# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jingsong You' _publ_contact_author_email jsyou@scu.edu.cn loop_ _publ_author_name 'Jingsong You' 'Siping Wei' 'Xiyu Li' 'Zhuang Yang' 'Jingbo Lan' 'Ge Gao' 'Ying Xue' data_CD4 _database_code_depnum_ccdc_archive 'CCDC 836083' _audit_creation_method SHELXL-97 _chemical_formula_moiety '2(C28 H24 Ag N6 O2 F6 P)' _chemical_formula_sum 'C56 H48 Ag2 F12 N12 O4 P2' _chemical_formula_weight 1458.74 _chemical_name_common ? _chemical_name_systematic ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_IT_number 13 _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 2/c' _space_group_name_Hall '-P 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 '-x, -y, -z' 4 'x, -y, z-1/2' _cell_angle_alpha 90.00 _cell_angle_beta 118.38(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 14.883(9) _cell_length_b 11.843(10) _cell_length_c 19.893(10) _cell_measurement_reflns_used 24 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 7.59 _cell_measurement_theta_min 4.64 _cell_volume 3085(4) _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_T_max 0.9696 _exptl_absorpt_correction_T_min 0.8116 _exptl_absorpt_correction_type 'empirical psi-scan method' _exptl_crystal_F_000 1464 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type CAD4 _diffrn_measurement_method Omega/2-Theta _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.2206 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 6044 _diffrn_reflns_theta_full 25.54 _diffrn_reflns_theta_max 25.54 _diffrn_reflns_theta_min 1.72 _diffrn_standards_decay_% 4.813 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _reflns_number_gt 1985 _reflns_number_total 5535 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.786 _refine_diff_density_min -1.833 _refine_diff_density_rms 0.138 _refine_ls_R_factor_all 0.2709 _refine_ls_R_factor_gt 0.0982 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 5535 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.2019 _refine_ls_wR_factor_ref 0.2388 _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.65679(7) 0.72123(8) 0.80814(4) 0.0594(4) Uani 1 d . . . P1 P 0.5000 0.3216(5) 0.7500 0.0726(14) Uani 1 d S . . F1 F 0.5486(6) 0.2230(8) 0.8104(5) 0.113(3) Uani 1 d . . . F2 F 0.5943(6) 0.3202(7) 0.7323(5) 0.103(3) Uani 1 d . . . F3 F 0.5530(8) 0.4156(10) 0.8144(6) 0.148(4) Uani 1 d . . . P2 P 0.0000 0.3290(10) 0.2500 0.256(9) Uani 1 d S . . F4 F 0.0978(13) 0.3357(11) 0.2481(12) 0.231(8) Uani 1 d . . . F5 F 0.0351(17) 0.2296(14) 0.3178(13) 0.256(9) Uani 1 d . . . F6 F 0.037(2) 0.419(2) 0.3231(17) 0.378(16) Uani 1 d . . . O1 O 0.8567(12) 1.1146(14) 0.9698(8) 0.171(7) Uani 1 d . . . O2 O 0.8620(8) 0.3150(9) 0.8132(7) 0.110(4) Uani 1 d . . . N1 N 0.6294(7) 0.8512(10) 0.9347(5) 0.078(3) Uani 1 d . . . N2 N 0.6629(11) 0.9446(12) 0.9838(7) 0.121(5) Uani 1 d . . . N3 N 0.7218(9) 0.9422(11) 0.9006(6) 0.091(4) Uani 1 d . . . N4 N 0.6462(7) 0.5790(9) 0.6680(5) 0.060(3) Uani 1 d . . . N5 N 0.6918(8) 0.4885(9) 0.6543(6) 0.071(3) Uani 1 d . . . N6 N 0.7492(7) 0.5112(8) 0.7769(5) 0.058(3) Uani 1 d . . . C1 C 0.640(2) 1.0187(15) 0.7315(13) 0.126(8) Uani 1 d . . . H1 H 0.6079 1.0616 0.7527 0.111(14) Uiso 1 calc R . . C2 C 0.597(3) 1.010(2) 0.6596(18) 0.177(12) Uani 1 d . . . H2 H 0.5353 1.0461 0.6310 0.111(14) Uiso 1 calc R . . C3 C 0.637(2) 0.951(3) 0.6224(16) 0.193(19) Uani 1 d . . . H3 H 0.6043 0.9484 0.5693 0.111(14) Uiso 1 calc R . . C4 C 0.721(2) 0.8979(18) 0.6627(14) 0.150(10) Uani 1 d . . . H4 H 0.7487 0.8559 0.6374 0.111(14) Uiso 1 calc R . . C5 C 0.7777(14) 0.9004(15) 0.7486(9) 0.109(5) Uani 1 d . . . H5 H 0.8372 0.8591 0.7766 0.111(14) Uiso 1 calc R . . C6 C 0.7368(13) 0.9664(14) 0.7829(13) 0.104(6) Uani 1 d . . . C7 C 0.7809(12) 0.9765(14) 0.8658(9) 0.085(5) Uani 1 d . . . H7 H 0.8441 0.9322 0.8889 0.05(2) Uiso 1 calc R . . C8 C 0.8100(14) 1.1020(16) 0.8906(14) 0.133(7) Uani 1 d . . . H8A H 0.8560 1.1285 0.8721 0.15(3) Uiso 1 calc R . . H8B H 0.7488 1.1482 0.8673 0.15(3) Uiso 1 calc R . . C9 C 0.7762(15) 1.1070(19) 0.9893(14) 0.183(12) Uani 1 d . . . H9A H 0.7279 1.1678 0.9647 0.15(3) Uiso 1 calc R . . H9B H 0.8042 1.1155 1.0441 0.15(3) Uiso 1 calc R . . C10 C 0.7214(13) 0.9944(17) 0.9646(10) 0.120(7) Uani 1 d . . . C11 C 0.6638(7) 0.8451(11) 0.8821(6) 0.055(3) Uani 1 d . . . C12 C 0.4353(10) 0.7738(12) 0.5557(6) 0.074(4) Uani 1 d . . . C13 C 0.4317(10) 0.7619(13) 0.4830(6) 0.082(4) Uani 1 d . . . H13 H 0.3835 0.8023 0.4413 0.111(14) Uiso 1 calc R . . C14 C 0.4940(11) 0.6963(13) 0.4746(6) 0.088(5) Uani 1 d . . . H14 H 0.4895 0.6900 0.4265 0.111(14) Uiso 1 calc R . . C15 C 0.5693(10) 0.6331(12) 0.5355(7) 0.078(4) Uani 1 d . . . H15 H 0.6160 0.5885 0.5291 0.111(14) Uiso 1 calc R . . C16 C 0.5703(8) 0.6409(10) 0.6075(5) 0.054(3) Uani 1 d . . . C17 C 0.5054(9) 0.7136(10) 0.6161(6) 0.065(3) Uani 1 d . . . H17 H 0.5093 0.7222 0.6639 0.111(14) Uiso 1 calc R . . C18 C 0.6775(9) 0.5937(10) 0.7445(6) 0.056(3) Uani 1 d . . . C19 C 0.7563(10) 0.4508(11) 0.7211(8) 0.074(4) Uani 1 d . . . C20 C 0.8297(11) 0.3576(14) 0.7376(10) 0.110(6) Uani 1 d . . . H20A H 0.7979 0.2975 0.7006 0.15(3) Uiso 1 calc R . . H20B H 0.8885 0.3845 0.7336 0.15(3) Uiso 1 calc R . . C21 C 0.8947(11) 0.4055(15) 0.8666(9) 0.104(5) Uani 1 d . . . H21A H 0.9380 0.4566 0.8567 0.15(3) Uiso 1 calc R . . H21B H 0.9335 0.3764 0.9182 0.15(3) Uiso 1 calc R . . C22 C 0.7940(9) 0.4723(11) 0.8578(6) 0.064(3) Uani 1 d . . . H22 H 0.7473 0.4199 0.8638 0.05(2) Uiso 1 calc R . . C23 C 0.8226(9) 0.5656(14) 0.9140(7) 0.074(4) Uani 1 d . . . C24 C 0.8887(11) 0.6540(15) 0.9238(8) 0.095(5) Uani 1 d . . . H24 H 0.9146 0.6570 0.8895 0.111(14) Uiso 1 calc R . . C25 C 0.9191(13) 0.7337(16) 0.9755(10) 0.113(6) Uani 1 d . . . H25 H 0.9609 0.7929 0.9767 0.111(14) Uiso 1 calc R . . C26 C 0.8821(15) 0.722(2) 1.0309(12) 0.154(11) Uani 1 d . . . H26 H 0.9109 0.7669 1.0746 0.111(14) Uiso 1 calc R . . C27 C 0.8134(18) 0.655(3) 1.0222(9) 0.206(18) Uani 1 d . . . H27 H 0.7803 0.6634 1.0514 0.111(14) Uiso 1 calc R . . C28 C 0.7837(12) 0.5628(19) 0.9674(10) 0.135(8) Uani 1 d . . . H28 H 0.7413 0.5048 0.9670 0.111(14) Uiso 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 0.0970(7) 0.0553(6) 0.0425(5) -0.0070(5) 0.0468(4) -0.0022(5) P1 0.083(3) 0.085(4) 0.064(3) 0.000 0.046(3) 0.000 F1 0.127(6) 0.140(8) 0.090(5) 0.039(6) 0.064(5) 0.049(5) F2 0.128(6) 0.116(8) 0.105(6) -0.018(5) 0.088(5) -0.033(5) F3 0.202(9) 0.152(10) 0.123(7) -0.090(7) 0.104(7) -0.072(7) P2 0.392(17) 0.093(7) 0.54(3) 0.000 0.43(2) 0.000 F4 0.345(16) 0.134(11) 0.43(2) -0.050(14) 0.365(19) -0.043(11) F5 0.40(2) 0.172(14) 0.36(2) -0.030(16) 0.31(2) -0.039(14) F6 0.51(3) 0.27(2) 0.57(5) -0.22(3) 0.44(4) -0.08(2) O1 0.232(14) 0.204(16) 0.136(11) -0.097(12) 0.135(11) -0.146(13) O2 0.163(9) 0.066(8) 0.093(8) 0.027(6) 0.053(7) 0.037(6) N1 0.106(7) 0.078(8) 0.059(6) -0.050(6) 0.047(6) -0.035(6) N2 0.186(12) 0.123(12) 0.104(9) -0.081(9) 0.110(10) -0.086(10) N3 0.142(9) 0.095(10) 0.073(7) -0.036(7) 0.081(7) -0.015(7) N4 0.080(6) 0.082(8) 0.037(5) -0.004(5) 0.043(5) 0.009(5) N5 0.114(8) 0.060(8) 0.061(6) 0.000(6) 0.060(7) 0.021(6) N6 0.090(7) 0.054(7) 0.041(5) 0.007(5) 0.040(5) 0.017(5) C1 0.26(3) 0.065(13) 0.125(14) -0.036(12) 0.155(18) -0.040(14) C2 0.31(4) 0.10(2) 0.16(3) 0.030(18) 0.14(3) -0.025(19) C3 0.23(3) 0.21(4) 0.106(19) 0.07(2) 0.050(19) -0.12(3) C4 0.32(3) 0.078(16) 0.18(2) -0.010(15) 0.22(2) -0.010(17) C5 0.187(16) 0.091(14) 0.102(12) -0.005(10) 0.113(12) 0.007(11) C6 0.119(13) 0.066(12) 0.18(2) 0.048(13) 0.116(14) 0.025(9) C7 0.101(10) 0.110(14) 0.093(10) -0.031(9) 0.087(10) -0.029(9) C8 0.172(16) 0.083(15) 0.20(2) -0.015(15) 0.133(17) -0.024(11) C9 0.21(2) 0.16(2) 0.25(3) -0.14(2) 0.16(2) -0.133(18) C10 0.155(14) 0.131(17) 0.132(14) -0.080(13) 0.116(13) -0.057(11) C11 0.068(7) 0.069(9) 0.048(6) -0.013(6) 0.045(6) -0.033(6) C12 0.109(9) 0.077(9) 0.049(6) 0.007(7) 0.046(7) 0.033(8) C13 0.109(9) 0.123(14) 0.039(6) 0.026(7) 0.055(7) 0.034(9) C14 0.140(12) 0.113(14) 0.039(6) 0.014(7) 0.066(8) 0.022(9) C15 0.148(11) 0.071(10) 0.075(9) -0.008(7) 0.100(9) 0.015(8) C16 0.080(7) 0.064(9) 0.030(5) 0.006(6) 0.036(6) 0.005(6) C17 0.125(9) 0.054(8) 0.036(5) 0.014(6) 0.055(6) 0.030(7) C18 0.108(8) 0.035(7) 0.041(6) 0.014(5) 0.047(6) -0.004(6) C19 0.102(10) 0.060(9) 0.066(8) -0.020(7) 0.045(8) 0.022(7) C20 0.123(12) 0.068(12) 0.120(14) 0.025(11) 0.041(11) 0.027(9) C21 0.112(11) 0.095(14) 0.088(11) 0.001(11) 0.034(10) 0.029(9) C22 0.087(8) 0.060(10) 0.044(7) 0.005(6) 0.030(6) 0.001(7) C23 0.076(9) 0.107(13) 0.045(7) 0.017(8) 0.034(7) 0.026(8) C24 0.105(11) 0.114(14) 0.050(8) 0.014(9) 0.024(8) -0.030(10) C25 0.119(13) 0.089(14) 0.084(12) -0.024(11) 0.010(11) 0.001(9) C26 0.074(12) 0.27(3) 0.059(12) -0.043(16) -0.015(11) 0.019(15) C27 0.111(17) 0.42(5) 0.033(9) -0.059(18) -0.010(12) 0.10(2) C28 0.118(14) 0.16(2) 0.085(13) 0.057(14) 0.014(11) -0.011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C11 2.044(12) . ? Ag1 C18 2.085(12) . ? P1 F1 1.582(9) . ? P1 F1 1.582(9) 2_656 ? P1 F2 1.602(7) . ? P1 F2 1.602(7) 2_656 ? P1 F3 1.595(9) 2_656 ? P1 F3 1.595(9) . ? P2 F4 1.476(11) 2 ? P2 F4 1.476(11) . ? P2 F5 1.68(2) . ? P2 F5 1.68(2) 2 ? P2 F6 1.67(2) . ? P2 F6 1.67(2) 2 ? O1 C8 1.40(2) . ? O1 C9 1.427(19) . ? O2 C20 1.434(19) . ? O2 C21 1.423(18) . ? N1 N2 1.401(14) . ? N1 C11 1.369(13) . ? N1 C12 1.407(16) 2_656 ? N2 C10 1.252(18) . ? N3 C7 1.412(16) . ? N3 C10 1.419(17) . ? N3 C11 1.379(15) . ? N4 N5 1.363(13) . ? N4 C16 1.403(13) . ? N4 C18 1.376(13) . ? N5 C19 1.294(14) . ? N6 C18 1.362(13) . ? N6 C19 1.367(14) . ? N6 C22 1.492(13) . ? C1 H1 0.9300 . ? C1 C2 1.26(3) . ? C1 C6 1.45(3) . ? C2 H2 0.9300 . ? C2 C3 1.34(4) . ? C3 H3 0.9300 . ? C3 C4 1.29(3) . ? C4 H4 0.9300 . ? C4 C5 1.51(3) . ? C5 H5 0.9300 . ? C5 C6 1.36(2) . ? C6 C7 1.46(2) . ? C7 H7 0.9800 . ? C7 C8 1.56(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.52(2) . ? C12 N1 1.407(16) 2_656 ? C12 C13 1.429(15) . ? C12 C17 1.360(15) . ? C13 H13 0.9300 . ? C13 C14 1.281(17) . ? C14 H14 0.9300 . ? C14 C15 1.412(17) . ? C15 H15 0.9300 . ? C15 C16 1.427(13) . ? C16 C17 1.364(15) . ? C17 H17 0.9300 . ? C19 C20 1.476(18) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.629(18) . ? C22 H22 0.9800 . ? C22 C23 1.482(18) . ? C23 C24 1.385(19) . ? C23 C28 1.43(2) . ? C24 H24 0.9300 . ? C24 C25 1.31(2) . ? C25 H25 0.9300 . ? C25 C26 1.45(3) . ? C26 H26 0.9300 . ? C26 C27 1.24(4) . ? C27 H27 0.9300 . ? C27 C28 1.45(3) . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 P1 F1 84.9(8) 2_656 . ? F1 P1 F2 87.5(5) 2_656 . ? F1 P1 F2 87.5(5) . 2_656 ? F1 P1 F2 91.6(5) . . ? F1 P1 F2 91.6(5) 2_656 2_656 ? F1 P1 F3 91.9(6) . . ? F1 P1 F3 176.7(7) 2_656 . ? F1 P1 F3 176.7(6) . 2_656 ? F1 P1 F3 91.9(6) 2_656 2_656 ? F2 P1 F2 178.8(8) . 2_656 ? F3 P1 F2 91.9(5) . . ? F3 P1 F2 88.9(5) 2_656 . ? F3 P1 F2 88.9(5) . 2_656 ? F3 P1 F2 91.9(5) 2_656 2_656 ? F3 P1 F3 91.4(10) . 2_656 ? F4 P2 F4 173.8(14) 2 . ? F4 P2 F5 97.2(11) . . ? F4 P2 F5 87.2(9) 2 . ? F4 P2 F5 87.2(9) . 2 ? F4 P2 F5 97.2(11) 2 2 ? F4 P2 F6 93.8(10) 2 2 ? F4 P2 F6 93.8(10) . . ? F4 P2 F6 82.3(10) . 2 ? F4 P2 F6 82.3(10) 2 . ? F5 P2 F5 90.7(13) 2 . ? F6 P2 F5 84.1(12) . . ? F6 P2 F5 84.1(12) 2 2 ? F6 P2 F5 174.8(13) 2 . ? F6 P2 F5 174.8(13) . 2 ? F6 P2 F6 101(2) . 2 ? O1 C8 C7 111.8(17) . . ? O1 C8 H8A 109.2 . . ? O1 C8 H8B 109.2 . . ? O1 C9 H9A 109.4 . . ? O1 C9 H9B 109.4 . . ? O1 C9 C10 111.0(16) . . ? O2 C20 C19 109.9(15) . . ? O2 C20 H20A 109.7 . . ? O2 C20 H20B 109.7 . . ? O2 C21 H21A 110.0 . . ? O2 C21 H21B 110.0 . . ? O2 C21 C22 108.4(11) . . ? N1 C11 Ag1 132.7(8) . . ? N1 C11 N3 99.5(9) . . ? N1 C12 C13 120.2(11) 2_656 . ? N2 N1 C12 117.3(11) . 2_656 ? N2 C10 N3 111.6(14) . . ? N2 C10 C9 131.3(15) . . ? N3 C7 C6 118.6(13) . . ? N3 C7 H7 107.5 . . ? N3 C7 C8 105.3(12) . . ? N3 C10 C9 116.3(16) . . ? N3 C11 Ag1 127.0(7) . . ? N4 C16 C15 116.5(10) . . ? N4 C18 Ag1 133.9(9) . . ? N5 N4 C16 120.9(9) . . ? N5 N4 C18 112.4(10) . . ? N5 C19 N6 110.3(10) . . ? N5 C19 C20 126.7(12) . . ? N6 C18 Ag1 122.8(7) . . ? N6 C18 N4 102.1(10) . . ? N6 C19 C20 123.0(13) . . ? N6 C22 C21 100.5(10) . . ? N6 C22 H22 110.3 . . ? C1 C2 H2 118.3 . . ? C1 C2 C3 123(4) . . ? C1 C6 C7 121.8(17) . . ? C2 C1 H1 117.9 . . ? C2 C1 C6 124(3) . . ? C2 C3 H3 121.2 . . ? C3 C2 H2 118.3 . . ? C3 C4 H4 118.3 . . ? C3 C4 C5 123(2) . . ? C4 C3 C2 118(3) . . ? C4 C3 H3 121.2 . . ? C4 C5 H5 121.9 . . ? C5 C4 H4 118.3 . . ? C5 C6 C1 115(2) . . ? C5 C6 C7 123.1(16) . . ? C6 C1 H1 117.9 . . ? C6 C5 C4 116.2(19) . . ? C6 C5 H5 121.9 . . ? C6 C7 H7 107.5 . . ? C6 C7 C8 110.0(16) . . ? C7 N3 C10 125.7(13) . . ? C7 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C8 O1 C9 105.6(16) . . ? C8 C7 H7 107.5 . . ? H8A C8 H8B 107.9 . . ? H9A C9 H9B 108.0 . . ? C10 N2 N1 103.2(12) . . ? C10 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C11 Ag1 C18 169.9(4) . . ? C11 N1 N2 115.9(10) . . ? C11 N1 C12 126.8(10) . 2_656 ? C11 N3 C7 124.4(10) . . ? C11 N3 C10 109.5(12) . . ? C12 C13 H13 119.6 . . ? C12 C17 C16 120.7(9) . . ? C12 C17 H17 119.6 . . ? C13 C14 H14 118.7 . . ? C13 C14 C15 122.6(10) . . ? C14 C13 C12 120.7(11) . . ? C14 C13 H13 119.6 . . ? C14 C15 H15 121.5 . . ? C14 C15 C16 116.9(10) . . ? C15 C14 H14 118.7 . . ? C16 C15 H15 121.5 . . ? C16 C17 H17 119.6 . . ? C17 C12 N1 120.6(10) . 2_656 ? C17 C12 C13 119.2(11) . . ? C17 C16 N4 123.4(9) . . ? C17 C16 C15 119.8(10) . . ? C18 N4 C16 126.5(10) . . ? C18 N6 C19 109.7(9) . . ? C18 N6 C22 125.4(9) . . ? C19 N5 N4 105.3(9) . . ? C19 N6 C22 123.2(10) . . ? C19 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C21 O2 C20 110.1(12) . . ? C21 C22 H22 110.3 . . ? H21A C21 H21B 108.4 . . ? C22 C21 H21A 110.0 . . ? C22 C21 H21B 110.0 . . ? C23 C22 N6 113.8(10) . . ? C23 C22 C21 111.1(11) . . ? C23 C22 H22 110.3 . . ? C23 C24 H24 116.1 . . ? C23 C28 C27 117(2) . . ? C23 C28 H28 121.5 . . ? C24 C23 C22 126.9(13) . . ? C24 C23 C28 115.0(16) . . ? C24 C25 H25 122.8 . . ? C24 C25 C26 114(2) . . ? C25 C24 C23 127.9(17) . . ? C25 C24 H24 116.1 . . ? C25 C26 H26 118.7 . . ? C26 C25 H25 122.8 . . ? C26 C27 H27 119.2 . . ? C26 C27 C28 122(2) . . ? C27 C26 C25 123(2) . . ? C27 C26 H26 118.7 . . ? C27 C28 H28 121.5 . . ? C28 C23 C22 118.0(16) . . ? C28 C27 H27 119.2 . . ? # Attachment '[(R)-1Ag]2BF4Cl.cif' data_110301_S1_WSP _database_code_depnum_ccdc_archive 'CCDC 836084' _audit_creation_method SHELXL-97 _chemical_absolute_configuration unk _chemical_formula_moiety ; 4(C14 H12 Ag0.5 N3 O), 4(B0.25 F), 12(Cl0.083333) ; _chemical_formula_sum 'C56 H48 Ag2 B Cl F4 N12 O4' _chemical_formula_weight 1291.06 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? 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' Ag Ag -0.8971 1.1015 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 6 2 2' _symmetry_space_group_name_Hall 'P 6 2' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z' 3 '-y, x-y, z' 4 '-x, -y, z' 5 '-x+y, -x, z' 6 'y, -x+y, z' 7 'x-y, -y, -z' 8 '-x, -x+y, -z' 9 'y, x, -z' 10 '-y, -x, -z' 11 '-x+y, y, -z' 12 'x, x-y, -z' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 22.2009(5) _cell_length_b 22.2009(5) _cell_length_c 12.58554(19) _cell_measurement_reflns_used 6655 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 29.1737 _cell_measurement_theta_min 3.1722 _cell_volume 5372.11(18) _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.98524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_F_000 1956 _exptl_crystal_colour colurless _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_special_details ? _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -9.00 28.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.8611 77.0000 120.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega 4.00 84.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.8611 77.0000 0.0000 80 #__ type_ start__ end____ width___ exp.time_ 3 omega -64.00 -37.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - -16.8924 108.0000 -68.0000 27 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0332126 _diffrn_orient_matrix_UB_12 0.0050425 _diffrn_orient_matrix_UB_13 0.0136256 _diffrn_orient_matrix_UB_21 -0.0125038 _diffrn_orient_matrix_UB_22 -0.0360117 _diffrn_orient_matrix_UB_23 -0.0073846 _diffrn_orient_matrix_UB_31 0.0100599 _diffrn_orient_matrix_UB_32 0.0061798 _diffrn_orient_matrix_UB_33 -0.0541951 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14796 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.24 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3134 _reflns_number_total 3659 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 5.818 _refine_diff_density_min -11.891 _refine_diff_density_rms 0.163 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0688 _refine_ls_abs_structure_Flack 0.05(7) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 183 _refine_ls_number_reflns 3659 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.1874 _refine_ls_wR_factor_ref 0.1963 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+0.9541P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 0.559183(13) 0.11837(3) 0.0000 0.0329(2) Uani 1 2 d S . . Cl1 Cl 0.6667 0.3333 0.0000 0.1067(14) Uani 1 6 d S . . Cl2 Cl 0.0000 0.0000 0.0000 0.1067(14) Uani 1 12 d S . . F1 F 0.4860(4) 0.0430(4) 0.4418(7) 0.144(4) Uani 1 1 d . . . O1 O 0.5500(3) 0.2344(3) 0.3954(4) 0.0556(13) Uani 1 1 d . . . N1 N 0.4292(3) 0.0862(3) 0.1428(4) 0.0339(11) Uani 1 1 d . . . N2 N 0.4100(4) 0.1025(3) 0.2385(5) 0.0450(16) Uani 1 1 d . . . N3 N 0.5223(3) 0.1515(3) 0.2199(4) 0.0358(12) Uani 1 1 d . . . C1 C 0.4972(3) 0.1160(3) 0.1283(4) 0.0329(12) Uani 1 1 d . . . C2 C 0.4692(4) 0.1430(3) 0.2822(5) 0.0405(14) Uani 1 1 d . . . C3 C 0.4812(4) 0.1790(4) 0.3891(5) 0.0524(18) Uani 1 1 d . . . H3A H 0.4486 0.1968 0.3979 0.063 Uiso 1 1 calc R . . H3B H 0.4725 0.1453 0.4469 0.063 Uiso 1 1 calc R . . C4 C 0.5977(5) 0.2122(4) 0.3682(4) 0.055(2) Uani 1 1 d . . . H4A H 0.5860 0.1692 0.4078 0.066 Uiso 1 1 calc R . . H4B H 0.6453 0.2484 0.3887 0.066 Uiso 1 1 calc R . . C5 C 0.5953(5) 0.1983(3) 0.2481(4) 0.0397(12) Uani 1 1 d . . . H5 H 0.6127 0.2432 0.2091 0.048 Uiso 1 1 calc R . . C6 C 0.6422(5) 0.1682(4) 0.2223(5) 0.0438(18) Uani 1 1 d . . . C7 C 0.6337(4) 0.1090(4) 0.2717(6) 0.0523(18) Uani 1 1 d . . . H7 H 0.5949 0.0833 0.3171 0.063 Uiso 1 1 calc R . . C8 C 0.6810(5) 0.0864(5) 0.2557(9) 0.060(2) Uani 1 1 d . . . H8 H 0.6743 0.0451 0.2894 0.072 Uiso 1 1 calc R . . C9 C 0.7393(5) 0.1249(5) 0.1893(8) 0.070(3) Uani 1 1 d . . . H9 H 0.7728 0.1106 0.1795 0.084 Uiso 1 1 calc R . . C10 C 0.7470(4) 0.1839(5) 0.1384(7) 0.061(2) Uani 1 1 d . . . H10 H 0.7853 0.2091 0.0918 0.074 Uiso 1 1 calc R . . C11 C 0.7004(4) 0.2063(4) 0.1542(5) 0.0523(18) Uani 1 1 d . . . H11 H 0.7068 0.2472 0.1198 0.063 Uiso 1 1 calc R . . C12 C 0.3748(3) 0.0417(3) 0.0693(5) 0.0364(13) Uani 1 1 d . . . C13 C 0.3853(3) 0.0000 0.0000 0.0334(14) Uani 1 2 d S . . H13 H 0.4281 0.0000 0.0000 0.040 Uiso 1 2 calc SR . . C14 C 0.3121(4) 0.0421(4) 0.0705(6) 0.0485(16) Uani 1 1 d . . . H14 H 0.3047 0.0707 0.1188 0.058 Uiso 1 1 calc R . . C15 C 0.2617(4) 0.0000 0.0000 0.055(2) Uani 1 2 d S . . H15 H 0.2189 0.0000 0.0000 0.066 Uiso 1 2 calc SR . . B1 B 0.5000 0.0000 0.5000 0.065(5) Uani 1 4 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0413(3) 0.0391(3) 0.0178(3) 0.000 0.0021(3) 0.01953(16) Cl1 0.116(2) 0.116(2) 0.087(3) 0.000 0.000 0.0582(11) Cl2 0.116(2) 0.116(2) 0.087(3) 0.000 0.000 0.0582(11) F1 0.203(8) 0.109(5) 0.160(8) 0.089(5) 0.081(6) 0.108(6) O1 0.071(3) 0.053(3) 0.036(3) -0.023(2) -0.003(2) 0.027(3) N1 0.048(3) 0.042(3) 0.018(2) -0.0046(19) 0.0028(19) 0.028(2) N2 0.054(4) 0.047(4) 0.033(3) -0.008(3) 0.006(3) 0.025(3) N3 0.046(3) 0.039(3) 0.023(2) -0.005(2) 0.000(2) 0.021(3) C1 0.041(3) 0.034(3) 0.023(2) -0.003(2) -0.002(2) 0.018(3) C2 0.059(4) 0.039(3) 0.024(3) 0.000(3) 0.004(3) 0.025(3) C3 0.074(5) 0.058(4) 0.030(3) -0.011(3) 0.008(3) 0.036(4) C4 0.072(6) 0.059(3) 0.030(3) -0.013(3) -0.013(4) 0.029(4) C5 0.052(4) 0.038(3) 0.030(2) -0.0013(19) -0.004(4) 0.023(4) C6 0.061(5) 0.041(4) 0.024(3) -0.009(3) -0.010(3) 0.022(4) C7 0.062(5) 0.045(4) 0.039(4) -0.003(3) -0.003(3) 0.019(4) C8 0.064(5) 0.051(5) 0.073(6) -0.016(4) -0.025(4) 0.034(4) C9 0.056(5) 0.085(7) 0.072(6) -0.046(5) -0.017(4) 0.037(5) C10 0.043(4) 0.071(5) 0.050(4) -0.027(4) 0.003(3) 0.013(4) C11 0.053(4) 0.050(4) 0.036(3) -0.015(3) -0.003(3) 0.013(3) C12 0.041(3) 0.040(3) 0.028(3) 0.003(2) 0.005(2) 0.020(3) C13 0.030(2) 0.041(4) 0.033(3) 0.011(5) 0.006(3) 0.0206(18) C14 0.048(4) 0.053(4) 0.048(4) -0.003(3) 0.009(3) 0.028(3) C15 0.044(3) 0.061(5) 0.065(5) 0.004(8) 0.002(4) 0.031(3) B1 0.104(11) 0.027(6) 0.038(6) 0.000 0.000 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C1 2.106(6) . ? Ag1 C1 2.106(6) 11_655 ? F1 B1 1.357(6) . ? O1 C3 1.404(10) . ? O1 C4 1.415(12) . ? N1 N2 1.385(8) . ? N1 C1 1.324(8) . ? N1 C12 1.448(8) . ? N2 C2 1.286(10) . ? N3 C1 1.349(8) . ? N3 C2 1.349(9) . ? N3 C5 1.467(11) . ? C2 C3 1.519(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.538(8) . ? C5 H5 1.0000 . ? C5 C6 1.526(13) . ? C6 C7 1.379(11) . ? C6 C11 1.423(11) . ? C7 H7 0.9500 . ? C7 C8 1.388(13) . ? C8 H8 0.9500 . ? C8 C9 1.413(15) . ? C9 H9 0.9500 . ? C9 C10 1.390(15) . ? C10 H10 0.9500 . ? C10 C11 1.369(12) . ? C11 H11 0.9500 . ? C12 C13 1.374(7) . ? C12 C14 1.398(10) . ? C13 C12 1.374(7) 7 ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C14 C15 1.366(9) . ? C15 C14 1.366(9) 7 ? C15 H15 0.9500 . ? B1 F1 1.357(6) 4_655 ? B1 F1 1.357(6) 7_556 ? B1 F1 1.357(6) 11_656 ? 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 F1 B1 F1 114.6(8) 11_656 7_556 ? F1 B1 F1 109.0(6) 7_556 . ? F1 B1 F1 114.6(8) 4_655 . ? F1 B1 F1 104.9(8) 4_655 7_556 ? F1 B1 F1 104.9(8) 11_656 . ? F1 B1 F1 109.0(6) 11_656 4_655 ? O1 C3 C2 109.8(6) . . ? O1 C3 H3A 109.7 . . ? O1 C3 H3B 109.7 . . ? O1 C4 H4A 109.5 . . ? O1 C4 H4B 109.5 . . ? O1 C4 C5 110.5(7) . . ? N1 C1 Ag1 133.3(4) . . ? N1 C1 N3 102.1(5) . . ? N2 N1 C12 118.3(5) . . ? N2 C2 N3 111.4(6) . . ? N2 C2 C3 126.6(7) . . ? N3 C1 Ag1 124.5(5) . . ? N3 C2 C3 122.0(6) . . ? N3 C5 C4 107.1(7) . . ? N3 C5 H5 109.0 . . ? N3 C5 C6 113.2(5) . . ? C1 Ag1 C1 177.6(3) . 11_655 ? C1 N1 N2 114.3(5) . . ? C1 N1 C12 127.4(5) . . ? C1 N3 C5 127.5(6) . . ? C2 N2 N1 102.4(6) . . ? C2 N3 C1 109.7(6) . . ? C2 N3 C5 122.6(5) . . ? C2 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C3 O1 C4 110.9(5) . . ? H3A C3 H3B 108.2 . . ? C4 C5 H5 109.0 . . ? H4A C4 H4B 108.1 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C6 C5 C4 109.5(7) . . ? C6 C5 H5 109.0 . . ? C6 C7 H7 119.6 . . ? C6 C7 C8 120.8(8) . . ? C6 C11 H11 120.1 . . ? C7 C6 C5 121.5(7) . . ? C7 C6 C11 119.4(8) . . ? C7 C8 H8 120.1 . . ? C7 C8 C9 119.8(9) . . ? C8 C7 H7 119.6 . . ? C8 C9 H9 120.4 . . ? C9 C8 H8 120.1 . . ? C9 C10 H10 119.4 . . ? C10 C9 C8 119.1(8) . . ? C10 C9 H9 120.4 . . ? C10 C11 C6 119.8(8) . . ? C10 C11 H11 120.1 . . ? C11 C6 C5 118.8(7) . . ? C11 C10 C9 121.1(8) . . ? C11 C10 H10 119.4 . . ? C12 C13 C12 119.1(7) . 7 ? C12 C13 H13 120.4 . . ? C12 C13 H13 120.4 7 . ? C12 C14 H14 121.1 . . ? C13 C12 N1 120.1(5) . . ? C13 C12 C14 121.1(6) . . ? C14 C12 N1 118.8(5) . . ? C14 C15 C14 123.0(9) . 7 ? C14 C15 H15 118.5 . . ? C14 C15 H15 118.5 7 . ? C15 C14 C12 117.8(6) . . ? C15 C14 H14 121.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C5 N3 -51.8(7) . . . . ? O1 C4 C5 C6 -174.9(6) . . . . ? N1 N2 C2 N3 -0.7(8) . . . . ? N1 N2 C2 C3 178.6(7) . . . . ? N1 C12 C13 C12 -179.8(6) . . . 7 ? N1 C12 C14 C15 179.6(5) . . . . ? N2 N1 C1 Ag1 -175.3(5) . . . . ? N2 N1 C1 N3 1.4(7) . . . . ? N2 N1 C12 C13 -151.4(5) . . . . ? N2 N1 C12 C14 28.6(8) . . . . ? N2 C2 C3 O1 -161.7(7) . . . . ? N3 C2 C3 O1 17.5(10) . . . . ? N3 C5 C6 C7 -63.6(8) . . . . ? N3 C5 C6 C11 123.0(6) . . . . ? C1 Ag1 C1 N1 -54.9(7) 11_655 . . . ? C1 Ag1 C1 N3 128.9(4) 11_655 . . . ? C1 N1 N2 C2 -0.5(7) . . . . ? C1 N1 C12 C13 30.9(8) . . . . ? C1 N1 C12 C14 -149.1(6) . . . . ? C1 N3 C2 N2 1.6(8) . . . . ? C1 N3 C2 C3 -177.7(6) . . . . ? C1 N3 C5 C4 -167.3(7) . . . . ? C1 N3 C5 C6 -46.4(8) . . . . ? C2 N3 C1 Ag1 175.4(4) . . . . ? C2 N3 C1 N1 -1.8(7) . . . . ? C2 N3 C5 C4 18.9(9) . . . . ? C2 N3 C5 C6 139.7(7) . . . . ? C3 O1 C4 C5 72.1(8) . . . . ? C4 O1 C3 C2 -51.1(8) . . . . ? C4 C5 C6 C7 55.9(9) . . . . ? C4 C5 C6 C11 -117.5(7) . . . . ? C5 N3 C1 Ag1 0.9(10) . . . . ? C5 N3 C1 N1 -176.3(6) . . . . ? C5 N3 C2 N2 176.5(6) . . . . ? C5 N3 C2 C3 -2.9(10) . . . . ? C5 C6 C7 C8 -173.2(7) . . . . ? C5 C6 C11 C10 173.5(6) . . . . ? C6 C7 C8 C9 0.8(12) . . . . ? C7 C6 C11 C10 0.0(10) . . . . ? C7 C8 C9 C10 -1.9(12) . . . . ? C8 C9 C10 C11 2.0(12) . . . . ? C9 C10 C11 C6 -1.1(11) . . . . ? C11 C6 C7 C8 0.2(11) . . . . ? C12 N1 N2 C2 -178.5(6) . . . . ? C12 N1 C1 Ag1 2.5(9) . . . . ? C12 N1 C1 N3 179.2(6) . . . . ? C12 C14 C15 C14 0.2(4) . . . 7 ? C13 C12 C14 C15 -0.4(9) . . . . ? C14 C12 C13 C12 0.2(4) . . . 7 ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.043 1692 230 ' ' _platon_squeeze_details ; ; # Attachment '[(R)-2Ag]3(BF4)3.cif' data_20100928_S3_WSP _database_code_depnum_ccdc_archive 'CCDC 836085' #TrackingRef '[(R)-2Ag]3(BF4)3.cif' _audit_creation_date 2011-02-11 _audit_creation_method ; Olex2 1.1 (compiled 2011.01.21 svn.r1625, GUI svn.r3464) ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '3(C30 H28 Ag N6 O2), 8.99991(B1 F2)' _chemical_formula_sum 'C90 H84 Ag3 B3 F12 N18 O6' _chemical_formula_weight 2097.77 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z+1/2' 3 '-y, x-y, z' 4 '-x, -y, z+1/2' 5 '-x+y, -x, z' 6 'y, -x+y, z+1/2' _cell_length_a 17.3366(4) _cell_length_b 17.3366(4) _cell_length_c 18.9739(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4938.72(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8832 _cell_measurement_temperature 294.15 _cell_measurement_theta_max 29.2052 _cell_measurement_theta_min 3.177 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.89193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2124 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 15602 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.18 _diffrn_ambient_temperature 294.15 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 60.00 86.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 20.1736 77.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -32.00 45.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 20.1736 -77.0000 -150.0000 77 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 27.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 20.1736 77.0000 -30.0000 37 #__ type_ start__ end____ width___ exp.time_ 4 omega -43.00 -18.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -17.0486 38.0000 30.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0162494 _diffrn_orient_matrix_UB_12 0.0294363 _diffrn_orient_matrix_UB_13 -0.007227 _diffrn_orient_matrix_UB_21 0.044353 _diffrn_orient_matrix_UB_22 0.0361612 _diffrn_orient_matrix_UB_23 -0.0016934 _diffrn_orient_matrix_UB_31 0.001145 _diffrn_orient_matrix_UB_32 -0.0075078 _diffrn_orient_matrix_UB_33 -0.0366542 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5038 _reflns_number_total 6563 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.831 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.088 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constro _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 6563 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0350 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.1095 _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. ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 0.164133(19) 0.704824(18) 0.00157(2) 0.03502(10) Uani 1 1 d . . . F1 F 0.3333 0.6667 -0.2293(6) 0.175(5) Uani 1 3 d S . . F2 F 0.2597(2) 0.5910(2) -0.1394(3) 0.0913(15) Uani 1 1 d . . . F3 F 0.3333 0.6667 0.0321(4) 0.121(3) Uani 1 3 d S . . F4 F 0.2479(2) 0.6147(3) 0.1261(2) 0.0822(13) Uani 1 1 d . . . F5 F 0.3333 0.6667 0.3168(5) 0.102(2) Uani 1 3 d S . . F6 F 0.3894(5) 0.6387(5) 0.4113(3) 0.156(3) Uani 1 1 d . . . O1 O 0.1625(3) 0.7255(3) 0.3033(3) 0.0635(14) Uani 1 1 d . . . O2 O 0.1226(3) 0.7098(2) -0.2947(2) 0.0566(11) Uani 1 1 d . . . N1 N 0.1902(3) 0.7526(3) 0.16085(19) 0.0344(9) Uani 1 1 d . . . N2 N 0.3056(3) 0.8866(3) 0.17228(18) 0.0400(9) Uani 1 1 d . . . N3 N 0.2832(2) 0.8616(2) 0.10238(18) 0.0304(8) Uani 1 1 d . . . N4 N 0.1310(3) 0.6676(3) -0.1579(2) 0.0320(9) Uani 1 1 d . . . N5 N 0.0589(3) 0.5239(3) -0.1753(2) 0.0398(9) Uani 1 1 d . . . N6 N 0.0767(2) 0.5461(2) -0.10468(18) 0.0338(8) Uani 1 1 d . . . C1 C 0.2152(3) 0.7808(3) 0.0937(2) 0.0323(10) Uani 1 1 d . . . C2 C 0.2470(3) 0.8170(3) 0.2061(2) 0.0402(11) Uani 1 1 d . . . C3 C 0.2426(4) 0.8018(4) 0.2835(3) 0.0561(15) Uani 1 1 d . . . H3A H 0.2925 0.7948 0.2979 0.067 Uiso 1 1 calc R . . H3B H 0.2476 0.8534 0.3077 0.067 Uiso 1 1 calc R . . C4 C 0.1477(4) 0.6518(4) 0.2583(3) 0.0542(14) Uani 1 1 d . . . H4A H 0.1026 0.5962 0.2790 0.065 Uiso 1 1 calc R . . H4B H 0.2023 0.6496 0.2541 0.065 Uiso 1 1 calc R . . C5 C 0.1170(4) 0.6639(4) 0.1847(3) 0.0408(12) Uani 1 1 d . . . H5 H 0.1133 0.6175 0.1530 0.049 Uiso 1 1 calc R . . C6 C 0.0278(3) 0.6603(4) 0.1866(3) 0.0523(13) Uani 1 1 d . . . H6A H -0.0142 0.6074 0.2123 0.063 Uiso 1 1 calc R . . H6B H 0.0348 0.7115 0.2127 0.063 Uiso 1 1 calc R . . C7 C -0.0114(3) 0.6592(4) 0.1163(3) 0.0517(14) Uani 1 1 d . . . C7CA C 0.1142(4) 0.9242(4) -0.2247(4) 0.0714(19) Uani 1 1 d . . . H7C H 0.0773 0.8867 -0.2600 0.086 Uiso 1 1 calc R . . C8 C -0.0498(4) 0.5816(5) 0.0736(4) 0.0762(19) Uani 1 1 d . . . H8 H -0.0490 0.5311 0.0889 0.091 Uiso 1 1 calc R . . C9 C -0.0882(5) 0.5803(6) 0.0096(5) 0.087(2) Uani 1 1 d . . . H9 H -0.1162 0.5279 -0.0164 0.105 Uiso 1 1 calc R . . C10 C -0.0858(5) 0.6525(7) -0.0148(4) 0.096(3) Uani 1 1 d . . . H10 H -0.1096 0.6513 -0.0590 0.115 Uiso 1 1 calc R . . C11 C -0.0501(7) 0.7261(8) 0.0225(4) 0.111(3) Uani 1 1 d . . . H11 H -0.0510 0.7755 0.0044 0.133 Uiso 1 1 calc R . . C12 C -0.0107(5) 0.7334(5) 0.0883(4) 0.085(2) Uani 1 1 d . . . H12 H 0.0156 0.7870 0.1128 0.102 Uiso 1 1 calc R . . C13 C 0.3397(3) 0.9222(3) 0.0483(2) 0.0319(9) Uani 1 1 d . . . C14 C 0.3748(2) 0.8923(2) -0.0031(3) 0.0302(8) Uani 1 1 d . . . H14 H 0.3618 0.8334 -0.0038 0.036 Uiso 1 1 calc R . . C15 C -0.0399(3) 0.4103(3) -0.0525(3) 0.0439(12) Uani 1 1 d . . . H15 H -0.0792 0.4085 -0.0867 0.053 Uiso 1 1 calc R . . C16 C 0.0475(3) 0.4776(3) -0.0539(2) 0.0304(9) Uani 1 1 d . . . C17 C 0.4149(3) 1.0705(2) -0.0002(4) 0.0415(9) Uani 1 1 d . . . H17 H 0.4275 1.1293 0.0001 0.050 Uiso 1 1 calc R . . C18 C 0.3603(3) 1.0104(3) 0.0515(3) 0.0418(11) Uani 1 1 d . . . H18 H 0.3379 1.0295 0.0878 0.050 Uiso 1 1 calc R . . C19 C 0.1199(3) 0.6336(3) -0.0929(2) 0.0317(9) Uani 1 1 d . . . C20 C 0.0945(3) 0.6009(3) -0.2059(2) 0.0381(11) Uani 1 1 d . . . C21 C 0.1013(4) 0.6209(4) -0.2838(3) 0.0533(14) Uani 1 1 d . . . H21A H 0.1469 0.6114 -0.3046 0.064 Uiso 1 1 calc R . . H21B H 0.0450 0.5809 -0.3065 0.064 Uiso 1 1 calc R . . C22 C 0.1966(3) 0.7717(3) -0.2542(3) 0.0450(12) Uani 1 1 d . . . H22B H 0.2159 0.8317 -0.2704 0.054 Uiso 1 1 calc R . . H22A H 0.2456 0.7604 -0.2602 0.054 Uiso 1 1 calc R . . C23 C 0.1709(3) 0.7633(3) -0.1771(3) 0.0371(11) Uani 1 1 d . . . H23 H 0.2244 0.7989 -0.1486 0.045 Uiso 1 1 calc R . . C24 C 0.1018(4) 0.7920(3) -0.1613(3) 0.0536(13) Uani 1 1 d . . . H24B H 0.0519 0.7614 -0.1934 0.064 Uiso 1 1 calc R . . H24A H 0.0796 0.7740 -0.1137 0.064 Uiso 1 1 calc R . . C25 C 0.1392(3) 0.8911(3) -0.1685(3) 0.0540(14) Uani 1 1 d . . . C26 C 0.2030(5) 0.9514(5) -0.1230(4) 0.085(2) Uani 1 1 d . . . H26 H 0.2236 0.9310 -0.0863 0.102 Uiso 1 1 calc R . . C27 C 0.2364(6) 1.0419(6) -0.1315(6) 0.114(3) Uani 1 1 d . . . H27 H 0.2823 1.0812 -0.1022 0.137 Uiso 1 1 calc R . . C28 C 0.2066(6) 1.0733(5) -0.1780(7) 0.116(4) Uani 1 1 d . . . H28 H 0.2252 1.1338 -0.1787 0.140 Uiso 1 1 calc R . . C29 C 0.1467(6) 1.0171(6) -0.2269(5) 0.101(3) Uani 1 1 d . . . H29 H 0.1270 1.0404 -0.2622 0.122 Uiso 1 1 calc R . . B1 B 0.3333 0.6667 -0.1643(9) 0.067(3) Uani 1 3 d S . . B2 B 0.3333 0.6667 0.1063(7) 0.046(2) Uani 1 3 d S . . B3 B 0.3333 0.6667 0.3957(11) 0.089(5) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03957(17) 0.03223(16) 0.02762(15) -0.0038(2) -0.0033(2) 0.01370(13) F1 0.208(8) 0.208(8) 0.110(9) 0.000 0.000 0.104(4) F2 0.0427(19) 0.0400(19) 0.181(5) -0.006(2) 0.015(2) 0.0131(16) F3 0.147(5) 0.147(5) 0.069(5) 0.000 0.000 0.073(2) F4 0.048(2) 0.053(2) 0.139(4) -0.003(2) 0.027(2) 0.0200(17) F5 0.105(4) 0.105(4) 0.095(5) 0.000 0.000 0.0523(18) F6 0.190(6) 0.219(7) 0.129(5) 0.009(5) -0.031(4) 0.156(6) O1 0.062(3) 0.090(3) 0.031(2) 0.009(2) 0.0101(19) 0.033(3) O2 0.073(3) 0.047(2) 0.039(2) 0.0076(17) -0.010(2) 0.022(2) N1 0.033(2) 0.040(2) 0.028(2) 0.0014(18) 0.0037(17) 0.0164(18) N2 0.049(2) 0.042(2) 0.028(2) -0.0067(17) -0.0028(17) 0.022(2) N3 0.0322(19) 0.034(2) 0.0230(17) 0.0004(16) 0.0048(15) 0.0153(17) N4 0.031(2) 0.0287(19) 0.035(2) -0.0036(18) -0.0052(18) 0.0137(18) N5 0.042(2) 0.037(2) 0.0299(19) -0.0034(17) -0.0126(18) 0.0123(18) N6 0.034(2) 0.033(2) 0.0302(19) -0.0067(16) -0.0108(16) 0.0137(17) C1 0.033(2) 0.039(3) 0.029(2) 0.0002(19) 0.0037(19) 0.021(2) C2 0.043(3) 0.049(3) 0.030(2) -0.005(2) 0.000(2) 0.024(2) C3 0.052(3) 0.075(4) 0.030(3) 0.001(3) 0.000(2) 0.023(3) C4 0.048(3) 0.065(4) 0.043(3) 0.019(3) 0.010(3) 0.023(3) C5 0.034(3) 0.046(3) 0.038(3) 0.005(2) 0.004(2) 0.017(3) C6 0.041(3) 0.062(3) 0.050(3) 0.008(3) 0.006(2) 0.022(3) C7 0.033(3) 0.063(4) 0.057(3) 0.004(3) 0.005(2) 0.023(3) C7CA 0.055(4) 0.055(4) 0.107(5) 0.022(4) 0.010(4) 0.030(3) C8 0.073(4) 0.083(5) 0.072(4) -0.007(4) -0.013(4) 0.039(4) C9 0.086(4) 0.119(6) 0.068(5) -0.025(5) -0.025(5) 0.060(4) C10 0.094(6) 0.154(8) 0.078(6) -0.022(5) -0.029(4) 0.091(6) C11 0.147(8) 0.147(8) 0.094(7) 0.009(6) -0.021(5) 0.115(8) C12 0.113(6) 0.091(5) 0.082(5) -0.010(4) -0.026(4) 0.074(5) C13 0.036(2) 0.032(2) 0.026(2) -0.0007(18) -0.0025(19) 0.016(2) C14 0.0352(19) 0.0256(17) 0.031(2) -0.006(3) -0.005(2) 0.0157(15) C15 0.033(3) 0.047(3) 0.043(3) -0.003(2) -0.011(2) 0.013(2) C16 0.032(2) 0.029(2) 0.029(2) 0.0005(18) -0.0002(18) 0.0141(18) C17 0.060(3) 0.0253(19) 0.034(2) 0.000(3) -0.003(4) 0.0174(18) C18 0.058(3) 0.040(3) 0.037(3) -0.006(2) -0.001(2) 0.032(2) C19 0.028(2) 0.033(2) 0.033(2) -0.0002(19) -0.0004(18) 0.015(2) C20 0.037(3) 0.038(3) 0.034(2) -0.006(2) -0.011(2) 0.015(2) C21 0.070(4) 0.050(3) 0.034(3) 0.001(2) -0.016(3) 0.026(3) C22 0.051(3) 0.038(3) 0.037(3) 0.005(2) -0.001(3) 0.016(2) C23 0.033(2) 0.030(2) 0.048(3) -0.001(2) -0.007(2) 0.015(2) C24 0.048(3) 0.043(3) 0.071(4) 0.011(3) 0.005(3) 0.024(3) C25 0.043(3) 0.044(3) 0.086(4) -0.002(3) -0.001(3) 0.031(3) C26 0.092(5) 0.063(4) 0.115(6) -0.013(4) -0.016(5) 0.051(4) C27 0.112(7) 0.072(5) 0.178(9) -0.048(6) -0.063(7) 0.060(5) C28 0.077(5) 0.046(4) 0.228(12) -0.010(6) -0.019(7) 0.033(4) C29 0.091(6) 0.086(6) 0.158(9) 0.044(6) 0.021(6) 0.067(5) B1 0.056(5) 0.056(5) 0.089(10) 0.000 0.000 0.028(2) B2 0.031(3) 0.031(3) 0.077(8) 0.000 0.000 0.0155(15) B3 0.072(6) 0.072(6) 0.123(15) 0.000 0.000 0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C1 2.099(4) . ? Ag1 C19 2.093(4) . ? F1 B1 1.235(18) . ? F2 B1 1.378(7) . ? F3 B2 1.409(14) . ? F4 B2 1.346(5) . ? F5 B3 1.50(2) . ? F6 B3 1.319(7) . ? O1 C3 1.408(7) . ? O1 C4 1.448(8) . ? O2 C21 1.410(6) . ? O2 C22 1.417(6) . ? N1 C1 1.356(6) . ? N1 C2 1.360(6) . ? N1 C5 1.494(7) . ? N2 N3 1.389(5) . ? N2 C2 1.294(6) . ? N3 C1 1.315(6) . ? N3 C13 1.445(5) . ? N4 C19 1.338(6) . ? N4 C20 1.355(6) . ? N4 C23 1.489(7) . ? N5 N6 1.386(5) . ? N5 C20 1.294(6) . ? N6 C16 1.412(6) . ? N6 C19 1.332(6) . ? C2 C3 1.489(6) . ? C4 C5 1.545(8) . ? C5 C6 1.519(7) . ? C6 C7 1.493(8) . ? C7 C8 1.418(9) . ? C7 C12 1.386(9) . ? C7CA C25 1.380(9) . ? C7CA C29 1.416(10) . ? C8 C9 1.379(10) . ? C9 C10 1.315(11) . ? C10 C11 1.313(11) . ? C11 C12 1.399(10) . ? C13 C14 1.382(7) . ? C13 C18 1.385(6) . ? C14 C16 1.391(7) 5_565 ? C15 C16 1.374(6) . ? C15 C17 1.402(8) 3_665 ? C16 C14 1.391(7) 3_665 ? C17 C15 1.402(8) 5_565 ? C17 C18 1.399(8) . ? C20 C21 1.510(7) . ? C22 C23 1.515(7) . ? C23 C24 1.540(7) . ? C24 C25 1.509(7) . ? C25 C26 1.379(9) . ? C26 C27 1.383(10) . ? C27 C28 1.275(13) . ? C28 C29 1.371(13) . ? B1 F2 1.378(7) 5_565 ? B1 F2 1.378(7) 3_665 ? B2 F4 1.346(5) 5_565 ? B2 F4 1.346(5) 3_665 ? B3 F6 1.319(7) 5_565 ? B3 F6 1.319(7) 3_665 ? 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 C19 Ag1 C1 176.90(17) . . ? C3 O1 C4 109.1(4) . . ? C21 O2 C22 113.0(4) . . ? C1 N1 C2 109.1(4) . . ? C1 N1 C5 127.6(4) . . ? C2 N1 C5 123.2(4) . . ? C2 N2 N3 102.4(4) . . ? N2 N3 C13 118.0(3) . . ? C1 N3 N2 114.4(3) . . ? C1 N3 C13 127.4(4) . . ? C19 N4 C20 109.9(4) . . ? C19 N4 C23 126.9(4) . . ? C20 N4 C23 123.0(4) . . ? C20 N5 N6 102.8(4) . . ? N5 N6 C16 119.3(3) . . ? C19 N6 N5 113.5(4) . . ? C19 N6 C16 127.1(4) . . ? N1 C1 Ag1 126.7(3) . . ? N3 C1 Ag1 130.2(3) . . ? N3 C1 N1 102.7(4) . . ? N1 C2 C3 121.7(5) . . ? N2 C2 N1 111.2(4) . . ? N2 C2 C3 126.9(5) . . ? O1 C3 C2 111.6(5) . . ? O1 C4 C5 109.6(5) . . ? N1 C5 C4 103.9(4) . . ? N1 C5 C6 111.8(4) . . ? C6 C5 C4 112.7(4) . . ? C7 C6 C5 115.3(5) . . ? C8 C7 C6 121.2(6) . . ? C12 C7 C6 122.5(6) . . ? C12 C7 C8 116.3(6) . . ? C25 C7CA C29 117.8(7) . . ? C9 C8 C7 120.8(7) . . ? C10 C9 C8 120.6(8) . . ? C11 C10 C9 120.7(8) . . ? C10 C11 C12 122.7(8) . . ? C7 C12 C11 118.7(8) . . ? C14 C13 N3 119.6(4) . . ? C14 C13 C18 121.7(4) . . ? C18 C13 N3 118.6(4) . . ? C13 C14 C16 118.3(4) . 5_565 ? C16 C15 C17 120.8(4) . 3_665 ? C14 C16 N6 118.6(4) 3_665 . ? C15 C16 N6 120.4(4) . . ? C15 C16 C14 120.9(4) . 3_665 ? C18 C17 C15 118.4(4) . 5_565 ? C13 C18 C17 119.8(4) . . ? N4 C19 Ag1 126.8(3) . . ? N6 C19 Ag1 130.3(3) . . ? N6 C19 N4 102.8(4) . . ? N4 C20 C21 120.8(4) . . ? N5 C20 N4 110.9(4) . . ? N5 C20 C21 128.2(4) . . ? O2 C21 C20 110.1(4) . . ? O2 C22 C23 109.9(4) . . ? N4 C23 C22 107.1(4) . . ? N4 C23 C24 108.0(4) . . ? C22 C23 C24 113.3(4) . . ? C25 C24 C23 112.9(4) . . ? C7CA C25 C24 119.8(5) . . ? C26 C25 C7CA 117.9(6) . . ? C26 C25 C24 122.1(5) . . ? C25 C26 C27 120.6(7) . . ? C28 C27 C26 122.4(8) . . ? C27 C28 C29 119.3(7) . . ? C28 C29 C7CA 121.1(8) . . ? F1 B1 F2 110.0(7) . 5_565 ? F1 B1 F2 110.0(7) . . ? F1 B1 F2 110.0(7) . 3_665 ? F2 B1 F2 108.9(7) 3_665 . ? F2 B1 F2 108.9(7) 3_665 5_565 ? F2 B1 F2 108.9(7) 5_565 . ? F4 B2 F3 106.2(6) 5_565 . ? F4 B2 F3 106.2(6) 3_665 . ? F4 B2 F3 106.2(6) . . ? F4 B2 F4 112.6(5) 3_665 . ? F4 B2 F4 112.6(5) . 5_565 ? F4 B2 F4 112.6(5) 3_665 5_565 ? F6 B3 F5 102.9(9) . . ? F6 B3 F5 102.9(9) 3_665 . ? F6 B3 F5 102.9(9) 5_565 . ? F6 B3 F6 115.1(7) 3_665 . ? F6 B3 F6 115.1(7) 3_665 5_565 ? F6 B3 F6 115.2(7) 5_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C5 N1 57.2(5) . . . . ? O1 C4 C5 C6 -64.1(6) . . . . ? O2 C22 C23 N4 52.2(5) . . . . ? O2 C22 C23 C24 -66.8(5) . . . . ? N1 C2 C3 O1 -14.7(8) . . . . ? N1 C5 C6 C7 71.2(6) . . . . ? N2 N3 C1 Ag1 -171.5(3) . . . . ? N2 N3 C1 N1 1.9(4) . . . . ? N2 N3 C13 C14 126.1(4) . . . . ? N2 N3 C13 C18 -51.1(5) . . . . ? N2 C2 C3 O1 170.5(5) . . . . ? N3 N2 C2 N1 -0.9(5) . . . . ? N3 N2 C2 C3 174.4(5) . . . . ? N3 C13 C14 C16 -179.0(4) . . . 5_565 ? N3 C13 C18 C17 -180.0(4) . . . . ? N4 C20 C21 O2 -18.2(7) . . . . ? N4 C23 C24 C25 171.4(5) . . . . ? N5 N6 C16 C14 131.5(4) . . . 3_665 ? N5 N6 C16 C15 -52.0(6) . . . . ? N5 N6 C19 Ag1 -179.7(3) . . . . ? N5 N6 C19 N4 -1.0(5) . . . . ? N5 C20 C21 O2 164.2(5) . . . . ? N6 N5 C20 N4 -1.1(5) . . . . ? N6 N5 C20 C21 176.6(5) . . . . ? C1 Ag1 C19 N4 -45(3) . . . . ? C1 Ag1 C19 N6 133(3) . . . . ? C1 N1 C2 N2 2.2(5) . . . . ? C1 N1 C2 C3 -173.4(5) . . . . ? C1 N1 C5 C4 152.5(4) . . . . ? C1 N1 C5 C6 -85.7(6) . . . . ? C1 N3 C13 C14 -48.2(6) . . . . ? C1 N3 C13 C18 134.6(5) . . . . ? C2 N1 C1 Ag1 171.4(3) . . . . ? C2 N1 C1 N3 -2.4(5) . . . . ? C2 N1 C5 C4 -23.0(6) . . . . ? C2 N1 C5 C6 98.9(5) . . . . ? C2 N2 N3 C1 -0.7(5) . . . . ? C2 N2 N3 C13 -175.7(4) . . . . ? C3 O1 C4 C5 -74.8(6) . . . . ? C4 O1 C3 C2 49.1(7) . . . . ? C4 C5 C6 C7 -172.1(5) . . . . ? C5 N1 C1 Ag1 -4.6(6) . . . . ? C5 N1 C1 N3 -178.4(4) . . . . ? C5 N1 C2 N2 178.4(4) . . . . ? C5 N1 C2 C3 2.8(7) . . . . ? C5 C6 C7 C8 74.1(7) . . . . ? C5 C6 C7 C12 -104.2(7) . . . . ? C6 C7 C8 C9 178.0(6) . . . . ? C6 C7 C12 C11 -179.1(7) . . . . ? C7 C8 C9 C10 3.8(11) . . . . ? C7CA C25 C26 C27 3.8(11) . . . . ? C8 C7 C12 C11 2.5(10) . . . . ? C8 C9 C10 C11 -2.9(13) . . . . ? C9 C10 C11 C12 2.0(15) . . . . ? C10 C11 C12 C7 -1.8(14) . . . . ? C12 C7 C8 C9 -3.5(10) . . . . ? C13 N3 C1 Ag1 2.9(6) . . . . ? C13 N3 C1 N1 176.4(4) . . . . ? C14 C13 C18 C17 2.9(7) . . . . ? C15 C17 C18 C13 -2.5(8) 5_565 . . . ? C16 N6 C19 Ag1 1.6(7) . . . . ? C16 N6 C19 N4 -179.8(4) . . . . ? C17 C15 C16 N6 -176.9(5) 3_665 . . . ? C17 C15 C16 C14 -0.5(8) 3_665 . . 3_665 ? C18 C13 C14 C16 -1.9(7) . . . 5_565 ? C19 Ag1 C1 N1 -152(3) . . . . ? C19 Ag1 C1 N3 20(3) . . . . ? C19 N4 C20 N5 0.6(6) . . . . ? C19 N4 C20 C21 -177.3(4) . . . . ? C19 N4 C23 C22 161.9(4) . . . . ? C19 N4 C23 C24 -75.7(6) . . . . ? C19 N6 C16 C14 -49.8(6) . . . 3_665 ? C19 N6 C16 C15 126.7(5) . . . . ? C20 N4 C19 Ag1 179.0(3) . . . . ? C20 N4 C19 N6 0.3(5) . . . . ? C20 N4 C23 C22 -22.9(6) . . . . ? C20 N4 C23 C24 99.5(5) . . . . ? C20 N5 N6 C16 -179.8(4) . . . . ? C20 N5 N6 C19 1.4(5) . . . . ? C21 O2 C22 C23 -70.8(6) . . . . ? C22 O2 C21 C20 50.1(7) . . . . ? C22 C23 C24 C25 -70.0(6) . . . . ? C23 N4 C19 Ag1 -5.3(6) . . . . ? C23 N4 C19 N6 176.0(4) . . . . ? C23 N4 C20 N5 -175.4(4) . . . . ? C23 N4 C20 C21 6.7(7) . . . . ? C23 C24 C25 C7CA 108.0(6) . . . . ? C23 C24 C25 C26 -67.5(8) . . . . ? C24 C25 C26 C27 179.4(7) . . . . ? C25 C7CA C29 C28 5.1(11) . . . . ? C25 C26 C27 C28 4.5(15) . . . . ? C26 C27 C28 C29 -7.8(17) . . . . ? C27 C28 C29 C7CA 3.0(15) . . . . ? C29 C7CA C25 C24 176.1(6) . . . . ? C29 C7CA C25 C26 -8.2(9) . . . . ? # Attachment '[(S)-2Ag]3(BF4)3.cif' data_20100728_S2_HP2_2 _database_code_depnum_ccdc_archive 'CCDC 836086' #TrackingRef '[(S)-2Ag]3(BF4)3.cif' _audit_creation_date 2011-03-06 _audit_creation_method ; Olex2 1.1 (compiled 2011.01.21 svn.r1625, GUI svn.r3464) ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '3(C30 H28 Ag N6 O2), 9(B0.3333 F1.3333)' _chemical_formula_sum 'C90 H84 Ag3 B3 F12 N18 O6' _chemical_formula_weight 2097.79 _chemical_absolute_configuration ad _chemical_melting_point ? 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z+1/2' 3 '-y, x-y, z' 4 '-x, -y, z+1/2' 5 '-x+y, -x, z' 6 'y, -x+y, z+1/2' _cell_length_a 17.3399(3) _cell_length_b 17.3399(3) _cell_length_c 18.6738(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4862.46(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8711 _cell_measurement_temperature 567.3 _cell_measurement_theta_max 28.8906 _cell_measurement_theta_min 3.2 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.96443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2124 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13681 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.21 _diffrn_ambient_temperature 567.3 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 34.00 101.20 0.8000 3.0000 omega____ theta____ kappa____ phi______ frames - 22.7314 179.0000 -60.0000 84 #__ type_ start__ end____ width___ exp.time_ 2 omega -37.00 27.00 0.8000 3.0000 omega____ theta____ kappa____ phi______ frames - 22.7314 -38.0000 -30.0000 80 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 8.60 0.8000 3.0000 omega____ theta____ kappa____ phi______ frames - -19.8407 -104.0000 35.0000 37 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0033221 _diffrn_orient_matrix_UB_12 0.0416843 _diffrn_orient_matrix_UB_13 -0.0073543 _diffrn_orient_matrix_UB_21 -0.0452539 _diffrn_orient_matrix_UB_22 -0.0221232 _diffrn_orient_matrix_UB_23 -0.0108662 _diffrn_orient_matrix_UB_31 -0.0131344 _diffrn_orient_matrix_UB_32 0.001846 _diffrn_orient_matrix_UB_33 0.0356461 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5190 _reflns_number_total 6407 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.928 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.100 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 397 _refine_ls_number_reflns 6407 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1156 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.457537(19) -0.293460(18) -0.50582(3) 0.03399(11) Uani 1 1 d . . . F1 F -0.6667 -0.3333 -0.7402(8) 0.181(5) Uani 1 3 d S . . F2 F -0.6691(3) -0.4090(2) -0.6472(3) 0.0925(14) Uani 1 1 d . . . F3 F -0.6667 -0.3333 -0.4737(5) 0.153(4) Uani 1 3 d S . . F4 F -0.6327(3) -0.3850(3) -0.3835(3) 0.0976(16) Uani 1 1 d . . . F5 F -0.6667 -0.3333 -0.1615(14) 0.249(8) Uani 1 3 d S . . F6 F -0.6380(8) -0.3894(7) -0.0925(7) 0.242(5) Uani 1 1 d . . . O1 O -0.4129(3) -0.2877(2) -0.8075(2) 0.0548(11) Uani 1 1 d . . . O2 O -0.8341(3) -0.5610(4) -0.1996(3) 0.0629(14) Uani 1 1 d . . . N1 N -0.4631(2) -0.3297(3) -0.6681(2) 0.0307(9) Uani 1 1 d . . . N2 N -0.5281(2) -0.4515(2) -0.61373(17) 0.0315(8) Uani 1 1 d . . . N3 N -0.5340(3) -0.4739(3) -0.68614(19) 0.0379(9) Uani 1 1 d . . . N4 N -0.8085(3) -0.5631(3) -0.34439(18) 0.0338(9) Uani 1 1 d . . . N5 N -0.7152(2) -0.5788(2) -0.40410(17) 0.0304(8) Uani 1 1 d . . . N6 N -0.6915(3) -0.5808(3) -0.33336(18) 0.0414(9) Uani 1 1 d . . . C1 C -0.2517(5) -0.0483(5) -0.6308(4) 0.084(2) Uani 1 1 d . . . H1 H -0.2949 -0.0702 -0.5951 0.101 Uiso 1 1 calc R . . C2 C -0.1949(6) 0.0411(6) -0.6347(6) 0.120(4) Uani 1 1 d . . . H2 H -0.2003 0.0790 -0.6025 0.144 Uiso 1 1 calc R . . C3 C -0.1318(6) 0.0743(5) -0.6843(8) 0.131(5) Uani 1 1 d . . . H3 H -0.0917 0.1352 -0.6855 0.157 Uiso 1 1 calc R . . C4 C -0.1254(5) 0.0208(6) -0.7326(5) 0.097(3) Uani 1 1 d . . . H4 H -0.0802 0.0442 -0.7667 0.116 Uiso 1 1 calc R . . C5 C -0.1884(4) -0.0725(4) -0.7318(4) 0.0691(18) Uani 1 1 d . . . H5 H -0.1887 -0.1092 -0.7682 0.083 Uiso 1 1 calc R . . C6 C -0.2480(3) -0.1070(4) -0.6770(3) 0.0523(13) Uani 1 1 d . . . C7 C -0.3097(3) -0.2063(3) -0.6717(3) 0.0509(13) Uani 1 1 d . . . H7A H -0.3058 -0.2258 -0.6239 0.061 Uiso 1 1 calc R . . H7B H -0.2901 -0.2359 -0.7052 0.061 Uiso 1 1 calc R . . C8 C -0.4067(3) -0.2346(3) -0.6877(2) 0.0343(10) Uani 1 1 d . . . H8 H -0.4240 -0.1989 -0.6583 0.041 Uiso 1 1 calc R . . C9 C -0.4250(3) -0.2258(3) -0.7652(2) 0.0451(12) Uani 1 1 d . . . H9B H -0.4856 -0.2374 -0.7704 0.054 Uiso 1 1 calc R . . H9A H -0.3848 -0.1656 -0.7815 0.054 Uiso 1 1 calc R . . C10 C -0.4806(4) -0.3756(4) -0.7953(2) 0.0495(13) Uani 1 1 d . . . H10A H -0.4654 -0.4161 -0.8188 0.059 Uiso 1 1 calc R . . H10B H -0.5357 -0.3844 -0.8161 0.059 Uiso 1 1 calc R . . C11 C -0.4941(3) -0.3965(3) -0.7172(2) 0.0360(10) Uani 1 1 d . . . C12 C -0.4851(3) -0.3645(3) -0.6018(2) 0.0311(9) Uani 1 1 d . . . C13 C -0.5673(3) -0.5211(3) -0.5618(2) 0.0288(8) Uani 1 1 d . . . C14 C -0.5451(3) -0.5864(3) -0.5606(3) 0.0416(11) Uani 1 1 d . . . H14 H -0.5065 -0.5870 -0.5948 0.050 Uiso 1 1 calc R . . C15 C -0.5807(3) -0.6522(3) -0.5079(4) 0.0415(9) Uani 1 1 d . . . H15 H -0.5673 -0.6979 -0.5074 0.050 Uiso 1 1 calc R . . C16 C -0.6372(3) -0.6484(3) -0.4554(2) 0.0364(10) Uani 1 1 d . . . H16 H -0.6596 -0.6902 -0.4187 0.044 Uiso 1 1 calc R . . C17 C -0.6586(3) -0.5825(3) -0.4591(2) 0.0316(9) Uani 1 1 d . . . C18 C -0.6243(2) -0.5165(2) -0.5106(3) 0.0295(8) Uani 1 1 d . . . H18 H -0.6383 -0.4713 -0.5114 0.035 Uiso 1 1 calc R . . C19 C -0.7840(3) -0.5668(3) -0.4123(2) 0.0319(9) Uani 1 1 d . . . C20 C -0.7508(3) -0.5692(3) -0.2984(2) 0.0403(11) Uani 1 1 d . . . C21 C -0.7537(4) -0.5570(5) -0.2196(2) 0.0604(16) Uani 1 1 d . . . H21B H -0.7483 -0.6031 -0.1946 0.073 Uiso 1 1 calc R . . H21A H -0.7038 -0.4998 -0.2057 0.073 Uiso 1 1 calc R . . C22 C -0.8495(4) -0.5052(4) -0.2450(3) 0.0544(14) Uani 1 1 d . . . H22A H -0.7952 -0.4483 -0.2499 0.065 Uiso 1 1 calc R . . H22B H -0.8945 -0.4945 -0.2239 0.065 Uiso 1 1 calc R . . C23 C -0.8810(4) -0.5482(4) -0.3198(3) 0.0397(12) Uani 1 1 d . . . H23 H -0.8855 -0.5060 -0.3519 0.048 Uiso 1 1 calc R . . C24 C -0.9697(3) -0.6343(4) -0.3172(3) 0.0516(13) Uani 1 1 d . . . H24A H -0.9616 -0.6785 -0.2919 0.062 Uiso 1 1 calc R . . H24B H -1.0112 -0.6240 -0.2897 0.062 Uiso 1 1 calc R . . C25 C -1.0102(3) -0.6712(3) -0.3877(3) 0.0455(12) Uani 1 1 d . . . C26 C -1.0066(5) -0.7406(4) -0.4176(4) 0.0757(19) Uani 1 1 d . . . H26 H -0.9787 -0.7669 -0.3936 0.091 Uiso 1 1 calc R . . C27 C -1.0466(6) -0.7734(5) -0.4875(4) 0.098(3) Uani 1 1 d . . . H27 H -1.0411 -0.8185 -0.5096 0.117 Uiso 1 1 calc R . . C28 C -1.0895(5) -0.7404(5) -0.5189(5) 0.098(3) Uani 1 1 d . . . H28 H -1.1186 -0.7652 -0.5618 0.118 Uiso 1 1 calc R . . C29 C -1.0934(5) -0.6730(5) -0.4922(4) 0.085(2) Uani 1 1 d . . . H29 H -1.1229 -0.6494 -0.5176 0.102 Uiso 1 1 calc R . . C30 C -1.0554(5) -0.6361(5) -0.4281(4) 0.0734(18) Uani 1 1 d . . . H30 H -1.0589 -0.5878 -0.4105 0.088 Uiso 1 1 calc R . . B1 B -0.6667 -0.3333 -0.6708(12) 0.077(5) Uani 1 3 d S . . B2 B -0.6667 -0.3333 -0.3978(6) 0.045(2) Uani 1 3 d S . . B3 B -0.6667 -0.3333 -0.0877(12) 0.099(6) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04450(19) 0.03121(16) 0.02533(15) -0.00348(19) -0.0003(2) 0.01823(13) F1 0.202(9) 0.202(9) 0.140(10) 0.000 0.000 0.101(5) F2 0.054(2) 0.039(2) 0.187(5) -0.001(2) -0.012(3) 0.0249(18) F3 0.185(7) 0.185(7) 0.089(7) 0.000 0.000 0.092(3) F4 0.058(2) 0.049(2) 0.188(5) -0.009(3) -0.033(3) 0.0288(19) F5 0.227(12) 0.227(12) 0.29(3) 0.000 0.000 0.113(6) F6 0.294(12) 0.240(10) 0.309(13) 0.036(9) -0.017(9) 0.221(10) O1 0.074(3) 0.046(2) 0.035(2) 0.0068(15) 0.021(2) 0.023(2) O2 0.060(3) 0.086(3) 0.029(2) -0.001(2) 0.0105(18) 0.027(2) N1 0.030(2) 0.028(2) 0.033(2) -0.0022(16) 0.0043(15) 0.0137(16) N2 0.038(2) 0.032(2) 0.0243(17) -0.0052(14) 0.0032(14) 0.0174(17) N3 0.054(2) 0.039(2) 0.0261(18) -0.0031(15) 0.0056(16) 0.027(2) N4 0.034(2) 0.043(2) 0.023(2) 0.0014(15) 0.0036(15) 0.0174(19) N5 0.035(2) 0.039(2) 0.0205(16) 0.0060(14) 0.0043(14) 0.0209(17) N6 0.043(2) 0.055(3) 0.0251(18) 0.0039(16) -0.0023(15) 0.023(2) C1 0.067(4) 0.062(4) 0.092(5) -0.011(4) 0.014(4) 0.007(4) C2 0.073(5) 0.064(5) 0.180(10) -0.053(6) 0.019(6) 0.002(4) C3 0.053(5) 0.035(4) 0.280(15) -0.005(6) -0.015(7) 0.003(4) C4 0.044(4) 0.077(6) 0.155(8) 0.023(5) 0.023(4) 0.020(4) C5 0.043(3) 0.049(3) 0.111(5) 0.019(3) 0.017(3) 0.019(3) C6 0.030(3) 0.045(3) 0.077(4) -0.003(3) -0.002(2) 0.015(2) C7 0.045(3) 0.041(3) 0.067(3) 0.011(2) 0.008(2) 0.022(2) C8 0.033(3) 0.030(2) 0.037(2) 0.0008(19) 0.0071(19) 0.014(2) C9 0.059(3) 0.038(3) 0.035(3) 0.001(2) 0.006(2) 0.022(2) C10 0.067(4) 0.043(3) 0.029(3) 0.000(2) 0.011(2) 0.020(3) C11 0.041(3) 0.037(3) 0.031(2) -0.0026(19) 0.0078(18) 0.021(2) C12 0.033(2) 0.032(2) 0.030(2) -0.0012(17) 0.0025(17) 0.018(2) C13 0.035(2) 0.028(2) 0.0237(19) -0.0053(16) -0.0008(16) 0.0157(18) C14 0.051(3) 0.046(3) 0.038(2) -0.007(2) 0.005(2) 0.032(2) C15 0.061(3) 0.045(2) 0.036(2) 0.004(3) -0.004(3) 0.039(2) C16 0.046(3) 0.031(2) 0.036(2) 0.0029(18) 0.001(2) 0.022(2) C17 0.034(2) 0.040(2) 0.0211(18) 0.0003(17) -0.0006(16) 0.019(2) C18 0.0334(19) 0.0345(19) 0.028(2) 0.003(2) 0.000(2) 0.0223(16) C19 0.032(2) 0.032(2) 0.027(2) 0.0024(16) 0.0038(17) 0.0116(19) C20 0.042(3) 0.044(3) 0.028(2) 0.0049(18) 0.0009(19) 0.017(2) C21 0.049(3) 0.095(5) 0.026(2) 0.003(3) -0.001(2) 0.027(3) C22 0.048(3) 0.070(4) 0.039(3) -0.013(3) 0.009(2) 0.024(3) C23 0.035(3) 0.046(3) 0.036(3) -0.002(2) 0.008(2) 0.019(2) C24 0.042(3) 0.058(3) 0.046(3) -0.003(2) 0.009(2) 0.018(3) C25 0.034(3) 0.042(3) 0.048(3) 0.003(2) 0.009(2) 0.009(2) C26 0.101(5) 0.058(4) 0.070(4) -0.015(3) -0.021(4) 0.040(4) C27 0.123(7) 0.064(5) 0.094(7) -0.027(4) -0.024(5) 0.038(5) C28 0.095(6) 0.060(4) 0.089(7) -0.006(4) -0.035(5) 0.001(4) C29 0.080(5) 0.083(5) 0.082(6) 0.002(4) -0.020(4) 0.033(4) C30 0.068(4) 0.073(4) 0.081(4) -0.013(3) -0.017(3) 0.036(4) B1 0.038(4) 0.038(4) 0.155(17) 0.000 0.000 0.019(2) B2 0.039(4) 0.039(4) 0.059(6) 0.000 0.000 0.0193(18) B3 0.104(10) 0.104(10) 0.091(13) 0.000 0.000 0.052(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C12 2.091(4) . ? Ag1 C19 2.103(4) 3_455 ? F1 B1 1.30(2) . ? F2 B1 1.364(8) . ? F3 B2 1.417(14) . ? F4 B2 1.323(5) . ? F5 B3 1.38(2) . ? F6 B3 1.297(8) . ? O1 C9 1.432(6) . ? O1 C10 1.400(6) . ? O2 C21 1.412(7) . ? O2 C22 1.408(9) . ? N1 C8 1.482(7) . ? N1 C11 1.360(6) . ? N1 C12 1.345(6) . ? N2 N3 1.397(5) . ? N2 C12 1.326(6) . ? N2 C13 1.427(5) . ? N3 C11 1.300(6) . ? N4 C19 1.349(5) . ? N4 C20 1.362(6) . ? N4 C23 1.478(7) . ? N5 N6 1.389(5) . ? N5 C17 1.443(5) . ? N5 C19 1.319(6) . ? N6 C20 1.315(6) . ? C1 H1 0.9300 . ? C1 C2 1.361(10) . ? C1 C6 1.360(9) . ? C2 H2 0.9300 . ? C2 C3 1.325(15) . ? C3 H3 0.9300 . ? C3 C4 1.338(14) . ? C4 H4 0.9300 . ? C4 C5 1.429(10) . ? C5 H5 0.9300 . ? C5 C6 1.361(8) . ? C6 C7 1.509(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.528(7) . ? C8 H8 0.9800 . ? C8 C9 1.506(7) . ? C9 H9B 0.9700 . ? C9 H9A 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.493(6) . ? C13 C14 1.367(6) . ? C13 C18 1.405(6) . ? C14 H14 0.9300 . ? C14 C15 1.396(8) . ? C15 H15 0.9300 . ? C15 C16 1.409(8) . ? C16 H16 0.9300 . ? C16 C17 1.369(6) . ? C17 C18 1.382(7) . ? C18 H18 0.9300 . ? C19 Ag1 2.103(4) 5_445 ? C20 C21 1.491(7) . ? C21 H21B 0.9700 . ? C21 H21A 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.549(7) . ? C23 H23 0.9800 . ? C23 C24 1.516(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 C25 1.479(7) . ? C25 C26 1.355(9) . ? C25 C30 1.424(9) . ? C26 H26 0.9300 . ? C26 C27 1.454(9) . ? C27 H27 0.9300 . ? C27 C28 1.286(11) . ? C28 H28 0.9300 . ? C28 C29 1.302(11) . ? C29 H29 0.9300 . ? C29 C30 1.362(10) . ? C30 H30 0.9300 . ? B1 F2 1.364(8) 3_455 ? B1 F2 1.364(8) 5_445 ? B2 F4 1.323(5) 5_445 ? B2 F4 1.323(5) 3_455 ? B3 F6 1.297(8) 5_445 ? B3 F6 1.297(8) 3_455 ? 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 C12 Ag1 C19 176.29(16) . 3_455 ? C10 O1 C9 111.7(4) . . ? C22 O2 C21 109.3(4) . . ? C11 N1 C8 122.7(4) . . ? C12 N1 C8 127.4(4) . . ? C12 N1 C11 109.7(4) . . ? N3 N2 C13 119.0(3) . . ? C12 N2 N3 113.6(3) . . ? C12 N2 C13 127.4(3) . . ? C11 N3 N2 102.6(4) . . ? C19 N4 C20 109.2(4) . . ? C19 N4 C23 128.1(4) . . ? C20 N4 C23 122.6(4) . . ? N6 N5 C17 117.4(3) . . ? C19 N5 N6 114.6(3) . . ? C19 N5 C17 127.8(3) . . ? C20 N6 N5 101.9(4) . . ? C2 C1 H1 118.7 . . ? C2 C1 C6 122.7(7) . . ? C6 C1 H1 118.7 . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.2(8) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.4(7) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 120.1 . . ? C3 C4 C5 119.8(8) . . ? C5 C4 H4 120.1 . . ? C4 C5 H5 120.4 . . ? C6 C5 C4 119.2(7) . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 117.2(6) . . ? C1 C6 C7 122.7(5) . . ? C5 C6 C7 120.0(5) . . ? C6 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C6 C7 C8 113.1(4) . . ? H7A C7 H7B 107.8 . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? N1 C8 C7 108.5(4) . . ? N1 C8 H8 109.0 . . ? N1 C8 C9 107.1(4) . . ? C7 C8 H8 109.0 . . ? C9 C8 C7 114.1(4) . . ? C9 C8 H8 109.0 . . ? O1 C9 C8 109.7(4) . . ? O1 C9 H9B 109.7 . . ? O1 C9 H9A 109.7 . . ? C8 C9 H9B 109.7 . . ? C8 C9 H9A 109.7 . . ? H9B C9 H9A 108.2 . . ? O1 C10 H10A 109.3 . . ? O1 C10 H10B 109.3 . . ? O1 C10 C11 111.5(4) . . ? H10A C10 H10B 108.0 . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? N1 C11 C10 120.3(4) . . ? N3 C11 N1 111.0(4) . . ? N3 C11 C10 128.7(4) . . ? N1 C12 Ag1 126.5(3) . . ? N2 C12 Ag1 130.3(3) . . ? N2 C12 N1 103.2(4) . . ? C14 C13 N2 119.9(4) . . ? C14 C13 C18 122.2(4) . . ? C18 C13 N2 117.8(4) . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.8(4) . . ? C15 C14 H14 120.1 . . ? C14 C15 H15 120.5 . . ? C14 C15 C16 119.0(4) . . ? C16 C15 H15 120.5 . . ? C15 C16 H16 120.3 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H16 120.3 . . ? C16 C17 N5 118.4(4) . . ? C16 C17 C18 122.8(4) . . ? C18 C17 N5 118.6(4) . . ? C13 C18 H18 121.6 . . ? C17 C18 C13 116.8(3) . . ? C17 C18 H18 121.6 . . ? N4 C19 Ag1 126.5(3) . 5_445 ? N5 C19 Ag1 129.8(3) . 5_445 ? N5 C19 N4 103.3(4) . . ? N4 C20 C21 122.2(5) . . ? N6 C20 N4 111.0(4) . . ? N6 C20 C21 126.6(5) . . ? O2 C21 C20 110.9(5) . . ? O2 C21 H21B 109.5 . . ? O2 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? H21B C21 H21A 108.1 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 C23 110.7(5) . . ? H22A C22 H22B 108.1 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? N4 C23 C22 103.9(4) . . ? N4 C23 H23 109.5 . . ? N4 C23 C24 111.8(4) . . ? C22 C23 H23 109.5 . . ? C24 C23 C22 112.7(4) . . ? C24 C23 H23 109.5 . . ? C23 C24 H24A 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C25 C24 C23 115.3(4) . . ? C25 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C26 C25 C24 121.9(6) . . ? C26 C25 C30 116.2(6) . . ? C30 C25 C24 121.9(5) . . ? C25 C26 H26 120.2 . . ? C25 C26 C27 119.5(7) . . ? C27 C26 H26 120.2 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.2(8) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 119.1 . . ? C27 C28 C29 121.8(9) . . ? C29 C28 H28 119.1 . . ? C28 C29 H29 119.1 . . ? C28 C29 C30 121.9(8) . . ? C30 C29 H29 119.1 . . ? C25 C30 H30 119.9 . . ? C29 C30 C25 120.3(7) . . ? C29 C30 H30 119.9 . . ? F1 B1 F2 108.9(9) . 5_445 ? F1 B1 F2 108.9(9) . . ? F1 B1 F2 108.9(9) . 3_455 ? F2 B1 F2 110.1(9) 5_445 . ? F2 B1 F2 110.1(9) 5_445 3_455 ? F2 B1 F2 110.1(9) 3_455 . ? F4 B2 F3 101.7(6) 3_455 . ? F4 B2 F3 101.7(6) 5_445 . ? F4 B2 F3 101.7(6) . . ? F4 B2 F4 116.0(4) 5_445 3_455 ? F4 B2 F4 116.0(4) 3_455 . ? F4 B2 F4 116.0(4) 5_445 . ? F6 B3 F5 86.1(11) . . ? F6 B3 F5 86.1(11) 3_455 . ? F6 B3 F5 86.1(11) 5_445 . ? F6 B3 F6 119.5(3) 5_445 . ? F6 B3 F6 119.5(3) 5_445 3_455 ? F6 B3 F6 119.5(3) 3_455 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C10 C11 N1 18.6(7) . . . . ? O1 C10 C11 N3 -161.9(5) . . . . ? O2 C22 C23 N4 -57.5(5) . . . . ? O2 C22 C23 C24 63.6(6) . . . . ? N1 C8 C9 O1 -53.5(5) . . . . ? N2 N3 C11 N1 1.4(5) . . . . ? N2 N3 C11 C10 -178.2(5) . . . . ? N2 C13 C14 C15 177.2(4) . . . . ? N2 C13 C18 C17 -177.3(4) . . . . ? N3 N2 C12 Ag1 179.3(3) . . . . ? N3 N2 C12 N1 0.4(5) . . . . ? N3 N2 C13 C14 54.1(6) . . . . ? N3 N2 C13 C18 -129.5(4) . . . . ? N4 C20 C21 O2 14.4(8) . . . . ? N4 C23 C24 C25 -72.7(6) . . . . ? N5 N6 C20 N4 1.7(5) . . . . ? N5 N6 C20 C21 -173.9(5) . . . . ? N5 C17 C18 C13 178.0(4) . . . . ? N6 N5 C17 C16 50.7(5) . . . . ? N6 N5 C17 C18 -125.6(4) . . . . ? N6 N5 C19 Ag1 171.3(3) . . . 5_445 ? N6 N5 C19 N4 -1.6(5) . . . . ? N6 C20 C21 O2 -170.4(5) . . . . ? C1 C2 C3 C4 2.5(18) . . . . ? C1 C6 C7 C8 66.8(8) . . . . ? C2 C1 C6 C5 -4.7(12) . . . . ? C2 C1 C6 C7 178.6(8) . . . . ? C2 C3 C4 C5 1.5(16) . . . . ? C3 C4 C5 C6 -7.2(12) . . . . ? C4 C5 C6 C1 8.5(10) . . . . ? C4 C5 C6 C7 -174.7(6) . . . . ? C5 C6 C7 C8 -109.9(6) . . . . ? C6 C1 C2 C3 -0.9(17) . . . . ? C6 C7 C8 N1 -169.7(4) . . . . ? C6 C7 C8 C9 70.9(6) . . . . ? C7 C8 C9 O1 66.7(5) . . . . ? C8 N1 C11 N3 173.4(4) . . . . ? C8 N1 C11 C10 -7.0(7) . . . . ? C8 N1 C12 Ag1 7.1(6) . . . . ? C8 N1 C12 N2 -173.9(4) . . . . ? C9 O1 C10 C11 -50.0(7) . . . . ? C10 O1 C9 C8 71.0(6) . . . . ? C11 N1 C8 C7 -99.8(5) . . . . ? C11 N1 C8 C9 23.9(6) . . . . ? C11 N1 C12 Ag1 -178.5(3) . . . . ? C11 N1 C12 N2 0.5(5) . . . . ? C12 N1 C8 C7 73.9(6) . . . . ? C12 N1 C8 C9 -162.4(4) . . . . ? C12 N1 C11 N3 -1.3(5) . . . . ? C12 N1 C11 C10 178.3(4) . . . . ? C12 N2 N3 C11 -1.1(5) . . . . ? C12 N2 C13 C14 -126.2(5) . . . . ? C12 N2 C13 C18 50.2(6) . . . . ? C13 N2 N3 C11 178.6(4) . . . . ? C13 N2 C12 Ag1 -0.4(7) . . . . ? C13 N2 C12 N1 -179.3(4) . . . . ? C13 C14 C15 C16 -1.8(8) . . . . ? C14 C13 C18 C17 -1.0(7) . . . . ? C14 C15 C16 C17 2.6(8) . . . . ? C15 C16 C17 N5 -178.8(4) . . . . ? C15 C16 C17 C18 -2.7(7) . . . . ? C16 C17 C18 C13 1.9(7) . . . . ? C17 N5 N6 C20 175.1(4) . . . . ? C17 N5 C19 Ag1 -3.3(6) . . . 5_445 ? C17 N5 C19 N4 -176.2(4) . . . . ? C18 C13 C14 C15 1.0(7) . . . . ? C19 Ag1 C12 N1 49(3) 3_455 . . . ? C19 Ag1 C12 N2 -130(2) 3_455 . . . ? C19 N4 C20 N6 -2.9(6) . . . . ? C19 N4 C20 C21 173.0(5) . . . . ? C19 N4 C23 C22 -152.7(5) . . . . ? C19 N4 C23 C24 85.5(6) . . . . ? C19 N5 N6 C20 0.0(5) . . . . ? C19 N5 C17 C16 -134.9(5) . . . . ? C19 N5 C17 C18 48.8(6) . . . . ? C20 N4 C19 Ag1 -170.6(3) . . . 5_445 ? C20 N4 C19 N5 2.6(5) . . . . ? C20 N4 C23 C22 22.4(6) . . . . ? C20 N4 C23 C24 -99.4(5) . . . . ? C21 O2 C22 C23 74.9(6) . . . . ? C22 O2 C21 C20 -48.7(7) . . . . ? C22 C23 C24 C25 170.8(5) . . . . ? C23 N4 C19 Ag1 5.0(6) . . . 5_445 ? C23 N4 C19 N5 178.2(4) . . . . ? C23 N4 C20 N6 -178.8(4) . . . . ? C23 N4 C20 C21 -2.9(7) . . . . ? C23 C24 C25 C26 102.1(7) . . . . ? C23 C24 C25 C30 -78.1(7) . . . . ? C24 C25 C26 C27 -179.2(6) . . . . ? C24 C25 C30 C29 -178.7(6) . . . . ? C25 C26 C27 C28 -4.0(12) . . . . ? C26 C25 C30 C29 1.2(10) . . . . ? C26 C27 C28 C29 5.0(14) . . . . ? C27 C28 C29 C30 -2.8(14) . . . . ? C28 C29 C30 C25 -0.4(12) . . . . ? C30 C25 C26 C27 0.9(10) . . . . ? # Attachment '[(S)-2Ag]3(PF6)3.cif' data_101117_S7_WSP _database_code_depnum_ccdc_archive 'CCDC 836087' _audit_creation_method SHELXL-97 _chemical_absolute_configuration unk _chemical_formula_moiety '3(C30 H28 Ag N6 O2)' _chemical_formula_sum 'C90 H84 Ag3 N18 O6' _chemical_formula_weight 1837.36 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z+1/2' 3 '-y, x-y, z' 4 '-x, -y, z+1/2' 5 '-x+y, -x, z' 6 'y, -x+y, z+1/2' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 17.2761(2) _cell_length_b 17.2761(2) _cell_length_c 18.7097(2) _cell_measurement_reflns_used 7587 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 29.2227 _cell_measurement_theta_min 2.9266 _cell_volume 4836.01(10) _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.9959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_F_000 1878 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_special_details ? _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -63.00 -38.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - -16.8924 179.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 43.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 -38.0000 120.0000 93 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 17.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 77.0000 150.0000 27 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0036003 _diffrn_orient_matrix_UB_12 0.0351879 _diffrn_orient_matrix_UB_13 -0.0161795 _diffrn_orient_matrix_UB_21 -0.0470568 _diffrn_orient_matrix_UB_22 -0.0280398 _diffrn_orient_matrix_UB_23 -0.0021208 _diffrn_orient_matrix_UB_31 -0.0046042 _diffrn_orient_matrix_UB_32 0.0149361 _diffrn_orient_matrix_UB_33 0.0342107 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13550 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.93 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5251 _reflns_number_total 5881 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 1.249 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.100 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0409 _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 5881 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.1165 _refine_ls_wR_factor_ref 0.1202 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+7.7428P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.16386(2) 0.54117(2) 0.17494(3) 0.01958(11) Uani 1 1 d . . . O1 O -0.1632(3) 0.5619(3) 0.4812(3) 0.0354(11) Uani 1 1 d . . . O2 O -0.1235(3) 0.5887(3) -0.1265(2) 0.0322(10) Uani 1 1 d . . . N1 N -0.1899(3) 0.5630(3) 0.3367(2) 0.0194(9) Uani 1 1 d . . . N2 N -0.2838(3) 0.5792(3) 0.2763(2) 0.0205(9) Uani 1 1 d . . . N3 N -0.3058(3) 0.5826(3) 0.3472(2) 0.0245(10) Uani 1 1 d . . . N4 N -0.0769(3) 0.4701(3) 0.0669(2) 0.0183(8) Uani 1 1 d . . . N5 N -0.0600(3) 0.4646(3) -0.0058(2) 0.0217(9) Uani 1 1 d . . . N6 N -0.1335(3) 0.5362(3) 0.0125(3) 0.0188(10) Uani 1 1 d . . . C1 C -0.2142(3) 0.5673(3) 0.2673(3) 0.0190(10) Uani 1 1 d . . . C2 C -0.2468(4) 0.5708(4) 0.3824(3) 0.0248(11) Uani 1 1 d . . . C3 C -0.2450(4) 0.5588(5) 0.4615(3) 0.0348(14) Uani 1 1 d . . . H3B H -0.2498 0.6066 0.4866 0.042 Uiso 1 1 calc R . . H3A H -0.2966 0.5005 0.4757 0.042 Uiso 1 1 calc R . . C4 C -0.1465(4) 0.5051(4) 0.4356(3) 0.0329(13) Uani 1 1 d . . . H4A H -0.2014 0.4460 0.4313 0.039 Uiso 1 1 calc R . . H4B H -0.0990 0.4960 0.4567 0.039 Uiso 1 1 calc R . . C5 C -0.1174(4) 0.5475(4) 0.3620(3) 0.0239(12) Uani 1 1 d . . . H5 H -0.1124 0.5047 0.3290 0.029 Uiso 1 1 calc R . . C6 C -0.0287(4) 0.6333(4) 0.3655(3) 0.0292(12) Uani 1 1 d . . . H6A H 0.0140 0.6221 0.3927 0.035 Uiso 1 1 calc R . . H6B H -0.0366 0.6783 0.3922 0.035 Uiso 1 1 calc R . . C7 C 0.0118(4) 0.6720(4) 0.2923(3) 0.0294(12) Uani 1 1 d . . . C8 C 0.0074(5) 0.7431(5) 0.2638(3) 0.0450(16) Uani 1 1 d . . . H8 H -0.0184 0.7710 0.2910 0.054 Uiso 1 1 calc R . . C9 C 0.0418(6) 0.7763(6) 0.1921(5) 0.075(3) Uani 1 1 d . . . H9 H 0.0342 0.8222 0.1711 0.090 Uiso 1 1 calc R . . C10 C 0.0828(6) 0.7421(5) 0.1575(4) 0.067(3) Uani 1 1 d . . . H10 H 0.1078 0.7656 0.1120 0.080 Uiso 1 1 calc R . . C11 C 0.0911(5) 0.6699(5) 0.1863(5) 0.061(2) Uani 1 1 d . . . H11 H 0.1211 0.6455 0.1603 0.073 Uiso 1 1 calc R . . C12 C 0.0540(4) 0.6361(4) 0.2538(4) 0.0375(14) Uani 1 1 d . . . H12 H 0.0581 0.5874 0.2732 0.045 Uiso 1 1 calc R . . C13 C -0.3397(3) 0.5826(3) 0.2217(2) 0.0187(10) Uani 1 1 d . . . C14 C -0.3615(3) 0.6499(3) 0.2243(3) 0.0245(11) Uani 1 1 d . . . H14 H -0.3386 0.6929 0.2616 0.029 Uiso 1 1 calc R . . C15 C -0.1092(3) 0.3738(3) 0.1687(3) 0.0166(9) Uani 1 1 d . . . H15 H -0.1700 0.3591 0.1670 0.020 Uiso 1 1 calc R . . C16 C -0.0476(3) 0.4301(3) 0.1188(3) 0.0218(11) Uani 1 1 d . . . C17 C 0.0417(4) 0.4505(4) 0.1194(3) 0.0235(11) Uani 1 1 d . . . H17 H 0.0821 0.4876 0.0835 0.028 Uiso 1 1 calc R . . C18 C 0.0698(3) 0.4155(3) 0.1735(5) 0.0260(9) Uani 1 1 d . . . H18 H 0.1303 0.4293 0.1752 0.031 Uiso 1 1 calc R . . C19 C -0.1204(3) 0.5147(3) 0.0793(3) 0.0201(10) Uani 1 1 d . . . C20 C -0.0955(3) 0.5065(3) -0.0372(3) 0.0213(11) Uani 1 1 d . . . C21 C -0.1031(4) 0.5202(4) -0.1156(3) 0.0324(13) Uani 1 1 d . . . H21B H -0.0459 0.5362 -0.1396 0.039 Uiso 1 1 calc R . . H21A H -0.1505 0.4640 -0.1370 0.039 Uiso 1 1 calc R . . C22 C -0.1987(4) 0.5758(4) -0.0838(3) 0.0286(12) Uani 1 1 d . . . H22A H -0.2483 0.5134 -0.0891 0.034 Uiso 1 1 calc R . . H22B H -0.2200 0.6162 -0.1008 0.034 Uiso 1 1 calc R . . C23 C -0.1726(4) 0.5946(3) -0.0061(3) 0.0218(11) Uani 1 1 d . . . H23 H -0.2270 0.5772 0.0236 0.026 Uiso 1 1 calc R . . C24 C -0.1025(4) 0.6908(4) 0.0097(3) 0.0319(13) Uani 1 1 d . . . H24A H -0.0522 0.7098 -0.0243 0.038 Uiso 1 1 calc R . . H24B H -0.0789 0.6943 0.0585 0.038 Uiso 1 1 calc R . . C25 C -0.1386(4) 0.7546(4) 0.0040(3) 0.0325(13) Uani 1 1 d . . . C26 C -0.2011(5) 0.7514(5) 0.0512(4) 0.0503(18) Uani 1 1 d . . . H26 H -0.2214 0.7085 0.0886 0.060 Uiso 1 1 calc R . . C27 C -0.2349(6) 0.8075(5) 0.0462(5) 0.066(2) Uani 1 1 d . . . H27 H -0.2808 0.8015 0.0776 0.079 Uiso 1 1 calc R . . C28 C -0.2005(6) 0.8738(5) -0.0058(7) 0.078(3) Uani 1 1 d . . . H28 H -0.2162 0.9192 -0.0057 0.094 Uiso 1 1 calc R . . C29 C -0.1444(5) 0.8738(4) -0.0570(5) 0.058(2) Uani 1 1 d . . . H29 H -0.1263 0.9151 -0.0954 0.069 Uiso 1 1 calc R . . C30 C -0.1139(4) 0.8136(4) -0.0529(4) 0.0430(16) Uani 1 1 d . . . H30 H -0.0759 0.8127 -0.0891 0.052 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 0.02163(17) 0.02465(18) 0.01610(16) 0.0003(2) 0.0020(2) 0.01430(13) O1 0.036(3) 0.043(3) 0.020(2) 0.0011(19) -0.0117(18) 0.015(2) O2 0.038(2) 0.039(3) 0.028(2) 0.015(2) 0.013(2) 0.025(2) N1 0.024(2) 0.022(2) 0.014(2) 0.0028(17) 0.0005(18) 0.013(2) N2 0.025(2) 0.023(2) 0.0137(19) 0.0001(17) -0.0009(17) 0.0122(18) N3 0.029(2) 0.034(3) 0.0124(19) -0.0037(18) 0.0004(17) 0.017(2) N4 0.016(2) 0.017(2) 0.021(2) 0.0035(17) 0.0046(16) 0.0076(17) N5 0.025(2) 0.032(2) 0.0152(19) 0.0010(18) 0.0050(17) 0.019(2) N6 0.014(2) 0.017(2) 0.025(2) 0.0031(18) 0.0067(18) 0.0074(18) C1 0.021(2) 0.016(2) 0.018(2) -0.0010(19) -0.003(2) 0.009(2) C2 0.025(3) 0.029(3) 0.016(2) -0.005(2) -0.005(2) 0.011(2) C3 0.039(3) 0.046(4) 0.017(3) -0.001(2) -0.003(2) 0.020(3) C4 0.023(3) 0.039(3) 0.030(3) 0.013(3) -0.001(2) 0.011(3) C5 0.017(3) 0.028(3) 0.024(3) 0.004(2) -0.004(2) 0.010(2) C6 0.024(3) 0.024(3) 0.032(3) 0.005(2) 0.000(2) 0.006(2) C7 0.017(3) 0.027(3) 0.030(3) -0.003(2) -0.009(2) 0.002(2) C8 0.054(4) 0.047(4) 0.036(3) 0.008(3) 0.011(3) 0.028(4) C9 0.083(6) 0.050(4) 0.091(8) 0.024(5) 0.020(5) 0.031(4) C10 0.066(5) 0.048(4) 0.034(4) -0.008(3) 0.024(3) -0.010(4) C11 0.045(4) 0.044(4) 0.081(7) 0.006(4) 0.027(5) 0.012(3) C12 0.027(3) 0.039(3) 0.048(4) 0.004(3) 0.007(3) 0.018(3) C13 0.017(2) 0.024(2) 0.0107(19) 0.0029(19) 0.0004(18) 0.007(2) C14 0.027(3) 0.018(2) 0.029(3) -0.003(2) -0.003(2) 0.011(2) C15 0.0146(18) 0.022(2) 0.013(2) -0.006(2) 0.001(2) 0.0087(16) C16 0.027(3) 0.024(3) 0.015(2) -0.002(2) 0.002(2) 0.013(2) C17 0.025(3) 0.023(3) 0.022(2) -0.001(2) 0.004(2) 0.011(2) C18 0.016(2) 0.036(2) 0.025(2) 0.000(4) 0.004(4) 0.0133(19) C19 0.014(2) 0.020(2) 0.023(2) 0.000(2) 0.0045(19) 0.006(2) C20 0.024(3) 0.023(3) 0.019(2) -0.002(2) 0.002(2) 0.014(2) C21 0.043(3) 0.047(4) 0.020(3) 0.006(2) 0.005(3) 0.032(3) C22 0.029(3) 0.031(3) 0.027(3) 0.006(2) 0.004(2) 0.016(3) C23 0.022(3) 0.018(3) 0.023(3) 0.001(2) -0.002(2) 0.009(2) C24 0.029(3) 0.024(3) 0.041(3) 0.002(2) -0.004(3) 0.012(2) C25 0.028(3) 0.017(3) 0.049(4) 0.004(3) -0.001(3) 0.010(2) C26 0.071(5) 0.030(3) 0.056(4) 0.005(3) 0.009(4) 0.031(4) C27 0.078(6) 0.042(4) 0.096(6) 0.010(4) 0.029(5) 0.043(4) C28 0.050(5) 0.025(3) 0.166(10) 0.013(5) 0.017(6) 0.023(3) C29 0.041(4) 0.027(3) 0.102(7) 0.027(4) -0.005(4) 0.015(3) C30 0.026(3) 0.020(3) 0.075(5) 0.004(3) 0.000(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C1 2.083(5) . ? Ag1 C19 2.078(5) . ? O1 C3 1.435(8) . ? O1 C4 1.436(9) . ? O2 C21 1.408(7) . ? O2 C22 1.446(7) . ? N1 C1 1.379(6) . ? N1 C2 1.358(7) . ? N1 C5 1.482(7) . ? N2 N3 1.390(6) . ? N2 C1 1.328(6) . ? N2 C13 1.428(6) . ? N3 C2 1.314(7) . ? N4 N5 1.405(6) . ? N4 C16 1.423(7) . ? N4 C19 1.338(6) . ? N5 C20 1.299(7) . ? N6 C19 1.354(7) . ? N6 C20 1.377(7) . ? N6 C23 1.509(7) . ? C2 C3 1.496(7) . ? C3 H3B 0.9900 . ? C3 H3A 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.523(8) . ? C5 H5 1.0000 . ? C5 C6 1.510(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.532(8) . ? C7 C8 1.377(9) . ? C7 C12 1.372(9) . ? C8 H8 0.9500 . ? C8 C9 1.464(11) . ? C9 H9 0.9500 . ? C9 C10 1.299(12) . ? C10 H10 0.9500 . ? C10 C11 1.429(12) . ? C11 H11 0.9500 . ? C11 C12 1.405(11) . ? C12 H12 0.9500 . ? C13 C14 1.390(7) . ? C13 C15 1.394(8) 3_565 ? C14 H14 0.9500 . ? C14 C18 1.359(9) 3_565 ? C15 C13 1.394(8) 5_455 ? C15 H15 0.9500 . ? C15 C16 1.385(7) . ? C16 C17 1.399(7) . ? C17 H17 0.9500 . ? C17 C18 1.387(9) . ? C18 C14 1.359(9) 5_455 ? C18 H18 0.9500 . ? C20 C21 1.503(7) . ? C21 H21B 0.9900 . ? C21 H21A 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.508(8) . ? C23 H23 1.0000 . ? C23 C24 1.518(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.518(8) . ? C25 C26 1.372(10) . ? C25 C30 1.385(9) . ? C26 H26 0.9500 . ? C26 C27 1.362(10) . ? C27 H27 0.9500 . ? C27 C28 1.390(13) . ? C28 H28 0.9500 . ? C28 C29 1.362(13) . ? C29 H29 0.9500 . ? C29 C30 1.383(9) . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C3 C2 109.7(5) . . ? O1 C3 H3B 109.7 . . ? O1 C3 H3A 109.7 . . ? O1 C4 H4A 109.7 . . ? O1 C4 H4B 109.7 . . ? O1 C4 C5 109.8(5) . . ? O2 C21 C20 110.7(5) . . ? O2 C21 H21B 109.5 . . ? O2 C21 H21A 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 C23 110.6(5) . . ? N1 C1 Ag1 126.8(4) . . ? N1 C2 C3 122.9(5) . . ? N1 C5 C4 105.7(5) . . ? N1 C5 H5 109.3 . . ? N1 C5 C6 111.8(5) . . ? N2 C1 Ag1 130.3(4) . . ? N2 C1 N1 102.2(4) . . ? N3 N2 C13 118.5(4) . . ? N3 C2 N1 110.9(4) . . ? N3 C2 C3 126.0(5) . . ? N4 C19 Ag1 130.1(4) . . ? N4 C19 N6 102.6(4) . . ? N5 N4 C16 119.4(4) . . ? N5 C20 N6 110.4(4) . . ? N5 C20 C21 129.2(5) . . ? N6 C19 Ag1 127.3(4) . . ? N6 C20 C21 120.3(5) . . ? N6 C23 H23 109.7 . . ? N6 C23 C24 107.9(4) . . ? C1 N1 C5 128.1(5) . . ? C1 N2 N3 114.6(4) . . ? C1 N2 C13 126.8(4) . . ? C2 N1 C1 109.5(4) . . ? C2 N1 C5 122.3(4) . . ? C2 N3 N2 102.8(4) . . ? C2 C3 H3B 109.7 . . ? C2 C3 H3A 109.7 . . ? C3 O1 C4 110.6(5) . . ? H3B C3 H3A 108.2 . . ? C4 C5 H5 109.3 . . ? H4A C4 H4B 108.2 . . ? C5 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C5 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C5 C6 C7 114.0(5) . . ? C6 C5 C4 111.2(5) . . ? C6 C5 H5 109.3 . . ? H6A C6 H6B 107.6 . . ? C7 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.8(7) . . ? C7 C12 C11 121.2(6) . . ? C7 C12 H12 119.4 . . ? C8 C7 C6 121.2(6) . . ? C8 C9 H9 120.5 . . ? C9 C8 H8 119.6 . . ? C9 C10 H10 119.1 . . ? C9 C10 C11 121.7(8) . . ? C10 C9 C8 118.9(8) . . ? C10 C9 H9 120.5 . . ? C10 C11 H11 120.7 . . ? C11 C10 H10 119.1 . . ? C11 C12 H12 119.4 . . ? C12 C7 C6 120.1(6) . . ? C12 C7 C8 118.7(6) . . ? C12 C11 C10 118.5(7) . . ? C12 C11 H11 120.7 . . ? C13 C14 H14 119.9 . . ? C13 C15 H15 121.6 5_455 . ? C14 C13 N2 118.8(4) . . ? C14 C13 C15 121.6(4) . 3_565 ? C14 C18 C17 120.5(4) 5_455 . ? C14 C18 H18 119.7 5_455 . ? C15 C13 N2 119.6(4) 3_565 . ? C15 C16 N4 117.8(4) . . ? C15 C16 C17 122.3(5) . . ? C16 C15 C13 116.8(4) . 5_455 ? C16 C15 H15 121.6 . . ? C16 C17 H17 120.7 . . ? C17 C16 N4 119.8(5) . . ? C17 C18 H18 119.7 . . ? C18 C14 C13 120.2(5) 3_565 . ? C18 C14 H14 119.9 3_565 . ? C18 C17 C16 118.6(5) . . ? C18 C17 H17 120.7 . . ? C19 Ag1 C1 176.38(19) . . ? C19 N4 N5 113.7(4) . . ? C19 N4 C16 126.9(4) . . ? C19 N6 C20 110.1(4) . . ? C19 N6 C23 126.1(4) . . ? C20 N5 N4 103.1(4) . . ? C20 N6 C23 123.3(4) . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? C21 O2 C22 111.9(4) . . ? H21B C21 H21A 108.1 . . ? C22 C23 N6 105.3(4) . . ? C22 C23 H23 109.7 . . ? C22 C23 C24 114.4(5) . . ? H22A C22 H22B 108.1 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C23 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C23 C24 C25 112.9(5) . . ? C24 C23 H23 109.7 . . ? H24A C24 H24B 107.8 . . ? C25 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C25 C26 H26 118.8 . . ? C25 C30 H30 119.9 . . ? C26 C25 C24 121.7(5) . . ? C26 C25 C30 118.1(6) . . ? C26 C27 H27 120.8 . . ? C26 C27 C28 118.4(8) . . ? C27 C26 C25 122.3(7) . . ? C27 C26 H26 118.8 . . ? C27 C28 H28 119.9 . . ? C28 C27 H27 120.8 . . ? C28 C29 H29 120.0 . . ? C28 C29 C30 120.0(7) . . ? C29 C28 C27 120.1(7) . . ? C29 C28 H28 119.9 . . ? C29 C30 C25 120.1(7) . . ? C29 C30 H30 119.9 . . ? C30 C25 C24 120.0(6) . . ? C30 C29 H29 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C5 N1 -56.2(6) . . . . ? O1 C4 C5 C6 65.3(6) . . . . ? O2 C22 C23 N6 -54.1(5) . . . . ? O2 C22 C23 C24 64.2(6) . . . . ? N1 C2 C3 O1 14.9(8) . . . . ? N1 C5 C6 C7 -71.3(7) . . . . ? N2 N3 C2 N1 1.7(6) . . . . ? N2 N3 C2 C3 -173.1(6) . . . . ? N2 C13 C14 C18 -179.2(5) . . . 3_565 ? N3 N2 C1 Ag1 171.2(4) . . . . ? N3 N2 C1 N1 -0.1(5) . . . . ? N3 N2 C13 C14 50.2(6) . . . . ? N3 N2 C13 C15 -127.4(5) . . . 3_565 ? N3 C2 C3 O1 -170.9(5) . . . . ? N4 N5 C20 N6 -0.5(6) . . . . ? N4 N5 C20 C21 -177.2(6) . . . . ? N4 C16 C17 C18 175.5(5) . . . . ? N5 N4 C16 C15 -129.4(5) . . . . ? N5 N4 C16 C17 52.6(7) . . . . ? N5 N4 C19 Ag1 178.9(3) . . . . ? N5 N4 C19 N6 1.5(5) . . . . ? N5 C20 C21 O2 -163.9(5) . . . . ? N6 C20 C21 O2 19.8(8) . . . . ? N6 C23 C24 C25 -171.1(5) . . . . ? C1 Ag1 C19 N4 -148(3) . . . . ? C1 Ag1 C19 N6 29(3) . . . . ? C1 N1 C2 N3 -1.9(6) . . . . ? C1 N1 C2 C3 173.1(5) . . . . ? C1 N1 C5 C4 -153.1(5) . . . . ? C1 N1 C5 C6 85.7(7) . . . . ? C1 N2 N3 C2 -1.0(6) . . . . ? C1 N2 C13 C14 -134.3(5) . . . . ? C1 N2 C13 C15 48.0(7) . . . 3_565 ? C2 N1 C1 Ag1 -170.5(4) . . . . ? C2 N1 C1 N2 1.1(5) . . . . ? C2 N1 C5 C4 23.3(7) . . . . ? C2 N1 C5 C6 -97.8(6) . . . . ? C3 O1 C4 C5 73.3(6) . . . . ? C4 O1 C3 C2 -48.2(7) . . . . ? C4 C5 C6 C7 170.8(5) . . . . ? C5 N1 C1 Ag1 6.3(7) . . . . ? C5 N1 C1 N2 178.0(5) . . . . ? C5 N1 C2 N3 -178.9(5) . . . . ? C5 N1 C2 C3 -3.9(8) . . . . ? C5 C6 C7 C8 102.2(7) . . . . ? C5 C6 C7 C12 -78.1(7) . . . . ? C6 C7 C8 C9 -176.5(6) . . . . ? C6 C7 C12 C11 179.6(6) . . . . ? C7 C8 C9 C10 -5.1(13) . . . . ? C8 C7 C12 C11 -0.7(9) . . . . ? C8 C9 C10 C11 3.2(13) . . . . ? C9 C10 C11 C12 -0.2(12) . . . . ? C10 C11 C12 C7 -1.1(10) . . . . ? C12 C7 C8 C9 3.8(10) . . . . ? C13 N2 N3 C2 175.0(4) . . . . ? C13 N2 C1 Ag1 -4.5(7) . . . . ? C13 N2 C1 N1 -175.7(4) . . . . ? C13 C15 C16 N4 -176.1(4) 5_455 . . . ? C13 C15 C16 C17 1.8(7) 5_455 . . . ? C15 C13 C14 C18 -1.6(8) 3_565 . . 3_565 ? C15 C16 C17 C18 -2.3(8) . . . . ? C16 N4 N5 C20 179.5(4) . . . . ? C16 N4 C19 Ag1 -1.3(7) . . . . ? C16 N4 C19 N6 -178.6(4) . . . . ? C16 C17 C18 C14 0.9(9) . . . 5_455 ? C19 Ag1 C1 N1 165(3) . . . . ? C19 Ag1 C1 N2 -4(3) . . . . ? C19 N4 N5 C20 -0.6(5) . . . . ? C19 N4 C16 C15 50.7(7) . . . . ? C19 N4 C16 C17 -127.3(5) . . . . ? C19 N6 C20 N5 1.5(6) . . . . ? C19 N6 C20 C21 178.5(5) . . . . ? C19 N6 C23 C22 -163.4(5) . . . . ? C19 N6 C23 C24 74.0(6) . . . . ? C20 N6 C19 Ag1 -179.2(4) . . . . ? C20 N6 C19 N4 -1.8(5) . . . . ? C20 N6 C23 C22 25.2(7) . . . . ? C20 N6 C23 C24 -97.4(6) . . . . ? C21 O2 C22 C23 72.4(6) . . . . ? C22 O2 C21 C20 -50.3(7) . . . . ? C22 C23 C24 C25 72.1(7) . . . . ? C23 N6 C19 Ag1 8.4(7) . . . . ? C23 N6 C19 N4 -174.1(4) . . . . ? C23 N6 C20 N5 174.1(4) . . . . ? C23 N6 C20 C21 -8.9(8) . . . . ? C23 C24 C25 C26 67.1(8) . . . . ? C23 C24 C25 C30 -107.9(6) . . . . ? C24 C25 C26 C27 -179.2(7) . . . . ? C24 C25 C30 C29 -177.9(6) . . . . ? C25 C26 C27 C28 -4.1(14) . . . . ? C26 C25 C30 C29 6.8(10) . . . . ? C26 C27 C28 C29 9.6(15) . . . . ? C27 C28 C29 C30 -6.9(14) . . . . ? C28 C29 C30 C25 -1.4(11) . . . . ? C30 C25 C26 C27 -4.1(12) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.226 239 36 ' ' 2 0.000 0.000 0.726 239 36 ' ' 3 0.333 0.667 0.377 278 94 ' ' 4 0.667 0.333 0.877 278 94 ' ' _platon_squeeze_details ; ; # Attachment '[(S)-2Au]3(BF4)3.cif' data_20101008_S3_WSP _database_code_depnum_ccdc_archive 'CCDC 836088' #TrackingRef '[(S)-2Au]3(BF4)3.cif' _audit_creation_date 2011-02-11 _audit_creation_method ; Olex2 1.1 (compiled 2011.01.21 svn.r1625, GUI svn.r3464) ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '3(C30 H28 Au N6 O2), 9(B1 F2)' _chemical_formula_sum 'C90 H84 Au3 B3 F12 N18 O6' _chemical_formula_weight 2365.09 _chemical_absolute_configuration ad _chemical_melting_point ? 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x-y, x, z+1/2' 3 '-y, x-y, z' 4 '-x, -y, z+1/2' 5 '-x+y, -x, z' 6 'y, -x+y, z+1/2' _cell_length_a 17.4164(4) _cell_length_b 17.4164(4) _cell_length_c 18.8187(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4943.51(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7210 _cell_measurement_temperature 294.15 _cell_measurement_theta_max 29.1925 _cell_measurement_theta_min 2.904 _exptl_absorpt_coefficient_mu 4.526 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.74876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colurless _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2316 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0507 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13406 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 3.46 _diffrn_ambient_temperature 294.15 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -79.00 28.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -16.8924 0.0000 30.0000 107 #__ type_ start__ end____ width___ exp.time_ 2 omega -53.00 -19.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.8611 -38.0000 120.0000 34 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0255371 _diffrn_orient_matrix_UB_12 0.018961 _diffrn_orient_matrix_UB_13 -0.0117863 _diffrn_orient_matrix_UB_21 0.0265997 _diffrn_orient_matrix_UB_22 0.0159201 _diffrn_orient_matrix_UB_23 -0.0309976 _diffrn_orient_matrix_UB_31 -0.0291843 _diffrn_orient_matrix_UB_32 -0.0399797 _diffrn_orient_matrix_UB_33 -0.0179247 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4581 _reflns_number_total 6306 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 1.248 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.129 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(10) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 6306 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0963 _refine_ls_wR_factor_ref 0.1002 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.835701(16) 0.540957(16) 0.86704(3) 0.03312(9) Uani 1 1 d . . . F1 F 0.7404(4) 0.3334(4) 0.7195(3) 0.0683(17) Uiso 1 1 d . . . F2 F 0.6667 0.3333 0.6377(11) 0.167(7) Uiso 1 3 d S . . F3 F 0.6369(6) 0.3896(7) 0.2698(5) 0.131(3) Uiso 1 1 d . . . F4 F 0.6667 0.3333 0.1786(10) 0.136(5) Uiso 1 3 d S . . F5 F 0.7509(4) 0.3625(4) -0.0063(3) 0.0607(16) Uiso 1 1 d . . . F6 F 0.6667 0.3333 -0.1005(6) 0.085(3) Uiso 1 3 d S . . O1 O 0.8778(5) 0.5910(5) 0.5698(4) 0.0479(19) Uani 1 1 d . . . O2 O 0.8428(5) 0.5587(5) 1.1691(5) 0.054(2) Uani 1 1 d . . . N1 N 0.8678(5) 0.5377(4) 0.7092(4) 0.0256(17) Uani 1 1 d . . . N2 N 0.9406(4) 0.4681(4) 0.6914(3) 0.0310(15) Uani 1 1 d . . . N3 N 0.9208(4) 0.4705(4) 0.7629(3) 0.0270(14) Uani 1 1 d . . . N4 N 0.8136(5) 0.5607(5) 1.0255(4) 0.0301(17) Uani 1 1 d . . . N5 N 0.8814(4) 0.3000(4) 1.0383(3) 0.0356(16) Uani 1 1 d . . . N6 N 0.8565(4) 0.2791(4) 0.9681(3) 0.0239(13) Uani 1 1 d . . . C1 C 0.9044(5) 0.5084(5) 0.6606(5) 0.0350(19) Uani 1 1 d . . . C2 C 0.9025(6) 0.5248(6) 0.5830(5) 0.044(2) Uani 1 1 d . . . H2B H 0.9606 0.5442 0.5628 0.053 Uiso 1 1 calc R . . H2A H 0.8604 0.4700 0.5598 0.053 Uiso 1 1 calc R . . C3 C 0.8038(5) 0.5776(6) 0.6110(5) 0.040(2) Uani 1 1 d . . . H3A H 0.7555 0.5174 0.6042 0.048 Uiso 1 1 calc R . . H3B H 0.7841 0.6178 0.5951 0.048 Uiso 1 1 calc R . . C4 C 0.8274(5) 0.5932(5) 0.6894(4) 0.029(2) Uani 1 1 d . . . H4 H 0.7736 0.5749 0.7175 0.035 Uiso 1 1 calc R . . C5 C 0.8965(5) 0.6907(5) 0.7065(5) 0.040(2) Uani 1 1 d . . . H5B H 0.9169 0.6940 0.7550 0.048 Uiso 1 1 calc R . . H5A H 0.9472 0.7096 0.6754 0.048 Uiso 1 1 calc R . . C6 C 0.8614(6) 0.7540(5) 0.6983(5) 0.043(2) Uani 1 1 d . . . C7 C 0.7991(9) 0.7506(8) 0.7427(7) 0.086(4) Uani 1 1 d . . . H7 H 0.7768 0.7080 0.7784 0.103 Uiso 1 1 calc R . . C8 C 0.7673(9) 0.8102(9) 0.7363(9) 0.097(5) Uani 1 1 d . . . H8 H 0.7261 0.8090 0.7684 0.117 Uiso 1 1 calc R . . C9 C 0.7963(10) 0.8662(8) 0.6853(12) 0.116(6) Uani 1 1 d . . . H9 H 0.7752 0.9057 0.6823 0.140 Uiso 1 1 calc R . . C10 C 0.8548(8) 0.8728(7) 0.6355(9) 0.091(5) Uani 1 1 d . . . H10 H 0.8734 0.9147 0.5993 0.109 Uiso 1 1 calc R . . C11 C 0.8868(6) 0.8115(6) 0.6415(6) 0.062(3) Uani 1 1 d . . . H11 H 0.9246 0.8105 0.6070 0.075 Uiso 1 1 calc R . . C12 C 0.8766(4) 0.5140(4) 0.7736(4) 0.0232(15) Uani 1 1 d . . . C13 C 0.9491(4) 0.4291(4) 0.8137(4) 0.0247(15) Uani 1 1 d . . . C14 C 0.8891(3) 0.3736(3) 0.8668(7) 0.0253(12) Uani 1 1 d . . . H14 H 0.8312 0.3629 0.8683 0.030 Uiso 1 1 calc R . . C15 C 0.9178(5) 0.3373(5) 0.9142(3) 0.0235(15) Uani 1 1 d . . . C16 C 1.0049(5) 0.3551(5) 0.9174(4) 0.0304(17) Uani 1 1 d . . . H16 H 1.0214 0.3286 0.9524 0.036 Uiso 1 1 calc R . . C17 C 1.0670(4) 0.4116(5) 0.8693(7) 0.0330(16) Uani 1 1 d . . . H17 H 1.1260 0.4258 0.8720 0.040 Uiso 1 1 calc R . . C18 C 1.0359(5) 0.4486(5) 0.8134(4) 0.0353(18) Uani 1 1 d . . . H18 H 1.0746 0.4848 0.7782 0.042 Uiso 1 1 calc R . . C19 C 0.8111(6) 0.2414(5) 1.0726(4) 0.0370(19) Uani 1 1 d . . . C20 C 0.7618(6) 0.5568(7) 1.1500(4) 0.047(2) Uani 1 1 d . . . H20B H 0.7579 0.6032 1.1753 0.056 Uiso 1 1 calc R . . H20A H 0.7115 0.5003 1.1638 0.056 Uiso 1 1 calc R . . C21 C 0.8557(6) 0.5008(6) 1.1245(5) 0.045(2) Uani 1 1 d . . . H21A H 0.8008 0.4447 1.1199 0.054 Uiso 1 1 calc R . . H21B H 0.9003 0.4894 1.1446 0.054 Uiso 1 1 calc R . . C22 C 0.8865(6) 0.5458(6) 1.0500(5) 0.033(2) Uani 1 1 d . . . H22 H 0.8908 0.5042 1.0175 0.040 Uiso 1 1 calc R . . C23 C 0.9753(5) 0.6304(6) 1.0526(4) 0.039(2) Uani 1 1 d . . . H23A H 0.9685 0.6737 1.0803 0.046 Uiso 1 1 calc R . . H23B H 1.0167 0.6184 1.0777 0.046 Uiso 1 1 calc R . . C24 C 1.0150(5) 0.6711(6) 0.9827(5) 0.042(2) Uani 1 1 d . . . C25 C 1.0130(8) 0.7429(7) 0.9540(6) 0.068(3) Uani 1 1 d . . . H25 H 0.9856 0.7692 0.9784 0.081 Uiso 1 1 calc R . . C26 C 1.0516(10) 0.7754(8) 0.8890(6) 0.089(4) Uani 1 1 d . . . H26 H 1.0509 0.8248 0.8709 0.107 Uiso 1 1 calc R . . C27 C 1.0886(8) 0.7407(7) 0.8520(6) 0.079(4) Uani 1 1 d . . . H27 H 1.1132 0.7640 0.8078 0.094 Uiso 1 1 calc R . . C28 C 1.0912(7) 0.6732(8) 0.8771(8) 0.080(4) Uani 1 1 d . . . H28 H 1.1214 0.6514 0.8508 0.095 Uiso 1 1 calc R . . C29 C 1.0538(7) 0.6322(8) 0.9380(6) 0.067(3) Uani 1 1 d . . . H29 H 1.0528 0.5802 0.9511 0.080 Uiso 1 1 calc R . . C30 C 0.7872(5) 0.5636(5) 0.9594(4) 0.0267(16) Uani 1 1 d . . . B1 B 0.6667 0.3333 0.7035(12) 0.057(5) Uiso 1 3 d S . . B2 B 0.6667 0.3333 0.2751(19) 0.117(11) Uiso 1 3 d S . . B3 B 0.6667 0.3333 -0.0225(8) 0.029(3) Uiso 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03359(15) 0.03870(16) 0.03071(14) -0.0005(3) 0.0022(3) 0.02080(12) O1 0.066(5) 0.061(5) 0.026(4) 0.015(4) 0.012(4) 0.039(4) O2 0.054(5) 0.069(5) 0.030(4) -0.005(3) -0.015(3) 0.023(4) N1 0.021(4) 0.022(4) 0.028(4) 0.001(3) 0.006(3) 0.007(3) N2 0.029(3) 0.037(4) 0.028(3) 0.007(3) 0.010(3) 0.018(3) N3 0.023(3) 0.027(3) 0.027(3) 0.003(3) 0.009(3) 0.009(3) N4 0.030(4) 0.032(4) 0.028(4) 0.005(3) 0.002(3) 0.016(3) N5 0.040(4) 0.039(4) 0.029(4) -0.002(3) -0.006(3) 0.020(3) N6 0.027(3) 0.026(3) 0.021(3) 0.004(3) 0.002(3) 0.014(3) C1 0.032(5) 0.033(5) 0.045(5) 0.006(4) 0.012(4) 0.020(4) C2 0.049(5) 0.056(6) 0.041(5) 0.010(4) 0.012(4) 0.036(5) C3 0.039(5) 0.042(5) 0.044(6) 0.004(4) -0.007(5) 0.024(5) C4 0.030(4) 0.029(5) 0.036(5) 0.005(4) 0.010(4) 0.020(4) C5 0.036(5) 0.035(5) 0.051(5) 0.006(4) -0.004(4) 0.019(4) C6 0.035(5) 0.018(4) 0.073(6) -0.003(4) 0.009(4) 0.010(4) C7 0.110(10) 0.045(7) 0.096(10) 0.011(6) 0.035(8) 0.034(7) C8 0.098(10) 0.059(8) 0.156(14) 0.026(9) 0.049(10) 0.055(8) C9 0.067(9) 0.042(7) 0.26(2) 0.001(10) -0.015(12) 0.040(7) C10 0.058(8) 0.046(7) 0.164(14) 0.029(8) -0.004(9) 0.023(6) C11 0.039(6) 0.035(5) 0.105(9) 0.003(5) -0.012(6) 0.013(4) C12 0.018(3) 0.022(4) 0.027(4) 0.004(3) 0.006(3) 0.008(3) C13 0.024(4) 0.023(4) 0.028(4) 0.000(3) -0.001(3) 0.013(3) C14 0.015(3) 0.026(3) 0.031(3) -0.002(6) -0.003(6) 0.008(2) C15 0.025(4) 0.027(4) 0.018(3) -0.006(3) -0.001(3) 0.013(3) C16 0.031(4) 0.041(5) 0.025(4) -0.001(3) -0.006(3) 0.022(4) C17 0.023(3) 0.053(4) 0.020(3) -0.024(6) -0.017(6) 0.016(3) C18 0.030(4) 0.040(5) 0.038(4) 0.002(4) 0.009(4) 0.018(4) C19 0.045(5) 0.035(5) 0.035(5) -0.002(4) -0.009(4) 0.023(4) C20 0.040(5) 0.066(7) 0.028(5) 0.001(4) -0.002(4) 0.021(5) C21 0.033(5) 0.061(6) 0.040(5) 0.011(5) -0.003(4) 0.023(5) C22 0.034(5) 0.040(5) 0.024(5) -0.010(4) -0.009(4) 0.017(4) C23 0.033(5) 0.046(5) 0.036(5) 0.002(4) -0.004(4) 0.019(4) C24 0.022(4) 0.037(5) 0.048(5) 0.000(4) -0.015(4) 0.002(4) C25 0.078(8) 0.043(6) 0.074(7) 0.003(5) 0.013(6) 0.024(6) C26 0.129(12) 0.042(6) 0.074(10) 0.015(6) 0.019(7) 0.025(7) C27 0.103(10) 0.046(6) 0.059(10) 0.012(5) 0.024(7) 0.016(6) C28 0.080(7) 0.084(8) 0.050(8) 0.011(7) 0.026(7) 0.023(6) C29 0.061(7) 0.069(7) 0.070(7) 0.000(6) 0.011(6) 0.032(6) C30 0.031(4) 0.025(4) 0.020(4) -0.008(3) -0.001(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C12 2.038(7) . ? Au1 C30 2.055(7) . ? F1 B1 1.318(8) . ? F2 B1 1.24(2) . ? F3 B2 1.322(10) . ? F4 B2 1.81(4) . ? F5 B3 1.326(7) . ? F6 B3 1.467(18) . ? O1 C2 1.439(11) . ? O1 C3 1.419(11) . ? O2 C20 1.440(12) . ? O2 C21 1.415(13) . ? N1 C1 1.352(10) . ? N1 C4 1.499(12) . ? N1 C12 1.315(10) . ? N2 N3 1.393(8) . ? N2 C1 1.292(10) . ? N3 C12 1.339(9) . ? N3 C13 1.425(9) . ? N4 C19 1.370(10) 3_655 ? N4 C22 1.491(13) . ? N4 C30 1.337(10) . ? N5 N6 1.383(8) . ? N5 C19 1.306(10) . ? N6 C15 1.453(9) . ? N6 C30 1.302(9) 5_665 ? C1 C2 1.492(11) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.519(12) . ? C4 H4 0.9800 . ? C4 C5 1.547(11) . ? C5 H5B 0.9700 . ? C5 H5A 0.9700 . ? C5 C6 1.512(11) . ? C6 C7 1.348(14) . ? C6 C11 1.378(13) . ? C7 H7 0.9300 . ? C7 C8 1.406(16) . ? C8 H8 0.9300 . ? C8 C9 1.28(2) . ? C9 H9 0.9300 . ? C9 C10 1.35(2) . ? C10 H10 0.9300 . ? C10 C11 1.435(15) . ? C11 H11 0.9300 . ? C13 C14 1.419(12) . ? C13 C18 1.373(10) . ? C14 H14 0.9300 . ? C14 C15 1.326(12) . ? C15 C16 1.389(10) . ? C16 H16 0.9300 . ? C16 C17 1.376(14) . ? C17 H17 0.9300 . ? C17 C18 1.471(14) . ? C18 H18 0.9300 . ? C19 N4 1.370(10) 5_665 ? C19 C20 1.479(10) 5_665 ? C20 C19 1.479(10) 3_655 ? C20 H20B 0.9700 . ? C20 H20A 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.564(13) . ? C22 H22 0.9800 . ? C22 C23 1.511(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.490(12) . ? C24 C25 1.381(13) . ? C24 C29 1.442(13) . ? C25 H25 0.9300 . ? C25 C26 1.374(14) . ? C26 H26 0.9300 . ? C26 C27 1.287(16) . ? C27 H27 0.9300 . ? C27 C28 1.288(16) . ? C28 H28 0.9300 . ? C28 C29 1.335(16) . ? C29 H29 0.9300 . ? C30 N6 1.302(9) 3_655 ? B1 F1 1.318(8) 3_655 ? B1 F1 1.318(8) 5_665 ? B2 F3 1.322(10) 5_665 ? B2 F3 1.322(10) 3_655 ? B3 F5 1.326(7) 3_655 ? B3 F5 1.326(7) 5_665 ? 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 F1 B1 F1 115.0(7) 5_665 3_655 ? F1 B1 F1 115.0(7) . 5_665 ? F1 B1 F1 115.0(7) . 3_655 ? F2 B1 F1 103.2(10) . 3_655 ? F2 B1 F1 103.2(10) . 5_665 ? F2 B1 F1 103.2(10) . . ? F3 B2 F3 119.4(4) 5_665 3_655 ? F3 B2 F3 119.5(4) 5_665 . ? F3 B2 F3 119.5(4) 3_655 . ? F3 B2 F4 85.7(17) . . ? F3 B2 F4 85.7(17) 3_655 . ? F3 B2 F4 85.7(17) 5_665 . ? F5 B3 F5 114.9(5) 5_665 3_655 ? F5 B3 F5 114.9(5) . 3_655 ? F5 B3 F5 114.9(5) . 5_665 ? F5 B3 F6 103.3(7) 3_655 . ? F5 B3 F6 103.3(7) . . ? F5 B3 F6 103.3(7) 5_665 . ? O1 C2 C1 111.6(7) . . ? O1 C2 H2B 109.3 . . ? O1 C2 H2A 109.3 . . ? O1 C3 H3A 109.4 . . ? O1 C3 H3B 109.4 . . ? O1 C3 C4 111.1(7) . . ? O2 C20 C19 110.7(8) . 3_655 ? O2 C20 H20B 109.5 . . ? O2 C20 H20A 109.5 . . ? O2 C21 H21A 110.1 . . ? O2 C21 H21B 110.1 . . ? O2 C21 C22 108.1(8) . . ? N1 C1 C2 121.9(7) . . ? N1 C4 C3 107.3(7) . . ? N1 C4 H4 109.7 . . ? N1 C4 C5 107.4(6) . . ? N1 C12 Au1 127.9(5) . . ? N1 C12 N3 103.2(6) . . ? N2 N3 C13 118.6(6) . . ? N2 C1 N1 110.6(8) . . ? N2 C1 C2 127.4(8) . . ? N3 C12 Au1 128.9(5) . . ? N4 C19 C20 122.5(8) 5_665 5_665 ? N4 C22 C21 104.8(7) . . ? N4 C22 H22 108.8 . . ? N4 C22 C23 112.7(7) . . ? N4 C30 Au1 126.7(6) . . ? N5 N6 C15 117.4(6) . . ? N5 C19 N4 110.1(7) . 5_665 ? N5 C19 C20 127.0(8) . 5_665 ? N6 C30 Au1 129.0(5) 3_655 . ? N6 C30 N4 104.1(6) 3_655 . ? C1 N1 C4 122.5(7) . . ? C1 N2 N3 102.8(6) . . ? C1 C2 H2B 109.3 . . ? C1 C2 H2A 109.3 . . ? H2B C2 H2A 108.0 . . ? C3 O1 C2 112.5(7) . . ? C3 C4 H4 109.7 . . ? C3 C4 C5 113.0(7) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C4 C5 H5B 108.8 . . ? C4 C5 H5A 108.8 . . ? C5 C4 H4 109.7 . . ? H5B C5 H5A 107.7 . . ? C6 C5 C4 113.7(7) . . ? C6 C5 H5B 108.8 . . ? C6 C5 H5A 108.8 . . ? C6 C7 H7 119.3 . . ? C6 C7 C8 121.4(11) . . ? C6 C11 C10 119.9(11) . . ? C6 C11 H11 120.1 . . ? C7 C6 C5 121.0(9) . . ? C7 C6 C11 118.2(9) . . ? C7 C8 H8 120.8 . . ? C8 C7 H7 119.3 . . ? C8 C9 H9 117.2 . . ? C8 C9 C10 125.6(11) . . ? C9 C8 C7 118.4(13) . . ? C9 C8 H8 120.8 . . ? C9 C10 H10 121.9 . . ? C9 C10 C11 116.2(12) . . ? C10 C9 H9 117.2 . . ? C10 C11 H11 120.1 . . ? C11 C6 C5 120.6(8) . . ? C11 C10 H10 121.9 . . ? C12 Au1 C30 176.7(3) . . ? C12 N1 C1 110.7(7) . . ? C12 N1 C4 126.7(7) . . ? C12 N3 N2 112.5(6) . . ? C12 N3 C13 128.8(6) . . ? C13 C14 H14 120.8 . . ? C13 C18 C17 119.3(7) . . ? C13 C18 H18 120.3 . . ? C14 C13 N3 119.6(6) . . ? C14 C15 N6 118.8(6) . . ? C14 C15 C16 123.4(7) . . ? C15 C14 C13 118.3(6) . . ? C15 C14 H14 120.8 . . ? C15 C16 H16 119.6 . . ? C16 C15 N6 117.7(6) . . ? C16 C17 H17 121.5 . . ? C16 C17 C18 116.9(6) . . ? C17 C16 C15 120.8(7) . . ? C17 C16 H16 119.6 . . ? C17 C18 H18 120.3 . . ? C18 C13 N3 119.2(6) . . ? C18 C13 C14 121.0(7) . . ? C18 C17 H17 121.5 . . ? C19 N4 C22 121.7(7) 3_655 . ? C19 N5 N6 102.7(6) . . ? C19 C20 H20B 109.5 3_655 . ? C19 C20 H20A 109.5 3_655 . ? H20B C20 H20A 108.1 . . ? C21 O2 C20 109.7(7) . . ? C21 C22 H22 108.8 . . ? H21A C21 H21B 108.4 . . ? C22 C21 H21A 110.1 . . ? C22 C21 H21B 110.1 . . ? C22 C23 H23A 108.3 . . ? C22 C23 H23B 108.3 . . ? C23 C22 C21 112.8(7) . . ? C23 C22 H22 108.8 . . ? H23A C23 H23B 107.4 . . ? C24 C23 C22 116.1(7) . . ? C24 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? C24 C25 H25 120.2 . . ? C24 C29 H29 121.0 . . ? C25 C24 C23 124.0(9) . . ? C25 C24 C29 115.3(9) . . ? C25 C26 H26 118.5 . . ? C26 C25 C24 119.5(11) . . ? C26 C25 H25 120.2 . . ? C26 C27 H27 120.5 . . ? C26 C27 C28 119.0(12) . . ? C27 C26 C25 123.0(11) . . ? C27 C26 H26 118.5 . . ? C27 C28 H28 117.6 . . ? C27 C28 C29 124.9(13) . . ? C28 C27 H27 120.5 . . ? C28 C29 C24 117.9(11) . . ? C28 C29 H29 121.0 . . ? C29 C24 C23 120.5(9) . . ? C29 C28 H28 117.6 . . ? C30 N4 C19 108.9(7) . 3_655 ? C30 N4 C22 129.3(7) . . ? C30 N6 N5 114.2(6) 5_665 . ? C30 N6 C15 128.2(6) 5_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C3 C4 N1 -52.3(8) . . . . ? O1 C3 C4 C5 65.8(9) . . . . ? O2 C21 C22 N4 -59.0(8) . . . . ? O2 C21 C22 C23 63.9(10) . . . . ? N1 C1 C2 O1 13.9(12) . . . . ? N1 C4 C5 C6 -172.6(7) . . . . ? N2 N3 C12 Au1 -177.5(5) . . . . ? N2 N3 C12 N1 0.8(8) . . . . ? N2 N3 C13 C14 -134.1(7) . . . . ? N2 N3 C13 C18 50.4(9) . . . . ? N2 C1 C2 O1 -164.5(8) . . . . ? N3 N2 C1 N1 2.6(9) . . . . ? N3 N2 C1 C2 -178.9(8) . . . . ? N3 C13 C14 C15 -178.7(7) . . . . ? N3 C13 C18 C17 175.1(7) . . . . ? N4 C22 C23 C24 -69.5(10) . . . . ? N5 N6 C15 C14 -124.3(8) . . . . ? N5 N6 C15 C16 52.7(9) . . . . ? N6 N5 C19 N4 1.0(8) . . . 5_665 ? N6 N5 C19 C20 -172.1(8) . . . 5_665 ? N6 C15 C16 C17 -178.2(7) . . . . ? C1 N1 C4 C3 21.8(10) . . . . ? C1 N1 C4 C5 -100.0(9) . . . . ? C1 N1 C12 Au1 179.2(5) . . . . ? C1 N1 C12 N3 0.8(8) . . . . ? C1 N2 N3 C12 -2.2(8) . . . . ? C1 N2 N3 C13 178.3(6) . . . . ? C2 O1 C3 C4 67.9(10) . . . . ? C3 O1 C2 C1 -45.5(11) . . . . ? C3 C4 C5 C6 69.2(9) . . . . ? C4 N1 C1 N2 174.9(7) . . . . ? C4 N1 C1 C2 -3.7(12) . . . . ? C4 N1 C12 Au1 2.0(11) . . . . ? C4 N1 C12 N3 -176.3(7) . . . . ? C4 C5 C6 C7 68.1(13) . . . . ? C4 C5 C6 C11 -106.4(10) . . . . ? C5 C6 C7 C8 178.8(11) . . . . ? C5 C6 C11 C10 -178.2(9) . . . . ? C6 C7 C8 C9 3(2) . . . . ? C7 C6 C11 C10 7.1(15) . . . . ? C7 C8 C9 C10 1(3) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C9 C10 C11 C6 -3.8(17) . . . . ? C11 C6 C7 C8 -6.6(19) . . . . ? C12 Au1 C30 N4 133(5) . . . . ? C12 Au1 C30 N6 -41(5) . . . 3_655 ? C12 N1 C1 N2 -2.3(10) . . . . ? C12 N1 C1 C2 179.0(8) . . . . ? C12 N1 C4 C3 -161.4(7) . . . . ? C12 N1 C4 C5 76.8(9) . . . . ? C12 N3 C13 C14 46.5(11) . . . . ? C12 N3 C13 C18 -129.0(8) . . . . ? C13 N3 C12 Au1 1.9(11) . . . . ? C13 N3 C12 N1 -179.8(7) . . . . ? C13 C14 C15 N6 -179.0(7) . . . . ? C13 C14 C15 C16 4.2(12) . . . . ? C14 C13 C18 C17 -0.3(11) . . . . ? C14 C15 C16 C17 -1.3(12) . . . . ? C15 C16 C17 C18 -2.4(12) . . . . ? C16 C17 C18 C13 3.1(12) . . . . ? C18 C13 C14 C15 -3.3(12) . . . . ? C19 N4 C22 C21 25.8(10) 3_655 . . . ? C19 N4 C22 C23 -97.1(9) 3_655 . . . ? C19 N4 C30 Au1 -173.3(6) 3_655 . . . ? C19 N4 C30 N6 2.4(8) 3_655 . . 3_655 ? C19 N5 N6 C15 174.8(6) . . . . ? C19 N5 N6 C30 0.6(8) . . . 5_665 ? C20 O2 C21 C22 75.0(9) . . . . ? C21 O2 C20 C19 -50.2(10) . . . 3_655 ? C21 C22 C23 C24 172.2(8) . . . . ? C22 N4 C30 Au1 3.8(11) . . . . ? C22 N4 C30 N6 179.4(7) . . . 3_655 ? C22 C23 C24 C25 101.5(11) . . . . ? C22 C23 C24 C29 -74.3(11) . . . . ? C23 C24 C25 C26 -180.0(10) . . . . ? C23 C24 C29 C28 -177.7(9) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C25 C24 C29 C28 6.2(14) . . . . ? C25 C26 C27 C28 -1(2) . . . . ? C26 C27 C28 C29 4(2) . . . . ? C27 C28 C29 C24 -6.4(18) . . . . ? C29 C24 C25 C26 -4.0(15) . . . . ? C30 Au1 C12 N1 67(5) . . . . ? C30 Au1 C12 N3 -115(5) . . . . ? C30 N4 C22 C21 -150.8(8) . . . . ? C30 N4 C22 C23 86.2(10) . . . . ? C30 N6 C15 C14 49.0(11) 5_665 . . . ? C30 N6 C15 C16 -133.9(8) 5_665 . . . ? # Attachment '[(S)-3Ag]3(PF6)2Cl.cif' data_110228_S4_WSP _database_code_depnum_ccdc_archive 'CCDC 836089' #TrackingRef '[(S)-3Ag]3(PF6)2Cl.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety ; C66 H85 Ag3 Cl N18 O6, C4 H8 O2, 2(F6 P), C H Cl3 ; _chemical_formula_sum 'C71 H93 Ag3 Cl4 F12 N18 O8 P2' _chemical_formula_weight 2082.99 _chemical_absolute_configuration unk _chemical_melting_point ? 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _cell_length_a 12.6553(3) _cell_length_b 13.0092(5) _cell_length_c 15.1663(4) _cell_angle_alpha 104.239(3) _cell_angle_beta 112.900(3) _cell_angle_gamma 99.765(3) _cell_volume 2128.74(12) _cell_formula_units_Z 1 _cell_measurement_reflns_used 12487 _cell_measurement_temperature 150.1 _cell_measurement_theta_max 29.1579 _cell_measurement_theta_min 2.9763 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.98515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1057 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 17685 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.98 _diffrn_ambient_temperature 150.1 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -1.00 55.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -16.8924 38.0000 30.0000 56 #__ type_ start__ end____ width___ exp.time_ 2 omega -8.00 85.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 77.0000 -120.0000 93 #__ type_ start__ end____ width___ exp.time_ 3 omega -43.00 50.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 -77.0000 -30.0000 93 #__ type_ start__ end____ width___ exp.time_ 4 omega 13.00 42.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 -62.0000 117.0000 29 #__ type_ start__ end____ width___ exp.time_ 5 omega -4.00 90.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 20.0174 77.0000 90.0000 94 #__ type_ start__ end____ width___ exp.time_ 6 omega -42.00 18.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -16.8924 38.0000 -150.0000 60 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0172113 _diffrn_orient_matrix_UB_12 -0.0179402 _diffrn_orient_matrix_UB_13 -0.0390926 _diffrn_orient_matrix_UB_21 -0.0071767 _diffrn_orient_matrix_UB_22 -0.053452 _diffrn_orient_matrix_UB_23 0.0044903 _diffrn_orient_matrix_UB_31 -0.0609316 _diffrn_orient_matrix_UB_32 -0.0170794 _diffrn_orient_matrix_UB_33 -0.0370717 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 12951 _reflns_number_total 13449 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 1.440 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.093 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(19) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1023 _refine_ls_number_reflns 13449 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0391 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+2.5636P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.1045 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.52472(3) 0.91730(3) 0.71407(3) 0.02490(10) Uani 1 1 d . . . Ag2 Ag 0.46060(3) 1.14041(3) 0.50596(3) 0.01876(9) Uani 1 1 d . . . Ag3 Ag 0.40505(3) 0.75719(3) 0.32980(3) 0.02334(10) Uani 1 1 d . . . Cl1 Cl 0.47457(14) 0.94211(11) 0.52168(10) 0.0283(3) Uani 1 1 d . . . Cl2 Cl 0.2973(5) 0.5226(4) 0.0646(3) 0.1443(19) Uani 1 1 d . . . Cl3 Cl 0.2291(3) 0.4528(3) -0.1479(3) 0.1110(12) Uani 1 1 d . . . Cl4 Cl 0.1517(3) 0.6271(2) -0.0534(2) 0.0770(7) Uani 1 1 d . . . P1 P 0.5663(2) 0.72657(18) 0.95079(15) 0.0459(5) Uani 1 1 d . . . P2 P 0.27583(15) 1.33524(16) 0.22454(14) 0.0411(4) Uani 1 1 d . . . F1 F 0.5676(6) 0.8242(6) 0.9071(5) 0.105(2) Uani 1 1 d . . . F2 F 0.6963(5) 0.7996(6) 1.0372(5) 0.0892(18) Uani 1 1 d . . . F3 F 0.5144(8) 0.7827(6) 1.0213(6) 0.113(3) Uani 1 1 d . . . F4 F 0.5652(7) 0.6304(5) 0.9977(6) 0.104(2) Uani 1 1 d . . . F5 F 0.6259(10) 0.6702(7) 0.8857(8) 0.165(5) Uani 1 1 d . . . F6 F 0.4382(6) 0.6533(8) 0.8638(5) 0.133(3) Uani 1 1 d . . . F7 F 0.4075(4) 1.3257(5) 0.2841(4) 0.0776(18) Uani 1 1 d . . . F8 F 0.2717(4) 1.3846(6) 0.3291(4) 0.093(2) Uani 1 1 d . . . F9 F 0.3354(6) 1.4570(5) 0.2384(5) 0.092(2) Uani 1 1 d . . . F10 F 0.2197(5) 1.2128(5) 0.2169(4) 0.0667(13) Uani 1 1 d . . . F11 F 0.1432(4) 1.3430(4) 0.1656(4) 0.0731(16) Uani 1 1 d . . . F12 F 0.2784(4) 1.2853(4) 0.1187(3) 0.0508(11) Uani 1 1 d . . . O1 O 1.0207(5) 1.0021(5) 0.9352(4) 0.0617(12) Uani 1 1 d . . . O2 O 0.0204(5) 1.2553(5) 0.4371(4) 0.0617(12) Uani 1 1 d . . . O3 O 0.0936(4) 0.7617(4) 0.7365(4) 0.0496(14) Uani 1 1 d . . . O4 O 0.8620(4) 0.7536(4) 0.3402(4) 0.0424(12) Uani 1 1 d . . . O5 O -0.1056(4) 0.5522(4) 0.1060(3) 0.0367(10) Uani 1 1 d . . . O6 O 0.8973(3) 1.4271(4) 0.5557(3) 0.0290(9) Uani 1 1 d . . . O7 O 0.7429(7) 1.4066(6) 1.2174(6) 0.081(2) Uani 1 1 d . . . O8 O 0.6159(5) 1.2496(5) 1.0958(4) 0.0524(14) Uani 1 1 d . . . N1 N 0.7940(4) 1.0135(4) 0.8588(3) 0.0270(11) Uani 1 1 d . . . N2 N 0.8473(5) 1.1969(4) 0.9224(4) 0.0365(13) Uani 1 1 d . . . N3 N 0.7241(4) 1.1506(4) 0.8566(3) 0.0220(9) Uani 1 1 d . . . N4 N 0.3681(4) 1.2449(4) 0.6617(3) 0.0220(9) Uani 1 1 d . . . N5 N 0.2795(4) 1.2893(4) 0.6719(4) 0.0288(11) Uani 1 1 d . . . N6 N 0.2333(4) 1.2037(4) 0.5120(4) 0.0208(10) Uani 1 1 d . . . N7 N 0.3529(4) 0.6717(4) 0.6293(3) 0.0222(10) Uani 1 1 d . . . N8 N 0.2514(4) 0.6081(4) 0.6274(4) 0.0307(11) Uani 1 1 d . . . N9 N 0.2936(4) 0.7855(4) 0.7089(4) 0.0248(11) Uani 1 1 d . . . N10 N 0.5941(4) 0.6459(4) 0.4432(3) 0.0195(9) Uani 1 1 d . . . N11 N 0.7011(4) 0.6232(4) 0.4549(4) 0.0291(11) Uani 1 1 d . . . N12 N 0.6522(4) 0.7224(4) 0.3556(4) 0.0221(10) Uani 1 1 d . . . N13 N 0.2060(4) 0.8294(4) 0.1762(3) 0.0180(9) Uani 1 1 d . . . N14 N 0.0842(4) 0.7971(4) 0.1088(3) 0.0233(10) Uani 1 1 d . . . N15 N 0.1277(4) 0.6856(4) 0.1961(3) 0.0207(9) Uani 1 1 d . . . N16 N 0.5550(4) 1.1622(4) 0.3450(3) 0.0186(9) Uani 1 1 d . . . N17 N 0.6424(4) 1.2254(4) 0.3292(4) 0.0252(10) Uani 1 1 d . . . N18 N 0.6821(4) 1.2737(4) 0.4907(3) 0.0200(9) Uani 1 1 d . . . C1 C 0.6895(5) 1.0393(4) 0.8163(4) 0.0208(11) Uani 1 1 d . . . C2 C 0.8851(6) 1.1104(5) 0.9216(5) 0.0401(16) Uani 1 1 d . . . C3 C 1.0113(7) 1.1083(7) 0.9780(6) 0.0563(11) Uani 1 1 d . . . H3a H 1.0678 1.1664 0.9728 0.068 Uiso 1 1 calc R . . H3b H 1.0324 1.1235 1.0510 0.068 Uiso 1 1 calc R . . C4 C 0.9301(7) 0.9180(7) 0.9353(6) 0.0563(11) Uani 1 1 d . . . H4a H 0.9286 0.9406 1.0020 0.068 Uiso 1 1 calc R . . H4b H 0.9502 0.8470 0.9254 0.068 Uiso 1 1 calc R . . C5 C 0.8081(6) 0.9017(5) 0.8515(5) 0.0294(13) Uani 1 1 d . . . H5 H 0.7470 0.8620 0.8677 0.035 Uiso 1 1 calc R . . C6 C 0.7818(6) 0.8343(6) 0.7442(5) 0.0340(14) Uani 1 1 d . . . H6 H 0.6973 0.8288 0.6989 0.041 Uiso 1 1 calc R . . C7 C 0.7847(8) 0.7170(6) 0.7374(6) 0.054(2) Uani 1 1 d . . . H7a H 0.7529 0.6706 0.6658 0.081 Uiso 1 1 calc R . . H7b H 0.7354 0.6870 0.7668 0.081 Uiso 1 1 calc R . . H7c H 0.8677 0.7174 0.7752 0.081 Uiso 1 1 calc R . . C8 C 0.8593(11) 0.8850(10) 0.7018(8) 0.079(3) Uani 1 1 d . . . H8a H 0.9440 0.9079 0.7517 0.119 Uiso 1 1 calc R . . H8b H 0.8372 0.9498 0.6875 0.119 Uiso 1 1 calc R . . H8c H 0.8468 0.8300 0.6387 0.119 Uiso 1 1 calc R . . C9 C 0.6517(5) 1.2223(4) 0.8447(4) 0.0233(12) Uani 1 1 d . . . C10 C 0.6926(5) 1.3263(5) 0.9234(4) 0.0288(13) Uani 1 1 d . . . H10 H 0.7664 1.3459 0.9830 0.035 Uiso 1 1 calc R . . C11 C 0.6259(6) 1.3978(6) 0.9132(5) 0.0359(15) Uani 1 1 d . . . H11 H 0.6542 1.4676 0.9660 0.043 Uiso 1 1 calc R . . C12 C 0.5176(6) 1.3719(5) 0.8278(4) 0.0314(13) Uani 1 1 d . . . H12 H 0.4710 1.4222 0.8217 0.038 Uiso 1 1 calc R . . C13 C 0.4795(5) 1.2702(4) 0.7518(4) 0.0204(11) Uani 1 1 d . . . C14 C 0.5447(5) 1.1954(4) 0.7587(4) 0.0212(11) Uani 1 1 d . . . H14 H 0.5164 1.1264 0.7050 0.025 Uiso 1 1 calc R . . C15 C 0.3425(5) 1.1925(4) 0.5640(4) 0.0207(11) Uani 1 1 d . . . C16 C 0.2004(5) 1.2637(5) 0.5797(4) 0.0258(12) Uani 1 1 d . . . C17 C 0.0891(8) 1.3011(7) 0.5446(6) 0.0563(11) Uani 1 1 d . . . H17a H 0.0395 1.2779 0.5771 0.068 Uiso 1 1 calc R . . H17b H 0.1128 1.3832 0.5661 0.068 Uiso 1 1 calc R . . C18 C 0.0956(8) 1.2580(7) 0.3869(6) 0.0563(11) Uani 1 1 d . . . H18a H 0.1545 1.3326 0.4162 0.068 Uiso 1 1 calc R . . H18b H 0.0459 1.2430 0.3134 0.068 Uiso 1 1 calc R . . C19 C 0.1614(5) 1.1713(5) 0.3999(5) 0.0278(13) Uani 1 1 d . . . H19 H 0.2169 1.1767 0.3679 0.033 Uiso 1 1 calc R . . C20 C 0.0757(5) 1.0524(5) 0.3527(4) 0.0281(12) Uani 1 1 d . . . H20 H 0.0157 1.0507 0.3803 0.034 Uiso 1 1 calc R . . C21 C 0.1388(6) 0.9672(5) 0.3775(5) 0.0353(14) Uani 1 1 d . . . H21a H 0.0809 0.8928 0.3415 0.053 Uiso 1 1 calc R . . H21b H 0.1739 0.9820 0.4511 0.053 Uiso 1 1 calc R . . H21c H 0.2026 0.9715 0.3560 0.053 Uiso 1 1 calc R . . C22 C 0.0072(7) 1.0207(7) 0.2363(5) 0.0507(19) Uani 1 1 d . . . H22a H 0.0647 1.0285 0.2082 0.076 Uiso 1 1 calc R . . H22b H -0.0427 1.0697 0.2201 0.076 Uiso 1 1 calc R . . H22c H -0.0441 0.9435 0.2064 0.076 Uiso 1 1 calc R . . C23 C 0.3798(5) 0.7807(5) 0.6782(4) 0.0219(11) Uani 1 1 d . . . C24 C 0.2192(5) 0.6823(5) 0.6769(4) 0.0303(14) Uani 1 1 d . . . C25 C 0.1146(7) 0.6603(6) 0.7008(6) 0.048(2) Uani 1 1 d . . . H25a H 0.0422 0.6094 0.6387 0.058 Uiso 1 1 calc R . . H25b H 0.1325 0.6246 0.7533 0.058 Uiso 1 1 calc R . . C26 C 0.2010(6) 0.8431(6) 0.8162(5) 0.0389(16) Uani 1 1 d . . . H26a H 0.2416 0.8103 0.8677 0.047 Uiso 1 1 calc R . . H26b H 0.1802 0.9063 0.8501 0.047 Uiso 1 1 calc R . . C27 C 0.2872(6) 0.8855(5) 0.7758(5) 0.0276(13) Uani 1 1 d . . . H27 H 0.3686 0.9213 0.8354 0.033 Uiso 1 1 calc R . . C28 C 0.2575(6) 0.9720(6) 0.7245(5) 0.0366(15) Uani 1 1 d . . . H28 H 0.3172 0.9870 0.6978 0.044 Uiso 1 1 calc R . . C29 C 0.1356(7) 0.9353(9) 0.6354(6) 0.060(2) Uani 1 1 d . . . H29a H 0.1226 0.8619 0.5889 0.090 Uiso 1 1 calc R . . H29b H 0.1303 0.9887 0.5994 0.090 Uiso 1 1 calc R . . H29c H 0.0741 0.9311 0.6595 0.090 Uiso 1 1 calc R . . C30 C 0.2791(8) 1.0810(6) 0.8051(7) 0.056(2) Uani 1 1 d . . . H30a H 0.2623 1.1370 0.7730 0.083 Uiso 1 1 calc R . . H30b H 0.3629 1.1069 0.8574 0.083 Uiso 1 1 calc R . . H30c H 0.2259 1.0690 0.8368 0.083 Uiso 1 1 calc R . . C31 C 0.4178(5) 0.6151(5) 0.5866(4) 0.0228(11) Uani 1 1 d . . . C32 C 0.4219(5) 0.5112(5) 0.5928(5) 0.0294(13) Uani 1 1 d . . . H32 H 0.3858 0.4813 0.6291 0.035 Uiso 1 1 calc R . . C33 C 0.4768(6) 0.4517(5) 0.5479(5) 0.0331(14) Uani 1 1 d . . . H33 H 0.4774 0.3799 0.5515 0.040 Uiso 1 1 calc R . . C34 C 0.5329(5) 0.4963(5) 0.4959(4) 0.0253(12) Uani 1 1 d . . . H34 H 0.5707 0.4548 0.4636 0.030 Uiso 1 1 calc R . . C35 C 0.5321(5) 0.6012(4) 0.4926(4) 0.0212(11) Uani 1 1 d . . . C36 C 0.4743(4) 0.6615(4) 0.5363(4) 0.0193(11) Uani 1 1 d . . . H36 H 0.4729 0.7331 0.5324 0.023 Uiso 1 1 calc R . . C37 C 0.5619(5) 0.7067(5) 0.3835(4) 0.0213(11) Uani 1 1 d . . . C38 C 0.7315(5) 0.6713(5) 0.3991(5) 0.0265(12) Uani 1 1 d . . . C39 C 0.8406(6) 0.6712(6) 0.3820(6) 0.0428(17) Uani 1 1 d . . . H39a H 0.9112 0.6859 0.4476 0.051 Uiso 1 1 calc R . . H39b H 0.8283 0.5974 0.3350 0.051 Uiso 1 1 calc R . . C40 C 0.7558(6) 0.7447(6) 0.2545(5) 0.0371(15) Uani 1 1 d . . . H40a H 0.7190 0.6666 0.2079 0.044 Uiso 1 1 calc R . . H40b H 0.7765 0.7907 0.2169 0.044 Uiso 1 1 calc R . . C41 C 0.6648(5) 0.7840(5) 0.2888(5) 0.0276(13) Uani 1 1 d . . . H41 H 0.5855 0.7596 0.2270 0.033 Uiso 1 1 calc R . . C42 C 0.6954(7) 0.9089(6) 0.3414(5) 0.0378(16) Uani 1 1 d . . . H42 H 0.6298 0.9211 0.3600 0.045 Uiso 1 1 calc R . . C43 C 0.6938(8) 0.9684(7) 0.2660(7) 0.058(2) Uani 1 1 d . . . H43a H 0.7662 0.9707 0.2562 0.087 Uiso 1 1 calc R . . H43b H 0.6918 1.0443 0.2928 0.087 Uiso 1 1 calc R . . H43c H 0.6224 0.9283 0.2006 0.087 Uiso 1 1 calc R . . C44 C 0.8132(8) 0.9581(7) 0.4398(7) 0.058(2) Uani 1 1 d . . . H44a H 0.8136 0.9146 0.4841 0.087 Uiso 1 1 calc R . . H44b H 0.8209 1.0352 0.4748 0.087 Uiso 1 1 calc R . . H44c H 0.8808 0.9563 0.4235 0.087 Uiso 1 1 calc R . . C45 C 0.2364(4) 0.7614(4) 0.2300(4) 0.0165(10) Uani 1 1 d . . . C46 C 0.0408(5) 0.7111(5) 0.1244(4) 0.0222(11) Uani 1 1 d . . . C47 C -0.0866(5) 0.6364(6) 0.0649(5) 0.0336(14) Uani 1 1 d . . . H47a H -0.1423 0.6811 0.0666 0.040 Uiso 1 1 calc R . . H47b H -0.1041 0.6019 -0.0071 0.040 Uiso 1 1 calc R . . C48 C -0.0073(6) 0.5055(5) 0.1328(5) 0.0374(15) Uani 1 1 d . . . H48a H 0.0129 0.4857 0.0752 0.045 Uiso 1 1 calc R . . H48b H -0.0309 0.4370 0.1466 0.045 Uiso 1 1 calc R . . C49 C 0.1011(5) 0.5881(5) 0.2261(5) 0.0256(12) Uani 1 1 d . . . H49 H 0.1703 0.5566 0.2413 0.031 Uiso 1 1 calc R . . C50 C 0.0780(7) 0.6188(7) 0.3200(6) 0.0520(8) Uani 1 1 d . . . H50 H 0.0062 0.6468 0.3032 0.062 Uiso 1 1 calc R . . C51 C 0.0525(7) 0.5157(7) 0.3476(6) 0.0520(8) Uani 1 1 d . . . H51a H -0.0246 0.4632 0.2944 0.078 Uiso 1 1 calc R . . H51b H 0.0491 0.5368 0.4129 0.078 Uiso 1 1 calc R . . H51c H 0.1166 0.4809 0.3533 0.078 Uiso 1 1 calc R . . C52 C 0.1843(7) 0.7068(7) 0.4123(6) 0.0520(8) Uani 1 1 d . . . H52a H 0.1682 0.7181 0.4717 0.078 Uiso 1 1 calc R . . H52b H 0.1970 0.7767 0.3989 0.078 Uiso 1 1 calc R . . H52c H 0.2565 0.6824 0.4261 0.078 Uiso 1 1 calc R . . C53 C 0.2827(5) 0.9226(4) 0.1747(4) 0.0204(11) Uani 1 1 d . . . C54 C 0.2508(5) 0.9409(5) 0.0824(4) 0.0263(12) Uani 1 1 d . . . H54 H 0.1809 0.8923 0.0230 0.032 Uiso 1 1 calc R . . C55 C 0.3222(6) 1.0307(5) 0.0785(4) 0.0299(13) Uani 1 1 d . . . H55 H 0.3019 1.0434 0.0156 0.036 Uiso 1 1 calc R . . C56 C 0.4224(5) 1.1022(5) 0.1645(4) 0.0271(12) Uani 1 1 d . . . H56 H 0.4709 1.1641 0.1612 0.032 Uiso 1 1 calc R . . C57 C 0.4519(5) 1.0835(5) 0.2558(4) 0.0201(11) Uani 1 1 d . . . C58 C 0.3834(4) 0.9931(4) 0.2623(4) 0.0172(10) Uani 1 1 d . . . H58 H 0.4049 0.9799 0.3250 0.021 Uiso 1 1 calc R . . C59 C 0.5756(5) 1.1907(4) 0.4421(4) 0.0194(11) Uani 1 1 d . . . C60 C 0.7169(5) 1.2927(5) 0.4196(4) 0.0210(11) Uani 1 1 d . . . C61 C 0.8254(5) 1.3856(5) 0.4490(5) 0.0252(12) Uani 1 1 d . . . H61a H 0.8730 1.3586 0.4149 0.030 Uiso 1 1 calc R . . H61b H 0.7998 1.4461 0.4259 0.030 Uiso 1 1 calc R . . C62 C 0.8266(5) 1.4498(5) 0.6062(5) 0.0315(14) Uani 1 1 d . . . H62a H 0.7738 1.4916 0.5741 0.038 Uiso 1 1 calc R . . H62b H 0.8796 1.4968 0.6783 0.038 Uiso 1 1 calc R . . C63 C 0.7499(5) 1.3428(6) 0.6016(4) 0.0319(14) Uani 1 1 d . . . H63 H 0.6924 1.3598 0.6293 0.038 Uiso 1 1 calc R . . C64 C 0.8285(7) 1.2807(7) 0.6616(6) 0.0520(8) Uani 1 1 d . . . H64 H 0.8961 1.2794 0.6432 0.062 Uiso 1 1 calc R . . C65 C 0.7666(7) 1.1644(7) 0.6457(6) 0.0520(8) Uani 1 1 d . . . H65a H 0.7046 1.1647 0.6691 0.078 Uiso 1 1 calc R . . H65b H 0.8254 1.1322 0.6844 0.078 Uiso 1 1 calc R . . H65c H 0.7294 1.1200 0.5730 0.078 Uiso 1 1 calc R . . C66 C 0.8817(7) 1.3532(7) 0.7752(6) 0.0520(8) Uani 1 1 d . . . H66a H 0.8193 1.3794 0.7883 0.078 Uiso 1 1 calc R . . H66b H 0.9481 1.4171 0.7913 0.078 Uiso 1 1 calc R . . H66c H 0.9116 1.3090 0.8180 0.078 Uiso 1 1 calc R . . C67 C 0.2648(10) 0.5635(10) -0.0376(7) 0.072(3) Uani 1 1 d . . . H67 H 0.3385 0.6203 -0.0239 0.086 Uiso 1 1 calc R . . C68 C 0.6445(9) 1.3548(8) 1.1514(7) 0.061(2) Uani 1 1 d . . . C69 C 0.5404(10) 1.4009(9) 1.1203(9) 0.082(3) Uani 1 1 d . . . H69a H 0.5362 1.4283 1.0646 0.123 Uiso 1 1 calc R . . H69b H 0.5509 1.4622 1.1786 0.123 Uiso 1 1 calc R . . H69c H 0.4658 1.3424 1.0972 0.123 Uiso 1 1 calc R . . C70 C 0.7104(9) 1.1978(8) 1.1204(6) 0.058(2) Uani 1 1 d . . . H70a H 0.7429 1.2035 1.1929 0.069 Uiso 1 1 calc R . . H70b H 0.7766 1.2354 1.1093 0.069 Uiso 1 1 calc R . . C71 C 0.6592(12) 1.0794(10) 1.0535(8) 0.081(3) Uani 1 1 d . . . H71a H 0.6052 1.0737 0.9843 0.121 Uiso 1 1 calc R . . H71b H 0.6141 1.0375 1.0799 0.121 Uiso 1 1 calc R . . H71c H 0.7244 1.0488 1.0522 0.121 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 0.01759(19) 0.0169(2) 0.0360(2) 0.00545(17) 0.01193(17) 0.00093(16) Ag2 0.01622(17) 0.0200(2) 0.02012(19) 0.00588(15) 0.00942(15) 0.00412(15) Ag3 0.01448(18) 0.0289(2) 0.0299(2) 0.01820(18) 0.00796(16) 0.00749(17) Cl1 0.0442(8) 0.0178(6) 0.0222(7) 0.0085(5) 0.0129(6) 0.0100(6) Cl2 0.213(5) 0.197(5) 0.140(3) 0.116(4) 0.125(4) 0.146(4) Cl3 0.132(3) 0.075(2) 0.121(3) -0.0123(17) 0.086(2) 0.0179(19) Cl4 0.0981(18) 0.0682(16) 0.0830(17) 0.0186(13) 0.0607(15) 0.0302(15) P1 0.0551(12) 0.0432(11) 0.0371(10) 0.0168(9) 0.0182(9) 0.0110(10) P2 0.0265(8) 0.0425(10) 0.0383(10) -0.0054(8) 0.0118(7) 0.0067(8) F1 0.100(5) 0.101(5) 0.099(5) 0.077(4) 0.012(4) 0.007(4) F2 0.072(4) 0.088(5) 0.077(4) 0.030(3) 0.006(3) 0.017(3) F3 0.145(6) 0.079(5) 0.156(7) 0.029(5) 0.114(6) 0.039(5) F4 0.159(7) 0.051(4) 0.118(5) 0.050(4) 0.061(5) 0.040(4) F5 0.209(10) 0.110(7) 0.177(9) -0.024(6) 0.158(8) -0.014(6) F6 0.085(5) 0.159(8) 0.084(5) 0.059(5) -0.008(4) -0.046(5) F7 0.043(3) 0.090(4) 0.059(3) -0.011(3) 0.001(2) 0.029(3) F8 0.048(3) 0.140(6) 0.047(3) -0.026(3) 0.018(2) 0.012(3) F9 0.097(5) 0.039(3) 0.116(5) 0.003(3) 0.048(4) -0.001(3) F10 0.076(3) 0.067(3) 0.061(3) 0.031(3) 0.034(3) 0.008(3) F11 0.046(3) 0.065(3) 0.070(3) -0.011(3) 0.005(2) 0.028(3) F12 0.051(2) 0.047(3) 0.041(2) 0.0023(19) 0.020(2) 0.004(2) O1 0.0335(19) 0.048(2) 0.065(3) 0.0010(19) -0.0078(18) 0.0217(19) O2 0.0335(19) 0.048(2) 0.065(3) 0.0010(19) -0.0078(18) 0.0217(19) O3 0.038(3) 0.049(3) 0.052(3) -0.006(2) 0.032(2) -0.008(2) O4 0.039(3) 0.048(3) 0.069(3) 0.031(3) 0.041(3) 0.023(2) O5 0.021(2) 0.030(2) 0.042(3) 0.015(2) -0.0002(18) -0.0041(19) O6 0.0160(18) 0.029(2) 0.039(2) 0.0094(19) 0.0130(18) 0.0020(18) O7 0.070(4) 0.071(5) 0.078(5) 0.012(4) 0.029(4) -0.004(4) O8 0.064(3) 0.048(3) 0.051(3) 0.020(3) 0.033(3) 0.010(3) N1 0.031(3) 0.022(3) 0.017(2) 0.0039(19) 0.004(2) 0.003(2) N2 0.022(2) 0.024(3) 0.036(3) 0.006(2) -0.009(2) 0.000(2) N3 0.018(2) 0.019(2) 0.018(2) 0.0062(18) -0.0010(18) -0.0007(19) N4 0.019(2) 0.024(2) 0.027(2) 0.0086(19) 0.0135(19) 0.0088(19) N5 0.028(2) 0.026(3) 0.035(3) 0.005(2) 0.019(2) 0.013(2) N6 0.023(2) 0.014(2) 0.024(2) 0.0046(18) 0.010(2) 0.007(2) N7 0.024(2) 0.023(2) 0.016(2) 0.0064(18) 0.0094(18) -0.003(2) N8 0.027(3) 0.026(3) 0.029(3) 0.004(2) 0.013(2) -0.008(2) N9 0.023(2) 0.022(3) 0.023(2) 0.001(2) 0.013(2) -0.004(2) N10 0.018(2) 0.017(2) 0.026(2) 0.0083(18) 0.0120(19) 0.0066(19) N11 0.026(2) 0.031(3) 0.044(3) 0.024(2) 0.018(2) 0.018(2) N12 0.020(2) 0.021(2) 0.029(3) 0.010(2) 0.012(2) 0.009(2) N13 0.016(2) 0.018(2) 0.015(2) 0.0076(17) 0.0025(17) 0.0032(18) N14 0.016(2) 0.023(2) 0.024(2) 0.0080(19) 0.0031(18) 0.006(2) N15 0.016(2) 0.016(2) 0.025(2) 0.0067(18) 0.0044(18) 0.0033(19) N16 0.019(2) 0.015(2) 0.021(2) 0.0061(17) 0.0114(18) 0.0002(18) N17 0.022(2) 0.027(3) 0.029(3) 0.011(2) 0.015(2) 0.003(2) N18 0.016(2) 0.021(2) 0.023(2) 0.0059(19) 0.0102(19) 0.0032(19) C1 0.026(3) 0.020(3) 0.017(3) 0.006(2) 0.010(2) 0.004(2) C2 0.035(3) 0.025(3) 0.030(3) 0.000(3) -0.007(3) 0.001(3) C3 0.049(2) 0.049(2) 0.048(2) 0.0130(18) -0.0028(18) 0.026(2) C4 0.049(2) 0.049(2) 0.048(2) 0.0130(18) -0.0028(18) 0.026(2) C5 0.036(3) 0.027(3) 0.028(3) 0.016(3) 0.010(3) 0.016(3) C6 0.034(3) 0.034(4) 0.032(3) 0.009(3) 0.011(3) 0.018(3) C7 0.066(5) 0.031(4) 0.044(4) -0.004(3) 0.011(4) 0.024(4) C8 0.121(9) 0.101(8) 0.068(6) 0.052(6) 0.068(6) 0.063(8) C9 0.027(3) 0.010(2) 0.024(3) 0.000(2) 0.010(2) -0.004(2) C10 0.026(3) 0.025(3) 0.018(3) -0.004(2) 0.001(2) 0.002(3) C11 0.043(4) 0.028(3) 0.019(3) -0.009(2) 0.011(3) 0.001(3) C12 0.037(3) 0.028(3) 0.027(3) 0.003(2) 0.014(3) 0.013(3) C13 0.021(3) 0.016(3) 0.021(3) 0.004(2) 0.010(2) 0.002(2) C14 0.027(3) 0.015(3) 0.022(3) 0.006(2) 0.013(2) 0.002(2) C15 0.019(3) 0.017(3) 0.028(3) 0.007(2) 0.013(2) 0.005(2) C16 0.023(3) 0.029(3) 0.031(3) 0.012(2) 0.014(2) 0.013(3) C17 0.049(2) 0.049(2) 0.048(2) 0.0130(18) -0.0028(18) 0.026(2) C18 0.049(2) 0.049(2) 0.048(2) 0.0130(18) -0.0028(18) 0.026(2) C19 0.021(3) 0.030(3) 0.030(3) 0.014(3) 0.007(2) 0.010(3) C20 0.021(3) 0.024(3) 0.029(3) 0.001(2) 0.009(2) 0.002(2) C21 0.033(3) 0.022(3) 0.040(4) 0.004(3) 0.011(3) 0.003(3) C22 0.048(4) 0.049(5) 0.033(4) 0.007(3) 0.001(3) 0.012(4) C23 0.020(2) 0.025(3) 0.015(3) 0.007(2) 0.005(2) 0.000(2) C24 0.030(3) 0.028(3) 0.021(3) -0.002(2) 0.013(2) -0.010(3) C25 0.047(4) 0.039(4) 0.056(5) 0.002(4) 0.037(4) -0.010(3) C26 0.048(4) 0.030(4) 0.038(4) 0.003(3) 0.029(3) 0.002(3) C27 0.031(3) 0.023(3) 0.027(3) 0.006(2) 0.014(3) 0.003(3) C28 0.046(4) 0.036(4) 0.045(4) 0.020(3) 0.032(3) 0.017(3) C29 0.053(5) 0.096(7) 0.056(5) 0.041(5) 0.034(4) 0.038(5) C30 0.076(6) 0.036(4) 0.082(6) 0.025(4) 0.057(5) 0.021(4) C31 0.019(3) 0.026(3) 0.020(3) 0.012(2) 0.003(2) 0.006(2) C32 0.032(3) 0.023(3) 0.029(3) 0.019(2) 0.008(3) -0.003(3) C33 0.032(3) 0.013(3) 0.058(4) 0.020(3) 0.019(3) 0.007(3) C34 0.020(3) 0.021(3) 0.030(3) 0.009(2) 0.007(2) 0.006(2) C35 0.017(2) 0.017(3) 0.027(3) 0.011(2) 0.007(2) 0.005(2) C36 0.016(2) 0.014(3) 0.020(3) 0.004(2) 0.004(2) 0.000(2) C37 0.018(2) 0.024(3) 0.018(3) 0.007(2) 0.005(2) 0.006(2) C38 0.029(3) 0.022(3) 0.035(3) 0.009(2) 0.018(3) 0.016(3) C39 0.041(4) 0.045(4) 0.073(5) 0.031(4) 0.044(4) 0.025(3) C40 0.050(4) 0.038(4) 0.044(4) 0.019(3) 0.035(3) 0.023(3) C41 0.027(3) 0.034(3) 0.028(3) 0.013(3) 0.016(3) 0.010(3) C42 0.056(4) 0.040(4) 0.047(4) 0.026(3) 0.041(4) 0.026(4) C43 0.073(6) 0.051(5) 0.089(6) 0.046(5) 0.056(5) 0.033(5) C44 0.068(5) 0.043(5) 0.063(5) 0.007(4) 0.042(5) 0.001(4) C45 0.012(2) 0.019(3) 0.017(2) 0.006(2) 0.0052(19) 0.004(2) C46 0.015(2) 0.025(3) 0.024(3) 0.009(2) 0.005(2) 0.009(2) C47 0.016(3) 0.036(4) 0.035(3) 0.012(3) 0.000(2) 0.001(3) C48 0.028(3) 0.019(3) 0.045(4) 0.005(3) 0.002(3) 0.001(3) C49 0.017(3) 0.014(3) 0.039(3) 0.009(2) 0.007(2) 0.002(2) C50 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C51 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C52 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C53 0.020(2) 0.018(3) 0.026(3) 0.008(2) 0.012(2) 0.005(2) C54 0.022(3) 0.024(3) 0.023(3) 0.008(2) 0.002(2) 0.002(2) C55 0.036(3) 0.035(3) 0.017(3) 0.017(2) 0.009(2) 0.003(3) C56 0.031(3) 0.025(3) 0.024(3) 0.012(2) 0.012(2) 0.003(3) C57 0.017(2) 0.022(3) 0.020(3) 0.005(2) 0.010(2) 0.004(2) C58 0.016(2) 0.020(3) 0.018(2) 0.006(2) 0.008(2) 0.008(2) C59 0.024(3) 0.021(3) 0.024(3) 0.013(2) 0.015(2) 0.013(2) C60 0.019(2) 0.026(3) 0.026(3) 0.014(2) 0.014(2) 0.011(2) C61 0.021(3) 0.022(3) 0.034(3) 0.012(2) 0.013(2) 0.006(2) C62 0.021(3) 0.030(3) 0.035(3) 0.002(3) 0.010(3) 0.006(3) C63 0.020(3) 0.037(4) 0.023(3) -0.001(3) 0.008(2) -0.008(3) C64 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C65 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C66 0.0493(18) 0.054(2) 0.0461(18) 0.0256(16) 0.0140(14) 0.0049(16) C67 0.079(7) 0.085(7) 0.060(6) 0.016(5) 0.042(5) 0.032(6) C68 0.066(6) 0.062(6) 0.069(6) 0.032(5) 0.044(5) 0.004(5) C69 0.084(7) 0.072(7) 0.122(9) 0.033(6) 0.077(7) 0.026(6) C70 0.080(6) 0.065(6) 0.049(5) 0.024(4) 0.044(5) 0.027(5) C71 0.129(10) 0.089(8) 0.072(7) 0.044(6) 0.072(7) 0.057(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 Cl1 2.8483(14) . ? Ag1 C1 2.104(6) . ? Ag1 C23 2.112(6) . ? Ag2 Cl1 2.6773(14) . ? Ag2 C15 2.131(5) . ? Ag2 C59 2.138(5) . ? Ag3 C37 2.116(5) . ? Ag3 C45 2.101(5) . ? Cl2 C67 1.684(11) . ? Cl3 C67 1.757(10) . ? Cl4 C67 1.738(10) . ? P1 F1 1.571(6) . ? P1 F2 1.583(6) . ? P1 F3 1.560(6) . ? P1 F4 1.584(6) . ? P1 F5 1.579(7) . ? P1 F6 1.572(7) . ? P2 F7 1.601(5) . ? P2 F8 1.583(5) . ? P2 F9 1.558(6) . ? P2 F10 1.587(6) . ? P2 F11 1.600(5) . ? P2 F12 1.592(4) . ? O1 C3 1.421(9) . ? O1 C4 1.445(11) . ? O2 C17 1.418(10) . ? O2 C18 1.433(12) . ? O3 C25 1.408(10) . ? O3 C26 1.426(8) . ? O4 C39 1.412(8) . ? O4 C40 1.423(8) . ? O5 C47 1.418(8) . ? O5 C48 1.437(8) . ? O6 C61 1.413(7) . ? O6 C62 1.409(7) . ? O7 C68 1.192(11) . ? O8 C68 1.320(11) . ? O8 C70 1.439(11) . ? N1 C1 1.367(7) . ? N1 C2 1.374(8) . ? N1 C5 1.477(8) . ? N2 N3 1.402(7) . ? N2 C2 1.295(9) . ? N3 C1 1.342(7) . ? N3 C9 1.409(7) . ? N4 N5 1.388(6) . ? N4 C13 1.444(7) . ? N4 C15 1.348(7) . ? N5 C16 1.279(8) . ? N6 C15 1.353(7) . ? N6 C16 1.373(7) . ? N6 C19 1.487(7) . ? N7 N8 1.391(6) . ? N7 C23 1.341(7) . ? N7 C31 1.421(7) . ? N8 C24 1.296(8) . ? N9 C23 1.347(7) . ? N9 C24 1.349(8) . ? N9 C27 1.476(8) . ? N10 N11 1.388(6) . ? N10 C35 1.425(7) . ? N10 C37 1.337(7) . ? N11 C38 1.300(8) . ? N12 C37 1.366(7) . ? N12 C38 1.346(7) . ? N12 C41 1.475(8) . ? N13 N14 1.393(6) . ? N13 C45 1.350(7) . ? N13 C53 1.429(7) . ? N14 C46 1.277(7) . ? N15 C45 1.367(7) . ? N15 C46 1.369(7) . ? N15 C49 1.478(7) . ? N16 N17 1.397(6) . ? N16 C57 1.440(7) . ? N16 C59 1.331(7) . ? N17 C60 1.287(7) . ? N18 C59 1.366(7) . ? N18 C60 1.372(7) . ? N18 C63 1.499(7) . ? C2 C3 1.499(10) . ? C3 H3a 0.9900 . ? C3 H3b 0.9900 . ? C4 H4a 0.9900 . ? C4 H4b 0.9900 . ? C4 C5 1.508(9) . ? C5 H5 1.0000 . ? C5 C6 1.519(9) . ? C6 H6 1.0000 . ? C6 C7 1.511(10) . ? C6 C8 1.512(11) . ? C7 H7a 0.9800 . ? C7 H7b 0.9800 . ? C7 H7c 0.9800 . ? C8 H8a 0.9800 . ? C8 H8b 0.9800 . ? C8 H8c 0.9800 . ? C9 C10 1.418(7) . ? C9 C14 1.378(8) . ? C10 H10 0.9500 . ? C10 C11 1.355(9) . ? C11 H11 0.9500 . ? C11 C12 1.384(9) . ? C12 H12 0.9500 . ? C12 C13 1.383(8) . ? C13 C14 1.376(8) . ? C14 H14 0.9500 . ? C16 C17 1.510(9) . ? C17 H17a 0.9900 . ? C17 H17b 0.9900 . ? C18 H18a 0.9900 . ? C18 H18b 0.9900 . ? C18 C19 1.518(9) . ? C19 H19 1.0000 . ? C19 C20 1.537(8) . ? C20 H20 1.0000 . ? C20 C21 1.509(9) . ? C20 C22 1.538(9) . ? C21 H21a 0.9800 . ? C21 H21b 0.9800 . ? C21 H21c 0.9800 . ? C22 H22a 0.9800 . ? C22 H22b 0.9800 . ? C22 H22c 0.9800 . ? C24 C25 1.503(8) . ? C25 H25a 0.9900 . ? C25 H25b 0.9900 . ? C26 H26a 0.9900 . ? C26 H26b 0.9900 . ? C26 C27 1.534(8) . ? C27 H27 1.0000 . ? C27 C28 1.536(9) . ? C28 H28 1.0000 . ? C28 C29 1.498(11) . ? C28 C30 1.529(10) . ? C29 H29a 0.9800 . ? C29 H29b 0.9800 . ? C29 H29c 0.9800 . ? C30 H30a 0.9800 . ? C30 H30b 0.9800 . ? C30 H30c 0.9800 . ? C31 C32 1.386(8) . ? C31 C36 1.400(8) . ? C32 H32 0.9500 . ? C32 C33 1.355(9) . ? C33 H33 0.9500 . ? C33 C34 1.409(9) . ? C34 H34 0.9500 . ? C34 C35 1.379(8) . ? C35 C36 1.381(8) . ? C36 H36 0.9500 . ? C38 C39 1.501(8) . ? C39 H39a 0.9900 . ? C39 H39b 0.9900 . ? C40 H40a 0.9900 . ? C40 H40b 0.9900 . ? C40 C41 1.548(8) . ? C41 H41 1.0000 . ? C41 C42 1.527(9) . ? C42 H42 1.0000 . ? C42 C43 1.527(10) . ? C42 C44 1.528(12) . ? C43 H43a 0.9800 . ? C43 H43b 0.9800 . ? C43 H43c 0.9800 . ? C44 H44a 0.9800 . ? C44 H44b 0.9800 . ? C44 H44c 0.9800 . ? C46 C47 1.504(8) . ? C47 H47a 0.9900 . ? C47 H47b 0.9900 . ? C48 H48a 0.9900 . ? C48 H48b 0.9900 . ? C48 C49 1.510(8) . ? C49 H49 1.0000 . ? C49 C50 1.536(10) . ? C50 H50 1.0000 . ? C50 C51 1.521(11) . ? C50 C52 1.519(11) . ? C51 H51a 0.9800 . ? C51 H51b 0.9800 . ? C51 H51c 0.9800 . ? C52 H52a 0.9800 . ? C52 H52b 0.9800 . ? C52 H52c 0.9800 . ? C53 C54 1.391(8) . ? C53 C58 1.384(7) . ? C54 H54 0.9500 . ? C54 C55 1.380(8) . ? C55 H55 0.9500 . ? C55 C56 1.375(8) . ? C56 H56 0.9500 . ? C56 C57 1.383(8) . ? C57 C58 1.386(7) . ? C58 H58 0.9500 . ? C60 C61 1.497(8) . ? C61 H61a 0.9900 . ? C61 H61b 0.9900 . ? C62 H62a 0.9900 . ? C62 H62b 0.9900 . ? C62 C63 1.526(9) . ? C63 H63 1.0000 . ? C63 C64 1.548(10) . ? C64 H64 1.0000 . ? C64 C65 1.494(11) . ? C64 C66 1.546(11) . ? C65 H65a 0.9800 . ? C65 H65b 0.9800 . ? C65 H65c 0.9800 . ? C66 H66a 0.9800 . ? C66 H66b 0.9800 . ? C66 H66c 0.9800 . ? C67 H67 1.0000 . ? C68 C69 1.497(14) . ? C69 H69a 0.9800 . ? C69 H69b 0.9800 . ? C69 H69c 0.9800 . ? C70 H70a 0.9900 . ? C70 H70b 0.9900 . ? C70 C71 1.485(14) . ? C71 H71a 0.9800 . ? C71 H71b 0.9800 . ? C71 H71c 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 C1 Ag1 Cl1 104.63(14) . . ? C1 Ag1 C23 152.2(2) . . ? C23 Ag1 Cl1 103.08(14) . . ? C15 Ag2 Cl1 109.25(15) . . ? C15 Ag2 C59 142.8(2) . . ? C59 Ag2 Cl1 107.95(14) . . ? C45 Ag3 C37 159.7(2) . . ? Ag2 Cl1 Ag1 117.65(5) . . ? F1 P1 F2 86.1(4) . . ? F1 P1 F4 178.4(4) . . ? F1 P1 F5 90.9(5) . . ? F2 P1 F4 93.2(4) . . ? F3 P1 F1 91.0(4) . . ? F3 P1 F2 88.1(4) . . ? F3 P1 F4 87.5(4) . . ? F3 P1 F5 176.4(6) . . ? F3 P1 F6 92.9(5) . . ? F5 P1 F2 88.9(5) . . ? F5 P1 F4 90.6(5) . . ? F6 P1 F1 93.8(4) . . ? F6 P1 F2 179.0(5) . . ? F6 P1 F4 86.9(4) . . ? F6 P1 F5 90.1(5) . . ? F7 P2 F11 178.9(4) . . ? F8 P2 F7 90.5(3) . . ? F8 P2 F10 90.7(3) . . ? F8 P2 F11 89.1(3) . . ? F8 P2 F12 179.3(3) . . ? F9 P2 F7 88.4(4) . . ? F9 P2 F8 87.0(4) . . ? F9 P2 F10 176.9(4) . . ? F9 P2 F11 92.6(4) . . ? F9 P2 F12 93.3(3) . . ? F10 P2 F7 89.5(3) . . ? F10 P2 F11 89.5(3) . . ? F10 P2 F12 89.1(3) . . ? F12 P2 F7 90.2(3) . . ? F12 P2 F11 90.2(3) . . ? C3 O1 C4 108.9(7) . . ? C17 O2 C18 111.4(6) . . ? C25 O3 C26 111.6(6) . . ? C39 O4 C40 110.9(5) . . ? C47 O5 C48 112.0(5) . . ? C62 O6 C61 110.4(4) . . ? C68 O8 C70 116.3(7) . . ? C1 N1 C2 108.5(5) . . ? C1 N1 C5 127.3(5) . . ? C2 N1 C5 123.8(5) . . ? C2 N2 N3 102.8(5) . . ? N2 N3 C9 118.3(5) . . ? C1 N3 N2 113.5(5) . . ? C1 N3 C9 128.1(5) . . ? N5 N4 C13 118.3(4) . . ? C15 N4 N5 113.5(4) . . ? C15 N4 C13 127.7(4) . . ? C16 N5 N4 103.4(4) . . ? C15 N6 C16 109.2(5) . . ? C15 N6 C19 128.3(4) . . ? C16 N6 C19 122.1(5) . . ? N8 N7 C31 117.8(5) . . ? C23 N7 N8 113.4(5) . . ? C23 N7 C31 128.7(5) . . ? C24 N8 N7 102.4(5) . . ? C23 N9 C24 109.4(5) . . ? C23 N9 C27 125.9(5) . . ? C24 N9 C27 124.5(5) . . ? N11 N10 C35 117.9(4) . . ? C37 N10 N11 113.6(4) . . ? C37 N10 C35 128.5(5) . . ? C38 N11 N10 102.6(4) . . ? C37 N12 C41 127.4(5) . . ? C38 N12 C37 108.9(5) . . ? C38 N12 C41 123.7(5) . . ? N14 N13 C53 117.6(4) . . ? C45 N13 N14 113.7(4) . . ? C45 N13 C53 128.6(4) . . ? C46 N14 N13 103.3(4) . . ? C45 N15 C46 109.1(4) . . ? C45 N15 C49 128.4(4) . . ? C46 N15 C49 122.5(4) . . ? N17 N16 C57 117.0(4) . . ? C59 N16 N17 113.8(4) . . ? C59 N16 C57 129.0(4) . . ? C60 N17 N16 103.2(4) . . ? C59 N18 C60 108.9(4) . . ? C59 N18 C63 128.2(4) . . ? C60 N18 C63 122.7(5) . . ? N1 C1 Ag1 122.4(4) . . ? N3 C1 Ag1 134.4(4) . . ? N3 C1 N1 103.2(5) . . ? N1 C2 C3 120.7(6) . . ? N2 C2 N1 112.0(6) . . ? N2 C2 C3 127.3(6) . . ? O1 C3 C2 109.1(6) . . ? O1 C3 H3a 109.9 . . ? O1 C3 H3b 109.9 . . ? C2 C3 H3a 109.9 . . ? C2 C3 H3b 109.9 . . ? H3a C3 H3b 108.3 . . ? O1 C4 H4a 109.6 . . ? O1 C4 H4b 109.6 . . ? O1 C4 C5 110.5(6) . . ? H4a C4 H4b 108.1 . . ? C5 C4 H4a 109.6 . . ? C5 C4 H4b 109.6 . . ? N1 C5 C4 106.7(5) . . ? N1 C5 H5 107.1 . . ? N1 C5 C6 111.8(5) . . ? C4 C5 H5 107.1 . . ? C4 C5 C6 116.6(6) . . ? C6 C5 H5 107.1 . . ? C5 C6 H6 106.5 . . ? C7 C6 C5 110.1(6) . . ? C7 C6 H6 106.5 . . ? C7 C6 C8 111.3(7) . . ? C8 C6 C5 115.5(7) . . ? C8 C6 H6 106.5 . . ? C6 C7 H7a 109.5 . . ? C6 C7 H7b 109.5 . . ? C6 C7 H7c 109.5 . . ? H7a C7 H7b 109.5 . . ? H7a C7 H7c 109.5 . . ? H7b C7 H7c 109.5 . . ? C6 C8 H8a 109.5 . . ? C6 C8 H8b 109.5 . . ? C6 C8 H8c 109.5 . . ? H8a C8 H8b 109.5 . . ? H8a C8 H8c 109.5 . . ? H8b C8 H8c 109.5 . . ? N3 C9 C10 118.4(5) . . ? C14 C9 N3 122.2(5) . . ? C14 C9 C10 119.4(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 C9 119.7(5) . . ? C11 C10 H10 120.2 . . ? C10 C11 H11 119.1 . . ? C10 C11 C12 121.7(6) . . ? C12 C11 H11 119.1 . . ? C11 C12 H12 121.1 . . ? C13 C12 C11 117.8(6) . . ? C13 C12 H12 121.1 . . ? C12 C13 N4 117.5(5) . . ? C14 C13 N4 120.0(5) . . ? C14 C13 C12 122.4(5) . . ? C9 C14 H14 120.5 . . ? C13 C14 C9 119.0(5) . . ? C13 C14 H14 120.5 . . ? N4 C15 Ag2 128.1(4) . . ? N4 C15 N6 102.4(4) . . ? N6 C15 Ag2 128.2(4) . . ? N5 C16 N6 111.5(5) . . ? N5 C16 C17 126.4(6) . . ? N6 C16 C17 121.9(6) . . ? O2 C17 C16 111.3(6) . . ? O2 C17 H17a 109.4 . . ? O2 C17 H17b 109.4 . . ? C16 C17 H17a 109.4 . . ? C16 C17 H17b 109.4 . . ? H17a C17 H17b 108.0 . . ? O2 C18 H18a 109.7 . . ? O2 C18 H18b 109.7 . . ? O2 C18 C19 109.9(7) . . ? H18a C18 H18b 108.2 . . ? C19 C18 H18a 109.7 . . ? C19 C18 H18b 109.7 . . ? N6 C19 C18 104.4(5) . . ? N6 C19 H19 109.2 . . ? N6 C19 C20 111.8(5) . . ? C18 C19 H19 109.2 . . ? C18 C19 C20 112.8(5) . . ? C20 C19 H19 109.2 . . ? C19 C20 H20 108.0 . . ? C19 C20 C22 110.0(6) . . ? C21 C20 C19 113.2(5) . . ? C21 C20 H20 108.0 . . ? C21 C20 C22 109.5(5) . . ? C22 C20 H20 108.0 . . ? C20 C21 H21a 109.5 . . ? C20 C21 H21b 109.5 . . ? C20 C21 H21c 109.5 . . ? H21a C21 H21b 109.5 . . ? H21a C21 H21c 109.5 . . ? H21b C21 H21c 109.5 . . ? C20 C22 H22a 109.5 . . ? C20 C22 H22b 109.5 . . ? C20 C22 H22c 109.5 . . ? H22a C22 H22b 109.5 . . ? H22a C22 H22c 109.5 . . ? H22b C22 H22c 109.5 . . ? N7 C23 Ag1 131.8(4) . . ? N7 C23 N9 102.9(5) . . ? N9 C23 Ag1 125.2(4) . . ? N8 C24 N9 112.0(5) . . ? N8 C24 C25 125.9(6) . . ? N9 C24 C25 122.1(6) . . ? O3 C25 C24 109.1(6) . . ? O3 C25 H25a 109.9 . . ? O3 C25 H25b 109.9 . . ? C24 C25 H25a 109.9 . . ? C24 C25 H25b 109.9 . . ? H25a C25 H25b 108.3 . . ? O3 C26 H26a 109.3 . . ? O3 C26 H26b 109.3 . . ? O3 C26 C27 111.7(5) . . ? H26a C26 H26b 107.9 . . ? C27 C26 H26a 109.3 . . ? C27 C26 H26b 109.3 . . ? N9 C27 C26 105.8(5) . . ? N9 C27 H27 107.1 . . ? N9 C27 C28 113.2(5) . . ? C26 C27 H27 107.1 . . ? C26 C27 C28 116.0(6) . . ? C28 C27 H27 107.1 . . ? C27 C28 H28 106.6 . . ? C29 C28 C27 115.1(7) . . ? C29 C28 H28 106.6 . . ? C29 C28 C30 112.2(7) . . ? C30 C28 C27 109.2(6) . . ? C30 C28 H28 106.6 . . ? C28 C29 H29a 109.5 . . ? C28 C29 H29b 109.5 . . ? C28 C29 H29c 109.5 . . ? H29a C29 H29b 109.5 . . ? H29a C29 H29c 109.5 . . ? H29b C29 H29c 109.5 . . ? C28 C30 H30a 109.5 . . ? C28 C30 H30b 109.5 . . ? C28 C30 H30c 109.5 . . ? H30a C30 H30b 109.5 . . ? H30a C30 H30c 109.5 . . ? H30b C30 H30c 109.5 . . ? C32 C31 N7 119.0(5) . . ? C32 C31 C36 120.0(5) . . ? C36 C31 N7 120.9(5) . . ? C31 C32 H32 119.6 . . ? C33 C32 C31 120.8(5) . . ? C33 C32 H32 119.6 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 120.0(5) . . ? C34 C33 H33 120.0 . . ? C33 C34 H34 120.5 . . ? C35 C34 C33 119.1(5) . . ? C35 C34 H34 120.5 . . ? C34 C35 N10 117.7(5) . . ? C34 C35 C36 121.3(5) . . ? C36 C35 N10 121.0(5) . . ? C31 C36 H36 120.7 . . ? C35 C36 C31 118.7(5) . . ? C35 C36 H36 120.7 . . ? N10 C37 Ag3 130.9(4) . . ? N10 C37 N12 102.7(4) . . ? N12 C37 Ag3 126.1(4) . . ? N11 C38 N12 112.1(5) . . ? N11 C38 C39 125.6(5) . . ? N12 C38 C39 122.2(5) . . ? O4 C39 C38 109.9(5) . . ? O4 C39 H39a 109.7 . . ? O4 C39 H39b 109.7 . . ? C38 C39 H39a 109.7 . . ? C38 C39 H39b 109.7 . . ? H39a C39 H39b 108.2 . . ? O4 C40 H40a 109.5 . . ? O4 C40 H40b 109.5 . . ? O4 C40 C41 110.6(5) . . ? H40a C40 H40b 108.1 . . ? C41 C40 H40a 109.5 . . ? C41 C40 H40b 109.5 . . ? N12 C41 C40 105.8(5) . . ? N12 C41 H41 107.7 . . ? N12 C41 C42 111.1(5) . . ? C40 C41 H41 107.7 . . ? C42 C41 C40 116.5(5) . . ? C42 C41 H41 107.7 . . ? C41 C42 H42 107.1 . . ? C43 C42 C41 109.4(6) . . ? C43 C42 H42 107.1 . . ? C43 C42 C44 111.7(7) . . ? C44 C42 C41 113.9(6) . . ? C44 C42 H42 107.1 . . ? C42 C43 H43a 109.5 . . ? C42 C43 H43b 109.5 . . ? C42 C43 H43c 109.5 . . ? H43a C43 H43b 109.5 . . ? H43a C43 H43c 109.5 . . ? H43b C43 H43c 109.5 . . ? C42 C44 H44a 109.5 . . ? C42 C44 H44b 109.5 . . ? C42 C44 H44c 109.5 . . ? H44a C44 H44b 109.5 . . ? H44a C44 H44c 109.5 . . ? H44b C44 H44c 109.5 . . ? N13 C45 Ag3 131.1(4) . . ? N13 C45 N15 101.9(4) . . ? N15 C45 Ag3 126.7(4) . . ? N14 C46 N15 111.9(5) . . ? N14 C46 C47 125.9(5) . . ? N15 C46 C47 121.9(5) . . ? O5 C47 C46 111.0(5) . . ? O5 C47 H47a 109.4 . . ? O5 C47 H47b 109.4 . . ? C46 C47 H47a 109.4 . . ? C46 C47 H47b 109.4 . . ? H47a C47 H47b 108.0 . . ? O5 C48 H48a 109.6 . . ? O5 C48 H48b 109.6 . . ? O5 C48 C49 110.1(5) . . ? H48a C48 H48b 108.2 . . ? C49 C48 H48a 109.6 . . ? C49 C48 H48b 109.6 . . ? N15 C49 C48 104.6(5) . . ? N15 C49 H49 109.3 . . ? N15 C49 C50 111.6(5) . . ? C48 C49 H49 109.3 . . ? C48 C49 C50 112.5(5) . . ? C50 C49 H49 109.3 . . ? C49 C50 H50 109.0 . . ? C51 C50 C49 109.2(7) . . ? C51 C50 H50 109.0 . . ? C52 C50 C49 112.7(6) . . ? C52 C50 H50 109.0 . . ? C52 C50 C51 108.0(6) . . ? C50 C51 H51a 109.5 . . ? C50 C51 H51b 109.5 . . ? C50 C51 H51c 109.5 . . ? H51a C51 H51b 109.5 . . ? H51a C51 H51c 109.5 . . ? H51b C51 H51c 109.5 . . ? C50 C52 H52a 109.5 . . ? C50 C52 H52b 109.5 . . ? C50 C52 H52c 109.5 . . ? H52a C52 H52b 109.5 . . ? H52a C52 H52c 109.5 . . ? H52b C52 H52c 109.5 . . ? C54 C53 N13 117.4(5) . . ? C58 C53 N13 121.2(5) . . ? C58 C53 C54 121.4(5) . . ? C53 C54 H54 120.6 . . ? C55 C54 C53 118.9(5) . . ? C55 C54 H54 120.6 . . ? C54 C55 H55 119.6 . . ? C56 C55 C54 120.8(5) . . ? C56 C55 H55 119.6 . . ? C55 C56 H56 120.3 . . ? C55 C56 C57 119.5(5) . . ? C57 C56 H56 120.3 . . ? C56 C57 N16 117.9(5) . . ? C56 C57 C58 121.4(5) . . ? C58 C57 N16 120.7(5) . . ? C53 C58 C57 118.0(5) . . ? C53 C58 H58 121.0 . . ? C57 C58 H58 121.0 . . ? N16 C59 Ag2 129.5(4) . . ? N16 C59 N18 102.7(4) . . ? N18 C59 Ag2 127.2(4) . . ? N17 C60 N18 111.3(5) . . ? N17 C60 C61 127.3(5) . . ? N18 C60 C61 121.4(5) . . ? O6 C61 C60 110.7(5) . . ? O6 C61 H61a 109.5 . . ? O6 C61 H61b 109.5 . . ? C60 C61 H61a 109.5 . . ? C60 C61 H61b 109.5 . . ? H61a C61 H61b 108.1 . . ? O6 C62 H62a 109.4 . . ? O6 C62 H62b 109.4 . . ? O6 C62 C63 111.1(5) . . ? H62a C62 H62b 108.0 . . ? C63 C62 H62a 109.4 . . ? C63 C62 H62b 109.4 . . ? N18 C63 C62 105.2(5) . . ? N18 C63 H63 109.9 . . ? N18 C63 C64 110.2(6) . . ? C62 C63 H63 109.9 . . ? C62 C63 C64 111.5(5) . . ? C64 C63 H63 109.9 . . ? C63 C64 H64 108.2 . . ? C65 C64 C63 116.5(6) . . ? C65 C64 H64 108.2 . . ? C65 C64 C66 109.9(6) . . ? C66 C64 C63 105.4(7) . . ? C66 C64 H64 108.2 . . ? C64 C65 H65a 109.5 . . ? C64 C65 H65b 109.5 . . ? C64 C65 H65c 109.5 . . ? H65a C65 H65b 109.5 . . ? H65a C65 H65c 109.5 . . ? H65b C65 H65c 109.5 . . ? C64 C66 H66a 109.5 . . ? C64 C66 H66b 109.5 . . ? C64 C66 H66c 109.5 . . ? H66a C66 H66b 109.5 . . ? H66a C66 H66c 109.5 . . ? H66b C66 H66c 109.5 . . ? Cl2 C67 Cl3 111.5(7) . . ? Cl2 C67 Cl4 110.7(5) . . ? Cl2 C67 H67 107.5 . . ? Cl3 C67 H67 107.5 . . ? Cl4 C67 Cl3 112.1(6) . . ? Cl4 C67 H67 107.5 . . ? O7 C68 O8 123.1(10) . . ? O7 C68 C69 124.6(10) . . ? O8 C68 C69 112.3(9) . . ? C68 C69 H69a 109.5 . . ? C68 C69 H69b 109.5 . . ? C68 C69 H69c 109.5 . . ? H69a C69 H69b 109.5 . . ? H69a C69 H69c 109.5 . . ? H69b C69 H69c 109.5 . . ? O8 C70 H70a 110.1 . . ? O8 C70 H70b 110.1 . . ? O8 C70 C71 108.0(8) . . ? H70a C70 H70b 108.4 . . ? C71 C70 H70a 110.1 . . ? C71 C70 H70b 110.1 . . ? C70 C71 H71a 109.5 . . ? C70 C71 H71b 109.5 . . ? C70 C71 H71c 109.5 . . ? H71a C71 H71b 109.5 . . ? H71a C71 H71c 109.5 . . ? H71b C71 H71c 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Ag1 C1 N1 -109.1(4) . . . . ? Cl1 Ag1 C1 N3 71.1(5) . . . . ? Cl1 Ag1 C23 N7 72.5(5) . . . . ? Cl1 Ag1 C23 N9 -113.1(4) . . . . ? Cl1 Ag2 C15 N4 84.1(5) . . . . ? Cl1 Ag2 C15 N6 -112.0(5) . . . . ? Cl1 Ag2 C59 N16 82.0(5) . . . . ? Cl1 Ag2 C59 N18 -109.1(4) . . . . ? O1 C4 C5 N1 -48.4(8) . . . . ? O1 C4 C5 C6 77.4(8) . . . . ? O2 C18 C19 N6 -60.2(7) . . . . ? O2 C18 C19 C20 61.4(7) . . . . ? O3 C26 C27 N9 -47.5(7) . . . . ? O3 C26 C27 C28 78.9(7) . . . . ? O4 C40 C41 N12 -51.6(7) . . . . ? O4 C40 C41 C42 72.4(7) . . . . ? O5 C48 C49 N15 -59.5(6) . . . . ? O5 C48 C49 C50 61.8(7) . . . . ? O6 C62 C63 N18 -54.0(6) . . . . ? O6 C62 C63 C64 65.5(7) . . . . ? N1 C2 C3 O1 15.0(11) . . . . ? N1 C5 C6 C7 -174.2(6) . . . . ? N1 C5 C6 C8 58.7(8) . . . . ? N2 N3 C1 Ag1 -179.5(4) . . . . ? N2 N3 C1 N1 0.7(6) . . . . ? N2 N3 C9 C10 -23.1(8) . . . . ? N2 N3 C9 C14 155.4(5) . . . . ? N2 C2 C3 O1 -163.7(8) . . . . ? N3 N2 C2 N1 0.7(8) . . . . ? N3 N2 C2 C3 179.5(8) . . . . ? N3 C9 C10 C11 178.8(6) . . . . ? N3 C9 C14 C13 -179.1(5) . . . . ? N4 N5 C16 N6 1.1(7) . . . . ? N4 N5 C16 C17 -173.5(7) . . . . ? N4 C13 C14 C9 179.0(5) . . . . ? N5 N4 C13 C12 -30.9(7) . . . . ? N5 N4 C13 C14 150.4(5) . . . . ? N5 N4 C15 Ag2 166.3(4) . . . . ? N5 N4 C15 N6 -0.9(6) . . . . ? N5 C16 C17 O2 -179.0(7) . . . . ? N6 C16 C17 O2 7.0(10) . . . . ? N6 C19 C20 C21 -54.8(7) . . . . ? N6 C19 C20 C22 -177.6(5) . . . . ? N7 N8 C24 N9 -0.3(7) . . . . ? N7 N8 C24 C25 -178.5(7) . . . . ? N7 C31 C32 C33 176.1(5) . . . . ? N7 C31 C36 C35 -177.4(5) . . . . ? N8 N7 C23 Ag1 176.1(4) . . . . ? N8 N7 C23 N9 0.8(6) . . . . ? N8 N7 C31 C32 -32.6(7) . . . . ? N8 N7 C31 C36 145.7(5) . . . . ? N8 C24 C25 O3 -168.0(6) . . . . ? N9 C24 C25 O3 13.9(10) . . . . ? N9 C27 C28 C29 64.7(7) . . . . ? N9 C27 C28 C30 -168.0(6) . . . . ? N10 N11 C38 N12 0.8(7) . . . . ? N10 N11 C38 C39 -178.7(6) . . . . ? N10 C35 C36 C31 -178.1(5) . . . . ? N11 N10 C35 C34 -37.3(7) . . . . ? N11 N10 C35 C36 142.0(5) . . . . ? N11 N10 C37 Ag3 175.1(4) . . . . ? N11 N10 C37 N12 0.4(6) . . . . ? N11 C38 C39 O4 -164.9(6) . . . . ? N12 C38 C39 O4 15.7(9) . . . . ? N12 C41 C42 C43 -173.7(6) . . . . ? N12 C41 C42 C44 60.4(7) . . . . ? N13 N14 C46 N15 -1.0(6) . . . . ? N13 N14 C46 C47 -174.4(6) . . . . ? N13 C53 C54 C55 179.4(5) . . . . ? N13 C53 C58 C57 -178.3(4) . . . . ? N14 N13 C45 Ag3 172.8(4) . . . . ? N14 N13 C45 N15 -1.7(6) . . . . ? N14 N13 C53 C54 -30.5(7) . . . . ? N14 N13 C53 C58 148.2(5) . . . . ? N14 C46 C47 O5 -176.9(5) . . . . ? N15 C46 C47 O5 10.3(8) . . . . ? N15 C49 C50 C51 -179.4(5) . . . . ? N15 C49 C50 C52 -59.5(8) . . . . ? N16 N17 C60 N18 1.0(6) . . . . ? N16 N17 C60 C61 -175.6(5) . . . . ? N16 C57 C58 C53 177.6(5) . . . . ? N17 N16 C57 C56 -23.8(7) . . . . ? N17 N16 C57 C58 157.6(5) . . . . ? N17 N16 C59 Ag2 169.6(4) . . . . ? N17 N16 C59 N18 -1.4(6) . . . . ? N17 C60 C61 O6 -168.8(5) . . . . ? N18 C60 C61 O6 14.8(7) . . . . ? N18 C63 C64 C65 -51.4(9) . . . . ? N18 C63 C64 C66 -173.6(5) . . . . ? C1 Ag1 Cl1 Ag2 -57.96(16) . . . . ? C1 Ag1 C23 N7 -102.7(6) . . . . ? C1 Ag1 C23 N9 71.8(7) . . . . ? C1 N1 C2 N2 -0.3(8) . . . . ? C1 N1 C2 C3 -179.2(7) . . . . ? C1 N1 C5 C4 -162.8(6) . . . . ? C1 N1 C5 C6 68.7(8) . . . . ? C1 N3 C9 C10 153.0(6) . . . . ? C1 N3 C9 C14 -28.5(9) . . . . ? C2 N1 C1 Ag1 179.9(4) . . . . ? C2 N1 C1 N3 -0.3(6) . . . . ? C2 N1 C5 C4 8.7(9) . . . . ? C2 N1 C5 C6 -119.9(7) . . . . ? C2 N2 N3 C1 -0.9(7) . . . . ? C2 N2 N3 C9 175.7(6) . . . . ? C3 O1 C4 C5 75.9(8) . . . . ? C4 O1 C3 C2 -54.4(9) . . . . ? C4 C5 C6 C7 62.7(8) . . . . ? C4 C5 C6 C8 -64.4(9) . . . . ? C5 N1 C1 Ag1 -7.6(8) . . . . ? C5 N1 C1 N3 172.3(5) . . . . ? C5 N1 C2 N2 -173.2(6) . . . . ? C5 N1 C2 C3 8.0(11) . . . . ? C9 N3 C1 Ag1 4.3(9) . . . . ? C9 N3 C1 N1 -175.5(5) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C10 C9 C14 C13 -0.6(8) . . . . ? C10 C11 C12 C13 -0.8(10) . . . . ? C11 C12 C13 N4 -178.3(5) . . . . ? C11 C12 C13 C14 0.3(9) . . . . ? C12 C13 C14 C9 0.3(8) . . . . ? C13 N4 N5 C16 172.6(5) . . . . ? C13 N4 C15 Ag2 -5.6(8) . . . . ? C13 N4 C15 N6 -172.7(5) . . . . ? C14 C9 C10 C11 0.2(9) . . . . ? C15 Ag2 Cl1 Ag1 -50.38(17) . . . . ? C15 Ag2 C59 N16 -99.8(5) . . . . ? C15 Ag2 C59 N18 69.2(6) . . . . ? C15 N4 N5 C16 -0.1(6) . . . . ? C15 N4 C13 C12 140.7(6) . . . . ? C15 N4 C13 C14 -38.0(8) . . . . ? C15 N6 C16 N5 -1.7(7) . . . . ? C15 N6 C16 C17 173.1(6) . . . . ? C15 N6 C19 C18 -146.6(6) . . . . ? C15 N6 C19 C20 91.2(7) . . . . ? C16 N6 C15 Ag2 -165.6(4) . . . . ? C16 N6 C15 N4 1.5(6) . . . . ? C16 N6 C19 C18 25.5(8) . . . . ? C16 N6 C19 C20 -96.8(6) . . . . ? C17 O2 C18 C19 73.0(8) . . . . ? C18 O2 C17 C16 -41.9(9) . . . . ? C18 C19 C20 C21 -172.1(6) . . . . ? C18 C19 C20 C22 65.1(7) . . . . ? C19 N6 C15 Ag2 7.2(8) . . . . ? C19 N6 C15 N4 174.4(5) . . . . ? C19 N6 C16 N5 -175.1(5) . . . . ? C19 N6 C16 C17 -0.3(9) . . . . ? C23 Ag1 Cl1 Ag2 124.37(17) . . . . ? C23 Ag1 C1 N1 66.0(7) . . . . ? C23 Ag1 C1 N3 -113.7(6) . . . . ? C23 N7 N8 C24 -0.3(6) . . . . ? C23 N7 C31 C32 143.0(6) . . . . ? C23 N7 C31 C36 -38.7(8) . . . . ? C23 N9 C24 N8 0.8(7) . . . . ? C23 N9 C24 C25 179.1(6) . . . . ? C23 N9 C27 C26 -162.0(6) . . . . ? C23 N9 C27 C28 70.0(8) . . . . ? C24 N9 C23 Ag1 -176.7(4) . . . . ? C24 N9 C23 N7 -0.9(6) . . . . ? C24 N9 C27 C26 11.6(8) . . . . ? C24 N9 C27 C28 -116.5(7) . . . . ? C25 O3 C26 C27 72.0(8) . . . . ? C26 O3 C25 C24 -50.6(8) . . . . ? C26 C27 C28 C29 -57.9(8) . . . . ? C26 C27 C28 C30 69.4(7) . . . . ? C27 N9 C23 Ag1 -2.3(8) . . . . ? C27 N9 C23 N7 173.4(5) . . . . ? C27 N9 C24 N8 -173.6(5) . . . . ? C27 N9 C24 C25 4.7(10) . . . . ? C31 N7 N8 C24 175.9(5) . . . . ? C31 N7 C23 Ag1 0.4(8) . . . . ? C31 N7 C23 N9 -175.0(5) . . . . ? C31 C32 C33 C34 1.4(9) . . . . ? C32 C31 C36 C35 0.8(8) . . . . ? C32 C33 C34 C35 0.7(9) . . . . ? C33 C34 C35 N10 177.3(5) . . . . ? C33 C34 C35 C36 -2.1(8) . . . . ? C34 C35 C36 C31 1.3(8) . . . . ? C35 N10 N11 C38 177.8(5) . . . . ? C35 N10 C37 Ag3 -3.2(9) . . . . ? C35 N10 C37 N12 -178.0(5) . . . . ? C36 C31 C32 C33 -2.2(9) . . . . ? C37 Ag3 C45 N13 -101.1(7) . . . . ? C37 Ag3 C45 N15 72.2(8) . . . . ? C37 N10 N11 C38 -0.8(6) . . . . ? C37 N10 C35 C34 141.0(6) . . . . ? C37 N10 C35 C36 -39.6(8) . . . . ? C37 N12 C38 N11 -0.6(7) . . . . ? C37 N12 C38 C39 178.9(6) . . . . ? C37 N12 C41 C40 -162.0(5) . . . . ? C37 N12 C41 C42 70.8(7) . . . . ? C38 N12 C37 Ag3 -175.0(4) . . . . ? C38 N12 C37 N10 0.1(6) . . . . ? C38 N12 C41 C40 17.8(8) . . . . ? C38 N12 C41 C42 -109.5(6) . . . . ? C39 O4 C40 C41 72.4(7) . . . . ? C40 O4 C39 C38 -50.3(7) . . . . ? C40 C41 C42 C43 65.1(8) . . . . ? C40 C41 C42 C44 -60.7(7) . . . . ? C41 N12 C37 Ag3 4.8(8) . . . . ? C41 N12 C37 N10 179.8(5) . . . . ? C41 N12 C38 N11 179.7(5) . . . . ? C41 N12 C38 C39 -0.8(9) . . . . ? C45 Ag3 C37 N10 -102.9(7) . . . . ? C45 Ag3 C37 N12 70.7(8) . . . . ? C45 N13 N14 C46 1.7(6) . . . . ? C45 N13 C53 C54 144.4(5) . . . . ? C45 N13 C53 C58 -36.9(8) . . . . ? C45 N15 C46 N14 0.1(6) . . . . ? C45 N15 C46 C47 173.7(5) . . . . ? C45 N15 C49 C48 -150.3(5) . . . . ? C45 N15 C49 C50 87.8(7) . . . . ? C46 N15 C45 Ag3 -173.9(4) . . . . ? C46 N15 C45 N13 1.0(6) . . . . ? C46 N15 C49 C48 28.0(7) . . . . ? C46 N15 C49 C50 -93.9(6) . . . . ? C47 O5 C48 C49 71.6(7) . . . . ? C48 O5 C47 C46 -42.4(7) . . . . ? C48 C49 C50 C51 63.4(7) . . . . ? C48 C49 C50 C52 -176.7(6) . . . . ? C49 N15 C45 Ag3 4.6(8) . . . . ? C49 N15 C45 N13 179.4(5) . . . . ? C49 N15 C46 N14 -178.5(5) . . . . ? C49 N15 C46 C47 -4.9(8) . . . . ? C53 N13 N14 C46 177.4(4) . . . . ? C53 N13 C45 Ag3 -2.2(8) . . . . ? C53 N13 C45 N15 -176.7(5) . . . . ? C53 C54 C55 C56 -1.0(9) . . . . ? C54 C53 C58 C57 0.3(8) . . . . ? C54 C55 C56 C57 0.2(9) . . . . ? C55 C56 C57 N16 -177.8(5) . . . . ? C55 C56 C57 C58 0.8(9) . . . . ? C56 C57 C58 C53 -1.0(8) . . . . ? C57 N16 N17 C60 175.3(4) . . . . ? C57 N16 C59 Ag2 -4.7(8) . . . . ? C57 N16 C59 N18 -175.7(5) . . . . ? C58 C53 C54 C55 0.7(8) . . . . ? C59 Ag2 Cl1 Ag1 128.49(16) . . . . ? C59 Ag2 C15 N4 -94.2(6) . . . . ? C59 Ag2 C15 N6 69.8(6) . . . . ? C59 N16 N17 C60 0.3(6) . . . . ? C59 N16 C57 C56 150.3(6) . . . . ? C59 N16 C57 C58 -28.3(8) . . . . ? C59 N18 C60 N17 -2.0(6) . . . . ? C59 N18 C60 C61 174.9(5) . . . . ? C59 N18 C63 C62 -155.9(5) . . . . ? C59 N18 C63 C64 83.8(7) . . . . ? C60 N18 C59 Ag2 -169.3(4) . . . . ? C60 N18 C59 N16 2.0(6) . . . . ? C60 N18 C63 C62 18.8(7) . . . . ? C60 N18 C63 C64 -101.5(6) . . . . ? C61 O6 C62 C63 74.1(6) . . . . ? C62 O6 C61 C60 -50.0(6) . . . . ? C62 C63 C64 C65 -167.9(6) . . . . ? C62 C63 C64 C66 69.9(7) . . . . ? C63 N18 C59 Ag2 6.0(8) . . . . ? C63 N18 C59 N16 177.3(5) . . . . ? C63 N18 C60 N17 -177.6(5) . . . . ? C63 N18 C60 C61 -0.7(8) . . . . ? C68 O8 C70 C71 177.3(7) . . . . ? C70 O8 C68 O7 1.4(11) . . . . ? C70 O8 C68 C69 -179.7(7) . . . . ?