# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dias947_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[HB(4-Cl-3,5-(CF3)2Pz)3]Ag(cyclooctene)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H15 Ag B Cl3 F18 N6' _chemical_formula_weight 942.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0504(7) _cell_length_b 11.7809(7) _cell_length_c 14.1755(9) _cell_angle_alpha 112.159(1) _cell_angle_beta 99.295(1) _cell_angle_gamma 101.201(1) _cell_volume 1619.61(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 29.32 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15682 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.37 _reflns_number_total 8054 _reflns_number_gt 7437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.6672P] 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 8054 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Ag Ag 0.311746(14) 0.112160(14) 0.315827(12) 0.02061(5) Uani 1 1 d . . . Cl1 Cl -0.20450(5) -0.01244(5) 0.02083(4) 0.02519(11) Uani 1 1 d . . . Cl2 Cl 0.19623(5) -0.02789(5) 0.67297(4) 0.02352(10) Uani 1 1 d . . . Cl3 Cl 0.41252(6) -0.40985(5) 0.06736(5) 0.03004(12) Uani 1 1 d . . . F1 F -0.06736(14) 0.25631(14) 0.21781(14) 0.0389(4) Uani 1 1 d . . . F2 F 0.12699(15) 0.29314(13) 0.29518(14) 0.0438(4) Uani 1 1 d . . . F3 F 0.0718(2) 0.24027(16) 0.12876(15) 0.0559(5) Uani 1 1 d . . . F4 F -0.25139(12) -0.27795(12) -0.00149(10) 0.0267(3) Uani 1 1 d . . . F5 F -0.09235(13) -0.34544(12) 0.04168(10) 0.0262(3) Uani 1 1 d . . . F6 F -0.21273(12) -0.29189(12) 0.14670(10) 0.0269(3) Uani 1 1 d . . . F7 F 0.47472(14) 0.07659(16) 0.65703(12) 0.0408(4) Uani 1 1 d . . . F8 F 0.40116(16) 0.23082(16) 0.65826(16) 0.0625(6) Uani 1 1 d . . . F9 F 0.50081(13) 0.14723(15) 0.54228(12) 0.0372(3) Uani 1 1 d . . . F10 F -0.05694(13) -0.18013(14) 0.52509(10) 0.0326(3) Uani 1 1 d . . . F11 F -0.00851(13) -0.32749(12) 0.40435(12) 0.0327(3) Uani 1 1 d . . . F12 F -0.11074(11) -0.20737(13) 0.36424(10) 0.0256(3) Uani 1 1 d . . . F13 F 0.45157(13) 0.00469(13) 0.10808(12) 0.0313(3) Uani 1 1 d . . . F14 F 0.56573(13) -0.12161(16) 0.11762(13) 0.0374(3) Uani 1 1 d . . . F15 F 0.41791(15) -0.17665(15) -0.02211(11) 0.0369(3) Uani 1 1 d . . . F16 F 0.19254(15) -0.36539(13) 0.31065(11) 0.0314(3) Uani 1 1 d . . . F17 F 0.25181(14) -0.50012(12) 0.18840(12) 0.0304(3) Uani 1 1 d . . . F18 F 0.06392(13) -0.47565(12) 0.15582(12) 0.0316(3) Uani 1 1 d . . . N1 N 0.08821(15) 0.04056(15) 0.24323(12) 0.0158(3) Uani 1 1 d . . . N2 N 0.03404(15) -0.08635(15) 0.20863(12) 0.0143(3) Uani 1 1 d . . . N3 N 0.26441(15) -0.00255(15) 0.41892(12) 0.0148(3) Uani 1 1 d . . . N4 N 0.14962(14) -0.09166(15) 0.37778(12) 0.0139(3) Uani 1 1 d . . . N5 N 0.27774(15) -0.11695(15) 0.17641(13) 0.0163(3) Uani 1 1 d . . . N6 N 0.20672(15) -0.19935(15) 0.20546(12) 0.0144(3) Uani 1 1 d . . . C1 C 0.01310(18) 0.08003(18) 0.18575(15) 0.0169(3) Uani 1 1 d . . . C2 C -0.08914(18) -0.02184(19) 0.11161(15) 0.0171(3) Uani 1 1 d . . . C3 C -0.07343(18) -0.12632(18) 0.12938(14) 0.0157(3) Uani 1 1 d . . . C4 C 0.0368(2) 0.2175(2) 0.20651(18) 0.0228(4) Uani 1 1 d . . . C5 C -0.15771(19) -0.26123(19) 0.07888(15) 0.0191(4) Uani 1 1 d . . . C6 C 0.29334(18) 0.02939(18) 0.52227(15) 0.0170(3) Uani 1 1 d . . . C7 C 0.19753(18) -0.03800(18) 0.54946(14) 0.0169(3) Uani 1 1 d . . . C8 C 0.10667(18) -0.11426(18) 0.45571(14) 0.0155(3) Uani 1 1 d . . . C9 C 0.4163(2) 0.1237(2) 0.59439(16) 0.0256(4) Uani 1 1 d . . . C10 C -0.01767(19) -0.20852(19) 0.43637(15) 0.0195(4) Uani 1 1 d . . . C11 C 0.35455(18) -0.17817(18) 0.12725(14) 0.0167(3) Uani 1 1 d . . . C12 C 0.33481(19) -0.30063(19) 0.12415(15) 0.0183(4) Uani 1 1 d . . . C13 C 0.24040(18) -0.31033(18) 0.17581(14) 0.0168(3) Uani 1 1 d . . . C14 C 0.4478(2) -0.1172(2) 0.08276(17) 0.0223(4) Uani 1 1 d . . . C15 C 0.1857(2) -0.41409(19) 0.20646(17) 0.0229(4) Uani 1 1 d . . . C16 C 0.4950(2) 0.2869(2) 0.39889(17) 0.0255(4) Uani 1 1 d . . . H16A H 0.4993 0.3404 0.4740 0.031 Uiso 1 1 calc R . . C17 C 0.4204(2) 0.3149(2) 0.32951(18) 0.0258(4) Uani 1 1 d . . . H17A H 0.3809 0.3840 0.3642 0.031 Uiso 1 1 calc R . . C18 C 0.4442(2) 0.3090(2) 0.22658(19) 0.0303(5) Uani 1 1 d . B . H18A H 0.3620 0.2932 0.1772 0.036 Uiso 1 1 calc R . . H18B H 0.4797 0.2365 0.1953 0.036 Uiso 1 1 calc R . . C19 C 0.5373(2) 0.4329(2) 0.2398(2) 0.0356(5) Uani 1 1 d . . . H19A H 0.5302 0.4340 0.1696 0.043 Uiso 1 1 calc R A 1 H19B H 0.5107 0.5064 0.2842 0.043 Uiso 1 1 calc R A 1 C20 C 0.6780(4) 0.4511(4) 0.2894(3) 0.0330(9) Uani 0.748(8) 1 d P B 1 H20A H 0.7005 0.3714 0.2521 0.040 Uiso 0.748(8) 1 calc PR B 1 H20B H 0.7317 0.5197 0.2775 0.040 Uiso 0.748(8) 1 calc PR B 1 C21 C 0.7117(3) 0.4849(3) 0.4079(3) 0.0369(10) Uani 0.748(8) 1 d P B 1 H21A H 0.6423 0.5140 0.4377 0.044 Uiso 0.748(8) 1 calc PR B 1 H21B H 0.7909 0.5564 0.4432 0.044 Uiso 0.748(8) 1 calc PR B 1 C20A C 0.6602(10) 0.4997(12) 0.3402(15) 0.042(4) Uani 0.252(8) 1 d P B 2 H20C H 0.7100 0.5800 0.3415 0.050 Uiso 0.252(8) 1 calc PR B 2 H20D H 0.6319 0.5207 0.4060 0.050 Uiso 0.252(8) 1 calc PR B 2 C21A C 0.7433(9) 0.4098(9) 0.3336(10) 0.036(3) Uani 0.252(8) 1 d P B 2 H21C H 0.8330 0.4532 0.3417 0.043 Uiso 0.252(8) 1 calc PR B 2 H21D H 0.7122 0.3337 0.2651 0.043 Uiso 0.252(8) 1 calc PR B 2 C22 C 0.7314(3) 0.3688(3) 0.4323(3) 0.0526(9) Uani 1 1 d . . . H22A H 0.8038 0.3431 0.4055 0.063 Uiso 1 1 calc R B 1 H22B H 0.7557 0.3978 0.5097 0.063 Uiso 1 1 calc R B 1 C23 C 0.6153(2) 0.2514(3) 0.3850(2) 0.0344(5) Uani 1 1 d . B . H23A H 0.6077 0.2045 0.3088 0.041 Uiso 1 1 calc R . . H23B H 0.6279 0.1938 0.4193 0.041 Uiso 1 1 calc R . . B B 0.0959(2) -0.1672(2) 0.25584(16) 0.0146(4) Uani 1 1 d . . . H1 H 0.026(2) -0.257(2) 0.2384(17) 0.009(5) 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 Ag 0.01727(8) 0.02003(8) 0.02441(8) 0.01357(6) 0.00264(6) -0.00136(5) Cl1 0.0237(2) 0.0313(3) 0.0236(2) 0.0161(2) 0.00134(18) 0.00882(19) Cl2 0.0246(2) 0.0347(3) 0.0143(2) 0.01232(19) 0.00855(17) 0.00780(19) Cl3 0.0375(3) 0.0265(3) 0.0374(3) 0.0149(2) 0.0248(2) 0.0180(2) F1 0.0276(7) 0.0267(7) 0.0662(10) 0.0195(7) 0.0138(7) 0.0148(6) F2 0.0372(8) 0.0187(6) 0.0583(10) 0.0093(7) -0.0100(7) 0.0030(6) F3 0.1013(15) 0.0336(8) 0.0621(11) 0.0345(8) 0.0557(11) 0.0245(9) F4 0.0247(6) 0.0262(6) 0.0213(6) 0.0082(5) -0.0036(5) 0.0020(5) F5 0.0289(6) 0.0204(6) 0.0237(6) 0.0043(5) 0.0033(5) 0.0078(5) F6 0.0261(6) 0.0267(6) 0.0238(6) 0.0118(5) 0.0060(5) -0.0035(5) F7 0.0301(7) 0.0566(10) 0.0313(7) 0.0262(7) -0.0053(6) -0.0020(7) F8 0.0337(9) 0.0323(8) 0.0711(13) -0.0230(8) -0.0024(8) 0.0053(7) F9 0.0235(7) 0.0502(9) 0.0322(7) 0.0215(7) 0.0021(6) -0.0065(6) F10 0.0277(7) 0.0454(8) 0.0226(6) 0.0152(6) 0.0126(5) -0.0017(6) F11 0.0267(7) 0.0217(6) 0.0522(9) 0.0190(6) 0.0124(6) 0.0032(5) F12 0.0168(6) 0.0360(7) 0.0255(6) 0.0159(5) 0.0055(5) 0.0047(5) F13 0.0331(7) 0.0275(7) 0.0453(8) 0.0225(6) 0.0224(6) 0.0093(5) F14 0.0202(6) 0.0575(10) 0.0549(9) 0.0394(8) 0.0189(6) 0.0155(6) F15 0.0486(9) 0.0435(8) 0.0231(7) 0.0170(6) 0.0199(6) 0.0075(7) F16 0.0522(9) 0.0293(7) 0.0273(7) 0.0197(6) 0.0223(6) 0.0168(6) F17 0.0384(8) 0.0224(6) 0.0431(8) 0.0187(6) 0.0221(6) 0.0159(6) F18 0.0270(7) 0.0205(6) 0.0454(8) 0.0124(6) 0.0148(6) 0.0013(5) N1 0.0161(7) 0.0156(7) 0.0168(7) 0.0078(6) 0.0064(6) 0.0033(6) N2 0.0139(7) 0.0152(7) 0.0136(7) 0.0061(6) 0.0048(6) 0.0026(6) N3 0.0141(7) 0.0154(7) 0.0148(7) 0.0071(6) 0.0036(6) 0.0026(6) N4 0.0140(7) 0.0146(7) 0.0143(7) 0.0073(6) 0.0056(6) 0.0025(6) N5 0.0156(7) 0.0191(8) 0.0173(7) 0.0104(6) 0.0065(6) 0.0042(6) N6 0.0156(7) 0.0151(7) 0.0134(7) 0.0072(6) 0.0043(6) 0.0030(6) C1 0.0167(8) 0.0198(9) 0.0187(9) 0.0106(7) 0.0083(7) 0.0065(7) C2 0.0166(8) 0.0231(9) 0.0152(8) 0.0106(7) 0.0063(7) 0.0064(7) C3 0.0157(8) 0.0195(9) 0.0125(8) 0.0071(7) 0.0053(6) 0.0044(7) C4 0.0221(10) 0.0224(10) 0.0300(11) 0.0155(8) 0.0101(8) 0.0075(8) C5 0.0192(9) 0.0202(9) 0.0156(8) 0.0070(7) 0.0024(7) 0.0032(7) C6 0.0179(9) 0.0180(9) 0.0149(8) 0.0064(7) 0.0048(7) 0.0054(7) C7 0.0178(9) 0.0206(9) 0.0145(8) 0.0081(7) 0.0067(7) 0.0070(7) C8 0.0165(8) 0.0176(8) 0.0154(8) 0.0085(7) 0.0068(7) 0.0057(7) C9 0.0239(10) 0.0282(11) 0.0178(9) 0.0067(8) 0.0044(8) -0.0009(8) C10 0.0195(9) 0.0233(10) 0.0189(9) 0.0119(8) 0.0084(7) 0.0041(7) C11 0.0167(8) 0.0212(9) 0.0141(8) 0.0090(7) 0.0052(7) 0.0052(7) C12 0.0198(9) 0.0202(9) 0.0158(8) 0.0068(7) 0.0067(7) 0.0074(7) C13 0.0191(9) 0.0160(8) 0.0143(8) 0.0056(7) 0.0052(7) 0.0042(7) C14 0.0224(10) 0.0276(10) 0.0241(10) 0.0150(8) 0.0120(8) 0.0093(8) C15 0.0295(11) 0.0188(9) 0.0273(10) 0.0125(8) 0.0150(8) 0.0095(8) C16 0.0265(10) 0.0218(10) 0.0251(10) 0.0103(8) 0.0059(8) -0.0001(8) C17 0.0242(10) 0.0199(10) 0.0315(11) 0.0112(8) 0.0062(8) 0.0023(8) C18 0.0323(12) 0.0284(11) 0.0285(11) 0.0158(9) 0.0019(9) 0.0023(9) C19 0.0362(13) 0.0335(12) 0.0416(14) 0.0268(11) 0.0049(11) 0.0012(10) C20 0.0313(18) 0.037(2) 0.0322(19) 0.0219(16) 0.0097(14) -0.0026(15) C21 0.0293(17) 0.0389(19) 0.0323(18) 0.0193(15) -0.0018(13) -0.0137(14) C20A 0.020(5) 0.030(6) 0.078(11) 0.030(7) 0.009(6) -0.001(4) C21A 0.020(4) 0.026(5) 0.066(8) 0.027(5) 0.013(4) 0.001(3) C22 0.0227(12) 0.073(2) 0.066(2) 0.0538(18) -0.0087(12) -0.0104(12) C23 0.0208(10) 0.0465(14) 0.0481(15) 0.0346(12) 0.0078(10) 0.0070(10) B 0.0154(9) 0.0158(9) 0.0128(9) 0.0067(7) 0.0042(7) 0.0028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag C16 2.347(2) . ? Ag N1 2.3636(16) . ? Ag C17 2.375(2) . ? Ag N3 2.3870(15) . ? Ag N5 2.5835(16) . ? Cl1 C2 1.7104(19) . ? Cl2 C7 1.7121(19) . ? Cl3 C12 1.7065(19) . ? F1 C4 1.329(2) . ? F2 C4 1.332(3) . ? F3 C4 1.326(3) . ? F4 C5 1.334(2) . ? F5 C5 1.338(2) . ? F6 C5 1.338(2) . ? F7 C9 1.357(3) . ? F8 C9 1.307(3) . ? F9 C9 1.331(3) . ? F10 C10 1.341(2) . ? F11 C10 1.331(2) . ? F12 C10 1.334(2) . ? F13 C14 1.333(2) . ? F14 C14 1.335(2) . ? F15 C14 1.333(3) . ? F16 C15 1.351(2) . ? F17 C15 1.333(2) . ? F18 C15 1.330(3) . ? N1 C1 1.337(2) . ? N1 N2 1.356(2) . ? N2 C3 1.359(2) . ? N2 B 1.552(3) . ? N3 C6 1.333(2) . ? N3 N4 1.354(2) . ? N4 C8 1.363(2) . ? N4 B 1.561(2) . ? N5 C11 1.333(2) . ? N5 N6 1.356(2) . ? N6 C13 1.360(2) . ? N6 B 1.553(2) . ? C1 C2 1.400(3) . ? C1 C4 1.493(3) . ? C2 C3 1.382(3) . ? C3 C5 1.502(3) . ? C6 C7 1.391(3) . ? C6 C9 1.494(3) . ? C7 C8 1.378(3) . ? C8 C10 1.501(3) . ? C11 C12 1.399(3) . ? C11 C14 1.496(3) . ? C12 C13 1.379(3) . ? C13 C15 1.499(3) . ? C16 C17 1.358(3) . ? C16 C23 1.490(3) . ? C16 H16A 1.0000 . ? C17 C18 1.503(3) . ? C17 H17A 1.0000 . ? C18 C19 1.541(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.537(5) . ? C19 C20A 1.614(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.536(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.576(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20A C21A 1.518(16) . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C21A C22 1.659(11) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22 C23 1.530(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? B H1 1.09(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Ag N1 146.98(7) . . ? C16 Ag C17 33.41(8) . . ? N1 Ag C17 117.26(7) . . ? C16 Ag N3 114.17(7) . . ? N1 Ag N3 83.58(5) . . ? C17 Ag N3 142.50(7) . . ? C16 Ag N5 131.05(7) . . ? N1 Ag N5 77.18(5) . . ? C17 Ag N5 131.96(7) . . ? N3 Ag N5 80.81(5) . . ? C1 N1 N2 106.13(15) . . ? C1 N1 Ag 130.26(13) . . ? N2 N1 Ag 115.86(11) . . ? N1 N2 C3 110.42(15) . . ? N1 N2 B 121.35(15) . . ? C3 N2 B 128.20(15) . . ? C6 N3 N4 106.21(15) . . ? C6 N3 Ag 133.14(13) . . ? N4 N3 Ag 114.14(11) . . ? N3 N4 C8 110.14(15) . . ? N3 N4 B 120.27(14) . . ? C8 N4 B 128.78(16) . . ? C11 N5 N6 105.76(15) . . ? C11 N5 Ag 133.71(13) . . ? N6 N5 Ag 108.12(11) . . ? N5 N6 C13 110.52(15) . . ? N5 N6 B 121.15(15) . . ? C13 N6 B 128.09(15) . . ? N1 C1 C2 111.00(17) . . ? N1 C1 C4 121.88(18) . . ? C2 C1 C4 127.03(18) . . ? C3 C2 C1 104.61(16) . . ? C3 C2 Cl1 129.69(16) . . ? C1 C2 Cl1 125.70(15) . . ? N2 C3 C2 107.81(17) . . ? N2 C3 C5 122.59(17) . . ? C2 C3 C5 129.52(17) . . ? F3 C4 F1 107.01(19) . . ? F3 C4 F2 107.7(2) . . ? F1 C4 F2 106.09(18) . . ? F3 C4 C1 112.19(18) . . ? F1 C4 C1 111.42(17) . . ? F2 C4 C1 112.09(17) . . ? F4 C5 F6 107.13(16) . . ? F4 C5 F5 107.74(15) . . ? F6 C5 F5 107.23(16) . . ? F4 C5 C3 110.76(16) . . ? F6 C5 C3 111.98(15) . . ? F5 C5 C3 111.76(16) . . ? N3 C6 C7 111.14(17) . . ? N3 C6 C9 121.76(17) . . ? C7 C6 C9 127.08(17) . . ? C8 C7 C6 104.88(16) . . ? C8 C7 Cl2 128.38(15) . . ? C6 C7 Cl2 126.74(15) . . ? N4 C8 C7 107.63(16) . . ? N4 C8 C10 123.55(17) . . ? C7 C8 C10 128.81(17) . . ? F8 C9 F9 110.0(2) . . ? F8 C9 F7 105.84(19) . . ? F9 C9 F7 104.26(18) . . ? F8 C9 C6 113.11(19) . . ? F9 C9 C6 112.39(17) . . ? F7 C9 C6 110.67(18) . . ? F11 C10 F12 107.58(17) . . ? F11 C10 F10 107.57(16) . . ? F12 C10 F10 106.48(16) . . ? F11 C10 C8 112.31(16) . . ? F12 C10 C8 112.33(16) . . ? F10 C10 C8 110.27(16) . . ? N5 C11 C12 111.51(16) . . ? N5 C11 C14 121.51(17) . . ? C12 C11 C14 126.99(17) . . ? C13 C12 C11 104.35(17) . . ? C13 C12 Cl3 129.49(16) . . ? C11 C12 Cl3 126.16(15) . . ? N6 C13 C12 107.86(17) . . ? N6 C13 C15 121.97(17) . . ? C12 C13 C15 129.98(18) . . ? F15 C14 F13 107.21(17) . . ? F15 C14 F14 106.81(17) . . ? F13 C14 F14 107.85(18) . . ? F15 C14 C11 111.49(18) . . ? F13 C14 C11 111.87(16) . . ? F14 C14 C11 111.35(17) . . ? F18 C15 F17 107.78(17) . . ? F18 C15 F16 107.08(17) . . ? F17 C15 F16 106.86(17) . . ? F18 C15 C13 113.52(18) . . ? F17 C15 C13 110.90(16) . . ? F16 C15 C13 110.41(17) . . ? C17 C16 C23 124.2(2) . . ? C17 C16 Ag 74.45(13) . . ? C23 C16 Ag 113.29(16) . . ? C17 C16 H16A 113.0 . . ? C23 C16 H16A 113.0 . . ? Ag C16 H16A 113.0 . . ? C16 C17 C18 125.0(2) . . ? C16 C17 Ag 72.14(13) . . ? C18 C17 Ag 112.32(15) . . ? C16 C17 H17A 113.4 . . ? C18 C17 H17A 113.4 . . ? Ag C17 H17A 113.4 . . ? C17 C18 C19 112.3(2) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 114.8(2) . . ? C20 C19 C20A 29.9(5) . . ? C18 C19 C20A 117.6(4) . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19A 108.6 . . ? C20A C19 H19A 127.8 . . ? C20 C19 H19B 108.6 . . ? C18 C19 H19B 108.6 . . ? C20A C19 H19B 80.2 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C19 115.2(3) . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 112.7(3) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21A C20A C19 109.7(11) . . ? C21A C20A H20C 109.7 . . ? C19 C20A H20C 109.7 . . ? C21A C20A H20D 109.7 . . ? C19 C20A H20D 109.7 . . ? H20C C20A H20D 108.2 . . ? C20A C21A C22 105.0(9) . . ? C20A C21A H21C 110.8 . . ? C22 C21A H21C 110.8 . . ? C20A C21A H21D 110.8 . . ? C22 C21A H21D 110.8 . . ? H21C C21A H21D 108.8 . . ? C23 C22 C21 115.2(2) . . ? C23 C22 C21A 104.3(4) . . ? C21 C22 C21A 45.2(4) . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? C21A C22 H22A 71.5 . . ? C23 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? C21A C22 H22B 145.4 . . ? H22A C22 H22B 107.5 . . ? C16 C23 C22 111.8(2) . . ? C16 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C16 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N2 B N6 108.93(14) . . ? N2 B N4 110.49(15) . . ? N6 B N4 109.24(15) . . ? N2 B H1 110.4(12) . . ? N6 B H1 108.6(11) . . ? N4 B H1 109.2(12) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.073 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 941720' ####################################################################### # # 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_dias951_0m_a _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[HB(4-(NO2)-3,5-(CF3)2Pz)3]Ag(cyclooctene)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H16 Ag B Cl F18 N9 O6' _chemical_formula_weight 1016.58 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' 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 9.1587(10) _cell_length_b 10.6707(12) _cell_length_c 19.284(2) _cell_angle_alpha 105.190(1) _cell_angle_beta 90.842(2) _cell_angle_gamma 105.294(1) _cell_volume 1747.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4749 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.73 _exptl_crystal_description platy _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16723 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8404 _reflns_number_gt 6847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8404 _refine_ls_number_parameters 554 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.019 _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 Ag Ag 0.25794(2) 0.33152(2) 0.229210(12) 0.01628(7) Uani 1 1 d . . . F1 F 0.5894(2) 0.4786(2) 0.22226(12) 0.0364(5) Uani 1 1 d . . . F2 F 0.8138(2) 0.48921(18) 0.26189(10) 0.0258(4) Uani 1 1 d . . . F3 F 0.7196(2) 0.3606(2) 0.15671(10) 0.0373(5) Uani 1 1 d . . . F4 F 0.6357(3) 0.0535(2) 0.40998(11) 0.0366(5) Uani 1 1 d . . . F5 F 0.6785(2) -0.05396(18) 0.30447(11) 0.0302(5) Uani 1 1 d . . . F6 F 0.4508(2) -0.07795(18) 0.33346(12) 0.0334(5) Uani 1 1 d . . . F7 F 0.1412(2) 0.0673(2) 0.07300(10) 0.0354(5) Uani 1 1 d . . . F8 F -0.0905(2) 0.0611(2) 0.09059(10) 0.0357(5) Uani 1 1 d . . . F9 F -0.0283(2) -0.12454(19) 0.05337(10) 0.0315(5) Uani 1 1 d . . . F10 F 0.1243(2) -0.17078(18) 0.35337(10) 0.0281(4) Uani 1 1 d . . . F11 F -0.1151(2) -0.21321(18) 0.32339(10) 0.0248(4) Uani 1 1 d . . . F12 F 0.0054(2) -0.02254(18) 0.39656(9) 0.0243(4) Uani 1 1 d . . . F13 F 0.0874(2) 0.55403(17) 0.34484(9) 0.0221(4) Uani 1 1 d . . . F14 F 0.3262(2) 0.65224(18) 0.36873(10) 0.0248(4) Uani 1 1 d . . . F15 F 0.1774(2) 0.66883(18) 0.45411(9) 0.0262(4) Uani 1 1 d . . . F16 F 0.4522(2) 0.20898(19) 0.49867(10) 0.0263(4) Uani 1 1 d . . . F17 F 0.2155(2) 0.12278(19) 0.50662(10) 0.0280(4) Uani 1 1 d . . . F18 F 0.3323(2) 0.31643(19) 0.57784(9) 0.0276(4) Uani 1 1 d . . . O1 O 0.9169(2) 0.2562(2) 0.23358(13) 0.0301(6) Uani 1 1 d . . . O2 O 0.9042(2) 0.1734(2) 0.32608(13) 0.0276(5) Uani 1 1 d . . . O3 O -0.2680(3) -0.1859(3) 0.15193(14) 0.0390(6) Uani 1 1 d . . . O4 O -0.1471(3) -0.3227(2) 0.17464(13) 0.0365(6) Uani 1 1 d . . . O5 O 0.3912(2) 0.5929(2) 0.57584(12) 0.0283(5) Uani 1 1 d . . . O6 O 0.1455(3) 0.5408(3) 0.57224(12) 0.0316(6) Uani 1 1 d . . . N1 N 0.4768(3) 0.2683(2) 0.27200(12) 0.0143(5) Uani 1 1 d . . . N2 N 0.4501(3) 0.1670(2) 0.30484(12) 0.0129(5) Uani 1 1 d . . . N3 N 0.8481(3) 0.2120(2) 0.28032(14) 0.0195(5) Uani 1 1 d . . . N4 N 0.1665(3) 0.0872(2) 0.21561(12) 0.0143(5) Uani 1 1 d . . . N5 N 0.1670(3) 0.0529(2) 0.27820(12) 0.0110(5) Uani 1 1 d . . . N6 N -0.1583(3) -0.2104(3) 0.17663(14) 0.0235(6) Uani 1 1 d . . . N7 N 0.2375(3) 0.3563(2) 0.35537(12) 0.0125(5) Uani 1 1 d . . . N8 N 0.2681(3) 0.2643(2) 0.38574(12) 0.0124(5) Uani 1 1 d . . . N9 N 0.2639(3) 0.5299(2) 0.54678(13) 0.0168(5) Uani 1 1 d . . . C1 C 0.6205(3) 0.2932(3) 0.25753(15) 0.0148(6) Uani 1 1 d . . . C2 C 0.6899(3) 0.2087(3) 0.28195(15) 0.0147(6) Uani 1 1 d . . . C3 C 0.5782(3) 0.1281(3) 0.31094(15) 0.0145(6) Uani 1 1 d . . . C4 C 0.6867(3) 0.4053(3) 0.22409(16) 0.0197(6) Uani 1 1 d . . . C5 C 0.5860(3) 0.0124(3) 0.34094(18) 0.0217(7) Uani 1 1 d . . . C6 C 0.0488(3) -0.0020(3) 0.17324(15) 0.0150(6) Uani 1 1 d . . . C7 C -0.0269(3) -0.0952(3) 0.20820(15) 0.0151(6) Uani 1 1 d . . . C8 C 0.0502(3) -0.0582(3) 0.27479(15) 0.0137(6) Uani 1 1 d . . . C9 C 0.0170(4) 0.0010(3) 0.09733(17) 0.0228(7) Uani 1 1 d . . . C10 C 0.0164(3) -0.1168(3) 0.33783(16) 0.0181(6) Uani 1 1 d . . . C11 C 0.2292(3) 0.4614(3) 0.40914(15) 0.0138(6) Uani 1 1 d . . . C12 C 0.2547(3) 0.4365(3) 0.47522(15) 0.0147(6) Uani 1 1 d . . . C13 C 0.2806(3) 0.3109(3) 0.45859(15) 0.0139(6) Uani 1 1 d . . . C14 C 0.2038(3) 0.5845(3) 0.39427(15) 0.0168(6) Uani 1 1 d . . . C15 C 0.3196(3) 0.2378(3) 0.51019(16) 0.0188(6) Uani 1 1 d . . . C16 C 0.2140(4) 0.5041(3) 0.18293(17) 0.0228(7) Uani 1 1 d . . . H16 H 0.1156 0.5240 0.1960 0.027 Uiso 1 1 calc R . . C17 C 0.1954(4) 0.3942(3) 0.12563(17) 0.0218(7) Uani 1 1 d . . . H17 H 0.0866 0.3517 0.1063 0.026 Uiso 1 1 calc R . . C18 C 0.3035(4) 0.3836(3) 0.06737(16) 0.0232(7) Uani 1 1 d . . . H18A H 0.2956 0.2871 0.0448 0.028 Uiso 1 1 calc R . . H18B H 0.4089 0.4285 0.0895 0.028 Uiso 1 1 calc R . . C19 C 0.2706(4) 0.4485(4) 0.00891(18) 0.0305(8) Uani 1 1 d . . . H19A H 0.1600 0.4169 -0.0056 0.037 Uiso 1 1 calc R . . H19B H 0.3227 0.4157 -0.0339 0.037 Uiso 1 1 calc R . . C20 C 0.3199(5) 0.6051(4) 0.03087(19) 0.0381(9) Uani 1 1 d . . . H20A H 0.4269 0.6363 0.0517 0.046 Uiso 1 1 calc R . . H20B H 0.3171 0.6348 -0.0135 0.046 Uiso 1 1 calc R . . C21 C 0.2281(5) 0.6760(4) 0.0838(2) 0.0427(10) Uani 1 1 d . . . H21A H 0.1276 0.6115 0.0829 0.051 Uiso 1 1 calc R . . H21B H 0.2106 0.7512 0.0669 0.051 Uiso 1 1 calc R . . C22 C 0.2975(5) 0.7332(4) 0.16200(19) 0.0342(9) Uani 1 1 d . . . H22A H 0.2232 0.7695 0.1919 0.041 Uiso 1 1 calc R . . H22B H 0.3885 0.8095 0.1646 0.041 Uiso 1 1 calc R . . C23 C 0.3438(4) 0.6304(3) 0.19458(18) 0.0276(7) Uani 1 1 d . . . H23A H 0.4327 0.6072 0.1717 0.033 Uiso 1 1 calc R . . H23B H 0.3731 0.6711 0.2469 0.033 Uiso 1 1 calc R . . B B 0.2964(3) 0.1309(3) 0.33951(17) 0.0124(6) Uani 1 1 d . . . Cl1 Cl 0.4705(3) 1.0451(3) 0.09836(16) 0.0620(7) Uani 0.50 1 d PD A -1 Cl2 Cl 0.4702(5) 0.9683(6) -0.0569(2) 0.1257(17) Uani 0.50 1 d PDU A -1 C24 C 0.5542(18) 0.9751(16) 0.0267(6) 0.103(5) Uani 0.50 1 d PDU A -1 H24A H 0.5513 0.8821 0.0276 0.124 Uiso 0.50 1 calc PR A -1 H24B H 0.6623 1.0275 0.0315 0.124 Uiso 0.50 1 calc PR A -1 H1 H 0.301(3) 0.070(3) 0.3729(13) -0.003(6) 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 Ag 0.01751(12) 0.01625(12) 0.01581(12) 0.00607(8) -0.00030(8) 0.00435(8) F1 0.0194(10) 0.0424(12) 0.0635(15) 0.0392(11) 0.0078(10) 0.0111(9) F2 0.0187(9) 0.0228(10) 0.0333(11) 0.0127(8) -0.0048(8) -0.0035(8) F3 0.0413(13) 0.0432(13) 0.0225(10) 0.0132(9) 0.0086(9) -0.0013(10) F4 0.0533(14) 0.0358(12) 0.0281(11) 0.0140(9) -0.0030(10) 0.0201(10) F5 0.0265(10) 0.0206(10) 0.0501(13) 0.0109(9) 0.0127(9) 0.0159(8) F6 0.0199(10) 0.0162(9) 0.0674(15) 0.0165(10) 0.0102(10) 0.0052(8) F7 0.0368(12) 0.0421(12) 0.0199(10) 0.0136(9) 0.0000(9) -0.0065(10) F8 0.0437(13) 0.0430(12) 0.0252(11) 0.0095(9) -0.0081(9) 0.0204(10) F9 0.0436(12) 0.0249(10) 0.0170(9) -0.0010(8) -0.0071(8) 0.0017(9) F10 0.0272(11) 0.0264(10) 0.0383(11) 0.0190(9) 0.0018(9) 0.0104(8) F11 0.0203(9) 0.0226(9) 0.0251(10) 0.0083(8) 0.0021(7) -0.0069(7) F12 0.0273(10) 0.0243(10) 0.0161(9) 0.0028(7) 0.0054(7) 0.0011(8) F13 0.0210(9) 0.0216(9) 0.0235(9) 0.0039(7) -0.0062(7) 0.0085(7) F14 0.0227(10) 0.0204(9) 0.0322(10) 0.0122(8) 0.0027(8) 0.0026(8) F15 0.0419(12) 0.0193(9) 0.0187(9) -0.0009(7) 0.0026(8) 0.0167(8) F16 0.0241(10) 0.0361(11) 0.0255(10) 0.0126(8) 0.0001(8) 0.0158(8) F17 0.0323(11) 0.0240(10) 0.0256(10) 0.0135(8) -0.0018(8) -0.0022(8) F18 0.0408(12) 0.0281(10) 0.0139(9) 0.0044(8) -0.0011(8) 0.0113(9) O1 0.0190(12) 0.0356(14) 0.0399(15) 0.0140(12) 0.0129(11) 0.0105(10) O2 0.0160(11) 0.0279(12) 0.0446(15) 0.0160(11) 0.0005(10) 0.0100(10) O3 0.0187(13) 0.0453(16) 0.0399(15) -0.0039(12) -0.0094(11) 0.0029(11) O4 0.0509(17) 0.0183(12) 0.0285(13) 0.0052(10) -0.0056(12) -0.0086(11) O5 0.0195(12) 0.0306(13) 0.0211(12) -0.0081(10) -0.0014(9) -0.0012(10) O6 0.0196(12) 0.0429(15) 0.0244(12) -0.0043(11) 0.0069(10) 0.0084(11) N1 0.0135(12) 0.0149(12) 0.0135(12) 0.0038(9) -0.0003(9) 0.0024(9) N2 0.0107(11) 0.0122(11) 0.0144(12) 0.0025(9) -0.0004(9) 0.0021(9) N3 0.0141(13) 0.0136(12) 0.0299(15) 0.0017(11) 0.0047(11) 0.0063(10) N4 0.0137(12) 0.0162(12) 0.0122(12) 0.0028(9) -0.0002(9) 0.0041(10) N5 0.0108(11) 0.0104(11) 0.0119(11) 0.0033(9) 0.0017(9) 0.0028(9) N6 0.0217(14) 0.0226(14) 0.0174(13) 0.0011(11) 0.0012(11) -0.0044(11) N7 0.0102(11) 0.0108(11) 0.0152(12) 0.0034(9) -0.0002(9) 0.0009(9) N8 0.0116(11) 0.0125(11) 0.0133(11) 0.0045(9) -0.0005(9) 0.0027(9) N9 0.0164(13) 0.0187(13) 0.0134(12) 0.0023(10) 0.0014(10) 0.0036(10) C1 0.0140(14) 0.0149(14) 0.0129(13) 0.0013(11) 0.0028(11) 0.0021(11) C2 0.0115(13) 0.0131(13) 0.0166(14) 0.0001(11) 0.0013(11) 0.0027(11) C3 0.0142(14) 0.0121(13) 0.0153(14) -0.0012(11) -0.0013(11) 0.0055(11) C4 0.0133(14) 0.0256(16) 0.0206(16) 0.0100(13) 0.0003(12) 0.0024(12) C5 0.0173(15) 0.0174(15) 0.0327(18) 0.0069(13) 0.0037(13) 0.0087(12) C6 0.0166(14) 0.0119(13) 0.0153(14) 0.0017(11) 0.0010(11) 0.0037(11) C7 0.0116(14) 0.0111(13) 0.0191(15) -0.0002(11) 0.0008(11) 0.0015(11) C8 0.0102(13) 0.0122(13) 0.0180(14) 0.0018(11) 0.0032(11) 0.0040(10) C9 0.0236(17) 0.0214(16) 0.0192(16) 0.0036(13) -0.0047(13) 0.0014(13) C10 0.0168(15) 0.0164(14) 0.0194(15) 0.0050(12) 0.0021(12) 0.0018(12) C11 0.0104(13) 0.0139(13) 0.0149(14) 0.0019(11) 0.0018(11) 0.0014(11) C12 0.0122(14) 0.0161(14) 0.0132(14) 0.0020(11) 0.0004(11) 0.0017(11) C13 0.0110(13) 0.0149(14) 0.0139(14) 0.0036(11) 0.0012(10) 0.0005(11) C14 0.0178(15) 0.0161(14) 0.0151(14) 0.0015(11) -0.0011(11) 0.0052(12) C15 0.0179(15) 0.0213(15) 0.0168(15) 0.0063(12) 0.0008(12) 0.0038(12) C16 0.0274(17) 0.0282(17) 0.0229(16) 0.0151(13) 0.0061(13) 0.0165(14) C17 0.0184(16) 0.0270(17) 0.0222(16) 0.0123(13) 0.0000(12) 0.0048(13) C18 0.0297(18) 0.0215(16) 0.0170(15) 0.0027(12) 0.0035(13) 0.0073(13) C19 0.038(2) 0.035(2) 0.0186(16) 0.0098(14) 0.0032(14) 0.0081(16) C20 0.051(2) 0.047(2) 0.0247(19) 0.0183(17) 0.0067(17) 0.0183(19) C21 0.055(3) 0.046(2) 0.043(2) 0.026(2) 0.007(2) 0.027(2) C22 0.055(3) 0.0253(18) 0.033(2) 0.0132(15) 0.0156(18) 0.0241(18) C23 0.042(2) 0.0231(17) 0.0181(16) 0.0058(13) -0.0011(14) 0.0097(15) B 0.0096(15) 0.0137(15) 0.0147(15) 0.0044(12) 0.0016(12) 0.0039(12) Cl1 0.0636(17) 0.0497(14) 0.0601(16) 0.0077(12) 0.0033(13) 0.0023(12) Cl2 0.080(3) 0.176(4) 0.081(2) -0.024(3) -0.022(2) 0.030(3) C24 0.087(8) 0.095(8) 0.127(10) -0.009(7) -0.010(7) 0.063(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag C16 2.365(3) . ? Ag C17 2.374(3) . ? Ag N7 2.393(2) . ? Ag N4 2.459(2) . ? Ag N1 2.472(2) . ? F1 C4 1.338(4) . ? F2 C4 1.331(3) . ? F3 C4 1.330(4) . ? F4 C5 1.320(4) . ? F5 C5 1.337(3) . ? F6 C5 1.333(3) . ? F7 C9 1.335(4) . ? F8 C9 1.330(4) . ? F9 C9 1.337(4) . ? F10 C10 1.335(3) . ? F11 C10 1.331(3) . ? F12 C10 1.328(3) . ? F13 C14 1.332(3) . ? F14 C14 1.341(3) . ? F15 C14 1.333(3) . ? F16 C15 1.337(3) . ? F17 C15 1.325(3) . ? F18 C15 1.338(3) . ? O1 N3 1.230(3) . ? O2 N3 1.225(3) . ? O3 N6 1.223(4) . ? O4 N6 1.220(4) . ? O5 N9 1.222(3) . ? O6 N9 1.218(3) . ? N1 C1 1.321(4) . ? N1 N2 1.361(3) . ? N2 C3 1.357(4) . ? N2 B 1.567(4) . ? N3 C2 1.441(4) . ? N4 C6 1.327(3) . ? N4 N5 1.351(3) . ? N5 C8 1.357(3) . ? N5 B 1.555(4) . ? N6 C7 1.461(4) . ? N7 C11 1.333(3) . ? N7 N8 1.351(3) . ? N8 C13 1.354(4) . ? N8 B 1.558(4) . ? N9 C12 1.462(4) . ? C1 C2 1.398(4) . ? C1 C4 1.500(4) . ? C2 C3 1.379(4) . ? C3 C5 1.511(4) . ? C6 C7 1.388(4) . ? C6 C9 1.498(4) . ? C7 C8 1.366(4) . ? C8 C10 1.507(4) . ? C11 C12 1.397(4) . ? C11 C14 1.490(4) . ? C12 C13 1.378(4) . ? C13 C15 1.506(4) . ? C16 C17 1.354(5) . ? C16 C23 1.506(5) . ? C16 H16 1.0000 . ? C17 C18 1.510(4) . ? C17 H17 1.0000 . ? C18 C19 1.533(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.549(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.509(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.528(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.541(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? B H1 1.04(3) . ? Cl1 C24 1.688(11) . ? Cl2 C24 1.751(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? 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 C16 Ag C17 33.22(11) . . ? C16 Ag N7 117.24(10) . . ? C17 Ag N7 147.21(10) . . ? C16 Ag N4 142.18(10) . . ? C17 Ag N4 113.54(10) . . ? N7 Ag N4 85.44(8) . . ? C16 Ag N1 138.17(10) . . ? C17 Ag N1 134.81(9) . . ? N7 Ag N1 74.47(8) . . ? N4 Ag N1 74.48(8) . . ? C1 N1 N2 107.1(2) . . ? C1 N1 Ag 132.55(19) . . ? N2 N1 Ag 118.76(16) . . ? C3 N2 N1 110.1(2) . . ? C3 N2 B 130.2(2) . . ? N1 N2 B 118.8(2) . . ? O2 N3 O1 125.2(3) . . ? O2 N3 C2 117.8(3) . . ? O1 N3 C2 117.0(3) . . ? C6 N4 N5 106.3(2) . . ? C6 N4 Ag 128.02(18) . . ? N5 N4 Ag 114.38(16) . . ? N4 N5 C8 110.3(2) . . ? N4 N5 B 120.6(2) . . ? C8 N5 B 128.9(2) . . ? O4 N6 O3 125.6(3) . . ? O4 N6 C7 117.5(3) . . ? O3 N6 C7 116.8(3) . . ? C11 N7 N8 107.0(2) . . ? C11 N7 Ag 131.49(19) . . ? N8 N7 Ag 120.10(17) . . ? N7 N8 C13 110.4(2) . . ? N7 N8 B 121.9(2) . . ? C13 N8 B 127.5(2) . . ? O6 N9 O5 125.2(3) . . ? O6 N9 C12 118.0(2) . . ? O5 N9 C12 116.8(2) . . ? N1 C1 C2 109.9(2) . . ? N1 C1 C4 119.8(3) . . ? C2 C1 C4 130.1(3) . . ? C3 C2 C1 105.9(2) . . ? C3 C2 N3 127.8(3) . . ? C1 C2 N3 126.2(3) . . ? N2 C3 C2 106.9(2) . . ? N2 C3 C5 123.9(3) . . ? C2 C3 C5 129.1(3) . . ? F3 C4 F2 107.5(2) . . ? F3 C4 F1 107.2(3) . . ? F2 C4 F1 107.1(3) . . ? F3 C4 C1 112.8(3) . . ? F2 C4 C1 111.3(2) . . ? F1 C4 C1 110.7(2) . . ? F4 C5 F6 107.9(3) . . ? F4 C5 F5 108.4(3) . . ? F6 C5 F5 106.1(2) . . ? F4 C5 C3 112.4(2) . . ? F6 C5 C3 111.7(2) . . ? F5 C5 C3 110.0(3) . . ? N4 C6 C7 110.5(2) . . ? N4 C6 C9 121.2(3) . . ? C7 C6 C9 128.2(3) . . ? C8 C7 C6 105.7(2) . . ? C8 C7 N6 129.1(3) . . ? C6 C7 N6 125.2(3) . . ? N5 C8 C7 107.2(2) . . ? N5 C8 C10 122.7(2) . . ? C7 C8 C10 130.0(3) . . ? F8 C9 F7 106.9(3) . . ? F8 C9 F9 107.5(3) . . ? F7 C9 F9 107.6(3) . . ? F8 C9 C6 113.0(3) . . ? F7 C9 C6 111.1(3) . . ? F9 C9 C6 110.5(3) . . ? F12 C10 F11 107.7(2) . . ? F12 C10 F10 107.8(2) . . ? F11 C10 F10 107.9(2) . . ? F12 C10 C8 111.0(2) . . ? F11 C10 C8 110.3(2) . . ? F10 C10 C8 111.9(2) . . ? N7 C11 C12 109.7(2) . . ? N7 C11 C14 120.9(2) . . ? C12 C11 C14 129.4(3) . . ? C13 C12 C11 105.8(2) . . ? C13 C12 N9 127.5(3) . . ? C11 C12 N9 126.5(3) . . ? N8 C13 C12 107.1(2) . . ? N8 C13 C15 125.3(3) . . ? C12 C13 C15 127.6(3) . . ? F13 C14 F15 108.5(2) . . ? F13 C14 F14 106.8(2) . . ? F15 C14 F14 107.4(2) . . ? F13 C14 C11 111.8(2) . . ? F15 C14 C11 111.2(2) . . ? F14 C14 C11 110.9(2) . . ? F17 C15 F16 107.3(2) . . ? F17 C15 F18 107.4(2) . . ? F16 C15 F18 107.4(2) . . ? F17 C15 C13 113.3(2) . . ? F16 C15 C13 111.8(2) . . ? F18 C15 C13 109.4(2) . . ? C17 C16 C23 123.4(3) . . ? C17 C16 Ag 73.76(18) . . ? C23 C16 Ag 116.6(2) . . ? C17 C16 H16 112.5 . . ? C23 C16 H16 112.5 . . ? Ag C16 H16 112.5 . . ? C16 C17 C18 123.9(3) . . ? C16 C17 Ag 73.03(18) . . ? C18 C17 Ag 115.9(2) . . ? C16 C17 H17 112.7 . . ? C18 C17 H17 112.7 . . ? Ag C17 H17 112.7 . . ? C17 C18 C19 112.4(3) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 115.4(3) . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C19 117.1(3) . . ? C21 C20 H20A 108.0 . . ? C19 C20 H20A 108.0 . . ? C21 C20 H20B 108.0 . . ? C19 C20 H20B 108.0 . . ? H20A C20 H20B 107.3 . . ? C20 C21 C22 116.3(3) . . ? C20 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? C20 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 114.6(3) . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C16 C23 C22 110.4(3) . . ? C16 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C16 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N5 B N8 111.7(2) . . ? N5 B N2 108.7(2) . . ? N8 B N2 108.5(2) . . ? N5 B H1 108.5(14) . . ? N8 B H1 108.5(14) . . ? N2 B H1 110.9(14) . . ? Cl1 C24 Cl2 114.3(8) . . ? Cl1 C24 H24A 108.7 . . ? Cl2 C24 H24A 108.7 . . ? Cl1 C24 H24B 108.7 . . ? Cl2 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.199 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 941721' ####################################################################### # # 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_rad4_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[HB(3,5-(CF3)2Pz)3]Ag(cyclooctene)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Ag B F18 N6' _chemical_formula_weight 839.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5488(4) _cell_length_b 16.9402(7) _cell_length_c 17.4895(7) _cell_angle_alpha 83.886(1) _cell_angle_beta 74.977(1) _cell_angle_gamma 81.857(1) _cell_volume 2980.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9538 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 34.08 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 100(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 'Bruker D8 Quest' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 58332 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 34.14 _reflns_number_total 24492 _reflns_number_gt 20048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.7656P] 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 24492 _refine_ls_number_parameters 891 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _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 0.797224(10) 0.098015(6) 0.272840(6) 0.01852(3) Uani 1 1 d . . . F1 F 0.78031(12) 0.06910(7) 0.08048(7) 0.0394(2) Uani 1 1 d . . . F2 F 0.88945(16) 0.12153(7) -0.03033(6) 0.0516(3) Uani 1 1 d . . . F3 F 0.99053(11) 0.06468(6) 0.05662(7) 0.0384(2) Uani 1 1 d . . . F4 F 0.90036(10) 0.42603(6) 0.01223(6) 0.0312(2) Uani 1 1 d . . . F5 F 0.95378(11) 0.42530(6) 0.12298(6) 0.0339(2) Uani 1 1 d . . . F6 F 0.74895(10) 0.44539(6) 0.11945(6) 0.0342(2) Uani 1 1 d . . . F7 F 1.12287(9) 0.05192(5) 0.36239(6) 0.02499(18) Uani 1 1 d . . . F8 F 1.05848(9) 0.09690(5) 0.47867(5) 0.02280(17) Uani 1 1 d . . . F9 F 0.92083(8) 0.04890(5) 0.42868(5) 0.02129(16) Uani 1 1 d . . . F10 F 1.01546(12) 0.41883(6) 0.26360(7) 0.0415(3) Uani 1 1 d . . . F11 F 1.05939(14) 0.40378(6) 0.37805(8) 0.0517(4) Uani 1 1 d . . . F12 F 0.85880(13) 0.43241(6) 0.36909(7) 0.0437(3) Uani 1 1 d . . . F13 F 0.46319(11) 0.08058(6) 0.32101(6) 0.0372(2) Uani 1 1 d . . . F14 F 0.31346(10) 0.14250(7) 0.41089(8) 0.0432(3) Uani 1 1 d . . . F15 F 0.49382(10) 0.08445(6) 0.43682(6) 0.0316(2) Uani 1 1 d . . . F16 F 0.60767(12) 0.44540(6) 0.35745(7) 0.0419(3) Uani 1 1 d . . . F17 F 0.40356(11) 0.44494(6) 0.35895(7) 0.0389(3) Uani 1 1 d . . . F18 F 0.54973(12) 0.44789(6) 0.24799(6) 0.0438(3) Uani 1 1 d . . . N1 N 0.83841(12) 0.19387(7) 0.16034(7) 0.0178(2) Uani 1 1 d . . . N2 N 0.83351(11) 0.27235(6) 0.17207(7) 0.01598(19) Uani 1 1 d . . . N3 N 0.91005(11) 0.18518(6) 0.32559(6) 0.01402(18) Uani 1 1 d . . . N4 N 0.89482(11) 0.26496(6) 0.30582(7) 0.01491(19) Uani 1 1 d . . . N5 N 0.63034(11) 0.20189(6) 0.31689(7) 0.01618(19) Uani 1 1 d . . . N6 N 0.65446(11) 0.27924(6) 0.30090(6) 0.01526(19) Uani 1 1 d . . . C1 C 0.86597(14) 0.18979(8) 0.08178(8) 0.0200(2) Uani 1 1 d . . . C2 C 0.87983(14) 0.26442(9) 0.04116(8) 0.0213(3) Uani 1 1 d . . . H2 H 0.8993 0.2772 -0.0146 0.026 Uiso 1 1 calc R . . C3 C 0.85880(13) 0.31533(8) 0.10045(8) 0.0180(2) Uani 1 1 d . . . C4 C 0.88143(18) 0.11119(10) 0.04731(9) 0.0291(3) Uani 1 1 d . . . C5 C 0.86472(15) 0.40360(9) 0.08958(9) 0.0224(3) Uani 1 1 d . . . C6 C 0.98578(12) 0.17428(7) 0.37684(7) 0.0139(2) Uani 1 1 d . . . C7 C 1.02296(13) 0.24575(8) 0.39132(8) 0.0180(2) Uani 1 1 d . . . H7 H 1.0768 0.2538 0.4251 0.022 Uiso 1 1 calc R . . C8 C 0.96337(14) 0.30184(8) 0.34518(8) 0.0184(2) Uani 1 1 d . . . C9 C 1.02167(13) 0.09289(7) 0.41184(8) 0.0163(2) Uani 1 1 d . . . C10 C 0.97265(19) 0.38957(9) 0.33864(11) 0.0306(4) Uani 1 1 d . . . C11 C 0.50284(13) 0.20356(8) 0.35473(8) 0.0179(2) Uani 1 1 d . . . C12 C 0.44112(14) 0.28142(9) 0.36399(8) 0.0195(2) Uani 1 1 d . . . H12 H 0.3514 0.2985 0.3887 0.023 Uiso 1 1 calc R . . C13 C 0.54033(14) 0.32769(8) 0.32902(8) 0.0177(2) Uani 1 1 d . . . C14 C 0.44362(14) 0.12769(9) 0.38109(9) 0.0239(3) Uani 1 1 d . . . C15 C 0.52694(16) 0.41683(9) 0.32274(9) 0.0265(3) Uani 1 1 d . . . C16 C 0.88368(16) -0.03225(8) 0.24040(9) 0.0239(3) Uani 1 1 d . . . H16 H 0.8958 -0.0403 0.1830 0.029 Uiso 1 1 calc R . . C17 C 0.75780(15) -0.03702(8) 0.28412(10) 0.0242(3) Uani 1 1 d . . . H17 H 0.6966 -0.0473 0.2521 0.029 Uiso 1 1 calc R . . C18 C 0.71948(16) -0.07045(9) 0.36934(10) 0.0271(3) Uani 1 1 d . . . H18A H 0.6273 -0.0486 0.3936 0.033 Uiso 1 1 calc R . . H18B H 0.7773 -0.0526 0.3990 0.033 Uiso 1 1 calc R . . C19 C 0.73049(16) -0.16245(9) 0.37766(11) 0.0297(3) Uani 1 1 d . . . H19A H 0.6809 -0.1792 0.4319 0.036 Uiso 1 1 calc R . . H19B H 0.6863 -0.1799 0.3399 0.036 Uiso 1 1 calc R . . C20 C 0.87023(16) -0.20666(9) 0.36329(10) 0.0279(3) Uani 1 1 d . . . H20A H 0.8642 -0.2627 0.3852 0.034 Uiso 1 1 calc R . . H20B H 0.9199 -0.1821 0.3936 0.034 Uiso 1 1 calc R . . C21 C 0.95050(16) -0.20724(9) 0.27593(10) 0.0270(3) Uani 1 1 d . . . H21A H 0.9950 -0.2621 0.2664 0.032 Uiso 1 1 calc R . . H21B H 0.8879 -0.1948 0.2416 0.032 Uiso 1 1 calc R . . C22 C 1.05503(16) -0.14929(9) 0.25002(10) 0.0273(3) Uani 1 1 d . . . H22A H 1.0917 -0.1501 0.1919 0.033 Uiso 1 1 calc R . . H22B H 1.1282 -0.1686 0.2756 0.033 Uiso 1 1 calc R . . C23 C 1.00431(15) -0.06227(8) 0.27009(10) 0.0250(3) Uani 1 1 d . . . H23A H 0.9828 -0.0591 0.3283 0.030 Uiso 1 1 calc R . . H23B H 1.0747 -0.0278 0.2457 0.030 Uiso 1 1 calc R . . B1 B 0.79427(15) 0.30235(8) 0.25697(9) 0.0155(2) Uani 1 1 d . . . H1B1 H 0.7891(16) 0.3665(10) 0.2548(10) 0.011(4) Uiso 1 1 d . . . Ag2 Ag 0.548396(10) 0.709352(6) 0.116131(5) 0.01637(2) Uani 1 1 d . . . F19 F 0.40530(13) 0.88809(6) 0.05927(6) 0.0420(3) Uani 1 1 d . . . F20 F 0.32854(18) 0.99772(8) 0.11338(7) 0.0725(5) Uani 1 1 d . . . F21 F 0.53621(16) 0.95899(10) 0.08492(8) 0.0668(4) Uani 1 1 d . . . F22 F 0.21491(9) 0.83685(6) 0.44262(6) 0.0297(2) Uani 1 1 d . . . F23 F 0.31467(10) 0.94197(5) 0.42727(5) 0.02736(19) Uani 1 1 d . . . F24 F 0.41932(10) 0.82577(6) 0.44371(6) 0.0309(2) Uani 1 1 d . . . F25 F 0.89030(9) 0.71430(6) 0.11720(5) 0.02703(19) Uani 1 1 d . . . F26 F 0.98987(9) 0.61262(7) 0.17215(6) 0.0365(2) Uani 1 1 d . . . F27 F 0.85421(9) 0.59583(5) 0.10363(5) 0.02523(18) Uani 1 1 d . . . F28 F 0.55190(12) 0.68196(6) 0.47476(5) 0.0342(2) Uani 1 1 d . . . F29 F 0.67908(11) 0.57024(7) 0.46488(6) 0.0371(2) Uani 1 1 d . . . F30 F 0.48062(10) 0.57646(5) 0.45215(5) 0.0288(2) Uani 1 1 d . . . F31 F 0.46361(11) 0.51647(6) 0.08891(6) 0.0350(2) Uani 1 1 d . . . F32 F 0.26037(12) 0.49263(6) 0.11750(6) 0.0378(2) Uani 1 1 d . . . F33 F 0.31609(11) 0.60434(6) 0.05621(6) 0.0345(2) Uani 1 1 d . . . F34 F 0.21970(11) 0.58550(7) 0.45083(6) 0.0354(2) Uani 1 1 d . . . F35 F 0.04498(10) 0.58874(7) 0.40793(6) 0.0358(2) Uani 1 1 d . . . F36 F 0.12153(9) 0.69800(6) 0.41571(6) 0.0302(2) Uani 1 1 d . . . N7 N 0.42569(12) 0.81287(7) 0.20269(6) 0.0175(2) Uani 1 1 d . . . N8 N 0.40245(11) 0.79441(6) 0.28216(6) 0.01503(19) Uani 1 1 d . . . N9 N 0.64564(11) 0.68072(7) 0.22454(6) 0.01494(19) Uani 1 1 d . . . N10 N 0.56712(11) 0.67343(6) 0.29915(6) 0.01407(18) Uani 1 1 d . . . N11 N 0.39107(11) 0.63443(7) 0.20321(6) 0.01597(19) Uani 1 1 d . . . N12 N 0.34410(11) 0.65358(6) 0.27940(6) 0.01498(19) Uani 1 1 d . . . C24 C 0.40272(14) 0.89229(8) 0.19341(8) 0.0193(2) Uani 1 1 d . . . C25 C 0.36540(14) 0.92723(8) 0.26566(8) 0.0195(2) Uani 1 1 d . . . H25 H 0.3442 0.9824 0.2748 0.023 Uiso 1 1 calc R . . C26 C 0.36655(12) 0.86294(7) 0.32067(8) 0.0159(2) Uani 1 1 d . . . C27 C 0.41786(19) 0.93418(9) 0.11269(9) 0.0303(3) Uani 1 1 d . . . C28 C 0.32941(14) 0.86612(8) 0.40888(8) 0.0193(2) Uani 1 1 d . . . C29 C 0.76552(13) 0.64577(8) 0.22895(8) 0.0157(2) Uani 1 1 d . . . C30 C 0.76756(14) 0.61516(8) 0.30571(8) 0.0181(2) Uani 1 1 d . . . H30 H 0.8402 0.5878 0.3242 0.022 Uiso 1 1 calc R . . C31 C 0.63982(13) 0.63385(7) 0.34831(7) 0.0161(2) Uani 1 1 d . . . C32 C 0.87479(13) 0.64199(9) 0.15577(8) 0.0206(2) Uani 1 1 d . . . C33 C 0.58637(16) 0.61564(8) 0.43516(8) 0.0221(3) Uani 1 1 d . . . C34 C 0.31244(13) 0.58370(8) 0.19204(8) 0.0172(2) Uani 1 1 d . . . C35 C 0.21347(13) 0.56926(8) 0.25958(8) 0.0192(2) Uani 1 1 d . . . H35 H 0.1457 0.5357 0.2667 0.023 Uiso 1 1 calc R . . C36 C 0.23655(13) 0.61501(8) 0.31389(8) 0.0169(2) Uani 1 1 d . . . C37 C 0.33864(16) 0.54905(9) 0.11375(9) 0.0244(3) Uani 1 1 d . . . C38 C 0.15710(14) 0.62197(9) 0.39762(9) 0.0227(3) Uani 1 1 d . . . C39 C 0.58670(14) 0.69242(9) -0.01860(8) 0.0208(3) Uani 1 1 d . . . H39 H 0.6029 0.6348 -0.0303 0.025 Uiso 1 1 calc R . . C40 C 0.69649(14) 0.72011(9) -0.00947(8) 0.0201(2) Uani 1 1 d . . . H40 H 0.7745 0.6781 -0.0156 0.024 Uiso 1 1 calc R . . C41 C 0.73495(15) 0.80284(9) -0.03619(8) 0.0234(3) Uani 1 1 d . . . H41A H 0.7914 0.8163 -0.0034 0.028 Uiso 1 1 calc R . . H41B H 0.6542 0.8419 -0.0275 0.028 Uiso 1 1 calc R . . C42 C 0.80967(15) 0.81027(11) -0.12416(9) 0.0279(3) Uani 1 1 d . . . H42A H 0.8507 0.8607 -0.1345 0.033 Uiso 1 1 calc R . . H42B H 0.8821 0.7657 -0.1338 0.033 Uiso 1 1 calc R . . C43 C 0.72667(16) 0.80961(11) -0.18434(9) 0.0314(3) Uani 1 1 d . . . H43A H 0.6481 0.8498 -0.1706 0.038 Uiso 1 1 calc R . . H43B H 0.7796 0.8269 -0.2375 0.038 Uiso 1 1 calc R . . C44 C 0.67928(18) 0.72971(12) -0.19007(9) 0.0339(4) Uani 1 1 d . . . H44A H 0.7343 0.6866 -0.1665 0.041 Uiso 1 1 calc R . . H44B H 0.6946 0.7206 -0.2469 0.041 Uiso 1 1 calc R . . C45 C 0.53374(18) 0.72243(12) -0.14947(9) 0.0338(4) Uani 1 1 d . . . H45A H 0.5158 0.6675 -0.1538 0.041 Uiso 1 1 calc R . . H45B H 0.4782 0.7597 -0.1785 0.041 Uiso 1 1 calc R . . C46 C 0.49168(15) 0.74030(10) -0.06103(9) 0.0256(3) Uani 1 1 d . . . H46A H 0.4914 0.7980 -0.0562 0.031 Uiso 1 1 calc R . . H46B H 0.4012 0.7262 -0.0369 0.031 Uiso 1 1 calc R . . B2 B 0.41791(14) 0.70625(8) 0.31720(8) 0.0147(2) Uani 1 1 d . . . H2B2 H 0.3809(16) 0.7051(10) 0.3778(10) 0.011(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02053(5) 0.01182(4) 0.02236(5) -0.00157(3) -0.00362(4) -0.00205(3) F1 0.0464(6) 0.0344(5) 0.0425(6) -0.0092(5) -0.0110(5) -0.0175(5) F2 0.0982(11) 0.0419(6) 0.0192(5) -0.0087(4) -0.0177(6) -0.0128(7) F3 0.0421(6) 0.0301(5) 0.0411(6) -0.0163(5) -0.0061(5) 0.0045(4) F4 0.0362(5) 0.0311(5) 0.0225(4) 0.0112(4) -0.0031(4) -0.0086(4) F5 0.0429(6) 0.0255(5) 0.0395(6) 0.0076(4) -0.0201(5) -0.0142(4) F6 0.0320(5) 0.0226(4) 0.0380(5) 0.0076(4) 0.0016(4) 0.0033(4) F7 0.0213(4) 0.0203(4) 0.0296(4) -0.0053(3) -0.0030(3) 0.0066(3) F8 0.0302(4) 0.0200(4) 0.0205(4) 0.0033(3) -0.0134(3) -0.0012(3) F9 0.0236(4) 0.0147(3) 0.0251(4) 0.0034(3) -0.0053(3) -0.0058(3) F10 0.0630(8) 0.0279(5) 0.0434(6) 0.0170(4) -0.0269(6) -0.0275(5) F11 0.0856(9) 0.0227(5) 0.0728(9) 0.0099(5) -0.0628(8) -0.0225(5) F12 0.0708(8) 0.0156(4) 0.0511(7) -0.0089(4) -0.0297(6) 0.0058(5) F13 0.0453(6) 0.0357(5) 0.0356(5) -0.0133(4) -0.0066(5) -0.0199(5) F14 0.0162(4) 0.0428(6) 0.0663(8) -0.0057(6) 0.0017(5) -0.0101(4) F15 0.0364(5) 0.0271(5) 0.0314(5) 0.0036(4) -0.0067(4) -0.0109(4) F16 0.0514(7) 0.0217(5) 0.0531(7) -0.0167(5) -0.0090(6) -0.0031(4) F17 0.0380(6) 0.0270(5) 0.0377(6) -0.0029(4) 0.0058(4) 0.0147(4) F18 0.0563(7) 0.0299(5) 0.0273(5) 0.0102(4) 0.0056(5) 0.0155(5) N1 0.0215(5) 0.0157(5) 0.0165(5) -0.0019(4) -0.0049(4) -0.0022(4) N2 0.0179(5) 0.0143(4) 0.0155(5) 0.0007(4) -0.0042(4) -0.0021(4) N3 0.0154(5) 0.0111(4) 0.0150(4) 0.0002(3) -0.0036(4) -0.0008(3) N4 0.0184(5) 0.0109(4) 0.0166(5) 0.0010(4) -0.0065(4) -0.0030(4) N5 0.0159(5) 0.0144(5) 0.0187(5) -0.0019(4) -0.0045(4) -0.0024(4) N6 0.0174(5) 0.0132(4) 0.0153(5) -0.0022(4) -0.0050(4) 0.0004(4) C1 0.0221(6) 0.0224(6) 0.0157(5) -0.0027(5) -0.0043(5) -0.0032(5) C2 0.0204(6) 0.0276(7) 0.0147(5) 0.0012(5) -0.0029(5) -0.0039(5) C3 0.0158(5) 0.0204(6) 0.0166(5) 0.0035(4) -0.0034(4) -0.0028(4) C4 0.0397(9) 0.0305(8) 0.0187(6) -0.0062(6) -0.0072(6) -0.0065(6) C5 0.0227(6) 0.0216(6) 0.0211(6) 0.0072(5) -0.0045(5) -0.0048(5) C6 0.0144(5) 0.0125(5) 0.0137(5) 0.0002(4) -0.0025(4) -0.0012(4) C7 0.0202(6) 0.0162(5) 0.0195(6) 0.0010(4) -0.0087(5) -0.0036(4) C8 0.0243(6) 0.0130(5) 0.0207(6) 0.0016(4) -0.0103(5) -0.0049(4) C9 0.0171(5) 0.0141(5) 0.0170(5) 0.0002(4) -0.0043(4) -0.0001(4) C10 0.0498(10) 0.0156(6) 0.0369(8) 0.0043(6) -0.0285(8) -0.0101(6) C11 0.0163(6) 0.0217(6) 0.0170(6) -0.0040(5) -0.0050(4) -0.0027(4) C12 0.0174(6) 0.0261(6) 0.0152(5) -0.0060(5) -0.0052(4) 0.0025(5) C13 0.0219(6) 0.0175(5) 0.0130(5) -0.0038(4) -0.0052(4) 0.0039(4) C14 0.0183(6) 0.0268(7) 0.0269(7) -0.0063(6) -0.0024(5) -0.0061(5) C15 0.0318(8) 0.0196(6) 0.0214(6) -0.0023(5) 0.0004(6) 0.0074(5) C16 0.0317(7) 0.0144(5) 0.0253(7) -0.0046(5) -0.0058(6) -0.0016(5) C17 0.0278(7) 0.0138(5) 0.0338(8) -0.0046(5) -0.0111(6) -0.0031(5) C18 0.0256(7) 0.0164(6) 0.0358(8) -0.0020(6) -0.0004(6) -0.0038(5) C19 0.0295(8) 0.0176(6) 0.0393(9) 0.0018(6) -0.0029(7) -0.0070(5) C20 0.0317(8) 0.0160(6) 0.0368(8) -0.0010(6) -0.0097(7) -0.0036(5) C21 0.0311(8) 0.0169(6) 0.0356(8) -0.0085(6) -0.0121(6) 0.0004(5) C22 0.0256(7) 0.0203(6) 0.0348(8) -0.0091(6) -0.0044(6) 0.0012(5) C23 0.0247(7) 0.0175(6) 0.0326(8) -0.0069(5) -0.0041(6) -0.0034(5) B1 0.0191(6) 0.0120(5) 0.0158(6) 0.0001(5) -0.0057(5) -0.0011(5) Ag2 0.01813(5) 0.02060(5) 0.00993(4) -0.00061(3) -0.00311(3) -0.00188(3) F19 0.0711(8) 0.0318(5) 0.0215(5) 0.0021(4) -0.0137(5) 0.0002(5) F20 0.1155(13) 0.0401(7) 0.0315(6) 0.0086(5) 0.0021(7) 0.0457(8) F21 0.0785(10) 0.0835(11) 0.0373(7) 0.0232(7) -0.0025(7) -0.0494(9) F22 0.0274(5) 0.0353(5) 0.0227(4) -0.0087(4) 0.0070(4) -0.0108(4) F23 0.0371(5) 0.0190(4) 0.0248(4) -0.0109(3) -0.0032(4) -0.0009(4) F24 0.0376(5) 0.0325(5) 0.0253(4) -0.0104(4) -0.0155(4) 0.0079(4) F25 0.0274(5) 0.0293(5) 0.0211(4) 0.0017(3) 0.0016(3) -0.0095(4) F26 0.0157(4) 0.0631(7) 0.0274(5) -0.0016(5) -0.0073(4) 0.0085(4) F27 0.0284(4) 0.0260(4) 0.0197(4) -0.0074(3) -0.0044(3) 0.0034(3) F28 0.0617(7) 0.0260(5) 0.0160(4) -0.0064(3) -0.0108(4) -0.0030(4) F29 0.0438(6) 0.0442(6) 0.0199(4) 0.0096(4) -0.0134(4) 0.0072(5) F30 0.0377(5) 0.0239(4) 0.0190(4) 0.0056(3) 0.0019(4) -0.0065(4) F31 0.0380(6) 0.0405(6) 0.0266(5) -0.0157(4) -0.0069(4) 0.0023(4) F32 0.0545(7) 0.0332(5) 0.0339(5) -0.0072(4) -0.0138(5) -0.0240(5) F33 0.0537(7) 0.0342(5) 0.0236(5) 0.0032(4) -0.0219(5) -0.0126(5) F34 0.0378(6) 0.0426(6) 0.0198(4) 0.0081(4) -0.0019(4) -0.0022(4) F35 0.0269(5) 0.0409(6) 0.0360(5) -0.0043(4) 0.0067(4) -0.0180(4) F36 0.0263(5) 0.0270(4) 0.0319(5) -0.0094(4) 0.0050(4) -0.0024(4) N7 0.0221(5) 0.0147(5) 0.0131(5) -0.0003(4) -0.0007(4) -0.0007(4) N8 0.0170(5) 0.0137(4) 0.0128(4) -0.0020(4) -0.0007(4) -0.0010(4) N9 0.0162(5) 0.0178(5) 0.0108(4) 0.0000(4) -0.0034(4) -0.0026(4) N10 0.0175(5) 0.0143(4) 0.0100(4) 0.0005(3) -0.0032(4) -0.0019(4) N11 0.0188(5) 0.0156(5) 0.0138(5) -0.0017(4) -0.0039(4) -0.0027(4) N12 0.0158(5) 0.0143(4) 0.0139(4) -0.0007(4) -0.0017(4) -0.0026(4) C24 0.0232(6) 0.0138(5) 0.0178(6) 0.0004(4) -0.0007(5) -0.0010(4) C25 0.0211(6) 0.0133(5) 0.0218(6) -0.0027(4) -0.0008(5) -0.0017(4) C26 0.0147(5) 0.0152(5) 0.0168(5) -0.0045(4) -0.0008(4) -0.0016(4) C27 0.0445(9) 0.0174(6) 0.0215(7) 0.0029(5) -0.0001(6) 0.0027(6) C28 0.0201(6) 0.0183(6) 0.0186(6) -0.0064(5) -0.0021(5) -0.0010(5) C29 0.0155(5) 0.0166(5) 0.0150(5) 0.0000(4) -0.0046(4) -0.0013(4) C30 0.0212(6) 0.0173(5) 0.0171(5) 0.0017(4) -0.0087(5) -0.0009(4) C31 0.0234(6) 0.0134(5) 0.0121(5) 0.0007(4) -0.0060(4) -0.0026(4) C32 0.0163(6) 0.0265(6) 0.0183(6) -0.0014(5) -0.0055(5) 0.0015(5) C33 0.0342(8) 0.0187(6) 0.0130(5) 0.0008(4) -0.0074(5) 0.0003(5) C34 0.0203(6) 0.0152(5) 0.0181(6) 0.0001(4) -0.0083(5) -0.0030(4) C35 0.0189(6) 0.0161(5) 0.0240(6) 0.0019(5) -0.0078(5) -0.0046(4) C36 0.0167(5) 0.0147(5) 0.0180(6) 0.0022(4) -0.0030(4) -0.0028(4) C37 0.0337(8) 0.0216(6) 0.0221(6) -0.0023(5) -0.0116(6) -0.0083(6) C38 0.0210(6) 0.0221(6) 0.0224(6) 0.0004(5) 0.0001(5) -0.0052(5) C39 0.0253(7) 0.0250(6) 0.0116(5) -0.0026(5) -0.0041(5) -0.0012(5) C40 0.0193(6) 0.0280(7) 0.0110(5) -0.0014(5) -0.0030(4) 0.0020(5) C41 0.0225(6) 0.0315(7) 0.0171(6) -0.0002(5) -0.0053(5) -0.0064(5) C42 0.0217(7) 0.0397(9) 0.0203(6) 0.0037(6) -0.0032(5) -0.0055(6) C43 0.0263(7) 0.0480(10) 0.0166(6) 0.0069(6) -0.0039(5) -0.0037(7) C44 0.0360(9) 0.0522(11) 0.0140(6) -0.0037(6) -0.0081(6) -0.0023(8) C45 0.0342(9) 0.0538(11) 0.0179(7) -0.0010(7) -0.0123(6) -0.0110(8) C46 0.0207(6) 0.0400(8) 0.0174(6) 0.0008(6) -0.0073(5) -0.0051(6) B2 0.0173(6) 0.0137(5) 0.0120(5) -0.0015(4) -0.0019(5) -0.0016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C16 2.3349(14) . ? Ag1 N5 2.3446(11) . ? Ag1 C17 2.3612(14) . ? Ag1 N1 2.4027(11) . ? Ag1 N3 2.4095(11) . ? F1 C4 1.338(2) . ? F2 C4 1.3325(19) . ? F3 C4 1.336(2) . ? F4 C5 1.3353(17) . ? F5 C5 1.3369(18) . ? F6 C5 1.3299(18) . ? F7 C9 1.3448(15) . ? F8 C9 1.3346(15) . ? F9 C9 1.3376(15) . ? F10 C10 1.338(2) . ? F11 C10 1.3396(18) . ? F12 C10 1.325(2) . ? F13 C14 1.3429(18) . ? F14 C14 1.3338(17) . ? F15 C14 1.3314(19) . ? F16 C15 1.332(2) . ? F17 C15 1.3353(18) . ? F18 C15 1.3305(18) . ? N1 C1 1.3360(17) . ? N1 N2 1.3584(15) . ? N2 C3 1.3630(16) . ? N2 B1 1.5547(18) . ? N3 C6 1.3304(16) . ? N3 N4 1.3563(14) . ? N4 C8 1.3656(17) . ? N4 B1 1.5558(18) . ? N5 C11 1.3340(17) . ? N5 N6 1.3562(15) . ? N6 C13 1.3652(16) . ? N6 B1 1.5591(19) . ? C1 C2 1.390(2) . ? C1 C4 1.490(2) . ? C2 C3 1.373(2) . ? C2 H2 0.9500 . ? C3 C5 1.495(2) . ? C6 C7 1.3911(18) . ? C6 C9 1.4870(17) . ? C7 C8 1.3710(18) . ? C7 H7 0.9500 . ? C8 C10 1.4936(19) . ? C11 C12 1.3919(19) . ? C11 C14 1.485(2) . ? C12 C13 1.372(2) . ? C12 H12 0.9500 . ? C13 C15 1.491(2) . ? C16 C17 1.358(2) . ? C16 C23 1.500(2) . ? C16 H16 1.0000 . ? C17 C18 1.509(2) . ? C17 H17 1.0000 . ? C18 C19 1.540(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.527(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.543(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.529(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.540(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? B1 H1B1 1.077(16) . ? Ag2 C39 2.3271(13) . ? Ag2 C40 2.3486(13) . ? Ag2 N9 2.3567(11) . ? Ag2 N11 2.3578(11) . ? Ag2 N7 2.4391(11) . ? F19 C27 1.322(2) . ? F20 C27 1.3252(19) . ? F21 C27 1.327(2) . ? F22 C28 1.3382(16) . ? F23 C28 1.3357(15) . ? F24 C28 1.3285(17) . ? F25 C32 1.3439(17) . ? F26 C32 1.3350(16) . ? F27 C32 1.3389(17) . ? F28 C33 1.3393(16) . ? F29 C33 1.3354(17) . ? F30 C33 1.3300(18) . ? F31 C37 1.3338(19) . ? F32 C37 1.3349(17) . ? F33 C37 1.3441(18) . ? F34 C38 1.3284(18) . ? F35 C38 1.3434(17) . ? F36 C38 1.3372(17) . ? N7 C24 1.3330(16) . ? N7 N8 1.3572(15) . ? N8 C26 1.3618(16) . ? N8 B2 1.5557(17) . ? N9 C29 1.3357(16) . ? N9 N10 1.3558(14) . ? N10 C31 1.3603(16) . ? N10 B2 1.5550(18) . ? N11 C34 1.3365(17) . ? N11 N12 1.3530(15) . ? N12 C36 1.3597(16) . ? N12 B2 1.5585(18) . ? C24 C25 1.3918(19) . ? C24 C27 1.491(2) . ? C25 C26 1.3753(19) . ? C25 H25 0.9500 . ? C26 C28 1.4949(19) . ? C29 C30 1.3911(18) . ? C29 C32 1.4842(19) . ? C30 C31 1.3711(19) . ? C30 H30 0.9500 . ? C31 C33 1.4919(18) . ? C34 C35 1.3844(19) . ? C34 C37 1.492(2) . ? C35 C36 1.3756(19) . ? C35 H35 0.9500 . ? C36 C38 1.4945(19) . ? C39 C40 1.361(2) . ? C39 C46 1.497(2) . ? C39 H39 1.0000 . ? C40 C41 1.507(2) . ? C40 H40 1.0000 . ? C41 C42 1.537(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.536(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.529(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.532(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.545(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? B2 H2B2 1.030(16) . ? 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 C16 Ag1 N5 155.83(5) . . ? C16 Ag1 C17 33.62(5) . . ? N5 Ag1 C17 122.79(5) . . ? C16 Ag1 N1 112.66(5) . . ? N5 Ag1 N1 79.47(4) . . ? C17 Ag1 N1 131.67(5) . . ? C16 Ag1 N3 123.94(5) . . ? N5 Ag1 N3 77.18(4) . . ? C17 Ag1 N3 140.59(5) . . ? N1 Ag1 N3 81.94(4) . . ? C1 N1 N2 105.85(11) . . ? C1 N1 Ag1 134.60(9) . . ? N2 N1 Ag1 119.54(8) . . ? N1 N2 C3 109.30(11) . . ? N1 N2 B1 121.37(10) . . ? C3 N2 B1 129.20(11) . . ? C6 N3 N4 106.22(10) . . ? C6 N3 Ag1 134.12(8) . . ? N4 N3 Ag1 119.57(8) . . ? N3 N4 C8 108.80(10) . . ? N3 N4 B1 121.07(10) . . ? C8 N4 B1 129.39(11) . . ? C11 N5 N6 106.24(11) . . ? C11 N5 Ag1 133.20(9) . . ? N6 N5 Ag1 120.47(8) . . ? N5 N6 C13 108.96(11) . . ? N5 N6 B1 121.81(10) . . ? C13 N6 B1 129.23(11) . . ? N1 C1 C2 112.03(12) . . ? N1 C1 C4 120.39(13) . . ? C2 C1 C4 127.56(13) . . ? C3 C2 C1 103.76(12) . . ? C3 C2 H2 128.1 . . ? C1 C2 H2 128.1 . . ? N2 C3 C2 109.06(12) . . ? N2 C3 C5 124.66(12) . . ? C2 C3 C5 126.27(12) . . ? F2 C4 F3 107.23(14) . . ? F2 C4 F1 107.50(14) . . ? F3 C4 F1 106.30(14) . . ? F2 C4 C1 110.58(14) . . ? F3 C4 C1 112.37(13) . . ? F1 C4 C1 112.56(14) . . ? F6 C5 F4 107.26(12) . . ? F6 C5 F5 107.83(13) . . ? F4 C5 F5 107.24(12) . . ? F6 C5 C3 112.72(12) . . ? F4 C5 C3 109.55(13) . . ? F5 C5 C3 111.98(12) . . ? N3 C6 C7 112.14(11) . . ? N3 C6 C9 120.73(11) . . ? C7 C6 C9 127.13(12) . . ? C8 C7 C6 103.43(11) . . ? C8 C7 H7 128.3 . . ? C6 C7 H7 128.3 . . ? N4 C8 C7 109.41(11) . . ? N4 C8 C10 125.32(12) . . ? C7 C8 C10 125.27(12) . . ? F8 C9 F9 108.07(11) . . ? F8 C9 F7 107.09(10) . . ? F9 C9 F7 106.62(10) . . ? F8 C9 C6 110.83(11) . . ? F9 C9 C6 111.88(10) . . ? F7 C9 C6 112.10(11) . . ? F12 C10 F10 107.11(13) . . ? F12 C10 F11 107.22(14) . . ? F10 C10 F11 106.88(15) . . ? F12 C10 C8 113.26(14) . . ? F10 C10 C8 112.74(14) . . ? F11 C10 C8 109.29(12) . . ? N5 C11 C12 111.87(12) . . ? N5 C11 C14 120.11(12) . . ? C12 C11 C14 128.02(13) . . ? C13 C12 C11 103.67(12) . . ? C13 C12 H12 128.2 . . ? C11 C12 H12 128.2 . . ? N6 C13 C12 109.25(12) . . ? N6 C13 C15 124.98(13) . . ? C12 C13 C15 125.77(13) . . ? F15 C14 F14 107.41(13) . . ? F15 C14 F13 106.39(13) . . ? F14 C14 F13 107.52(13) . . ? F15 C14 C11 112.74(12) . . ? F14 C14 C11 110.56(13) . . ? F13 C14 C11 111.93(12) . . ? F18 C15 F16 107.67(14) . . ? F18 C15 F17 107.06(13) . . ? F16 C15 F17 107.22(13) . . ? F18 C15 C13 112.82(12) . . ? F16 C15 C13 112.55(13) . . ? F17 C15 C13 109.22(13) . . ? C17 C16 C23 124.11(14) . . ? C17 C16 Ag1 74.25(8) . . ? C23 C16 Ag1 113.00(9) . . ? C17 C16 H16 113.1 . . ? C23 C16 H16 113.1 . . ? Ag1 C16 H16 113.1 . . ? C16 C17 C18 125.18(14) . . ? C16 C17 Ag1 72.12(8) . . ? C18 C17 Ag1 112.53(10) . . ? C16 C17 H17 113.3 . . ? C18 C17 H17 113.3 . . ? Ag1 C17 H17 113.3 . . ? C17 C18 C19 112.93(13) . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 116.29(13) . . ? C20 C19 H19A 108.2 . . ? C18 C19 H19A 108.2 . . ? C20 C19 H19B 108.2 . . ? C18 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? C19 C20 C21 115.94(14) . . ? C19 C20 H20A 108.3 . . ? C21 C20 H20A 108.3 . . ? C19 C20 H20B 108.3 . . ? C21 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? C22 C21 C20 116.07(13) . . ? C22 C21 H21A 108.3 . . ? C20 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? C20 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 114.66(13) . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C16 C23 C22 111.26(13) . . ? C16 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C16 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N2 B1 N4 111.43(11) . . ? N2 B1 N6 109.24(11) . . ? N4 B1 N6 108.99(10) . . ? N2 B1 H1B1 111.1(9) . . ? N4 B1 H1B1 108.5(9) . . ? N6 B1 H1B1 107.5(9) . . ? C39 Ag2 C40 33.84(5) . . ? C39 Ag2 N9 142.44(4) . . ? C40 Ag2 N9 115.67(4) . . ? C39 Ag2 N11 116.58(5) . . ? C40 Ag2 N11 146.26(5) . . ? N9 Ag2 N11 79.79(4) . . ? C39 Ag2 N7 134.49(4) . . ? C40 Ag2 N7 130.29(4) . . ? N9 Ag2 N7 79.19(4) . . ? N11 Ag2 N7 80.33(4) . . ? C24 N7 N8 105.89(11) . . ? C24 N7 Ag2 134.19(9) . . ? N8 N7 Ag2 117.26(8) . . ? N7 N8 C26 109.36(10) . . ? N7 N8 B2 121.45(10) . . ? C26 N8 B2 129.19(11) . . ? C29 N9 N10 105.98(10) . . ? C29 N9 Ag2 131.26(9) . . ? N10 N9 Ag2 119.44(8) . . ? N9 N10 C31 109.15(10) . . ? N9 N10 B2 120.89(10) . . ? C31 N10 B2 129.95(11) . . ? C34 N11 N12 105.92(11) . . ? C34 N11 Ag2 133.39(9) . . ? N12 N11 Ag2 119.21(8) . . ? N11 N12 C36 109.25(11) . . ? N11 N12 B2 121.16(10) . . ? C36 N12 B2 129.38(11) . . ? N7 C24 C25 112.14(12) . . ? N7 C24 C27 120.83(12) . . ? C25 C24 C27 127.03(12) . . ? C26 C25 C24 103.54(11) . . ? C26 C25 H25 128.2 . . ? C24 C25 H25 128.2 . . ? N8 C26 C25 109.07(11) . . ? N8 C26 C28 124.65(12) . . ? C25 C26 C28 126.23(12) . . ? F19 C27 F20 107.37(16) . . ? F19 C27 F21 105.62(14) . . ? F20 C27 F21 107.47(16) . . ? F19 C27 C24 112.97(13) . . ? F20 C27 C24 111.06(13) . . ? F21 C27 C24 112.00(16) . . ? F24 C28 F23 107.30(11) . . ? F24 C28 F22 106.93(12) . . ? F23 C28 F22 107.22(11) . . ? F24 C28 C26 113.28(11) . . ? F23 C28 C26 109.67(11) . . ? F22 C28 C26 112.14(12) . . ? N9 C29 C30 111.95(11) . . ? N9 C29 C32 119.37(11) . . ? C30 C29 C32 128.65(12) . . ? C31 C30 C29 103.53(11) . . ? C31 C30 H30 128.2 . . ? C29 C30 H30 128.2 . . ? N10 C31 C30 109.39(11) . . ? N10 C31 C33 124.18(12) . . ? C30 C31 C33 126.43(12) . . ? F26 C32 F27 107.37(12) . . ? F26 C32 F25 107.25(12) . . ? F27 C32 F25 106.06(11) . . ? F26 C32 C29 111.34(11) . . ? F27 C32 C29 112.29(12) . . ? F25 C32 C29 112.20(11) . . ? F30 C33 F29 107.45(12) . . ? F30 C33 F28 106.94(12) . . ? F29 C33 F28 107.31(12) . . ? F30 C33 C31 113.37(12) . . ? F29 C33 C31 109.40(12) . . ? F28 C33 C31 112.09(11) . . ? N11 C34 C35 112.14(12) . . ? N11 C34 C37 119.97(12) . . ? C35 C34 C37 127.89(13) . . ? C36 C35 C34 103.52(12) . . ? C36 C35 H35 128.2 . . ? C34 C35 H35 128.2 . . ? N12 C36 C35 109.18(12) . . ? N12 C36 C38 124.80(12) . . ? C35 C36 C38 126.03(12) . . ? F31 C37 F32 107.91(13) . . ? F31 C37 F33 106.23(13) . . ? F32 C37 F33 106.91(12) . . ? F31 C37 C34 112.48(12) . . ? F32 C37 C34 110.80(13) . . ? F33 C37 C34 112.20(12) . . ? F34 C38 F36 107.20(13) . . ? F34 C38 F35 107.50(12) . . ? F36 C38 F35 106.79(12) . . ? F34 C38 C36 113.28(12) . . ? F36 C38 C36 112.49(12) . . ? F35 C38 C36 109.26(12) . . ? C40 C39 C46 123.34(14) . . ? C40 C39 Ag2 73.94(8) . . ? C46 C39 Ag2 116.45(10) . . ? C40 C39 H39 112.5 . . ? C46 C39 H39 112.5 . . ? Ag2 C39 H39 112.5 . . ? C39 C40 C41 125.35(13) . . ? C39 C40 Ag2 72.21(8) . . ? C41 C40 Ag2 114.70(9) . . ? C39 C40 H40 112.7 . . ? C41 C40 H40 112.7 . . ? Ag2 C40 H40 112.7 . . ? C40 C41 C42 112.48(13) . . ? C40 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? C40 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C43 C42 C41 115.95(13) . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? C41 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 116.23(14) . . ? C44 C43 H43A 108.2 . . ? C42 C43 H43A 108.2 . . ? C44 C43 H43B 108.2 . . ? C42 C43 H43B 108.2 . . ? H43A C43 H43B 107.4 . . ? C43 C44 C45 115.63(15) . . ? C43 C44 H44A 108.4 . . ? C45 C44 H44A 108.4 . . ? C43 C44 H44B 108.4 . . ? C45 C44 H44B 108.4 . . ? H44A C44 H44B 107.4 . . ? C44 C45 C46 114.71(13) . . ? C44 C45 H45A 108.6 . . ? C46 C45 H45A 108.6 . . ? C44 C45 H45B 108.6 . . ? C46 C45 H45B 108.6 . . ? H45A C45 H45B 107.6 . . ? C39 C46 C45 109.14(13) . . ? C39 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? C39 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? N10 B2 N8 109.27(10) . . ? N10 B2 N12 109.15(10) . . ? N8 B2 N12 110.27(10) . . ? N10 B2 H2B2 108.6(9) . . ? N8 B2 H2B2 108.6(9) . . ? N12 B2 H2B2 110.9(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 34.14 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.909 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.088 #===END _database_code_depnum_ccdc_archive 'CCDC 941722'