . ? S3 C30 1.696(16) . ? S3 C29 2.065(18) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? O1W O2W 1.28(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 N1 Ag1 N3 120.0(2) . 1_456 ? N1 Ag1 N2 119.9(2) . 1_546 ? N3 Ag1 N2 119.1(2) 1_456 1_546 ? C2 C1 C6 122.5(6) . . ? C2 C1 O1 118.7(5) . . ? C6 C1 O1 118.4(6) . . ? C1 C2 C3 117.8(6) . . ? C1 C2 H2A 121.1 . . ? C3 C2 H2A 121.1 . . ? C2 C3 C4 122.3(6) . . ? C2 C3 O2 117.6(5) . . ? C4 C3 O2 120.0(6) . . ? C5 C4 C3 117.2(6) . . ? C5 C4 H4A 121.4 . . ? C3 C4 H4A 121.4 . . ? C6 C5 C4 123.2(6) . . ? C6 C5 O3 118.6(6) . . ? C4 C5 O3 117.8(6) . . ? C5 C6 C1 116.8(6) . . ? C5 C6 H6A 121.6 . . ? C1 C6 H6A 121.6 . . ? O4 C7 O1 123.2(6) . . ? O4 C7 C10 124.9(6) . . ? O1 C7 C10 111.8(6) . . ? O5 C8 O2 124.3(7) . . ? O5 C8 C15 124.9(7) . . ? O2 C8 C15 110.8(6) . . ? O6 C9 O3 123.5(7) . . ? O6 C9 C20 125.6(7) . . ? O3 C9 C20 110.9(6) . . ? C14 C10 C11 119.7(6) . . ? C14 C10 C7 122.2(6) . . ? C11 C10 C7 118.1(7) . . ? C12 C11 C10 117.8(7) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? N1 C12 C11 123.1(6) . . ? N1 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N1 C13 C14 122.7(7) . . ? N1 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C10 118.1(6) . . ? C13 C14 H14A 120.9 . . ? C10 C14 H14A 120.9 . . ? C16 C15 C19 118.3(7) . . ? C16 C15 C8 121.8(6) . . ? C19 C15 C8 119.9(7) . . ? C15 C16 C17 119.1(7) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? N2 C17 C16 122.1(8) . . ? N2 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? N2 C18 C19 123.4(7) . . ? N2 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? C18 C19 C15 119.6(8) . . ? C18 C19 H19A 120.2 . . ? C15 C19 H19A 120.2 . . ? C21 C20 C24 118.9(7) . . ? C21 C20 C9 122.7(6) . . ? C24 C20 C9 118.4(7) . . ? C20 C21 C22 119.6(7) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? N3 C22 C21 121.2(8) . . ? N3 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? N3 C23 C24 123.2(7) . . ? N3 C23 H23A 118.4 . . ? C24 C23 H23A 118.4 . . ? C23 C24 C20 118.6(8) . . ? C23 C24 H24A 120.7 . . ? C20 C24 H24A 120.7 . . ? C7 O1 C1 118.3(5) . . ? C8 O2 C3 117.8(6) . . ? C9 O3 C5 118.7(5) . . ? F2 B1 F3 110.0(9) . . ? F2 B1 F1 111.5(7) . . ? F3 B1 F1 114.4(9) . . ? F2 B1 F4 101.2(9) . . ? F3 B1 F4 112.0(9) . . ? F1 B1 F4 106.9(8) . . ? C12 N1 C13 118.5(6) . . ? C12 N1 Ag1 119.9(4) . . ? C13 N1 Ag1 121.5(5) . . ? C18 N2 C17 117.5(7) . . ? C18 N2 Ag1 124.1(5) . 1_564 ? C17 N2 Ag1 117.3(6) . 1_564 ? C23 N3 C22 118.6(6) . . ? C23 N3 Ag1 122.9(5) . 1_654 ? C22 N3 Ag1 118.5(5) . 1_654 ? S1 O7 S1' 27.0(3) . . ? O7 S1 C25 105.8(11) . . ? O7 S1 C26 98.9(9) . . ? C25 S1 C26 97.2(10) . . ? O7 S1' C26' 104.4(12) . . ? O7 S1' C25' 99.4(11) . . ? C26' S1' C25' 96.8(12) . . ? O8 S2 C27 105.3(5) . . ? O8 S2 C28 106.9(4) . . ? C27 S2 C28 98.3(6) . . ? S2 C27 H27A 109.5 . . ? S2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S2 C28 H28A 109.5 . . ? S2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 S3 C30 116.8(10) . . ? O9 S3 C29 100.0(9) . . ? C30 S3 C29 93.3(7) . . ? S3 C29 H29A 109.5 . . ? S3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? S3 C30 H30A 109.5 . . ? S3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 24.14 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.649 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 940527' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H38.50 Ag F6 N3 O11.75 S3 Sb' _chemical_formula_weight 1068.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 11.2552(11) _cell_length_b 13.6464(14) _cell_length_c 16.3098(16) _cell_angle_alpha 110.448(2) _cell_angle_beta 100.874(2) _cell_angle_gamma 95.504(2) _cell_volume 2269.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.6475 _cell_measurement_theta_max 30.2499 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1067 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8356 _exptl_absorpt_correction_T_max 0.8652 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number 8741 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19119 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9730 _reflns_number_gt 7291 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1005P)^2^+3.0476P] 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 goem _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9730 _refine_ls_number_parameters 565 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.089 _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 -0.02394(3) 0.18017(3) 0.37720(2) 0.03579(13) Uani 1 1 d . . . N1 N 0.0235(4) 0.2511(3) 0.5308(3) 0.0384(9) Uani 1 1 d . . . N2 N 0.0988(4) 0.2554(3) 1.3100(3) 0.0391(9) Uani 1 1 d . . . N3 N 0.8112(4) 1.0514(3) 1.2973(3) 0.0366(9) Uani 1 1 d . . . Sb1 Sb 0.46290(3) 0.69672(3) 0.42412(3) 0.04807(14) Uani 1 1 d . . . C1 C 0.3074(4) 0.4902(4) 0.9381(3) 0.0312(9) Uani 1 1 d . . . C2 C 0.2625(4) 0.4421(4) 0.9908(3) 0.0307(9) Uani 1 1 d . . . H2A H 0.2016 0.3796 0.9650 0.037 Uiso 1 1 calc R . . C3 C 0.3104(4) 0.4892(4) 1.0825(3) 0.0307(9) Uani 1 1 d . . . C4 C 0.3993(4) 0.5792(4) 1.1220(3) 0.0333(10) Uani 1 1 d . . . H4A H 0.4317 0.6098 1.1854 0.040 Uiso 1 1 calc R . . C5 C 0.4391(4) 0.6229(3) 1.0657(3) 0.0301(9) Uani 1 1 d . . . C6 C 0.3962(4) 0.5807(4) 0.9738(3) 0.0299(9) Uani 1 1 d . . . H6A H 0.4262 0.6123 0.9366 0.036 Uiso 1 1 calc R . . C7 C 0.1472(5) 0.4468(4) 0.8094(3) 0.0358(10) Uani 1 1 d . . . C8 C 0.3136(5) 0.3820(4) 1.1691(4) 0.0392(11) Uani 1 1 d . . . C9 C 0.5015(4) 0.8066(4) 1.1469(3) 0.0356(10) Uani 1 1 d . . . C10 C 0.1072(4) 0.3755(4) 0.7128(3) 0.0309(9) Uani 1 1 d . . . C11 C 0.1795(4) 0.3108(4) 0.6669(3) 0.0361(10) Uani 1 1 d . . . H11A H 0.2590 0.3079 0.6974 0.043 Uiso 1 1 calc R . . C12 C 0.1350(5) 0.2507(4) 0.5765(3) 0.0411(11) Uani 1 1 d . . . H12A H 0.1858 0.2071 0.5454 0.049 Uiso 1 1 calc R . . C13 C -0.0483(4) 0.3119(4) 0.5747(3) 0.0373(11) Uani 1 1 d . . . H13A H -0.1282 0.3115 0.5425 0.045 Uiso 1 1 calc R . . C14 C -0.0102(5) 0.3756(4) 0.6654(3) 0.0365(11) Uani 1 1 d . . . H14A H -0.0628 0.4185 0.6949 0.044 Uiso 1 1 calc R . . C15 C 0.2383(5) 0.3409(4) 1.2201(3) 0.0353(10) Uani 1 1 d . . . C16 C 0.1189(5) 0.3586(4) 1.2196(3) 0.0373(11) Uani 1 1 d . . . H16A H 0.0830 0.3998 1.1885 0.045 Uiso 1 1 calc R . . C17 C 0.0536(5) 0.3142(4) 1.2661(3) 0.0383(11) Uani 1 1 d . . . H17A H -0.0279 0.3266 1.2664 0.046 Uiso 1 1 calc R . . C18 C 0.2129(5) 0.2390(5) 1.3110(4) 0.0487(14) Uani 1 1 d . . . H18A H 0.2461 0.1975 1.3428 0.058 Uiso 1 1 calc R . . C19 C 0.2858(5) 0.2810(5) 1.2666(4) 0.0496(14) Uani 1 1 d . . . H19A H 0.3677 0.2683 1.2685 0.060 Uiso 1 1 calc R . . C20 C 0.6125(4) 0.8914(4) 1.1984(3) 0.0321(10) Uani 1 1 d . . . C21 C 0.5955(5) 0.9942(4) 1.2419(4) 0.0472(13) Uani 1 1 d . . . H21A H 0.5152 1.0110 1.2386 0.057 Uiso 1 1 calc R . . C22 C 0.6972(5) 1.0714(4) 1.2901(4) 0.0442(12) Uani 1 1 d . . . H22A H 0.6855 1.1421 1.3195 0.053 Uiso 1 1 calc R . . C23 C 0.8261(4) 0.9527(4) 1.2553(4) 0.0417(12) Uani 1 1 d . . . H23A H 0.9075 0.9383 1.2601 0.050 Uiso 1 1 calc R . . C24 C 0.7301(4) 0.8693(4) 1.2048(4) 0.0389(11) Uani 1 1 d . . . H24A H 0.7447 0.7995 1.1758 0.047 Uiso 1 1 calc R . . O7 O 0.1233(4) 0.0457(4) 0.3801(4) 0.0671(13) Uani 1 1 d . . . S1 S 0.17728(15) -0.05004(12) 0.38062(11) 0.0520(4) Uani 1 1 d . . . C25 C 0.2309(8) -0.0311(6) 0.4953(5) 0.0700(19) Uani 1 1 d . . . H25A H 0.1607 -0.0385 0.5215 0.105 Uiso 1 1 calc R . . H25B H 0.2804 0.0400 0.5281 0.105 Uiso 1 1 calc R . . H25C H 0.2815 -0.0846 0.4997 0.105 Uiso 1 1 calc R . . C26 C 0.3204(7) -0.0330(6) 0.3528(6) 0.072(2) Uani 1 1 d . . . H26A H 0.3065 -0.0409 0.2895 0.108 Uiso 1 1 calc R . . H26B H 0.3672 -0.0867 0.3623 0.108 Uiso 1 1 calc R . . H26C H 0.3669 0.0380 0.3912 0.108 Uiso 1 1 calc R . . S2 S -0.20830(16) 0.42575(13) 0.37379(12) 0.0559(4) Uani 1 1 d . . . O8 O -0.1665(4) 0.3291(4) 0.3803(3) 0.0641(12) Uani 1 1 d . . . C28 C -0.1935(8) 0.5173(5) 0.4852(6) 0.075(2) Uani 1 1 d . . . H28A H -0.1062 0.5436 0.5150 0.113 Uiso 1 1 calc R . . H28B H -0.2320 0.4818 0.5189 0.113 Uiso 1 1 calc R . . H28C H -0.2341 0.5771 0.4832 0.113 Uiso 1 1 calc R . . C27 C -0.3707(7) 0.3957(9) 0.3407(7) 0.098(3) Uani 1 1 d . . . H27A H -0.3967 0.3443 0.2784 0.146 Uiso 1 1 calc R . . H27B H -0.4035 0.4608 0.3449 0.146 Uiso 1 1 calc R . . H27C H -0.4019 0.3653 0.3805 0.146 Uiso 1 1 calc R . . S3 S 0.07360(14) 0.78092(13) 1.13909(12) 0.0639(5) Uani 1 1 d . . . O9 O -0.0591(4) 0.7549(4) 1.1391(4) 0.0880(19) Uani 1 1 d . . . C30 C 0.1468(8) 0.6948(7) 1.1763(10) 0.117(4) Uani 1 1 d . . . H30A H 0.1489 0.7128 1.2403 0.176 Uiso 1 1 calc R . . H30B H 0.2310 0.7002 1.1683 0.176 Uiso 1 1 calc R . . H30C H 0.1025 0.6221 1.1416 0.176 Uiso 1 1 calc R . . C29 C 0.0885(10) 0.7225(13) 1.0262(7) 0.163(7) Uani 1 1 d . . . H29A H 0.0513 0.7616 0.9908 0.244 Uiso 1 1 calc R . . H29B H 0.0467 0.6483 0.9997 0.244 Uiso 1 1 calc R . . H29C H 0.1758 0.7255 1.0259 0.244 Uiso 1 1 calc R . . O1 O 0.2651(3) 0.4399(3) 0.8445(2) 0.0348(7) Uani 1 1 d . . . O2 O 0.2558(3) 0.4474(3) 1.1372(2) 0.0385(8) Uani 1 1 d . . . O3 O 0.5344(3) 0.7125(3) 1.1047(2) 0.0361(7) Uani 1 1 d . . . O4 O 0.0871(4) 0.5023(3) 0.8512(3) 0.0490(10) Uani 1 1 d . . . O5 O 0.4106(4) 0.3606(4) 1.1575(3) 0.0613(12) Uani 1 1 d . . . O6 O 0.3986(3) 0.8199(3) 1.1454(3) 0.0543(11) Uani 1 1 d . . . F2 F 0.4038(9) 0.7741(8) 0.5175(6) 0.200(4) Uani 1 1 d U A . F4 F 0.5166(8) 0.6093(7) 0.3295(4) 0.157(3) Uani 1 1 d U A . F3 F 0.3271(8) 0.7166(9) 0.3486(8) 0.100(3) Uani 0.50 1 d PU A 1 F5 F 0.5431(14) 0.8239(11) 0.4316(13) 0.160(6) Uani 0.50 1 d PU A 1 F6 F 0.3770(17) 0.5773(12) 0.4216(13) 0.148(5) Uani 0.50 1 d PU A 1 F1 F 0.5969(14) 0.6815(12) 0.4971(10) 0.116(5) Uani 0.50 1 d PU A 1 F6' F 0.3129(14) 0.6238(17) 0.3591(15) 0.185(6) Uani 0.50 1 d PU A 2 F5' F 0.6182(14) 0.7416(17) 0.4880(12) 0.150(6) Uani 0.50 1 d PU A 2 F3' F 0.484(2) 0.7642(15) 0.3483(14) 0.194(7) Uani 0.50 1 d PU A 2 F1' F 0.467(2) 0.6012(14) 0.4796(13) 0.162(5) Uani 0.50 1 d PU A 2 O1W O -0.120(2) 0.0686(16) 1.0935(12) 0.176(8) Uani 0.50 1 d PU . . O3W O 0.2116(18) 0.1484(15) 1.0019(11) 0.145(6) Uani 0.50 1 d PU . . O2W O 0.5000 1.0000 1.0000 0.193(12) Uani 0.50 2 d SPU . . O4W O 0.557(2) 1.1428(17) 1.0656(13) 0.167(7) Uani 0.50 1 d PU . . O1W' O 0.060(2) 0.0400(12) 1.0807(12) 0.172(8) Uani 0.50 1 d PU . . O3W' O 0.100(3) 0.030(2) 0.968(2) 0.209(10) Uani 0.50 1 d PU . . 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 0.0394(2) 0.0323(2) 0.0281(2) 0.00701(15) 0.00459(15) -0.00492(15) N1 0.045(2) 0.032(2) 0.029(2) 0.0036(17) 0.0063(18) 0.0011(18) N2 0.037(2) 0.040(2) 0.042(2) 0.018(2) 0.0105(18) 0.0011(18) N3 0.033(2) 0.031(2) 0.038(2) 0.0055(18) 0.0067(17) 0.0016(17) Sb1 0.0372(2) 0.0533(2) 0.0524(3) 0.01718(19) 0.01118(17) 0.01160(17) C1 0.025(2) 0.035(2) 0.028(2) 0.0061(19) 0.0043(17) 0.0071(18) C2 0.027(2) 0.030(2) 0.031(2) 0.0091(19) 0.0052(18) -0.0026(18) C3 0.030(2) 0.035(2) 0.031(2) 0.015(2) 0.0110(18) 0.0071(19) C4 0.031(2) 0.038(3) 0.027(2) 0.009(2) 0.0041(18) 0.0046(19) C5 0.023(2) 0.026(2) 0.034(2) 0.0053(18) 0.0050(17) -0.0004(17) C6 0.027(2) 0.031(2) 0.033(2) 0.0129(19) 0.0086(18) 0.0037(18) C7 0.042(3) 0.032(2) 0.029(2) 0.007(2) 0.007(2) 0.009(2) C8 0.036(3) 0.047(3) 0.039(3) 0.024(2) 0.005(2) 0.005(2) C9 0.029(2) 0.032(2) 0.043(3) 0.013(2) 0.005(2) 0.0001(19) C10 0.033(2) 0.031(2) 0.025(2) 0.0090(19) 0.0015(18) 0.0051(18) C11 0.030(2) 0.038(3) 0.036(3) 0.010(2) 0.0039(19) 0.008(2) C12 0.042(3) 0.043(3) 0.035(3) 0.007(2) 0.010(2) 0.014(2) C13 0.029(2) 0.041(3) 0.036(3) 0.013(2) -0.0004(19) 0.005(2) C14 0.033(2) 0.038(3) 0.031(2) 0.006(2) 0.0030(19) 0.011(2) C15 0.034(2) 0.037(3) 0.036(3) 0.017(2) 0.008(2) 0.001(2) C16 0.044(3) 0.036(3) 0.039(3) 0.019(2) 0.015(2) 0.012(2) C17 0.039(3) 0.043(3) 0.041(3) 0.020(2) 0.018(2) 0.013(2) C18 0.040(3) 0.062(4) 0.058(3) 0.041(3) 0.010(3) 0.008(3) C19 0.033(3) 0.069(4) 0.060(4) 0.041(3) 0.010(2) 0.010(3) C20 0.024(2) 0.028(2) 0.038(3) 0.006(2) 0.0064(18) -0.0003(17) C21 0.030(3) 0.035(3) 0.070(4) 0.012(3) 0.013(3) 0.006(2) C22 0.043(3) 0.025(2) 0.057(3) 0.007(2) 0.013(2) 0.003(2) C23 0.022(2) 0.037(3) 0.054(3) 0.005(2) 0.005(2) 0.0024(19) C24 0.030(2) 0.028(2) 0.046(3) 0.002(2) 0.006(2) 0.0011(19) O7 0.061(3) 0.059(3) 0.080(3) 0.024(2) 0.008(2) 0.026(2) S1 0.0551(9) 0.0386(7) 0.0578(9) 0.0136(7) 0.0110(7) 0.0087(6) C25 0.087(5) 0.058(4) 0.069(5) 0.032(4) 0.011(4) 0.019(4) C26 0.065(4) 0.068(5) 0.085(5) 0.023(4) 0.032(4) 0.017(4) S2 0.0610(10) 0.0492(8) 0.0717(11) 0.0324(8) 0.0270(8) 0.0152(7) O8 0.071(3) 0.054(3) 0.072(3) 0.019(2) 0.021(2) 0.036(2) C28 0.079(5) 0.039(3) 0.095(6) 0.005(4) 0.031(4) 0.008(3) C27 0.064(5) 0.125(8) 0.089(6) 0.031(6) -0.006(4) 0.035(5) S3 0.0349(7) 0.0512(9) 0.0708(11) -0.0160(8) 0.0112(7) -0.0007(6) O9 0.031(2) 0.065(3) 0.121(5) -0.022(3) 0.018(3) 0.004(2) C30 0.065(5) 0.074(6) 0.221(14) 0.047(7) 0.065(7) 0.019(4) C29 0.085(7) 0.238(16) 0.072(6) -0.050(8) 0.015(5) 0.017(9) O1 0.0278(16) 0.0410(18) 0.0251(16) 0.0042(14) 0.0006(13) 0.0004(14) O2 0.0377(19) 0.047(2) 0.0414(19) 0.0257(17) 0.0161(15) 0.0068(15) O3 0.0256(16) 0.0287(16) 0.0420(19) 0.0020(14) 0.0064(14) -0.0035(13) O4 0.047(2) 0.051(2) 0.0356(19) 0.0010(17) 0.0006(16) 0.0220(18) O5 0.045(2) 0.087(3) 0.086(3) 0.061(3) 0.032(2) 0.027(2) O6 0.0247(19) 0.039(2) 0.085(3) 0.010(2) 0.0055(18) 0.0034(15) F2 0.206(8) 0.232(9) 0.167(7) 0.023(6) 0.106(6) 0.138(7) F4 0.194(7) 0.195(7) 0.067(3) 0.017(4) 0.035(4) 0.091(6) F3 0.058(5) 0.091(6) 0.134(8) 0.047(6) -0.031(5) 0.026(5) F5 0.150(9) 0.109(8) 0.198(12) 0.099(9) -0.041(8) -0.074(7) F6 0.148(10) 0.118(8) 0.185(10) 0.092(8) 0.016(8) -0.031(7) F1 0.109(8) 0.128(9) 0.091(6) 0.044(7) -0.041(6) 0.049(7) F6' 0.096(8) 0.199(11) 0.199(11) 0.028(10) -0.003(8) -0.002(9) F5' 0.083(7) 0.200(13) 0.112(9) 0.016(10) -0.001(7) -0.020(9) F3' 0.271(14) 0.161(11) 0.169(11) 0.125(10) 0.003(10) -0.020(10) F1' 0.199(11) 0.159(9) 0.156(9) 0.107(8) 0.031(8) 0.004(9) O1W 0.298(19) 0.121(12) 0.083(9) 0.037(9) 0.023(11) -0.034(12) O3W 0.176(14) 0.146(12) 0.095(10) 0.029(9) 0.015(9) 0.038(11) O2W 0.29(2) 0.207(19) 0.148(17) 0.135(16) 0.054(14) 0.101(16) O4W 0.264(17) 0.166(13) 0.125(12) 0.097(11) 0.064(11) 0.083(12) O1W' 0.248(16) 0.083(9) 0.117(11) -0.005(8) -0.049(11) 0.061(10) O3W' 0.227(14) 0.195(13) 0.217(13) 0.088(10) 0.060(9) 0.038(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 Ag1 N3 2.256(4) 1_444 ? Ag1 N1 2.280(4) . ? Ag1 N2 2.291(4) 1_554 ? Ag1 O7 2.594(4) . ? N1 C12 1.335(7) . ? N1 C13 1.336(7) . ? N2 C18 1.322(7) . ? N2 C17 1.326(7) . ? N2 Ag1 2.291(4) 1_556 ? N3 C23 1.324(6) . ? N3 C22 1.330(7) . ? N3 Ag1 2.256(4) 1_666 ? Sb1 F5' 1.782(15) . ? Sb1 F6 1.797(12) . ? Sb1 F6' 1.797(15) . ? Sb1 F2 1.808(7) . ? Sb1 F1 1.813(10) . ? Sb1 F3' 1.817(14) . ? Sb1 F1' 1.828(14) . ? Sb1 F5 1.830(10) . ? Sb1 F4 1.837(6) . ? Sb1 F3 1.878(7) . ? C1 C6 1.380(6) . ? C1 C2 1.387(7) . ? C1 O1 1.399(5) . ? C2 C3 1.377(7) . ? C2 H2A 0.9500 . ? C3 C4 1.377(7) . ? C3 O2 1.411(5) . ? C4 C5 1.373(7) . ? C4 H4A 0.9500 . ? C5 C6 1.371(7) . ? C5 O3 1.413(5) . ? C6 H6A 0.9500 . ? C7 O4 1.185(6) . ? C7 O1 1.368(6) . ? C7 C10 1.487(6) . ? C8 O5 1.189(6) . ? C8 O2 1.341(6) . ? C8 C15 1.492(7) . ? C9 O6 1.187(6) . ? C9 O3 1.353(6) . ? C9 C20 1.501(6) . ? C10 C11 1.381(7) . ? C10 C14 1.400(6) . ? C11 C12 1.376(7) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.386(7) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C19 1.376(7) . ? C15 C16 1.388(7) . ? C16 C17 1.389(7) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.396(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C24 1.378(7) . ? C20 C21 1.385(7) . ? C21 C22 1.374(7) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.383(7) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? O7 S1 1.495(4) . ? S1 C26 1.770(7) . ? S1 C25 1.771(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? S2 O8 1.473(4) . ? S2 C27 1.769(8) . ? S2 C28 1.775(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? S3 O9 1.502(5) . ? S3 C30 1.710(10) . ? S3 C29 1.781(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O1W O3W' 1.44(3) 2_557 ? O3W O3W' 1.80(3) . ? O3W' O1W 1.44(3) 2_557 ? 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 N3 Ag1 N1 121.76(16) 1_444 . ? N3 Ag1 N2 122.45(16) 1_444 1_554 ? N1 Ag1 N2 115.68(16) . 1_554 ? N3 Ag1 O7 93.36(15) 1_444 . ? N1 Ag1 O7 90.30(16) . . ? N2 Ag1 O7 89.56(16) 1_554 . ? C12 N1 C13 118.7(4) . . ? C12 N1 Ag1 119.6(3) . . ? C13 N1 Ag1 120.3(3) . . ? C18 N2 C17 118.6(4) . . ? C18 N2 Ag1 121.9(3) . 1_556 ? C17 N2 Ag1 119.5(3) . 1_556 ? C23 N3 C22 117.9(4) . . ? C23 N3 Ag1 120.3(3) . 1_666 ? C22 N3 Ag1 121.9(3) . 1_666 ? F5' Sb1 F6 119.9(9) . . ? F5' Sb1 F6' 167.6(10) . . ? F6 Sb1 F6' 49.0(9) . . ? F5' Sb1 F2 92.7(7) . . ? F6 Sb1 F2 89.8(7) . . ? F6' Sb1 F2 92.9(7) . . ? F5' Sb1 F1 29.0(7) . . ? F6 Sb1 F1 90.9(8) . . ? F6' Sb1 F1 139.4(10) . . ? F2 Sb1 F1 93.3(6) . . ? F5' Sb1 F3' 93.2(10) . . ? F6 Sb1 F3' 139.3(9) . . ? F6' Sb1 F3' 94.8(11) . . ? F2 Sb1 F3' 113.2(8) . . ? F1 Sb1 F3' 119.1(9) . . ? F5' Sb1 F1' 82.7(9) . . ? F6 Sb1 F1' 37.9(6) . . ? F6' Sb1 F1' 86.8(10) . . ? F2 Sb1 F1' 84.1(7) . . ? F1 Sb1 F1' 54.0(8) . . ? F3' Sb1 F1' 162.5(10) . . ? F5' Sb1 F5 61.7(8) . . ? F6 Sb1 F5 175.7(9) . . ? F6' Sb1 F5 129.9(10) . . ? F2 Sb1 F5 86.1(8) . . ? F1 Sb1 F5 90.6(7) . . ? F3' Sb1 F5 42.3(7) . . ? F1' Sb1 F5 142.4(8) . . ? F5' Sb1 F4 89.3(7) . . ? F6 Sb1 F4 85.9(7) . . ? F6' Sb1 F4 84.4(7) . . ? F2 Sb1 F4 175.8(5) . . ? F1 Sb1 F4 86.6(6) . . ? F3' Sb1 F4 70.3(8) . . ? F1' Sb1 F4 92.5(7) . . ? F5 Sb1 F4 98.1(7) . . ? F5' Sb1 F3 149.1(8) . . ? F6 Sb1 F3 91.0(7) . . ? F6' Sb1 F3 42.5(8) . . ? F2 Sb1 F3 86.7(5) . . ? F1 Sb1 F3 178.1(7) . . ? F3' Sb1 F3 59.2(8) . . ? F1' Sb1 F3 127.9(8) . . ? F5 Sb1 F3 87.5(6) . . ? F4 Sb1 F3 93.5(5) . . ? C6 C1 C2 122.7(4) . . ? C6 C1 O1 119.6(4) . . ? C2 C1 O1 117.5(4) . . ? C3 C2 C1 116.8(4) . . ? C3 C2 H2A 121.6 . . ? C1 C2 H2A 121.6 . . ? C4 C3 C2 123.0(4) . . ? C4 C3 O2 119.6(4) . . ? C2 C3 O2 117.0(4) . . ? C5 C4 C3 117.0(4) . . ? C5 C4 H4A 121.5 . . ? C3 C4 H4A 121.5 . . ? C6 C5 C4 123.5(4) . . ? C6 C5 O3 118.7(4) . . ? C4 C5 O3 117.7(4) . . ? C5 C6 C1 116.9(4) . . ? C5 C6 H6A 121.5 . . ? C1 C6 H6A 121.5 . . ? O4 C7 O1 124.0(4) . . ? O4 C7 C10 125.8(5) . . ? O1 C7 C10 110.1(4) . . ? O5 C8 O2 124.1(5) . . ? O5 C8 C15 125.7(5) . . ? O2 C8 C15 110.2(4) . . ? O6 C9 O3 124.6(4) . . ? O6 C9 C20 124.4(5) . . ? O3 C9 C20 111.0(4) . . ? C11 C10 C14 118.2(4) . . ? C11 C10 C7 124.0(4) . . ? C14 C10 C7 117.7(4) . . ? C12 C11 C10 119.3(4) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? N1 C12 C11 122.8(5) . . ? N1 C12 H12A 118.6 . . ? C11 C12 H12A 118.6 . . ? N1 C13 C14 122.2(4) . . ? N1 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C13 C14 C10 118.8(4) . . ? C13 C14 H14A 120.6 . . ? C10 C14 H14A 120.6 . . ? C19 C15 C16 118.6(5) . . ? C19 C15 C8 119.9(5) . . ? C16 C15 C8 121.5(4) . . ? C15 C16 C17 117.8(5) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? N2 C17 C16 123.7(5) . . ? N2 C17 H17A 118.2 . . ? C16 C17 H17A 118.2 . . ? N2 C18 C19 121.9(5) . . ? N2 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C15 C19 C18 119.5(5) . . ? C15 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C24 C20 C21 119.3(4) . . ? C24 C20 C9 122.0(4) . . ? C21 C20 C9 118.7(4) . . ? C22 C21 C20 118.6(5) . . ? C22 C21 H21A 120.7 . . ? C20 C21 H21A 120.7 . . ? N3 C22 C21 122.8(5) . . ? N3 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? N3 C23 C24 123.9(5) . . ? N3 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C20 C24 C23 117.4(5) . . ? C20 C24 H24A 121.3 . . ? C23 C24 H24A 121.3 . . ? S1 O7 Ag1 164.5(3) . . ? O7 S1 C26 105.3(3) . . ? O7 S1 C25 106.3(3) . . ? C26 S1 C25 99.1(4) . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 S2 C27 106.4(4) . . ? O8 S2 C28 107.5(3) . . ? C27 S2 C28 97.9(4) . . ? S2 C28 H28A 109.5 . . ? S2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S2 C27 H27A 109.5 . . ? S2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O9 S3 C30 106.0(4) . . ? O9 S3 C29 108.0(4) . . ? C30 S3 C29 95.3(7) . . ? S3 C30 H30A 109.5 . . ? S3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? S3 C29 H29A 109.5 . . ? S3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C7 O1 C1 115.9(4) . . ? C8 O2 C3 118.0(4) . . ? C9 O3 C5 116.3(4) . . ? O1W O3W' O3W 120(2) 2_557 . ? 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 N3 Ag1 N1 C12 124.8(4) 1_444 . . . ? N2 Ag1 N1 C12 -59.0(4) 1_554 . . . ? O7 Ag1 N1 C12 30.7(4) . . . . ? N3 Ag1 N1 C13 -69.0(4) 1_444 . . . ? N2 Ag1 N1 C13 107.2(4) 1_554 . . . ? O7 Ag1 N1 C13 -163.2(4) . . . . ? C6 C1 C2 C3 0.3(7) . . . . ? O1 C1 C2 C3 176.3(4) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? C1 C2 C3 O2 173.3(4) . . . . ? C2 C3 C4 C5 0.8(7) . . . . ? O2 C3 C4 C5 -172.9(4) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? C3 C4 C5 O3 -177.1(4) . . . . ? C4 C5 C6 C1 0.8(7) . . . . ? O3 C5 C6 C1 176.9(4) . . . . ? C2 C1 C6 C5 -0.5(7) . . . . ? O1 C1 C6 C5 -176.3(4) . . . . ? O4 C7 C10 C11 -179.0(5) . . . . ? O1 C7 C10 C11 1.1(7) . . . . ? O4 C7 C10 C14 2.2(8) . . . . ? O1 C7 C10 C14 -177.8(4) . . . . ? C14 C10 C11 C12 1.2(8) . . . . ? C7 C10 C11 C12 -177.6(5) . . . . ? C13 N1 C12 C11 -0.5(8) . . . . ? Ag1 N1 C12 C11 165.9(4) . . . . ? C10 C11 C12 N1 -0.7(8) . . . . ? C12 N1 C13 C14 1.1(8) . . . . ? Ag1 N1 C13 C14 -165.2(4) . . . . ? N1 C13 C14 C10 -0.5(8) . . . . ? C11 C10 C14 C13 -0.6(7) . . . . ? C7 C10 C14 C13 178.3(5) . . . . ? O5 C8 C15 C19 6.9(9) . . . . ? O2 C8 C15 C19 -173.3(5) . . . . ? O5 C8 C15 C16 -171.0(6) . . . . ? O2 C8 C15 C16 8.8(7) . . . . ? C19 C15 C16 C17 -0.3(8) . . . . ? C8 C15 C16 C17 177.6(5) . . . . ? C18 N2 C17 C16 1.0(8) . . . . ? Ag1 N2 C17 C16 -176.7(4) 1_556 . . . ? C15 C16 C17 N2 -0.5(8) . . . . ? C17 N2 C18 C19 -0.6(9) . . . . ? Ag1 N2 C18 C19 177.1(5) 1_556 . . . ? C16 C15 C19 C18 0.7(9) . . . . ? C8 C15 C19 C18 -177.3(5) . . . . ? N2 C18 C19 C15 -0.2(10) . . . . ? O6 C9 C20 C24 173.6(5) . . . . ? O3 C9 C20 C24 -4.5(7) . . . . ? O6 C9 C20 C21 -5.2(8) . . . . ? O3 C9 C20 C21 176.8(5) . . . . ? C24 C20 C21 C22 0.3(9) . . . . ? C9 C20 C21 C22 179.1(5) . . . . ? C23 N3 C22 C21 0.6(9) . . . . ? Ag1 N3 C22 C21 -179.9(5) 1_666 . . . ? C20 C21 C22 N3 -0.6(9) . . . . ? C22 N3 C23 C24 -0.3(9) . . . . ? Ag1 N3 C23 C24 -179.8(4) 1_666 . . . ? C21 C20 C24 C23 -0.1(8) . . . . ? C9 C20 C24 C23 -178.8(5) . . . . ? N3 C23 C24 C20 0.0(9) . . . . ? N3 Ag1 O7 S1 -29.4(12) 1_444 . . . ? N1 Ag1 O7 S1 92.5(12) . . . . ? N2 Ag1 O7 S1 -151.9(12) 1_554 . . . ? Ag1 O7 S1 C26 163.4(12) . . . . ? Ag1 O7 S1 C25 -92.0(12) . . . . ? O4 C7 O1 C1 9.6(7) . . . . ? C10 C7 O1 C1 -170.4(4) . . . . ? C6 C1 O1 C7 -110.1(5) . . . . ? C2 C1 O1 C7 73.8(5) . . . . ? O5 C8 O2 C3 3.5(8) . . . . ? C15 C8 O2 C3 -176.3(4) . . . . ? C4 C3 O2 C8 -84.8(6) . . . . ? C2 C3 O2 C8 101.1(5) . . . . ? O6 C9 O3 C5 -7.6(8) . . . . ? C20 C9 O3 C5 170.4(4) . . . . ? C6 C5 O3 C9 105.4(5) . . . . ? C4 C5 O3 C9 -78.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.553 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 940528' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H19 Ag F3 N3 O10' _chemical_formula_weight 722.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 10.6004(12) _cell_length_b 11.6175(14) _cell_length_c 12.1474(14) _cell_angle_alpha 83.729(2) _cell_angle_beta 83.464(2) _cell_angle_gamma 74.505(2) _cell_volume 1427.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.6475 _cell_measurement_theta_max 30.2499 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9044 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12077 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.08 _reflns_number_total 6133 _reflns_number_gt 5214 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0851P)^2^+2.6802P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6133 _refine_ls_number_parameters 396 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.072 _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 0.44760(3) -0.32786(3) 0.82513(2) 0.03405(13) Uani 1 1 d . . . C1 C 0.0386(4) 0.0281(3) 0.2580(3) 0.0265(7) Uani 1 1 d . . . C2 C 0.0644(3) 0.1346(3) 0.2111(3) 0.0266(7) Uani 1 1 d . . . H2A H 0.1236 0.1674 0.2395 0.032 Uiso 1 1 calc R . . C3 C -0.0022(4) 0.1900(3) 0.1198(3) 0.0255(7) Uani 1 1 d . . . C4 C -0.0969(4) 0.1472(3) 0.0804(3) 0.0269(7) Uani 1 1 d . . . H4A H -0.1429 0.1873 0.0208 0.032 Uiso 1 1 calc R . . C5 C -0.1206(4) 0.0416(3) 0.1336(3) 0.0266(7) Uani 1 1 d . . . C6 C -0.0520(4) -0.0210(3) 0.2214(3) 0.0281(7) Uani 1 1 d . . . H6A H -0.0666 -0.0930 0.2541 0.034 Uiso 1 1 calc R . . C7 C 0.2328(4) -0.0583(4) 0.3498(3) 0.0310(8) Uani 1 1 d . . . C8 C 0.0649(4) 0.3085(3) -0.0364(3) 0.0287(8) Uani 1 1 d . . . C9 C -0.2947(4) -0.0568(3) 0.1494(3) 0.0279(7) Uani 1 1 d . . . C10 C 0.2783(4) -0.1134(3) 0.4589(3) 0.0296(8) Uani 1 1 d . . . C11 C 0.1979(4) -0.1562(4) 0.5418(3) 0.0327(8) Uani 1 1 d . . . H11A H 0.1102 -0.1487 0.5321 0.039 Uiso 1 1 calc R . . C12 C 0.2499(4) -0.2104(4) 0.6393(3) 0.0325(8) Uani 1 1 d . . . H12A H 0.1954 -0.2400 0.6941 0.039 Uiso 1 1 calc R A . C13 C 0.4500(4) -0.1778(4) 0.5802(4) 0.0425(10) Uani 1 1 d . . . H13A H 0.5359 -0.1827 0.5940 0.051 Uiso 1 1 calc R A . C14 C 0.4080(4) -0.1248(4) 0.4792(4) 0.0408(10) Uani 1 1 d . . . H14A H 0.4651 -0.0970 0.4255 0.049 Uiso 1 1 calc R . . C15 C 0.1426(4) 0.3992(3) -0.0632(3) 0.0274(7) Uani 1 1 d . . . C16 C 0.1921(4) 0.4454(3) 0.0177(3) 0.0310(8) Uani 1 1 d . . . H16A H 0.1733 0.4246 0.0927 0.037 Uiso 1 1 calc R . . C17 C 0.2709(4) 0.5238(4) -0.0160(4) 0.0354(9) Uani 1 1 d . . . H17A H 0.3038 0.5555 0.0382 0.042 Uiso 1 1 calc R . . C18 C 0.2533(5) 0.5095(4) -0.1999(4) 0.0378(9) Uani 1 1 d . . . H18A H 0.2745 0.5307 -0.2745 0.045 Uiso 1 1 calc R . . C19 C 0.1735(4) 0.4317(4) -0.1741(3) 0.0357(9) Uani 1 1 d . . . H19A H 0.1413 0.4018 -0.2300 0.043 Uiso 1 1 calc R . . C20 C -0.3621(3) -0.1131(3) 0.0767(3) 0.0247(7) Uani 1 1 d . . . C21 C -0.3454(3) -0.0969(3) -0.0383(3) 0.0251(7) Uani 1 1 d . . . H21A H -0.2932 -0.0484 -0.0731 0.030 Uiso 1 1 calc R . . C22 C -0.4082(4) -0.1543(3) -0.1000(3) 0.0282(7) Uani 1 1 d . . . H22A H -0.3977 -0.1426 -0.1772 0.034 Uiso 1 1 calc R . . C23 C -0.4995(4) -0.2400(3) 0.0579(3) 0.0295(8) Uani 1 1 d . . . H23A H -0.5523 -0.2889 0.0909 0.035 Uiso 1 1 calc R . . C24 C -0.4418(4) -0.1855(3) 0.1257(3) 0.0282(7) Uani 1 1 d . . . H24A H -0.4558 -0.1969 0.2026 0.034 Uiso 1 1 calc R . . N1 N 0.3742(3) -0.2225(3) 0.6591(3) 0.0353(7) Uani 1 1 d . . . N2 N 0.3014(4) 0.5558(3) -0.1232(3) 0.0360(8) Uani 1 1 d . . . N3 N -0.4837(3) -0.2262(3) -0.0541(3) 0.0279(6) Uani 1 1 d . . . O1 O 0.0989(3) -0.0305(2) 0.3531(2) 0.0302(6) Uani 1 1 d . . . O2 O 0.0319(3) 0.2946(2) 0.0746(2) 0.0285(5) Uani 1 1 d . . . O3 O -0.2097(3) -0.0019(2) 0.0853(2) 0.0306(6) Uani 1 1 d . . . O4 O 0.3029(3) -0.0424(3) 0.2688(2) 0.0463(8) Uani 1 1 d . . . O5 O 0.0387(3) 0.2538(3) -0.1040(2) 0.0414(7) Uani 1 1 d . . . O6 O -0.3124(3) -0.0595(3) 0.2483(2) 0.0423(7) Uani 1 1 d . . . O7 O 0.6907(6) -0.3867(6) 0.7186(4) 0.1030(19) Uani 1 1 d U A . F1 F 0.8362(8) -0.6801(6) 0.6769(7) 0.164(2) Uani 1 1 d U . . F2 F 0.9218(5) -0.5424(7) 0.6749(6) 0.148(2) Uani 1 1 d U . . F3 F 0.8047(7) -0.5498(7) 0.5491(5) 0.158(2) Uani 1 1 d U . . C25 C 0.8139(8) -0.5673(9) 0.6573(8) 0.095(2) Uani 1 1 d U A . C26 C 0.6913(7) -0.4933(9) 0.7240(6) 0.0806(18) Uani 1 1 d U . . C28 C 0.2217(6) 0.2080(6) 0.3960(6) 0.0677(18) Uani 1 1 d . . . O9 O 0.1622(10) 0.2240(9) 0.4969(12) 0.202(5) Uani 1 1 d . . . O8 O 0.6196(15) -0.5659(13) 0.7682(12) 0.103(3) Uiso 0.50 1 d PU A 1 O8A O 0.6061(12) -0.5139(11) 0.7726(10) 0.077(2) Uiso 0.50 1 d PU A 2 C29 C 0.468(3) 0.444(3) -0.472(3) 0.311(14) Uiso 1 1 d . . . O10 O 0.491(3) 0.364(3) -0.355(3) 0.437(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03729(19) 0.0392(2) 0.03232(18) 0.00417(12) -0.01112(12) -0.02084(14) C1 0.0259(17) 0.0289(18) 0.0244(17) 0.0014(14) -0.0045(13) -0.0074(14) C2 0.0240(17) 0.0302(18) 0.0280(18) 0.0005(14) -0.0046(13) -0.0111(14) C3 0.0264(17) 0.0243(17) 0.0275(17) 0.0004(13) -0.0021(13) -0.0106(14) C4 0.0267(17) 0.0278(18) 0.0274(18) 0.0003(14) -0.0070(14) -0.0083(14) C5 0.0268(17) 0.0286(18) 0.0283(18) -0.0024(14) -0.0047(14) -0.0128(14) C6 0.0281(18) 0.0276(18) 0.0298(18) 0.0017(14) -0.0039(14) -0.0103(14) C7 0.0277(18) 0.038(2) 0.0261(18) 0.0022(15) -0.0025(14) -0.0073(16) C8 0.0291(18) 0.0255(17) 0.0321(19) 0.0021(15) -0.0052(14) -0.0088(15) C9 0.0255(17) 0.0283(18) 0.0321(19) -0.0025(14) -0.0026(14) -0.0105(14) C10 0.0294(18) 0.0326(19) 0.0253(18) 0.0026(15) -0.0036(14) -0.0069(15) C11 0.0255(18) 0.042(2) 0.0284(19) 0.0029(16) -0.0014(14) -0.0069(16) C12 0.0304(19) 0.037(2) 0.0272(18) 0.0037(15) -0.0006(15) -0.0071(16) C13 0.032(2) 0.060(3) 0.037(2) 0.012(2) -0.0106(17) -0.018(2) C14 0.033(2) 0.058(3) 0.033(2) 0.0099(19) -0.0047(16) -0.0194(19) C15 0.0251(17) 0.0210(16) 0.036(2) 0.0003(14) -0.0057(14) -0.0065(14) C16 0.0320(19) 0.0314(19) 0.0316(19) 0.0021(15) -0.0067(15) -0.0120(16) C17 0.039(2) 0.036(2) 0.038(2) -0.0001(17) -0.0117(17) -0.0182(17) C18 0.049(2) 0.037(2) 0.032(2) 0.0029(16) -0.0034(17) -0.0226(19) C19 0.044(2) 0.038(2) 0.032(2) 0.0018(16) -0.0074(17) -0.0215(18) C20 0.0214(16) 0.0235(16) 0.0293(18) -0.0021(14) -0.0047(13) -0.0050(13) C21 0.0220(16) 0.0268(17) 0.0277(17) 0.0032(14) -0.0032(13) -0.0101(13) C22 0.0283(18) 0.0287(18) 0.0285(18) 0.0038(14) -0.0065(14) -0.0099(15) C23 0.0277(18) 0.0309(19) 0.0325(19) 0.0018(15) -0.0006(14) -0.0148(15) C24 0.0269(18) 0.0338(19) 0.0263(18) -0.0007(14) -0.0012(13) -0.0129(15) N1 0.0338(18) 0.0426(19) 0.0286(17) 0.0026(14) -0.0051(13) -0.0096(15) N2 0.0397(19) 0.0368(18) 0.0368(18) 0.0043(14) -0.0071(14) -0.0201(15) N3 0.0250(15) 0.0294(16) 0.0325(16) 0.0024(13) -0.0060(12) -0.0132(12) O1 0.0278(13) 0.0370(14) 0.0265(13) 0.0064(11) -0.0071(10) -0.0109(11) O2 0.0332(14) 0.0268(13) 0.0297(13) 0.0001(10) -0.0049(10) -0.0148(11) O3 0.0340(14) 0.0328(14) 0.0315(14) 0.0024(11) -0.0096(11) -0.0192(11) O4 0.0338(16) 0.064(2) 0.0303(15) 0.0141(14) 0.0017(12) -0.0030(14) O5 0.061(2) 0.0386(16) 0.0348(16) -0.0030(12) -0.0027(14) -0.0316(15) O6 0.0410(16) 0.065(2) 0.0292(15) -0.0099(14) 0.0013(12) -0.0280(15) O7 0.101(4) 0.121(4) 0.058(3) -0.016(3) -0.009(3) 0.026(4) F1 0.162(5) 0.114(4) 0.202(6) -0.031(4) 0.000(5) -0.011(4) F2 0.068(3) 0.174(5) 0.196(5) -0.073(4) -0.015(3) 0.003(3) F3 0.130(4) 0.206(6) 0.104(4) -0.055(4) 0.011(3) 0.023(4) C25 0.078(4) 0.111(5) 0.089(4) -0.031(4) -0.023(3) 0.000(4) C26 0.065(3) 0.115(4) 0.056(3) -0.014(3) -0.030(3) 0.000(4) C28 0.055(3) 0.087(4) 0.067(4) -0.043(3) -0.024(3) -0.005(3) O9 0.147(8) 0.131(7) 0.329(16) -0.039(9) 0.047(9) -0.057(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 N3 2.271(3) 1_656 ? Ag1 N2 2.310(3) 1_546 ? Ag1 N1 2.341(3) . ? Ag1 O8A 2.453(12) . ? C1 C6 1.375(5) . ? C1 C2 1.387(5) . ? C1 O1 1.404(4) . ? C2 C3 1.386(5) . ? C2 H2A 0.9300 . ? C3 C4 1.382(5) . ? C3 O2 1.398(4) . ? C4 C5 1.392(5) . ? C4 H4A 0.9300 . ? C5 C6 1.385(5) . ? C5 O3 1.393(4) . ? C6 H6A 0.9300 . ? C7 O4 1.191(5) . ? C7 O1 1.366(5) . ? C7 C10 1.481(5) . ? C8 O5 1.190(5) . ? C8 O2 1.358(5) . ? C8 C15 1.491(5) . ? C9 O6 1.193(5) . ? C9 O3 1.365(4) . ? C9 C20 1.495(5) . ? C10 C11 1.382(5) . ? C10 C14 1.393(6) . ? C11 C12 1.379(5) . ? C11 H11A 0.9300 . ? C12 N1 1.334(5) . ? C12 H12A 0.9300 . ? C13 N1 1.332(5) . ? C13 C14 1.377(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.382(5) . ? C15 C19 1.385(6) . ? C16 C17 1.394(5) . ? C16 H16A 0.9300 . ? C17 N2 1.341(6) . ? C17 H17A 0.9300 . ? C18 N2 1.335(6) . ? C18 C19 1.385(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.386(5) . ? C20 C24 1.391(5) . ? C21 C22 1.383(5) . ? C21 H21A 0.9300 . ? C22 N3 1.343(5) . ? C22 H22A 0.9300 . ? C23 N3 1.348(5) . ? C23 C24 1.374(5) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? N2 Ag1 2.310(3) 1_564 ? N3 Ag1 2.271(3) 1_454 ? O7 C26 1.231(11) . ? F1 C25 1.268(11) . ? F2 C25 1.298(10) . ? F3 C25 1.319(10) . ? C25 C26 1.550(11) . ? C26 O8A 1.088(13) . ? C26 O8 1.314(17) . ? C28 O9 1.321(13) . ? C29 C29 1.66(5) 2_664 ? C29 O10 1.62(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 N3 Ag1 N2 123.53(12) 1_656 1_546 ? N3 Ag1 N1 117.41(12) 1_656 . ? N2 Ag1 N1 103.46(12) 1_546 . ? N3 Ag1 O8A 115.0(3) 1_656 . ? N2 Ag1 O8A 86.1(3) 1_546 . ? N1 Ag1 O8A 106.3(3) . . ? C6 C1 C2 123.4(3) . . ? C6 C1 O1 116.5(3) . . ? C2 C1 O1 119.9(3) . . ? C3 C2 C1 116.9(3) . . ? C3 C2 H2A 121.5 . . ? C1 C2 H2A 121.5 . . ? C4 C3 C2 122.6(3) . . ? C4 C3 O2 123.7(3) . . ? C2 C3 O2 113.7(3) . . ? C3 C4 C5 117.4(3) . . ? C3 C4 H4A 121.3 . . ? C5 C4 H4A 121.3 . . ? C6 C5 C4 122.6(3) . . ? C6 C5 O3 122.4(3) . . ? C4 C5 O3 114.8(3) . . ? C1 C6 C5 117.1(3) . . ? C1 C6 H6A 121.5 . . ? C5 C6 H6A 121.5 . . ? O4 C7 O1 124.1(4) . . ? O4 C7 C10 125.0(4) . . ? O1 C7 C10 110.9(3) . . ? O5 C8 O2 125.0(3) . . ? O5 C8 C15 123.9(4) . . ? O2 C8 C15 111.1(3) . . ? O6 C9 O3 125.1(3) . . ? O6 C9 C20 125.2(3) . . ? O3 C9 C20 109.7(3) . . ? C11 C10 C14 118.0(4) . . ? C11 C10 C7 122.8(4) . . ? C14 C10 C7 119.2(3) . . ? C12 C11 C10 118.9(4) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? N1 C12 C11 123.5(4) . . ? N1 C12 H12A 118.2 . . ? C11 C12 H12A 118.2 . . ? N1 C13 C14 123.4(4) . . ? N1 C13 H13A 118.3 . . ? C14 C13 H13A 118.3 . . ? C13 C14 C10 118.8(4) . . ? C13 C14 H14A 120.6 . . ? C10 C14 H14A 120.6 . . ? C16 C15 C19 119.1(3) . . ? C16 C15 C8 122.6(3) . . ? C19 C15 C8 118.1(3) . . ? C15 C16 C17 118.4(4) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? N2 C17 C16 123.0(4) . . ? N2 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? N2 C18 C19 123.3(4) . . ? N2 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C18 C19 C15 118.5(4) . . ? C18 C19 H19A 120.7 . . ? C15 C19 H19A 120.7 . . ? C21 C20 C24 119.0(3) . . ? C21 C20 C9 121.9(3) . . ? C24 C20 C9 119.1(3) . . ? C22 C21 C20 118.6(3) . . ? C22 C21 H21A 120.7 . . ? C20 C21 H21A 120.7 . . ? N3 C22 C21 123.2(3) . . ? N3 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? N3 C23 C24 123.4(3) . . ? N3 C23 H23A 118.3 . . ? C24 C23 H23A 118.3 . . ? C23 C24 C20 118.5(3) . . ? C23 C24 H24A 120.7 . . ? C20 C24 H24A 120.7 . . ? C12 N1 C13 117.3(3) . . ? C12 N1 Ag1 118.4(3) . . ? C13 N1 Ag1 124.3(3) . . ? C18 N2 C17 117.7(3) . . ? C18 N2 Ag1 120.5(3) . 1_564 ? C17 N2 Ag1 121.5(3) . 1_564 ? C22 N3 C23 117.3(3) . . ? C22 N3 Ag1 115.5(2) . 1_454 ? C23 N3 Ag1 126.8(2) . 1_454 ? C7 O1 C1 118.4(3) . . ? C8 O2 C3 119.2(3) . . ? C9 O3 C5 120.9(3) . . ? F1 C25 F2 105.1(8) . . ? F1 C25 F3 103.8(8) . . ? F2 C25 F3 106.7(9) . . ? F1 C25 C26 115.2(9) . . ? F2 C25 C26 112.9(7) . . ? F3 C25 C26 112.3(7) . . ? O8A C26 O7 113.8(10) . . ? O8A C26 O8 26.3(9) . . ? O7 C26 O8 140.1(10) . . ? O8A C26 C25 134.7(12) . . ? O7 C26 C25 111.5(8) . . ? O8 C26 C25 108.4(10) . . ? C26 O8A Ag1 109.9(10) . . ? C29 C29 O10 130(4) 2_664 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.201 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 940529' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag Cl3 F3 N3 O10 S2' _chemical_formula_weight 895.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8496(15) _cell_length_b 12.2389(17) _cell_length_c 13.0651(18) _cell_angle_alpha 92.079(2) _cell_angle_beta 93.681(2) _cell_angle_gamma 92.701(2) _cell_volume 1728.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.439 _cell_measurement_theta_max 53.004 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.8970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14669 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.33 _reflns_number_total 7559 _reflns_number_gt 5245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1353P)^2^+9.0821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7559 _refine_ls_number_parameters 501 _refine_ls_number_restraints 609 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2107 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.841 _refine_ls_shift/su_max 0.037 _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 0.31322(2) 0.278908(19) 1.119262(16) 0.04548(6) Uani 1 1 d . . . Cl1 Cl -0.08371(14) 0.65010(14) 0.39501(14) 0.1215(6) Uani 1 1 d U . . Cl2 Cl 0.07898(16) 0.48049(11) 0.34546(13) 0.1149(5) Uani 1 1 d . . . Cl3 Cl 0.16766(13) 0.66632(11) 0.46956(11) 0.0973(4) Uani 1 1 d . . . C1 C 0.6168(2) -0.0222(2) 0.60422(19) 0.0339(5) Uani 1 1 d U . . C2 C 0.5616(2) -0.1179(2) 0.5560(2) 0.0363(6) Uani 1 1 d U . . H2A H 0.4932 -0.1561 0.5826 0.044 Uiso 1 1 calc R . . C3 C 0.6130(3) -0.1533(2) 0.46732(19) 0.0364(6) Uani 1 1 d U . . C4 C 0.7110(3) -0.0985(2) 0.4261(2) 0.0378(6) Uani 1 1 d U . . H4A H 0.7447 -0.1257 0.3654 0.045 Uiso 1 1 calc R . . C5 C 0.7584(2) -0.0035(2) 0.47573(19) 0.0355(6) Uani 1 1 d U . . C6 C 0.7142(2) 0.0362(2) 0.56602(19) 0.0339(5) Uani 1 1 d U . . H6A H 0.7495 0.1012 0.6003 0.041 Uiso 1 1 calc R . . C7 C 0.5248(2) -0.0310(2) 0.76576(19) 0.0334(5) Uani 1 1 d U . . C8 C 0.5931(3) -0.3439(2) 0.4361(2) 0.0393(6) Uani 1 1 d U . . C9 C 0.8260(2) 0.1161(2) 0.3532(2) 0.0385(6) Uani 1 1 d U . . C10 C 0.4647(2) 0.0414(2) 0.83926(19) 0.0341(6) Uani 1 1 d U . . C11 C 0.4906(3) 0.1541(2) 0.8445(2) 0.0438(6) Uani 1 1 d U B . H11A H 0.5434 0.1874 0.7981 0.053 Uiso 1 1 calc R . . C12 C 0.4375(3) 0.2165(2) 0.9189(2) 0.0462(7) Uani 1 1 d U . . H12A H 0.4568 0.2931 0.9234 0.055 Uiso 1 1 calc R B . C13 C 0.3339(3) 0.0661(2) 0.9773(2) 0.0395(6) Uani 1 1 d U . . H13A H 0.2776 0.0356 1.0225 0.047 Uiso 1 1 calc R B . C14 C 0.3846(2) -0.0038(2) 0.90654(19) 0.0368(6) Uani 1 1 d U B . H14A H 0.3648 -0.0804 0.9045 0.044 Uiso 1 1 calc R . . C15 C 0.5285(3) -0.4311(2) 0.3666(2) 0.0368(6) Uani 1 1 d U . . C16 C 0.5730(3) -0.5353(2) 0.3653(2) 0.0445(7) Uani 1 1 d U . . H16A H 0.6426 -0.5517 0.4089 0.053 Uiso 1 1 calc R . . C17 C 0.5145(3) -0.6149(2) 0.2996(2) 0.0426(6) Uani 1 1 d U . . H17A H 0.5455 -0.6862 0.2993 0.051 Uiso 1 1 calc R . . C18 C 0.3735(3) -0.4966(2) 0.2400(2) 0.0421(6) Uani 1 1 d U . . H18A H 0.3024 -0.4828 0.1969 0.050 Uiso 1 1 calc R . . C19 C 0.4265(3) -0.4108(2) 0.3031(2) 0.0409(6) Uani 1 1 d U . . H19A H 0.3934 -0.3403 0.3025 0.049 Uiso 1 1 calc R . . C20 C 0.9371(2) 0.1620(2) 0.30484(19) 0.0361(6) Uani 1 1 d U . . C21 C 1.0530(2) 0.1760(2) 0.3564(2) 0.0397(6) Uani 1 1 d U . . H21A H 1.0655 0.1575 0.4262 0.048 Uiso 1 1 calc R . . C22 C 1.1492(3) 0.2174(2) 0.3039(2) 0.0413(6) Uani 1 1 d U . . H22A H 1.2280 0.2289 0.3397 0.050 Uiso 1 1 calc R . . C23 C 1.0266(3) 0.2292(2) 0.1563(2) 0.0422(6) Uani 1 1 d U . . H23A H 1.0176 0.2471 0.0861 0.051 Uiso 1 1 calc R . . C24 C 0.9231(3) 0.1905(2) 0.2027(2) 0.0414(6) Uani 1 1 d U . . H24A H 0.8446 0.1835 0.1659 0.050 Uiso 1 1 calc R . . C28 C 0.0656(5) 0.6193(4) 0.3687(3) 0.0845(14) Uani 1 1 d . . . H28A H 0.0877 0.6582 0.3059 0.101 Uiso 1 1 calc R . . N1 N 0.3607(2) 0.1745(2) 0.98476(17) 0.0401(6) Uani 1 1 d . B . N2 N 0.4161(2) -0.59684(19) 0.23610(17) 0.0403(6) Uani 1 1 d . . . N3 N 1.1380(2) 0.24254(19) 0.20462(17) 0.0386(6) Uani 1 1 d . . . O1 O 0.56390(18) 0.02847(14) 0.68742(14) 0.0378(5) Uani 1 1 d U . . O2 O 0.55494(19) -0.24484(15) 0.41241(15) 0.0432(5) Uani 1 1 d U . . O3 O 0.85815(16) 0.05326(16) 0.43395(13) 0.0377(5) Uani 1 1 d U . . O4 O 0.53769(19) -0.12660(15) 0.77408(14) 0.0414(5) Uani 1 1 d U . . O5 O 0.6706(2) -0.35833(18) 0.50295(19) 0.0635(7) Uani 1 1 d U . . O6 O 0.72250(18) 0.1294(2) 0.32396(17) 0.0563(6) Uani 1 1 d U . . O8 O 0.2192(3) 0.7707(2) 0.2230(2) 0.0671(7) Uani 1 1 d U . . O9 O 0.2042(3) 0.8226(2) 0.04327(18) 0.0706(8) Uani 1 1 d U . . F2 F -0.0244(3) 0.9295(3) 0.0929(2) 0.1134(10) Uani 1 1 d U . . F3 F -0.0056(3) 0.8879(2) 0.2498(2) 0.0986(9) Uani 1 1 d . . . S2 S 0.14974(9) 0.78798(8) 0.13181(7) 0.0386(2) Uani 0.7167(13) 1 d P A 1 O7 O 0.0561(4) 0.7016(3) 0.1094(3) 0.0748(11) Uani 0.7167(13) 1 d PU A 1 C25 C 0.0628(5) 0.9048(4) 0.1660(4) 0.0599(13) Uani 0.7167(13) 1 d PU A 1 F1 F 0.1393(4) 0.9931(2) 0.1871(3) 0.0877(12) Uani 0.7167(13) 1 d P A 1 S2A S 0.1646(3) 0.8486(2) 0.1458(2) 0.0467(7) Uani 0.2833(13) 1 d P A 2 O7A O 0.2128(8) 0.9571(7) 0.1785(7) 0.061(2) Uani 0.2833(13) 1 d PU A 2 C25A C 0.0019(12) 0.8597(9) 0.1585(9) 0.051(2) Uani 0.2833(13) 1 d PU A 2 F1A F -0.0616(9) 0.7673(9) 0.1321(11) 0.119(4) Uani 0.2833(13) 1 d P A 2 S1 S 0.2870(2) 0.48886(17) 0.90856(15) 0.1443(7) Uani 1 1 d DU . . O10 O 0.3306(6) 0.4451(4) 1.0046(4) 0.1221(14) Uani 0.759(5) 1 d PDU B 1 C26 C 0.1578(6) 0.5087(6) 0.9410(5) 0.1090(16) Uani 0.759(5) 1 d PDU B 1 H26A H 0.1564 0.5034 1.0156 0.164 Uiso 0.759(5) 1 calc PR B 1 H26B H 0.0990 0.4537 0.9070 0.164 Uiso 0.759(5) 1 calc PR B 1 H26C H 0.1346 0.5819 0.9215 0.164 Uiso 0.759(5) 1 calc PR B 1 C27 C 0.3186(8) 0.6154(5) 0.9126(7) 0.1240(19) Uani 0.759(5) 1 d PDU B 1 H27A H 0.4083 0.6291 0.9238 0.186 Uiso 0.759(5) 1 calc PR B 1 H27B H 0.2775 0.6501 0.9690 0.186 Uiso 0.759(5) 1 calc PR B 1 H27C H 0.2899 0.6461 0.8476 0.186 Uiso 0.759(5) 1 calc PR B 1 O10' O 0.2010(12) 0.4421(14) 0.9871(10) 0.1344(18) Uiso 0.241(5) 1 d PDU B 2 C26' C 0.1493(8) 0.515(2) 0.880(2) 0.134(2) Uiso 0.241(5) 1 d PDU B 2 H26D H 0.1046 0.4742 0.8211 0.161 Uiso 0.241(5) 1 calc PR B 2 H26E H 0.1245 0.5915 0.8917 0.161 Uiso 0.241(5) 1 calc PR B 2 C27' C 0.3940(11) 0.511(2) 0.9920(10) 0.115(4) Uiso 0.241(5) 1 d PDU B 2 H27D H 0.4659 0.4712 0.9734 0.172 Uiso 0.241(5) 1 calc PR B 2 H27E H 0.3675 0.4875 1.0582 0.172 Uiso 0.241(5) 1 calc PR B 2 H27F H 0.4165 0.5901 0.9972 0.172 Uiso 0.241(5) 1 calc PR B 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 0.04602(11) 0.05265(12) 0.03759(10) -0.00933(9) 0.01239(8) -0.00390(9) Cl1 0.1001(9) 0.1291(11) 0.1403(12) 0.0061(10) 0.0339(8) 0.0227(8) Cl2 0.1477(11) 0.0662(6) 0.1342(11) -0.0024(7) 0.0416(9) 0.0016(7) Cl3 0.1105(8) 0.0841(7) 0.1015(8) 0.0087(6) 0.0265(7) 0.0206(6) C1 0.0398(10) 0.0344(10) 0.0279(9) -0.0017(9) 0.0039(9) 0.0059(9) C2 0.0408(11) 0.0354(10) 0.0326(10) 0.0031(9) 0.0018(9) 0.0013(9) C3 0.0442(11) 0.0356(10) 0.0287(10) -0.0027(9) -0.0012(9) 0.0019(9) C4 0.0418(11) 0.0412(11) 0.0300(10) -0.0024(9) 0.0008(9) 0.0049(10) C5 0.0361(10) 0.0433(11) 0.0272(10) 0.0021(9) 0.0015(9) 0.0016(9) C6 0.0367(10) 0.0350(10) 0.0297(10) -0.0017(9) 0.0019(9) 0.0004(9) C7 0.0378(10) 0.0343(10) 0.0284(9) 0.0025(8) 0.0035(9) 0.0009(9) C8 0.0444(11) 0.0391(11) 0.0340(10) 0.0009(9) 0.0024(9) -0.0001(10) C9 0.0356(10) 0.0489(11) 0.0307(10) -0.0008(9) 0.0018(9) -0.0005(10) C10 0.0367(10) 0.0373(11) 0.0282(10) 0.0002(9) 0.0026(9) 0.0020(9) C11 0.0523(12) 0.0398(12) 0.0404(11) 0.0048(10) 0.0159(10) -0.0043(11) C12 0.0554(13) 0.0411(12) 0.0434(12) 0.0002(10) 0.0157(11) 0.0016(11) C13 0.0396(11) 0.0482(12) 0.0306(11) 0.0011(10) 0.0060(9) -0.0048(10) C14 0.0376(11) 0.0420(11) 0.0298(10) -0.0009(9) 0.0021(9) -0.0063(10) C15 0.0412(11) 0.0364(11) 0.0319(10) -0.0018(9) 0.0010(9) -0.0038(10) C16 0.0508(13) 0.0409(12) 0.0401(12) -0.0019(10) -0.0080(11) 0.0007(11) C17 0.0534(13) 0.0362(11) 0.0375(11) 0.0007(10) -0.0003(11) 0.0003(11) C18 0.0391(12) 0.0468(12) 0.0390(12) -0.0030(10) -0.0040(10) 0.0016(10) C19 0.0433(12) 0.0398(11) 0.0391(11) -0.0023(10) 0.0002(10) 0.0037(10) C20 0.0322(10) 0.0470(12) 0.0293(10) 0.0012(9) 0.0023(9) 0.0023(9) C21 0.0371(11) 0.0524(12) 0.0291(10) -0.0005(10) -0.0004(9) 0.0007(10) C22 0.0319(11) 0.0549(13) 0.0357(11) -0.0061(10) -0.0020(10) 0.0006(10) C23 0.0404(12) 0.0555(13) 0.0299(11) 0.0016(10) 0.0001(10) -0.0015(11) C24 0.0344(11) 0.0569(13) 0.0317(11) 0.0005(10) -0.0019(10) -0.0040(11) C28 0.109(3) 0.073(2) 0.076(2) 0.020(2) 0.033(2) 0.002(2) N1 0.0443(11) 0.0468(12) 0.0303(10) 0.0010(9) 0.0104(9) 0.0030(10) N2 0.0430(12) 0.0420(11) 0.0346(11) -0.0053(9) 0.0012(9) -0.0062(10) N3 0.0348(10) 0.0447(12) 0.0355(11) -0.0072(9) 0.0027(9) -0.0003(9) O1 0.0496(10) 0.0305(8) 0.0344(8) -0.0010(7) 0.0135(8) 0.0012(8) O2 0.0534(11) 0.0336(9) 0.0403(10) -0.0067(8) -0.0077(9) 0.0004(8) O3 0.0330(8) 0.0506(10) 0.0294(8) 0.0024(8) 0.0027(7) -0.0018(8) O4 0.0547(11) 0.0366(9) 0.0327(9) 0.0009(7) -0.0001(8) 0.0045(8) O5 0.0745(14) 0.0434(11) 0.0666(13) -0.0047(10) -0.0349(11) 0.0010(10) O6 0.0306(9) 0.0806(14) 0.0587(12) 0.0250(11) 0.0013(9) -0.0008(10) O8 0.0741(14) 0.0690(14) 0.0606(13) 0.0180(11) 0.0076(12) 0.0105(12) O9 0.0974(16) 0.0693(14) 0.0479(12) 0.0069(11) 0.0222(12) 0.0079(13) F2 0.1075(18) 0.131(2) 0.105(2) 0.0199(17) -0.0104(16) 0.0531(16) F3 0.1180(17) 0.0903(16) 0.0951(16) 0.0044(13) 0.0527(13) 0.0224(14) S2 0.0462(5) 0.0351(4) 0.0348(4) 0.0016(4) 0.0057(4) 0.0002(4) O7 0.086(2) 0.0576(18) 0.077(2) -0.0106(17) 0.0018(19) -0.0227(17) C25 0.071(3) 0.056(2) 0.055(2) 0.008(2) 0.010(2) 0.017(2) F1 0.130(3) 0.0384(14) 0.095(2) -0.0138(14) 0.026(2) 0.0011(16) S2A 0.0491(13) 0.0491(14) 0.0413(13) 0.0070(11) -0.0001(11) -0.0030(12) O7A 0.062(4) 0.066(4) 0.055(4) 0.005(3) 0.009(3) -0.019(3) C25A 0.060(4) 0.043(4) 0.052(4) 0.001(4) 0.006(4) 0.005(4) F1A 0.066(5) 0.096(6) 0.187(11) -0.011(7) -0.013(6) -0.028(5) S1 0.1960(15) 0.1334(11) 0.1052(10) 0.0075(9) -0.0054(11) 0.0432(12) O10 0.170(3) 0.110(2) 0.087(2) 0.015(2) 0.000(2) 0.027(2) C26 0.159(3) 0.096(3) 0.078(3) 0.003(3) 0.033(3) 0.033(3) C27 0.147(4) 0.108(3) 0.123(4) -0.008(3) 0.033(3) 0.049(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 2.237(2) . ? Ag1 N3 2.298(2) 1_456 ? Ag1 N2 2.311(2) 1_566 ? Ag1 O10 2.577(5) . ? Cl1 C28 1.734(5) . ? Cl2 C28 1.730(5) . ? Cl3 C28 1.729(5) . ? C1 C6 1.378(4) . ? C1 O1 1.400(3) . ? C1 C2 1.400(4) . ? C2 C3 1.382(4) . ? C2 H2A 0.9500 . ? C3 C4 1.379(4) . ? C3 O2 1.409(3) . ? C4 C5 1.372(4) . ? C4 H4A 0.9500 . ? C5 C6 1.382(4) . ? C5 O3 1.408(3) . ? C6 H6A 0.9500 . ? C7 O4 1.193(3) . ? C7 O1 1.356(3) . ? C7 C10 1.485(4) . ? C8 O5 1.197(4) . ? C8 O2 1.340(3) . ? C8 C15 1.494(4) . ? C9 O6 1.184(3) . ? C9 O3 1.365(3) . ? C9 C20 1.492(4) . ? C10 C14 1.386(4) . ? C10 C11 1.393(4) . ? C11 C12 1.385(4) . ? C11 H11A 0.9500 . ? C12 N1 1.335(4) . ? C12 H12A 0.9500 . ? C13 N1 1.343(4) . ? C13 C14 1.394(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C19 1.378(4) . ? C15 C16 1.385(4) . ? C16 C17 1.377(4) . ? C16 H16A 0.9500 . ? C17 N2 1.342(4) . ? C17 H17A 0.9500 . ? C18 N2 1.332(4) . ? C18 C19 1.391(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.388(4) . ? C20 C24 1.393(4) . ? C21 C22 1.373(4) . ? C21 H21A 0.9500 . ? C22 N3 1.343(4) . ? C22 H22A 0.9500 . ? C23 N3 1.328(3) . ? C23 C24 1.383(4) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C28 H28A 1.0000 . ? N2 Ag1 2.311(2) 1_544 ? N3 Ag1 2.298(2) 1_654 ? O8 S2 1.397(3) . ? O8 S2A 1.524(4) . ? O9 S2 1.402(3) . ? O9 S2A 1.462(4) . ? F2 C25A 1.261(12) . ? F2 C25 1.353(6) . ? F3 C25A 1.238(12) . ? F3 C25 1.378(6) . ? S2 O7 1.440(4) . ? S2 C25 1.808(5) . ? C25 F1 1.341(6) . ? S2A O7A 1.444(9) . ? S2A C25A 1.795(13) . ? C25A F1A 1.319(15) . ? S1 O10 1.443(5) . ? S1 C26 1.518(6) . ? S1 C27' 1.549(11) . ? S1 O10' 1.538(12) . ? S1 C27 1.569(6) . ? S1 C26' 1.569(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O10' C26' 1.77(3) . ? C26' H26D 0.9900 . ? C26' H26E 0.9900 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 121.70(8) . 1_456 ? N1 Ag1 N2 136.97(9) . 1_566 ? N3 Ag1 N2 99.38(8) 1_456 1_566 ? N1 Ag1 O10 87.79(13) . . ? N3 Ag1 O10 121.00(15) 1_456 . ? N2 Ag1 O10 80.77(13) 1_566 . ? C6 C1 O1 115.4(2) . . ? C6 C1 C2 123.3(2) . . ? O1 C1 C2 120.8(2) . . ? C3 C2 C1 115.7(2) . . ? C3 C2 H2A 122.1 . . ? C1 C2 H2A 122.1 . . ? C4 C3 C2 123.4(2) . . ? C4 C3 O2 118.8(2) . . ? C2 C3 O2 117.6(2) . . ? C5 C4 C3 117.8(2) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C4 C5 C6 122.4(2) . . ? C4 C5 O3 118.2(2) . . ? C6 C5 O3 119.3(2) . . ? C1 C6 C5 117.3(2) . . ? C1 C6 H6A 121.4 . . ? C5 C6 H6A 121.4 . . ? O4 C7 O1 124.9(2) . . ? O4 C7 C10 125.6(2) . . ? O1 C7 C10 109.5(2) . . ? O5 C8 O2 123.5(3) . . ? O5 C8 C15 125.6(3) . . ? O2 C8 C15 110.9(2) . . ? O6 C9 O3 123.7(3) . . ? O6 C9 C20 124.7(3) . . ? O3 C9 C20 111.6(2) . . ? C14 C10 C11 119.1(2) . . ? C14 C10 C7 119.7(2) . . ? C11 C10 C7 121.2(2) . . ? C12 C11 C10 118.5(3) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N1 C12 C11 123.4(3) . . ? N1 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? N1 C13 C14 123.3(3) . . ? N1 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C10 C14 C13 118.1(2) . . ? C10 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C19 C15 C16 119.0(2) . . ? C19 C15 C8 122.0(2) . . ? C16 C15 C8 119.1(2) . . ? C17 C16 C15 118.9(3) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? N2 C17 C16 123.4(3) . . ? N2 C17 H17A 118.3 . . ? C16 C17 H17A 118.3 . . ? N2 C18 C19 124.1(3) . . ? N2 C18 H18A 118.0 . . ? C19 C18 H18A 118.0 . . ? C15 C19 C18 117.9(3) . . ? C15 C19 H19A 121.0 . . ? C18 C19 H19A 121.0 . . ? C21 C20 C24 118.9(2) . . ? C21 C20 C9 123.2(2) . . ? C24 C20 C9 117.9(2) . . ? C22 C21 C20 118.2(2) . . ? C22 C21 H21A 120.9 . . ? C20 C21 H21A 120.9 . . ? N3 C22 C21 123.6(2) . . ? N3 C22 H22A 118.2 . . ? C21 C22 H22A 118.2 . . ? N3 C23 C24 123.4(3) . . ? N3 C23 H23A 118.3 . . ? C24 C23 H23A 118.3 . . ? C23 C24 C20 118.2(2) . . ? C23 C24 H24A 120.9 . . ? C20 C24 H24A 120.9 . . ? Cl2 C28 Cl3 110.3(3) . . ? Cl2 C28 Cl1 111.9(3) . . ? Cl3 C28 Cl1 109.7(3) . . ? Cl2 C28 H28A 108.3 . . ? Cl3 C28 H28A 108.3 . . ? Cl1 C28 H28A 108.3 . . ? C12 N1 C13 117.6(2) . . ? C12 N1 Ag1 118.75(19) . . ? C13 N1 Ag1 122.48(18) . . ? C18 N2 C17 116.8(2) . . ? C18 N2 Ag1 116.37(18) . 1_544 ? C17 N2 Ag1 126.87(19) . 1_544 ? C23 N3 C22 117.6(2) . . ? C23 N3 Ag1 122.32(18) . 1_654 ? C22 N3 Ag1 119.30(17) . 1_654 ? C7 O1 C1 120.8(2) . . ? C8 O2 C3 117.6(2) . . ? C9 O3 C5 114.9(2) . . ? S2 O8 S2A 29.97(12) . . ? S2 O9 S2A 30.89(13) . . ? C25A F2 C25 37.3(6) . . ? C25A F3 C25 36.9(6) . . ? O8 S2 O9 122.35(18) . . ? O8 S2 O7 111.3(2) . . ? O9 S2 O7 112.2(2) . . ? O8 S2 C25 102.6(2) . . ? O9 S2 C25 101.9(2) . . ? O7 S2 C25 103.8(2) . . ? F1 C25 F2 108.8(4) . . ? F1 C25 F3 108.2(4) . . ? F2 C25 F3 102.5(4) . . ? F1 C25 S2 110.2(4) . . ? F2 C25 S2 113.9(3) . . ? F3 C25 S2 112.9(3) . . ? O7A S2A O9 109.0(4) . . ? O7A S2A O8 106.5(4) . . ? O9 S2A O8 110.4(2) . . ? O7A S2A C25A 101.9(5) . . ? O9 S2A C25A 117.2(4) . . ? O8 S2A C25A 111.1(4) . . ? F3 C25A F2 116.8(9) . . ? F3 C25A F1A 112.9(11) . . ? F2 C25A F1A 108.6(10) . . ? F3 C25A S2A 104.2(8) . . ? F2 C25A S2A 101.6(8) . . ? F1A C25A S2A 112.2(9) . . ? O10 S1 C26 95.4(4) . . ? O10 S1 C27' 41.5(9) . . ? C26 S1 C27' 116.3(6) . . ? O10 S1 O10' 56.3(6) . . ? C26 S1 O10' 43.5(6) . . ? C27' S1 O10' 91.9(8) . . ? O10 S1 C27 108.7(4) . . ? C26 S1 C27 90.3(4) . . ? C27' S1 C27 73.1(10) . . ? O10' S1 C27 118.5(7) . . ? O10 S1 C26' 124.7(10) . . ? C26 S1 C26' 30.2(10) . . ? C27' S1 C26' 142.5(12) . . ? O10' S1 C26' 69.3(11) . . ? C27 S1 C26' 87.5(9) . . ? S1 O10 Ag1 144.1(3) . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S1 O10' C26' 56.2(6) . . ? S1 C26' O10' 54.5(7) . . ? S1 C26' H26D 118.3 . . ? O10' C26' H26D 118.3 . . ? S1 C26' H26E 118.3 . . ? O10' C26' H26E 118.3 . . ? H26D C26' H26E 115.5 . . ? S1 C27' H27D 109.5 . . ? S1 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? S1 C27' H27F 109.4 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.33 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.740 _refine_diff_density_min -1.768 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 940530'