# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Catherine E.Housecroft' _publ_contact_author_name 'Catherine Housecroft' _publ_contact_author_email Catherine.Housecroft@unibas.ch _publ_section_title ; Same head, different scaffold: a plethora of structural motifs assembled from silver(I) and ditopic 2,2'-bipyridine ligands ; # Attachment '- GQ132.CIF' data_3t _database_code_depnum_ccdc_archive 'CCDC 774872' #TrackingRef '- GQ132.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H44 Ag2 N12, 2(C2 H3 N), 2(B F4)' _chemical_formula_sum 'C54 H50 Ag2 B2 F8 N14' _chemical_formula_weight 1284.44 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1952(9) _cell_length_b 13.7577(17) _cell_length_c 13.8979(15) _cell_angle_alpha 62.529(9) _cell_angle_beta 79.016(9) _cell_angle_gamma 80.401(10) _cell_volume 1359.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6905 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details '(Blessing, 1951)' _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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53061 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.50 _reflns_number_total 6823 _reflns_number_gt 6636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.6621P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6823 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.008 _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 0.672234(14) 0.600175(11) 0.572308(10) 0.02864(5) Uani 1 1 d . . . C4 C 0.8899(2) 0.57752(15) 0.78472(14) 0.0297(3) Uani 1 1 d . . . H4A H 0.8698 0.5281 0.7590 0.036 Uiso 1 1 calc R . . N2 N 0.97060(15) 0.65335(10) 0.55027(11) 0.0210(2) Uani 1 1 d . . . N3 N 0.81302(16) 0.59630(11) 0.42258(11) 0.0211(2) Uani 1 1 d . . . N4 N 0.49485(17) 0.49585(12) 0.27076(11) 0.0253(3) Uani 1 1 d . . . N5 N 0.44376(16) 0.27876(12) 0.34856(12) 0.0266(3) Uani 1 1 d . . . N6 N 0.3426(2) 0.15471(13) 0.56652(15) 0.0347(3) Uani 1 1 d . . . C3 C 0.8368(3) 0.55898(19) 0.89196(17) 0.0421(4) Uani 1 1 d . . . H3A H 0.7790 0.4964 0.9411 0.051 Uiso 1 1 calc R . . C2 C 0.8685(3) 0.6320(2) 0.92700(17) 0.0446(5) Uani 1 1 d . . . H2A H 0.8346 0.6203 1.0005 0.054 Uiso 1 1 calc R . . C1 C 0.9505(3) 0.7223(2) 0.85279(18) 0.0440(5) Uani 1 1 d . . . H1A H 0.9705 0.7732 0.8767 0.053 Uiso 1 1 calc R . . N1 N 1.0035(2) 0.74234(14) 0.74911(14) 0.0359(3) Uani 1 1 d . . . C5 C 0.97324(19) 0.67006(13) 0.71594(13) 0.0238(3) Uani 1 1 d . . . C6 C 1.04159(18) 0.69394(12) 0.60134(13) 0.0225(3) Uani 1 1 d . . . C7 C 1.1806(2) 0.75529(14) 0.55128(15) 0.0277(3) Uani 1 1 d . . . H7A H 1.2280 0.7834 0.5896 0.033 Uiso 1 1 calc R . . C8 C 1.2475(2) 0.77436(15) 0.44612(15) 0.0307(3) Uani 1 1 d . . . H8A H 1.3422 0.8150 0.4111 0.037 Uiso 1 1 calc R . . C9 C 1.17417(19) 0.73315(14) 0.39218(14) 0.0276(3) Uani 1 1 d . . . H9A H 1.2172 0.7453 0.3194 0.033 Uiso 1 1 calc R . . C10 C 1.03620(18) 0.67366(12) 0.44706(13) 0.0224(3) Uani 1 1 d . . . C11 C 0.95604(19) 0.63265(13) 0.38853(13) 0.0235(3) Uani 1 1 d . . . H11A H 1.0139 0.6334 0.3222 0.028 Uiso 1 1 calc R . . C12 C 0.74631(18) 0.56147(13) 0.35408(13) 0.0240(3) Uani 1 1 d . . . H12A H 0.7272 0.4826 0.3956 0.029 Uiso 1 1 calc R . . H12B H 0.8283 0.5709 0.2888 0.029 Uiso 1 1 calc R . . C13 C 0.5832(2) 0.62897(13) 0.31845(14) 0.0257(3) Uani 1 1 d . . . H13A H 0.4954 0.6084 0.3824 0.031 Uiso 1 1 calc R . . H13B H 0.5972 0.7080 0.2905 0.031 Uiso 1 1 calc R . . C14 C 0.5285(2) 0.61068(14) 0.23007(14) 0.0301(3) Uani 1 1 d . . . H14A H 0.4265 0.6596 0.2052 0.036 Uiso 1 1 calc R . . H14B H 0.6172 0.6298 0.1666 0.036 Uiso 1 1 calc R . . C15 C 0.5602(2) 0.44447(16) 0.21506(14) 0.0309(3) Uani 1 1 d . . . H15A H 0.6321 0.4808 0.1494 0.037 Uiso 1 1 calc R . . C16 C 0.5281(2) 0.33031(16) 0.24891(15) 0.0306(3) Uani 1 1 d . . . C17 C 0.5800(3) 0.28177(19) 0.17855(18) 0.0405(4) Uani 1 1 d . . . H17A H 0.6426 0.3198 0.1092 0.049 Uiso 1 1 calc R . . C18 C 0.5381(3) 0.1765(2) 0.2124(2) 0.0462(5) Uani 1 1 d . . . H18A H 0.5695 0.1415 0.1658 0.055 Uiso 1 1 calc R . . C19 C 0.4505(3) 0.12323(17) 0.31425(19) 0.0413(4) Uani 1 1 d . . . H19A H 0.4201 0.0511 0.3385 0.050 Uiso 1 1 calc R . . C20 C 0.4063(2) 0.17614(14) 0.38201(16) 0.0294(3) Uani 1 1 d . . . C21 C 0.3160(2) 0.12228(13) 0.49393(16) 0.0298(3) Uani 1 1 d . . . C22 C 0.2076(3) 0.04365(16) 0.52034(19) 0.0414(4) Uani 1 1 d . . . H22A H 0.1918 0.0217 0.4674 0.050 Uiso 1 1 calc R . . C23 C 0.1233(3) -0.00190(18) 0.6244(2) 0.0509(6) Uani 1 1 d . . . H23A H 0.0482 -0.0557 0.6442 0.061 Uiso 1 1 calc R . . C24 C 0.1483(3) 0.03081(18) 0.6995(2) 0.0466(5) Uani 1 1 d . . . H24A H 0.0907 0.0007 0.7717 0.056 Uiso 1 1 calc R . . C25 C 0.2597(3) 0.10882(17) 0.66740(19) 0.0414(4) Uani 1 1 d . . . H25A H 0.2783 0.1309 0.7196 0.050 Uiso 1 1 calc R . . B1 B 0.8710(11) 0.2494(9) -0.0703(7) 0.0381(15) Uani 0.704(13) 1 d P A 1 F10 F 0.8620(18) 0.1666(9) 0.0259(10) 0.051(2) Uani 0.704(13) 1 d P A 1 F11 F 1.036(2) 0.2873(11) -0.1005(11) 0.066(2) Uani 0.704(13) 1 d P A 1 F12 F 0.8452(7) 0.2158(3) -0.14556(19) 0.0548(10) Uani 0.704(13) 1 d P A 1 F13 F 0.7464(6) 0.3308(2) -0.0695(3) 0.0548(8) Uani 0.704(13) 1 d P A 1 B1' B 0.923(3) 0.2418(18) -0.0853(18) 0.040(4) Uani 0.296(13) 1 d P A 2 F10' F 0.877(4) 0.1597(16) 0.039(2) 0.036(2) Uani 0.296(13) 1 d P A 2 F11' F 1.040(5) 0.291(3) -0.092(3) 0.064(6) Uani 0.296(13) 1 d P A 2 F12' F 0.945(2) 0.1830(8) -0.1443(5) 0.066(4) Uani 0.296(13) 1 d P A 2 F13' F 0.8009(13) 0.3273(6) -0.1242(15) 0.078(5) Uani 0.296(13) 1 d P A 2 N100 N 0.6023(5) 0.0478(4) -0.1894(3) 0.1058(13) Uani 1 1 d . . . C100 C 0.6697(4) 0.0102(3) -0.1153(3) 0.0639(7) Uani 1 1 d . . . C101 C 0.7550(4) -0.0369(3) -0.0191(3) 0.0667(7) Uani 1 1 d . . . H10A H 0.7411 0.0153 0.0122 0.100 Uiso 1 1 calc R . . H10B H 0.8740 -0.0527 -0.0395 0.100 Uiso 1 1 calc R . . H10C H 0.7074 -0.1053 0.0352 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02445(7) 0.04003(8) 0.02728(8) -0.02000(6) 0.00519(5) -0.01226(5) C4 0.0327(8) 0.0322(8) 0.0274(8) -0.0133(6) -0.0041(6) -0.0103(6) N2 0.0174(5) 0.0233(6) 0.0233(6) -0.0102(5) -0.0041(4) -0.0036(4) N3 0.0195(5) 0.0247(6) 0.0225(6) -0.0127(5) -0.0035(4) -0.0030(4) N4 0.0221(6) 0.0323(7) 0.0234(6) -0.0112(5) -0.0036(5) -0.0100(5) N5 0.0193(6) 0.0312(7) 0.0341(7) -0.0181(6) -0.0048(5) -0.0024(5) N6 0.0322(7) 0.0294(7) 0.0449(9) -0.0172(6) -0.0074(6) -0.0044(6) C3 0.0506(11) 0.0464(11) 0.0287(9) -0.0135(8) 0.0007(8) -0.0191(9) C2 0.0526(12) 0.0585(13) 0.0293(9) -0.0234(9) -0.0015(8) -0.0146(10) C1 0.0569(12) 0.0523(12) 0.0358(10) -0.0277(9) -0.0022(9) -0.0178(10) N1 0.0446(9) 0.0388(8) 0.0328(8) -0.0206(7) -0.0026(6) -0.0148(7) C5 0.0217(6) 0.0263(7) 0.0260(7) -0.0122(6) -0.0080(5) -0.0017(5) C6 0.0188(6) 0.0227(6) 0.0268(7) -0.0103(6) -0.0069(5) -0.0018(5) C7 0.0216(7) 0.0305(7) 0.0360(8) -0.0167(7) -0.0061(6) -0.0065(6) C8 0.0206(7) 0.0351(8) 0.0372(9) -0.0151(7) 0.0001(6) -0.0117(6) C9 0.0200(7) 0.0345(8) 0.0272(7) -0.0125(6) 0.0008(6) -0.0077(6) C10 0.0171(6) 0.0257(7) 0.0250(7) -0.0110(6) -0.0033(5) -0.0038(5) C11 0.0199(6) 0.0307(7) 0.0217(7) -0.0126(6) -0.0015(5) -0.0048(5) C12 0.0203(6) 0.0314(7) 0.0264(7) -0.0175(6) -0.0035(5) -0.0036(5) C13 0.0236(7) 0.0259(7) 0.0296(7) -0.0120(6) -0.0073(6) -0.0041(5) C14 0.0323(8) 0.0320(8) 0.0250(7) -0.0070(6) -0.0086(6) -0.0118(6) C15 0.0263(7) 0.0445(9) 0.0247(7) -0.0166(7) 0.0023(6) -0.0129(7) C16 0.0229(7) 0.0418(9) 0.0335(8) -0.0222(7) -0.0033(6) -0.0029(6) C17 0.0365(9) 0.0533(12) 0.0400(10) -0.0299(9) -0.0042(8) 0.0020(8) C18 0.0509(12) 0.0520(12) 0.0527(12) -0.0394(11) -0.0137(10) 0.0089(10) C19 0.0460(11) 0.0353(9) 0.0549(12) -0.0290(9) -0.0195(9) 0.0070(8) C20 0.0235(7) 0.0289(7) 0.0418(9) -0.0191(7) -0.0126(6) 0.0026(6) C21 0.0240(7) 0.0233(7) 0.0433(9) -0.0132(7) -0.0131(7) 0.0006(6) C22 0.0423(10) 0.0312(9) 0.0527(12) -0.0142(8) -0.0155(9) -0.0117(8) C23 0.0442(11) 0.0349(10) 0.0634(14) -0.0072(10) -0.0106(10) -0.0183(9) C24 0.0412(10) 0.0354(10) 0.0481(12) -0.0060(9) -0.0037(9) -0.0049(8) C25 0.0423(10) 0.0348(9) 0.0462(11) -0.0168(8) -0.0072(8) -0.0027(8) B1 0.048(4) 0.044(3) 0.027(2) -0.0170(18) -0.009(3) -0.010(3) F10 0.059(3) 0.063(4) 0.031(4) -0.018(3) -0.013(2) -0.005(2) F11 0.076(4) 0.071(6) 0.042(3) -0.012(3) -0.002(2) -0.027(4) F12 0.086(3) 0.0543(15) 0.0353(10) -0.0241(10) -0.0161(12) -0.0124(16) F13 0.0656(17) 0.0515(12) 0.0509(16) -0.0253(11) -0.0155(13) 0.0024(11) B1' 0.052(11) 0.030(5) 0.034(8) -0.008(5) -0.014(7) -0.001(7) F10' 0.056(6) 0.034(4) 0.014(3) -0.002(2) -0.015(3) -0.011(3) F11' 0.095(13) 0.060(10) 0.054(9) -0.034(8) -0.005(7) -0.031(8) F12' 0.120(10) 0.053(4) 0.034(3) -0.020(2) -0.009(4) -0.027(5) F13' 0.054(4) 0.043(3) 0.118(11) -0.007(4) -0.047(6) -0.001(3) N100 0.105(3) 0.133(3) 0.0687(19) -0.015(2) -0.0215(18) -0.062(2) C100 0.0546(14) 0.0726(18) 0.0594(16) -0.0220(14) 0.0016(12) -0.0255(13) C101 0.0627(16) 0.0616(16) 0.0686(18) -0.0233(14) -0.0119(14) -0.0001(13) _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 2.1980(13) . ? Ag1 N4 2.2768(14) 2_666 ? Ag1 N5 2.3772(15) 2_666 ? Ag1 N2 2.5908(13) . ? C4 C3 1.384(3) . ? C4 C5 1.385(2) . ? C4 H4A 0.9500 . ? N2 C6 1.3362(19) . ? N2 C10 1.346(2) . ? N3 C11 1.270(2) . ? N3 C12 1.4632(19) . ? N4 C15 1.267(2) . ? N4 C14 1.468(2) . ? N4 Ag1 2.2768(14) 2_666 ? N5 C20 1.337(2) . ? N5 C16 1.338(2) . ? N5 Ag1 2.3772(15) 2_666 ? N6 C25 1.338(3) . ? N6 C21 1.340(2) . ? C3 C2 1.379(3) . ? C3 H3A 0.9500 . ? C2 C1 1.374(3) . ? C2 H2A 0.9500 . ? C1 N1 1.333(3) . ? C1 H1A 0.9500 . ? N1 C5 1.346(2) . ? C5 C6 1.482(2) . ? C6 C7 1.404(2) . ? C7 C8 1.376(3) . ? C7 H7A 0.9500 . ? C8 C9 1.386(2) . ? C8 H8A 0.9500 . ? C9 C10 1.391(2) . ? C9 H9A 0.9500 . ? C10 C11 1.470(2) . ? C11 H11A 0.9500 . ? C12 C13 1.519(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.518(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.472(3) . ? C15 H15A 0.9500 . ? C16 C17 1.390(3) . ? C17 C18 1.382(3) . ? C17 H17A 0.9500 . ? C18 C19 1.374(4) . ? C18 H18A 0.9500 . ? C19 C20 1.401(3) . ? C19 H19A 0.9500 . ? C20 C21 1.482(3) . ? C21 C22 1.387(2) . ? C22 C23 1.375(4) . ? C22 H22A 0.9500 . ? C23 C24 1.370(4) . ? C23 H23A 0.9500 . ? C24 C25 1.383(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? B1 F10 1.295(15) . ? B1 F12 1.385(9) . ? B1 F13 1.387(8) . ? B1 F11 1.446(16) . ? B1' F11' 1.23(4) . ? B1' F12' 1.37(2) . ? B1' F13' 1.380(19) . ? B1' F10' 1.58(3) . ? N100 C100 1.124(4) . ? C100 C101 1.450(4) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 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 N3 Ag1 N4 144.08(5) . 2_666 ? N3 Ag1 N5 142.63(5) . 2_666 ? N4 Ag1 N5 72.22(5) 2_666 2_666 ? N3 Ag1 N2 71.50(4) . . ? N4 Ag1 N2 128.47(4) 2_666 . ? N5 Ag1 N2 91.64(4) 2_666 . ? C3 C4 C5 118.24(17) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? C6 N2 C10 117.72(13) . . ? C6 N2 Ag1 133.20(10) . . ? C10 N2 Ag1 105.21(9) . . ? C11 N3 C12 117.13(13) . . ? C11 N3 Ag1 119.12(11) . . ? C12 N3 Ag1 123.59(10) . . ? C15 N4 C14 118.97(15) . . ? C15 N4 Ag1 115.87(12) . 2_666 ? C14 N4 Ag1 125.15(11) . 2_666 ? C20 N5 C16 118.72(16) . . ? C20 N5 Ag1 127.10(12) . 2_666 ? C16 N5 Ag1 112.70(11) . 2_666 ? C25 N6 C21 117.71(17) . . ? C2 C3 C4 119.49(19) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C1 C2 C3 118.30(19) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? N1 C1 C2 123.67(19) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 N1 C5 117.59(17) . . ? N1 C5 C4 122.71(16) . . ? N1 C5 C6 115.18(14) . . ? C4 C5 C6 122.06(15) . . ? N2 C6 C7 122.30(15) . . ? N2 C6 C5 118.36(13) . . ? C7 C6 C5 119.32(14) . . ? C8 C7 C6 119.33(15) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C7 C8 C9 118.83(15) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C8 C9 C10 118.44(16) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? N2 C10 C9 123.37(14) . . ? N2 C10 C11 118.34(13) . . ? C9 C10 C11 118.27(14) . . ? N3 C11 C10 123.08(14) . . ? N3 C11 H11A 118.5 . . ? C10 C11 H11A 118.5 . . ? N3 C12 C13 110.40(13) . . ? N3 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N3 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 111.54(14) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N4 C14 C13 111.10(13) . . ? N4 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N4 C15 C16 122.06(16) . . ? N4 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? N5 C16 C17 123.03(18) . . ? N5 C16 C15 116.23(15) . . ? C17 C16 C15 120.72(18) . . ? C18 C17 C16 118.1(2) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? C19 C18 C17 119.28(19) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 119.45(19) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? N5 C20 C19 121.37(19) . . ? N5 C20 C21 116.36(15) . . ? C19 C20 C21 122.28(17) . . ? N6 C21 C22 122.35(19) . . ? N6 C21 C20 116.73(15) . . ? C22 C21 C20 120.91(18) . . ? C23 C22 C21 118.8(2) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C24 C23 C22 119.60(19) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 118.3(2) . . ? C23 C24 H24A 120.9 . . ? C25 C24 H24A 120.9 . . ? N6 C25 C24 123.3(2) . . ? N6 C25 H25A 118.4 . . ? C24 C25 H25A 118.4 . . ? F10 B1 F12 109.0(9) . . ? F10 B1 F13 108.8(8) . . ? F12 B1 F13 108.7(6) . . ? F10 B1 F11 109.5(10) . . ? F12 B1 F11 108.2(7) . . ? F13 B1 F11 112.5(9) . . ? F11' B1' F12' 118(2) . . ? F11' B1' F13' 101(2) . . ? F12' B1' F13' 109.3(17) . . ? F11' B1' F10' 108(2) . . ? F12' B1' F10' 107.6(17) . . ? F13' B1' F10' 112.6(17) . . ? N100 C100 C101 179.0(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.479 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.066 # Attachment '- GQ133.CIF' data_gq133 _database_code_depnum_ccdc_archive 'CCDC 774873' #TrackingRef '- GQ133.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 Ag2 N12, 2(B F4)' _chemical_formula_sum 'C48 H40 Ag2 B2 F8 N12' _chemical_formula_weight 1174.28 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7811(17) _cell_length_b 13.3183(19) _cell_length_c 15.009(2) _cell_angle_alpha 88.944(11) _cell_angle_beta 88.793(12) _cell_angle_gamma 66.108(11) _cell_volume 2335.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10480 _cell_measurement_theta_min 5.51 _cell_measurement_theta_max 62.07 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details '(Blessing 1951)' _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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51650 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 31.00 _reflns_number_total 14764 _reflns_number_gt 13138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+1.1916P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14764 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.021 _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 0.622582(11) 0.212386(10) 0.317614(8) 0.03218(4) Uani 1 1 d . . . Ag2 Ag 0.800469(11) -0.016319(10) 0.241279(8) 0.03312(4) Uani 1 1 d . . . N1A N 0.46211(15) 0.37016(14) 0.23643(13) 0.0450(4) Uani 1 1 d . . . N2A N 0.68414(13) 0.32837(12) 0.22911(10) 0.0325(3) Uani 1 1 d . . . N3A N 0.81370(13) 0.17935(12) 0.35082(11) 0.0342(3) Uani 1 1 d . . . N4A N 0.83101(12) -0.04961(11) 0.39024(9) 0.0298(3) Uani 1 1 d . . . N5A N 0.86207(12) -0.21955(11) 0.27072(9) 0.0284(2) Uani 1 1 d . . . N6A N 0.92361(16) -0.36540(14) 0.06543(12) 0.0432(4) Uani 1 1 d . . . C1A C 0.35354(19) 0.38258(19) 0.23828(18) 0.0527(5) Uani 1 1 d . . . H1AA H 0.3311 0.3411 0.2808 0.063 Uiso 1 1 calc R . . C2A C 0.2723(2) 0.45202(18) 0.18203(17) 0.0514(5) Uani 1 1 d . . . H2AA H 0.1953 0.4592 0.1854 0.062 Uiso 1 1 calc R . . C3A C 0.3060(3) 0.5107(2) 0.1208(2) 0.0674(7) Uani 1 1 d . . . H3AA H 0.2523 0.5589 0.0801 0.081 Uiso 1 1 calc R . . C4A C 0.4176(2) 0.4999(2) 0.11816(19) 0.0623(7) Uani 1 1 d . . . H4AA H 0.4416 0.5412 0.0765 0.075 Uiso 1 1 calc R . . C5A C 0.49411(17) 0.42794(14) 0.17706(12) 0.0368(4) Uani 1 1 d . . . C6A C 0.61651(18) 0.40999(15) 0.17766(12) 0.0378(4) Uani 1 1 d . . . C7A C 0.6593(2) 0.4754(2) 0.12828(16) 0.0563(6) Uani 1 1 d . . . H7AA H 0.6100 0.5342 0.0923 0.068 Uiso 1 1 calc R . . C8A C 0.7738(3) 0.4534(2) 0.13250(18) 0.0646(7) Uani 1 1 d . . . H8AA H 0.8047 0.4962 0.0986 0.077 Uiso 1 1 calc R . . C9A C 0.8435(2) 0.3690(2) 0.18615(16) 0.0516(5) Uani 1 1 d . . . H9AA H 0.9229 0.3523 0.1898 0.062 Uiso 1 1 calc R . . C10A C 0.79456(17) 0.30901(15) 0.23483(12) 0.0362(3) Uani 1 1 d . . . C11A C 0.86169(16) 0.22479(16) 0.29966(13) 0.0380(4) Uani 1 1 d . . . H11A H 0.9419 0.2043 0.3032 0.046 Uiso 1 1 calc R . . C12A C 0.87957(18) 0.10605(16) 0.42200(14) 0.0419(4) Uani 1 1 d . . . H12A H 0.8874 0.1502 0.4717 0.050 Uiso 1 1 calc R . . H12B H 0.9572 0.0596 0.3993 0.050 Uiso 1 1 calc R . . C13A C 0.82144(17) 0.03351(14) 0.45574(11) 0.0361(4) Uani 1 1 d . . . H13A H 0.8571 -0.0030 0.5121 0.043 Uiso 1 1 calc R . . H13B H 0.7396 0.0792 0.4683 0.043 Uiso 1 1 calc R . . C14A C 0.86612(15) -0.14813(14) 0.41744(11) 0.0322(3) Uani 1 1 d . . . H14A H 0.8802 -0.1630 0.4792 0.039 Uiso 1 1 calc R . . C15A C 0.88614(15) -0.24062(13) 0.35775(11) 0.0311(3) Uani 1 1 d . . . C16A C 0.9335(2) -0.34578(15) 0.39349(14) 0.0441(4) Uani 1 1 d . . . H16A H 0.9468 -0.3573 0.4556 0.053 Uiso 1 1 calc R . . C17A C 0.9611(2) -0.43362(16) 0.33675(16) 0.0523(5) Uani 1 1 d . . . H17A H 0.9937 -0.5068 0.3592 0.063 Uiso 1 1 calc R . . C18A C 0.94068(19) -0.41352(15) 0.24777(14) 0.0437(4) Uani 1 1 d . . . H18A H 0.9613 -0.4728 0.2074 0.052 Uiso 1 1 calc R . . C19A C 0.88926(15) -0.30504(13) 0.21636(11) 0.0316(3) Uani 1 1 d . . . C20A C 0.86295(15) -0.28323(14) 0.12016(11) 0.0322(3) Uani 1 1 d . . . C21A C 0.77775(16) -0.18682(16) 0.09051(12) 0.0361(3) Uani 1 1 d . . . H21A H 0.7367 -0.1301 0.1313 0.043 Uiso 1 1 calc R . . C22A C 0.75273(19) -0.17356(19) 0.00076(13) 0.0435(4) Uani 1 1 d . . . H22A H 0.6941 -0.1079 -0.0211 0.052 Uiso 1 1 calc R . . C23A C 0.8142(2) -0.25725(19) -0.05640(13) 0.0475(5) Uani 1 1 d . . . H23A H 0.7992 -0.2508 -0.1184 0.057 Uiso 1 1 calc R . . C24A C 0.8978(2) -0.35008(19) -0.02143(14) 0.0489(5) Uani 1 1 d . . . H24A H 0.9403 -0.4075 -0.0612 0.059 Uiso 1 1 calc R . . N1B N 1.01845(16) -0.07240(17) 0.21166(13) 0.0494(4) Uani 1 1 d . . . N2B N 0.84348(14) 0.08163(12) 0.12468(10) 0.0362(3) Uani 1 1 d . . . N3B N 0.63220(13) 0.08162(12) 0.15490(10) 0.0342(3) Uani 1 1 d . . . N4B N 0.51711(13) 0.11070(12) 0.33153(11) 0.0355(3) Uani 1 1 d . . . N5B N 0.52924(13) 0.24462(12) 0.46781(10) 0.0339(3) Uani 1 1 d . . . N6B N 0.6742(2) 0.3651(2) 0.59852(15) 0.0623(5) Uani 1 1 d . . . C1B C 1.1010(2) -0.1423(2) 0.26140(18) 0.0578(6) Uani 1 1 d . . . H1BA H 1.0863 -0.1970 0.2942 0.069 Uiso 1 1 calc R . . C2B C 1.2073(2) -0.1399(3) 0.2682(2) 0.0685(7) Uani 1 1 d . . . H2BA H 1.2646 -0.1919 0.3043 0.082 Uiso 1 1 calc R . . C3B C 1.2280(2) -0.0605(3) 0.2214(3) 0.0802(10) Uani 1 1 d . . . H3BA H 1.3006 -0.0569 0.2242 0.096 Uiso 1 1 calc R . . C4B C 1.1434(2) 0.0136(2) 0.1707(2) 0.0673(8) Uani 1 1 d . . . H4BA H 1.1556 0.0705 0.1392 0.081 Uiso 1 1 calc R . . C5B C 1.03987(18) 0.00468(17) 0.16560(15) 0.0429(4) Uani 1 1 d . . . C6B C 0.94728(19) 0.07720(17) 0.10715(13) 0.0415(4) Uani 1 1 d . . . C7B C 0.9674(2) 0.1369(2) 0.03541(16) 0.0543(6) Uani 1 1 d . . . H7BA H 1.0422 0.1330 0.0235 0.065 Uiso 1 1 calc R . . C8B C 0.8786(3) 0.2002(2) -0.01677(15) 0.0596(6) Uani 1 1 d . . . H8BA H 0.8911 0.2409 -0.0654 0.071 Uiso 1 1 calc R . . C9B C 0.7706(3) 0.20501(19) 0.00121(14) 0.0530(6) Uani 1 1 d . . . H9BA H 0.7075 0.2487 -0.0345 0.064 Uiso 1 1 calc R . . C10B C 0.75655(19) 0.14389(15) 0.07322(12) 0.0400(4) Uani 1 1 d . . . C11B C 0.64413(18) 0.14472(15) 0.09507(12) 0.0396(4) Uani 1 1 d . . . H11B H 0.5789 0.1934 0.0639 0.048 Uiso 1 1 calc R . . C12B C 0.51832(17) 0.08379(17) 0.16960(14) 0.0418(4) Uani 1 1 d . . . H12C H 0.5032 0.0388 0.1240 0.050 Uiso 1 1 calc R . . H12D H 0.4604 0.1601 0.1635 0.050 Uiso 1 1 calc R . . C13B C 0.50812(19) 0.03971(17) 0.26123(15) 0.0440(4) Uani 1 1 d . . . H13C H 0.4335 0.0338 0.2672 0.053 Uiso 1 1 calc R . . H13D H 0.5693 -0.0348 0.2685 0.053 Uiso 1 1 calc R . . C14B C 0.45514(16) 0.12379(16) 0.40073(14) 0.0395(4) Uani 1 1 d . . . H14B H 0.4012 0.0914 0.4036 0.047 Uiso 1 1 calc R . . C15B C 0.46379(16) 0.18757(16) 0.47708(13) 0.0378(4) Uani 1 1 d . . . C16B C 0.40932(19) 0.1824(2) 0.55695(15) 0.0496(5) Uani 1 1 d . . . H16B H 0.3610 0.1438 0.5610 0.060 Uiso 1 1 calc R . . C17B C 0.4266(2) 0.2342(2) 0.63015(15) 0.0560(6) Uani 1 1 d . . . H17B H 0.3904 0.2316 0.6856 0.067 Uiso 1 1 calc R . . C18B C 0.4966(2) 0.28951(19) 0.62222(13) 0.0493(5) Uani 1 1 d . . . H18B H 0.5117 0.3235 0.6726 0.059 Uiso 1 1 calc R . . C19B C 0.54538(16) 0.29521(16) 0.53895(12) 0.0384(4) Uani 1 1 d . . . C20B C 0.61762(18) 0.35815(16) 0.52654(14) 0.0420(4) Uani 1 1 d . . . C21B C 0.62423(19) 0.40724(16) 0.44557(15) 0.0433(4) Uani 1 1 d . . . H21B H 0.5810 0.4026 0.3963 0.052 Uiso 1 1 calc R . . C22B C 0.6947(2) 0.46307(18) 0.43773(19) 0.0563(6) Uani 1 1 d . . . H22B H 0.7025 0.4956 0.3825 0.068 Uiso 1 1 calc R . . C23B C 0.7533(3) 0.4705(2) 0.5116(2) 0.0723(8) Uani 1 1 d . . . H23B H 0.8019 0.5088 0.5087 0.087 Uiso 1 1 calc R . . C24B C 0.7398(3) 0.4215(3) 0.5888(2) 0.0809(10) Uani 1 1 d . . . H24B H 0.7798 0.4279 0.6395 0.097 Uiso 1 1 calc R . . B1 B 0.5300(9) 0.7549(10) 0.1124(10) 0.049(2) Uani 0.544(15) 1 d P A 3 F10 F 0.5720(9) 0.7215(8) 0.0342(8) 0.0652(19) Uani 0.544(15) 1 d P A 3 F11 F 0.4439(10) 0.7277(11) 0.1587(6) 0.0618(14) Uani 0.544(15) 1 d P A 3 F12 F 0.6209(4) 0.7157(8) 0.1700(2) 0.0667(19) Uani 0.544(15) 1 d P A 3 F13 F 0.4882(6) 0.8665(5) 0.1015(7) 0.083(2) Uani 0.544(15) 1 d P A 3 B1' B 0.5017(13) 0.7913(13) 0.1102(10) 0.054(3) Uani 0.456(15) 1 d P A 4 F10' F 0.5523(10) 0.7059(8) 0.0361(7) 0.060(2) Uani 0.456(15) 1 d P A 4 F11' F 0.4354(13) 0.7396(13) 0.1319(10) 0.078(3) Uani 0.456(15) 1 d P A 4 F12' F 0.5778(9) 0.7928(12) 0.1714(3) 0.081(3) Uani 0.456(15) 1 d P A 4 F13' F 0.4365(11) 0.8958(7) 0.0805(4) 0.080(2) Uani 0.456(15) 1 d P A 4 B2 B 0.1383(7) 0.2659(6) 0.3533(4) 0.0393(12) Uani 0.622(4) 1 d P B 1 F20 F 0.2038(8) 0.3097(7) 0.3979(7) 0.0513(10) Uani 0.622(4) 1 d P B 1 F21 F 0.1198(5) 0.3037(6) 0.2654(4) 0.0741(17) Uani 0.622(4) 1 d P B 1 F22 F 0.03202(18) 0.29900(19) 0.39470(13) 0.0479(6) Uani 0.622(4) 1 d P B 1 F23 F 0.1895(3) 0.1533(2) 0.3568(2) 0.0800(10) Uani 0.622(4) 1 d P B 1 B2' B 0.1580(10) 0.2457(11) 0.3277(6) 0.038(2) Uani 0.378(4) 1 d P B 2 F20' F 0.1869(15) 0.3000(15) 0.3894(13) 0.065(3) Uani 0.378(4) 1 d P B 2 F21' F 0.0849(8) 0.3184(8) 0.2699(8) 0.057(2) Uani 0.378(4) 1 d P B 2 F22' F 0.1111(5) 0.1776(5) 0.3661(3) 0.0733(16) Uani 0.378(4) 1 d P B 2 F23' F 0.2542(3) 0.1807(3) 0.2795(3) 0.0552(11) Uani 0.378(4) 1 d P 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 0.03507(6) 0.03409(6) 0.03273(6) 0.00534(4) -0.00243(5) -0.01966(5) Ag2 0.03853(7) 0.03311(6) 0.02782(6) 0.00733(4) -0.00704(5) -0.01462(5) N1A 0.0378(8) 0.0422(8) 0.0540(10) 0.0179(7) -0.0047(7) -0.0158(7) N2A 0.0401(7) 0.0330(7) 0.0309(7) -0.0002(5) -0.0015(6) -0.0215(6) N3A 0.0345(7) 0.0289(6) 0.0404(8) -0.0024(5) -0.0070(6) -0.0137(5) N4A 0.0308(6) 0.0293(6) 0.0267(6) 0.0012(5) -0.0043(5) -0.0092(5) N5A 0.0300(6) 0.0272(6) 0.0293(6) 0.0012(5) 0.0015(5) -0.0131(5) N6A 0.0525(10) 0.0381(8) 0.0414(8) -0.0112(6) 0.0126(7) -0.0209(7) C1A 0.0408(10) 0.0491(11) 0.0660(14) 0.0156(10) -0.0037(10) -0.0164(9) C2A 0.0421(10) 0.0456(11) 0.0624(14) -0.0007(10) -0.0112(10) -0.0130(9) C3A 0.0612(15) 0.0701(16) 0.0690(17) 0.0275(13) -0.0309(13) -0.0243(13) C4A 0.0659(15) 0.0646(15) 0.0604(14) 0.0329(12) -0.0248(12) -0.0307(12) C5A 0.0480(10) 0.0317(8) 0.0341(8) 0.0059(6) -0.0086(7) -0.0196(7) C6A 0.0520(10) 0.0369(8) 0.0334(8) 0.0069(6) -0.0058(7) -0.0273(8) C7A 0.0755(16) 0.0593(13) 0.0514(12) 0.0232(10) -0.0133(11) -0.0456(13) C8A 0.0821(18) 0.0775(17) 0.0612(15) 0.0210(13) -0.0051(13) -0.0610(16) C9A 0.0565(13) 0.0644(13) 0.0530(12) 0.0017(10) 0.0029(10) -0.0442(11) C10A 0.0417(9) 0.0396(8) 0.0366(8) -0.0040(7) 0.0008(7) -0.0257(7) C11A 0.0341(8) 0.0402(9) 0.0447(10) -0.0076(7) -0.0030(7) -0.0198(7) C12A 0.0418(9) 0.0365(9) 0.0463(10) -0.0003(7) -0.0186(8) -0.0139(7) C13A 0.0415(9) 0.0321(8) 0.0278(7) -0.0013(6) -0.0098(6) -0.0072(7) C14A 0.0368(8) 0.0326(7) 0.0256(7) 0.0045(6) -0.0044(6) -0.0124(6) C15A 0.0347(8) 0.0279(7) 0.0311(7) 0.0037(6) -0.0005(6) -0.0130(6) C16A 0.0605(12) 0.0328(8) 0.0368(9) 0.0091(7) -0.0045(8) -0.0166(8) C17A 0.0735(15) 0.0280(8) 0.0505(12) 0.0072(8) -0.0031(11) -0.0157(9) C18A 0.0553(12) 0.0282(8) 0.0466(10) -0.0028(7) 0.0022(9) -0.0160(8) C19A 0.0336(8) 0.0303(7) 0.0333(8) -0.0023(6) 0.0037(6) -0.0156(6) C20A 0.0360(8) 0.0346(8) 0.0315(7) -0.0057(6) 0.0062(6) -0.0199(6) C21A 0.0377(8) 0.0406(9) 0.0312(8) -0.0049(6) 0.0015(7) -0.0171(7) C22A 0.0489(11) 0.0525(11) 0.0336(9) -0.0014(8) -0.0013(8) -0.0249(9) C23A 0.0658(14) 0.0605(12) 0.0296(8) -0.0057(8) 0.0048(8) -0.0397(11) C24A 0.0644(13) 0.0497(11) 0.0383(10) -0.0152(8) 0.0169(9) -0.0293(10) N1B 0.0388(9) 0.0669(12) 0.0445(9) 0.0074(8) 0.0021(7) -0.0239(8) N2B 0.0463(8) 0.0342(7) 0.0293(7) -0.0029(5) 0.0021(6) -0.0177(6) N3B 0.0392(7) 0.0316(7) 0.0313(7) -0.0001(5) -0.0090(6) -0.0134(6) N4B 0.0346(7) 0.0352(7) 0.0407(8) 0.0056(6) -0.0058(6) -0.0182(6) N5B 0.0306(7) 0.0362(7) 0.0310(7) 0.0049(5) -0.0016(5) -0.0095(6) N6B 0.0679(14) 0.0702(14) 0.0500(11) -0.0127(10) -0.0111(10) -0.0283(11) C1B 0.0404(11) 0.0716(16) 0.0581(14) 0.0110(11) -0.0005(10) -0.0198(11) C2B 0.0369(11) 0.0699(17) 0.091(2) 0.0026(15) -0.0079(12) -0.0132(11) C3B 0.0406(13) 0.0688(17) 0.136(3) 0.0017(18) -0.0081(16) -0.0273(12) C4B 0.0461(12) 0.0528(13) 0.109(2) -0.0016(14) 0.0054(14) -0.0270(11) C5B 0.0408(10) 0.0439(10) 0.0474(10) -0.0109(8) 0.0105(8) -0.0207(8) C6B 0.0504(11) 0.0414(9) 0.0380(9) -0.0091(7) 0.0125(8) -0.0243(8) C7B 0.0699(15) 0.0586(13) 0.0458(11) -0.0091(10) 0.0204(11) -0.0386(12) C8B 0.093(2) 0.0582(13) 0.0361(10) 0.0020(9) 0.0133(11) -0.0406(14) C9B 0.0840(17) 0.0480(11) 0.0293(9) 0.0063(8) -0.0019(10) -0.0293(11) C10B 0.0586(12) 0.0354(8) 0.0259(7) 0.0000(6) -0.0013(7) -0.0189(8) C11B 0.0507(10) 0.0348(8) 0.0288(8) 0.0025(6) -0.0111(7) -0.0122(7) C12B 0.0400(9) 0.0429(9) 0.0441(10) -0.0037(8) -0.0128(8) -0.0177(8) C13B 0.0458(10) 0.0428(10) 0.0536(11) -0.0034(8) -0.0027(9) -0.0283(8) C14B 0.0346(8) 0.0423(9) 0.0457(10) 0.0110(8) -0.0038(7) -0.0202(7) C15B 0.0315(8) 0.0419(9) 0.0366(8) 0.0118(7) -0.0008(7) -0.0120(7) C16B 0.0434(10) 0.0587(12) 0.0431(10) 0.0163(9) 0.0046(8) -0.0180(9) C17B 0.0554(13) 0.0631(14) 0.0371(10) 0.0146(9) 0.0090(9) -0.0123(11) C18B 0.0524(12) 0.0536(12) 0.0289(8) 0.0039(8) -0.0015(8) -0.0080(9) C19B 0.0371(9) 0.0395(9) 0.0305(8) 0.0025(6) -0.0026(7) -0.0072(7) C20B 0.0419(10) 0.0387(9) 0.0394(9) -0.0098(7) -0.0002(8) -0.0098(7) C21B 0.0466(10) 0.0343(8) 0.0458(10) -0.0084(7) 0.0050(8) -0.0130(8) C22B 0.0592(14) 0.0387(10) 0.0724(16) -0.0159(10) 0.0132(12) -0.0213(10) C23B 0.0732(18) 0.0638(16) 0.093(2) -0.0249(15) 0.0034(16) -0.0407(15) C24B 0.087(2) 0.090(2) 0.079(2) -0.0275(18) -0.0145(17) -0.0472(19) B1 0.041(4) 0.055(5) 0.056(3) -0.017(4) 0.003(3) -0.024(3) F10 0.072(3) 0.085(4) 0.048(2) 0.003(2) -0.0058(18) -0.041(3) F11 0.052(2) 0.080(3) 0.064(3) 0.012(3) -0.005(2) -0.038(2) F12 0.058(2) 0.113(5) 0.0433(14) -0.0062(19) -0.0017(13) -0.049(3) F13 0.074(3) 0.042(2) 0.137(6) -0.028(3) 0.019(3) -0.028(2) B1' 0.054(7) 0.073(10) 0.042(3) -0.017(6) 0.003(4) -0.033(6) F10' 0.079(5) 0.046(2) 0.038(2) 0.0078(17) -0.020(3) -0.007(3) F11' 0.071(5) 0.083(5) 0.101(8) 0.002(5) 0.005(5) -0.055(4) F12' 0.104(5) 0.137(8) 0.0337(16) -0.001(2) -0.012(2) -0.081(6) F13' 0.113(6) 0.055(3) 0.072(3) -0.011(2) -0.004(3) -0.033(4) B2 0.048(3) 0.040(2) 0.030(3) 0.003(2) -0.007(2) -0.018(2) F20 0.050(2) 0.069(2) 0.048(3) -0.0092(18) -0.0088(17) -0.0361(17) F21 0.087(4) 0.103(4) 0.0269(14) 0.005(2) 0.003(2) -0.034(3) F22 0.0464(11) 0.0636(13) 0.0399(10) 0.0037(9) -0.0046(8) -0.0286(10) F23 0.083(2) 0.0369(12) 0.108(3) -0.0107(13) -0.0138(19) -0.0110(13) B2' 0.038(4) 0.058(6) 0.023(4) 0.004(3) -0.009(3) -0.025(4) F20' 0.067(6) 0.101(6) 0.047(3) -0.022(3) -0.011(3) -0.052(4) F21' 0.060(4) 0.041(2) 0.049(4) 0.0010(19) -0.015(3) 0.001(2) F22' 0.076(3) 0.128(4) 0.046(2) 0.039(2) -0.023(2) -0.073(3) F23' 0.0363(17) 0.056(2) 0.062(2) -0.0069(17) -0.0067(15) -0.0070(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 N4B 2.2697(15) . ? Ag1 N3A 2.3625(15) . ? Ag1 N2A 2.3737(14) . ? Ag1 N5B 2.4893(15) . ? Ag1 N1A 2.5742(17) . ? Ag1 Ag2 3.1889(6) . ? Ag2 N4A 2.2820(14) . ? Ag2 N2B 2.3500(16) . ? Ag2 N3B 2.4063(15) . ? Ag2 N5A 2.5270(14) . ? Ag2 N1B 2.6062(18) . ? N1A C1A 1.329(3) . ? N1A C5A 1.330(2) . ? N2A C6A 1.327(2) . ? N2A C10A 1.332(2) . ? N3A C11A 1.263(2) . ? N3A C12A 1.462(2) . ? N4A C14A 1.265(2) . ? N4A C13A 1.460(2) . ? N5A C19A 1.336(2) . ? N5A C15A 1.346(2) . ? N6A C20A 1.339(2) . ? N6A C24A 1.343(3) . ? C1A C2A 1.370(3) . ? C1A H1AA 0.9500 . ? C2A C3A 1.368(4) . ? C2A H2AA 0.9500 . ? C3A C4A 1.374(4) . ? C3A H3AA 0.9500 . ? C4A C5A 1.379(3) . ? C4A H4AA 0.9500 . ? C5A C6A 1.484(3) . ? C6A C7A 1.397(3) . ? C7A C8A 1.374(4) . ? C7A H7AA 0.9500 . ? C8A C9A 1.375(4) . ? C8A H8AA 0.9500 . ? C9A C10A 1.388(3) . ? C9A H9AA 0.9500 . ? C10A C11A 1.469(3) . ? C11A H11A 0.9500 . ? C12A C13A 1.513(3) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.470(2) . ? C14A H14A 0.9500 . ? C15A C16A 1.384(2) . ? C16A C17A 1.381(3) . ? C16A H16A 0.9500 . ? C17A C18A 1.367(3) . ? C17A H17A 0.9500 . ? C18A C19A 1.400(2) . ? C18A H18A 0.9500 . ? C19A C20A 1.486(2) . ? C20A C21A 1.378(3) . ? C21A C22A 1.383(3) . ? C21A H21A 0.9500 . ? C22A C23A 1.376(3) . ? C22A H22A 0.9500 . ? C23A C24A 1.369(4) . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? N1B C1B 1.323(3) . ? N1B C5B 1.342(3) . ? N2B C6B 1.325(3) . ? N2B C10B 1.336(3) . ? N3B C11B 1.267(2) . ? N3B C12B 1.456(3) . ? N4B C14B 1.264(3) . ? N4B C13B 1.466(3) . ? N5B C19B 1.336(2) . ? N5B C15B 1.343(2) . ? N6B C24B 1.338(4) . ? N6B C20B 1.338(3) . ? C1B C2B 1.378(4) . ? C1B H1BA 0.9500 . ? C2B C3B 1.369(5) . ? C2B H2BA 0.9500 . ? C3B C4B 1.366(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.379(3) . ? C4B H4BA 0.9500 . ? C5B C6B 1.480(3) . ? C6B C7B 1.407(3) . ? C7B C8B 1.360(4) . ? C7B H7BA 0.9500 . ? C8B C9B 1.377(4) . ? C8B H8BA 0.9500 . ? C9B C10B 1.393(3) . ? C9B H9BA 0.9500 . ? C10B C11B 1.463(3) . ? C11B H11B 0.9500 . ? C12B C13B 1.509(3) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.471(3) . ? C14B H14B 0.9500 . ? C15B C16B 1.388(3) . ? C16B C17B 1.375(4) . ? C16B H16B 0.9500 . ? C17B C18B 1.373(4) . ? C17B H17B 0.9500 . ? C18B C19B 1.399(3) . ? C18B H18B 0.9500 . ? C19B C20B 1.484(3) . ? C20B C21B 1.387(3) . ? C21B C22B 1.383(3) . ? C21B H21B 0.9500 . ? C22B C23B 1.378(4) . ? C22B H22B 0.9500 . ? C23B C24B 1.362(5) . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? B1 F10 1.290(18) . ? B1 F13 1.369(10) . ? B1 F12 1.380(12) . ? B1 F11 1.451(18) . ? B1' F11' 1.32(2) . ? B1' F12' 1.358(16) . ? B1' F13' 1.372(14) . ? B1' F10' 1.539(19) . ? B2 F23 1.372(7) . ? B2 F22 1.384(7) . ? B2 F20 1.387(9) . ? B2 F21 1.393(9) . ? B2' F20' 1.332(16) . ? B2' F21' 1.354(15) . ? B2' F23' 1.381(11) . ? B2' F22' 1.386(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4B Ag1 N3A 133.78(5) . . ? N4B Ag1 N2A 149.14(5) . . ? N3A Ag1 N2A 69.84(5) . . ? N4B Ag1 N5B 71.49(6) . . ? N3A Ag1 N5B 102.30(5) . . ? N2A Ag1 N5B 129.45(5) . . ? N4B Ag1 N1A 92.88(6) . . ? N3A Ag1 N1A 133.06(5) . . ? N2A Ag1 N1A 64.94(5) . . ? N5B Ag1 N1A 96.80(6) . . ? N4B Ag1 Ag2 79.68(4) . . ? N3A Ag1 Ag2 67.77(4) . . ? N2A Ag1 Ag2 97.46(4) . . ? N5B Ag1 Ag2 126.62(4) . . ? N1A Ag1 Ag2 129.19(5) . . ? N4A Ag2 N2B 139.69(5) . . ? N4A Ag2 N3B 133.38(5) . . ? N2B Ag2 N3B 70.01(6) . . ? N4A Ag2 N5A 71.27(5) . . ? N2B Ag2 N5A 132.14(5) . . ? N3B Ag2 N5A 119.45(5) . . ? N4A Ag2 N1B 90.90(6) . . ? N2B Ag2 N1B 65.43(6) . . ? N3B Ag2 N1B 133.49(6) . . ? N5A Ag2 N1B 83.36(6) . . ? N4A Ag2 Ag1 80.25(4) . . ? N2B Ag2 Ag1 88.30(4) . . ? N3B Ag2 Ag1 62.96(4) . . ? N5A Ag2 Ag1 139.19(3) . . ? N1B Ag2 Ag1 126.52(5) . . ? C1A N1A C5A 118.61(18) . . ? C1A N1A Ag1 123.20(14) . . ? C5A N1A Ag1 116.91(13) . . ? C6A N2A C10A 119.62(16) . . ? C6A N2A Ag1 124.70(12) . . ? C10A N2A Ag1 115.67(12) . . ? C11A N3A C12A 119.35(16) . . ? C11A N3A Ag1 116.20(13) . . ? C12A N3A Ag1 124.35(12) . . ? C14A N4A C13A 117.30(14) . . ? C14A N4A Ag2 117.85(11) . . ? C13A N4A Ag2 124.68(10) . . ? C19A N5A C15A 117.82(14) . . ? C19A N5A Ag2 132.30(11) . . ? C15A N5A Ag2 109.03(10) . . ? C20A N6A C24A 116.76(19) . . ? N1A C1A C2A 123.4(2) . . ? N1A C1A H1AA 118.3 . . ? C2A C1A H1AA 118.3 . . ? C3A C2A C1A 117.6(2) . . ? C3A C2A H2AA 121.2 . . ? C1A C2A H2AA 121.2 . . ? C2A C3A C4A 119.9(2) . . ? C2A C3A H3AA 120.0 . . ? C4A C3A H3AA 120.0 . . ? C3A C4A C5A 118.8(2) . . ? C3A C4A H4AA 120.6 . . ? C5A C4A H4AA 120.6 . . ? N1A C5A C4A 121.6(2) . . ? N1A C5A C6A 116.18(16) . . ? C4A C5A C6A 122.20(19) . . ? N2A C6A C7A 121.2(2) . . ? N2A C6A C5A 116.17(15) . . ? C7A C6A C5A 122.67(19) . . ? C8A C7A C6A 119.1(2) . . ? C8A C7A H7AA 120.5 . . ? C6A C7A H7AA 120.5 . . ? C7A C8A C9A 119.5(2) . . ? C7A C8A H8AA 120.2 . . ? C9A C8A H8AA 120.2 . . ? C8A C9A C10A 118.2(2) . . ? C8A C9A H9AA 120.9 . . ? C10A C9A H9AA 120.9 . . ? N2A C10A C9A 122.33(19) . . ? N2A C10A C11A 116.62(16) . . ? C9A C10A C11A 120.95(18) . . ? N3A C11A C10A 120.54(17) . . ? N3A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? N3A C12A C13A 110.85(15) . . ? N3A C12A H12A 109.5 . . ? C13A C12A H12A 109.5 . . ? N3A C12A H12B 109.5 . . ? C13A C12A H12B 109.5 . . ? H12A C12A H12B 108.1 . . ? N4A C13A C12A 110.95(16) . . ? N4A C13A H13A 109.4 . . ? C12A C13A H13A 109.4 . . ? N4A C13A H13B 109.4 . . ? C12A C13A H13B 109.4 . . ? H13A C13A H13B 108.0 . . ? N4A C14A C15A 122.96(15) . . ? N4A C14A H14A 118.5 . . ? C15A C14A H14A 118.5 . . ? N5A C15A C16A 123.21(16) . . ? N5A C15A C14A 118.75(14) . . ? C16A C15A C14A 117.99(16) . . ? C17A C16A C15A 118.48(18) . . ? C17A C16A H16A 120.8 . . ? C15A C16A H16A 120.8 . . ? C18A C17A C16A 118.93(18) . . ? C18A C17A H17A 120.5 . . ? C16A C17A H17A 120.5 . . ? C17A C18A C19A 119.66(18) . . ? C17A C18A H18A 120.2 . . ? C19A C18A H18A 120.2 . . ? N5A C19A C18A 121.83(17) . . ? N5A C19A C20A 118.51(15) . . ? C18A C19A C20A 119.66(16) . . ? N6A C20A C21A 122.71(17) . . ? N6A C20A C19A 115.44(16) . . ? C21A C20A C19A 121.77(15) . . ? C20A C21A C22A 119.23(18) . . ? C20A C21A H21A 120.4 . . ? C22A C21A H21A 120.4 . . ? C23A C22A C21A 118.8(2) . . ? C23A C22A H22A 120.6 . . ? C21A C22A H22A 120.6 . . ? C24A C23A C22A 118.18(19) . . ? C24A C23A H23A 120.9 . . ? C22A C23A H23A 120.9 . . ? N6A C24A C23A 124.32(19) . . ? N6A C24A H24A 117.8 . . ? C23A C24A H24A 117.8 . . ? C1B N1B C5B 118.0(2) . . ? C1B N1B Ag2 124.77(15) . . ? C5B N1B Ag2 112.47(14) . . ? C6B N2B C10B 119.30(17) . . ? C6B N2B Ag2 124.07(14) . . ? C10B N2B Ag2 116.63(13) . . ? C11B N3B C12B 117.71(17) . . ? C11B N3B Ag2 114.74(13) . . ? C12B N3B Ag2 127.27(12) . . ? C14B N4B C13B 118.39(16) . . ? C14B N4B Ag1 117.62(13) . . ? C13B N4B Ag1 123.69(12) . . ? C19B N5B C15B 118.62(16) . . ? C19B N5B Ag1 130.96(13) . . ? C15B N5B Ag1 109.82(12) . . ? C24B N6B C20B 116.6(3) . . ? N1B C1B C2B 123.5(3) . . ? N1B C1B H1BA 118.3 . . ? C2B C1B H1BA 118.3 . . ? C3B C2B C1B 118.1(3) . . ? C3B C2B H2BA 120.9 . . ? C1B C2B H2BA 120.9 . . ? C4B C3B C2B 119.4(2) . . ? C4B C3B H3BA 120.3 . . ? C2B C3B H3BA 120.3 . . ? C3B C4B C5B 119.2(3) . . ? C3B C4B H4BA 120.4 . . ? C5B C4B H4BA 120.4 . . ? N1B C5B C4B 121.8(2) . . ? N1B C5B C6B 116.07(18) . . ? C4B C5B C6B 122.1(2) . . ? N2B C6B C7B 121.2(2) . . ? N2B C6B C5B 116.36(17) . . ? C7B C6B C5B 122.5(2) . . ? C8B C7B C6B 119.3(2) . . ? C8B C7B H7BA 120.3 . . ? C6B C7B H7BA 120.3 . . ? C7B C8B C9B 119.7(2) . . ? C7B C8B H8BA 120.2 . . ? C9B C8B H8BA 120.2 . . ? C8B C9B C10B 118.1(2) . . ? C8B C9B H9BA 121.0 . . ? C10B C9B H9BA 121.0 . . ? N2B C10B C9B 122.4(2) . . ? N2B C10B C11B 116.93(16) . . ? C9B C10B C11B 120.6(2) . . ? N3B C11B C10B 121.17(17) . . ? N3B C11B H11B 119.4 . . ? C10B C11B H11B 119.4 . . ? N3B C12B C13B 110.68(15) . . ? N3B C12B H12C 109.5 . . ? C13B C12B H12C 109.5 . . ? N3B C12B H12D 109.5 . . ? C13B C12B H12D 109.5 . . ? H12C C12B H12D 108.1 . . ? N4B C13B C12B 111.66(15) . . ? N4B C13B H13C 109.3 . . ? C12B C13B H13C 109.3 . . ? N4B C13B H13D 109.3 . . ? C12B C13B H13D 109.3 . . ? H13C C13B H13D 107.9 . . ? N4B C14B C15B 122.16(17) . . ? N4B C14B H14B 118.9 . . ? C15B C14B H14B 118.9 . . ? N5B C15B C16B 122.4(2) . . ? N5B C15B C14B 118.22(16) . . ? C16B C15B C14B 119.29(19) . . ? C17B C16B C15B 118.8(2) . . ? C17B C16B H16B 120.6 . . ? C15B C16B H16B 120.6 . . ? C18B C17B C16B 119.3(2) . . ? C18B C17B H17B 120.4 . . ? C16B C17B H17B 120.4 . . ? C17B C18B C19B 119.1(2) . . ? C17B C18B H18B 120.5 . . ? C19B C18B H18B 120.5 . . ? N5B C19B C18B 121.7(2) . . ? N5B C19B C20B 117.39(17) . . ? C18B C19B C20B 120.86(19) . . ? N6B C20B C21B 122.7(2) . . ? N6B C20B C19B 115.6(2) . . ? C21B C20B C19B 121.67(18) . . ? C22B C21B C20B 118.9(2) . . ? C22B C21B H21B 120.5 . . ? C20B C21B H21B 120.5 . . ? C23B C22B C21B 118.7(3) . . ? C23B C22B H22B 120.7 . . ? C21B C22B H22B 120.7 . . ? C24B C23B C22B 118.3(3) . . ? C24B C23B H23B 120.9 . . ? C22B C23B H23B 120.9 . . ? N6B C24B C23B 124.8(3) . . ? N6B C24B H24B 117.6 . . ? C23B C24B H24B 117.6 . . ? F10 B1 F13 101.7(11) . . ? F10 B1 F12 106.2(8) . . ? F13 B1 F12 112.2(10) . . ? F10 B1 F11 125.5(12) . . ? F13 B1 F11 108.6(9) . . ? F12 B1 F11 102.7(10) . . ? F11' B1' F12' 117.8(13) . . ? F11' B1' F13' 110.2(12) . . ? F12' B1' F13' 110.6(10) . . ? F11' B1' F10' 86.7(14) . . ? F12' B1' F10' 115.1(10) . . ? F13' B1' F10' 114.7(11) . . ? F23 B2 F22 107.9(5) . . ? F23 B2 F20 110.1(7) . . ? F22 B2 F20 109.2(6) . . ? F23 B2 F21 111.0(5) . . ? F22 B2 F21 107.1(6) . . ? F20 B2 F21 111.4(8) . . ? F20' B2' F21' 109.4(13) . . ? F20' B2' F23' 109.6(12) . . ? F21' B2' F23' 107.3(8) . . ? F20' B2' F22' 111.3(11) . . ? F21' B2' F22' 111.4(9) . . ? F23' B2' F22' 107.8(9) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.800 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.055 # Attachment '- GQ136.CIF' data_gq136 _database_code_depnum_ccdc_archive 'CCDC 774874' #TrackingRef '- GQ136.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C52 H48 Ag3 N12), 12(B F4), 7(C2 H3 N), 2(H2 O)' _chemical_formula_sum 'C222 H217 Ag12 B12 F48 N55 O2' _chemical_formula_weight 6023.69 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.618(3) _cell_length_b 24.416(5) _cell_length_c 15.972(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.12(3) _cell_angle_gamma 90.00 _cell_volume 6044(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20534 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 50.87 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3002 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8174 _exptl_absorpt_correction_T_max 0.9022 _exptl_absorpt_process_details '(Blessing 1951)' _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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 163348 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13825 _reflns_number_gt 12903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+9.9329P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13825 _refine_ls_number_parameters 896 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.200 _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 0.017813(18) 0.226889(11) 0.670917(17) 0.04102(7) Uani 1 1 d . . . Ag2 Ag -0.109266(17) 0.236642(11) 0.502825(17) 0.04034(7) Uani 1 1 d . . . Ag3 Ag -0.312033(18) 0.293713(12) 0.284681(16) 0.04424(8) Uani 1 1 d . . . N1A N 0.02778(17) 0.31470(11) 0.64804(16) 0.0354(5) Uani 1 1 d . . . N2A N 0.05833(17) 0.24681(12) 0.51486(16) 0.0360(6) Uani 1 1 d . . . N3A N -0.04941(18) 0.15975(11) 0.45935(16) 0.0365(6) Uani 1 1 d . . . N4A N -0.3282(2) 0.19645(14) 0.33389(19) 0.0482(7) Uani 1 1 d . . . N5A N -0.37984(19) 0.29298(14) 0.40337(18) 0.0461(7) Uani 1 1 d . . . N6A N -0.3127(2) 0.38636(15) 0.3502(2) 0.0547(8) Uani 1 1 d . . . C1A C -0.0084(2) 0.35097(15) 0.6959(2) 0.0425(7) Uani 1 1 d . . . H1AA H -0.0394 0.3377 0.7393 0.051 Uiso 1 1 calc R . . C2A C -0.0023(3) 0.40693(16) 0.6846(3) 0.0512(9) Uani 1 1 d . . . H2AA H -0.0297 0.4317 0.7187 0.061 Uiso 1 1 calc R . . C3A C 0.0443(3) 0.42612(16) 0.6229(3) 0.0555(10) Uani 1 1 d . . . H3AA H 0.0502 0.4644 0.6144 0.067 Uiso 1 1 calc R . . C4A C 0.0822(3) 0.38917(16) 0.5736(2) 0.0500(9) Uani 1 1 d . . . H4AA H 0.1152 0.4017 0.5313 0.060 Uiso 1 1 calc R . . C5A C 0.0718(2) 0.33328(14) 0.5864(2) 0.0387(7) Uani 1 1 d . . . C6A C 0.1057(2) 0.29238(15) 0.5299(2) 0.0398(7) Uani 1 1 d . . . C7A C 0.1810(2) 0.30117(17) 0.4935(2) 0.0483(8) Uani 1 1 d . . . H7AA H 0.2135 0.3338 0.5049 0.058 Uiso 1 1 calc R . . C8A C 0.2077(3) 0.26202(19) 0.4407(2) 0.0531(9) Uani 1 1 d . . . H8AA H 0.2599 0.2667 0.4167 0.064 Uiso 1 1 calc R . . C9A C 0.1578(2) 0.21574(17) 0.4226(2) 0.0477(8) Uani 1 1 d . . . H9AA H 0.1745 0.1886 0.3852 0.057 Uiso 1 1 calc R . . C10A C 0.0830(2) 0.20965(15) 0.4602(2) 0.0391(7) Uani 1 1 d . . . C11A C 0.0276(2) 0.16135(15) 0.44160(19) 0.0392(7) Uani 1 1 d . . . H11A H 0.0501 0.1304 0.4155 0.047 Uiso 1 1 calc R . . C12A C -0.0972(2) 0.10813(14) 0.4471(2) 0.0415(7) Uani 1 1 d . . . H12A H -0.0923 0.0880 0.5013 0.050 Uiso 1 1 calc R . . H12B H -0.0707 0.0852 0.4061 0.050 Uiso 1 1 calc R . . C13A C -0.1915(2) 0.11669(15) 0.4155(2) 0.0434(7) Uani 1 1 d . . . H13A H -0.2145 0.1460 0.4494 0.052 Uiso 1 1 calc R . . H13B H -0.2234 0.0826 0.4246 0.052 Uiso 1 1 calc R . . C14A C -0.2084(3) 0.13208(16) 0.3233(2) 0.0482(8) Uani 1 1 d . . . H14A H -0.1909 0.1014 0.2886 0.058 Uiso 1 1 calc R . . H14B H -0.1730 0.1644 0.3127 0.058 Uiso 1 1 calc R . . C15A C -0.3034(3) 0.14518(17) 0.2968(3) 0.0559(10) Uani 1 1 d . . . H15A H -0.3142 0.1479 0.2345 0.067 Uiso 1 1 calc R . . H15B H -0.3394 0.1150 0.3148 0.067 Uiso 1 1 calc R . . C16A C -0.3781(3) 0.19494(19) 0.3900(2) 0.0549(10) Uani 1 1 d . . . H16A H -0.4002 0.1606 0.4052 0.066 Uiso 1 1 calc R . . C17A C -0.4032(2) 0.2446(2) 0.4329(2) 0.0531(10) Uani 1 1 d . . . C18A C -0.4489(3) 0.2408(3) 0.5022(3) 0.0719(14) Uani 1 1 d . . . H18A H -0.4655 0.2061 0.5219 0.086 Uiso 1 1 calc R . . C19A C -0.4696(3) 0.2880(3) 0.5416(3) 0.0834(18) Uani 1 1 d . . . H19A H -0.5011 0.2865 0.5888 0.100 Uiso 1 1 calc R . . C20A C -0.4445(3) 0.3369(3) 0.5126(3) 0.0725(15) Uani 1 1 d . . . H20A H -0.4580 0.3699 0.5399 0.087 Uiso 1 1 calc R . . C21A C -0.3985(2) 0.3391(2) 0.4421(2) 0.0531(10) Uani 1 1 d . . . C22A C -0.3672(3) 0.39108(19) 0.4087(3) 0.0576(11) Uani 1 1 d . . . C23A C -0.3916(4) 0.4420(3) 0.4368(4) 0.0849(18) Uani 1 1 d . . . H23A H -0.4298 0.4444 0.4786 0.102 Uiso 1 1 calc R . . C24A C -0.3604(5) 0.4887(3) 0.4043(5) 0.105(2) Uani 1 1 d . . . H24A H -0.3767 0.5237 0.4230 0.126 Uiso 1 1 calc R . . C25A C -0.3053(5) 0.4844(2) 0.3441(4) 0.095(2) Uani 1 1 d . . . H25A H -0.2832 0.5162 0.3200 0.115 Uiso 1 1 calc R . . C26A C -0.2824(4) 0.4321(2) 0.3190(3) 0.0723(14) Uani 1 1 d . . . H26A H -0.2434 0.4290 0.2780 0.087 Uiso 1 1 calc R . . N1B N -0.2134(2) 0.21449(12) 0.60137(19) 0.0436(7) Uani 1 1 d . . . N2B N -0.17640(17) 0.31447(11) 0.54285(16) 0.0349(5) Uani 1 1 d . . . N3B N -0.08100(18) 0.31963(12) 0.40650(17) 0.0395(6) Uani 1 1 d . . . N4B N -0.25108(18) 0.29153(12) 0.16570(17) 0.0378(6) Uani 1 1 d . . . N5B N -0.39636(16) 0.36123(11) 0.16043(16) 0.0337(5) Uani 1 1 d . . . N6B N -0.53719(17) 0.33869(12) 0.24254(18) 0.0385(6) Uani 1 1 d . . . C1B C -0.2342(3) 0.16413(15) 0.6251(2) 0.0499(9) Uani 1 1 d . . . H1BA H -0.2091 0.1337 0.6002 0.060 Uiso 1 1 calc R . . C2B C -0.2900(3) 0.15403(16) 0.6836(2) 0.0474(8) Uani 1 1 d . . . H2BA H -0.3037 0.1177 0.6983 0.057 Uiso 1 1 calc R . . C3B C -0.3255(2) 0.19859(17) 0.7201(2) 0.0504(9) Uani 1 1 d . . . H3BA H -0.3635 0.1934 0.7614 0.061 Uiso 1 1 calc R . . C4B C -0.3050(3) 0.25064(16) 0.6958(2) 0.0474(8) Uani 1 1 d . . . H4BA H -0.3289 0.2817 0.7203 0.057 Uiso 1 1 calc R . . C5B C -0.2491(2) 0.25752(14) 0.6354(2) 0.0372(7) Uani 1 1 d . . . C6B C -0.2269(2) 0.31267(14) 0.6040(2) 0.0372(7) Uani 1 1 d . . . C7B C -0.2588(3) 0.36098(16) 0.6356(2) 0.0483(8) Uani 1 1 d . . . H7BA H -0.2951 0.3594 0.6791 0.058 Uiso 1 1 calc R . . C8B C -0.2376(3) 0.41057(16) 0.6035(3) 0.0524(9) Uani 1 1 d . . . H8BA H -0.2589 0.4435 0.6248 0.063 Uiso 1 1 calc R . . C9B C -0.1851(3) 0.41235(15) 0.5400(2) 0.0470(8) Uani 1 1 d . . . H9BA H -0.1692 0.4463 0.5172 0.056 Uiso 1 1 calc R . . C10B C -0.1562(2) 0.36296(14) 0.5107(2) 0.0387(7) Uani 1 1 d . . . C11B C -0.1012(2) 0.36307(15) 0.4422(2) 0.0408(7) Uani 1 1 d . . . H11B H -0.0802 0.3971 0.4242 0.049 Uiso 1 1 calc R . . C12B C -0.0246(2) 0.32555(17) 0.3396(2) 0.0460(8) Uani 1 1 d . . . H12C H 0.0227 0.2983 0.3483 0.055 Uiso 1 1 calc R . . H12D H 0.0015 0.3626 0.3426 0.055 Uiso 1 1 calc R . . C13B C -0.0756(2) 0.31708(15) 0.2535(2) 0.0425(7) Uani 1 1 d . . . H13C H -0.1221 0.3448 0.2449 0.051 Uiso 1 1 calc R . . H13D H -0.0369 0.3229 0.2096 0.051 Uiso 1 1 calc R . . C14B C -0.1152(2) 0.26060(15) 0.2424(2) 0.0427(7) Uani 1 1 d . . . H14C H -0.1463 0.2525 0.2913 0.051 Uiso 1 1 calc R . . H14D H -0.0684 0.2333 0.2420 0.051 Uiso 1 1 calc R . . C15B C -0.1776(2) 0.25449(16) 0.1616(2) 0.0444(8) Uani 1 1 d . . . H15C H -0.1480 0.2637 0.1121 0.053 Uiso 1 1 calc R . . H15D H -0.1982 0.2162 0.1555 0.053 Uiso 1 1 calc R . . C16B C -0.2648(2) 0.32888(14) 0.1103(2) 0.0377(7) Uani 1 1 d . . . H16B H -0.2294 0.3301 0.0661 0.045 Uiso 1 1 calc R . . C17B C -0.3331(2) 0.37029(14) 0.11150(19) 0.0358(6) Uani 1 1 d . . . C18B C -0.3283(2) 0.41804(15) 0.0657(2) 0.0433(7) Uani 1 1 d . . . H18B H -0.2841 0.4229 0.0305 0.052 Uiso 1 1 calc R . . C19B C -0.3891(3) 0.45876(16) 0.0722(2) 0.0496(9) Uani 1 1 d . . . H19B H -0.3878 0.4916 0.0407 0.060 Uiso 1 1 calc R . . C20B C -0.4513(2) 0.45093(15) 0.1249(2) 0.0446(8) Uani 1 1 d . . . H20B H -0.4923 0.4788 0.1317 0.054 Uiso 1 1 calc R . . C21B C -0.4532(2) 0.40132(14) 0.1683(2) 0.0365(6) Uani 1 1 d . . . C22B C -0.5171(2) 0.39120(14) 0.2284(2) 0.0371(7) Uani 1 1 d . . . C23B C -0.5506(2) 0.43427(16) 0.2707(2) 0.0462(8) Uani 1 1 d . . . H23B H -0.5357 0.4711 0.2596 0.055 Uiso 1 1 calc R . . C24B C -0.6062(3) 0.42269(18) 0.3293(3) 0.0530(9) Uani 1 1 d . . . H24B H -0.6304 0.4515 0.3587 0.064 Uiso 1 1 calc R . . C25B C -0.6260(3) 0.36900(18) 0.3448(3) 0.0532(9) Uani 1 1 d . . . H25B H -0.6632 0.3601 0.3855 0.064 Uiso 1 1 calc R . . C26B C -0.5905(2) 0.32814(17) 0.2998(2) 0.0484(8) Uani 1 1 d . . . H26B H -0.6047 0.2911 0.3100 0.058 Uiso 1 1 calc R . . B1 B 0.3816(5) 0.1439(4) 0.4177(5) 0.090(2) Uani 1 1 d . . . F10 F 0.3901(6) 0.1909(3) 0.3823(6) 0.093(3) Uani 0.574(17) 1 d PU A 1 F11 F 0.3013(9) 0.1243(5) 0.4207(11) 0.105(4) Uani 0.574(17) 1 d P A 1 F12 F 0.4269(10) 0.1027(5) 0.3756(9) 0.112(4) Uani 0.574(17) 1 d P A 1 F13 F 0.4292(10) 0.1431(5) 0.5015(7) 0.157(6) Uani 0.574(17) 1 d PU A 1 F10' F 0.347(2) 0.1790(11) 0.3457(14) 0.208(10) Uani 0.426(17) 1 d PU A 2 F11' F 0.3160(15) 0.1175(11) 0.4397(14) 0.157(10) Uani 0.426(17) 1 d P A 2 F12' F 0.4432(15) 0.1239(9) 0.4003(16) 0.142(7) Uani 0.426(17) 1 d P A 2 F13' F 0.3843(8) 0.1809(11) 0.4803(12) 0.179(10) Uani 0.426(17) 1 d PU A 2 B2 B 0.0109(3) 0.09869(18) 0.2128(3) 0.0507(10) Uani 1 1 d . . . F20 F -0.0055(2) 0.06624(10) 0.27953(18) 0.0755(8) Uani 1 1 d . . . F21 F -0.06557(19) 0.11929(13) 0.1711(2) 0.0805(8) Uani 1 1 d D . . F22 F 0.06270(18) 0.14230(10) 0.24217(17) 0.0674(7) Uani 1 1 d . . . F23 F 0.05228(18) 0.06754(10) 0.15709(16) 0.0617(6) Uani 1 1 d . . . B3 B -0.3397(17) 0.0515(10) 0.8748(17) 0.045(4) Uani 0.69(3) 1 d P B 1 F30 F -0.3227(10) 0.0286(3) 0.8018(5) 0.088(3) Uani 0.69(3) 1 d P B 1 F31 F -0.2810(7) 0.0446(4) 0.9379(5) 0.083(3) Uani 0.69(3) 1 d P B 1 F32 F -0.4186(10) 0.0381(8) 0.8957(12) 0.080(3) Uani 0.69(3) 1 d P B 1 F33 F -0.3415(13) 0.1099(7) 0.8666(13) 0.061(3) Uani 0.69(3) 1 d P B 1 B3' B -0.356(4) 0.061(2) 0.867(3) 0.037(6) Uani 0.31(3) 1 d P B 2 F30' F -0.366(2) 0.0276(12) 0.7973(15) 0.148(10) Uani 0.31(3) 1 d P B 2 F31' F -0.2703(13) 0.0341(10) 0.911(3) 0.114(10) Uani 0.31(3) 1 d P B 2 F32' F -0.421(3) 0.0374(18) 0.912(3) 0.088(9) Uani 0.31(3) 1 d P B 2 F33' F -0.352(3) 0.1092(17) 0.848(3) 0.069(9) Uani 0.31(3) 1 d P B 2 N100 N -0.1886(4) 0.02654(19) 0.5830(3) 0.0864(14) Uani 1 1 d . . . C100 C -0.2085(4) -0.0022(2) 0.6303(3) 0.0713(14) Uani 1 1 d . . . C101 C -0.2213(4) -0.0400(2) 0.6967(3) 0.0819(15) Uani 1 1 d . . . H10C H -0.2063 -0.0771 0.6801 0.123 Uiso 1 1 calc R . . H10D H -0.2819 -0.0391 0.7069 0.123 Uiso 1 1 calc R . . H10E H -0.1844 -0.0296 0.7484 0.123 Uiso 1 1 calc R . . N200 N 0.1452(7) 0.5146(4) 0.8114(7) 0.134(4) Uani 0.75 1 d P C 1 C200 C 0.0926(9) 0.5203(5) 0.8429(8) 0.118(4) Uani 0.75 1 d P C 1 C201 C 0.0111(12) 0.5362(6) 0.8604(11) 0.181(7) Uani 0.75 1 d P C 1 H20C H 0.0162 0.5691 0.8958 0.272 Uiso 0.75 1 calc PR C 1 H20D H -0.0146 0.5065 0.8903 0.272 Uiso 0.75 1 calc PR C 1 H20E H -0.0256 0.5440 0.8075 0.272 Uiso 0.75 1 calc PR C 1 O100 O 0.0997(14) 0.4949(9) 0.9408(18) 0.130(8) Uani 0.25 1 d P D 2 O200 O -0.1899(14) 0.1149(7) 0.0525(15) 0.142(10) Uani 0.25 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04479(14) 0.04060(13) 0.03908(13) 0.00306(10) 0.01076(10) -0.00090(10) Ag2 0.04054(13) 0.04113(13) 0.04136(14) -0.00223(10) 0.01298(10) 0.00484(10) Ag3 0.04449(14) 0.06028(17) 0.02911(12) -0.00103(11) 0.00921(10) 0.00455(12) N1A 0.0364(13) 0.0397(14) 0.0292(12) 0.0013(10) 0.0003(10) -0.0013(11) N2A 0.0363(13) 0.0465(15) 0.0249(12) 0.0050(11) 0.0027(10) 0.0044(11) N3A 0.0408(14) 0.0398(14) 0.0289(12) -0.0008(11) 0.0045(10) 0.0046(11) N4A 0.0495(17) 0.0566(19) 0.0355(15) 0.0037(13) -0.0062(13) 0.0008(14) N5A 0.0376(15) 0.071(2) 0.0294(13) -0.0033(13) 0.0027(11) 0.0059(14) N6A 0.066(2) 0.060(2) 0.0348(15) -0.0073(14) -0.0061(14) 0.0059(16) C1A 0.0415(18) 0.0474(19) 0.0372(17) -0.0053(14) -0.0006(14) 0.0006(14) C2A 0.051(2) 0.049(2) 0.051(2) -0.0075(17) -0.0045(17) 0.0041(16) C3A 0.066(3) 0.043(2) 0.054(2) 0.0048(17) -0.0071(19) -0.0027(18) C4A 0.056(2) 0.051(2) 0.0416(19) 0.0096(16) -0.0009(16) -0.0062(17) C5A 0.0367(16) 0.0486(18) 0.0289(14) 0.0069(13) -0.0026(12) -0.0021(14) C6A 0.0389(16) 0.0525(19) 0.0274(14) 0.0105(13) 0.0024(12) 0.0004(14) C7A 0.0449(19) 0.062(2) 0.0390(18) 0.0113(16) 0.0072(15) -0.0069(16) C8A 0.0439(19) 0.077(3) 0.0415(19) 0.0082(18) 0.0172(16) -0.0008(18) C9A 0.0435(19) 0.066(2) 0.0352(17) 0.0052(16) 0.0122(14) 0.0077(17) C10A 0.0384(16) 0.0529(19) 0.0264(14) 0.0059(13) 0.0057(12) 0.0073(14) C11A 0.0421(17) 0.0487(18) 0.0272(14) -0.0004(13) 0.0062(12) 0.0101(14) C12A 0.0461(18) 0.0405(17) 0.0373(17) -0.0007(13) 0.0034(14) 0.0023(14) C13A 0.0494(19) 0.0433(18) 0.0369(17) 0.0038(14) 0.0025(14) -0.0015(15) C14A 0.060(2) 0.051(2) 0.0324(16) -0.0016(15) -0.0004(15) 0.0016(17) C15A 0.065(3) 0.055(2) 0.043(2) -0.0007(17) -0.0128(18) 0.0016(19) C16A 0.050(2) 0.069(3) 0.041(2) 0.0112(18) -0.0082(16) -0.0107(19) C17A 0.0386(18) 0.087(3) 0.0329(17) 0.0024(18) 0.0010(14) -0.0060(18) C18A 0.054(2) 0.121(4) 0.041(2) 0.002(2) 0.0061(18) -0.027(3) C19A 0.055(3) 0.154(6) 0.044(2) -0.017(3) 0.018(2) -0.019(3) C20A 0.047(2) 0.126(5) 0.045(2) -0.028(3) 0.0081(18) 0.010(3) C21A 0.0398(18) 0.083(3) 0.0350(17) -0.0143(18) -0.0017(14) 0.0115(18) C22A 0.055(2) 0.074(3) 0.0401(19) -0.0123(18) -0.0104(17) 0.023(2) C23A 0.087(4) 0.089(4) 0.072(3) -0.028(3) -0.016(3) 0.042(3) C24A 0.139(6) 0.077(4) 0.087(4) -0.019(3) -0.034(4) 0.046(4) C25A 0.143(6) 0.060(3) 0.070(4) 0.006(3) -0.039(4) 0.000(3) C26A 0.102(4) 0.063(3) 0.046(2) 0.002(2) -0.015(2) -0.004(3) N1B 0.0523(17) 0.0407(15) 0.0411(15) -0.0014(12) 0.0187(13) 0.0009(13) N2B 0.0360(13) 0.0382(13) 0.0301(12) -0.0012(10) 0.0021(10) 0.0033(11) N3B 0.0340(13) 0.0499(16) 0.0343(14) 0.0074(12) 0.0034(11) -0.0012(12) N4B 0.0378(14) 0.0481(15) 0.0280(13) -0.0044(11) 0.0057(10) 0.0039(12) N5B 0.0320(13) 0.0419(14) 0.0267(12) -0.0022(10) 0.0019(10) 0.0003(10) N6B 0.0337(13) 0.0438(15) 0.0389(14) -0.0035(12) 0.0080(11) -0.0002(11) C1B 0.068(2) 0.0423(19) 0.0434(19) -0.0025(15) 0.0208(18) -0.0004(17) C2B 0.053(2) 0.049(2) 0.0411(18) 0.0022(15) 0.0094(15) -0.0085(16) C3B 0.0453(19) 0.066(2) 0.0432(19) 0.0025(17) 0.0164(16) -0.0033(17) C4B 0.050(2) 0.052(2) 0.0430(19) -0.0043(16) 0.0165(16) 0.0043(16) C5B 0.0333(15) 0.0472(18) 0.0308(15) -0.0066(13) 0.0024(12) 0.0004(13) C6B 0.0350(15) 0.0423(17) 0.0337(15) -0.0058(13) 0.0018(12) 0.0020(13) C7B 0.051(2) 0.049(2) 0.047(2) -0.0095(16) 0.0120(16) 0.0037(16) C8B 0.057(2) 0.044(2) 0.056(2) -0.0117(17) 0.0070(18) 0.0053(17) C9B 0.053(2) 0.0399(18) 0.0464(19) -0.0013(15) -0.0005(16) 0.0012(15) C10B 0.0380(16) 0.0406(17) 0.0357(16) 0.0009(13) -0.0030(13) 0.0007(13) C11B 0.0408(17) 0.0432(18) 0.0370(16) 0.0068(14) -0.0011(13) -0.0041(14) C12B 0.0363(17) 0.066(2) 0.0366(17) 0.0126(16) 0.0074(14) -0.0034(16) C13B 0.0375(16) 0.057(2) 0.0339(16) 0.0115(15) 0.0066(13) 0.0015(15) C14B 0.0436(18) 0.0490(19) 0.0362(17) 0.0046(14) 0.0076(14) 0.0094(15) C15B 0.0452(18) 0.053(2) 0.0358(17) -0.0042(15) 0.0101(14) 0.0113(15) C16B 0.0362(16) 0.0498(18) 0.0277(14) -0.0040(13) 0.0061(12) -0.0001(13) C17B 0.0338(15) 0.0439(17) 0.0291(14) -0.0039(12) 0.0023(12) -0.0014(13) C18B 0.0451(19) 0.0469(19) 0.0391(17) 0.0019(14) 0.0094(14) -0.0034(15) C19B 0.060(2) 0.0434(19) 0.047(2) 0.0071(15) 0.0107(17) 0.0000(16) C20B 0.0474(19) 0.0410(18) 0.0460(19) -0.0007(15) 0.0075(15) 0.0037(15) C21B 0.0358(15) 0.0431(17) 0.0300(14) -0.0033(12) 0.0017(12) 0.0016(13) C22B 0.0324(15) 0.0457(18) 0.0332(15) -0.0025(13) 0.0033(12) 0.0031(13) C23B 0.0479(19) 0.0470(19) 0.0441(19) -0.0054(15) 0.0077(15) 0.0074(15) C24B 0.051(2) 0.062(2) 0.048(2) -0.0103(18) 0.0123(17) 0.0107(18) C25B 0.045(2) 0.069(3) 0.049(2) -0.0057(18) 0.0183(16) 0.0008(18) C26B 0.0429(19) 0.055(2) 0.049(2) -0.0028(17) 0.0154(16) -0.0026(16) B1 0.070(4) 0.114(6) 0.091(5) -0.030(4) 0.029(4) -0.033(4) F10 0.101(5) 0.078(4) 0.094(6) 0.015(4) -0.009(4) -0.009(4) F11 0.066(5) 0.088(5) 0.168(12) -0.043(5) 0.043(6) -0.010(4) F12 0.116(9) 0.093(7) 0.145(10) 0.013(6) 0.085(8) 0.035(6) F13 0.189(12) 0.162(10) 0.104(6) 0.055(6) -0.044(7) -0.100(8) F10' 0.25(2) 0.27(2) 0.120(14) 0.036(14) 0.087(15) 0.125(18) F11' 0.115(14) 0.28(2) 0.090(9) -0.055(11) 0.072(10) -0.077(13) F12' 0.107(9) 0.137(15) 0.201(17) -0.050(11) 0.092(10) -0.013(10) F13' 0.081(7) 0.32(2) 0.148(13) -0.138(15) 0.072(8) -0.065(10) B2 0.064(3) 0.046(2) 0.047(2) -0.0028(18) 0.026(2) -0.0085(19) F20 0.118(2) 0.0539(14) 0.0646(16) 0.0038(12) 0.0516(16) -0.0099(14) F21 0.0693(18) 0.086(2) 0.087(2) -0.0036(16) 0.0128(15) 0.0065(15) F22 0.0796(17) 0.0589(14) 0.0675(16) -0.0088(12) 0.0247(14) -0.0199(13) F23 0.0808(17) 0.0565(14) 0.0541(14) -0.0031(11) 0.0330(12) 0.0021(12) B3 0.056(11) 0.027(8) 0.055(8) 0.005(5) 0.013(7) 0.020(6) F30 0.136(8) 0.070(4) 0.065(3) -0.016(3) 0.039(4) 0.027(4) F31 0.097(6) 0.080(4) 0.068(4) 0.007(3) -0.006(3) 0.026(3) F32 0.076(5) 0.070(5) 0.099(9) 0.001(5) 0.027(5) -0.021(4) F33 0.063(4) 0.039(5) 0.081(8) 0.000(5) 0.011(4) 0.001(3) B3' 0.050(15) 0.026(15) 0.037(9) 0.010(9) 0.011(9) 0.032(9) F30' 0.14(2) 0.22(2) 0.096(11) -0.094(14) 0.060(13) -0.058(15) F31' 0.062(7) 0.054(9) 0.23(3) 0.052(13) 0.056(13) 0.014(7) F32' 0.126(17) 0.072(13) 0.081(12) -0.032(10) 0.071(12) -0.045(10) F33' 0.071(15) 0.058(14) 0.085(19) 0.033(11) 0.036(14) 0.032(11) N100 0.136(4) 0.069(3) 0.059(2) 0.003(2) 0.034(3) -0.007(3) C100 0.105(4) 0.058(3) 0.058(3) -0.015(2) 0.037(3) -0.014(3) C101 0.100(4) 0.082(4) 0.065(3) 0.003(3) 0.016(3) -0.014(3) N200 0.136(8) 0.140(8) 0.132(8) -0.016(6) 0.045(7) -0.070(7) C200 0.123(9) 0.108(8) 0.122(9) -0.012(7) 0.014(8) -0.067(8) C201 0.217(18) 0.124(11) 0.198(17) -0.044(10) 0.008(14) -0.059(12) O100 0.110(16) 0.112(15) 0.17(2) -0.037(15) 0.014(15) -0.008(12) O200 0.16(2) 0.066(11) 0.18(2) 0.000(12) -0.055(17) 0.027(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1A 2.184(3) . ? Ag1 N6B 2.203(3) 4_666 ? Ag1 N5B 2.551(3) 4_666 ? Ag1 Ag3 3.0692(10) 4_666 ? Ag1 Ag2 3.1437(11) . ? Ag2 N3A 2.245(3) . ? Ag2 N2B 2.299(3) . ? Ag2 N1B 2.460(3) . ? Ag2 N2A 2.613(3) . ? Ag2 N3B 2.614(3) . ? Ag3 N4B 2.229(3) . ? Ag3 N5A 2.283(3) . ? Ag3 N6A 2.493(3) . ? Ag3 N4A 2.524(3) . ? Ag3 Ag1 3.0692(10) 4_565 ? N1A C1A 1.339(4) . ? N1A C5A 1.348(4) . ? N2A C6A 1.342(5) . ? N2A C10A 1.348(4) . ? N3A C11A 1.271(4) . ? N3A C12A 1.465(4) . ? N4A C16A 1.259(5) . ? N4A C15A 1.458(5) . ? N5A C21A 1.334(5) . ? N5A C17A 1.340(6) . ? N6A C26A 1.333(6) . ? N6A C22A 1.344(6) . ? C1A C2A 1.383(5) . ? C1A H1AA 0.9500 . ? C2A C3A 1.377(6) . ? C2A H2AA 0.9500 . ? C3A C4A 1.379(6) . ? C3A H3AA 0.9500 . ? C4A C5A 1.392(5) . ? C4A H4AA 0.9500 . ? C5A C6A 1.487(5) . ? C6A C7A 1.391(5) . ? C7A C8A 1.373(6) . ? C7A H7AA 0.9500 . ? C8A C9A 1.382(6) . ? C8A H8AA 0.9500 . ? C9A C10A 1.386(5) . ? C9A H9AA 0.9500 . ? C10A C11A 1.471(5) . ? C11A H11A 0.9500 . ? C12A C13A 1.511(5) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.512(5) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.525(6) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.469(6) . ? C16A H16A 0.9500 . ? C17A C18A 1.393(6) . ? C18A C19A 1.371(8) . ? C18A H18A 0.9500 . ? C19A C20A 1.357(8) . ? C19A H19A 0.9500 . ? C20A C21A 1.410(6) . ? C20A H20A 0.9500 . ? C21A C22A 1.483(7) . ? C22A C23A 1.392(6) . ? C23A C24A 1.367(10) . ? C23A H23A 0.9500 . ? C24A C25A 1.372(10) . ? C24A H24A 0.9500 . ? C25A C26A 1.398(8) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? N1B C5B 1.336(4) . ? N1B C1B 1.338(5) . ? N2B C6B 1.330(4) . ? N2B C10B 1.344(4) . ? N3B C11B 1.263(5) . ? N3B C12B 1.474(4) . ? N4B C16B 1.271(4) . ? N4B C15B 1.469(4) . ? N5B C21B 1.337(4) . ? N5B C17B 1.351(4) . ? N5B Ag1 2.551(3) 4_565 ? N6B C26B 1.336(4) . ? N6B C22B 1.346(4) . ? N6B Ag1 2.203(3) 4_565 ? C1B C2B 1.376(5) . ? C1B H1BA 0.9500 . ? C2B C3B 1.382(6) . ? C2B H2BA 0.9500 . ? C3B C4B 1.378(6) . ? C3B H3BA 0.9500 . ? C4B C5B 1.389(5) . ? C4B H4BA 0.9500 . ? C5B C6B 1.492(5) . ? C6B C7B 1.399(5) . ? C7B C8B 1.372(6) . ? C7B H7BA 0.9500 . ? C8B C9B 1.381(6) . ? C8B H8BA 0.9500 . ? C9B C10B 1.389(5) . ? C9B H9BA 0.9500 . ? C10B C11B 1.472(5) . ? C11B H11B 0.9500 . ? C12B C13B 1.516(5) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.513(5) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.525(5) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17B 1.472(5) . ? C16B H16B 0.9500 . ? C17B C18B 1.383(5) . ? C18B C19B 1.388(5) . ? C18B H18B 0.9500 . ? C19B C20B 1.375(5) . ? C19B H19B 0.9500 . ? C20B C21B 1.398(5) . ? C20B H20B 0.9500 . ? C21B C22B 1.489(4) . ? C22B C23B 1.387(5) . ? C23B C24B 1.383(5) . ? C23B H23B 0.9500 . ? C24B C25B 1.376(6) . ? C24B H24B 0.9500 . ? C25B C26B 1.385(5) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? B1 F12' 1.14(2) . ? B1 F11' 1.30(2) . ? B1 F10 1.296(12) . ? B1 F13' 1.345(14) . ? B1 F11 1.348(15) . ? B1 F12 1.443(14) . ? B1 F13 1.447(12) . ? B1 F10' 1.48(2) . ? B2 F20 1.377(5) . ? B2 F22 1.384(5) . ? B2 F21 1.388(6) . ? B2 F23 1.390(5) . ? B3 F31 1.29(3) . ? B3 F30 1.35(3) . ? B3 F32 1.36(3) . ? B3 F33 1.43(3) . ? B3' F33' 1.22(7) . ? B3' F30' 1.38(6) . ? B3' F32' 1.44(7) . ? B3' F31' 1.58(4) . ? N100 C100 1.104(6) . ? C100 C101 1.439(7) . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? N200 C200 1.026(15) . ? C200 C201 1.391(19) . ? C201 H20C 0.9800 . ? C201 H20D 0.9800 . ? C201 H20E 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 N1A Ag1 N6B 147.24(10) . 4_666 ? N1A Ag1 N5B 140.18(9) . 4_666 ? N6B Ag1 N5B 70.31(9) 4_666 4_666 ? N1A Ag1 Ag3 100.69(7) . 4_666 ? N6B Ag1 Ag3 86.45(7) 4_666 4_666 ? N5B Ag1 Ag3 58.48(6) 4_666 4_666 ? N1A Ag1 Ag2 80.40(7) . . ? N6B Ag1 Ag2 104.66(8) 4_666 . ? N5B Ag1 Ag2 106.80(6) 4_666 . ? Ag3 Ag1 Ag2 157.923(16) 4_666 . ? N3A Ag2 N2B 177.23(10) . . ? N3A Ag2 N1B 110.35(10) . . ? N2B Ag2 N1B 69.10(10) . . ? N3A Ag2 N2A 69.54(10) . . ? N2B Ag2 N2A 112.85(9) . . ? N1B Ag2 N2A 135.22(10) . . ? N3A Ag2 N3B 111.03(10) . . ? N2B Ag2 N3B 68.85(10) . . ? N1B Ag2 N3B 136.07(9) . . ? N2A Ag2 N3B 74.27(9) . . ? N3A Ag2 Ag1 87.58(7) . . ? N2B Ag2 Ag1 94.97(7) . . ? N1B Ag2 Ag1 80.47(8) . . ? N2A Ag2 Ag1 54.81(6) . . ? N3B Ag2 Ag1 115.25(6) . . ? N4B Ag3 N5A 177.05(11) . . ? N4B Ag3 N6A 113.82(11) . . ? N5A Ag3 N6A 68.42(12) . . ? N4B Ag3 N4A 108.23(11) . . ? N5A Ag3 N4A 70.09(12) . . ? N6A Ag3 N4A 135.84(11) . . ? N4B Ag3 Ag1 85.49(7) . 4_565 ? N5A Ag3 Ag1 91.93(8) . 4_565 ? N6A Ag3 Ag1 110.40(8) . 4_565 ? N4A Ag3 Ag1 85.25(7) . 4_565 ? C1A N1A C5A 118.9(3) . . ? C1A N1A Ag1 120.7(2) . . ? C5A N1A Ag1 120.4(2) . . ? C6A N2A C10A 118.6(3) . . ? C6A N2A Ag2 128.1(2) . . ? C10A N2A Ag2 104.6(2) . . ? C11A N3A C12A 118.5(3) . . ? C11A N3A Ag2 119.0(2) . . ? C12A N3A Ag2 122.4(2) . . ? C16A N4A C15A 118.9(4) . . ? C16A N4A Ag3 110.1(3) . . ? C15A N4A Ag3 129.7(3) . . ? C21A N5A C17A 119.8(3) . . ? C21A N5A Ag3 121.9(3) . . ? C17A N5A Ag3 118.3(3) . . ? C26A N6A C22A 118.2(4) . . ? C26A N6A Ag3 125.7(3) . . ? C22A N6A Ag3 113.9(3) . . ? N1A C1A C2A 122.5(4) . . ? N1A C1A H1AA 118.7 . . ? C2A C1A H1AA 118.7 . . ? C3A C2A C1A 118.8(4) . . ? C3A C2A H2AA 120.6 . . ? C1A C2A H2AA 120.6 . . ? C2A C3A C4A 119.2(4) . . ? C2A C3A H3AA 120.4 . . ? C4A C3A H3AA 120.4 . . ? C3A C4A C5A 119.4(4) . . ? C3A C4A H4AA 120.3 . . ? C5A C4A H4AA 120.3 . . ? N1A C5A C4A 121.1(3) . . ? N1A C5A C6A 118.0(3) . . ? C4A C5A C6A 120.8(3) . . ? N2A C6A C7A 121.9(3) . . ? N2A C6A C5A 115.8(3) . . ? C7A C6A C5A 122.2(3) . . ? C8A C7A C6A 119.1(4) . . ? C8A C7A H7AA 120.5 . . ? C6A C7A H7AA 120.5 . . ? C7A C8A C9A 119.4(3) . . ? C7A C8A H8AA 120.3 . . ? C9A C8A H8AA 120.3 . . ? C8A C9A C10A 118.7(4) . . ? C8A C9A H9AA 120.6 . . ? C10A C9A H9AA 120.6 . . ? N2A C10A C9A 122.2(3) . . ? N2A C10A C11A 117.5(3) . . ? C9A C10A C11A 120.3(3) . . ? N3A C11A C10A 122.0(3) . . ? N3A C11A H11A 119.0 . . ? C10A C11A H11A 119.0 . . ? N3A C12A C13A 112.6(3) . . ? N3A C12A H12A 109.1 . . ? C13A C12A H12A 109.1 . . ? N3A C12A H12B 109.1 . . ? C13A C12A H12B 109.1 . . ? H12A C12A H12B 107.8 . . ? C12A C13A C14A 113.9(3) . . ? C12A C13A H13A 108.8 . . ? C14A C13A H13A 108.8 . . ? C12A C13A H13B 108.8 . . ? C14A C13A H13B 108.8 . . ? H13A C13A H13B 107.7 . . ? C13A C14A C15A 111.7(3) . . ? C13A C14A H14A 109.3 . . ? C15A C14A H14A 109.3 . . ? C13A C14A H14B 109.3 . . ? C15A C14A H14B 109.3 . . ? H14A C14A H14B 107.9 . . ? N4A C15A C14A 111.5(3) . . ? N4A C15A H15A 109.3 . . ? C14A C15A H15A 109.3 . . ? N4A C15A H15B 109.3 . . ? C14A C15A H15B 109.3 . . ? H15A C15A H15B 108.0 . . ? N4A C16A C17A 122.2(4) . . ? N4A C16A H16A 118.9 . . ? C17A C16A H16A 118.9 . . ? N5A C17A C18A 121.8(5) . . ? N5A C17A C16A 117.6(3) . . ? C18A C17A C16A 120.6(5) . . ? C19A C18A C17A 118.8(5) . . ? C19A C18A H18A 120.6 . . ? C17A C18A H18A 120.6 . . ? C20A C19A C18A 119.3(4) . . ? C20A C19A H19A 120.3 . . ? C18A C19A H19A 120.3 . . ? C19A C20A C21A 120.2(5) . . ? C19A C20A H20A 119.9 . . ? C21A C20A H20A 119.9 . . ? N5A C21A C20A 120.1(5) . . ? N5A C21A C22A 117.0(3) . . ? C20A C21A C22A 122.9(4) . . ? N6A C22A C23A 121.6(5) . . ? N6A C22A C21A 116.2(4) . . ? C23A C22A C21A 122.2(5) . . ? C24A C23A C22A 119.8(6) . . ? C24A C23A H23A 120.1 . . ? C22A C23A H23A 120.1 . . ? C23A C24A C25A 119.1(6) . . ? C23A C24A H24A 120.4 . . ? C25A C24A H24A 120.4 . . ? C24A C25A C26A 118.4(6) . . ? C24A C25A H25A 120.8 . . ? C26A C25A H25A 120.8 . . ? N6A C26A C25A 122.9(6) . . ? N6A C26A H26A 118.6 . . ? C25A C26A H26A 118.6 . . ? C5B N1B C1B 118.6(3) . . ? C5B N1B Ag2 115.4(2) . . ? C1B N1B Ag2 125.9(2) . . ? C6B N2B C10B 119.9(3) . . ? C6B N2B Ag2 120.6(2) . . ? C10B N2B Ag2 119.0(2) . . ? C11B N3B C12B 116.8(3) . . ? C11B N3B Ag2 108.4(2) . . ? C12B N3B Ag2 131.5(2) . . ? C16B N4B C15B 118.4(3) . . ? C16B N4B Ag3 121.6(2) . . ? C15B N4B Ag3 118.1(2) . . ? C21B N5B C17B 118.4(3) . . ? C21B N5B Ag1 104.5(2) . 4_565 ? C17B N5B Ag1 127.1(2) . 4_565 ? C26B N6B C22B 118.5(3) . . ? C26B N6B Ag1 122.1(3) . 4_565 ? C22B N6B Ag1 119.4(2) . 4_565 ? N1B C1B C2B 123.6(3) . . ? N1B C1B H1BA 118.2 . . ? C2B C1B H1BA 118.2 . . ? C1B C2B C3B 117.8(4) . . ? C1B C2B H2BA 121.1 . . ? C3B C2B H2BA 121.1 . . ? C4B C3B C2B 119.2(3) . . ? C4B C3B H3BA 120.4 . . ? C2B C3B H3BA 120.4 . . ? C3B C4B C5B 119.7(3) . . ? C3B C4B H4BA 120.2 . . ? C5B C4B H4BA 120.2 . . ? N1B C5B C4B 121.1(3) . . ? N1B C5B C6B 116.5(3) . . ? C4B C5B C6B 122.3(3) . . ? N2B C6B C7B 120.5(3) . . ? N2B C6B C5B 117.4(3) . . ? C7B C6B C5B 122.1(3) . . ? C8B C7B C6B 119.7(3) . . ? C8B C7B H7BA 120.1 . . ? C6B C7B H7BA 120.1 . . ? C7B C8B C9B 119.7(3) . . ? C7B C8B H8BA 120.2 . . ? C9B C8B H8BA 120.2 . . ? C8B C9B C10B 117.9(4) . . ? C8B C9B H9BA 121.1 . . ? C10B C9B H9BA 121.1 . . ? N2B C10B C9B 122.3(3) . . ? N2B C10B C11B 118.2(3) . . ? C9B C10B C11B 119.5(3) . . ? N3B C11B C10B 122.4(3) . . ? N3B C11B H11B 118.8 . . ? C10B C11B H11B 118.8 . . ? N3B C12B C13B 110.5(3) . . ? N3B C12B H12C 109.5 . . ? C13B C12B H12C 109.5 . . ? N3B C12B H12D 109.5 . . ? C13B C12B H12D 109.5 . . ? H12C C12B H12D 108.1 . . ? C14B C13B C12B 113.1(3) . . ? C14B C13B H13C 109.0 . . ? C12B C13B H13C 109.0 . . ? C14B C13B H13D 109.0 . . ? C12B C13B H13D 109.0 . . ? H13C C13B H13D 107.8 . . ? C13B C14B C15B 113.4(3) . . ? C13B C14B H14C 108.9 . . ? C15B C14B H14C 108.9 . . ? C13B C14B H14D 108.9 . . ? C15B C14B H14D 108.9 . . ? H14C C14B H14D 107.7 . . ? N4B C15B C14B 108.8(3) . . ? N4B C15B H15C 109.9 . . ? C14B C15B H15C 109.9 . . ? N4B C15B H15D 109.9 . . ? C14B C15B H15D 109.9 . . ? H15C C15B H15D 108.3 . . ? N4B C16B C17B 122.9(3) . . ? N4B C16B H16B 118.5 . . ? C17B C16B H16B 118.5 . . ? N5B C17B C18B 122.4(3) . . ? N5B C17B C16B 118.6(3) . . ? C18B C17B C16B 119.0(3) . . ? C17B C18B C19B 118.8(3) . . ? C17B C18B H18B 120.6 . . ? C19B C18B H18B 120.6 . . ? C20B C19B C18B 119.2(3) . . ? C20B C19B H19B 120.4 . . ? C18B C19B H19B 120.4 . . ? C19B C20B C21B 118.9(3) . . ? C19B C20B H20B 120.5 . . ? C21B C20B H20B 120.5 . . ? N5B C21B C20B 122.2(3) . . ? N5B C21B C22B 116.4(3) . . ? C20B C21B C22B 121.4(3) . . ? N6B C22B C23B 122.1(3) . . ? N6B C22B C21B 117.1(3) . . ? C23B C22B C21B 120.8(3) . . ? C24B C23B C22B 118.8(4) . . ? C24B C23B H23B 120.6 . . ? C22B C23B H23B 120.6 . . ? C25B C24B C23B 119.4(4) . . ? C25B C24B H24B 120.3 . . ? C23B C24B H24B 120.3 . . ? C24B C25B C26B 118.7(4) . . ? C24B C25B H25B 120.7 . . ? C26B C25B H25B 120.7 . . ? N6B C26B C25B 122.7(4) . . ? N6B C26B H26B 118.7 . . ? C25B C26B H26B 118.7 . . ? F12' B1 F11' 124.9(17) . . ? F12' B1 F10 97.8(14) . . ? F11' B1 F10 133.4(16) . . ? F12' B1 F13' 121.2(13) . . ? F11' B1 F13' 94.9(12) . . ? F10 B1 F13' 74.5(13) . . ? F12' B1 F11 132.3(13) . . ? F10 B1 F11 118.4(10) . . ? F13' B1 F11 98.9(8) . . ? F11' B1 F12 103.3(12) . . ? F10 B1 F12 109.4(9) . . ? F13' B1 F12 147.5(11) . . ? F11 B1 F12 106.4(9) . . ? F12' B1 F13 82.4(15) . . ? F11' B1 F13 94.4(15) . . ? F10 B1 F13 110.3(7) . . ? F13' B1 F13 50.0(9) . . ? F11 B1 F13 109.6(11) . . ? F12 B1 F13 101.4(11) . . ? F12' B1 F10' 106.9(16) . . ? F11' B1 F10' 106.0(17) . . ? F13' B1 F10' 99.4(14) . . ? F11 B1 F10' 89.1(14) . . ? F12 B1 F10' 101.0(10) . . ? F13 B1 F10' 145.1(14) . . ? F20 B2 F22 109.7(4) . . ? F20 B2 F21 110.4(4) . . ? F22 B2 F21 108.4(4) . . ? F20 B2 F23 109.1(4) . . ? F22 B2 F23 109.8(3) . . ? F21 B2 F23 109.4(4) . . ? F31 B3 F30 115.2(15) . . ? F31 B3 F32 111(2) . . ? F30 B3 F32 113(2) . . ? F31 B3 F33 102(2) . . ? F30 B3 F33 110(2) . . ? F32 B3 F33 104.8(17) . . ? F33' B3' F30' 112(4) . . ? F33' B3' F32' 126(4) . . ? F30' B3' F32' 98(5) . . ? F33' B3' F31' 117(5) . . ? F30' B3' F31' 97(3) . . ? F32' B3' F31' 102(3) . . ? N100 C100 C101 171.6(7) . . ? C100 C101 H10C 109.5 . . ? C100 C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? C100 C101 H10E 109.5 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? N200 C200 C201 161.0(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.535 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.073 # Attachment '- GQ144.CIF' data_gq144 _database_code_depnum_ccdc_archive 'CCDC 774875' #TrackingRef '- GQ144.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H64 Ag4 N24, 4(B F4), 3(H2 O)' _chemical_formula_sum 'C88 H70 Ag4 B4 F16 N24 O3' _chemical_formula_weight 2290.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1675(15) _cell_length_b 13.4693(16) _cell_length_c 13.8590(17) _cell_angle_alpha 66.869(9) _cell_angle_beta 81.171(10) _cell_angle_gamma 89.390(10) _cell_volume 2230.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15050 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 46.39 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; One peak of residual electron density of 3.60eA-3 lies 0.899A from Ag2 and results from fourier truncation surrounding the heavy atom and therefore remains unassigned. The data from this crystal was less than perfect, but attempts to collect better data from other crystals was unsuccessful. ; _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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48929 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7765 _reflns_number_gt 7308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+8.2714P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7765 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.44955(3) -0.30164(4) 0.66632(3) 0.05252(17) Uani 1 1 d . . . Ag2 Ag 0.74543(4) 0.09311(4) 0.48432(4) 0.06085(19) Uani 1 1 d . . . N1 N 0.3578(4) -0.4464(4) 0.6185(5) 0.0573(12) Uani 1 1 d . . . N2 N 0.4738(3) -0.2657(4) 0.4808(4) 0.0439(10) Uani 1 1 d . . . N3 N 0.5609(3) -0.1366(4) 0.5618(4) 0.0438(10) Uani 1 1 d . . . N4 N 0.6130(3) -0.0640(4) 0.5903(4) 0.0448(10) Uani 1 1 d . . . N5 N 0.7092(3) 0.0654(4) 0.6624(4) 0.0530(12) Uani 1 1 d . . . N6 N 0.8205(4) 0.2406(5) 0.5132(5) 0.0603(14) Uani 1 1 d . . . C1 C 0.3100(5) -0.5387(6) 0.6884(7) 0.0680(17) Uani 1 1 d . . . H1A H 0.2927 -0.5473 0.7605 0.082 Uiso 1 1 calc R . . C2 C 0.2839(5) -0.6232(6) 0.6618(7) 0.071(2) Uani 1 1 d . . . H2A H 0.2486 -0.6875 0.7140 0.085 Uiso 1 1 calc R . . C3 C 0.3101(5) -0.6115(6) 0.5595(8) 0.075(2) Uani 1 1 d . . . H3A H 0.2940 -0.6683 0.5390 0.090 Uiso 1 1 calc R . . C4 C 0.3600(5) -0.5169(6) 0.4852(7) 0.0660(18) Uani 1 1 d . . . H4A H 0.3792 -0.5076 0.4131 0.079 Uiso 1 1 calc R . . C5 C 0.3821(4) -0.4345(5) 0.5180(6) 0.0550(15) Uani 1 1 d . . . C6 C 0.4347(4) -0.3292(5) 0.4402(5) 0.0510(13) Uani 1 1 d . . . C7 C 0.4437(5) -0.2982(6) 0.3312(6) 0.0626(17) Uani 1 1 d . . . H7A H 0.4139 -0.3431 0.3035 0.075 Uiso 1 1 calc R . . C8 C 0.4955(5) -0.2031(7) 0.2637(6) 0.0666(18) Uani 1 1 d . . . H8A H 0.5024 -0.1816 0.1890 0.080 Uiso 1 1 calc R . . C9 C 0.5382(4) -0.1375(6) 0.3058(5) 0.0554(14) Uani 1 1 d . . . H9A H 0.5754 -0.0713 0.2609 0.066 Uiso 1 1 calc R . . C10 C 0.5242(4) -0.1727(5) 0.4147(5) 0.0460(12) Uani 1 1 d . . . C11 C 0.5696(4) -0.1065(4) 0.4618(4) 0.0425(11) Uani 1 1 d . . . H11A H 0.6061 -0.0400 0.4165 0.051 Uiso 1 1 calc R . . C12 C 0.6068(4) -0.0942(5) 0.6901(5) 0.0505(13) Uani 1 1 d . . . H12A H 0.5690 -0.1593 0.7372 0.061 Uiso 1 1 calc R . . C13 C 0.6590(4) -0.0270(6) 0.7324(5) 0.0569(15) Uani 1 1 d . . . C14 C 0.6546(5) -0.0597(7) 0.8392(6) 0.0721(19) Uani 1 1 d . . . H14A H 0.6172 -0.1244 0.8879 0.087 Uiso 1 1 calc R . . C15 C 0.7077(7) 0.0064(9) 0.8745(7) 0.089(3) Uani 1 1 d . . . H15A H 0.7084 -0.0145 0.9483 0.107 Uiso 1 1 calc R . . C16 C 0.7584(6) 0.1012(8) 0.8021(7) 0.079(2) Uani 1 1 d . . . H16A H 0.7938 0.1465 0.8253 0.095 Uiso 1 1 calc R . . C17 C 0.7572(5) 0.1294(6) 0.6961(6) 0.0637(18) Uani 1 1 d . . . C18 C 0.8077(4) 0.2322(6) 0.6123(6) 0.0623(17) Uani 1 1 d . . . C19 C 0.8392(5) 0.3192(8) 0.6377(8) 0.082(3) Uani 1 1 d . . . H19A H 0.8317 0.3129 0.7092 0.099 Uiso 1 1 calc R . . C20 C 0.8809(5) 0.4123(7) 0.5544(9) 0.083(3) Uani 1 1 d . . . H20A H 0.9016 0.4718 0.5688 0.099 Uiso 1 1 calc R . . C21 C 0.8930(5) 0.4214(7) 0.4537(8) 0.078(2) Uani 1 1 d . . . H21A H 0.9221 0.4859 0.3966 0.094 Uiso 1 1 calc R . . C22 C 0.8615(5) 0.3330(6) 0.4357(7) 0.0679(18) Uani 1 1 d . . . H22A H 0.8695 0.3386 0.3644 0.081 Uiso 1 1 calc R . . N7 N 0.2857(4) -0.2503(4) 0.7493(4) 0.0496(11) Uani 1 1 d . . . N8 N 0.3874(4) -0.4240(4) 0.8449(4) 0.0520(11) Uani 1 1 d . . . N9 N 0.5851(4) -0.4104(5) 0.7584(4) 0.0579(12) Uani 1 1 d . . . C23 C 0.2352(4) -0.3252(5) 0.8288(5) 0.0537(14) Uani 1 1 d . . . H23A H 0.1651 -0.3177 0.8529 0.064 Uiso 1 1 calc R . . C24 C 0.2871(4) -0.4249(5) 0.8837(5) 0.0535(14) Uani 1 1 d . . . C25 C 0.2356(5) -0.5121(6) 0.9667(5) 0.0652(17) Uani 1 1 d . . . H25A H 0.1646 -0.5107 0.9923 0.078 Uiso 1 1 calc R . . C26 C 0.2911(6) -0.6027(7) 1.0123(6) 0.077(2) Uani 1 1 d . . . H26A H 0.2580 -0.6649 1.0697 0.092 Uiso 1 1 calc R . . C27 C 0.3941(5) -0.6016(6) 0.9738(6) 0.0711(19) Uani 1 1 d . . . H27A H 0.4326 -0.6630 1.0046 0.085 Uiso 1 1 calc R . . C28 C 0.4413(5) -0.5102(5) 0.8895(5) 0.0566(14) Uani 1 1 d . . . C29 C 0.5525(4) -0.5017(5) 0.8428(5) 0.0541(14) Uani 1 1 d . . . C30 C 0.6186(5) -0.5807(6) 0.8855(6) 0.0634(16) Uani 1 1 d . . . H30A H 0.5935 -0.6445 0.9459 0.076 Uiso 1 1 calc R . . C31 C 0.7216(5) -0.5678(6) 0.8408(6) 0.0667(17) Uani 1 1 d . . . H31A H 0.7675 -0.6230 0.8685 0.080 Uiso 1 1 calc R . . C32 C 0.7560(5) -0.4733(6) 0.7554(5) 0.0628(16) Uani 1 1 d . . . H32A H 0.8266 -0.4608 0.7241 0.075 Uiso 1 1 calc R . . C33 C 0.6858(5) -0.3974(6) 0.7163(5) 0.0635(16) Uani 1 1 d . . . H33A H 0.7095 -0.3326 0.6566 0.076 Uiso 1 1 calc R . . N10 N 0.7620(3) 0.1568(4) 0.3039(4) 0.0498(11) Uani 1 1 d . . . N11 N 0.8454(3) -0.0333(4) 0.4164(4) 0.0478(11) Uani 1 1 d . . . N12 N 0.9164(4) -0.2540(4) 0.6413(5) 0.0623(13) Uani 1 1 d . . . C34 C 0.7903(4) 0.0941(5) 0.2572(5) 0.0523(13) Uani 1 1 d . . . H34A H 0.7824 0.1138 0.1851 0.063 Uiso 1 1 calc R . . C35 C 0.8356(4) -0.0092(5) 0.3147(5) 0.0524(13) Uani 1 1 d . . . C36 C 0.8671(5) -0.0760(6) 0.2619(6) 0.0615(16) Uani 1 1 d . . . H36A H 0.8587 -0.0567 0.1900 0.074 Uiso 1 1 calc R . . C37 C 0.9112(5) -0.1715(6) 0.3169(6) 0.0654(17) Uani 1 1 d . . . H37A H 0.9344 -0.2186 0.2829 0.079 Uiso 1 1 calc R . . C38 C 0.9210(4) -0.1972(5) 0.4208(6) 0.0574(15) Uani 1 1 d . . . H38A H 0.9497 -0.2631 0.4599 0.069 Uiso 1 1 calc R . . C39 C 0.8882(4) -0.1258(5) 0.4698(5) 0.0494(13) Uani 1 1 d . . . C40 C 0.9035(4) -0.1488(5) 0.5800(5) 0.0506(13) Uani 1 1 d . . . C41 C 0.9070(4) -0.0686(5) 0.6170(5) 0.0535(14) Uani 1 1 d . . . H41A H 0.8981 0.0042 0.5724 0.064 Uiso 1 1 calc R . . C42 C 0.9235(5) -0.0949(6) 0.7196(6) 0.0641(17) Uani 1 1 d . . . H42A H 0.9259 -0.0403 0.7466 0.077 Uiso 1 1 calc R . . C43 C 0.9366(5) -0.2007(6) 0.7827(6) 0.0655(17) Uani 1 1 d . . . H43A H 0.9475 -0.2206 0.8539 0.079 Uiso 1 1 calc R . . C44 C 0.9333(5) -0.2771(6) 0.7401(6) 0.0683(17) Uani 1 1 d . . . H44A H 0.9437 -0.3500 0.7833 0.082 Uiso 1 1 calc R . . B1 B 0.6225(7) 0.1376(8) 0.0514(7) 0.075(2) Uani 1 1 d . . . F10 F 0.7158(3) 0.1950(4) 0.0058(4) 0.0882(13) Uani 1 1 d . . . F11 F 0.5791(4) 0.1681(6) 0.1297(5) 0.126(2) Uani 1 1 d . . . F12 F 0.5602(4) 0.1577(5) -0.0232(4) 0.0989(15) Uani 1 1 d . . . F13 F 0.6420(5) 0.0288(4) 0.0941(4) 0.1151(19) Uani 1 1 d . . . B2 B 1.0217(7) -0.6130(9) 0.8630(9) 0.088(3) Uani 1 1 d . . . F20 F 1.1056(4) -0.6752(5) 0.8750(6) 0.131(2) Uani 1 1 d . . . F21 F 0.9608(5) -0.6368(8) 0.9568(6) 0.156(3) Uani 1 1 d . . . F22 F 1.0609(6) -0.5071(6) 0.8196(6) 0.141(2) Uani 1 1 d . . . F23 F 0.9720(6) -0.6325(8) 0.7942(7) 0.160(3) Uani 1 1 d . . . O1 O -0.0776(9) -0.1080(10) -0.0250(9) 0.137(4) Uani 0.75 1 d P . . O2 O 0.1110(10) -0.0779(10) -0.0055(9) 0.140(4) Uani 0.75 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0488(3) 0.0569(3) 0.0463(3) -0.0153(2) -0.00471(18) -0.00375(19) Ag2 0.0741(3) 0.0596(3) 0.0542(3) -0.0298(2) -0.0059(2) -0.0009(2) N1 0.047(3) 0.060(3) 0.072(3) -0.033(3) -0.010(2) 0.000(2) N2 0.031(2) 0.055(3) 0.054(3) -0.030(2) -0.0062(18) 0.0044(18) N3 0.038(2) 0.047(2) 0.048(3) -0.022(2) -0.0064(18) 0.0029(18) N4 0.039(2) 0.053(3) 0.047(3) -0.026(2) -0.0060(19) 0.0027(19) N5 0.037(2) 0.076(3) 0.064(3) -0.046(3) -0.012(2) 0.007(2) N6 0.042(3) 0.072(4) 0.087(4) -0.051(3) -0.015(3) 0.005(2) C1 0.058(4) 0.060(4) 0.084(5) -0.027(4) -0.011(3) -0.005(3) C2 0.047(3) 0.058(4) 0.114(6) -0.041(4) -0.013(4) -0.003(3) C3 0.042(3) 0.070(4) 0.133(7) -0.062(5) -0.016(4) 0.002(3) C4 0.044(3) 0.083(5) 0.097(5) -0.064(4) -0.009(3) 0.007(3) C5 0.032(3) 0.063(4) 0.084(4) -0.042(3) -0.012(3) 0.006(2) C6 0.034(3) 0.069(4) 0.065(4) -0.042(3) -0.009(2) 0.008(2) C7 0.043(3) 0.094(5) 0.072(4) -0.055(4) -0.012(3) 0.008(3) C8 0.054(4) 0.107(6) 0.053(4) -0.046(4) -0.012(3) 0.020(4) C9 0.045(3) 0.075(4) 0.049(3) -0.028(3) -0.007(2) 0.007(3) C10 0.032(2) 0.061(3) 0.051(3) -0.029(3) -0.005(2) 0.009(2) C11 0.037(2) 0.047(3) 0.043(3) -0.018(2) -0.005(2) 0.003(2) C12 0.040(3) 0.064(3) 0.051(3) -0.027(3) -0.006(2) 0.006(2) C13 0.044(3) 0.086(5) 0.056(3) -0.043(3) -0.012(3) 0.014(3) C14 0.061(4) 0.110(6) 0.057(4) -0.044(4) -0.011(3) 0.009(4) C15 0.085(5) 0.152(9) 0.062(5) -0.070(6) -0.024(4) 0.029(6) C16 0.068(4) 0.118(7) 0.077(5) -0.063(5) -0.016(4) 0.003(4) C17 0.044(3) 0.098(5) 0.079(4) -0.064(4) -0.018(3) 0.020(3) C18 0.033(3) 0.078(4) 0.098(5) -0.058(4) -0.013(3) 0.007(3) C19 0.045(3) 0.118(7) 0.131(7) -0.097(6) -0.023(4) 0.020(4) C20 0.037(3) 0.079(5) 0.151(9) -0.070(6) -0.006(4) -0.006(3) C21 0.046(3) 0.078(5) 0.127(7) -0.058(5) -0.013(4) 0.003(3) C22 0.044(3) 0.063(4) 0.104(6) -0.039(4) -0.016(3) 0.001(3) N7 0.046(2) 0.058(3) 0.048(3) -0.024(2) -0.010(2) 0.007(2) N8 0.042(2) 0.060(3) 0.048(3) -0.015(2) -0.004(2) 0.001(2) N9 0.042(2) 0.072(3) 0.049(3) -0.012(2) -0.008(2) 0.000(2) C23 0.038(3) 0.069(4) 0.056(3) -0.026(3) -0.008(2) 0.005(3) C24 0.043(3) 0.067(4) 0.047(3) -0.019(3) -0.006(2) 0.001(3) C25 0.047(3) 0.082(5) 0.054(4) -0.016(3) -0.001(3) 0.001(3) C26 0.063(4) 0.077(5) 0.062(4) -0.003(4) 0.004(3) -0.005(3) C27 0.051(3) 0.072(4) 0.068(4) -0.006(3) -0.003(3) 0.005(3) C28 0.047(3) 0.065(4) 0.050(3) -0.014(3) -0.006(3) 0.007(3) C29 0.048(3) 0.061(4) 0.049(3) -0.017(3) -0.009(2) 0.002(3) C30 0.051(3) 0.068(4) 0.065(4) -0.020(3) -0.008(3) 0.011(3) C31 0.055(4) 0.070(4) 0.071(4) -0.025(4) -0.009(3) 0.014(3) C32 0.043(3) 0.085(5) 0.062(4) -0.033(4) 0.000(3) 0.004(3) C33 0.048(3) 0.077(4) 0.054(4) -0.016(3) -0.004(3) -0.003(3) N10 0.043(2) 0.058(3) 0.052(3) -0.025(2) -0.009(2) 0.006(2) N11 0.033(2) 0.054(3) 0.063(3) -0.031(2) -0.0041(19) 0.0040(19) N12 0.054(3) 0.060(3) 0.071(4) -0.025(3) -0.008(3) 0.009(2) C34 0.037(3) 0.071(4) 0.055(3) -0.033(3) -0.003(2) 0.003(2) C35 0.036(3) 0.064(4) 0.064(4) -0.035(3) -0.002(2) 0.002(2) C36 0.050(3) 0.072(4) 0.076(4) -0.046(4) -0.005(3) 0.001(3) C37 0.054(3) 0.066(4) 0.093(5) -0.051(4) -0.005(3) 0.003(3) C38 0.041(3) 0.054(3) 0.085(5) -0.037(3) -0.007(3) 0.004(2) C39 0.031(2) 0.052(3) 0.068(4) -0.028(3) -0.001(2) 0.000(2) C40 0.029(2) 0.055(3) 0.065(4) -0.023(3) 0.000(2) 0.001(2) C41 0.035(3) 0.055(3) 0.070(4) -0.028(3) 0.002(2) -0.001(2) C42 0.043(3) 0.079(4) 0.076(4) -0.041(4) 0.001(3) -0.003(3) C43 0.041(3) 0.087(5) 0.069(4) -0.030(4) -0.012(3) 0.007(3) C44 0.061(4) 0.069(4) 0.069(4) -0.020(4) -0.014(3) 0.014(3) B1 0.076(5) 0.085(6) 0.065(5) -0.031(5) -0.009(4) 0.004(4) F10 0.068(3) 0.092(3) 0.088(3) -0.019(3) -0.011(2) 0.011(2) F11 0.082(3) 0.212(7) 0.139(5) -0.137(5) 0.011(3) -0.019(4) F12 0.109(4) 0.114(4) 0.087(3) -0.045(3) -0.039(3) 0.005(3) F13 0.176(6) 0.087(3) 0.060(3) -0.009(2) -0.009(3) 0.010(4) B2 0.056(5) 0.096(7) 0.100(7) -0.027(6) -0.014(5) 0.013(5) F20 0.066(3) 0.108(4) 0.190(7) -0.031(4) -0.013(3) 0.018(3) F21 0.108(5) 0.238(9) 0.128(6) -0.088(6) 0.006(4) 0.031(5) F22 0.181(7) 0.101(5) 0.149(6) -0.046(4) -0.061(5) 0.032(4) F23 0.109(5) 0.254(10) 0.177(7) -0.134(7) -0.063(5) 0.042(5) O1 0.140(9) 0.161(10) 0.110(8) -0.043(7) -0.053(7) 0.051(8) O2 0.164(10) 0.154(10) 0.112(8) -0.054(7) -0.052(7) 0.075(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N8 2.390(5) . ? Ag1 N2 2.391(5) . ? Ag1 N3 2.465(5) . ? Ag1 N9 2.477(5) . ? Ag1 N7 2.507(5) . ? Ag2 N10 2.277(5) . ? Ag2 N5 2.318(5) . ? Ag2 N6 2.424(5) . ? Ag2 N11 2.519(4) . ? Ag2 N4 2.554(5) . ? N1 C5 1.325(9) . ? N1 C1 1.328(9) . ? N2 C10 1.333(7) . ? N2 C6 1.339(7) . ? N3 C11 1.268(7) . ? N3 N4 1.409(7) . ? N4 C12 1.269(7) . ? N5 C17 1.334(8) . ? N5 C13 1.342(9) . ? N6 C18 1.317(9) . ? N6 C22 1.334(9) . ? C1 C2 1.389(10) . ? C1 H1A 0.9500 . ? C2 C3 1.353(12) . ? C2 H2A 0.9500 . ? C3 C4 1.377(11) . ? C3 H3A 0.9500 . ? C4 C5 1.403(8) . ? C4 H4A 0.9500 . ? C5 C6 1.498(9) . ? C6 C7 1.386(9) . ? C7 C8 1.365(11) . ? C7 H7A 0.9500 . ? C8 C9 1.396(10) . ? C8 H8A 0.9500 . ? C9 C10 1.376(8) . ? C9 H9A 0.9500 . ? C10 C11 1.472(8) . ? C11 H11A 0.9500 . ? C12 C13 1.479(8) . ? C12 H12A 0.9500 . ? C13 C14 1.360(9) . ? C14 C15 1.408(12) . ? C14 H14A 0.9500 . ? C15 C16 1.375(13) . ? C15 H15A 0.9500 . ? C16 C17 1.367(11) . ? C16 H16A 0.9500 . ? C17 C18 1.492(11) . ? C18 C19 1.432(10) . ? C19 C20 1.374(13) . ? C19 H19A 0.9500 . ? C20 C21 1.336(13) . ? C20 H20A 0.9500 . ? C21 C22 1.389(10) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? N7 C23 1.261(8) . ? N7 N10 1.385(7) 2_656 ? N8 C28 1.336(8) . ? N8 C24 1.347(7) . ? N9 C29 1.338(8) . ? N9 C33 1.348(8) . ? C23 C24 1.479(9) . ? C23 H23A 0.9500 . ? C24 C25 1.370(9) . ? C25 C26 1.392(10) . ? C25 H25A 0.9500 . ? C26 C27 1.378(10) . ? C26 H26A 0.9500 . ? C27 C28 1.389(9) . ? C27 H27A 0.9500 . ? C28 C29 1.494(8) . ? C29 C30 1.373(9) . ? C30 C31 1.385(9) . ? C30 H30A 0.9500 . ? C31 C32 1.375(10) . ? C31 H31A 0.9500 . ? C32 C33 1.375(10) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? N10 C34 1.273(7) . ? N10 N7 1.385(7) 2_656 ? N11 C35 1.343(8) . ? N11 C39 1.344(7) . ? N12 C44 1.334(9) . ? N12 C40 1.361(8) . ? C34 C35 1.478(9) . ? C34 H34A 0.9500 . ? C35 C36 1.390(8) . ? C36 C37 1.387(10) . ? C36 H36A 0.9500 . ? C37 C38 1.369(10) . ? C37 H37A 0.9500 . ? C38 C39 1.410(8) . ? C38 H38A 0.9500 . ? C39 C40 1.479(9) . ? C40 C41 1.369(8) . ? C41 C42 1.376(10) . ? C41 H41A 0.9500 . ? C42 C43 1.373(10) . ? C42 H42A 0.9500 . ? C43 C44 1.376(10) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? B1 F11 1.352(10) . ? B1 F12 1.359(10) . ? B1 F10 1.380(11) . ? B1 F13 1.386(11) . ? B2 F21 1.340(13) . ? B2 F23 1.341(13) . ? B2 F20 1.370(11) . ? B2 F22 1.382(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ag1 N2 148.10(17) . . ? N8 Ag1 N3 142.21(16) . . ? N2 Ag1 N3 68.97(15) . . ? N8 Ag1 N9 66.49(16) . . ? N2 Ag1 N9 113.23(16) . . ? N3 Ag1 N9 95.94(16) . . ? N8 Ag1 N7 65.70(16) . . ? N2 Ag1 N7 118.82(15) . . ? N3 Ag1 N7 108.71(15) . . ? N9 Ag1 N7 127.41(16) . . ? N10 Ag2 N5 166.56(18) . . ? N10 Ag2 N6 103.1(2) . . ? N5 Ag2 N6 69.4(2) . . ? N10 Ag2 N11 69.54(17) . . ? N5 Ag2 N11 123.89(17) . . ? N6 Ag2 N11 125.10(15) . . ? N10 Ag2 N4 116.53(16) . . ? N5 Ag2 N4 67.90(16) . . ? N6 Ag2 N4 136.22(17) . . ? N11 Ag2 N4 87.55(14) . . ? C5 N1 C1 118.2(6) . . ? C10 N2 C6 118.9(5) . . ? C10 N2 Ag1 116.8(3) . . ? C6 N2 Ag1 124.1(4) . . ? C11 N3 N4 112.2(5) . . ? C11 N3 Ag1 114.7(4) . . ? N4 N3 Ag1 132.9(3) . . ? C12 N4 N3 113.0(5) . . ? C12 N4 Ag2 113.1(4) . . ? N3 N4 Ag2 132.6(3) . . ? C17 N5 C13 120.3(6) . . ? C17 N5 Ag2 118.9(5) . . ? C13 N5 Ag2 119.1(4) . . ? C18 N6 C22 119.0(6) . . ? C18 N6 Ag2 116.1(5) . . ? C22 N6 Ag2 124.4(5) . . ? N1 C1 C2 123.5(8) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 118.2(7) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 119.7(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 118.7(7) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N1 C5 C4 121.7(6) . . ? N1 C5 C6 117.4(5) . . ? C4 C5 C6 120.9(6) . . ? N2 C6 C7 120.9(6) . . ? N2 C6 C5 116.7(5) . . ? C7 C6 C5 122.3(6) . . ? C8 C7 C6 119.9(6) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 119.3(6) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C10 C9 C8 117.3(6) . . ? C10 C9 H9A 121.3 . . ? C8 C9 H9A 121.3 . . ? N2 C10 C9 123.5(5) . . ? N2 C10 C11 117.7(5) . . ? C9 C10 C11 118.8(5) . . ? N3 C11 C10 121.2(5) . . ? N3 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? N4 C12 C13 119.3(6) . . ? N4 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? N5 C13 C14 122.4(6) . . ? N5 C13 C12 117.8(5) . . ? C14 C13 C12 119.8(7) . . ? C13 C14 C15 117.2(8) . . ? C13 C14 H14A 121.4 . . ? C15 C14 H14A 121.4 . . ? C16 C15 C14 119.9(7) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 119.2(7) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? N5 C17 C16 120.9(8) . . ? N5 C17 C18 116.3(6) . . ? C16 C17 C18 122.8(7) . . ? N6 C18 C19 121.0(8) . . ? N6 C18 C17 117.3(5) . . ? C19 C18 C17 121.7(7) . . ? C20 C19 C18 117.3(8) . . ? C20 C19 H19A 121.3 . . ? C18 C19 H19A 121.3 . . ? C21 C20 C19 121.7(7) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 117.5(9) . . ? C20 C21 H21A 121.2 . . ? C22 C21 H21A 121.2 . . ? N6 C22 C21 123.5(8) . . ? N6 C22 H22A 118.3 . . ? C21 C22 H22A 118.3 . . ? C23 N7 N10 119.5(5) . 2_656 ? C23 N7 Ag1 116.0(4) . . ? N10 N7 Ag1 122.1(3) 2_656 . ? C28 N8 C24 119.6(5) . . ? C28 N8 Ag1 118.5(4) . . ? C24 N8 Ag1 118.3(4) . . ? C29 N9 C33 118.0(5) . . ? C29 N9 Ag1 116.1(4) . . ? C33 N9 Ag1 124.1(4) . . ? N7 C23 C24 118.7(5) . . ? N7 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? N8 C24 C25 122.9(6) . . ? N8 C24 C23 115.1(5) . . ? C25 C24 C23 122.0(5) . . ? C24 C25 C26 117.6(6) . . ? C24 C25 H25A 121.2 . . ? C26 C25 H25A 121.2 . . ? C27 C26 C25 119.7(7) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 119.5(6) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? N8 C28 C27 120.7(6) . . ? N8 C28 C29 116.1(5) . . ? C27 C28 C29 123.2(6) . . ? N9 C29 C30 121.6(6) . . ? N9 C29 C28 116.0(5) . . ? C30 C29 C28 122.4(6) . . ? C29 C30 C31 120.2(7) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C32 C31 C30 118.5(6) . . ? C32 C31 H31A 120.7 . . ? C30 C31 H31A 120.7 . . ? C31 C32 C33 118.4(6) . . ? C31 C32 H32A 120.8 . . ? C33 C32 H32A 120.8 . . ? N9 C33 C32 123.3(6) . . ? N9 C33 H33A 118.4 . . ? C32 C33 H33A 118.4 . . ? C34 N10 N7 119.4(5) . 2_656 ? C34 N10 Ag2 119.4(4) . . ? N7 N10 Ag2 118.7(3) 2_656 . ? C35 N11 C39 118.8(5) . . ? C35 N11 Ag2 110.2(4) . . ? C39 N11 Ag2 129.9(4) . . ? C44 N12 C40 117.4(6) . . ? N10 C34 C35 120.2(6) . . ? N10 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? N11 C35 C36 123.0(6) . . ? N11 C35 C34 117.6(5) . . ? C36 C35 C34 119.3(6) . . ? C37 C36 C35 118.3(7) . . ? C37 C36 H36A 120.8 . . ? C35 C36 H36A 120.8 . . ? C38 C37 C36 119.1(6) . . ? C38 C37 H37A 120.4 . . ? C36 C37 H37A 120.4 . . ? C37 C38 C39 119.9(6) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? N11 C39 C38 120.8(6) . . ? N11 C39 C40 118.3(5) . . ? C38 C39 C40 120.8(5) . . ? N12 C40 C41 122.1(6) . . ? N12 C40 C39 115.9(5) . . ? C41 C40 C39 121.9(6) . . ? C40 C41 C42 119.2(6) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C43 C42 C41 119.5(7) . . ? C43 C42 H42A 120.2 . . ? C41 C42 H42A 120.2 . . ? C42 C43 C44 118.4(7) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? N12 C44 C43 123.4(7) . . ? N12 C44 H44A 118.3 . . ? C43 C44 H44A 118.3 . . ? F11 B1 F12 110.5(8) . . ? F11 B1 F10 108.1(7) . . ? F12 B1 F10 110.1(7) . . ? F11 B1 F13 109.8(8) . . ? F12 B1 F13 110.6(8) . . ? F10 B1 F13 107.6(7) . . ? F21 B2 F23 111.3(9) . . ? F21 B2 F20 110.7(9) . . ? F23 B2 F20 107.1(10) . . ? F21 B2 F22 111.7(11) . . ? F23 B2 F22 110.1(10) . . ? F20 B2 F22 105.6(8) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.599 _refine_diff_density_min -1.716 _refine_diff_density_rms 0.099