# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chen, Jhy-Der' _publ_contact_author_email jdchen@cycu.edu.tw loop_ _publ_author_name 'Chia-Jun Wu' 'Ming-Jhe Sie' 'Hui-Lin Hsiao' 'Jhy-Der Chen' data_1 _database_code_depnum_ccdc_archive 'CCDC 809206' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H11 Ag N4 O6' _chemical_formula_weight 427.13 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' 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.3854(9) _cell_length_b 8.8391(12) _cell_length_c 26.129(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1474.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 4.69 _cell_measurement_theta_max 10.97 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9141 _exptl_absorpt_correction_T_max 0.9917 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2133 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1943 _reflns_number_gt 1234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(8) _refine_ls_number_reflns 1943 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.91078(12) -0.29187(9) 0.81751(3) 0.0539(3) Uani 1 1 d . . . O1 O 0.0989(10) -0.1744(6) 0.8925(2) 0.0501(17) Uani 1 1 d . . . O2 O 0.3808(15) 0.5564(8) 0.9701(3) 0.089(3) Uani 1 1 d . . . O3 O 0.7118(12) 0.4883(9) 0.9563(3) 0.061(2) Uani 1 1 d . . . O4 O 1.021(4) -0.042(3) 0.7824(15) 0.062(6) Uani 0.60 1 d P A 1 O4' O 1.091(6) 0.003(6) 0.781(3) 0.102(18) Uani 0.40 1 d P A 2 O5 O 0.719(3) 0.020(2) 0.8113(10) 0.067(6) Uani 0.60 1 d P A 1 O5' O 0.786(4) -0.043(3) 0.8102(17) 0.070(11) Uani 0.40 1 d P A 2 O6 O 0.915(3) 0.1795(11) 0.7727(5) 0.053(4) Uani 0.60 1 d P A 1 O6' O 0.855(5) 0.179(4) 0.7946(10) 0.116(15) Uiso 0.40 1 d P A 2 N1 N 0.5901(13) -0.4036(7) 0.8194(3) 0.0368(17) Uani 1 1 d . A . N2 N 0.2285(13) -0.4193(8) 0.8331(3) 0.038(2) Uani 1 1 d . . . N3 N 0.4161(12) -0.2007(8) 0.8531(2) 0.0376(17) Uani 1 1 d . A . H3A H 0.5252 -0.1493 0.8447 0.045 Uiso 1 1 calc R . . N4 N 0.898(2) 0.0485(11) 0.7916(3) 0.052(3) Uani 1 1 d . . . C1 C 0.591(2) -0.5485(11) 0.8029(4) 0.058(3) Uani 1 1 d . . . H1 H 0.7154 -0.5909 0.7911 0.070 Uiso 1 1 calc R A . C2 C 0.4150(17) -0.6325(10) 0.8033(3) 0.045(2) Uani 1 1 d . A . H2 H 0.4175 -0.7335 0.7934 0.054 Uiso 1 1 calc R . . C3 C 0.2365(17) -0.5667(9) 0.8182(4) 0.042(2) Uani 1 1 d . . . H3B H 0.1140 -0.6236 0.8184 0.050 Uiso 1 1 calc R A . C4 C 0.4097(18) -0.3488(8) 0.8344(3) 0.032(2) Uani 1 1 d . . . C5 C 0.2737(15) -0.1264(11) 0.8827(3) 0.035(2) Uani 1 1 d . . . C6 C 0.3405(14) 0.0255(11) 0.9028(4) 0.035(3) Uani 1 1 d . A . C7 C 0.1933(17) 0.1342(11) 0.9118(4) 0.046(3) Uani 1 1 d . . . H7 H 0.0537 0.1119 0.9049 0.055 Uiso 1 1 calc R A . C8 C 0.2425(18) 0.2758(13) 0.9306(4) 0.052(3) Uani 1 1 d . A . H8 H 0.1390 0.3479 0.9363 0.062 Uiso 1 1 calc R . . C9 C 0.4519(13) 0.3072(11) 0.9408(3) 0.034(2) Uani 1 1 d . . . C10 C 0.6029(17) 0.1986(10) 0.9338(3) 0.044(2) Uani 1 1 d . A . H10 H 0.7416 0.2202 0.9419 0.053 Uiso 1 1 calc R . . C11 C 0.5510(17) 0.0573(11) 0.9148(4) 0.048(3) Uani 1 1 d . . . H11 H 0.6539 -0.0158 0.9101 0.057 Uiso 1 1 calc R A . C12 C 0.511(2) 0.4651(13) 0.9576(4) 0.049(3) Uani 1 1 d . A . C13 C 0.781(2) 0.6390(10) 0.9700(4) 0.073(4) Uani 1 1 d . . . H13A H 0.9313 0.6439 0.9680 0.109 Uiso 1 1 calc R . . H13B H 0.7376 0.6617 1.0043 0.109 Uiso 1 1 calc R . . H13C H 0.7213 0.7112 0.9468 0.109 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 Ag 0.0339(3) 0.0427(4) 0.0851(5) -0.0122(5) 0.0022(6) -0.0038(5) O1 0.041(3) 0.046(4) 0.063(4) -0.013(3) 0.016(4) -0.008(5) O2 0.073(6) 0.047(5) 0.146(8) -0.046(5) -0.013(6) 0.008(5) O3 0.054(6) 0.048(5) 0.082(6) -0.020(5) 0.002(5) -0.013(5) O4 0.044(14) 0.056(11) 0.086(14) 0.021(10) 0.033(15) -0.001(12) O4' 0.03(2) 0.16(5) 0.11(3) 0.00(3) 0.03(2) -0.02(2) O5 0.049(12) 0.071(14) 0.082(13) 0.002(13) 0.051(12) 0.021(9) O5' 0.026(14) 0.045(16) 0.14(3) 0.06(2) 0.017(17) 0.009(13) O6 0.101(10) 0.009(6) 0.048(7) -0.005(5) 0.032(9) 0.002(8) N1 0.034(4) 0.020(4) 0.056(4) -0.006(5) 0.013(7) -0.001(5) N2 0.030(4) 0.025(5) 0.059(6) 0.000(4) -0.003(5) -0.002(4) N3 0.025(3) 0.031(4) 0.057(4) -0.017(4) 0.009(5) -0.003(6) N4 0.073(8) 0.027(5) 0.056(6) -0.014(5) 0.002(7) 0.009(8) C1 0.036(5) 0.057(7) 0.082(9) -0.004(6) 0.012(8) -0.002(8) C2 0.046(5) 0.027(4) 0.060(7) -0.012(5) 0.000(7) -0.009(6) C3 0.041(6) 0.028(5) 0.057(6) 0.001(6) -0.013(8) -0.016(5) C4 0.031(5) 0.020(4) 0.047(6) -0.010(4) -0.011(6) 0.010(6) C5 0.031(5) 0.040(6) 0.034(6) 0.000(5) 0.004(5) -0.010(5) C6 0.032(6) 0.031(6) 0.043(6) -0.007(5) 0.007(5) -0.008(5) C7 0.038(6) 0.046(6) 0.055(7) -0.010(6) 0.021(6) 0.002(6) C8 0.057(7) 0.041(6) 0.057(7) -0.019(6) 0.010(6) 0.018(7) C9 0.036(6) 0.031(5) 0.034(5) -0.012(5) 0.007(4) -0.006(6) C10 0.038(5) 0.035(5) 0.060(6) -0.025(6) 0.004(6) -0.013(8) C11 0.039(8) 0.037(6) 0.067(7) -0.013(6) 0.001(6) 0.010(6) C12 0.068(9) 0.037(7) 0.044(7) -0.010(6) -0.009(7) 0.002(7) C13 0.097(9) 0.030(6) 0.091(9) 0.002(6) -0.015(8) -0.025(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.274(8) . ? Ag O5' 2.35(2) . ? Ag N2 2.356(8) 1_655 ? Ag O4 2.49(2) . ? Ag O1 2.522(6) 1_655 ? O1 C5 1.221(11) . ? O1 Ag 2.522(6) 1_455 ? O2 C12 1.204(13) . ? O3 C12 1.299(13) . ? O3 C13 1.449(11) . ? O4 N4 1.15(3) . ? O4' N4 1.33(5) . ? O5 N4 1.28(2) . ? O5' N4 1.18(3) . ? O6 N4 1.264(14) . ? O6' N4 1.19(3) . ? N1 C4 1.310(13) . ? N1 C1 1.351(11) . ? N2 C4 1.314(13) . ? N2 C3 1.361(10) . ? N2 Ag 2.356(8) 1_455 ? N3 C5 1.363(11) . ? N3 C4 1.398(9) . ? N3 H3A 0.8600 . ? C1 C2 1.348(14) . ? C1 H1 0.9300 . ? C2 C3 1.338(13) . ? C2 H2 0.9300 . ? C3 H3B 0.9300 . ? C5 C6 1.503(13) . ? C6 C7 1.365(12) . ? C6 C11 1.408(14) . ? C7 C8 1.382(13) . ? C7 H7 0.9300 . ? C8 C9 1.391(14) . ? C8 H8 0.9300 . ? C9 C10 1.373(13) . ? C9 C12 1.510(14) . ? C10 C11 1.384(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag O5' 95.9(8) . . ? N1 Ag N2 124.3(2) . 1_655 ? O5' Ag N2 139.0(8) . 1_655 ? N1 Ag O4 130.3(7) . . ? O5' Ag O4 40.1(9) . . ? N2 Ag O4 104.2(7) 1_655 . ? N1 Ag O1 126.2(3) . 1_655 ? O5' Ag O1 80.7(10) . 1_655 ? N2 Ag O1 69.7(2) 1_655 1_655 ? O4 Ag O1 77.7(9) . 1_655 ? C5 O1 Ag 114.6(6) . 1_455 ? C12 O3 C13 116.2(10) . . ? N4 O4 Ag 110.5(15) . . ? N4 O5' Ag 118.0(18) . . ? C4 N1 C1 116.7(9) . . ? C4 N1 Ag 129.7(6) . . ? C1 N1 Ag 113.6(8) . . ? C4 N2 C3 115.3(8) . . ? C4 N2 Ag 122.4(6) . 1_455 ? C3 N2 Ag 116.2(7) . 1_455 ? C5 N3 C4 129.1(9) . . ? C5 N3 H3A 115.5 . . ? C4 N3 H3A 115.5 . . ? O4 N4 O5' 91.2(18) . . ? O4 N4 O6' 148(2) . . ? O5' N4 O6' 120(2) . . ? O4 N4 O6 120.1(17) . . ? O5' N4 O6 146.9(19) . . ? O6' N4 O6 32.5(14) . . ? O4 N4 O5 123.8(17) . . ? O5' N4 O5 32.8(11) . . ? O6' N4 O5 88(2) . . ? O6 N4 O5 114.5(15) . . ? O4 N4 O4' 27(3) . . ? O5' N4 O4' 116(3) . . ? O6' N4 O4' 122(3) . . ? O6 N4 O4' 97(3) . . ? O5 N4 O4' 149(3) . . ? C2 C1 N1 121.0(11) . . ? C2 C1 H1 119.5 . . ? N1 C1 H1 119.5 . . ? C3 C2 C1 118.3(8) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 N2 122.1(9) . . ? C2 C3 H3B 118.9 . . ? N2 C3 H3B 118.9 . . ? N1 C4 N2 126.3(7) . . ? N1 C4 N3 115.1(9) . . ? N2 C4 N3 118.6(10) . . ? O1 C5 N3 124.1(9) . . ? O1 C5 C6 119.8(9) . . ? N3 C5 C6 116.0(8) . . ? C7 C6 C11 118.5(10) . . ? C7 C6 C5 119.6(9) . . ? C11 C6 C5 121.8(9) . . ? C6 C7 C8 122.9(11) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C9 117.9(11) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 120.7(9) . . ? C10 C9 C12 120.6(9) . . ? C8 C9 C12 118.6(9) . . ? C9 C10 C11 120.7(10) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C6 119.3(11) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? O2 C12 O3 125.6(11) . . ? O2 C12 C9 121.8(11) . . ? O3 C12 C9 112.7(10) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.492 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.105 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 809207' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 Ag2 Cl N5 O9' _chemical_formula_weight 631.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5500(10) _cell_length_b 10.0750(11) _cell_length_c 12.7547(17) _cell_angle_alpha 89.399(10) _cell_angle_beta 80.098(11) _cell_angle_gamma 71.088(10) _cell_volume 903.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 5.20 _cell_measurement_theta_max 12.42 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.379 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7897 _exptl_absorpt_correction_T_max 0.9477 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3959 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3171 _reflns_number_gt 2591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.5883P] 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 3171 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 2.00686(6) -0.34263(4) 0.91519(3) 0.05055(13) Uani 1 1 d . . . Ag2 Ag 1.47860(6) 0.30062(3) 0.83946(3) 0.05198(13) Uani 1 1 d . . . Cl Cl 1.69538(18) -0.17424(13) 0.53764(9) 0.0480(3) Uani 1 1 d . . . O1 O 1.7513(5) -0.1669(3) 1.0474(2) 0.0475(8) Uani 1 1 d . . . O2 O 1.8214(6) 0.1528(4) 1.5105(3) 0.0621(10) Uani 1 1 d . . . O3 O 1.7313(6) 0.3593(4) 1.4371(3) 0.0659(11) Uani 1 1 d . . . O4 O 1.806(4) -0.491(4) 0.977(2) 0.068(7) Uani 0.50 1 d P . . O4' O 1.752(4) -0.466(3) 0.975(2) 0.060(6) Uani 0.50 1 d P . . O5 O 1.797(5) -0.681(4) 0.945(3) 0.049(5) Uani 0.50 1 d P . . O5' O 1.763(5) -0.687(3) 0.931(3) 0.060(7) Uani 0.50 1 d P . . O6 O 1.5963(6) -0.5080(4) 0.8737(3) 0.0682(11) Uani 1 1 d . . . O7 O 1.2053(6) 0.4631(4) 0.7997(3) 0.0603(10) Uani 1 1 d . . . O8 O 1.2973(6) 0.3139(4) 0.6683(3) 0.0695(12) Uani 1 1 d . . . O9 O 1.0119(7) 0.4609(4) 0.6959(4) 0.0950(17) Uani 1 1 d . . . N1 N 1.8131(5) -0.1643(3) 0.8266(3) 0.0341(8) Uani 1 1 d . . . N2 N 1.6464(5) 0.0705(3) 0.7893(3) 0.0317(7) Uani 1 1 d . . . N3 N 1.7442(5) 0.0246(3) 0.9516(3) 0.0310(7) Uani 1 1 d . . . H3A H 1.7462 0.1093 0.9551 0.037 Uiso 1 1 calc R . . N4 N 1.7188(6) -0.5557(4) 0.9280(3) 0.0409(9) Uani 1 1 d . . . N5 N 1.1687(6) 0.4118(4) 0.7193(3) 0.0468(10) Uani 1 1 d . . . C1 C 1.7966(6) -0.2074(4) 0.7304(3) 0.0382(10) Uani 1 1 d . . . H1 H 1.8456 -0.3027 0.7105 0.046 Uiso 1 1 calc R . . C2 C 1.7094(6) -0.1147(4) 0.6609(3) 0.0343(9) Uani 1 1 d . . . C3 C 1.6356(6) 0.0259(4) 0.6924(3) 0.0348(9) Uani 1 1 d . . . H3B H 1.5776 0.0907 0.6460 0.042 Uiso 1 1 calc R . . C4 C 1.7351(5) -0.0275(4) 0.8518(3) 0.0288(8) Uani 1 1 d . . . C5 C 1.7504(6) -0.0462(4) 1.0440(3) 0.0315(9) Uani 1 1 d . . . C6 C 1.7585(6) 0.0318(4) 1.1409(3) 0.0305(9) Uani 1 1 d . . . C7 C 1.6750(6) 0.1766(4) 1.1595(3) 0.0332(9) Uani 1 1 d . . . H7 H 1.6157 0.2310 1.1081 0.040 Uiso 1 1 calc R . . C8 C 1.6800(6) 0.2400(4) 1.2549(3) 0.0357(9) Uani 1 1 d . . . H8 H 1.6241 0.3366 1.2673 0.043 Uiso 1 1 calc R . . C9 C 1.7686(6) 0.1586(5) 1.3310(3) 0.0352(9) Uani 1 1 d . . . C10 C 1.8512(6) 0.0147(5) 1.3138(3) 0.0379(10) Uani 1 1 d . . . H10 H 1.9097 -0.0392 1.3657 0.045 Uiso 1 1 calc R . . C11 C 1.8467(6) -0.0493(4) 1.2188(3) 0.0378(10) Uani 1 1 d . . . H11 H 1.9023 -0.1460 1.2071 0.045 Uiso 1 1 calc R . . C12 C 1.7765(6) 0.2215(5) 1.4363(3) 0.0401(10) Uani 1 1 d . . . C13 C 1.7397(11) 0.4267(6) 1.5350(5) 0.081(2) Uani 1 1 d . . . H13A H 1.7022 0.5265 1.5280 0.121 Uiso 1 1 calc R . . H13B H 1.8673 0.3929 1.5490 0.121 Uiso 1 1 calc R . . H13C H 1.6551 0.4054 1.5928 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 0.0525(2) 0.03467(19) 0.0556(2) -0.00384(15) -0.01771(18) 0.00214(16) Ag2 0.0637(3) 0.03072(19) 0.0626(3) -0.00167(16) -0.0324(2) -0.00607(17) Cl 0.0578(7) 0.0538(7) 0.0334(5) -0.0090(5) -0.0119(5) -0.0176(6) O1 0.074(2) 0.0314(16) 0.0368(17) 0.0013(13) 0.0007(16) -0.0221(16) O2 0.088(3) 0.066(2) 0.0378(18) 0.0095(17) -0.0251(18) -0.026(2) O3 0.107(3) 0.051(2) 0.048(2) -0.0018(16) -0.034(2) -0.025(2) O4 0.073(16) 0.099(13) 0.066(9) 0.018(8) -0.037(10) -0.062(12) O4' 0.060(13) 0.091(12) 0.047(8) -0.031(9) 0.002(8) -0.052(10) O5 0.041(6) 0.057(9) 0.055(8) 0.014(6) -0.022(5) -0.018(5) O5' 0.073(18) 0.029(6) 0.073(13) 0.008(6) -0.013(10) -0.011(9) O6 0.069(3) 0.064(2) 0.066(2) 0.0057(19) -0.037(2) -0.001(2) O7 0.074(2) 0.0459(19) 0.052(2) -0.0153(16) -0.0296(18) 0.0033(17) O8 0.090(3) 0.046(2) 0.053(2) -0.0174(17) -0.023(2) 0.010(2) O9 0.079(3) 0.062(3) 0.147(5) -0.015(3) -0.073(3) -0.001(2) N1 0.039(2) 0.0290(17) 0.0327(18) -0.0021(14) -0.0100(15) -0.0063(15) N2 0.0356(19) 0.0263(16) 0.0314(18) 0.0009(13) -0.0069(15) -0.0071(14) N3 0.0401(19) 0.0248(16) 0.0308(17) 0.0004(13) -0.0104(15) -0.0121(14) N4 0.047(2) 0.042(2) 0.038(2) 0.0017(18) -0.0108(18) -0.0192(19) N5 0.056(3) 0.0300(19) 0.055(2) -0.0030(17) -0.027(2) -0.0049(18) C1 0.041(2) 0.031(2) 0.040(2) -0.0078(18) -0.0058(19) -0.0086(18) C2 0.032(2) 0.040(2) 0.032(2) -0.0039(17) -0.0071(17) -0.0127(18) C3 0.035(2) 0.037(2) 0.032(2) 0.0030(17) -0.0077(18) -0.0106(18) C4 0.030(2) 0.0296(19) 0.029(2) 0.0003(16) -0.0081(16) -0.0110(16) C5 0.029(2) 0.028(2) 0.033(2) -0.0015(16) -0.0005(17) -0.0062(16) C6 0.030(2) 0.032(2) 0.030(2) 0.0035(16) -0.0030(17) -0.0120(17) C7 0.037(2) 0.033(2) 0.029(2) 0.0028(16) -0.0093(17) -0.0094(18) C8 0.038(2) 0.029(2) 0.038(2) -0.0032(17) -0.0045(19) -0.0090(18) C9 0.034(2) 0.045(2) 0.029(2) 0.0015(18) -0.0048(17) -0.0178(19) C10 0.043(3) 0.042(2) 0.031(2) 0.0080(18) -0.0103(19) -0.015(2) C11 0.040(2) 0.033(2) 0.037(2) 0.0042(18) -0.0070(19) -0.0072(19) C12 0.039(2) 0.052(3) 0.033(2) 0.000(2) -0.0080(19) -0.018(2) C13 0.123(6) 0.063(4) 0.063(4) -0.019(3) -0.040(4) -0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.338(3) . ? Ag1 O7 2.376(3) 1_645 ? Ag1 O4 2.40(3) 2_947 ? Ag1 O4 2.49(3) . ? Ag1 O1 2.536(3) . ? Ag1 O5 2.57(3) 2_947 ? Ag2 N2 2.288(3) . ? Ag2 O7 2.312(3) . ? Ag2 O6 2.442(4) 1_565 ? Cl C2 1.721(4) . ? O1 C5 1.214(5) . ? O2 C12 1.197(6) . ? O3 C12 1.317(6) . ? O3 C13 1.447(6) . ? O4 N4 1.30(3) . ? O4 Ag1 2.40(3) 2_947 ? O4' N4 1.21(3) . ? O5 N4 1.24(4) . ? O5 Ag1 2.57(3) 2_947 ? O5' N4 1.25(3) . ? O6 N4 1.221(5) . ? O6 Ag2 2.442(4) 1_545 ? O7 N5 1.264(5) . ? O7 Ag1 2.376(3) 1_465 ? O8 N5 1.230(5) . ? O9 N5 1.215(5) . ? N1 C4 1.329(5) . ? N1 C1 1.345(5) . ? N2 C4 1.340(5) . ? N2 C3 1.344(5) . ? N3 C5 1.371(5) . ? N3 C4 1.403(5) . ? N3 H3A 0.8600 . ? C1 C2 1.369(6) . ? C1 H1 0.9300 . ? C2 C3 1.379(6) . ? C3 H3B 0.9300 . ? C5 C6 1.493(5) . ? C6 C7 1.393(6) . ? C6 C11 1.399(6) . ? C7 C8 1.392(6) . ? C7 H7 0.9300 . ? C8 C9 1.384(6) . ? C8 H8 0.9300 . ? C9 C10 1.383(6) . ? C9 C12 1.509(6) . ? C10 C11 1.389(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O7 112.98(12) . 1_645 ? N1 Ag1 O4 174.0(7) . 2_947 ? O7 Ag1 O4 73.0(7) 1_645 2_947 ? N1 Ag1 O4 104.0(7) . . ? O7 Ag1 O4 87.0(7) 1_645 . ? O4 Ag1 O4 76.5(10) 2_947 . ? N1 Ag1 O1 69.28(11) . . ? O7 Ag1 O1 168.07(13) 1_645 . ? O4 Ag1 O1 105.0(7) 2_947 . ? O4 Ag1 O1 81.1(7) . . ? N1 Ag1 O5 128.1(9) . 2_947 ? O7 Ag1 O5 105.8(9) 1_645 2_947 ? O4 Ag1 O5 47.2(11) 2_947 2_947 ? O4 Ag1 O5 111.3(11) . 2_947 ? O1 Ag1 O5 79.8(9) . 2_947 ? N2 Ag2 O7 135.05(12) . . ? N2 Ag2 O6 129.12(13) . 1_565 ? O7 Ag2 O6 89.51(13) . 1_565 ? C5 O1 Ag1 116.3(3) . . ? C12 O3 C13 115.9(4) . . ? N4 O4 Ag1 107(2) . 2_947 ? N4 O4 Ag1 133(2) . . ? Ag1 O4 Ag1 103.5(10) 2_947 . ? N4 O5 Ag1 100.8(18) . 2_947 ? N4 O6 Ag2 106.0(3) . 1_545 ? N5 O7 Ag2 106.2(3) . . ? N5 O7 Ag1 128.5(3) . 1_465 ? Ag2 O7 Ag1 123.94(14) . 1_465 ? C4 N1 C1 116.4(4) . . ? C4 N1 Ag1 130.1(3) . . ? C1 N1 Ag1 113.1(3) . . ? C4 N2 C3 116.7(3) . . ? C4 N2 Ag2 126.1(3) . . ? C3 N2 Ag2 116.6(3) . . ? C5 N3 C4 126.4(3) . . ? C5 N3 H3A 116.8 . . ? C4 N3 H3A 116.8 . . ? O4' N4 O6 112.8(15) . . ? O4' N4 O5 119(2) . . ? O6 N4 O5 127.5(13) . . ? O4' N4 O5' 135(2) . . ? O6 N4 O5' 111.3(13) . . ? O5 N4 O5' 16(2) . . ? O4' N4 O4 18(3) . . ? O6 N4 O4 129.2(15) . . ? O5 N4 O4 103(2) . . ? O5' N4 O4 119.5(19) . . ? O9 N5 O8 123.6(4) . . ? O9 N5 O7 119.3(4) . . ? O8 N5 O7 117.1(4) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 118.2(4) . . ? C1 C2 Cl 120.1(3) . . ? C3 C2 Cl 121.7(3) . . ? N2 C3 C2 120.9(4) . . ? N2 C3 H3B 119.5 . . ? C2 C3 H3B 119.5 . . ? N1 C4 N2 126.0(4) . . ? N1 C4 N3 119.5(3) . . ? N2 C4 N3 114.5(3) . . ? O1 C5 N3 122.1(4) . . ? O1 C5 C6 121.2(4) . . ? N3 C5 C6 116.7(3) . . ? C7 C6 C11 119.6(4) . . ? C7 C6 C5 123.8(4) . . ? C11 C6 C5 116.5(4) . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 C12 117.3(4) . . ? C8 C9 C12 122.0(4) . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C6 120.0(4) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? O2 C12 O3 123.9(4) . . ? O2 C12 C9 123.3(4) . . ? O3 C12 C9 112.8(4) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.747 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.093 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 809208' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 Ag2 Br N5 O9' _chemical_formula_weight 675.91 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5949(9) _cell_length_b 10.1026(14) _cell_length_c 12.8377(16) _cell_angle_alpha 89.295(10) _cell_angle_beta 79.941(11) _cell_angle_gamma 70.855(10) _cell_volume 915.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.82 _cell_measurement_theta_max 11.92 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 4.385 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8377 _exptl_absorpt_correction_T_max 0.9941 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4003 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3211 _reflns_number_gt 2161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.9316P] 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 3211 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.50812(8) 0.65699(5) 0.41882(5) 0.05328(19) Uani 1 1 d . . . Ag2 Ag -0.01993(9) 1.29996(5) 0.34077(5) 0.0547(2) Uani 1 1 d . . . Br Br 0.20275(10) 0.81567(7) 0.03151(5) 0.0448(2) Uani 1 1 d . . . O1 O 0.2540(7) 0.8326(4) 0.5501(3) 0.0504(13) Uani 1 1 d . . . O2 O 0.3189(8) 1.1500(5) 1.0094(4) 0.0622(15) Uani 1 1 d . . . O3 O 0.2314(8) 1.3563(5) 0.9369(4) 0.0631(15) Uani 1 1 d . . . O4' O 0.292(5) 0.504(3) 0.476(3) 0.061(8) Uani 0.50 1 d P . . O4 O 0.258(6) 0.547(3) 0.473(3) 0.077(12) Uani 0.50 1 d P . . O5 O 0.280(4) 0.327(3) 0.4545(17) 0.037(4) Uani 0.50 1 d P . . O5' O 0.278(5) 0.305(3) 0.4225(17) 0.051(6) Uani 0.50 1 d P . . O6 O 0.0952(8) 0.4933(5) 0.3733(4) 0.0691(16) Uani 1 1 d . . . O7 O -0.2959(8) 1.4629(5) 0.3019(4) 0.0645(15) Uani 1 1 d . . . O8 O -0.4816(9) 1.4570(6) 0.1958(6) 0.091(2) Uani 1 1 d . . . O9 O -0.1955(8) 1.3122(5) 0.1718(4) 0.0640(15) Uani 1 1 d . . . N1 N 0.3127(7) 0.8351(5) 0.3314(4) 0.0352(13) Uani 1 1 d . . . N2 N 0.1496(7) 1.0690(5) 0.2917(4) 0.0336(12) Uani 1 1 d . . . N3 N 0.2434(7) 1.0250(5) 0.4542(4) 0.0321(12) Uani 1 1 d . . . H3A H 0.2429 1.1100 0.4580 0.038 Uiso 1 1 calc R . . N4 N 0.2157(9) 0.4450(7) 0.4283(4) 0.0430(14) Uani 1 1 d . . . N5 N -0.3277(9) 1.4110(6) 0.2212(5) 0.0496(16) Uani 1 1 d . . . C1 C 0.2995(9) 0.7904(6) 0.2356(5) 0.0383(16) Uani 1 1 d . . . H1 H 0.3494 0.6951 0.2165 0.046 Uiso 1 1 calc R . . C2 C 0.2136(8) 0.8828(6) 0.1651(5) 0.0328(15) Uani 1 1 d . . . C3 C 0.1387(9) 1.0239(6) 0.1964(5) 0.0351(15) Uani 1 1 d . . . H3B H 0.0799 1.0883 0.1504 0.042 Uiso 1 1 calc R . . C4 C 0.2349(8) 0.9726(6) 0.3561(4) 0.0301(14) Uani 1 1 d . . . C5 C 0.2525(8) 0.9524(6) 0.5458(5) 0.0325(15) Uani 1 1 d . . . C6 C 0.2595(8) 1.0316(6) 0.6423(4) 0.0320(15) Uani 1 1 d . . . C7 C 0.1776(9) 1.1759(6) 0.6605(5) 0.0355(15) Uani 1 1 d . . . H7 H 0.1197 1.2304 0.6091 0.043 Uiso 1 1 calc R . . C8 C 0.1816(9) 1.2395(6) 0.7553(5) 0.0390(16) Uani 1 1 d . . . H8 H 0.1248 1.3359 0.7681 0.047 Uiso 1 1 calc R . . C9 C 0.2718(8) 1.1568(6) 0.8307(5) 0.0339(15) Uani 1 1 d . . . C10 C 0.3554(9) 1.0144(6) 0.8116(5) 0.0360(15) Uani 1 1 d . . . H10 H 0.4159 0.9603 0.8623 0.043 Uiso 1 1 calc R . . C11 C 0.3506(9) 0.9511(6) 0.7186(5) 0.0374(16) Uani 1 1 d . . . H11 H 0.4080 0.8546 0.7065 0.045 Uiso 1 1 calc R . . C12 C 0.2769(10) 1.2181(7) 0.9360(5) 0.0418(16) Uani 1 1 d . . . C13 C 0.2349(14) 1.4223(8) 1.0366(6) 0.080(3) Uani 1 1 d . . . H13A H 0.2006 1.5219 1.0301 0.120 Uiso 1 1 calc R . . H13B H 0.3601 1.3862 1.0530 0.120 Uiso 1 1 calc R . . H13C H 0.1465 1.4021 1.0922 0.120 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 0.0551(4) 0.0362(3) 0.0587(4) -0.0054(2) -0.0194(3) 0.0030(3) Ag2 0.0672(4) 0.0309(3) 0.0659(4) -0.0040(3) -0.0327(3) -0.0053(3) Br 0.0524(5) 0.0465(4) 0.0348(4) -0.0081(3) -0.0103(3) -0.0139(3) O1 0.080(4) 0.031(3) 0.039(3) -0.004(2) 0.000(3) -0.022(2) O2 0.087(4) 0.064(3) 0.042(3) 0.007(3) -0.026(3) -0.025(3) O3 0.097(4) 0.042(3) 0.057(3) -0.005(2) -0.033(3) -0.022(3) O4' 0.095(17) 0.050(15) 0.074(14) 0.011(11) -0.049(14) -0.056(14) O4 0.104(18) 0.07(2) 0.064(16) -0.040(15) 0.017(14) -0.056(16) O5 0.059(9) 0.028(9) 0.024(12) -0.015(8) -0.013(10) -0.011(7) O5' 0.097(12) 0.033(10) 0.019(12) -0.012(7) -0.002(10) -0.018(8) O6 0.072(4) 0.066(4) 0.062(4) 0.006(3) -0.037(3) -0.001(3) O7 0.076(4) 0.045(3) 0.059(3) -0.024(2) -0.026(3) 0.005(3) O8 0.064(4) 0.065(4) 0.146(6) -0.015(4) -0.066(4) 0.002(3) O9 0.074(4) 0.047(3) 0.053(3) -0.020(2) -0.022(3) 0.010(3) N1 0.041(3) 0.024(3) 0.038(3) -0.004(2) -0.013(3) -0.004(2) N2 0.037(3) 0.024(3) 0.036(3) -0.003(2) -0.007(3) -0.005(2) N3 0.044(3) 0.026(3) 0.030(3) -0.001(2) -0.011(3) -0.014(2) N4 0.051(4) 0.046(4) 0.036(3) 0.000(3) -0.007(3) -0.021(3) N5 0.058(4) 0.032(3) 0.056(4) -0.003(3) -0.023(4) -0.004(3) C1 0.041(4) 0.031(3) 0.040(4) -0.006(3) -0.008(3) -0.008(3) C2 0.032(4) 0.037(3) 0.029(3) -0.005(3) -0.007(3) -0.010(3) C3 0.037(4) 0.034(3) 0.035(4) 0.007(3) -0.012(3) -0.010(3) C4 0.026(3) 0.032(3) 0.032(4) 0.002(3) -0.008(3) -0.009(3) C5 0.024(4) 0.033(4) 0.035(4) -0.004(3) 0.002(3) -0.006(3) C6 0.027(3) 0.033(3) 0.031(3) 0.001(3) -0.004(3) -0.003(3) C7 0.043(4) 0.031(3) 0.031(3) 0.003(3) -0.005(3) -0.011(3) C8 0.037(4) 0.031(3) 0.045(4) -0.006(3) -0.006(3) -0.007(3) C9 0.025(4) 0.043(4) 0.031(3) 0.001(3) -0.004(3) -0.008(3) C10 0.035(4) 0.038(4) 0.033(4) 0.002(3) -0.007(3) -0.009(3) C11 0.043(4) 0.031(3) 0.033(4) -0.001(3) -0.003(3) -0.007(3) C12 0.042(4) 0.044(4) 0.042(4) 0.004(3) -0.010(3) -0.017(3) C13 0.112(8) 0.057(5) 0.074(6) -0.022(4) -0.039(6) -0.020(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 N1 2.341(5) . ? Ag1 O7 2.386(4) 1_645 ? Ag1 O4' 2.41(3) 2_666 ? Ag1 O4 2.50(4) . ? Ag1 O5 2.52(2) 2_666 ? Ag1 O1 2.531(4) . ? Ag2 N2 2.299(4) . ? Ag2 O7 2.331(5) . ? Ag2 O6 2.454(6) 1_565 ? Br C2 1.876(6) . ? O1 C5 1.207(7) . ? O2 C12 1.187(7) . ? O3 C12 1.324(8) . ? O3 C13 1.458(8) . ? O4' N4 1.19(3) . ? O4' Ag1 2.41(3) 2_666 ? O4 N4 1.34(3) . ? O5 N4 1.20(3) . ? O5 Ag1 2.52(2) 2_666 ? O5' N4 1.33(3) . ? O6 N4 1.224(7) . ? O6 Ag2 2.454(6) 1_545 ? O7 N5 1.261(7) . ? O7 Ag1 2.386(4) 1_465 ? O8 N5 1.209(7) . ? O9 N5 1.242(7) . ? N1 C4 1.337(7) . ? N1 C1 1.347(7) . ? N2 C3 1.335(7) . ? N2 C4 1.343(7) . ? N3 C5 1.378(7) . ? N3 C4 1.392(7) . ? N3 H3A 0.8600 . ? C1 C2 1.379(8) . ? C1 H1 0.9300 . ? C2 C3 1.386(8) . ? C3 H3B 0.9300 . ? C5 C6 1.501(8) . ? C6 C7 1.389(8) . ? C6 C11 1.396(8) . ? C7 C8 1.393(8) . ? C7 H7 0.9300 . ? C8 C9 1.392(8) . ? C8 H8 0.9300 . ? C9 C10 1.374(8) . ? C9 C12 1.505(9) . ? C10 C11 1.373(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O7 112.42(17) . 1_645 ? N1 Ag1 O4' 172.9(7) . 2_666 ? O7 Ag1 O4' 73.9(9) 1_645 2_666 ? N1 Ag1 O4 93.2(9) . . ? O7 Ag1 O4 93.2(8) 1_645 . ? O4' Ag1 O4 89.8(12) 2_666 . ? N1 Ag1 O5 129.5(7) . 2_666 ? O7 Ag1 O5 103.1(6) 1_645 2_666 ? O4' Ag1 O5 43.9(10) 2_666 2_666 ? O4 Ag1 O5 120.1(11) . 2_666 ? N1 Ag1 O1 69.06(16) . . ? O7 Ag1 O1 167.92(18) 1_645 . ? O4' Ag1 O1 105.6(9) 2_666 . ? O4 Ag1 O1 74.7(8) . . ? O5 Ag1 O1 83.5(6) 2_666 . ? N2 Ag2 O7 135.27(17) . . ? N2 Ag2 O6 129.26(18) . 1_565 ? O7 Ag2 O6 89.29(18) . 1_565 ? C5 O1 Ag1 116.1(4) . . ? C12 O3 C13 115.1(6) . . ? N4 O4' Ag1 111(2) . 2_666 ? N4 O4 Ag1 133(2) . . ? N4 O5 Ag1 104.1(13) . 2_666 ? N4 O6 Ag2 105.0(4) . 1_545 ? N5 O7 Ag2 105.2(4) . . ? N5 O7 Ag1 130.4(4) . 1_465 ? Ag2 O7 Ag1 123.2(2) . 1_465 ? C4 N1 C1 117.0(5) . . ? C4 N1 Ag1 130.2(4) . . ? C1 N1 Ag1 112.3(4) . . ? C3 N2 C4 117.7(5) . . ? C3 N2 Ag2 116.5(4) . . ? C4 N2 Ag2 125.1(4) . . ? C5 N3 C4 125.7(5) . . ? C5 N3 H3A 117.2 . . ? C4 N3 H3A 117.2 . . ? O4' N4 O5 101(2) . . ? O4' N4 O6 129.5(17) . . ? O5 N4 O6 129.2(12) . . ? O4' N4 O5' 118(2) . . ? O5 N4 O5' 20.6(14) . . ? O6 N4 O5' 111.8(13) . . ? O4' N4 O4 18(3) . . ? O5 N4 O4 118.9(19) . . ? O6 N4 O4 111.3(17) . . ? O5' N4 O4 137(2) . . ? O8 N5 O9 123.2(6) . . ? O8 N5 O7 120.0(6) . . ? O9 N5 O7 116.8(6) . . ? N1 C1 C2 121.5(5) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 117.8(5) . . ? C1 C2 Br 119.9(4) . . ? C3 C2 Br 122.3(4) . . ? N2 C3 C2 121.1(5) . . ? N2 C3 H3B 119.5 . . ? C2 C3 H3B 119.5 . . ? N1 C4 N2 124.9(5) . . ? N1 C4 N3 119.6(5) . . ? N2 C4 N3 115.4(5) . . ? O1 C5 N3 123.1(6) . . ? O1 C5 C6 120.9(6) . . ? N3 C5 C6 116.0(5) . . ? C7 C6 C11 119.4(5) . . ? C7 C6 C5 124.4(5) . . ? C11 C6 C5 116.2(5) . . ? C6 C7 C8 120.4(6) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 119.1(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 120.3(6) . . ? C10 C9 C12 117.7(5) . . ? C8 C9 C12 121.9(5) . . ? C11 C10 C9 120.8(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C6 119.9(6) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? O2 C12 O3 123.8(6) . . ? O2 C12 C9 123.8(6) . . ? O3 C12 C9 112.3(6) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.734 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.110 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 809209' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H10 Ag I N4 O6' _chemical_formula_weight 553.02 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4597(7) _cell_length_b 8.0105(6) _cell_length_c 13.5106(10) _cell_angle_alpha 88.204(7) _cell_angle_beta 86.411(8) _cell_angle_gamma 80.948(8) _cell_volume 795.53(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 6.01 _cell_measurement_theta_max 13.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.248 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7948 _exptl_absorpt_correction_T_max 0.9533 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3482 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2781 _reflns_number_gt 2602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+2.0979P] 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 2781 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 1.29310(6) 1.42819(4) 1.12683(3) 0.04940(12) Uani 1 1 d . . . I I 1.24231(4) 1.16767(3) 1.006665(19) 0.03570(10) Uani 1 1 d . . . O1 O 1.1735(4) 0.4155(4) 1.2958(2) 0.0496(8) Uani 1 1 d . . . O2 O 0.3711(4) 0.1865(4) 1.5756(3) 0.0477(8) Uani 1 1 d . . . O3 O 0.6189(4) 0.0559(4) 1.6465(2) 0.0486(8) Uani 1 1 d . . . O4 O 1.6252(6) 1.3090(5) 1.1376(3) 0.0666(11) Uani 1 1 d . . . O5 O 1.8547(5) 1.4392(5) 1.1150(4) 0.0759(12) Uani 1 1 d . . . O6 O 1.596(3) 1.585(2) 1.1309(9) 0.067(3) Uani 0.60 1 d P . . O6' O 1.577(3) 1.554(3) 1.0877(17) 0.097(9) Uani 0.40 1 d P . . N1 N 1.1622(5) 0.7044(4) 1.1618(2) 0.0325(7) Uani 1 1 d . . . N2 N 0.9544(5) 0.6502(4) 1.2944(3) 0.0338(7) Uani 1 1 d . . . H2A H 0.8502 0.6904 1.3220 0.041 Uiso 1 1 calc R . . N3 N 0.9604(5) 0.9231(4) 1.2446(3) 0.0393(8) Uani 1 1 d . . . N4 N 1.6905(6) 1.4412(5) 1.1216(3) 0.0460(9) Uani 1 1 d . . . C1 C 1.0330(5) 0.7612(5) 1.2301(3) 0.0313(8) Uani 1 1 d . . . C2 C 1.0195(6) 1.0371(5) 1.1826(3) 0.0388(9) Uani 1 1 d . . . H2B H 0.9707 1.1507 1.1892 0.047 Uiso 1 1 calc R . . C3 C 1.1526(5) 0.9902(5) 1.1081(3) 0.0297(8) Uani 1 1 d . . . C4 C 1.2219(5) 0.8213(5) 1.1006(3) 0.0326(8) Uani 1 1 d . . . H4 H 1.3125 0.7873 1.0517 0.039 Uiso 1 1 calc R . . C5 C 1.0200(6) 0.4853(5) 1.3198(3) 0.0346(9) Uani 1 1 d . . . C6 C 0.8918(6) 0.3963(5) 1.3824(3) 0.0321(8) Uani 1 1 d . . . C7 C 0.9639(6) 0.2783(5) 1.4534(3) 0.0381(9) Uani 1 1 d . . . H7 H 1.0891 0.2542 1.4586 0.046 Uiso 1 1 calc R . . C8 C 0.8504(6) 0.1973(5) 1.5159(3) 0.0346(9) Uani 1 1 d . . . H8 H 0.8990 0.1205 1.5639 0.041 Uiso 1 1 calc R . . C9 C 0.6628(6) 0.2306(5) 1.5072(3) 0.0322(8) Uani 1 1 d . . . C10 C 0.5918(6) 0.3431(5) 1.4342(3) 0.0350(9) Uani 1 1 d . . . H10 H 0.4671 0.3624 1.4266 0.042 Uiso 1 1 calc R . . C11 C 0.7051(6) 0.4268(5) 1.3729(3) 0.0354(9) Uani 1 1 d . . . H11 H 0.6563 0.5037 1.3250 0.042 Uiso 1 1 calc R . . C12 C 0.5337(6) 0.1561(5) 1.5781(3) 0.0339(9) Uani 1 1 d . . . C13 C 0.5049(7) -0.0186(7) 1.7207(4) 0.0529(13) Uani 1 1 d . . . H13A H 0.5802 -0.0890 1.7655 0.079 Uiso 1 1 calc R . . H13B H 0.4304 -0.0856 1.6888 0.079 Uiso 1 1 calc R . . H13C H 0.4287 0.0695 1.7570 0.079 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 Ag 0.0625(3) 0.03049(19) 0.0532(2) -0.00162(15) 0.01857(18) -0.00958(16) I 0.04036(17) 0.03185(15) 0.03652(16) 0.00798(11) 0.00037(11) -0.01340(11) O1 0.0423(18) 0.0488(19) 0.0499(19) 0.0198(15) 0.0142(15) 0.0059(15) O2 0.0364(18) 0.0509(19) 0.055(2) 0.0177(15) 0.0052(14) -0.0099(14) O3 0.0434(18) 0.058(2) 0.0442(18) 0.0249(15) 0.0027(14) -0.0160(15) O4 0.069(3) 0.053(2) 0.081(3) 0.005(2) 0.005(2) -0.0263(19) O5 0.048(2) 0.066(3) 0.113(4) 0.012(2) 0.005(2) -0.0123(19) O6 0.065(6) 0.048(5) 0.079(8) 0.021(5) 0.015(6) 0.012(4) O6' 0.040(8) 0.091(17) 0.14(2) 0.077(16) 0.032(12) 0.016(9) N1 0.0351(18) 0.0273(17) 0.0346(18) 0.0035(13) 0.0040(14) -0.0066(14) N2 0.0311(17) 0.0307(18) 0.0381(18) 0.0065(14) 0.0113(14) -0.0063(14) N3 0.042(2) 0.0301(18) 0.044(2) 0.0037(15) 0.0092(16) -0.0041(15) N4 0.048(2) 0.046(2) 0.041(2) 0.0101(17) 0.0095(17) -0.0068(19) C1 0.033(2) 0.029(2) 0.034(2) 0.0040(16) 0.0006(16) -0.0090(16) C2 0.043(2) 0.027(2) 0.045(2) 0.0042(17) 0.0060(19) -0.0057(17) C3 0.031(2) 0.0283(19) 0.031(2) 0.0061(15) -0.0022(15) -0.0107(15) C4 0.033(2) 0.029(2) 0.036(2) 0.0035(16) 0.0055(16) -0.0076(16) C5 0.036(2) 0.034(2) 0.032(2) 0.0046(16) 0.0046(17) -0.0057(17) C6 0.039(2) 0.0282(19) 0.030(2) 0.0017(15) 0.0040(16) -0.0083(16) C7 0.035(2) 0.038(2) 0.041(2) 0.0070(18) 0.0017(18) -0.0064(18) C8 0.041(2) 0.031(2) 0.031(2) 0.0074(16) 0.0016(17) -0.0067(17) C9 0.037(2) 0.0275(19) 0.032(2) 0.0030(15) 0.0044(16) -0.0080(16) C10 0.034(2) 0.034(2) 0.037(2) 0.0035(17) -0.0002(17) -0.0065(17) C11 0.042(2) 0.031(2) 0.032(2) 0.0065(16) -0.0012(17) -0.0055(17) C12 0.041(2) 0.029(2) 0.033(2) 0.0020(16) 0.0020(17) -0.0093(17) C13 0.055(3) 0.064(3) 0.043(3) 0.025(2) 0.001(2) -0.024(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 Ag N1 2.324(3) 1_565 ? Ag O1 2.404(3) 1_565 ? Ag O6' 2.51(2) . ? Ag O4 2.523(4) . ? Ag I 2.7700(5) . ? I C3 2.100(4) . ? O1 C5 1.222(5) . ? O1 Ag 2.404(3) 1_545 ? O2 C12 1.201(5) . ? O3 C12 1.331(5) . ? O3 C13 1.449(5) . ? O4 N4 1.240(5) . ? O5 N4 1.220(6) . ? O6 O6' 0.67(3) . ? O6 N4 1.258(17) . ? O6' N4 1.24(2) . ? N1 C1 1.328(5) . ? N1 C4 1.341(5) . ? N1 Ag 2.324(3) 1_545 ? N2 C5 1.375(5) . ? N2 C1 1.393(5) . ? N2 H2A 0.8600 . ? N3 C2 1.328(5) . ? N3 C1 1.340(5) . ? C2 C3 1.386(6) . ? C2 H2B 0.9300 . ? C3 C4 1.374(6) . ? C4 H4 0.9300 . ? C5 C6 1.487(5) . ? C6 C11 1.389(6) . ? C6 C7 1.397(6) . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.395(6) . ? C8 H8 0.9300 . ? C9 C10 1.387(6) . ? C9 C12 1.493(5) . ? C10 C11 1.381(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag O1 75.25(11) 1_565 1_565 ? N1 Ag O6' 84.4(6) 1_565 . ? O1 Ag O6' 119.5(6) 1_565 . ? N1 Ag O4 125.37(12) 1_565 . ? O1 Ag O4 103.44(13) 1_565 . ? O6' Ag O4 47.9(6) . . ? N1 Ag I 139.32(9) 1_565 . ? O1 Ag I 116.44(9) 1_565 . ? O6' Ag I 115.8(6) . . ? O4 Ag I 91.28(10) . . ? C3 I Ag 103.11(11) . . ? C5 O1 Ag 120.8(3) . 1_545 ? C12 O3 C13 116.5(4) . . ? N4 O4 Ag 98.9(3) . . ? O6' O6 N4 73(3) . . ? O6 O6' N4 76(3) . . ? O6 O6' Ag 105(4) . . ? N4 O6' Ag 99.8(14) . . ? C1 N1 C4 116.2(3) . . ? C1 N1 Ag 129.6(3) . 1_545 ? C4 N1 Ag 114.2(3) . 1_545 ? C5 N2 C1 129.1(3) . . ? C5 N2 H2A 115.5 . . ? C1 N2 H2A 115.5 . . ? C2 N3 C1 116.7(4) . . ? O5 N4 O6' 124.9(12) . . ? O5 N4 O4 121.0(4) . . ? O6' N4 O4 111.1(13) . . ? O5 N4 O6 115.4(10) . . ? O6' N4 O6 31.2(14) . . ? O4 N4 O6 122.1(10) . . ? N1 C1 N3 126.3(4) . . ? N1 C1 N2 121.0(4) . . ? N3 C1 N2 112.6(3) . . ? N3 C2 C3 121.3(4) . . ? N3 C2 H2B 119.4 . . ? C3 C2 H2B 119.4 . . ? C4 C3 C2 117.8(4) . . ? C4 C3 I 120.4(3) . . ? C2 C3 I 121.8(3) . . ? N1 C4 C3 121.7(4) . . ? N1 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? O1 C5 N2 123.5(4) . . ? O1 C5 C6 121.2(4) . . ? N2 C5 C6 115.2(3) . . ? C11 C6 C7 119.4(4) . . ? C11 C6 C5 122.6(4) . . ? C7 C6 C5 118.1(4) . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 C12 118.4(4) . . ? C8 C9 C12 121.9(4) . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C6 120.2(4) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? O2 C12 O3 123.6(4) . . ? O2 C12 C9 124.1(4) . . ? O3 C12 C9 112.3(4) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.385 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.101 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 809210' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag B Br F4 N3 O3.50' _chemical_formula_weight 566.88 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.106(3) _cell_length_b 10.7290(18) _cell_length_c 13.434(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.41(2) _cell_angle_gamma 90.00 _cell_volume 1812.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.46 _cell_measurement_theta_max 11.63 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 3.383 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8154 _exptl_absorpt_correction_T_max 0.9958 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4051 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3189 _reflns_number_gt 1841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+2.5381P] 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 3189 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.2500 0.41629(9) 0.2500 0.0430(3) Uani 1 2 d S . . Ag2 Ag -0.2500 0.34923(9) 0.2500 0.0426(3) Uani 1 2 d S . . Br Br -0.09935(7) 0.72856(9) 0.00008(7) 0.0552(3) Uani 1 1 d . . . O1 O 0.1563(4) 0.2475(5) 0.3093(4) 0.0484(15) Uani 1 1 d . . . O2 O 0.1319(5) -0.1571(6) 0.7123(4) 0.0601(17) Uani 1 1 d . . . O3 O 0.0848(5) 0.0082(6) 0.7913(4) 0.0594(17) Uani 1 1 d . . . O4 O 0.2500 -0.2269(18) 0.2500 0.191(7) Uani 1 2 d S . . N1 N 0.0730(4) 0.4762(6) 0.2123(5) 0.0337(16) Uani 1 1 d . . . N2 N -0.1019(5) 0.4842(6) 0.2334(5) 0.0375(16) Uani 1 1 d . . . N3 N 0.0267(5) 0.3647(6) 0.3454(4) 0.0353(16) Uani 1 1 d . . . H3A H -0.0084 0.3744 0.3902 0.042 Uiso 1 1 calc R . . C1 C 0.0416(6) 0.5596(7) 0.1343(6) 0.039(2) Uani 1 1 d . . . H1 H 0.0892 0.5828 0.0977 0.046 Uiso 1 1 calc R . . C2 C -0.0583(6) 0.6111(7) 0.1073(5) 0.035(2) Uani 1 1 d . . . C3 C -0.1288(6) 0.5691(8) 0.1581(6) 0.042(2) Uani 1 1 d . . . H3B H -0.1977 0.6009 0.1394 0.051 Uiso 1 1 calc R . . C4 C 0.0003(6) 0.4451(7) 0.2597(5) 0.031(2) Uani 1 1 d . . . C5 C 0.1023(6) 0.2719(8) 0.3660(6) 0.0352(19) Uani 1 1 d . . . C6 C 0.1096(6) 0.1977(8) 0.4629(6) 0.0346(19) Uani 1 1 d . . . C7 C 0.0855(6) 0.2429(8) 0.5489(6) 0.045(2) Uani 1 1 d . . . H7 H 0.0657 0.3259 0.5506 0.054 Uiso 1 1 calc R . . C8 C 0.0901(6) 0.1671(8) 0.6332(6) 0.045(2) Uani 1 1 d . . . H8 H 0.0747 0.1998 0.6914 0.054 Uiso 1 1 calc R . . C9 C 0.1175(6) 0.0425(8) 0.6312(6) 0.040(2) Uani 1 1 d . . . C10 C 0.1420(6) -0.0022(9) 0.5454(7) 0.046(2) Uani 1 1 d . . . H10 H 0.1618 -0.0852 0.5437 0.056 Uiso 1 1 calc R . . C11 C 0.1378(6) 0.0745(8) 0.4599(6) 0.048(2) Uani 1 1 d . . . H11 H 0.1539 0.0425 0.4018 0.058 Uiso 1 1 calc R . . C12 C 0.1134(6) -0.0461(9) 0.7148(7) 0.048(2) Uani 1 1 d . . . C13 C 0.0730(8) -0.0732(10) 0.8736(7) 0.076(3) Uani 1 1 d . . . H13A H 0.0527 -0.0248 0.9250 0.114 Uiso 1 1 calc R . . H13B H 0.1394 -0.1144 0.9050 0.114 Uiso 1 1 calc R . . H13C H 0.0192 -0.1344 0.8452 0.114 Uiso 1 1 calc R . . C14 C 0.1654(12) -0.1389(12) 0.1853(13) 0.160(8) Uani 1 1 d . . . H14A H 0.1563 -0.1522 0.1119 0.191 Uiso 1 1 calc R . . H14B H 0.0977 -0.1532 0.1995 0.191 Uiso 1 1 calc R . . C15 C 0.1991(7) -0.0238(11) 0.2120(9) 0.085(4) Uani 1 1 d . . . H15A H 0.1480 0.0191 0.2397 0.102 Uiso 1 1 calc R . . H15B H 0.2042 0.0211 0.1509 0.102 Uiso 1 1 calc R . . B B 0.3122(9) 0.6143(10) 0.0192(8) 0.048(3) Uani 1 1 d . . . F1 F 0.3653(4) 0.5634(6) -0.0483(4) 0.0804(18) Uani 1 1 d . . . F2 F 0.2403(6) 0.6970(6) -0.0368(5) 0.115(2) Uani 1 1 d . . . F3 F 0.3841(5) 0.6683(6) 0.1015(4) 0.0871(19) Uani 1 1 d . . . F4 F 0.2599(4) 0.5210(5) 0.0543(4) 0.0648(15) 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 0.0289(5) 0.0527(6) 0.0510(6) 0.000 0.0174(4) 0.000 Ag2 0.0372(5) 0.0445(6) 0.0485(5) 0.000 0.0159(4) 0.000 Br 0.0571(6) 0.0525(6) 0.0531(5) 0.0186(5) 0.0111(4) -0.0014(5) O1 0.049(4) 0.047(4) 0.060(4) 0.007(3) 0.032(3) 0.008(3) O2 0.062(4) 0.041(4) 0.074(4) 0.018(4) 0.014(3) 0.009(4) O3 0.076(5) 0.050(4) 0.055(4) 0.016(4) 0.023(3) 0.004(4) O4 0.21(2) 0.161(17) 0.211(18) 0.000 0.074(16) 0.000 N1 0.026(3) 0.041(4) 0.038(4) 0.001(3) 0.015(3) -0.002(3) N2 0.030(4) 0.047(4) 0.039(4) 0.007(4) 0.016(3) 0.003(4) N3 0.033(4) 0.043(4) 0.034(4) 0.005(3) 0.016(3) 0.002(4) C1 0.039(5) 0.045(6) 0.032(4) -0.003(4) 0.010(4) -0.013(5) C2 0.037(5) 0.038(5) 0.031(4) 0.003(4) 0.011(4) 0.000(4) C3 0.040(5) 0.046(6) 0.038(5) 0.001(4) 0.005(4) -0.001(5) C4 0.036(4) 0.033(5) 0.025(4) -0.006(4) 0.011(4) -0.002(4) C5 0.034(5) 0.031(5) 0.042(5) 0.000(4) 0.014(4) -0.013(4) C6 0.027(4) 0.033(5) 0.046(5) 0.004(4) 0.012(4) -0.001(4) C7 0.048(5) 0.041(6) 0.047(5) 0.014(5) 0.016(4) 0.003(5) C8 0.049(5) 0.048(6) 0.037(5) 0.007(5) 0.010(4) 0.002(5) C9 0.028(4) 0.041(6) 0.052(5) 0.013(5) 0.011(4) -0.003(4) C10 0.035(5) 0.041(5) 0.062(6) 0.009(5) 0.013(4) 0.006(4) C11 0.049(5) 0.047(6) 0.051(5) 0.009(5) 0.017(4) 0.013(5) C12 0.030(5) 0.049(7) 0.058(6) 0.012(5) -0.001(4) 0.008(5) C13 0.084(8) 0.085(8) 0.061(6) 0.037(6) 0.025(6) 0.004(6) C14 0.120(13) 0.058(10) 0.239(19) -0.018(11) -0.051(12) 0.009(9) C15 0.060(7) 0.071(8) 0.115(10) 0.028(7) 0.011(6) 0.001(6) B 0.053(7) 0.050(8) 0.039(6) -0.004(5) 0.008(6) -0.010(6) F1 0.087(4) 0.098(5) 0.074(3) -0.016(3) 0.052(3) -0.016(4) F2 0.133(6) 0.076(5) 0.122(5) 0.023(4) 0.011(5) 0.044(5) F3 0.087(4) 0.105(5) 0.074(4) -0.025(4) 0.031(3) -0.044(4) F4 0.061(3) 0.077(4) 0.060(3) 0.012(3) 0.022(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.321(6) 2 ? Ag1 N1 2.321(6) . ? Ag1 O1 2.445(5) . ? Ag1 O1 2.445(5) 2 ? Ag2 N2 2.481(6) 2_455 ? Ag2 N2 2.481(6) . ? Ag2 O2 2.542(6) 4 ? Ag2 O2 2.542(6) 3_556 ? Br C2 1.875(7) . ? O1 C5 1.206(8) . ? O2 C12 1.217(10) . ? O2 Ag2 2.542(6) 3_556 ? O3 C12 1.324(10) . ? O3 C13 1.451(9) . ? O4 C14 1.527(15) 2 ? O4 C14 1.527(15) . ? N1 C4 1.329(9) . ? N1 C1 1.350(9) . ? N2 C3 1.333(9) . ? N2 C4 1.353(9) . ? N3 C5 1.377(10) . ? N3 C4 1.402(9) . ? N3 H3A 0.8600 . ? C1 C2 1.372(10) . ? C1 H1 0.9300 . ? C2 C3 1.371(10) . ? C3 H3B 0.9300 . ? C5 C6 1.506(10) . ? C6 C7 1.370(10) . ? C6 C11 1.376(11) . ? C7 C8 1.381(10) . ? C7 H7 0.9300 . ? C8 C9 1.387(11) . ? C8 H8 0.9300 . ? C9 C10 1.368(11) . ? C9 C12 1.483(11) . ? C10 C11 1.401(11) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.326(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C15 1.432(18) 2 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? B F2 1.357(12) . ? B F3 1.363(11) . ? B F4 1.371(11) . ? B F1 1.400(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 147.8(3) 2 . ? N1 Ag1 O1 134.2(2) 2 . ? N1 Ag1 O1 73.3(2) . . ? N1 Ag1 O1 73.3(2) 2 2 ? N1 Ag1 O1 134.2(2) . 2 ? O1 Ag1 O1 84.4(3) . 2 ? N2 Ag2 N2 108.6(3) 2_455 . ? N2 Ag2 O2 92.5(2) 2_455 4 ? N2 Ag2 O2 154.59(19) . 4 ? N2 Ag2 O2 154.59(19) 2_455 3_556 ? N2 Ag2 O2 92.5(2) . 3_556 ? O2 Ag2 O2 71.6(3) 4 3_556 ? C5 O1 Ag1 118.9(5) . . ? C12 O2 Ag2 154.5(6) . 3_556 ? C12 O3 C13 116.2(8) . . ? C14 O4 C14 103.6(16) 2 . ? C4 N1 C1 115.8(6) . . ? C4 N1 Ag1 129.3(5) . . ? C1 N1 Ag1 114.8(5) . . ? C3 N2 C4 116.1(6) . . ? C3 N2 Ag2 114.9(5) . . ? C4 N2 Ag2 122.6(5) . . ? C5 N3 C4 127.3(6) . . ? C5 N3 H3A 116.3 . . ? C4 N3 H3A 116.3 . . ? N1 C1 C2 122.1(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 117.6(7) . . ? C3 C2 Br 121.1(6) . . ? C1 C2 Br 121.3(6) . . ? N2 C3 C2 122.1(7) . . ? N2 C3 H3B 118.9 . . ? C2 C3 H3B 118.9 . . ? N1 C4 N2 126.1(7) . . ? N1 C4 N3 120.3(7) . . ? N2 C4 N3 113.6(6) . . ? O1 C5 N3 123.2(7) . . ? O1 C5 C6 121.8(8) . . ? N3 C5 C6 115.0(7) . . ? C7 C6 C11 119.5(7) . . ? C7 C6 C5 124.6(8) . . ? C11 C6 C5 115.7(7) . . ? C6 C7 C8 121.0(8) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C9 120.2(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 118.5(8) . . ? C10 C9 C12 118.8(8) . . ? C8 C9 C12 122.5(8) . . ? C9 C10 C11 121.4(8) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C6 C11 C10 119.2(8) . . ? C6 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? O2 C12 O3 123.6(9) . . ? O2 C12 C9 123.8(9) . . ? O3 C12 C9 112.6(8) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 O4 106.8(13) . . ? C15 C14 H14A 110.4 . . ? O4 C14 H14A 110.4 . . ? C15 C14 H14B 110.4 . . ? O4 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C14 C15 C15 111.4(7) . 2 ? C14 C15 H15A 109.4 . . ? C15 C15 H15A 109.4 2 . ? C14 C15 H15B 109.4 . . ? C15 C15 H15B 109.4 2 . ? H15A C15 H15B 108.0 . . ? F2 B F3 112.6(9) . . ? F2 B F4 109.3(9) . . ? F3 B F4 109.3(8) . . ? F2 B F1 106.9(8) . . ? F3 B F1 109.6(8) . . ? F4 B F1 109.1(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.874 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.127 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 809211' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Ag2 B2 F8 I4 N12 O14' _chemical_formula_weight 1986.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8556(12) _cell_length_b 10.8736(14) _cell_length_c 15.375(2) _cell_angle_alpha 92.219(9) _cell_angle_beta 95.523(9) _cell_angle_gamma 94.117(10) _cell_volume 1634.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.15 _cell_measurement_theta_max 12.39 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 2.583 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8024 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6737 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5668 _reflns_number_gt 3824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.6032P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5668 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag -0.07931(6) 0.54799(5) 0.19357(3) 0.04104(17) Uani 1 1 d . . . I1 I -0.20346(5) 0.36779(5) -0.18275(3) 0.04821(17) Uani 1 1 d . . . I2 I -0.24528(6) 0.51705(5) 0.55669(3) 0.05061(17) Uani 1 1 d . . . O1 O -0.3225(5) 0.5831(5) 0.2304(3) 0.0485(13) Uani 1 1 d . . . O2 O -0.6693(7) 1.1126(5) 0.3855(4) 0.0682(18) Uani 1 1 d . . . O3 O -0.6944(6) 0.9618(4) 0.4789(3) 0.0499(14) Uani 1 1 d . . . O4 O -0.0287(6) 0.3408(5) 0.1385(3) 0.0564(15) Uani 1 1 d . . . O5 O 0.4056(7) -0.1449(7) 0.0330(4) 0.082(2) Uani 1 1 d . . . O6 O 0.2860(5) -0.1024(5) -0.0908(3) 0.0515(14) Uani 1 1 d . . . O7 O -0.6080(9) 1.3259(8) 0.3011(5) 0.088(3) Uani 1 1 d . . . H7B H -0.649(12) 1.271(10) 0.318(7) 0.09(5) Uiso 1 1 d . . . N1 N -0.2296(6) 0.5544(5) 0.0659(3) 0.0378(14) Uani 1 1 d . . . N2 N -0.3988(7) 0.6352(6) -0.0323(4) 0.0499(17) Uani 1 1 d . . . N3 N -0.3813(6) 0.6957(5) 0.1132(3) 0.0394(15) Uani 1 1 d . . . H3A H -0.4217 0.7599 0.0973 0.047 Uiso 1 1 calc R . . N4 N -0.0941(6) 0.4169(5) 0.3114(3) 0.0384(14) Uani 1 1 d . . . N5 N -0.0764(7) 0.2410(5) 0.3982(4) 0.0496(17) Uani 1 1 d . . . N6 N -0.0123(6) 0.2296(5) 0.2604(4) 0.0430(15) Uani 1 1 d . . . H6 H 0.0099 0.1583 0.2766 0.052 Uiso 1 1 calc R . . C1 C -0.1956(8) 0.4836(7) -0.0007(4) 0.0412(18) Uani 1 1 d . . . H1 H -0.1270 0.4302 0.0101 0.049 Uiso 1 1 calc R . . C2 C -0.2584(7) 0.4866(7) -0.0846(4) 0.0392(17) Uani 1 1 d . . . C3 C -0.3592(8) 0.5672(7) -0.0981(5) 0.050(2) Uani 1 1 d . . . H3B H -0.4007 0.5744 -0.1545 0.060 Uiso 1 1 calc R . . C4 C -0.3328(7) 0.6249(6) 0.0471(4) 0.0334(16) Uani 1 1 d . . . C5 C -0.3719(7) 0.6747(7) 0.2007(4) 0.0402(18) Uani 1 1 d . . . C6 C -0.4297(7) 0.7678(6) 0.2575(4) 0.0350(17) Uani 1 1 d . . . C7 C -0.4351(8) 0.8894(7) 0.2386(5) 0.0454(19) Uani 1 1 d . . . H7 H -0.3951 0.9192 0.1904 0.054 Uiso 1 1 calc R . . C8 C -0.5003(8) 0.9686(7) 0.2914(5) 0.047(2) Uani 1 1 d . . . H8 H -0.5021 1.0514 0.2786 0.056 Uiso 1 1 calc R . . C9 C -0.5620(7) 0.9265(7) 0.3620(4) 0.0389(17) Uani 1 1 d . . . C10 C -0.5490(8) 0.8047(7) 0.3844(4) 0.0423(18) Uani 1 1 d . . . H10 H -0.5852 0.7757 0.4341 0.051 Uiso 1 1 calc R . . C11 C -0.4825(8) 0.7273(7) 0.3329(4) 0.0450(19) Uani 1 1 d . . . H11 H -0.4726 0.6465 0.3487 0.054 Uiso 1 1 calc R . . C12 C -0.6453(8) 1.0111(7) 0.4093(5) 0.0421(18) Uani 1 1 d . . . C13 C -0.7865(9) 1.0372(8) 0.5234(5) 0.060(2) Uani 1 1 d . . . H13A H -0.8169 0.9946 0.5724 0.091 Uiso 1 1 calc R . . H13B H -0.8640 1.0517 0.4834 0.091 Uiso 1 1 calc R . . H13C H -0.7388 1.1147 0.5436 0.091 Uiso 1 1 calc R . . C14 C -0.1420(7) 0.4753(7) 0.3796(5) 0.0435(19) Uani 1 1 d . . . H14 H -0.1627 0.5569 0.3742 0.052 Uiso 1 1 calc R . . C15 C -0.1618(7) 0.4211(7) 0.4563(5) 0.0414(18) Uani 1 1 d . . . C16 C -0.1266(9) 0.3020(7) 0.4631(5) 0.053(2) Uani 1 1 d . . . H16 H -0.1380 0.2625 0.5148 0.063 Uiso 1 1 calc R . . C17 C -0.0650(7) 0.3000(6) 0.3245(4) 0.0380(17) Uani 1 1 d . . . C18 C 0.0107(8) 0.2531(7) 0.1761(4) 0.0392(17) Uani 1 1 d . . . C19 C 0.0885(7) 0.1597(6) 0.1301(4) 0.0352(16) Uani 1 1 d . . . C20 C 0.1682(8) 0.0777(7) 0.1749(4) 0.048(2) Uani 1 1 d . . . H20 H 0.1742 0.0778 0.2356 0.057 Uiso 1 1 calc R . . C21 C 0.2382(9) -0.0035(7) 0.1288(5) 0.052(2) Uani 1 1 d . . . H21 H 0.2868 -0.0617 0.1587 0.062 Uiso 1 1 calc R . . C22 C 0.2378(7) -0.0003(6) 0.0391(5) 0.0386(17) Uani 1 1 d . . . C23 C 0.1589(7) 0.0836(6) -0.0062(4) 0.0386(18) Uani 1 1 d . . . H23 H 0.1547 0.0846 -0.0669 0.046 Uiso 1 1 calc R . . C24 C 0.0878(8) 0.1642(6) 0.0394(4) 0.0404(18) Uani 1 1 d . . . H24 H 0.0388 0.2223 0.0096 0.048 Uiso 1 1 calc R . . C25 C 0.3193(9) -0.0897(7) -0.0055(5) 0.047(2) Uani 1 1 d . . . C26 C 0.3589(9) -0.1920(8) -0.1367(5) 0.063(2) Uani 1 1 d . . . H26A H 0.3269 -0.1960 -0.1978 0.094 Uiso 1 1 calc R . . H26B H 0.3430 -0.2717 -0.1131 0.094 Uiso 1 1 calc R . . H26C H 0.4551 -0.1677 -0.1294 0.094 Uiso 1 1 calc R . . C27 C -0.4745(10) 1.3448(9) 0.3400(6) 0.074(3) Uani 1 1 d . . . H27A H -0.4222 1.2793 0.3211 0.110 Uiso 1 1 calc R . . H27B H -0.4746 1.3456 0.4024 0.110 Uiso 1 1 calc R . . H27C H -0.4345 1.4223 0.3233 0.110 Uiso 1 1 calc R . . B B -0.0198(11) 0.8448(8) 0.2951(6) 0.051(3) Uani 1 1 d . . . F1 F -0.0758(6) 0.8046(5) 0.2122(3) 0.0849(17) Uani 1 1 d . . . F2 F -0.0836(7) 0.7771(5) 0.3545(4) 0.0949(19) Uani 1 1 d . . . F3 F -0.0382(6) 0.9679(4) 0.3092(4) 0.0902(19) Uani 1 1 d . . . F4 F 0.1171(5) 0.8285(6) 0.3023(4) 0.0873(18) 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 Ag 0.0486(4) 0.0406(3) 0.0363(3) 0.0010(2) 0.0071(3) 0.0159(3) I1 0.0478(3) 0.0555(3) 0.0414(3) -0.0182(2) 0.0116(2) 0.0061(3) I2 0.0556(4) 0.0583(4) 0.0394(3) -0.0099(2) 0.0142(2) 0.0082(3) O1 0.061(4) 0.051(3) 0.041(3) 0.012(2) 0.020(3) 0.026(3) O2 0.104(5) 0.040(3) 0.070(4) 0.007(3) 0.042(4) 0.024(3) O3 0.065(4) 0.045(3) 0.046(3) -0.003(2) 0.034(3) 0.009(3) O4 0.091(5) 0.046(3) 0.037(3) 0.004(2) 0.010(3) 0.033(3) O5 0.092(5) 0.112(5) 0.055(4) 0.011(4) 0.013(3) 0.080(5) O6 0.061(4) 0.055(3) 0.043(3) -0.003(2) 0.014(3) 0.025(3) O7 0.093(6) 0.083(6) 0.082(5) 0.027(4) -0.021(4) -0.013(5) N1 0.039(4) 0.048(4) 0.029(3) -0.007(3) 0.003(3) 0.022(3) N2 0.063(5) 0.061(4) 0.028(3) 0.000(3) 0.001(3) 0.031(4) N3 0.049(4) 0.039(3) 0.033(3) -0.001(3) 0.008(3) 0.022(3) N4 0.045(4) 0.038(4) 0.036(3) 0.003(3) 0.008(3) 0.012(3) N5 0.076(5) 0.038(4) 0.040(4) 0.010(3) 0.021(3) 0.015(3) N6 0.054(4) 0.033(3) 0.046(4) 0.005(3) 0.015(3) 0.018(3) C1 0.044(5) 0.045(4) 0.037(4) 0.001(3) 0.005(3) 0.018(4) C2 0.040(4) 0.042(4) 0.034(4) -0.010(3) 0.006(3) 0.000(4) C3 0.055(5) 0.064(5) 0.035(4) 0.002(4) 0.006(4) 0.028(4) C4 0.039(4) 0.032(4) 0.031(4) -0.001(3) 0.009(3) 0.005(3) C5 0.042(4) 0.053(5) 0.032(4) 0.007(3) 0.016(3) 0.020(4) C6 0.033(4) 0.040(4) 0.035(4) -0.005(3) 0.009(3) 0.013(3) C7 0.060(5) 0.038(4) 0.044(4) 0.000(3) 0.028(4) 0.012(4) C8 0.068(6) 0.032(4) 0.044(4) 0.002(3) 0.020(4) 0.009(4) C9 0.045(5) 0.038(4) 0.035(4) -0.008(3) 0.015(3) 0.004(3) C10 0.048(5) 0.050(5) 0.032(4) -0.001(3) 0.017(3) 0.006(4) C11 0.058(5) 0.040(4) 0.039(4) 0.009(3) 0.012(4) 0.008(4) C12 0.045(5) 0.045(5) 0.036(4) -0.008(3) 0.011(3) 0.000(4) C13 0.066(6) 0.061(6) 0.060(5) -0.008(4) 0.033(5) 0.015(5) C14 0.048(5) 0.038(4) 0.047(4) -0.004(3) 0.010(4) 0.021(4) C15 0.035(4) 0.050(5) 0.039(4) -0.010(3) 0.002(3) 0.012(4) C16 0.078(6) 0.052(5) 0.033(4) 0.008(4) 0.021(4) 0.011(5) C17 0.046(5) 0.029(4) 0.039(4) -0.005(3) 0.006(3) 0.009(3) C18 0.047(5) 0.034(4) 0.036(4) 0.000(3) 0.000(3) 0.006(4) C19 0.037(4) 0.029(4) 0.039(4) -0.003(3) 0.005(3) 0.007(3) C20 0.058(5) 0.064(5) 0.028(4) 0.007(3) 0.007(3) 0.045(4) C21 0.068(6) 0.047(5) 0.045(5) 0.013(4) 0.011(4) 0.035(4) C22 0.039(4) 0.039(4) 0.042(4) 0.006(3) 0.014(3) 0.014(3) C23 0.047(5) 0.043(4) 0.028(4) 0.006(3) 0.007(3) 0.013(4) C24 0.052(5) 0.035(4) 0.037(4) 0.004(3) 0.009(4) 0.015(4) C25 0.059(5) 0.039(4) 0.048(5) 0.010(4) 0.022(4) 0.019(4) C26 0.073(6) 0.065(6) 0.056(5) -0.010(4) 0.026(5) 0.017(5) C27 0.066(7) 0.075(7) 0.080(7) -0.005(5) 0.014(6) 0.001(5) B 0.067(7) 0.037(5) 0.053(6) -0.004(4) 0.018(5) 0.025(5) F1 0.094(4) 0.089(4) 0.070(3) -0.011(3) -0.011(3) 0.026(3) F2 0.116(5) 0.068(4) 0.108(5) 0.027(3) 0.041(4) 0.009(3) F3 0.133(5) 0.042(3) 0.108(4) -0.003(3) 0.072(4) 0.018(3) F4 0.061(4) 0.113(5) 0.086(4) -0.031(3) -0.002(3) 0.026(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 Ag N1 2.349(5) . ? Ag N4 2.357(5) . ? Ag O4 2.477(5) . ? Ag O1 2.566(5) . ? Ag I1 2.8927(9) 2_565 ? I1 C2 2.084(6) . ? I1 Ag 2.8926(9) 2_565 ? I2 C15 2.096(7) . ? O1 C5 1.225(8) . ? O2 C12 1.208(9) . ? O3 C12 1.332(9) . ? O3 C13 1.465(8) . ? O4 C18 1.204(8) . ? O5 C25 1.199(9) . ? O6 C25 1.320(9) . ? O6 C26 1.452(8) . ? O7 C27 1.390(12) . ? O7 H7B 0.76(10) . ? N1 C4 1.334(8) . ? N1 C1 1.340(8) . ? N2 C3 1.335(9) . ? N2 C4 1.339(8) . ? N3 C5 1.369(8) . ? N3 C4 1.394(8) . ? N3 H3A 0.8600 . ? N4 C17 1.341(8) . ? N4 C14 1.347(8) . ? N5 C16 1.331(9) . ? N5 C17 1.333(9) . ? N6 C18 1.367(9) . ? N6 C17 1.388(8) . ? N6 H6 0.8600 . ? C1 C2 1.379(9) . ? C1 H1 0.9300 . ? C2 C3 1.377(10) . ? C3 H3B 0.9300 . ? C5 C6 1.490(9) . ? C6 C7 1.368(10) . ? C6 C11 1.390(9) . ? C7 C8 1.392(9) . ? C7 H7 0.9300 . ? C8 C9 1.372(10) . ? C8 H8 0.9300 . ? C9 C10 1.393(10) . ? C9 C12 1.491(9) . ? C10 C11 1.377(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.362(10) . ? C14 H14 0.9300 . ? C15 C16 1.370(10) . ? C16 H16 0.9300 . ? C18 C19 1.509(9) . ? C19 C20 1.389(9) . ? C19 C24 1.398(9) . ? C20 C21 1.375(9) . ? C20 H20 0.9300 . ? C21 C22 1.382(10) . ? C21 H21 0.9300 . ? C22 C23 1.403(9) . ? C22 C25 1.492(9) . ? C23 C24 1.373(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? B F2 1.367(11) . ? B F4 1.368(11) . ? B F3 1.376(10) . ? B F1 1.381(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N4 128.9(2) . . ? N1 Ag O4 86.75(18) . . ? N4 Ag O4 73.64(18) . . ? N1 Ag O1 68.86(17) . . ? N4 Ag O1 80.31(17) . . ? O4 Ag O1 119.13(19) . . ? N1 Ag I1 116.96(15) . 2_565 ? N4 Ag I1 109.53(15) . 2_565 ? O4 Ag I1 88.91(15) . 2_565 ? O1 Ag I1 151.94(12) . 2_565 ? C2 I1 Ag 102.0(2) . 2_565 ? C5 O1 Ag 116.1(4) . . ? C12 O3 C13 115.2(6) . . ? C18 O4 Ag 131.4(5) . . ? C25 O6 C26 115.4(6) . . ? C27 O7 H7B 114(9) . . ? C4 N1 C1 115.8(6) . . ? C4 N1 Ag 130.7(4) . . ? C1 N1 Ag 113.2(4) . . ? C3 N2 C4 117.0(6) . . ? C5 N3 C4 127.3(6) . . ? C5 N3 H3A 116.3 . . ? C4 N3 H3A 116.3 . . ? C17 N4 C14 114.9(6) . . ? C17 N4 Ag 134.2(4) . . ? C14 N4 Ag 110.9(4) . . ? C16 N5 C17 117.0(6) . . ? C18 N6 C17 131.6(6) . . ? C18 N6 H6 114.2 . . ? C17 N6 H6 114.2 . . ? N1 C1 C2 122.7(6) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 116.9(6) . . ? C3 C2 I1 123.3(5) . . ? C1 C2 I1 119.7(5) . . ? N2 C3 C2 121.6(7) . . ? N2 C3 H3B 119.2 . . ? C2 C3 H3B 119.2 . . ? N1 C4 N2 125.8(6) . . ? N1 C4 N3 120.0(6) . . ? N2 C4 N3 114.2(6) . . ? O1 C5 N3 122.1(6) . . ? O1 C5 C6 121.9(6) . . ? N3 C5 C6 116.0(6) . . ? C7 C6 C11 118.8(6) . . ? C7 C6 C5 123.6(6) . . ? C11 C6 C5 117.5(6) . . ? C6 C7 C8 120.1(7) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 121.1(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 118.7(6) . . ? C8 C9 C12 118.7(7) . . ? C10 C9 C12 122.5(6) . . ? C11 C10 C9 119.8(7) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C6 121.1(7) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? O2 C12 O3 123.3(7) . . ? O2 C12 C9 123.5(7) . . ? O3 C12 C9 113.1(7) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 123.5(7) . . ? N4 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C14 C15 C16 116.8(6) . . ? C14 C15 I2 120.6(5) . . ? C16 C15 I2 122.6(6) . . ? N5 C16 C15 122.1(7) . . ? N5 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? N5 C17 N4 125.8(6) . . ? N5 C17 N6 113.0(6) . . ? N4 C17 N6 121.1(6) . . ? O4 C18 N6 123.8(6) . . ? O4 C18 C19 120.4(6) . . ? N6 C18 C19 115.9(6) . . ? C20 C19 C24 119.5(6) . . ? C20 C19 C18 122.7(6) . . ? C24 C19 C18 117.6(6) . . ? C21 C20 C19 119.6(6) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 121.3(7) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 C25 117.8(6) . . ? C23 C22 C25 123.0(6) . . ? C24 C23 C22 119.7(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.6(6) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? O5 C25 O6 123.8(7) . . ? O5 C25 C22 122.9(7) . . ? O6 C25 C22 113.3(7) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O7 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F2 B F4 110.6(8) . . ? F2 B F3 109.7(7) . . ? F4 B F3 109.3(8) . . ? F2 B F1 108.4(8) . . ? F4 B F1 108.8(7) . . ? F3 B F1 110.2(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.689 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.122 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 809212' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Ag2 F12 I4 N12 O12 P2' _chemical_formula_weight 2038.24 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6037(19) _cell_length_b 11.6541(16) _cell_length_c 13.053(3) _cell_angle_alpha 73.417(13) _cell_angle_beta 77.433(14) _cell_angle_gamma 72.924(13) _cell_volume 1599.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 12.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 2.696 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7300 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6470 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _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 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5583 _reflns_number_gt 5099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+6.6592P] 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 SHELXL _refine_ls_extinction_coef 0.0082(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5583 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.66225(4) -0.01783(4) 0.64114(3) 0.04820(12) Uani 1 1 d . . . I1 I 0.15721(3) 0.07419(4) 0.53453(3) 0.05403(12) Uani 1 1 d . . . I2 I 0.95311(5) 0.13394(5) 0.88127(5) 0.08668(17) Uani 1 1 d . . . O1 O 0.6497(4) -0.0783(4) 0.8320(3) 0.0588(11) Uani 1 1 d . . . O2 O 0.6597(4) -0.3955(5) 1.3992(3) 0.0621(11) Uani 1 1 d . . . O3 O 0.8326(4) -0.3344(4) 1.3353(3) 0.0607(11) Uani 1 1 d . . . O4 O 0.5559(4) 0.1746(4) 0.5242(3) 0.0558(10) Uani 1 1 d . . . O5 O 0.3944(5) 0.6293(4) 0.0322(4) 0.0723(13) Uani 1 1 d . . . O6 O 0.2726(4) 0.5023(5) 0.0813(4) 0.0687(12) Uani 1 1 d . . . N1 N 0.4611(4) -0.0419(4) 0.7098(3) 0.0450(10) Uani 1 1 d . . . N2 N 0.3071(5) -0.1339(6) 0.8259(4) 0.0624(14) Uani 1 1 d . . . N3 N 0.4833(4) -0.1592(4) 0.8882(3) 0.0469(10) Uani 1 1 d . . . H3A H 0.4548 -0.2126 0.9403 0.056 Uiso 1 1 calc R . . N4 N 0.7347(4) 0.1580(4) 0.6472(4) 0.0482(11) Uani 1 1 d . . . N5 N 0.7620(5) 0.3587(4) 0.6165(4) 0.0529(12) Uani 1 1 d . . . N6 N 0.6519(4) 0.3245(4) 0.5089(3) 0.0443(10) Uani 1 1 d . . . H6 H 0.6562 0.3975 0.4720 0.053 Uiso 1 1 calc R . . C1 C 0.3837(5) 0.0087(5) 0.6356(4) 0.0467(12) Uani 1 1 d . . . H1 H 0.4095 0.0581 0.5698 0.056 Uiso 1 1 calc R . . C2 C 0.2706(5) -0.0096(5) 0.6530(4) 0.0466(12) Uani 1 1 d . . . C3 C 0.2352(6) -0.0859(6) 0.7506(5) 0.0624(16) Uani 1 1 d . . . H3B H 0.1595 -0.1037 0.7631 0.075 Uiso 1 1 calc R . . C4 C 0.4165(5) -0.1081(5) 0.8015(4) 0.0435(12) Uani 1 1 d . . . C5 C 0.5864(5) -0.1364(5) 0.9020(4) 0.0439(12) Uani 1 1 d . . . C6 C 0.6202(5) -0.1883(5) 1.0136(4) 0.0437(12) Uani 1 1 d . . . C7 C 0.5322(5) -0.1897(6) 1.1057(4) 0.0507(13) Uani 1 1 d . . . H7 H 0.4499 -0.1602 1.0988 0.061 Uiso 1 1 calc R . . C8 C 0.5679(5) -0.2352(6) 1.2073(5) 0.0529(14) Uani 1 1 d . . . H8 H 0.5099 -0.2339 1.2689 0.064 Uiso 1 1 calc R . . C9 C 0.6906(5) -0.2828(5) 1.2165(4) 0.0433(11) Uani 1 1 d . . . C10 C 0.7772(5) -0.2815(6) 1.1253(5) 0.0568(15) Uani 1 1 d . . . H10 H 0.8593 -0.3131 1.1324 0.068 Uiso 1 1 calc R . . C11 C 0.7434(5) -0.2340(6) 1.0237(5) 0.0567(15) Uani 1 1 d . . . H11 H 0.8022 -0.2324 0.9625 0.068 Uiso 1 1 calc R . . C12 C 0.7243(6) -0.3433(5) 1.3275(4) 0.0482(13) Uani 1 1 d . . . C13 C 0.8788(7) -0.4030(7) 1.4354(5) 0.0673(18) Uani 1 1 d . . . H13A H 0.9576 -0.3906 1.4332 0.101 Uiso 1 1 calc R . . H13B H 0.8856 -0.4894 1.4447 0.101 Uiso 1 1 calc R . . H13C H 0.8240 -0.3747 1.4947 0.101 Uiso 1 1 calc R . . C14 C 0.8020(5) 0.1207(5) 0.7268(5) 0.0537(14) Uani 1 1 d . . . H14 H 0.8166 0.0382 0.7643 0.064 Uiso 1 1 calc R . . C15 C 0.8501(5) 0.1979(6) 0.7552(4) 0.0509(13) Uani 1 1 d . . . C16 C 0.8284(6) 0.3190(6) 0.6970(5) 0.0545(14) Uani 1 1 d . . . H16 H 0.8606 0.3742 0.7142 0.065 Uiso 1 1 calc R . . C17 C 0.7192(5) 0.2760(5) 0.5948(4) 0.0430(12) Uani 1 1 d . . . C18 C 0.5801(5) 0.2724(5) 0.4753(4) 0.0411(11) Uani 1 1 d . . . C19 C 0.5269(5) 0.3442(5) 0.3745(4) 0.0405(11) Uani 1 1 d . . . C20 C 0.5815(5) 0.4269(5) 0.2933(4) 0.0467(12) Uani 1 1 d . . . H20 H 0.6540 0.4409 0.3000 0.056 Uiso 1 1 calc R . . C21 C 0.5259(5) 0.4876(5) 0.2027(5) 0.0507(13) Uani 1 1 d . . . H21 H 0.5617 0.5434 0.1484 0.061 Uiso 1 1 calc R . . C22 C 0.4190(5) 0.4679(5) 0.1904(4) 0.0415(11) Uani 1 1 d . . . C23 C 0.3673(5) 0.3823(5) 0.2693(5) 0.0473(12) Uani 1 1 d . . . H23 H 0.2964 0.3662 0.2610 0.057 Uiso 1 1 calc R . . C24 C 0.4215(5) 0.3210(5) 0.3604(4) 0.0439(12) Uani 1 1 d . . . H24 H 0.3869 0.2631 0.4133 0.053 Uiso 1 1 calc R . . C25 C 0.3629(5) 0.5422(5) 0.0928(5) 0.0499(13) Uani 1 1 d . . . C26 C 0.2031(7) 0.5706(8) -0.0065(6) 0.073(2) Uani 1 1 d . . . H26A H 0.1407 0.5310 -0.0048 0.109 Uiso 1 1 calc R . . H26B H 0.2564 0.5725 -0.0742 0.109 Uiso 1 1 calc R . . H26C H 0.1663 0.6535 0.0013 0.109 Uiso 1 1 calc R . . P P 0.00477(18) 0.6970(2) 0.72778(16) 0.0716(5) Uani 1 1 d . . . F1 F 0.0188(9) 0.7244(11) 0.8300(7) 0.215(5) Uani 1 1 d . . . F2 F 0.1101(9) 0.5847(9) 0.7352(9) 0.201(4) Uani 1 1 d . . . F3 F -0.0063(12) 0.6831(10) 0.6215(8) 0.279(6) Uani 1 1 d . . . F4 F -0.076(2) 0.636(3) 0.783(3) 0.523(18) Uani 1 1 d . . . F5 F -0.0867(14) 0.8106(13) 0.7120(10) 0.403(8) Uani 1 1 d . . . F6 F 0.087(2) 0.7664(17) 0.6642(17) 0.441(13) 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 Ag 0.0529(2) 0.0517(2) 0.0394(2) 0.00388(17) -0.01601(17) -0.01953(18) I1 0.0469(2) 0.0639(2) 0.0477(2) -0.00284(17) -0.02173(16) -0.00758(17) I2 0.1080(4) 0.0830(3) 0.0832(3) -0.0024(2) -0.0669(3) -0.0233(3) O1 0.063(2) 0.078(3) 0.0375(19) 0.0127(18) -0.0211(17) -0.035(2) O2 0.062(2) 0.082(3) 0.037(2) -0.001(2) -0.0119(18) -0.020(2) O3 0.074(3) 0.065(2) 0.050(2) 0.0063(18) -0.035(2) -0.027(2) O4 0.060(2) 0.045(2) 0.062(2) 0.0145(18) -0.0315(19) -0.0221(17) O5 0.091(3) 0.068(3) 0.061(3) 0.023(2) -0.039(2) -0.040(2) O6 0.075(3) 0.081(3) 0.059(2) 0.012(2) -0.041(2) -0.036(2) N1 0.048(2) 0.048(2) 0.039(2) 0.0049(18) -0.0178(18) -0.0190(19) N2 0.056(3) 0.085(4) 0.046(3) 0.010(2) -0.018(2) -0.034(3) N3 0.055(2) 0.051(2) 0.036(2) 0.0070(18) -0.0192(19) -0.022(2) N4 0.048(2) 0.045(2) 0.053(3) 0.001(2) -0.022(2) -0.0150(19) N5 0.066(3) 0.050(3) 0.048(2) 0.000(2) -0.023(2) -0.023(2) N6 0.053(2) 0.042(2) 0.040(2) 0.0044(17) -0.0175(19) -0.0203(19) C1 0.051(3) 0.049(3) 0.038(3) 0.006(2) -0.017(2) -0.019(2) C2 0.055(3) 0.049(3) 0.038(3) -0.001(2) -0.021(2) -0.013(2) C3 0.059(3) 0.076(4) 0.055(3) 0.009(3) -0.023(3) -0.034(3) C4 0.050(3) 0.040(3) 0.041(3) 0.002(2) -0.016(2) -0.015(2) C5 0.052(3) 0.041(3) 0.033(2) 0.003(2) -0.017(2) -0.008(2) C6 0.052(3) 0.041(3) 0.038(3) 0.000(2) -0.018(2) -0.013(2) C7 0.049(3) 0.058(3) 0.041(3) -0.010(2) -0.011(2) -0.006(3) C8 0.048(3) 0.066(4) 0.039(3) -0.010(3) -0.008(2) -0.007(3) C9 0.052(3) 0.048(3) 0.033(2) -0.004(2) -0.016(2) -0.016(2) C10 0.047(3) 0.069(4) 0.051(3) -0.001(3) -0.020(3) -0.012(3) C11 0.045(3) 0.079(4) 0.039(3) -0.002(3) -0.011(2) -0.013(3) C12 0.063(3) 0.045(3) 0.040(3) -0.008(2) -0.020(2) -0.011(2) C13 0.082(4) 0.070(4) 0.052(3) 0.006(3) -0.040(3) -0.019(3) C14 0.055(3) 0.049(3) 0.056(3) 0.005(2) -0.027(3) -0.015(3) C15 0.050(3) 0.065(3) 0.040(3) -0.005(2) -0.020(2) -0.015(3) C16 0.066(3) 0.062(3) 0.047(3) -0.008(3) -0.021(3) -0.028(3) C17 0.036(2) 0.045(3) 0.043(3) 0.000(2) -0.010(2) -0.012(2) C18 0.043(2) 0.040(3) 0.037(2) 0.001(2) -0.013(2) -0.011(2) C19 0.042(2) 0.041(2) 0.037(2) 0.002(2) -0.012(2) -0.013(2) C20 0.044(3) 0.057(3) 0.040(3) 0.003(2) -0.013(2) -0.023(2) C21 0.056(3) 0.050(3) 0.046(3) 0.006(2) -0.014(2) -0.024(2) C22 0.044(3) 0.044(3) 0.038(2) -0.005(2) -0.010(2) -0.014(2) C23 0.049(3) 0.047(3) 0.050(3) -0.002(2) -0.019(2) -0.018(2) C24 0.043(3) 0.045(3) 0.043(3) 0.002(2) -0.011(2) -0.020(2) C25 0.050(3) 0.052(3) 0.047(3) -0.003(2) -0.012(2) -0.016(2) C26 0.067(4) 0.086(5) 0.063(4) 0.001(3) -0.040(3) -0.014(4) P 0.0610(10) 0.0847(12) 0.0622(10) -0.0098(9) -0.0298(8) 0.0002(9) F1 0.203(8) 0.305(12) 0.127(5) -0.093(7) -0.096(6) 0.046(8) F2 0.183(8) 0.175(8) 0.215(9) -0.060(7) -0.106(7) 0.066(6) F3 0.365(12) 0.262(9) 0.191(6) -0.155(6) -0.200(7) 0.164(9) F4 0.39(2) 0.66(4) 0.60(4) -0.17(3) 0.16(3) -0.40(2) F5 0.448(13) 0.393(13) 0.264(10) -0.225(9) -0.257(9) 0.342(11) F6 0.67(3) 0.328(17) 0.35(2) -0.113(15) 0.22(2) -0.354(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag O1 2.371(4) . ? Ag N1 2.379(4) . ? Ag N4 2.459(5) . ? Ag O4 2.474(4) . ? Ag I1 2.8353(8) 2_656 ? I1 C2 2.085(5) . ? I1 Ag 2.8354(8) 2_656 ? I2 C15 2.079(5) . ? O1 C5 1.217(7) . ? O2 C12 1.202(7) . ? O3 C12 1.319(7) . ? O3 C13 1.445(7) . ? O4 C18 1.216(6) . ? O5 C25 1.194(7) . ? O6 C25 1.315(7) . ? O6 C26 1.449(7) . ? N1 C4 1.317(7) . ? N1 C1 1.355(7) . ? N2 C3 1.321(8) . ? N2 C4 1.340(7) . ? N3 C5 1.357(7) . ? N3 C4 1.401(7) . ? N3 H3A 0.8600 . ? N4 C17 1.327(7) . ? N4 C14 1.331(7) . ? N5 C17 1.325(8) . ? N5 C16 1.333(8) . ? N6 C18 1.366(7) . ? N6 C17 1.395(7) . ? N6 H6 0.8600 . ? C1 C2 1.351(8) . ? C1 H1 0.9300 . ? C2 C3 1.386(8) . ? C3 H3B 0.9300 . ? C5 C6 1.499(7) . ? C6 C11 1.392(8) . ? C6 C7 1.397(8) . ? C7 C8 1.386(8) . ? C7 H7 0.9300 . ? C8 C9 1.386(8) . ? C8 H8 0.9300 . ? C9 C10 1.381(8) . ? C9 C12 1.499(7) . ? C10 C11 1.378(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.355(9) . ? C14 H14 0.9300 . ? C15 C16 1.376(9) . ? C16 H16 0.9300 . ? C18 C19 1.495(7) . ? C19 C24 1.387(7) . ? C19 C20 1.392(7) . ? C20 C21 1.379(8) . ? C20 H20 0.9300 . ? C21 C22 1.376(8) . ? C21 H21 0.9300 . ? C22 C23 1.383(7) . ? C22 C25 1.482(8) . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? P F4 1.305(17) . ? P F6 1.403(15) . ? P F5 1.426(9) . ? P F3 1.479(8) . ? P F2 1.502(8) . ? P F1 1.509(8) . ? 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 Ag N1 73.61(14) . . ? O1 Ag N4 87.40(16) . . ? N1 Ag N4 124.31(16) . . ? O1 Ag O4 129.87(16) . . ? N1 Ag O4 83.38(14) . . ? N4 Ag O4 69.74(14) . . ? O1 Ag I1 135.04(11) . 2_656 ? N1 Ag I1 136.52(12) . 2_656 ? N4 Ag I1 93.35(12) . 2_656 ? O4 Ag I1 91.66(11) . 2_656 ? C2 I1 Ag 95.87(16) . 2_656 ? C5 O1 Ag 132.5(4) . . ? C12 O3 C13 115.9(5) . . ? C18 O4 Ag 135.0(4) . . ? C25 O6 C26 118.8(5) . . ? C4 N1 C1 114.7(5) . . ? C4 N1 Ag 131.3(3) . . ? C1 N1 Ag 113.3(3) . . ? C3 N2 C4 116.6(5) . . ? C5 N3 C4 129.3(4) . . ? C5 N3 H3A 115.3 . . ? C4 N3 H3A 115.3 . . ? C17 N4 C14 116.0(5) . . ? C17 N4 Ag 135.9(4) . . ? C14 N4 Ag 108.0(4) . . ? C17 N5 C16 116.8(5) . . ? C18 N6 C17 129.1(4) . . ? C18 N6 H6 115.4 . . ? C17 N6 H6 115.4 . . ? C2 C1 N1 122.7(5) . . ? C2 C1 H1 118.6 . . ? N1 C1 H1 118.6 . . ? C1 C2 C3 117.6(5) . . ? C1 C2 I1 119.9(4) . . ? C3 C2 I1 122.4(4) . . ? N2 C3 C2 121.1(6) . . ? N2 C3 H3B 119.4 . . ? C2 C3 H3B 119.4 . . ? N1 C4 N2 127.1(5) . . ? N1 C4 N3 121.0(5) . . ? N2 C4 N3 111.9(4) . . ? O1 C5 N3 124.9(5) . . ? O1 C5 C6 120.0(5) . . ? N3 C5 C6 115.1(4) . . ? C11 C6 C7 120.2(5) . . ? C11 C6 C5 118.0(5) . . ? C7 C6 C5 121.8(5) . . ? C8 C7 C6 119.8(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.4(5) . . ? C10 C9 C12 121.7(5) . . ? C8 C9 C12 117.8(5) . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C6 119.2(5) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? O2 C12 O3 124.9(5) . . ? O2 C12 C9 122.9(5) . . ? O3 C12 C9 112.2(5) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 122.7(5) . . ? N4 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C14 C15 C16 117.2(5) . . ? C14 C15 I2 120.8(4) . . ? C16 C15 I2 122.0(4) . . ? N5 C16 C15 121.3(6) . . ? N5 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? N5 C17 N4 125.9(5) . . ? N5 C17 N6 113.3(5) . . ? N4 C17 N6 120.8(5) . . ? O4 C18 N6 123.5(5) . . ? O4 C18 C19 120.0(5) . . ? N6 C18 C19 116.5(4) . . ? C24 C19 C20 119.5(5) . . ? C24 C19 C18 117.3(4) . . ? C20 C19 C18 123.2(5) . . ? C21 C20 C19 118.7(5) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C22 C21 C20 121.8(5) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 119.3(5) . . ? C21 C22 C25 117.9(5) . . ? C23 C22 C25 122.8(5) . . ? C24 C23 C22 119.6(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C19 121.0(5) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? O5 C25 O6 123.6(6) . . ? O5 C25 C22 124.2(6) . . ? O6 C25 C22 112.2(5) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F4 P F6 176.7(19) . . ? F4 P F5 91.4(14) . . ? F6 P F5 86.0(12) . . ? F4 P F3 95.6(16) . . ? F6 P F3 82.3(11) . . ? F5 P F3 89.5(6) . . ? F4 P F2 94.7(14) . . ? F6 P F2 87.9(11) . . ? F5 P F2 173.8(9) . . ? F3 P F2 88.6(5) . . ? F4 P F1 89.5(15) . . ? F6 P F1 92.4(11) . . ? F5 P F1 87.1(6) . . ? F3 P F1 173.9(8) . . ? F2 P F1 94.3(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.330 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.143 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 809213' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Ag2 F12 I4 N12 O12 Sb2' _chemical_formula_weight 2219.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6733(10) _cell_length_b 12.0649(8) _cell_length_c 12.8161(19) _cell_angle_alpha 77.832(11) _cell_angle_beta 74.406(10) _cell_angle_gamma 74.254(8) _cell_volume 1654.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 12.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 3.357 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3650 _exptl_absorpt_correction_T_max 0.5266 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6695 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5769 _reflns_number_gt 4879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+6.6733P] 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 SHELXL _refine_ls_extinction_coef 0.0062(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5769 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.51307(5) 0.84201(4) 0.85692(4) 0.05344(16) Uani 1 1 d . . . I1 I 0.43101(4) 1.32773(4) 0.96120(4) 0.06146(16) Uani 1 1 d . . . I2 I 0.36280(6) 0.54592(6) 0.62184(5) 0.0917(2) Uani 1 1 d . . . O1 O 0.5705(5) 0.8551(4) 0.6620(4) 0.0689(14) Uani 1 1 d . . . O2 O 0.8978(5) 0.8378(4) 0.0925(4) 0.0661(13) Uani 1 1 d . . . O3 O 0.8324(5) 0.6731(4) 0.1568(4) 0.0664(13) Uani 1 1 d . . . O4 O 0.3247(4) 0.9427(4) 0.9743(4) 0.0587(12) Uani 1 1 d . . . O5 O -0.1297(5) 1.1003(5) 1.4657(4) 0.0768(15) Uani 1 1 d . . . O6 O -0.0002(5) 1.2172(4) 1.4184(4) 0.0716(14) Uani 1 1 d . . . N1 N 0.5426(5) 1.0340(4) 0.7877(4) 0.0477(12) Uani 1 1 d . . . N2 N 0.6284(6) 1.1835(5) 0.6666(5) 0.0688(17) Uani 1 1 d . . . N3 N 0.6563(5) 1.0120(5) 0.6070(4) 0.0516(13) Uani 1 1 d . . . H3A H 0.7118 1.0377 0.5559 0.062 Uiso 1 1 calc R . . N4 N 0.3388(5) 0.7713(5) 0.8489(4) 0.0558(14) Uani 1 1 d . . . N5 N 0.1401(5) 0.7375(5) 0.8818(4) 0.0576(14) Uani 1 1 d . . . N6 N 0.1752(5) 0.8492(4) 0.9874(4) 0.0484(12) Uani 1 1 d . . . H6 H 0.1026 0.8447 1.0238 0.058 Uiso 1 1 calc R . . C1 C 0.4933(6) 1.1075(6) 0.8624(5) 0.0519(15) Uani 1 1 d . . . H1 H 0.4465 1.0816 0.9297 0.062 Uiso 1 1 calc R . . C2 C 0.5096(6) 1.2185(5) 0.8427(5) 0.0490(14) Uani 1 1 d . . . C3 C 0.5806(7) 1.2529(6) 0.7421(6) 0.069(2) Uani 1 1 d . . . H3B H 0.5954 1.3272 0.7271 0.082 Uiso 1 1 calc R . . C4 C 0.6054(5) 1.0776(5) 0.6927(5) 0.0474(14) Uani 1 1 d . . . C5 C 0.6312(6) 0.9137(5) 0.5923(5) 0.0477(14) Uani 1 1 d . . . C6 C 0.6844(6) 0.8816(5) 0.4798(5) 0.0487(14) Uani 1 1 d . . . C7 C 0.6926(6) 0.9625(6) 0.3872(5) 0.0532(15) Uani 1 1 d . . . H7 H 0.6656 1.0415 0.3924 0.064 Uiso 1 1 calc R . . C8 C 0.7414(6) 0.9263(6) 0.2854(5) 0.0570(16) Uani 1 1 d . . . H8 H 0.7468 0.9815 0.2226 0.068 Uiso 1 1 calc R . . C9 C 0.7819(6) 0.8099(6) 0.2762(5) 0.0494(14) Uani 1 1 d . . . C10 C 0.7706(7) 0.7284(6) 0.3684(5) 0.0635(18) Uani 1 1 d . . . H10 H 0.7962 0.6495 0.3625 0.076 Uiso 1 1 calc R . . C11 C 0.7213(8) 0.7635(6) 0.4703(5) 0.0664(19) Uani 1 1 d . . . H11 H 0.7126 0.7081 0.5327 0.080 Uiso 1 1 calc R . . C12 C 0.8440(6) 0.7768(6) 0.1648(5) 0.0527(15) Uani 1 1 d . . . C13 C 0.8992(7) 0.6280(7) 0.0564(6) 0.073(2) Uani 1 1 d . . . H13A H 0.8844 0.5529 0.0588 0.109 Uiso 1 1 calc R . . H13B H 0.9850 0.6208 0.0483 0.109 Uiso 1 1 calc R . . H13C H 0.8726 0.6802 -0.0046 0.109 Uiso 1 1 calc R . . C14 C 0.3755(6) 0.7029(6) 0.7701(6) 0.0606(17) Uani 1 1 d . . . H14A H 0.4566 0.6906 0.7315 0.073 Uiso 1 1 calc R . . C15 C 0.2989(6) 0.6512(6) 0.7447(5) 0.0550(16) Uani 1 1 d . . . C16 C 0.1792(7) 0.6715(6) 0.8029(6) 0.0627(18) Uani 1 1 d . . . H16 H 0.1245 0.6380 0.7865 0.075 Uiso 1 1 calc R . . C17 C 0.2221(5) 0.7842(5) 0.9011(5) 0.0446(13) Uani 1 1 d . . . C18 C 0.2272(6) 0.9189(5) 1.0229(5) 0.0446(13) Uani 1 1 d . . . C19 C 0.1567(5) 0.9700(5) 1.1241(4) 0.0421(12) Uani 1 1 d . . . C20 C 0.0724(6) 0.9199(5) 1.2037(5) 0.0517(15) Uani 1 1 d . . . H20 H 0.0569 0.8510 1.1955 0.062 Uiso 1 1 calc R . . C21 C 0.0108(6) 0.9716(6) 1.2958(5) 0.0556(16) Uani 1 1 d . . . H21 H -0.0461 0.9375 1.3492 0.067 Uiso 1 1 calc R . . C22 C 0.0336(6) 1.0744(5) 1.3088(5) 0.0460(13) Uani 1 1 d . . . C23 C 0.1198(6) 1.1244(5) 1.2310(5) 0.0506(15) Uani 1 1 d . . . H23 H 0.1369 1.1921 1.2405 0.061 Uiso 1 1 calc R . . C24 C 0.1807(6) 1.0720(6) 1.1385(5) 0.0510(15) Uani 1 1 d . . . H24 H 0.2384 1.1056 1.0855 0.061 Uiso 1 1 calc R . . C25 C -0.0420(6) 1.1305(6) 1.4058(5) 0.0540(15) Uani 1 1 d . . . C26 C -0.0703(8) 1.2851(7) 1.5052(6) 0.079(2) Uani 1 1 d . . . H26A H -0.0298 1.3442 1.5060 0.118 Uiso 1 1 calc R . . H26B H -0.0769 1.2349 1.5744 0.118 Uiso 1 1 calc R . . H26C H -0.1504 1.3210 1.4925 0.118 Uiso 1 1 calc R . . Sb Sb 0.80469(6) 0.49919(5) 0.76804(5) 0.0812(2) Uani 1 1 d . . . F1 F 0.9214(10) 0.3665(7) 0.7609(8) 0.188(4) Uani 1 1 d . A . F2 F 0.7734(10) 0.4721(8) 0.9159(6) 0.194(4) Uani 1 1 d . A . F3 F 0.9241(15) 0.5619(11) 0.7898(14) 0.296(8) Uani 1 1 d . A . F4 F 0.6476(19) 0.581(2) 0.8065(16) 0.260(16) Uani 0.50 1 d P A 1 F4' F 0.7411(14) 0.6608(9) 0.7606(12) 0.113(4) Uani 0.50 1 d P A 2 F5 F 0.8731(16) 0.5414(12) 0.6207(9) 0.130(5) Uani 0.50 1 d P A 1 F5' F 0.761(2) 0.4861(16) 0.6446(14) 0.171(8) Uani 0.50 1 d P A 1 F6 F 0.683(2) 0.474(2) 0.746(2) 0.192(8) Uiso 0.50 1 d P A 2 F6' F 0.745(2) 0.3520(17) 0.802(2) 0.214(10) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0580(3) 0.0597(3) 0.0431(3) -0.0210(2) 0.0061(2) -0.0213(2) I1 0.0738(3) 0.0552(3) 0.0524(3) -0.0275(2) -0.0011(2) -0.0079(2) I2 0.0958(4) 0.1039(5) 0.0898(4) -0.0690(4) 0.0019(3) -0.0273(3) O1 0.091(4) 0.073(3) 0.044(2) -0.027(2) 0.021(2) -0.042(3) O2 0.086(3) 0.070(3) 0.039(2) -0.016(2) 0.000(2) -0.020(3) O3 0.074(3) 0.077(3) 0.055(3) -0.038(2) 0.006(2) -0.026(3) O4 0.054(3) 0.066(3) 0.059(3) -0.034(2) 0.015(2) -0.029(2) O5 0.074(3) 0.095(4) 0.061(3) -0.041(3) 0.024(3) -0.036(3) O6 0.090(4) 0.072(3) 0.058(3) -0.039(2) 0.012(3) -0.033(3) N1 0.053(3) 0.052(3) 0.040(3) -0.020(2) 0.006(2) -0.020(2) N2 0.092(4) 0.060(4) 0.050(3) -0.022(3) 0.018(3) -0.033(3) N3 0.056(3) 0.059(3) 0.039(3) -0.024(2) 0.010(2) -0.021(3) N4 0.050(3) 0.065(3) 0.057(3) -0.034(3) 0.008(2) -0.020(3) N5 0.053(3) 0.072(4) 0.053(3) -0.030(3) 0.000(2) -0.019(3) N6 0.050(3) 0.058(3) 0.038(2) -0.019(2) 0.008(2) -0.022(2) C1 0.055(4) 0.063(4) 0.039(3) -0.022(3) 0.005(3) -0.021(3) C2 0.055(4) 0.051(3) 0.042(3) -0.023(3) -0.001(3) -0.011(3) C3 0.091(5) 0.058(4) 0.055(4) -0.020(3) 0.009(4) -0.030(4) C4 0.047(3) 0.057(4) 0.038(3) -0.019(3) 0.006(2) -0.017(3) C5 0.050(3) 0.053(3) 0.038(3) -0.017(3) 0.000(3) -0.011(3) C6 0.050(3) 0.055(4) 0.040(3) -0.022(3) 0.004(3) -0.013(3) C7 0.063(4) 0.051(4) 0.042(3) -0.018(3) -0.006(3) -0.005(3) C8 0.072(4) 0.062(4) 0.031(3) -0.008(3) -0.007(3) -0.010(3) C9 0.053(4) 0.062(4) 0.035(3) -0.021(3) -0.004(3) -0.012(3) C10 0.089(5) 0.050(4) 0.050(4) -0.022(3) 0.002(3) -0.021(4) C11 0.098(6) 0.054(4) 0.042(3) -0.012(3) 0.002(3) -0.023(4) C12 0.053(4) 0.065(4) 0.041(3) -0.020(3) -0.010(3) -0.006(3) C13 0.073(5) 0.090(5) 0.059(4) -0.045(4) 0.004(4) -0.017(4) C14 0.059(4) 0.062(4) 0.063(4) -0.031(3) 0.003(3) -0.017(3) C15 0.067(4) 0.053(4) 0.049(3) -0.024(3) -0.003(3) -0.017(3) C16 0.067(4) 0.070(5) 0.064(4) -0.030(4) -0.011(3) -0.027(4) C17 0.050(3) 0.046(3) 0.039(3) -0.011(2) -0.003(3) -0.017(3) C18 0.051(3) 0.040(3) 0.040(3) -0.011(2) 0.000(3) -0.011(3) C19 0.045(3) 0.045(3) 0.035(3) -0.012(2) -0.002(2) -0.010(3) C20 0.064(4) 0.048(3) 0.043(3) -0.017(3) 0.005(3) -0.022(3) C21 0.066(4) 0.058(4) 0.041(3) -0.015(3) 0.011(3) -0.028(3) C22 0.052(3) 0.049(3) 0.035(3) -0.013(2) 0.000(2) -0.012(3) C23 0.058(4) 0.048(3) 0.050(3) -0.019(3) -0.002(3) -0.019(3) C24 0.054(4) 0.057(4) 0.044(3) -0.016(3) 0.004(3) -0.024(3) C25 0.063(4) 0.053(4) 0.042(3) -0.018(3) 0.003(3) -0.012(3) C26 0.099(6) 0.068(5) 0.066(5) -0.040(4) 0.003(4) -0.011(4) Sb 0.0963(4) 0.0720(4) 0.0708(4) -0.0395(3) -0.0181(3) 0.0096(3) F1 0.229(10) 0.130(6) 0.185(8) -0.081(6) -0.066(7) 0.056(6) F2 0.275(11) 0.172(8) 0.092(5) -0.056(5) 0.008(6) -0.002(7) F3 0.360(19) 0.217(12) 0.40(2) -0.016(13) -0.149(16) -0.178(13) F4 0.192(18) 0.36(3) 0.193(18) -0.21(2) -0.114(16) 0.20(2) F4' 0.142(11) 0.054(6) 0.151(11) -0.022(6) -0.043(9) -0.022(6) F5 0.186(15) 0.116(10) 0.067(7) -0.017(6) 0.006(8) -0.032(10) F5' 0.23(2) 0.161(14) 0.115(11) -0.086(11) -0.087(13) 0.060(14) F6' 0.22(2) 0.139(15) 0.33(3) -0.047(17) -0.10(2) -0.063(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.382(5) . ? Ag O1 2.389(4) . ? Ag N4 2.443(5) . ? Ag O4 2.473(4) . ? Ag I1 2.8520(8) 2_677 ? I1 C2 2.079(5) . ? I1 Ag 2.8520(8) 2_677 ? I2 C15 2.084(6) . ? O1 C5 1.210(7) . ? O2 C12 1.202(8) . ? O3 C12 1.321(8) . ? O3 C13 1.444(7) . ? O4 C18 1.220(7) . ? O5 C25 1.197(8) . ? O6 C25 1.323(8) . ? O6 C26 1.451(8) . ? N1 C4 1.325(7) . ? N1 C1 1.348(7) . ? N2 C3 1.322(9) . ? N2 C4 1.331(8) . ? N3 C5 1.358(8) . ? N3 C4 1.395(7) . ? N3 H3A 0.8600 . ? N4 C17 1.329(8) . ? N4 C14 1.346(8) . ? N5 C16 1.325(8) . ? N5 C17 1.332(8) . ? N6 C18 1.367(8) . ? N6 C17 1.395(7) . ? N6 H6 0.8600 . ? C1 C2 1.365(9) . ? C1 H1 0.9300 . ? C2 C3 1.381(9) . ? C3 H3B 0.9300 . ? C5 C6 1.495(8) . ? C6 C7 1.368(9) . ? C6 C11 1.394(9) . ? C7 C8 1.386(8) . ? C7 H7 0.9300 . ? C8 C9 1.375(9) . ? C8 H8 0.9300 . ? C9 C10 1.370(9) . ? C9 C12 1.500(8) . ? C10 C11 1.382(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.357(9) . ? C14 H14A 0.9300 . ? C15 C16 1.378(10) . ? C16 H16 0.9300 . ? C18 C19 1.492(7) . ? C19 C20 1.378(8) . ? C19 C24 1.392(8) . ? C20 C21 1.382(8) . ? C20 H20 0.9300 . ? C21 C22 1.387(9) . ? C21 H21 0.9300 . ? C22 C23 1.381(8) . ? C22 C25 1.491(8) . ? C23 C24 1.389(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? Sb F6 1.63(2) . ? Sb F1 1.799(7) . ? Sb F2 1.806(7) . ? Sb F4 1.822(14) . ? Sb F5' 1.837(13) . ? Sb F3 1.861(11) . ? Sb F5 1.862(11) . ? Sb F4' 1.880(11) . ? Sb F6' 2.004(18) . ? F5 F5' 1.56(2) . ? F6 F6' 1.56(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag O1 73.59(16) . . ? N1 Ag N4 125.3(2) . . ? O1 Ag N4 86.95(17) . . ? N1 Ag O4 83.92(15) . . ? O1 Ag O4 129.47(19) . . ? N4 Ag O4 70.04(15) . . ? N1 Ag I1 134.78(12) . 2_677 ? O1 Ag I1 136.19(14) . 2_677 ? N4 Ag I1 94.20(14) . 2_677 ? O4 Ag I1 91.18(12) . 2_677 ? C2 I1 Ag 96.49(18) . 2_677 ? C5 O1 Ag 132.1(4) . . ? C12 O3 C13 116.1(6) . . ? C18 O4 Ag 134.8(4) . . ? C25 O6 C26 117.9(6) . . ? C4 N1 C1 115.6(5) . . ? C4 N1 Ag 131.2(4) . . ? C1 N1 Ag 113.0(4) . . ? C3 N2 C4 116.4(6) . . ? C5 N3 C4 129.6(5) . . ? C5 N3 H3A 115.2 . . ? C4 N3 H3A 115.2 . . ? C17 N4 C14 115.4(5) . . ? C17 N4 Ag 136.3(4) . . ? C14 N4 Ag 108.3(4) . . ? C16 N5 C17 116.5(6) . . ? C18 N6 C17 129.7(5) . . ? C18 N6 H6 115.1 . . ? C17 N6 H6 115.1 . . ? N1 C1 C2 122.3(5) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 116.9(5) . . ? C1 C2 I1 120.5(4) . . ? C3 C2 I1 122.6(5) . . ? N2 C3 C2 122.2(6) . . ? N2 C3 H3B 118.9 . . ? C2 C3 H3B 118.9 . . ? N1 C4 N2 126.5(5) . . ? N1 C4 N3 121.1(5) . . ? N2 C4 N3 112.4(5) . . ? O1 C5 N3 124.6(5) . . ? O1 C5 C6 121.1(5) . . ? N3 C5 C6 114.4(5) . . ? C7 C6 C11 119.4(5) . . ? C7 C6 C5 123.0(6) . . ? C11 C6 C5 117.6(6) . . ? C6 C7 C8 119.8(6) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.9(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.6(5) . . ? C10 C9 C12 122.1(6) . . ? C8 C9 C12 118.2(6) . . ? C9 C10 C11 120.0(6) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 120.3(6) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? O2 C12 O3 124.7(6) . . ? O2 C12 C9 123.6(6) . . ? O3 C12 C9 111.7(6) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 122.6(6) . . ? N4 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C14 C15 C16 117.3(6) . . ? C14 C15 I2 120.3(5) . . ? C16 C15 I2 122.4(5) . . ? N5 C16 C15 121.8(6) . . ? N5 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? N4 C17 N5 126.4(5) . . ? N4 C17 N6 120.4(5) . . ? N5 C17 N6 113.2(5) . . ? O4 C18 N6 123.1(5) . . ? O4 C18 C19 119.9(5) . . ? N6 C18 C19 116.9(5) . . ? C20 C19 C24 119.2(5) . . ? C20 C19 C18 123.3(5) . . ? C24 C19 C18 117.5(5) . . ? C19 C20 C21 120.3(6) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 120.1(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.3(5) . . ? C23 C22 C25 122.0(6) . . ? C21 C22 C25 117.7(5) . . ? C22 C23 C24 119.0(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C19 120.9(5) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? O5 C25 O6 123.9(6) . . ? O5 C25 C22 124.1(6) . . ? O6 C25 C22 112.1(5) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F6 Sb F1 107.5(9) . . ? F6 Sb F2 100.8(9) . . ? F1 Sb F2 90.7(4) . . ? F6 Sb F4 53.0(11) . . ? F1 Sb F4 153.2(12) . . ? F2 Sb F4 77.3(7) . . ? F6 Sb F5' 46.3(9) . . ? F1 Sb F5' 92.9(5) . . ? F2 Sb F5' 146.2(10) . . ? F4 Sb F5' 84.7(7) . . ? F6 Sb F3 167.4(10) . . ? F1 Sb F3 84.9(6) . . ? F2 Sb F3 80.8(6) . . ? F4 Sb F3 116.0(10) . . ? F5' Sb F3 133.0(10) . . ? F6 Sb F5 95.1(10) . . ? F1 Sb F5 86.5(6) . . ? F2 Sb F5 163.9(7) . . ? F4 Sb F5 111.3(9) . . ? F5' Sb F5 49.8(8) . . ? F3 Sb F5 83.2(8) . . ? F6 Sb F4' 94.1(9) . . ? F1 Sb F4' 156.5(6) . . ? F2 Sb F4' 94.4(5) . . ? F4 Sb F4' 49.9(10) . . ? F5' Sb F4' 95.6(7) . . ? F3 Sb F4' 73.3(6) . . ? F5 Sb F4' 82.3(6) . . ? F6 Sb F6' 49.6(9) . . ? F1 Sb F6' 64.3(7) . . ? F2 Sb F6' 78.0(8) . . ? F4 Sb F6' 89.5(13) . . ? F5' Sb F6' 73.4(11) . . ? F3 Sb F6' 142.0(8) . . ? F5 Sb F6' 114.6(9) . . ? F4' Sb F6' 139.2(8) . . ? F5' F5 Sb 64.2(7) . . ? F5 F5' Sb 65.9(8) . . ? F6' F6 Sb 77.6(12) . . ? F6 F6' Sb 52.8(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.336 _refine_diff_density_min -1.952 _refine_diff_density_rms 0.104 #===END