Supplementary Material (ESI) for Organic and Biomolecular Chemistry This journal is © The Royal Society of Chemistry 2004 data_global _audit_creation_date 2004-01-26 _journal_coden_Cambridge 177 loop_ _publ_author_name 'Jay S. Siegel' 'Eric L. Elliot' 'Gerardo A. Hernandez' 'Anthony Linden' _publ_contact_author_name 'Prof Jay S. Siegel' _publ_contact_author_address ; Organic Chemistry Institute University of Zurich Winterthuererstr 190 Zurich CH-8057 SWITZERLAND ; _publ_contact_author_email JSS@OCI.UNIZH.CH _publ_requested_journal 'Organic & Biomolecular Chemistry' _publ_section_title ; Anion Mediated Structural Motifs in Silver (I) Complexes with Corannulene ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Blessing, R. H. (1995). Acta Cryst. A51, 33--38. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius (2000). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Spek, A. L. (2003). PLATON. University of Utrecht, The Netherlands. ; #========================================================================== data_2_(116B) _database_code_depnum_ccdc_archive 'CCDC 246840' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H10 Ag Cl O4' _chemical_formula_weight 457.60 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b a m' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 55 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 20.362(2) _cell_length_b 7.2285(13) _cell_length_c 10.2891(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1514.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 175(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method ? _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.533 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 175(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4 diffractometer' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2733 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.98 _reflns_number_total 2102 _reflns_number_observed 1542 _reflns_observed_criterion 'I > 2\s(I)' _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+5.8391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2100 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.5000 -0.27886(5) 0.0382(2) Uani 1 2 d S . . C1 C 0.4212(4) 0.2631(10) -0.2353(7) 0.066(2) Uani 1 1 d . . . H1 H 0.4358 0.2159 -0.3164 0.079 Uiso 1 1 calc R . . C2 C 0.4616(3) 0.2488(8) -0.1284(7) 0.0525(17) Uani 1 1 d . . . H2 H 0.5042 0.1975 -0.1392 0.063 Uiso 1 1 calc R . . C3 C 0.4416(3) 0.3092(10) 0.0000 0.0362(16) Uani 1 2 d S . . C4 C 0.3842(3) 0.4105(9) 0.0000 0.0239(12) Uani 1 2 d S . . C5 C 0.3441(3) 0.4304(7) -0.1106(4) 0.0314(10) Uani 1 1 d . . . C6 C 0.3572(4) 0.3480(9) -0.2271(5) 0.0530(18) Uani 1 1 d . . . C7 C 0.2981(6) 0.3292(12) -0.3085(7) 0.095(4) Uani 1 1 d . . . H7 H 0.3042 0.2921 -0.3963 0.113 Uiso 1 1 calc R . . C8 C 0.2374(6) 0.3601(13) -0.2689(11) 0.108(5) Uani 1 1 d . . . H8 H 0.2018 0.3421 -0.3271 0.130 Uiso 1 1 calc R . . C9 C 0.2254(4) 0.4188(9) -0.1428(12) 0.086(4) Uani 1 1 d . . . C10 C 0.1660(3) 0.4033(9) -0.0622(15) 0.133(9) Uani 1 1 d . . . H10 H 0.1249 0.3926 -0.1053 0.160 Uiso 1 1 calc R . . C11 C 0.2799(3) 0.4672(7) -0.0672(7) 0.0438(14) Uani 1 1 d . . . Cl1 Cl 0.57870(11) 0.2343(5) -0.5000 0.0584(7) Uani 1 2 d S . . O1 O 0.5655(4) 0.1882(14) -0.6190(7) 0.132(3) Uani 1 1 d . . . O2 O 0.6362(5) 0.3515(14) -0.5000 0.088(3) Uani 1 2 d S . . O3 O 0.6186(9) 0.0359(19) -0.5000 0.066(4) Uani 0.50 2 d SP . . O3' O 0.5237(7) 0.401(2) -0.5000 0.061(4) Uani 0.50 2 d SP . . 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 0.0411(3) 0.0400(3) 0.0336(3) 0.000 0.000 -0.0156(2) C1 0.098(6) 0.043(4) 0.055(4) -0.026(3) 0.049(4) -0.040(4) C2 0.040(3) 0.030(3) 0.088(5) -0.009(3) 0.032(3) -0.006(2) C3 0.024(3) 0.020(3) 0.065(5) 0.000 0.000 -0.001(2) C4 0.026(3) 0.020(3) 0.026(3) 0.000 0.000 -0.004(2) C5 0.047(3) 0.022(2) 0.025(2) 0.0067(18) -0.0087(19) -0.0131(19) C6 0.095(5) 0.041(3) 0.023(3) 0.005(2) -0.007(3) -0.039(3) C7 0.180(10) 0.066(5) 0.038(4) 0.027(3) -0.059(5) -0.076(6) C8 0.133(9) 0.068(6) 0.124(9) 0.050(6) -0.101(8) -0.057(6) C9 0.055(4) 0.024(3) 0.179(10) 0.034(5) -0.062(5) -0.011(3) C10 0.032(3) 0.027(3) 0.34(3) 0.023(6) -0.049(7) 0.003(2) C11 0.037(3) 0.016(2) 0.079(4) 0.011(2) -0.017(3) -0.0011(17) Cl1 0.0474(11) 0.101(2) 0.0270(8) 0.000 0.000 -0.0107(12) O1 0.121(6) 0.193(9) 0.082(5) -0.063(6) -0.030(4) 0.042(6) O2 0.089(6) 0.086(7) 0.091(6) 0.000 0.000 -0.024(5) O3 0.107(12) 0.047(8) 0.045(7) 0.000 0.000 0.027(8) O3' 0.060(7) 0.096(12) 0.027(5) 0.000 0.000 0.042(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 C1 2.389(6) 2_665 ? Ag1 C1 2.389(6) . ? Ag1 O3' 2.433(5) . ? Ag1 O3' 2.433(5) 5_664 ? Ag1 C2 2.510(6) 2_665 ? Ag1 C2 2.511(6) . ? C1 C2 1.378(11) . ? C1 C6 1.442(11) . ? C1 H1 0.9500 . ? C2 C3 1.450(7) . ? C2 H2 0.9500 . ? C3 C4 1.379(9) . ? C3 C2 1.450(7) 6 ? C4 C5 1.408(6) . ? C4 C5 1.408(6) 6 ? C5 C6 1.365(8) . ? C5 C11 1.407(8) . ? C6 C7 1.472(11) . ? C7 C8 1.321(16) . ? C7 H7 0.9500 . ? C8 C9 1.386(17) . ? C8 H8 0.9500 . ? C9 C11 1.401(9) . ? C9 C10 1.471(15) . ? C10 C10 1.28(3) 6 ? C10 H10 0.9500 . ? C11 C11 1.383(14) 6 ? Cl1 O1 1.297(6) 6_554 ? Cl1 O1 1.297(6) . ? Cl1 O2 1.445(9) . ? Cl1 O3' 1.646(13) . ? Cl1 O3 1.649(14) . ? O3' O3' 1.72(3) 5_664 ? O3' Ag1 2.433(5) 5_664 ? 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 C1 158.4(3) 2_665 . ? C1 Ag1 O3' 104.6(5) 2_665 . ? C1 Ag1 O3' 95.7(5) . . ? C1 Ag1 O3' 95.7(5) 2_665 5_664 ? C1 Ag1 O3' 104.6(5) . 5_664 ? O3' Ag1 O3' 41.5(6) . 5_664 ? C1 Ag1 C2 32.5(2) 2_665 2_665 ? C1 Ag1 C2 127.7(2) . 2_665 ? O3' Ag1 C2 136.6(5) . 2_665 ? O3' Ag1 C2 115.2(4) 5_664 2_665 ? C1 Ag1 C2 127.7(2) 2_665 . ? C1 Ag1 C2 32.5(2) . . ? O3' Ag1 C2 115.2(4) . . ? O3' Ag1 C2 136.6(5) 5_664 . ? C2 Ag1 C2 103.9(3) 2_665 . ? C2 C1 C6 121.7(5) . . ? C2 C1 Ag1 78.6(4) . . ? C6 C1 Ag1 108.2(4) . . ? C2 C1 H1 119.2 . . ? C6 C1 H1 119.2 . . ? Ag1 C1 H1 83.2 . . ? C1 C2 C3 122.4(5) . . ? C1 C2 Ag1 68.9(4) . . ? C3 C2 Ag1 115.6(4) . . ? C1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? Ag1 C2 H2 85.8 . . ? C4 C3 C2 113.5(4) . 6 ? C4 C3 C2 113.5(4) . . ? C2 C3 C2 131.3(7) 6 . ? C3 C4 C5 123.1(3) . . ? C3 C4 C5 123.1(3) . 6 ? C5 C4 C5 107.9(6) . 6 ? C6 C5 C11 122.9(5) . . ? C6 C5 C4 123.5(6) . . ? C11 C5 C4 107.5(5) . . ? C5 C6 C1 114.4(6) . . ? C5 C6 C7 112.4(8) . . ? C1 C6 C7 131.7(7) . . ? C8 C7 C6 125.0(8) . . ? C8 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? C7 C8 C9 120.4(7) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C11 117.1(9) . . ? C8 C9 C10 130.5(8) . . ? C11 C9 C10 111.0(10) . . ? C10 C10 C9 124.3(6) 6 . ? C10 C10 H10 117.8 6 . ? C9 C10 H10 117.8 . . ? C11 C11 C9 123.7(6) 6 . ? C11 C11 C5 108.5(3) 6 . ? C9 C11 C5 120.9(7) . . ? O1 Cl1 O1 141.5(10) 6_554 . ? O1 Cl1 O2 108.5(5) 6_554 . ? O1 Cl1 O2 108.5(5) . . ? O1 Cl1 O3' 92.7(4) 6_554 . ? O1 Cl1 O3' 92.7(4) . . ? O2 Cl1 O3' 97.0(8) . . ? O1 Cl1 O3 83.0(5) 6_554 . ? O1 Cl1 O3 83.0(5) . . ? O2 Cl1 O3 96.3(8) . . ? O3' Cl1 O3 166.7(9) . . ? Cl1 O3' O3' 171.3(18) . 5_664 ? Cl1 O3' Ag1 110.5(3) . . ? O3' O3' Ag1 69.3(3) 5_664 . ? Cl1 O3' Ag1 110.5(3) . 5_664 ? O3' O3' Ag1 69.3(3) 5_664 5_664 ? Ag1 O3' Ag1 138.5(6) . 5_664 ? 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 C1 Ag1 C1 C2 -29.8(3) 2_665 . . . ? O3' Ag1 C1 C2 129.9(4) . . . . ? O3' Ag1 C1 C2 171.1(4) 5_664 . . . ? C2 Ag1 C1 C2 -49.6(6) 2_665 . . . ? C1 Ag1 C1 C6 90.0(4) 2_665 . . . ? O3' Ag1 C1 C6 -110.3(5) . . . . ? O3' Ag1 C1 C6 -69.1(5) 5_664 . . . ? C2 Ag1 C1 C6 70.3(6) 2_665 . . . ? C2 Ag1 C1 C6 119.8(5) . . . . ? C6 C1 C2 C3 3.1(10) . . . . ? Ag1 C1 C2 C3 107.6(6) . . . . ? C6 C1 C2 Ag1 -104.5(6) . . . . ? C1 Ag1 C2 C1 166.6(2) 2_665 . . . ? O3' Ag1 C2 C1 -57.6(5) . . . . ? O3' Ag1 C2 C1 -12.6(6) 5_664 . . . ? C2 Ag1 C2 C1 141.6(4) 2_665 . . . ? C1 Ag1 C2 C3 49.7(6) 2_665 . . . ? C1 Ag1 C2 C3 -116.9(6) . . . . ? O3' Ag1 C2 C3 -174.5(5) . . . . ? O3' Ag1 C2 C3 -129.5(6) 5_664 . . . ? C2 Ag1 C2 C3 24.8(4) 2_665 . . . ? C1 C2 C3 C4 -10.9(9) . . . . ? Ag1 C2 C3 C4 69.3(7) . . . . ? C1 C2 C3 C2 152.9(6) . . . 6 ? Ag1 C2 C3 C2 -126.9(7) . . . 6 ? C2 C3 C4 C5 -158.1(5) 6 . . . ? C2 C3 C4 C5 8.7(9) . . . . ? C2 C3 C4 C5 -8.7(9) 6 . . 6 ? C2 C3 C4 C5 158.1(5) . . . 6 ? C3 C4 C5 C6 1.8(9) . . . . ? C5 C4 C5 C6 -151.6(4) 6 . . . ? C3 C4 C5 C11 154.9(6) . . . . ? C5 C4 C5 C11 1.4(7) 6 . . . ? C11 C5 C6 C1 -159.0(5) . . . . ? C4 C5 C6 C1 -9.9(8) . . . . ? C11 C5 C6 C7 8.8(7) . . . . ? C4 C5 C6 C7 157.8(5) . . . . ? C2 C1 C6 C5 7.4(8) . . . . ? Ag1 C1 C6 C5 -80.3(5) . . . . ? C2 C1 C6 C7 -157.4(6) . . . . ? Ag1 C1 C6 C7 115.0(6) . . . . ? C5 C6 C7 C8 -10.1(10) . . . . ? C1 C6 C7 C8 154.9(9) . . . . ? C6 C7 C8 C9 1.5(13) . . . . ? C7 C8 C9 C11 8.5(11) . . . . ? C7 C8 C9 C10 -156.7(8) . . . . ? C8 C9 C10 C10 155.0(7) . . . 6 ? C11 C9 C10 C10 -10.9(6) . . . 6 ? C8 C9 C11 C11 -157.2(5) . . . 6 ? C10 C9 C11 C11 10.8(6) . . . 6 ? C8 C9 C11 C5 -9.6(9) . . . . ? C10 C9 C11 C5 158.4(5) . . . . ? C6 C5 C11 C11 152.4(4) . . . 6 ? C4 C5 C11 C11 -0.9(5) . . . 6 ? C6 C5 C11 C9 0.4(8) . . . . ? C4 C5 C11 C9 -152.9(6) . . . . ? O1 Cl1 O3' Ag1 22.4(9) 6_554 . . . ? O1 Cl1 O3' Ag1 164.2(8) . . . . ? O2 Cl1 O3' Ag1 -86.7(7) . . . . ? O3 Cl1 O3' Ag1 93.3(7) . . . . ? O1 Cl1 O3' Ag1 -164.2(8) 6_554 . . 5_664 ? O1 Cl1 O3' Ag1 -22.3(9) . . . 5_664 ? O2 Cl1 O3' Ag1 86.7(7) . . . 5_664 ? O3 Cl1 O3' Ag1 -93.3(7) . . . 5_664 ? C1 Ag1 O3' Cl1 88.8(9) 2_665 . . . ? C1 Ag1 O3' Cl1 -83.6(9) . . . . ? O3' Ag1 O3' Cl1 170.7(19) 5_664 . . . ? C2 Ag1 O3' Cl1 95.7(9) 2_665 . . . ? C2 Ag1 O3' Cl1 -56.5(10) . . . . ? C1 Ag1 O3' O3' -81.9(11) 2_665 . . 5_664 ? C1 Ag1 O3' O3' 105.7(11) . . . 5_664 ? C2 Ag1 O3' O3' -75.0(12) 2_665 . . 5_664 ? C2 Ag1 O3' O3' 132.8(10) . . . 5_664 ? C1 Ag1 O3' Ag1 -81.9(11) 2_665 . . 5_664 ? C1 Ag1 O3' Ag1 105.7(11) . . . 5_664 ? O3' Ag1 O3' Ag1 -0.002(2) 5_664 . . 5_664 ? C2 Ag1 O3' Ag1 -75.0(12) 2_665 . . 5_664 ? C2 Ag1 O3' Ag1 132.8(10) . . . 5_664 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.055 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.150 #========================================================================== data_3_(117C) _database_code_depnum_ccdc_archive 'CCDC 246841' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H20 Ag2 F6 O6 S2' _chemical_formula_weight 1014.44 _chemical_melting_point ? _chemical_compound_source ? 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6903(15) _cell_length_b 22.206(2) _cell_length_c 12.8975(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.637(8) _cell_angle_gamma 90.00 _cell_volume 3463.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 12.55 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .73 _exptl_crystal_size_mid .68 _exptl_crystal_size_min .45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method ? _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4 diffractometer' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 95.43 _diffrn_reflns_number 6368 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6080 _reflns_number_gt 5221 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 52 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+25.4628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6080 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.78419(4) 0.08280(2) 0.50105(4) 0.03356(17) Uani 1 1 d . . . Ag2 Ag -0.48022(4) 0.09272(2) 0.27687(4) 0.03354(17) Uani 1 1 d . . . S1 S -0.71811(13) 0.02515(7) 0.29139(14) 0.0310(4) Uani 1 1 d . . . S2 S -0.24689(13) 0.02305(8) 0.29607(14) 0.0313(4) Uani 1 1 d . . . O1 O -0.7420(5) 0.0080(3) 0.3894(4) 0.0497(14) Uani 1 1 d . . . O2 O -0.7578(4) 0.0835(2) 0.2500(5) 0.0436(12) Uani 1 1 d . . . O3 O -0.6073(4) 0.0116(2) 0.2906(5) 0.0413(12) Uani 1 1 d . . . O4 O -0.3617(4) 0.0079(2) 0.2742(4) 0.0416(12) Uani 1 1 d . . . O5 O -0.2251(5) 0.0845(2) 0.2777(6) 0.0566(16) Uani 1 1 d . . . O6 O -0.1766(5) -0.0018(3) 0.3954(5) 0.0568(16) Uani 1 1 d . . . F1 F -0.9080(4) -0.0196(3) 0.1806(5) 0.0678(15) Uani 1 1 d . . . F2 F -0.7871(4) -0.0190(3) 0.0958(4) 0.0628(14) Uani 1 1 d . . . F3 F -0.7752(4) -0.0840(2) 0.2212(4) 0.0544(12) Uani 1 1 d . . . F4 F -0.1044(6) -0.0100(4) 0.2009(8) 0.127(3) Uani 1 1 d . . . F5 F -0.2693(8) -0.0002(5) 0.0938(6) 0.130(4) Uani 1 1 d . . . F6 F -0.2235(8) -0.0782(3) 0.2040(8) 0.124(4) Uani 1 1 d . . . C1 C -0.9349(5) 0.1404(3) 0.3804(5) 0.0313(14) Uani 1 1 d . . . H1A H -0.9288 0.1120 0.3275 0.038 Uiso 1 1 calc R . . C2 C -0.9796(5) 0.1221(3) 0.4624(6) 0.0346(15) Uani 1 1 d . . . H2B H -1.0028 0.0815 0.4637 0.042 Uiso 1 1 calc R . . C3 C -0.9914(5) 0.1635(3) 0.5453(5) 0.0302(14) Uani 1 1 d . . . C4 C -1.0660(6) 0.1604(3) 0.6116(6) 0.0364(15) Uani 1 1 d . . . H4A H -1.0953 0.1226 0.6234 0.044 Uiso 1 1 calc R . . C5 C -1.0949(6) 0.2115(3) 0.6577(6) 0.0370(16) Uani 1 1 d . . . H5B H -1.1428 0.2077 0.7014 0.044 Uiso 1 1 calc R . . C6 C -1.0547(5) 0.2703(3) 0.6416(5) 0.0314(14) Uani 1 1 d . . . C7 C -1.1019(6) 0.3297(3) 0.6479(6) 0.0361(16) Uani 1 1 d . . . H7A H -1.1512 0.3349 0.6898 0.043 Uiso 1 1 calc R . . C8 C -1.0759(6) 0.3790(3) 0.5935(5) 0.0345(15) Uani 1 1 d . . . H8A H -1.1092 0.4167 0.5990 0.041 Uiso 1 1 calc R . . C9 C -1.0004(5) 0.3756(3) 0.5289(5) 0.0299(14) Uani 1 1 d . . . C10 C -0.9882(6) 0.4133(3) 0.4435(6) 0.0361(16) Uani 1 1 d . . . H10A H -1.0137 0.4538 0.4394 0.043 Uiso 1 1 calc R . . C11 C -0.9408(5) 0.3933(3) 0.3673(5) 0.0333(15) Uani 1 1 d . . . H11A H -0.9346 0.4202 0.3122 0.040 Uiso 1 1 calc R . . C12 C -0.9000(5) 0.3323(3) 0.3681(5) 0.0299(14) Uani 1 1 d . . . C13 C -0.8834(6) 0.2969(3) 0.2806(5) 0.0357(15) Uani 1 1 d . . . H13A H -0.8740 0.3169 0.2190 0.043 Uiso 1 1 calc R . . C14 C -0.8806(5) 0.2346(3) 0.2837(6) 0.0362(16) Uani 1 1 d . . . H14A H -0.8674 0.2129 0.2254 0.043 Uiso 1 1 calc R . . C15 C -0.8977(5) 0.2020(3) 0.3743(5) 0.0300(14) Uani 1 1 d . . . C16 C -0.8986(5) 0.2369(3) 0.4618(5) 0.0290(14) Uani 1 1 d . . . C17 C -0.9436(5) 0.2182(3) 0.5435(5) 0.0280(13) Uani 1 1 d . . . C18 C -0.9737(5) 0.2704(3) 0.5911(5) 0.0269(13) Uani 1 1 d . . . C19 C -0.9457(5) 0.3210(3) 0.5382(5) 0.0267(13) Uani 1 1 d . . . C20 C -0.8985(5) 0.3005(3) 0.4589(5) 0.0278(13) Uani 1 1 d . . . C21 C -0.5727(6) 0.1009(4) 0.5818(6) 0.0420(18) Uani 1 1 d . . . H21A H -0.5629 0.0592 0.5982 0.050 Uiso 1 1 calc R . . C22 C -0.6333(6) 0.1343(5) 0.6311(6) 0.052(2) Uani 1 1 d . . . H22A H -0.6635 0.1154 0.6819 0.063 Uiso 1 1 calc R . . C23 C -0.6529(6) 0.1967(5) 0.6090(6) 0.055(3) Uani 1 1 d . . . C24 C -0.6798(8) 0.2409(7) 0.6776(9) 0.083(4) Uani 1 1 d . . . H24A H -0.7101 0.2284 0.7330 0.100 Uiso 1 1 calc R . . C25 C -0.6632(10) 0.2987(8) 0.6652(10) 0.104(6) Uani 1 1 d . . . H25A H -0.6849 0.3262 0.7113 0.125 Uiso 1 1 calc R . . C26 C -0.6140(11) 0.3234(4) 0.5860(11) 0.095(5) Uani 1 1 d . . . C27 C -0.5522(19) 0.3747(6) 0.5796(15) 0.154(12) Uani 1 1 d . . . H27A H -0.5650 0.4084 0.6194 0.185 Uiso 1 1 calc R . . C28 C -0.4796(18) 0.3836(6) 0.5276(13) 0.141(11) Uani 1 1 d . . . H28A H -0.4456 0.4218 0.5287 0.169 Uiso 1 1 calc R . . C29 C -0.4517(14) 0.3314(5) 0.4660(9) 0.103(6) Uani 1 1 d . . . C30 C -0.3561(16) 0.3195(8) 0.4370(10) 0.127(9) Uani 1 1 d . . . H30A H -0.3104 0.3525 0.4316 0.153 Uiso 1 1 calc R . . C31 C -0.3239(10) 0.2614(8) 0.4153(7) 0.101(6) Uani 1 1 d . . . H31A H -0.2571 0.2558 0.3978 0.121 Uiso 1 1 calc R . . C32 C -0.3935(7) 0.2097(5) 0.4199(6) 0.056(2) Uani 1 1 d . . . C33 C -0.3645(6) 0.1468(5) 0.4382(6) 0.060(3) Uani 1 1 d . . . H33A H -0.3006 0.1326 0.4222 0.072 Uiso 1 1 calc R . . C34 C -0.4258(6) 0.1063(4) 0.4783(6) 0.0424(18) Uani 1 1 d . . . H34A H -0.4042 0.0652 0.4879 0.051 Uiso 1 1 calc R . . C35 C -0.5230(5) 0.1266(3) 0.5056(5) 0.0280(13) Uani 1 1 d . . . C36 C -0.5559(5) 0.1845(3) 0.4743(5) 0.0251(13) Uani 1 1 d . . . C37 C -0.6206(6) 0.2182(3) 0.5236(6) 0.0388(17) Uani 1 1 d . . . C38 C -0.6000(8) 0.2793(4) 0.5108(7) 0.061(3) Uani 1 1 d . . . C39 C -0.5231(9) 0.2837(3) 0.4530(7) 0.065(3) Uani 1 1 d . . . C40 C -0.4925(6) 0.2244(4) 0.4314(5) 0.0413(18) Uani 1 1 d . . . C41 C -0.8025(6) -0.0283(3) 0.1907(6) 0.0381(16) Uani 1 1 d . . . C42 C -0.2089(9) -0.0194(6) 0.1918(10) 0.077(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0327(3) 0.0323(3) 0.0331(3) 0.0003(2) 0.0062(2) 0.0024(2) Ag2 0.0317(3) 0.0374(3) 0.0288(3) -0.0023(2) 0.0051(2) 0.0039(2) S1 0.0286(8) 0.0297(8) 0.0348(9) -0.0025(7) 0.0095(7) 0.0017(6) S2 0.0274(8) 0.0310(8) 0.0383(9) 0.0029(7) 0.0143(7) -0.0027(6) O1 0.061(4) 0.049(3) 0.043(3) 0.003(2) 0.021(3) 0.010(3) O2 0.038(3) 0.035(3) 0.061(3) 0.008(2) 0.021(3) 0.007(2) O3 0.028(2) 0.030(3) 0.062(3) -0.013(2) 0.008(2) 0.002(2) O4 0.028(2) 0.039(3) 0.061(3) 0.005(2) 0.018(2) 0.001(2) O5 0.052(3) 0.036(3) 0.085(5) 0.017(3) 0.026(3) -0.014(3) O6 0.047(3) 0.064(4) 0.048(3) 0.026(3) -0.003(3) -0.015(3) F1 0.025(2) 0.079(4) 0.096(4) -0.022(3) 0.014(2) -0.009(2) F2 0.064(3) 0.084(4) 0.037(3) -0.014(2) 0.011(2) -0.011(3) F3 0.052(3) 0.036(2) 0.078(4) -0.012(2) 0.025(3) -0.006(2) F4 0.086(5) 0.143(7) 0.199(9) -0.024(6) 0.115(6) -0.006(5) F5 0.143(7) 0.210(10) 0.050(4) -0.019(5) 0.050(5) -0.054(7) F6 0.148(7) 0.081(5) 0.196(9) -0.064(5) 0.133(7) -0.021(5) C1 0.028(3) 0.025(3) 0.032(3) -0.002(3) -0.003(3) 0.006(3) C2 0.028(3) 0.020(3) 0.045(4) 0.006(3) -0.004(3) -0.002(3) C3 0.023(3) 0.030(3) 0.032(3) 0.004(3) 0.001(3) -0.005(3) C4 0.033(4) 0.031(4) 0.043(4) 0.006(3) 0.008(3) -0.002(3) C5 0.031(4) 0.044(4) 0.036(4) 0.001(3) 0.011(3) -0.004(3) C6 0.026(3) 0.037(4) 0.028(3) 0.003(3) 0.002(3) -0.001(3) C7 0.031(4) 0.042(4) 0.031(4) -0.004(3) 0.003(3) 0.006(3) C8 0.029(3) 0.036(4) 0.030(3) -0.005(3) -0.003(3) 0.005(3) C9 0.024(3) 0.031(3) 0.027(3) -0.006(3) -0.004(3) 0.000(3) C10 0.028(3) 0.038(4) 0.035(4) -0.004(3) -0.003(3) -0.002(3) C11 0.028(3) 0.035(4) 0.031(3) 0.005(3) 0.001(3) -0.007(3) C12 0.021(3) 0.033(3) 0.031(3) 0.000(3) 0.000(3) -0.005(3) C13 0.033(4) 0.045(4) 0.027(3) 0.007(3) 0.006(3) -0.005(3) C14 0.026(3) 0.050(4) 0.031(4) -0.003(3) 0.006(3) 0.002(3) C15 0.021(3) 0.035(4) 0.029(3) -0.002(3) 0.001(3) 0.005(3) C16 0.015(3) 0.034(3) 0.032(3) 0.003(3) -0.003(2) 0.002(2) C17 0.015(3) 0.038(4) 0.026(3) 0.002(3) -0.001(2) 0.005(2) C18 0.020(3) 0.031(3) 0.024(3) -0.001(3) -0.002(2) -0.001(2) C19 0.015(3) 0.030(3) 0.029(3) -0.002(3) -0.003(2) -0.002(2) C20 0.014(3) 0.035(3) 0.029(3) 0.000(3) -0.001(2) -0.003(2) C21 0.042(4) 0.046(4) 0.027(3) 0.006(3) -0.005(3) -0.019(3) C22 0.034(4) 0.088(7) 0.029(4) 0.002(4) 0.001(3) -0.020(4) C23 0.018(3) 0.107(8) 0.034(4) -0.030(5) -0.001(3) 0.003(4) C24 0.040(5) 0.133(11) 0.060(6) -0.056(7) -0.008(4) 0.034(6) C25 0.070(8) 0.145(14) 0.059(7) -0.053(8) -0.035(6) 0.074(9) C26 0.094(8) 0.046(6) 0.081(8) -0.032(5) -0.071(7) 0.043(6) C27 0.20(2) 0.034(8) 0.115(15) -0.013(8) -0.119(15) 0.026(10) C28 0.21(2) 0.021(5) 0.091(11) 0.030(6) -0.110(13) -0.041(9) C29 0.142(12) 0.046(6) 0.064(7) 0.035(5) -0.055(8) -0.060(7) C30 0.156(15) 0.112(12) 0.059(7) 0.051(7) -0.051(8) -0.115(12) C31 0.073(7) 0.187(16) 0.029(5) 0.025(7) -0.004(5) -0.078(9) C32 0.047(5) 0.091(7) 0.024(4) -0.003(4) 0.002(3) -0.034(5) C33 0.026(4) 0.118(9) 0.033(4) -0.027(5) 0.005(3) -0.004(5) C34 0.044(4) 0.043(4) 0.031(4) -0.014(3) -0.002(3) 0.011(3) C35 0.034(3) 0.020(3) 0.023(3) -0.004(2) -0.003(3) 0.000(3) C36 0.022(3) 0.025(3) 0.020(3) -0.004(2) -0.005(2) -0.001(2) C37 0.027(3) 0.041(4) 0.033(4) -0.013(3) -0.012(3) 0.012(3) C38 0.065(6) 0.042(5) 0.045(5) -0.012(4) -0.031(5) 0.024(4) C39 0.091(7) 0.025(4) 0.038(4) 0.010(3) -0.041(5) -0.013(4) C40 0.042(4) 0.049(4) 0.022(3) 0.002(3) -0.006(3) -0.021(3) C41 0.026(3) 0.038(4) 0.051(4) -0.005(3) 0.012(3) 0.000(3) C42 0.058(6) 0.103(9) 0.091(8) -0.018(7) 0.054(6) -0.016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.364(5) . ? Ag1 O6 2.381(5) 3_456 ? Ag1 C22 2.417(8) . ? Ag1 C1 2.432(6) . ? Ag1 C2 2.531(7) . ? Ag1 C21 2.599(7) . ? Ag2 C8 2.392(6) 4_665 ? Ag2 O4 2.418(5) . ? Ag2 O3 2.459(5) . ? Ag2 C33 2.466(8) . ? Ag2 C34 2.496(7) . ? Ag2 C7 2.562(7) 4_665 ? S1 O2 1.433(5) . ? S1 O1 1.437(6) . ? S1 O3 1.441(5) . ? S1 C41 1.844(7) . ? S2 O5 1.426(5) . ? S2 O6 1.432(6) . ? S2 O4 1.438(5) . ? S2 C42 1.823(11) . ? O6 Ag1 2.380(5) 3_456 ? F1 C41 1.319(8) . ? F2 C41 1.313(9) . ? F3 C41 1.312(9) . ? F4 C42 1.312(12) . ? F5 C42 1.334(15) . ? F6 C42 1.335(14) . ? C1 C2 1.404(10) . ? C1 C15 1.457(10) . ? C1 H1A 0.9500 . ? C2 C3 1.452(10) . ? C2 H2B 0.9500 . ? C3 C17 1.361(9) . ? C3 C4 1.457(10) . ? C4 C5 1.380(10) . ? C4 H4A 0.9500 . ? C5 C6 1.439(10) . ? C5 H5B 0.9500 . ? C6 C18 1.374(9) . ? C6 C7 1.462(10) . ? C7 C8 1.392(10) . ? C7 Ag2 2.561(7) 4_566 ? C7 H7A 0.9500 . ? C8 C9 1.449(10) . ? C8 Ag2 2.392(6) 4_566 ? C8 H8A 0.9500 . ? C9 C19 1.385(9) . ? C9 C10 1.429(10) . ? C10 C11 1.373(10) . ? C10 H10A 0.9500 . ? C11 C12 1.449(10) . ? C11 H11A 0.9500 . ? C12 C20 1.362(9) . ? C12 C13 1.442(10) . ? C13 C14 1.384(11) . ? C13 H13A 0.9500 . ? C14 C15 1.445(10) . ? C14 H14A 0.9500 . ? C15 C16 1.371(9) . ? C16 C17 1.404(9) . ? C16 C20 1.414(9) . ? C17 C18 1.417(9) . ? C18 C19 1.415(9) . ? C19 C20 1.408(9) . ? C21 C22 1.357(13) . ? C21 C35 1.437(10) . ? C21 H21A 0.9500 . ? C22 C23 1.423(14) . ? C22 H22A 0.9500 . ? C23 C37 1.372(12) . ? C23 C24 1.430(12) . ? C24 C25 1.32(2) . ? C24 H24A 0.9500 . ? C25 C26 1.46(2) . ? C25 H25A 0.9500 . ? C26 C27 1.40(2) . ? C26 C38 1.426(14) . ? C27 C28 1.31(3) . ? C27 H27A 0.9500 . ? C28 C29 1.51(3) . ? C28 H28A 0.9500 . ? C29 C39 1.372(14) . ? C29 C30 1.40(3) . ? C30 C31 1.41(2) . ? C30 H30A 0.9500 . ? C31 C32 1.461(14) . ? C31 H31A 0.9500 . ? C32 C40 1.349(13) . ? C32 C33 1.444(15) . ? C33 C34 1.389(13) . ? C33 H33A 0.9500 . ? C34 C35 1.453(10) . ? C34 H34A 0.9500 . ? C35 C36 1.375(9) . ? C36 C37 1.399(9) . ? C36 C40 1.416(10) . ? C37 C38 1.400(13) . ? C38 C39 1.399(15) . ? C39 C40 1.425(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 O6 86.3(2) . 3_456 ? O1 Ag1 C22 118.5(3) . . ? O6 Ag1 C22 102.9(3) 3_456 . ? O1 Ag1 C1 105.0(2) . . ? O6 Ag1 C1 119.9(2) 3_456 . ? C22 Ag1 C1 120.0(3) . . ? O1 Ag1 C2 120.7(2) . . ? O6 Ag1 C2 90.7(2) 3_456 . ? C22 Ag1 C2 119.8(3) . . ? C1 Ag1 C2 32.8(2) . . ? O1 Ag1 C21 87.5(2) . . ? O6 Ag1 C21 104.9(2) 3_456 . ? C22 Ag1 C21 31.1(3) . . ? C1 Ag1 C21 133.8(2) . . ? C2 Ag1 C21 148.9(2) . . ? C8 Ag2 O4 108.8(2) 4_665 . ? C8 Ag2 O3 96.7(2) 4_665 . ? O4 Ag2 O3 81.66(16) . . ? C8 Ag2 C33 134.5(3) 4_665 . ? O4 Ag2 C33 100.3(3) . . ? O3 Ag2 C33 122.1(3) . . ? C8 Ag2 C34 153.5(2) 4_665 . ? O4 Ag2 C34 97.6(2) . . ? O3 Ag2 C34 89.7(2) . . ? C33 Ag2 C34 32.5(3) . . ? C8 Ag2 C7 32.4(2) 4_665 4_665 ? O4 Ag2 C7 140.3(2) . 4_665 ? O3 Ag2 C7 105.0(2) . 4_665 ? C33 Ag2 C7 108.0(3) . 4_665 ? C34 Ag2 C7 121.1(2) . 4_665 ? O2 S1 O1 115.1(3) . . ? O2 S1 O3 114.8(3) . . ? O1 S1 O3 114.7(3) . . ? O2 S1 C41 104.8(3) . . ? O1 S1 C41 102.5(4) . . ? O3 S1 C41 102.7(3) . . ? O5 S2 O6 114.7(4) . . ? O5 S2 O4 115.3(3) . . ? O6 S2 O4 113.9(3) . . ? O5 S2 C42 105.3(5) . . ? O6 S2 C42 103.2(5) . . ? O4 S2 C42 102.3(4) . . ? S1 O1 Ag1 119.7(3) . . ? S1 O3 Ag2 120.7(3) . . ? S2 O4 Ag2 114.3(3) . . ? S2 O6 Ag1 127.9(3) . 3_456 ? C2 C1 C15 121.7(6) . . ? C2 C1 Ag1 77.5(4) . . ? C15 C1 Ag1 108.9(4) . . ? C2 C1 H1A 119.2 . . ? C15 C1 H1A 119.2 . . ? Ag1 C1 H1A 83.7 . . ? C1 C2 C3 121.8(6) . . ? C1 C2 Ag1 69.7(4) . . ? C3 C2 Ag1 112.7(4) . . ? C1 C2 H2B 119.1 . . ? C3 C2 H2B 119.1 . . ? Ag1 C2 H2B 87.7 . . ? C17 C3 C2 114.0(6) . . ? C17 C3 C4 115.1(6) . . ? C2 C3 C4 129.3(6) . . ? C5 C4 C3 121.3(6) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 122.1(6) . . ? C4 C5 H5B 118.9 . . ? C6 C5 H5B 118.9 . . ? C18 C6 C5 114.7(6) . . ? C18 C6 C7 113.7(6) . . ? C5 C6 C7 130.0(6) . . ? C8 C7 C6 121.2(6) . . ? C8 C7 Ag2 67.1(4) . 4_566 ? C6 C7 Ag2 117.8(4) . 4_566 ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? Ag2 C7 H7A 85.5 4_566 . ? C7 C8 C9 123.3(6) . . ? C7 C8 Ag2 80.5(4) . 4_566 ? C9 C8 Ag2 110.9(4) . 4_566 ? C7 C8 H8A 118.4 . . ? C9 C8 H8A 118.4 . . ? Ag2 C8 H8A 78.4 4_566 . ? C19 C9 C10 114.3(6) . . ? C19 C9 C8 113.4(6) . . ? C10 C9 C8 131.2(6) . . ? C11 C10 C9 122.4(7) . . ? C11 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? C10 C11 C12 122.1(6) . . ? C10 C11 H11A 119.0 . . ? C12 C11 H11A 119.0 . . ? C20 C12 C13 115.0(6) . . ? C20 C12 C11 113.7(6) . . ? C13 C12 C11 129.8(6) . . ? C14 C13 C12 122.1(6) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 120.9(6) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C16 C15 C14 115.1(6) . . ? C16 C15 C1 113.7(6) . . ? C14 C15 C1 130.0(6) . . ? C15 C16 C17 123.9(6) . . ? C15 C16 C20 122.8(6) . . ? C17 C16 C20 108.6(6) . . ? C3 C17 C16 124.1(6) . . ? C3 C17 C18 122.8(6) . . ? C16 C17 C18 108.0(6) . . ? C6 C18 C19 124.2(6) . . ? C6 C18 C17 122.9(6) . . ? C19 C18 C17 107.5(6) . . ? C9 C19 C20 122.2(6) . . ? C9 C19 C18 123.1(6) . . ? C20 C19 C18 108.5(6) . . ? C12 C20 C19 124.0(6) . . ? C12 C20 C16 122.7(6) . . ? C19 C20 C16 107.4(6) . . ? C22 C21 C35 122.2(7) . . ? C22 C21 Ag1 67.0(4) . . ? C35 C21 Ag1 113.7(4) . . ? C22 C21 H21A 118.9 . . ? C35 C21 H21A 118.9 . . ? Ag1 C21 H21A 89.4 . . ? C21 C22 C23 121.8(7) . . ? C21 C22 Ag1 81.9(5) . . ? C23 C22 Ag1 105.6(5) . . ? C21 C22 H22A 119.1 . . ? C23 C22 H22A 119.1 . . ? Ag1 C22 H22A 82.5 . . ? C37 C23 C22 115.1(7) . . ? C37 C23 C24 116.3(11) . . ? C22 C23 C24 127.2(10) . . ? C25 C24 C23 121.1(13) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 124.8(10) . . ? C24 C25 H25A 117.6 . . ? C26 C25 H25A 117.6 . . ? C27 C26 C38 109.3(17) . . ? C27 C26 C25 135.7(14) . . ? C38 C26 C25 112.7(11) . . ? C28 C27 C26 130.3(19) . . ? C28 C27 H27A 114.8 . . ? C26 C27 H27A 114.8 . . ? C27 C28 C29 118.0(13) . . ? C27 C28 H28A 121.0 . . ? C29 C28 H28A 121.0 . . ? C39 C29 C30 114.6(14) . . ? C39 C29 C28 113.9(17) . . ? C30 C29 C28 130.5(13) . . ? C29 C30 C31 123.7(10) . . ? C29 C30 H30A 118.2 . . ? C31 C30 H30A 118.2 . . ? C30 C31 C32 119.9(13) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C40 C32 C33 114.5(7) . . ? C40 C32 C31 114.1(11) . . ? C33 C32 C31 129.7(11) . . ? C34 C33 C32 122.9(7) . . ? C34 C33 Ag2 74.9(5) . . ? C32 C33 Ag2 106.0(5) . . ? C34 C33 H33A 118.5 . . ? C32 C33 H33A 118.5 . . ? Ag2 C33 H33A 89.1 . . ? C33 C34 C35 120.1(7) . . ? C33 C34 Ag2 72.6(4) . . ? C35 C34 Ag2 107.6(4) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? Ag2 C34 H34A 89.8 . . ? C36 C35 C21 114.5(6) . . ? C36 C35 C34 115.0(6) . . ? C21 C35 C34 128.6(7) . . ? C35 C36 C37 122.4(6) . . ? C35 C36 C40 122.8(6) . . ? C37 C36 C40 108.9(6) . . ? C23 C37 C36 122.5(7) . . ? C23 C37 C38 122.9(8) . . ? C36 C37 C38 108.0(8) . . ? C39 C38 C37 108.4(7) . . ? C39 C38 C26 124.4(11) . . ? C37 C38 C26 121.2(12) . . ? C29 C39 C38 122.1(12) . . ? C29 C39 C40 121.9(13) . . ? C38 C39 C40 108.4(7) . . ? C32 C40 C36 123.4(8) . . ? C32 C40 C39 124.3(8) . . ? C36 C40 C39 106.3(8) . . ? F3 C41 F2 109.1(6) . . ? F3 C41 F1 109.6(6) . . ? F2 C41 F1 108.6(7) . . ? F3 C41 S1 110.5(5) . . ? F2 C41 S1 109.7(5) . . ? F1 C41 S1 109.3(5) . . ? F4 C42 F5 108.0(10) . . ? F4 C42 F6 108.6(11) . . ? F5 C42 F6 111.4(11) . . ? F4 C42 S2 109.8(9) . . ? F5 C42 S2 109.2(9) . . ? F6 C42 S2 109.9(7) . . ? 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 O2 S1 O1 Ag1 -20.4(5) . . . . ? O3 S1 O1 Ag1 116.0(3) . . . . ? C41 S1 O1 Ag1 -133.5(4) . . . . ? O6 Ag1 O1 S1 173.7(4) 3_456 . . . ? C22 Ag1 O1 S1 -83.6(5) . . . . ? C1 Ag1 O1 S1 53.7(4) . . . . ? C2 Ag1 O1 S1 85.1(4) . . . . ? C21 Ag1 O1 S1 -81.1(4) . . . . ? O2 S1 O3 Ag2 18.9(5) . . . . ? O1 S1 O3 Ag2 -117.6(4) . . . . ? C41 S1 O3 Ag2 132.0(4) . . . . ? C8 Ag2 O3 S1 -68.7(4) 4_665 . . . ? O4 Ag2 O3 S1 -176.7(4) . . . . ? C33 Ag2 O3 S1 86.3(4) . . . . ? C34 Ag2 O3 S1 85.5(4) . . . . ? C7 Ag2 O3 S1 -36.7(4) 4_665 . . . ? O5 S2 O4 Ag2 -21.4(5) . . . . ? O6 S2 O4 Ag2 114.3(4) . . . . ? C42 S2 O4 Ag2 -135.1(5) . . . . ? C8 Ag2 O4 S2 102.1(3) 4_665 . . . ? O3 Ag2 O4 S2 -163.7(4) . . . . ? C33 Ag2 O4 S2 -42.4(4) . . . . ? C34 Ag2 O4 S2 -75.2(4) . . . . ? C7 Ag2 O4 S2 92.8(4) 4_665 . . . ? O5 S2 O6 Ag1 153.8(4) . . . 3_456 ? O4 S2 O6 Ag1 17.8(6) . . . 3_456 ? C42 S2 O6 Ag1 -92.2(6) . . . 3_456 ? O1 Ag1 C1 C2 124.1(4) . . . . ? O6 Ag1 C1 C2 29.7(5) 3_456 . . . ? C22 Ag1 C1 C2 -99.4(4) . . . . ? C21 Ag1 C1 C2 -134.7(4) . . . . ? O1 Ag1 C1 C15 -116.4(5) . . . . ? O6 Ag1 C1 C15 149.2(4) 3_456 . . . ? C22 Ag1 C1 C15 20.1(6) . . . . ? C2 Ag1 C1 C15 119.5(6) . . . . ? C21 Ag1 C1 C15 -15.2(6) . . . . ? C15 C1 C2 C3 0.2(10) . . . . ? Ag1 C1 C2 C3 104.8(6) . . . . ? C15 C1 C2 Ag1 -104.6(6) . . . . ? O1 Ag1 C2 C1 -68.5(4) . . . . ? O6 Ag1 C2 C1 -154.6(4) 3_456 . . . ? C22 Ag1 C2 C1 100.1(4) . . . . ? C21 Ag1 C2 C1 84.1(6) . . . . ? O1 Ag1 C2 C3 174.5(4) . . . . ? O6 Ag1 C2 C3 88.5(5) 3_456 . . . ? C22 Ag1 C2 C3 -16.9(6) . . . . ? C1 Ag1 C2 C3 -117.0(6) . . . . ? C21 Ag1 C2 C3 -32.8(7) . . . . ? C1 C2 C3 C17 -7.5(9) . . . . ? Ag1 C2 C3 C17 71.9(6) . . . . ? C1 C2 C3 C4 156.9(7) . . . . ? Ag1 C2 C3 C4 -123.7(6) . . . . ? C17 C3 C4 C5 7.3(10) . . . . ? C2 C3 C4 C5 -156.9(7) . . . . ? C3 C4 C5 C6 1.0(11) . . . . ? C4 C5 C6 C18 -9.2(10) . . . . ? C4 C5 C6 C7 155.5(7) . . . . ? C18 C6 C7 C8 8.4(9) . . . . ? C5 C6 C7 C8 -156.5(7) . . . . ? C18 C6 C7 Ag2 -70.4(7) . . . 4_566 ? C5 C6 C7 Ag2 124.8(7) . . . 4_566 ? C6 C7 C8 C9 -0.9(10) . . . . ? Ag2 C7 C8 C9 108.8(6) 4_566 . . . ? C6 C7 C8 Ag2 -109.7(6) . . . 4_566 ? C7 C8 C9 C19 -8.1(9) . . . . ? Ag2 C8 C9 C19 84.2(6) 4_566 . . . ? C7 C8 C9 C10 158.5(7) . . . . ? Ag2 C8 C9 C10 -109.3(7) 4_566 . . . ? C19 C9 C10 C11 9.5(9) . . . . ? C8 C9 C10 C11 -156.9(7) . . . . ? C9 C10 C11 C12 0.0(10) . . . . ? C10 C11 C12 C20 -9.0(9) . . . . ? C10 C11 C12 C13 156.5(7) . . . . ? C20 C12 C13 C14 8.0(9) . . . . ? C11 C12 C13 C14 -157.3(7) . . . . ? C12 C13 C14 C15 1.8(10) . . . . ? C13 C14 C15 C16 -9.9(9) . . . . ? C13 C14 C15 C1 156.8(7) . . . . ? C2 C1 C15 C16 7.2(9) . . . . ? Ag1 C1 C15 C16 -79.5(6) . . . . ? C2 C1 C15 C14 -159.6(7) . . . . ? Ag1 C1 C15 C14 113.7(7) . . . . ? C14 C15 C16 C17 161.4(6) . . . . ? C1 C15 C16 C17 -7.5(9) . . . . ? C14 C15 C16 C20 8.5(9) . . . . ? C1 C15 C16 C20 -160.4(6) . . . . ? C2 C3 C17 C16 7.7(9) . . . . ? C4 C3 C17 C16 -159.1(6) . . . . ? C2 C3 C17 C18 159.3(6) . . . . ? C4 C3 C17 C18 -7.4(9) . . . . ? C15 C16 C17 C3 -0.1(10) . . . . ? C20 C16 C17 C3 156.1(6) . . . . ? C15 C16 C17 C18 -155.3(6) . . . . ? C20 C16 C17 C18 1.0(7) . . . . ? C5 C6 C18 C19 160.2(6) . . . . ? C7 C6 C18 C19 -7.1(9) . . . . ? C5 C6 C18 C17 9.3(9) . . . . ? C7 C6 C18 C17 -157.9(6) . . . . ? C3 C17 C18 C6 -1.1(10) . . . . ? C16 C17 C18 C6 154.5(6) . . . . ? C3 C17 C18 C19 -156.1(6) . . . . ? C16 C17 C18 C19 -0.5(7) . . . . ? C10 C9 C19 C20 -10.3(9) . . . . ? C8 C9 C19 C20 158.6(6) . . . . ? C10 C9 C19 C18 -159.3(6) . . . . ? C8 C9 C19 C18 9.6(9) . . . . ? C6 C18 C19 C9 -2.1(10) . . . . ? C17 C18 C19 C9 152.5(6) . . . . ? C6 C18 C19 C20 -154.8(6) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C13 C12 C20 C19 -159.4(6) . . . . ? C11 C12 C20 C19 8.4(9) . . . . ? C13 C12 C20 C16 -9.7(9) . . . . ? C11 C12 C20 C16 158.0(6) . . . . ? C9 C19 C20 C12 1.3(9) . . . . ? C18 C19 C20 C12 154.3(6) . . . . ? C9 C19 C20 C16 -152.2(6) . . . . ? C18 C19 C20 C16 0.7(7) . . . . ? C15 C16 C20 C12 1.5(10) . . . . ? C17 C16 C20 C12 -155.0(6) . . . . ? C15 C16 C20 C19 155.5(6) . . . . ? C17 C16 C20 C19 -1.1(7) . . . . ? O1 Ag1 C21 C22 -175.9(5) . . . . ? O6 Ag1 C21 C22 -90.4(5) 3_456 . . . ? C1 Ag1 C21 C22 75.7(6) . . . . ? C2 Ag1 C21 C22 27.4(7) . . . . ? O1 Ag1 C21 C35 67.7(5) . . . . ? O6 Ag1 C21 C35 153.1(5) 3_456 . . . ? C22 Ag1 C21 C35 -116.5(8) . . . . ? C1 Ag1 C21 C35 -40.8(7) . . . . ? C2 Ag1 C21 C35 -89.0(7) . . . . ? C35 C21 C22 C23 1.0(11) . . . . ? Ag1 C21 C22 C23 -103.3(7) . . . . ? C35 C21 C22 Ag1 104.4(6) . . . . ? O1 Ag1 C22 C21 4.7(6) . . . . ? O6 Ag1 C22 C21 97.5(5) 3_456 . . . ? C1 Ag1 C22 C21 -126.1(5) . . . . ? C2 Ag1 C22 C21 -164.1(4) . . . . ? O1 Ag1 C22 C23 125.6(5) . . . . ? O6 Ag1 C22 C23 -141.6(5) 3_456 . . . ? C1 Ag1 C22 C23 -5.3(7) . . . . ? C2 Ag1 C22 C23 -43.2(6) . . . . ? C21 Ag1 C22 C23 120.9(8) . . . . ? C21 C22 C23 C37 9.2(10) . . . . ? Ag1 C22 C23 C37 -80.8(7) . . . . ? C21 C22 C23 C24 -156.7(8) . . . . ? Ag1 C22 C23 C24 113.4(8) . . . . ? C37 C23 C24 C25 -6.7(12) . . . . ? C22 C23 C24 C25 159.0(9) . . . . ? C23 C24 C25 C26 -2.1(15) . . . . ? C24 C25 C26 C27 -151.5(14) . . . . ? C24 C25 C26 C38 8.8(14) . . . . ? C38 C26 C27 C28 -9(2) . . . . ? C25 C26 C27 C28 152.3(17) . . . . ? C26 C27 C28 C29 -2(3) . . . . ? C27 C28 C29 C39 12.9(18) . . . . ? C27 C28 C29 C30 -154.4(15) . . . . ? C39 C29 C30 C31 -11.2(16) . . . . ? C28 C29 C30 C31 156.1(11) . . . . ? C29 C30 C31 C32 1.6(16) . . . . ? C30 C31 C32 C40 8.2(12) . . . . ? C30 C31 C32 C33 -156.2(10) . . . . ? C40 C32 C33 C34 -8.1(11) . . . . ? C31 C32 C33 C34 156.4(9) . . . . ? C40 C32 C33 Ag2 74.1(7) . . . . ? C31 C32 C33 Ag2 -121.5(8) . . . . ? C8 Ag2 C33 C34 142.5(5) 4_665 . . . ? O4 Ag2 C33 C34 -88.0(5) . . . . ? O3 Ag2 C33 C34 -1.5(6) . . . . ? C7 Ag2 C33 C34 120.2(5) 4_665 . . . ? C8 Ag2 C33 C32 21.9(7) 4_665 . . . ? O4 Ag2 C33 C32 151.4(5) . . . . ? O3 Ag2 C33 C32 -122.1(6) . . . . ? C34 Ag2 C33 C32 -120.6(8) . . . . ? C7 Ag2 C33 C32 -0.4(6) 4_665 . . . ? C32 C33 C34 C35 -1.1(11) . . . . ? Ag2 C33 C34 C35 -100.6(6) . . . . ? C32 C33 C34 Ag2 99.5(7) . . . . ? C8 Ag2 C34 C33 -76.9(8) 4_665 . . . ? O4 Ag2 C34 C33 97.2(5) . . . . ? O3 Ag2 C34 C33 178.7(5) . . . . ? C7 Ag2 C34 C33 -73.8(6) 4_665 . . . ? C8 Ag2 C34 C35 40.0(9) 4_665 . . . ? O4 Ag2 C34 C35 -145.9(5) . . . . ? O3 Ag2 C34 C35 -64.4(5) . . . . ? C33 Ag2 C34 C35 116.9(8) . . . . ? C7 Ag2 C34 C35 43.0(6) 4_665 . . . ? C22 C21 C35 C36 -9.7(9) . . . . ? Ag1 C21 C35 C36 67.1(7) . . . . ? C22 C21 C35 C34 153.9(7) . . . . ? Ag1 C21 C35 C34 -129.3(6) . . . . ? C33 C34 C35 C36 8.9(9) . . . . ? Ag2 C34 C35 C36 -70.8(6) . . . . ? C33 C34 C35 C21 -154.6(7) . . . . ? Ag2 C34 C35 C21 125.7(6) . . . . ? C21 C35 C36 C37 8.1(9) . . . . ? C34 C35 C36 C37 -157.7(6) . . . . ? C21 C35 C36 C40 158.0(6) . . . . ? C34 C35 C36 C40 -7.8(9) . . . . ? C22 C23 C37 C36 -10.9(10) . . . . ? C24 C23 C37 C36 156.6(7) . . . . ? C22 C23 C37 C38 -159.1(7) . . . . ? C24 C23 C37 C38 8.4(11) . . . . ? C35 C36 C37 C23 2.2(10) . . . . ? C40 C36 C37 C23 -151.3(7) . . . . ? C35 C36 C37 C38 154.5(6) . . . . ? C40 C36 C37 C38 0.9(7) . . . . ? C23 C37 C38 C39 152.5(7) . . . . ? C36 C37 C38 C39 0.4(8) . . . . ? C23 C37 C38 C26 -1.4(12) . . . . ? C36 C37 C38 C26 -153.5(8) . . . . ? C27 C26 C38 C39 9.1(12) . . . . ? C25 C26 C38 C39 -156.5(9) . . . . ? C27 C26 C38 C37 158.6(9) . . . . ? C25 C26 C38 C37 -7.0(12) . . . . ? C30 C29 C39 C38 157.1(9) . . . . ? C28 C29 C39 C38 -12.4(13) . . . . ? C30 C29 C39 C40 11.1(13) . . . . ? C28 C29 C39 C40 -158.4(9) . . . . ? C37 C38 C39 C29 -151.5(8) . . . . ? C26 C38 C39 C29 1.3(13) . . . . ? C37 C38 C39 C40 -1.5(8) . . . . ? C26 C38 C39 C40 151.3(7) . . . . ? C33 C32 C40 C36 9.5(10) . . . . ? C31 C32 C40 C36 -157.5(7) . . . . ? C33 C32 C40 C39 158.3(7) . . . . ? C31 C32 C40 C39 -8.6(11) . . . . ? C35 C36 C40 C32 -1.6(10) . . . . ? C37 C36 C40 C32 151.8(7) . . . . ? C35 C36 C40 C39 -155.2(6) . . . . ? C37 C36 C40 C39 -1.8(7) . . . . ? C29 C39 C40 C32 -1.2(13) . . . . ? C38 C39 C40 C32 -151.3(8) . . . . ? C29 C39 C40 C36 152.1(8) . . . . ? C38 C39 C40 C36 2.0(8) . . . . ? O2 S1 C41 F3 -178.6(5) . . . . ? O1 S1 C41 F3 -58.1(6) . . . . ? O3 S1 C41 F3 61.1(6) . . . . ? O2 S1 C41 F2 61.0(6) . . . . ? O1 S1 C41 F2 -178.5(5) . . . . ? O3 S1 C41 F2 -59.3(6) . . . . ? O2 S1 C41 F1 -57.9(6) . . . . ? O1 S1 C41 F1 62.6(6) . . . . ? O3 S1 C41 F1 -178.2(5) . . . . ? O5 S2 C42 F4 58.9(11) . . . . ? O6 S2 C42 F4 -61.7(10) . . . . ? O4 S2 C42 F4 179.8(9) . . . . ? O5 S2 C42 F5 -59.2(8) . . . . ? O6 S2 C42 F5 -179.9(7) . . . . ? O4 S2 C42 F5 61.7(8) . . . . ? O5 S2 C42 F6 178.3(8) . . . . ? O6 S2 C42 F6 57.7(9) . . . . ? O4 S2 C42 F6 -60.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.803 _refine_diff_density_min -2.109 _refine_diff_density_rms 0.166 #========================================================================== data_4_(SG0311) _database_code_depnum_ccdc_archive 'CCDC 246842' _audit_creation_method SHELXL-97 _audit_creation_date 03-05-05 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C20 H10, 2(Ag 1+), 2(B F4 1-)' _chemical_formula_sum 'C20 H10 Ag2 B2 F8' _chemical_formula_weight 639.64 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 40 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 20 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ag Ag 4 -0.8971 1.1015 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; B B 4 0.0013 0.0007 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 16 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5741(2) _cell_length_b 9.6621(2) _cell_length_c 10.6735(2) _cell_angle_alpha 98.3042(13) _cell_angle_beta 110.3937(13) _cell_angle_gamma 101.4884(9) _cell_volume 882.01(3) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 30014 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.869 _exptl_special_details ; Solvent used: toluene / hexane Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.917(2) Frames collected: 386 Seconds exposure per frame: 12 Degrees rotation per frame: 2.0 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 24787 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 30.04 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 5144 _reflns_number_gt 4337 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2003)' _refine_special_details ; Three of the F-atoms in one BF4- anion are disordered over two orientations which are related by a pivot of approximately 30/% about the fourth B-F bond. Two sets of positions were defined for these F-atoms and the site occupation factor of the major conformation refined to 0.643(5). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.2366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom & difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5144 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.071 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.112 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 0.36731(2) 0.36920(2) 0.67760(2) 0.03190(8) Uani 1 1 d . . . Ag2 Ag 0.24467(2) 0.24313(2) 0.10321(2) 0.02479(7) Uani 1 1 d . . . C1 C 0.1928(3) 0.0301(3) 0.3533(2) 0.0190(5) Uani 1 1 d . . . C2 C 0.0863(3) -0.0710(3) 0.2306(2) 0.0188(4) Uani 1 1 d . A . C3 C -0.0130(3) -0.1739(3) 0.2661(2) 0.0187(4) Uani 1 1 d . . . C4 C 0.0345(3) -0.1370(3) 0.4110(2) 0.0192(5) Uani 1 1 d . A . C5 C 0.1610(3) -0.0120(3) 0.4644(3) 0.0200(5) Uani 1 1 d . . . C6 C 0.4150(3) 0.1242(3) 0.6178(3) 0.0248(5) Uani 1 1 d . A . H6 H 0.4899 0.1647 0.7088 0.030 Uiso 1 1 d R . . C7 C 0.4462(3) 0.1646(3) 0.5083(3) 0.0253(5) Uani 1 1 d . . . H7 H 0.5424 0.2309 0.5262 0.030 Uiso 1 1 calc R A . C8 C 0.3359(3) 0.1081(3) 0.3680(3) 0.0220(5) Uani 1 1 d . A . C9 C 0.3644(3) 0.0932(3) 0.2420(3) 0.0244(5) Uani 1 1 d . . . H9 H 0.4560 0.1531 0.2418 0.029 Uiso 1 1 d R A . C10 C 0.2600(3) -0.0075(3) 0.1208(3) 0.0238(5) Uani 1 1 d . A . H10 H 0.2823 -0.0146 0.0404 0.029 Uiso 1 1 d R . . C11 C 0.1181(3) -0.1015(3) 0.1159(3) 0.0212(5) Uani 1 1 d . . . C12 C 0.0263(3) -0.2411(3) 0.0224(3) 0.0236(5) Uani 1 1 d . . . H12 H 0.0338 -0.2645 -0.0642 0.028 Uiso 1 1 d R . . C13 C -0.0734(3) -0.3426(3) 0.0568(3) 0.0237(5) Uani 1 1 d . . . H13 H -0.1323 -0.4324 -0.0073 0.028 Uiso 1 1 d R A . C14 C -0.0878(3) -0.3126(3) 0.1888(3) 0.0209(5) Uani 1 1 d . A . C15 C -0.1379(3) -0.4137(3) 0.2613(3) 0.0244(5) Uani 1 1 d . . . H15 H -0.2040 -0.5073 0.2109 0.029 Uiso 1 1 d R A . C16 C -0.0913(3) -0.3772(3) 0.4045(3) 0.0252(5) Uani 1 1 d . . . H16 H -0.1273 -0.4464 0.4488 0.030 Uiso 1 1 d R . . C17 C 0.0105(3) -0.2365(3) 0.4863(3) 0.0222(5) Uani 1 1 d . . . C18 C 0.1115(3) -0.1932(3) 0.6305(3) 0.0267(5) Uani 1 1 d . A . H18 H 0.0921 -0.2506 0.6909 0.032 Uiso 1 1 calc R . . C19 C 0.2354(3) -0.0705(3) 0.6827(3) 0.0258(5) Uani 1 1 d . . . H19 H 0.2989 -0.0462 0.7780 0.031 Uiso 1 1 calc R A . C20 C 0.2714(3) 0.0221(3) 0.5968(3) 0.0227(5) Uani 1 1 d . A . F1A F 0.5194(7) 0.1243(5) 1.0092(6) 0.0394(16) Uani 0.357(5) 1 d P A 1 F2A F 0.6679(7) 0.3276(7) 0.9932(7) 0.055(2) Uani 0.357(5) 1 d P A 1 F3A F 0.4073(8) 0.2759(9) 0.8987(6) 0.058(2) Uani 0.357(5) 1 d P A 1 F1B F 0.4059(4) 0.1808(5) 0.9379(4) 0.0565(14) Uani 0.643(5) 1 d P A 2 F2B F 0.6645(4) 0.2427(4) 1.0690(3) 0.0518(11) Uani 0.643(5) 1 d P A 2 F3B F 0.5654(4) 0.3784(4) 0.9257(3) 0.0485(10) Uani 0.643(5) 1 d P A 2 F4 F 0.5184(2) 0.3622(3) 1.1216(2) 0.0525(6) Uani 1 1 d . . . B1 B 0.5378(4) 0.2843(4) 1.0105(3) 0.0305(7) Uani 1 1 d . . . F5 F 0.7773(3) 0.3787(3) 0.7010(2) 0.0550(6) Uani 1 1 d . A . F6 F 0.6221(2) 0.5245(2) 0.70676(19) 0.0368(4) Uani 1 1 d . . . F7 F 0.8576(2) 0.6184(2) 0.7073(2) 0.0506(6) Uani 1 1 d . A . F8 F 0.6701(2) 0.4644(2) 0.51419(18) 0.0405(5) Uani 1 1 d . A . B2 B 0.7338(4) 0.4946(4) 0.6568(3) 0.0279(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02146(11) 0.02681(12) 0.04722(15) 0.00938(10) 0.01397(10) 0.00437(8) Ag2 0.02239(11) 0.02541(11) 0.02595(11) 0.00844(8) 0.00766(8) 0.00649(8) C1 0.0182(11) 0.0180(11) 0.0211(11) 0.0054(9) 0.0065(9) 0.0067(9) C2 0.0168(11) 0.0184(11) 0.0219(11) 0.0065(9) 0.0070(9) 0.0057(9) C3 0.0163(11) 0.0209(11) 0.0194(11) 0.0066(9) 0.0063(9) 0.0056(9) C4 0.0162(11) 0.0209(11) 0.0206(11) 0.0043(9) 0.0073(9) 0.0053(9) C5 0.0178(11) 0.0214(12) 0.0221(11) 0.0051(9) 0.0085(9) 0.0070(9) C6 0.0219(12) 0.0208(12) 0.0253(12) 0.0005(10) 0.0034(10) 0.0060(10) C7 0.0183(12) 0.0190(12) 0.0326(14) 0.0040(10) 0.0049(10) 0.0026(9) C8 0.0198(12) 0.0190(12) 0.0276(13) 0.0083(10) 0.0083(10) 0.0058(9) C9 0.0187(12) 0.0250(13) 0.0334(14) 0.0131(11) 0.0119(10) 0.0063(10) C10 0.0237(12) 0.0291(13) 0.0263(12) 0.0135(10) 0.0140(10) 0.0109(10) C11 0.0210(12) 0.0232(12) 0.0219(11) 0.0092(9) 0.0084(9) 0.0085(10) C12 0.0255(12) 0.0266(13) 0.0189(11) 0.0044(10) 0.0074(10) 0.0102(10) C13 0.0235(12) 0.0199(12) 0.0231(12) 0.0020(9) 0.0050(10) 0.0056(10) C14 0.0149(11) 0.0221(12) 0.0234(12) 0.0069(9) 0.0043(9) 0.0042(9) C15 0.0161(11) 0.0221(12) 0.0312(13) 0.0071(10) 0.0059(10) 0.0020(9) C16 0.0199(12) 0.0249(13) 0.0352(14) 0.0145(11) 0.0132(11) 0.0058(10) C17 0.0182(11) 0.0274(13) 0.0250(12) 0.0098(10) 0.0110(10) 0.0075(10) C18 0.0267(13) 0.0346(15) 0.0241(12) 0.0131(11) 0.0123(10) 0.0109(11) C19 0.0265(13) 0.0324(14) 0.0195(12) 0.0066(10) 0.0080(10) 0.0111(11) C20 0.0220(12) 0.0236(12) 0.0223(12) 0.0025(9) 0.0081(10) 0.0089(10) F1A 0.055(4) 0.029(3) 0.046(3) 0.012(2) 0.031(3) 0.013(2) F2A 0.043(4) 0.052(4) 0.065(4) -0.013(3) 0.040(3) -0.013(3) F3A 0.058(4) 0.062(5) 0.041(3) 0.008(3) -0.004(3) 0.030(4) F1B 0.047(2) 0.056(3) 0.0429(19) -0.0142(18) 0.0197(17) -0.0228(19) F2B 0.055(2) 0.062(2) 0.0421(18) 0.0124(16) 0.0122(16) 0.0356(18) F3B 0.061(2) 0.053(2) 0.0395(17) 0.0204(15) 0.0263(17) 0.0124(17) F4 0.0424(11) 0.0622(14) 0.0401(11) -0.0138(9) 0.0271(9) -0.0159(10) B1 0.0264(15) 0.0406(18) 0.0217(14) 0.0044(13) 0.0111(12) 0.0021(13) F5 0.0398(11) 0.0537(13) 0.0600(13) 0.0155(11) 0.0003(10) 0.0208(10) F6 0.0308(9) 0.0378(10) 0.0391(10) -0.0024(8) 0.0205(8) -0.0007(7) F7 0.0370(10) 0.0497(12) 0.0476(11) -0.0167(9) 0.0242(9) -0.0204(9) F8 0.0415(10) 0.0471(11) 0.0244(8) 0.0038(8) 0.0143(8) -0.0062(8) B2 0.0219(14) 0.0311(16) 0.0245(14) -0.0021(12) 0.0100(12) -0.0023(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 F6 2.4856(17) . ? Ag1 C16 2.499(3) 2_556 ? Ag1 C6 2.533(3) . ? Ag1 F3A 2.579(8) . ? Ag1 C15 2.594(3) 2_556 ? Ag2 C13 2.383(3) 2 ? Ag2 C9 2.389(3) . ? Ag2 C12 2.465(3) 2 ? Ag2 C10 2.485(3) . ? Ag2 F6 2.5539(17) 2_666 ? Ag2 F4 2.5702(19) 1_554 ? C1 C8 1.369(3) . ? C1 C5 1.416(3) . ? C1 C2 1.418(3) . ? C2 C11 1.368(3) . ? C2 C3 1.420(3) . ? C3 C14 1.369(3) . ? C3 C4 1.419(3) . ? C4 C17 1.373(4) . ? C4 C5 1.410(3) . ? C5 C20 1.382(4) . ? C6 C7 1.392(4) . ? C6 C20 1.447(4) . ? C6 H6 0.9500 . ? C7 C8 1.445(4) . ? C7 H7 0.9500 . ? C8 C9 1.456(4) . ? C9 C10 1.403(4) . ? C9 H9 0.9500 . ? C10 C11 1.455(4) . ? C10 H10 0.9500 . ? C11 C12 1.455(4) . ? C12 C13 1.408(4) . ? C12 H12 0.9500 . ? C13 C14 1.456(4) . ? C13 H13 0.9500 . ? C14 C15 1.440(4) . ? C15 C16 1.402(4) . ? C15 H15 0.9500 . ? C16 C17 1.448(4) . ? C16 H16 0.9500 . ? C17 C18 1.448(4) . ? C18 C19 1.382(4) . ? C18 H18 0.9500 . ? C19 C20 1.447(4) . ? C19 H19 0.9500 . ? F1A B1 1.518(6) . ? F2A B1 1.317(6) . ? F3A B1 1.373(7) . ? F1B B1 1.337(5) . ? F2B B1 1.327(5) . ? F3B B1 1.422(5) . ? F4 B1 1.400(4) . ? F5 B2 1.361(4) . ? F6 B2 1.410(4) . ? F7 B2 1.389(4) . ? F8 B2 1.388(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F6 Ag1 C16 138.25(8) . 2_556 ? F6 Ag1 C6 98.09(8) . . ? C16 Ag1 C6 116.50(9) 2_556 . ? F6 Ag1 F3A 107.05(18) . . ? C16 Ag1 F3A 103.27(18) 2_556 . ? C6 Ag1 F3A 76.74(17) . . ? F6 Ag1 C15 134.77(7) . 2_556 ? C16 Ag1 C15 31.89(9) 2_556 2_556 ? C6 Ag1 C15 125.75(9) . 2_556 ? F3A Ag1 C15 76.66(17) . 2_556 ? C13 Ag2 C9 166.24(9) 2 . ? C13 Ag2 C12 33.72(9) 2 2 ? C9 Ag2 C12 133.84(9) . 2 ? C13 Ag2 C10 134.31(9) 2 . ? C9 Ag2 C10 33.37(9) . . ? C12 Ag2 C10 109.71(9) 2 . ? C13 Ag2 F6 96.77(8) 2 2_666 ? C9 Ag2 F6 94.29(8) . 2_666 ? C12 Ag2 F6 108.87(7) 2 2_666 ? C10 Ag2 F6 127.45(8) . 2_666 ? C13 Ag2 F4 106.34(9) 2 1_554 ? C9 Ag2 F4 85.47(9) . 1_554 ? C12 Ag2 F4 140.01(9) 2 1_554 ? C10 Ag2 F4 101.56(8) . 1_554 ? F6 Ag2 F4 67.43(6) 2_666 1_554 ? C8 C1 C5 122.8(2) . . ? C8 C1 C2 123.6(2) . . ? C5 C1 C2 107.8(2) . . ? C11 C2 C1 123.0(2) . . ? C11 C2 C3 123.1(2) . . ? C1 C2 C3 108.1(2) . . ? C14 C3 C4 122.7(2) . . ? C14 C3 C2 123.8(2) . . ? C4 C3 C2 107.7(2) . . ? C17 C4 C5 122.8(2) . . ? C17 C4 C3 123.3(2) . . ? C5 C4 C3 108.2(2) . . ? C20 C5 C4 123.3(2) . . ? C20 C5 C1 123.0(2) . . ? C4 C5 C1 108.3(2) . . ? C7 C6 C20 121.7(2) . . ? C7 C6 Ag1 89.21(17) . . ? C20 C6 Ag1 103.49(17) . . ? C7 C6 H6 119.2 . . ? C20 C6 H6 119.2 . . ? Ag1 C6 H6 77.0 . . ? C6 C7 C8 121.7(2) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C1 C8 C7 115.0(2) . . ? C1 C8 C9 114.6(2) . . ? C7 C8 C9 128.7(2) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 Ag2 77.10(16) . . ? C8 C9 Ag2 110.39(17) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? Ag2 C9 H9 82.6 . . ? C9 C10 C11 121.2(2) . . ? C9 C10 Ag2 69.53(15) . . ? C11 C10 Ag2 113.77(17) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? Ag2 C10 H10 86.9 . . ? C2 C11 C12 114.7(2) . . ? C2 C11 C10 115.1(2) . . ? C12 C11 C10 128.5(2) . . ? C13 C12 C11 121.8(2) . . ? C13 C12 Ag2 69.96(15) . 2 ? C11 C12 Ag2 112.39(17) . 2 ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? Ag2 C12 H12 87.7 2 . ? C12 C13 C14 121.2(2) . . ? C12 C13 Ag2 76.32(16) . 2 ? C14 C13 Ag2 109.88(17) . 2 ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? Ag2 C13 H13 83.9 2 . ? C3 C14 C15 115.1(2) . . ? C3 C14 C13 114.6(2) . . ? C15 C14 C13 128.7(2) . . ? C16 C15 C14 121.6(2) . . ? C16 C15 Ag1 70.31(15) . 2_556 ? C14 C15 Ag1 113.64(18) . 2_556 ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? Ag1 C15 H15 86.2 2_556 . ? C15 C16 C17 121.4(2) . . ? C15 C16 Ag1 77.79(15) . 2_556 ? C17 C16 Ag1 110.56(17) . 2_556 ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? Ag1 C16 H16 81.8 2_556 . ? C4 C17 C18 114.8(2) . . ? C4 C17 C16 114.4(2) . . ? C18 C17 C16 129.7(2) . . ? C19 C18 C17 121.7(2) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 122.1(2) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C5 C20 C6 114.4(2) . . ? C5 C20 C19 114.2(2) . . ? C6 C20 C19 130.2(2) . . ? B1 F3A Ag1 132.2(6) . . ? B1 F4 Ag2 106.59(17) . 1_556 ? F2B B1 F1B 117.8(4) . . ? F2A B1 F3A 114.1(6) . . ? F2A B1 F4 118.7(4) . . ? F2B B1 F4 103.8(3) . . ? F1B B1 F4 107.3(3) . . ? F3A B1 F4 104.3(4) . . ? F2B B1 F3B 109.1(3) . . ? F1B B1 F3B 108.9(3) . . ? F4 B1 F3B 109.6(3) . . ? F2A B1 F1A 104.8(5) . . ? F3A B1 F1A 100.3(5) . . ? F4 B1 F1A 113.3(3) . . ? B2 F6 Ag1 130.95(16) . . ? B2 F6 Ag2 106.67(15) . 2_666 ? Ag1 F6 Ag2 120.65(7) . 2_666 ? F5 B2 F8 110.5(3) . . ? F5 B2 F7 111.6(3) . . ? F8 B2 F7 109.7(3) . . ? F5 B2 F6 108.6(3) . . ? F8 B2 F6 109.0(2) . . ? F7 B2 F6 107.3(2) . . ? 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 C8 C1 C2 C11 1.0(4) . . . . ? C5 C1 C2 C11 -152.6(2) . . . . ? C8 C1 C2 C3 154.7(2) . . . . ? C5 C1 C2 C3 1.0(3) . . . . ? C11 C2 C3 C14 -0.7(4) . . . . ? C1 C2 C3 C14 -154.3(2) . . . . ? C11 C2 C3 C4 152.7(2) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C14 C3 C4 C17 0.3(4) . . . . ? C2 C3 C4 C17 -153.4(2) . . . . ? C14 C3 C4 C5 154.2(2) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C17 C4 C5 C20 -0.3(4) . . . . ? C3 C4 C5 C20 -154.3(2) . . . . ? C17 C4 C5 C1 154.2(2) . . . . ? C3 C4 C5 C1 0.2(3) . . . . ? C8 C1 C5 C20 0.0(4) . . . . ? C2 C1 C5 C20 153.9(2) . . . . ? C8 C1 C5 C4 -154.6(2) . . . . ? C2 C1 C5 C4 -0.8(3) . . . . ? F6 Ag1 C6 C7 -57.07(16) . . . . ? C16 Ag1 C6 C7 98.83(17) 2_556 . . . ? F3A Ag1 C6 C7 -162.8(2) . . . . ? C15 Ag1 C6 C7 134.72(16) 2_556 . . . ? F6 Ag1 C6 C20 -179.54(17) . . . . ? C16 Ag1 C6 C20 -23.6(2) 2_556 . . . ? F3A Ag1 C6 C20 74.7(2) . . . . ? C15 Ag1 C6 C20 12.3(2) 2_556 . . . ? C20 C6 C7 C8 0.8(4) . . . . ? Ag1 C6 C7 C8 -104.6(2) . . . . ? C5 C1 C8 C7 -9.4(4) . . . . ? C2 C1 C8 C7 -159.2(2) . . . . ? C5 C1 C8 C9 157.0(2) . . . . ? C2 C1 C8 C9 7.2(4) . . . . ? C6 C7 C8 C1 8.9(4) . . . . ? C6 C7 C8 C9 -155.3(3) . . . . ? C1 C8 C9 C10 -7.6(4) . . . . ? C7 C8 C9 C10 156.6(3) . . . . ? C1 C8 C9 Ag2 79.5(2) . . . . ? C7 C8 C9 Ag2 -116.3(3) . . . . ? C13 Ag2 C9 C10 30.6(5) 2 . . . ? C12 Ag2 C9 C10 52.58(19) 2 . . . ? F6 Ag2 C9 C10 174.02(14) 2_666 . . . ? F4 Ag2 C9 C10 -119.06(15) 1_554 . . . ? C13 Ag2 C9 C8 -88.6(4) 2 . . . ? C12 Ag2 C9 C8 -66.6(2) 2 . . . ? C10 Ag2 C9 C8 -119.2(2) . . . . ? F6 Ag2 C9 C8 54.82(18) 2_666 . . . ? F4 Ag2 C9 C8 121.74(18) 1_554 . . . ? C8 C9 C10 C11 0.1(4) . . . . ? Ag2 C9 C10 C11 -106.1(2) . . . . ? C8 C9 C10 Ag2 106.2(2) . . . . ? C13 Ag2 C10 C9 -170.26(15) 2 . . . ? C12 Ag2 C10 C9 -142.52(15) 2 . . . ? F6 Ag2 C10 C9 -7.52(18) 2_666 . . . ? F4 Ag2 C10 C9 62.80(15) 1_554 . . . ? C13 Ag2 C10 C11 -54.1(2) 2 . . . ? C9 Ag2 C10 C11 116.1(2) . . . . ? C12 Ag2 C10 C11 -26.4(2) 2 . . . ? F6 Ag2 C10 C11 108.60(18) 2_666 . . . ? F4 Ag2 C10 C11 178.92(17) 1_554 . . . ? C1 C2 C11 C12 157.7(2) . . . . ? C3 C2 C11 C12 7.9(4) . . . . ? C1 C2 C11 C10 -8.6(4) . . . . ? C3 C2 C11 C10 -158.4(2) . . . . ? C9 C10 C11 C2 7.9(4) . . . . ? Ag2 C10 C11 C2 -71.7(3) . . . . ? C9 C10 C11 C12 -156.1(3) . . . . ? Ag2 C10 C11 C12 124.2(2) . . . . ? C2 C11 C12 C13 -7.1(4) . . . . ? C10 C11 C12 C13 157.0(3) . . . . ? C2 C11 C12 Ag2 72.4(2) . . . 2 ? C10 C11 C12 Ag2 -123.4(2) . . . 2 ? C11 C12 C13 C14 -0.6(4) . . . . ? Ag2 C12 C13 C14 -105.2(2) 2 . . . ? C11 C12 C13 Ag2 104.5(2) . . . 2 ? C4 C3 C14 C15 9.9(4) . . . . ? C2 C3 C14 C15 159.4(2) . . . . ? C4 C3 C14 C13 -156.8(2) . . . . ? C2 C3 C14 C13 -7.3(4) . . . . ? C12 C13 C14 C3 7.7(4) . . . . ? Ag2 C13 C14 C3 -78.0(2) 2 . . . ? C12 C13 C14 C15 -156.8(3) . . . . ? Ag2 C13 C14 C15 117.5(3) 2 . . . ? C3 C14 C15 C16 -9.7(4) . . . . ? C13 C14 C15 C16 154.8(3) . . . . ? C3 C14 C15 Ag1 71.0(2) . . . 2_556 ? C13 C14 C15 Ag1 -124.6(2) . . . 2_556 ? C14 C15 C16 C17 -0.5(4) . . . . ? Ag1 C15 C16 C17 -106.8(2) 2_556 . . . ? C14 C15 C16 Ag1 106.3(2) . . . 2_556 ? C5 C4 C17 C18 8.7(4) . . . . ? C3 C4 C17 C18 158.8(2) . . . . ? C5 C4 C17 C16 -160.7(2) . . . . ? C3 C4 C17 C16 -10.5(4) . . . . ? C15 C16 C17 C4 10.5(4) . . . . ? Ag1 C16 C17 C4 -77.5(2) 2_556 . . . ? C15 C16 C17 C18 -156.9(3) . . . . ? Ag1 C16 C17 C18 115.1(3) 2_556 . . . ? C4 C17 C18 C19 -8.5(4) . . . . ? C16 C17 C18 C19 158.8(3) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C4 C5 C20 C6 160.6(2) . . . . ? C1 C5 C20 C6 9.7(4) . . . . ? C4 C5 C20 C19 -8.1(4) . . . . ? C1 C5 C20 C19 -158.9(2) . . . . ? C7 C6 C20 C5 -10.0(4) . . . . ? Ag1 C6 C20 C5 87.6(2) . . . . ? C7 C6 C20 C19 156.4(3) . . . . ? Ag1 C6 C20 C19 -106.0(3) . . . . ? C18 C19 C20 C5 8.0(4) . . . . ? C18 C19 C20 C6 -158.4(3) . . . . ? F6 Ag1 F3A B1 -8.4(6) . . . . ? C16 Ag1 F3A B1 -159.3(5) 2_556 . . . ? C6 Ag1 F3A B1 86.1(6) . . . . ? C15 Ag1 F3A B1 -141.6(6) 2_556 . . . ? Ag1 F3A B1 F2A -12.2(8) . . . . ? Ag1 F3A B1 F4 118.9(5) . . . . ? Ag1 F3A B1 F1A -123.7(5) . . . . ? Ag2 F4 B1 F2A 177.4(5) 1_556 . . . ? Ag2 F4 B1 F2B -124.3(3) 1_556 . . . ? Ag2 F4 B1 F1B 1.1(4) 1_556 . . . ? Ag2 F4 B1 F3A 49.1(5) 1_556 . . . ? Ag2 F4 B1 F3B 119.2(3) 1_556 . . . ? Ag2 F4 B1 F1A -59.0(4) 1_556 . . . ? C16 Ag1 F6 B2 -125.2(3) 2_556 . . . ? C6 Ag1 F6 B2 21.5(3) . . . . ? F3A Ag1 F6 B2 100.0(3) . . . . ? C15 Ag1 F6 B2 -172.0(2) 2_556 . . . ? C16 Ag1 F6 Ag2 71.92(15) 2_556 . . 2_666 ? C6 Ag1 F6 Ag2 -141.36(10) . . . 2_666 ? F3A Ag1 F6 Ag2 -62.83(18) . . . 2_666 ? C15 Ag1 F6 Ag2 25.12(15) 2_556 . . 2_666 ? Ag1 F6 B2 F5 -57.3(3) . . . . ? Ag2 F6 B2 F5 107.3(2) 2_666 . . . ? Ag1 F6 B2 F8 63.2(3) . . . . ? Ag2 F6 B2 F8 -132.15(19) 2_666 . . . ? Ag1 F6 B2 F7 -178.08(17) . . . . ? Ag2 F6 B2 F7 -13.4(3) 2_666 . . . ? # End of CIF ============================================================