# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_email jdchen@cycu.edu.tw loop_ _publ_author_name 'Jhy-Der Chen' 'Hui-Lin Hsiao' 'Chia-Jun Wu' 'Wayne Hsu' 'Chun-Wei Yeh' 'Ming-Yuan Xie' data_L1 _database_code_depnum_ccdc_archive 'CCDC 888032' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N2 O3' _chemical_formula_weight 256.26 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' _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 5.7769(12) _cell_length_b 7.8170(18) _cell_length_c 13.529(3) _cell_angle_alpha 90.857(14) _cell_angle_beta 100.574(13) _cell_angle_gamma 106.749(13) _cell_volume 573.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2529 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.59 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10218 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.1203 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.49 _reflns_number_total 2851 _reflns_number_gt 1496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0435P)^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_number_reflns 2851 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 O1 O -0.1075(3) 0.6711(2) 0.37027(11) 0.0207(4) Uani 1 1 d . . . O2 O -0.1787(3) 0.1291(2) -0.06353(12) 0.0288(5) Uani 1 1 d . . . O3 O 0.2292(3) 0.2612(2) -0.04253(11) 0.0220(4) Uani 1 1 d . . . N1 N 0.2510(3) 0.6100(3) 0.43910(13) 0.0177(5) Uani 1 1 d . . . H1A H 0.3291 0.5331 0.4330 0.021 Uiso 1 1 calc R . . N2 N 0.5534(3) 0.7154(3) 0.57992(13) 0.0178(5) Uani 1 1 d . . . C1 C 0.6651(4) 0.8371(3) 0.65796(16) 0.0182(5) Uani 1 1 d . . . H1B H 0.8139 0.8305 0.6954 0.022 Uiso 1 1 calc R . . C2 C 0.5741(4) 0.9713(3) 0.68642(17) 0.0198(5) Uani 1 1 d . . . H2B H 0.6595 1.0534 0.7407 0.024 Uiso 1 1 calc R . . C3 C 0.3515(4) 0.9791(3) 0.63131(16) 0.0195(5) Uani 1 1 d . . . H3A H 0.2828 1.0665 0.6486 0.023 Uiso 1 1 calc R . . C4 C 0.2313(4) 0.8563(3) 0.55025(16) 0.0198(6) Uani 1 1 d . . . H4A H 0.0800 0.8586 0.5131 0.024 Uiso 1 1 calc R . . C5 C 0.3410(4) 0.7294(3) 0.52539(16) 0.0163(5) Uani 1 1 d . . . C6 C 0.0544(4) 0.6012(3) 0.36373(16) 0.0173(5) Uani 1 1 d . . . C7 C 0.0516(4) 0.5018(3) 0.26764(16) 0.0157(5) Uani 1 1 d . . . C8 C -0.1720(4) 0.3905(3) 0.21368(16) 0.0183(5) Uani 1 1 d . . . H8A H -0.3147 0.3743 0.2396 0.022 Uiso 1 1 calc R . . C9 C -0.1842(4) 0.3038(3) 0.12212(17) 0.0190(5) Uani 1 1 d . . . H9A H -0.3337 0.2282 0.0873 0.023 Uiso 1 1 calc R . . C10 C 0.0291(4) 0.3303(3) 0.08203(16) 0.0163(5) Uani 1 1 d . . . C11 C 0.2501(4) 0.4443(3) 0.13434(17) 0.0178(5) Uani 1 1 d . . . H11A H 0.3911 0.4652 0.1068 0.021 Uiso 1 1 calc R . . C12 C 0.2636(4) 0.5275(3) 0.22737(16) 0.0173(5) Uani 1 1 d . . . H12A H 0.4141 0.6006 0.2629 0.021 Uiso 1 1 calc R . . C13 C 0.0104(4) 0.2299(3) -0.01523(17) 0.0190(5) Uani 1 1 d . . . C14 C 0.2321(4) 0.1626(3) -0.13403(17) 0.0237(6) Uani 1 1 d . . . H14A H 0.3963 0.1572 -0.1335 0.036 Uiso 1 1 calc R . . H14B H 0.1798 0.2221 -0.1917 0.036 Uiso 1 1 calc R . . H14C H 0.1223 0.0433 -0.1373 0.036 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 O1 0.0178(8) 0.0274(10) 0.0200(9) -0.0012(7) 0.0021(7) 0.0124(7) O2 0.0212(8) 0.0377(12) 0.0237(9) -0.0084(8) 0.0001(7) 0.0060(8) O3 0.0245(8) 0.0265(10) 0.0163(9) -0.0042(7) 0.0072(7) 0.0079(7) N1 0.0205(9) 0.0200(12) 0.0157(10) -0.0027(9) 0.0002(8) 0.0131(8) N2 0.0165(9) 0.0215(12) 0.0162(10) 0.0006(9) 0.0019(8) 0.0077(8) C1 0.0148(10) 0.0219(14) 0.0165(12) 0.0009(10) 0.0024(9) 0.0038(10) C2 0.0229(12) 0.0171(13) 0.0178(12) -0.0005(10) 0.0033(10) 0.0037(10) C3 0.0236(11) 0.0184(14) 0.0200(13) 0.0000(10) 0.0068(10) 0.0101(10) C4 0.0197(11) 0.0228(15) 0.0177(12) -0.0023(11) 0.0017(10) 0.0087(10) C5 0.0180(11) 0.0193(14) 0.0129(12) 0.0011(10) 0.0039(9) 0.0072(10) C6 0.0151(11) 0.0204(14) 0.0160(12) 0.0046(10) 0.0024(9) 0.0046(10) C7 0.0179(11) 0.0189(13) 0.0132(12) 0.0032(10) 0.0019(9) 0.0108(10) C8 0.0179(11) 0.0203(14) 0.0177(12) 0.0002(10) 0.0039(9) 0.0069(10) C9 0.0165(11) 0.0214(14) 0.0189(12) -0.0004(11) 0.0009(9) 0.0069(10) C10 0.0197(11) 0.0163(13) 0.0138(12) 0.0025(10) 0.0017(9) 0.0077(9) C11 0.0171(11) 0.0196(14) 0.0192(12) 0.0048(10) 0.0059(9) 0.0078(10) C12 0.0167(10) 0.0169(13) 0.0176(12) 0.0006(10) 0.0013(9) 0.0053(9) C13 0.0196(11) 0.0219(14) 0.0174(12) 0.0039(11) 0.0040(10) 0.0086(10) C14 0.0277(12) 0.0259(15) 0.0203(13) -0.0013(11) 0.0082(11) 0.0105(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.226(3) . ? O2 C13 1.211(3) . ? O3 C13 1.338(2) . ? O3 C14 1.454(3) . ? N1 C6 1.365(3) . ? N1 C5 1.404(3) . ? N1 H1A 0.8600 . ? N2 C1 1.342(3) . ? N2 C5 1.345(3) . ? C1 C2 1.380(3) . ? C1 H1B 0.9300 . ? C2 C3 1.381(3) . ? C2 H2B 0.9300 . ? C3 C4 1.382(3) . ? C3 H3A 0.9300 . ? C4 C5 1.389(3) . ? C4 H4A 0.9300 . ? C6 C7 1.500(3) . ? C7 C12 1.394(3) . ? C7 C8 1.395(3) . ? C8 C9 1.383(3) . ? C8 H8A 0.9300 . ? C9 C10 1.399(3) . ? C9 H9A 0.9300 . ? C10 C11 1.385(3) . ? C10 C13 1.493(3) . ? C11 C12 1.387(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 C13 O3 C14 116.17(17) . . ? C6 N1 C5 127.8(2) . . ? C6 N1 H1A 116.1 . . ? C5 N1 H1A 116.1 . . ? C1 N2 C5 116.9(2) . . ? N2 C1 C2 124.5(2) . . ? N2 C1 H1B 117.8 . . ? C2 C1 H1B 117.8 . . ? C1 C2 C3 117.5(2) . . ? C1 C2 H2B 121.2 . . ? C3 C2 H2B 121.2 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N2 C5 C4 122.7(2) . . ? N2 C5 N1 113.1(2) . . ? C4 C5 N1 124.1(2) . . ? O1 C6 N1 124.4(2) . . ? O1 C6 C7 120.82(19) . . ? N1 C6 C7 114.7(2) . . ? C12 C7 C8 119.2(2) . . ? C12 C7 C6 121.60(19) . . ? C8 C7 C6 119.09(19) . . ? C9 C8 C7 120.8(2) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 119.5(2) . . ? C11 C10 C13 122.3(2) . . ? C9 C10 C13 118.22(19) . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 120.0(2) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? O2 C13 O3 123.4(2) . . ? O2 C13 C10 124.5(2) . . ? O3 C13 C10 112.03(18) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.273 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.078 #===END data_L2 _database_code_depnum_ccdc_archive 'CCDC 888033' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N2 O3' _chemical_formula_weight 256.26 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 3.9462(2) _cell_length_b 28.9809(11) _cell_length_c 5.2402(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.337(2) _cell_angle_gamma 90.00 _cell_volume 596.69(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4156 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 28.31 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9602 _exptl_absorpt_correction_T_max 0.9798 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5559 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2651 _reflns_number_gt 2390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0811P)^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 SHELXL _refine_ls_extinction_coef 0.108(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(13) _refine_ls_number_reflns 2651 _refine_ls_number_parameters 174 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 O1 O 0.3946(5) 0.30154(5) 1.2881(3) 0.0510(4) Uani 1 1 d . . . O2 O 0.1461(6) 0.06834(6) 0.9791(4) 0.0671(6) Uani 1 1 d . . . O3 O -0.1427(5) 0.09171(5) 0.6167(4) 0.0527(4) Uani 1 1 d . . . N1 N 0.4608(6) 0.44053(6) 0.6927(4) 0.0514(5) Uani 1 1 d . . . N2 N 0.4061(4) 0.31870(5) 0.8659(3) 0.0355(4) Uani 1 1 d . . . H2A H 0.3783 0.3075 0.7134 0.043 Uiso 1 1 calc R . . C1 C 0.6483(7) 0.45722(7) 0.8980(5) 0.0500(6) Uani 1 1 d . . . H1B H 0.6983 0.4886 0.9031 0.060 Uiso 1 1 calc R . . C2 C 0.7708(6) 0.43013(7) 1.1024(4) 0.0464(5) Uani 1 1 d . . . H2B H 0.9016 0.4431 1.2409 0.056 Uiso 1 1 calc R . . C3 C 0.6973(6) 0.38345(7) 1.0994(4) 0.0406(4) Uani 1 1 d . . . H3A H 0.7797 0.3644 1.2338 0.049 Uiso 1 1 calc R . . C4 C 0.4977(5) 0.36600(6) 0.8907(3) 0.0322(4) Uani 1 1 d . . . C5 C 0.3889(6) 0.39558(7) 0.6929(4) 0.0429(5) Uani 1 1 d . . . H5A H 0.2582 0.3834 0.5519 0.051 Uiso 1 1 calc R . . C6 C 0.3591(5) 0.28980(6) 1.0622(4) 0.0325(4) Uani 1 1 d . . . C7 C 0.2651(5) 0.24113(5) 0.9886(4) 0.0310(4) Uani 1 1 d . . . C8 C 0.0805(5) 0.22872(6) 0.7617(4) 0.0351(4) Uani 1 1 d . . . H8A H 0.0070 0.2512 0.6424 0.042 Uiso 1 1 calc R . . C9 C 0.0052(5) 0.18244(6) 0.7125(4) 0.0369(4) Uani 1 1 d . . . H9A H -0.1220 0.1742 0.5610 0.044 Uiso 1 1 calc R . . C10 C 0.1173(5) 0.14850(6) 0.8864(4) 0.0332(4) Uani 1 1 d . . . C11 C 0.3020(6) 0.16097(6) 1.1127(4) 0.0397(4) Uani 1 1 d . . . H11A H 0.3796 0.1384 1.2298 0.048 Uiso 1 1 calc R . . C12 C 0.3722(5) 0.20693(7) 1.1659(4) 0.0381(4) Uani 1 1 d . . . H12A H 0.4914 0.2151 1.3208 0.046 Uiso 1 1 calc R . . C13 C 0.0443(6) 0.09869(6) 0.8355(4) 0.0398(5) Uani 1 1 d . . . C14 C -0.2223(8) 0.04400(8) 0.5475(6) 0.0601(7) Uani 1 1 d . . . H14A H -0.3677 0.0432 0.3901 0.090 Uiso 1 1 calc R . . H14B H -0.3363 0.0297 0.6810 0.090 Uiso 1 1 calc R . . H14C H -0.0156 0.0276 0.5258 0.090 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 O1 0.0912(13) 0.0326(7) 0.0305(7) -0.0036(5) 0.0120(7) -0.0126(7) O2 0.1062(16) 0.0257(7) 0.0655(12) 0.0067(7) -0.0126(10) 0.0022(8) O3 0.0758(11) 0.0262(7) 0.0543(10) -0.0036(6) -0.0035(8) -0.0086(6) N1 0.0803(14) 0.0251(8) 0.0490(12) 0.0066(7) 0.0077(10) -0.0027(8) N2 0.0534(9) 0.0233(7) 0.0298(8) -0.0026(5) 0.0048(6) -0.0041(6) C1 0.0748(16) 0.0237(9) 0.0532(14) -0.0044(8) 0.0155(11) -0.0084(9) C2 0.0604(13) 0.0358(11) 0.0429(11) -0.0085(8) 0.0045(9) -0.0150(9) C3 0.0528(11) 0.0314(9) 0.0372(10) 0.0000(7) 0.0018(8) -0.0061(8) C4 0.0413(9) 0.0250(8) 0.0310(9) -0.0009(6) 0.0081(7) -0.0019(7) C5 0.0611(13) 0.0311(9) 0.0360(10) 0.0011(7) 0.0026(9) -0.0040(8) C6 0.0430(10) 0.0256(8) 0.0295(9) -0.0017(6) 0.0065(7) -0.0014(7) C7 0.0377(9) 0.0229(7) 0.0330(9) 0.0004(6) 0.0067(7) -0.0008(6) C8 0.0481(10) 0.0244(8) 0.0322(9) 0.0029(7) 0.0011(7) -0.0006(7) C9 0.0451(10) 0.0261(9) 0.0383(10) 0.0008(7) -0.0027(8) -0.0029(7) C10 0.0402(9) 0.0240(8) 0.0360(10) 0.0009(6) 0.0073(7) 0.0003(7) C11 0.0560(12) 0.0268(9) 0.0357(10) 0.0053(7) 0.0006(9) 0.0035(8) C12 0.0497(11) 0.0307(9) 0.0327(9) 0.0015(7) -0.0018(8) -0.0003(7) C13 0.0512(11) 0.0240(9) 0.0453(11) 0.0009(7) 0.0093(9) -0.0001(7) C14 0.0775(17) 0.0318(10) 0.0705(17) -0.0130(10) 0.0035(13) -0.0130(10) _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 O1 C6 1.227(2) . ? O2 C13 1.202(3) . ? O3 C13 1.320(3) . ? O3 C14 1.456(3) . ? N1 C5 1.333(3) . ? N1 C1 1.338(3) . ? N2 C6 1.353(2) . ? N2 C4 1.421(2) . ? N2 H2A 0.8600 . ? C1 C2 1.379(3) . ? C1 H1B 0.9300 . ? C2 C3 1.383(3) . ? C2 H2B 0.9300 . ? C3 C4 1.383(3) . ? C3 H3A 0.9300 . ? C4 C5 1.382(3) . ? C5 H5A 0.9300 . ? C6 C7 1.500(2) . ? C7 C8 1.383(3) . ? C7 C12 1.397(3) . ? C8 C9 1.393(3) . ? C8 H8A 0.9300 . ? C9 C10 1.385(3) . ? C9 H9A 0.9300 . ? C10 C11 1.381(3) . ? C10 C13 1.491(3) . ? C11 C12 1.384(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 C13 O3 C14 116.86(19) . . ? C5 N1 C1 117.03(19) . . ? C6 N2 C4 125.41(15) . . ? C6 N2 H2A 117.3 . . ? C4 N2 H2A 117.3 . . ? N1 C1 C2 123.13(18) . . ? N1 C1 H1B 118.4 . . ? C2 C1 H1B 118.4 . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2B 120.3 . . ? C3 C2 H2B 120.3 . . ? C4 C3 C2 118.0(2) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C5 C4 C3 118.73(17) . . ? C5 C4 N2 118.11(18) . . ? C3 C4 N2 123.14(16) . . ? N1 C5 C4 123.7(2) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? O1 C6 N2 123.41(17) . . ? O1 C6 C7 120.80(17) . . ? N2 C6 C7 115.77(16) . . ? C8 C7 C12 119.34(16) . . ? C8 C7 C6 124.30(16) . . ? C12 C7 C6 116.36(17) . . ? C7 C8 C9 119.73(17) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C10 C9 C8 120.84(19) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 119.32(18) . . ? C11 C10 C13 118.98(17) . . ? C9 C10 C13 121.70(19) . . ? C10 C11 C12 120.32(17) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.42(19) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? O2 C13 O3 124.0(2) . . ? O2 C13 C10 123.3(2) . . ? O3 C13 C10 112.74(17) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.311 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.049 #===END data_L3 _database_code_depnum_ccdc_archive 'CCDC 888034' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 N2 O5' _chemical_formula_weight 292.29 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2328(4) _cell_length_b 11.2111(5) _cell_length_c 17.3601(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.222(3) _cell_angle_gamma 90.00 _cell_volume 1393.22(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1477 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.51 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5970 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10195 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2454 _reflns_number_gt 1384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0421P)^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_number_reflns 2454 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 O1 O 0.2877(2) 0.17346(14) 0.07547(8) 0.0535(5) Uani 1 1 d . . . O2 O 0.1204(2) -0.09963(15) -0.31072(9) 0.0598(5) Uani 1 1 d . . . O3 O 0.0476(2) 0.09474(14) -0.31896(8) 0.0544(5) Uani 1 1 d . . . N1 N 0.4421(3) -0.03288(18) 0.34320(10) 0.0470(5) Uani 1 1 d . . . N2 N 0.2887(2) -0.02484(15) 0.10014(9) 0.0379(5) Uani 1 1 d . . . H2A H 0.2695 -0.0940 0.0790 0.046 Uiso 1 1 calc R . . C1 C 0.4079(3) -0.1256(2) 0.21778(12) 0.0438(6) Uani 1 1 d . . . H1B H 0.4206 -0.1941 0.1888 0.053 Uiso 1 1 calc R . . C2 C 0.4579(3) -0.1262(2) 0.29735(12) 0.0496(7) Uani 1 1 d . . . H2B H 0.5057 -0.1966 0.3206 0.059 Uiso 1 1 calc R . . C3 C 0.3719(3) 0.0657(2) 0.30751(12) 0.0448(6) Uani 1 1 d . . . H3A H 0.3572 0.1321 0.3382 0.054 Uiso 1 1 calc R . . C4 C 0.3193(3) 0.0763(2) 0.22823(12) 0.0426(6) Uani 1 1 d . . . H4A H 0.2719 0.1478 0.2065 0.051 Uiso 1 1 calc R . . C5 C 0.3389(3) -0.02191(19) 0.18169(11) 0.0341(5) Uani 1 1 d . . . C6 C 0.2677(3) 0.0707(2) 0.05183(12) 0.0385(6) Uani 1 1 d . . . C7 C 0.2216(3) 0.04558(19) -0.03384(11) 0.0348(6) Uani 1 1 d . . . C8 C 0.2397(3) -0.0649(2) -0.06738(12) 0.0458(6) Uani 1 1 d . . . H8A H 0.2785 -0.1301 -0.0361 0.055 Uiso 1 1 calc R . . C9 C 0.2003(3) -0.0790(2) -0.14723(12) 0.0472(6) Uani 1 1 d . . . H9A H 0.2139 -0.1535 -0.1692 0.057 Uiso 1 1 calc R . . C10 C 0.1411(3) 0.0164(2) -0.19449(11) 0.0362(6) Uani 1 1 d . . . C11 C 0.1209(3) 0.1265(2) -0.16154(11) 0.0412(6) Uani 1 1 d . . . H11A H 0.0801 0.1912 -0.1930 0.049 Uiso 1 1 calc R . . C12 C 0.1610(3) 0.14122(19) -0.08185(12) 0.0415(6) Uani 1 1 d . . . H12A H 0.1472 0.2159 -0.0601 0.050 Uiso 1 1 calc R . . C13 C 0.1030(3) -0.0044(2) -0.28023(12) 0.0432(6) Uani 1 1 d . . . C14 C 0.0054(4) 0.0835(2) -0.40318(12) 0.0671(8) Uani 1 1 d . . . H14A H -0.0300 0.1600 -0.4255 0.101 Uiso 1 1 calc R . . H14B H -0.0954 0.0281 -0.4161 0.101 Uiso 1 1 calc R . . H14C H 0.1140 0.0551 -0.4235 0.101 Uiso 1 1 calc R . . O4 O 0.2555(2) 0.71904(14) 0.06090(8) 0.0630(5) Uani 1 1 d . . . H4C H 0.2139 0.6757 0.0948 0.076 Uiso 1 1 d R . . H4D H 0.3466 0.6830 0.0452 0.076 Uiso 1 1 d R . . O5 O 0.4494(2) 0.37038(14) 0.00536(8) 0.0665(6) Uani 1 1 d . . . H5C H 0.4013 0.3088 0.0231 0.080 Uiso 1 1 d R . . H5D H 0.4839 0.4174 0.0431 0.080 Uiso 1 1 d 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 O1 0.0855(14) 0.0343(11) 0.0388(9) 0.0002(8) 0.0028(8) -0.0088(9) O2 0.0853(14) 0.0533(12) 0.0429(10) -0.0081(9) 0.0172(9) 0.0027(10) O3 0.0724(13) 0.0559(12) 0.0330(9) 0.0046(8) 0.0012(8) 0.0011(9) N1 0.0557(14) 0.0462(14) 0.0387(11) -0.0011(10) 0.0055(9) 0.0036(10) N2 0.0508(13) 0.0321(11) 0.0303(10) -0.0012(8) 0.0040(9) -0.0060(9) C1 0.0550(17) 0.0357(15) 0.0391(14) -0.0033(11) 0.0014(11) 0.0053(12) C2 0.0600(18) 0.0441(16) 0.0427(15) 0.0052(12) 0.0007(12) 0.0080(13) C3 0.0552(17) 0.0399(15) 0.0392(14) -0.0028(11) 0.0065(12) 0.0013(12) C4 0.0483(15) 0.0404(15) 0.0390(14) 0.0043(11) 0.0061(11) -0.0004(12) C5 0.0333(14) 0.0360(14) 0.0330(13) -0.0004(10) 0.0048(10) -0.0037(10) C6 0.0376(15) 0.0384(16) 0.0393(14) 0.0048(11) 0.0052(10) -0.0062(11) C7 0.0348(14) 0.0365(15) 0.0332(12) 0.0010(10) 0.0047(10) -0.0045(11) C8 0.0622(18) 0.0373(16) 0.0386(14) 0.0077(11) 0.0091(12) 0.0075(12) C9 0.0646(18) 0.0383(16) 0.0392(14) -0.0026(11) 0.0091(12) 0.0068(13) C10 0.0348(14) 0.0402(15) 0.0345(12) -0.0003(11) 0.0076(10) -0.0023(11) C11 0.0474(15) 0.0387(15) 0.0359(13) 0.0072(11) 0.0007(10) -0.0012(11) C12 0.0474(15) 0.0355(14) 0.0402(13) -0.0005(11) 0.0012(11) 0.0008(11) C13 0.0422(16) 0.0510(18) 0.0379(14) 0.0052(13) 0.0110(11) -0.0045(13) C14 0.084(2) 0.084(2) 0.0315(14) 0.0063(13) 0.0031(13) -0.0039(17) O4 0.0972(15) 0.0483(11) 0.0463(10) 0.0046(8) 0.0199(9) -0.0026(10) O5 0.0997(15) 0.0577(12) 0.0433(10) -0.0032(8) 0.0140(9) -0.0241(10) _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 O1 C6 1.225(2) . ? O2 C13 1.206(3) . ? O3 C13 1.331(3) . ? O3 C14 1.456(2) . ? N1 C2 1.330(3) . ? N1 C3 1.332(3) . ? N2 C6 1.355(3) . ? N2 C5 1.411(2) . ? N2 H2A 0.8600 . ? C1 C2 1.377(3) . ? C1 C5 1.380(3) . ? C1 H1B 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.380(3) . ? C3 H3A 0.9300 . ? C4 C5 1.385(3) . ? C4 H4A 0.9300 . ? C6 C7 1.503(3) . ? C7 C8 1.382(3) . ? C7 C12 1.390(3) . ? C8 C9 1.384(3) . ? C8 H8A 0.9300 . ? C9 C10 1.378(3) . ? C9 H9A 0.9300 . ? C10 C11 1.377(3) . ? C10 C13 1.493(3) . ? C11 C12 1.382(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O4 H4C 0.8501 . ? O4 H4D 0.8500 . ? O5 H5C 0.8500 . ? O5 H5D 0.8500 . ? 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 C13 O3 C14 116.11(19) . . ? C2 N1 C3 115.74(19) . . ? C6 N2 C5 126.34(19) . . ? C6 N2 H2A 116.8 . . ? C5 N2 H2A 116.8 . . ? C2 C1 C5 119.1(2) . . ? C2 C1 H1B 120.5 . . ? C5 C1 H1B 120.5 . . ? N1 C2 C1 124.3(2) . . ? N1 C2 H2B 117.8 . . ? C1 C2 H2B 117.8 . . ? N1 C3 C4 124.6(2) . . ? N1 C3 H3A 117.7 . . ? C4 C3 H3A 117.7 . . ? C3 C4 C5 118.4(2) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C1 C5 C4 117.76(19) . . ? C1 C5 N2 117.41(19) . . ? C4 C5 N2 124.80(19) . . ? O1 C6 N2 122.6(2) . . ? O1 C6 C7 120.4(2) . . ? N2 C6 C7 117.0(2) . . ? C8 C7 C12 118.63(19) . . ? C8 C7 C6 124.3(2) . . ? C12 C7 C6 117.1(2) . . ? C7 C8 C9 120.4(2) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C10 C9 C8 120.6(2) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.4(2) . . ? C11 C10 C13 122.6(2) . . ? C9 C10 C13 118.0(2) . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C7 120.7(2) . . ? C11 C12 H12A 119.6 . . ? C7 C12 H12A 119.6 . . ? O2 C13 O3 124.1(2) . . ? O2 C13 C10 124.1(2) . . ? O3 C13 C10 111.8(2) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? H4C O4 H4D 108.5 . . ? H5C O5 H5D 108.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.125 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.039 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 888035' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 Ag4 N12 O24' _chemical_formula_weight 1704.54 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1294(2) _cell_length_b 11.4747(2) _cell_length_c 15.7778(3) _cell_angle_alpha 95.4790(10) _cell_angle_beta 102.8020(10) _cell_angle_gamma 90.9920(10) _cell_volume 1427.53(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.28 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6827 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25304 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7039 _reflns_number_gt 5169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0218P)^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_number_reflns 7039 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.85782(2) -0.776740(17) 0.023620(13) 0.01743(5) Uani 1 1 d . . . Ag2 Ag 0.49606(2) -1.050330(17) -0.099440(13) 0.01702(5) Uani 1 1 d . . . N1 N 0.9570(2) -0.60814(18) 0.09641(13) 0.0138(5) Uani 1 1 d . . . N2 N 1.1675(2) -0.69566(18) 0.18961(13) 0.0149(5) Uani 1 1 d . . . H2A H 1.1400 -0.7574 0.1533 0.018 Uiso 1 1 calc R . . N3 N 0.3907(2) -1.22949(18) -0.15730(13) 0.0141(5) Uani 1 1 d . . . N4 N 0.1758(3) -1.15361(18) -0.25484(13) 0.0149(5) Uani 1 1 d . . . H4A H 0.1903 -1.0929 -0.2171 0.018 Uiso 1 1 calc R . . N5 N 1.1301(3) -0.92908(18) -0.04276(13) 0.0136(5) Uani 1 1 d . . . N6 N 0.5116(3) -0.78062(19) -0.09177(14) 0.0171(5) Uani 1 1 d . . . O1 O 1.3332(2) -0.62967(16) 0.32282(11) 0.0224(5) Uani 1 1 d . . . O2 O 1.4260(2) -1.26643(16) 0.28936(13) 0.0284(5) Uani 1 1 d . . . O3 O 1.5842(2) -1.17917(16) 0.41512(12) 0.0217(5) Uani 1 1 d . . . O4 O 0.0213(2) -1.22274(16) -0.38962(12) 0.0265(5) Uani 1 1 d . . . O5 O 0.0076(2) -0.58619(16) -0.38324(12) 0.0218(5) Uani 1 1 d . . . O6 O -0.2321(2) -0.66452(15) -0.47227(11) 0.0183(4) Uani 1 1 d . . . O7 O 0.9799(2) -0.90272(16) -0.07164(11) 0.0193(4) Uani 1 1 d . . . O8 O 1.2198(2) -0.86981(16) 0.02193(11) 0.0181(4) Uani 1 1 d . . . O9 O 1.1864(2) -1.01684(15) -0.07987(11) 0.0166(4) Uani 1 1 d . . . O10 O 0.5997(2) -0.86587(15) -0.05843(11) 0.0171(4) Uani 1 1 d . . . O11 O 0.5757(2) -0.68093(16) -0.07300(12) 0.0261(5) Uani 1 1 d . . . O12 O 0.3707(2) -0.80367(16) -0.13920(12) 0.0252(5) Uani 1 1 d . . . C1 C 0.8778(3) -0.5124(2) 0.06744(17) 0.0163(6) Uani 1 1 d . . . H1A H 0.7835 -0.5229 0.0213 0.020 Uiso 1 1 calc R . . C2 C 0.9291(3) -0.4008(2) 0.10258(17) 0.0177(6) Uani 1 1 d . . . H2B H 0.8686 -0.3370 0.0825 0.021 Uiso 1 1 calc R . . C3 C 1.0739(3) -0.3851(2) 0.16903(18) 0.0207(6) Uani 1 1 d . . . H3A H 1.1144 -0.3098 0.1924 0.025 Uiso 1 1 calc R . . C4 C 1.1573(3) -0.4806(2) 0.20024(17) 0.0168(6) Uani 1 1 d . . . H4B H 1.2536 -0.4712 0.2452 0.020 Uiso 1 1 calc R . . C5 C 1.0946(3) -0.5916(2) 0.16306(16) 0.0137(6) Uani 1 1 d . . . C6 C 1.2781(3) -0.7101(2) 0.26702(16) 0.0145(6) Uani 1 1 d . . . C7 C 1.3292(3) -0.8336(2) 0.27971(16) 0.0152(6) Uani 1 1 d . . . C8 C 1.4580(3) -0.8493(2) 0.35196(18) 0.0244(7) Uani 1 1 d . . . H8A H 1.5112 -0.7844 0.3881 0.029 Uiso 1 1 calc R . . C9 C 1.5069(4) -0.9602(2) 0.37026(19) 0.0265(7) Uani 1 1 d . . . H9A H 1.5913 -0.9694 0.4194 0.032 Uiso 1 1 calc R . . C10 C 1.4318(3) -1.0582(2) 0.31628(17) 0.0177(6) Uani 1 1 d . . . C11 C 1.3062(3) -1.0437(2) 0.24340(16) 0.0147(6) Uani 1 1 d . . . H11A H 1.2560 -1.1088 0.2066 0.018 Uiso 1 1 calc R . . C12 C 1.2548(3) -0.9326(2) 0.22501(16) 0.0155(6) Uani 1 1 d . . . H12A H 1.1701 -0.9238 0.1759 0.019 Uiso 1 1 calc R . . C13 C 1.4781(3) -1.1796(2) 0.33614(17) 0.0187(6) Uani 1 1 d . . . C14 C 1.6359(3) -1.2929(2) 0.44023(18) 0.0230(7) Uani 1 1 d . . . H14A H 1.7117 -1.2840 0.4967 0.034 Uiso 1 1 calc R . . H14B H 1.6920 -1.3306 0.3982 0.034 Uiso 1 1 calc R . . H14C H 1.5384 -1.3398 0.4425 0.034 Uiso 1 1 calc R . . C15 C 0.4773(3) -1.3205(2) -0.12545(17) 0.0149(6) Uani 1 1 d . . . H15A H 0.5648 -1.3055 -0.0762 0.018 Uiso 1 1 calc R . . C16 C 0.4434(3) -1.4346(2) -0.16183(17) 0.0182(6) Uani 1 1 d . . . H16A H 0.5066 -1.4954 -0.1382 0.022 Uiso 1 1 calc R . . C17 C 0.3118(3) -1.4560(2) -0.23486(17) 0.0179(6) Uani 1 1 d . . . H17A H 0.2866 -1.5321 -0.2613 0.021 Uiso 1 1 calc R . . C18 C 0.2185(3) -1.3656(2) -0.26833(17) 0.0148(6) Uani 1 1 d . . . H18A H 0.1292 -1.3794 -0.3169 0.018 Uiso 1 1 calc R . . C19 C 0.2613(3) -1.2534(2) -0.22767(16) 0.0130(6) Uani 1 1 d . . . C20 C 0.0716(3) -1.1415(2) -0.33470(17) 0.0161(6) Uani 1 1 d . . . C21 C 0.0279(3) -1.0173(2) -0.34942(16) 0.0144(6) Uani 1 1 d . . . C22 C -0.1030(3) -0.9994(2) -0.41956(18) 0.0244(7) Uani 1 1 d . . . H22A H -0.1637 -1.0633 -0.4537 0.029 Uiso 1 1 calc R . . C23 C -0.1429(3) -0.8875(2) -0.43859(18) 0.0256(7) Uani 1 1 d . . . H23A H -0.2320 -0.8764 -0.4851 0.031 Uiso 1 1 calc R . . C24 C -0.0533(3) -0.7918(2) -0.38995(17) 0.0145(6) Uani 1 1 d . . . C25 C 0.0772(3) -0.8089(2) -0.31987(17) 0.0185(6) Uani 1 1 d . . . H25A H 0.1384 -0.7449 -0.2862 0.022 Uiso 1 1 calc R . . C26 C 0.1166(3) -0.9210(2) -0.29995(17) 0.0194(6) Uani 1 1 d . . . H26A H 0.2040 -0.9319 -0.2526 0.023 Uiso 1 1 calc R . . C27 C -0.0864(3) -0.6695(2) -0.41342(17) 0.0157(6) Uani 1 1 d . . . C28 C -0.2663(3) -0.5506(2) -0.50238(18) 0.0210(6) Uani 1 1 d . . . H28A H -0.3698 -0.5553 -0.5461 0.031 Uiso 1 1 calc R . . H28B H -0.1755 -0.5250 -0.5269 0.031 Uiso 1 1 calc R . . H28C H -0.2763 -0.4956 -0.4541 0.031 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 0.01602(10) 0.01246(11) 0.02007(11) -0.00277(9) -0.00212(9) 0.00106(8) Ag2 0.01634(10) 0.01135(11) 0.02074(11) -0.00074(9) -0.00039(9) -0.00026(8) N1 0.0133(10) 0.0118(11) 0.0154(11) 0.0004(9) 0.0019(9) -0.0022(9) N2 0.0158(11) 0.0094(11) 0.0165(11) -0.0017(9) -0.0015(9) -0.0011(9) N3 0.0118(10) 0.0144(12) 0.0161(11) 0.0040(10) 0.0020(9) 0.0008(9) N4 0.0198(11) 0.0106(11) 0.0126(11) -0.0024(9) 0.0012(9) 0.0010(9) N5 0.0148(11) 0.0112(11) 0.0144(11) 0.0030(10) 0.0020(9) -0.0004(9) N6 0.0199(11) 0.0144(12) 0.0159(12) 0.0013(10) 0.0019(10) 0.0001(10) O1 0.0320(11) 0.0161(10) 0.0152(10) -0.0024(8) -0.0011(9) -0.0006(9) O2 0.0336(11) 0.0142(10) 0.0294(12) -0.0016(9) -0.0083(10) -0.0003(9) O3 0.0257(10) 0.0137(10) 0.0215(10) 0.0027(8) -0.0042(9) 0.0039(8) O4 0.0401(12) 0.0139(10) 0.0188(10) -0.0005(9) -0.0066(9) 0.0031(9) O5 0.0235(10) 0.0148(10) 0.0242(11) 0.0030(9) -0.0010(9) -0.0022(8) O6 0.0163(9) 0.0151(10) 0.0215(10) 0.0055(8) -0.0012(8) 0.0007(8) O7 0.0117(9) 0.0211(10) 0.0212(10) -0.0036(9) -0.0026(8) 0.0053(8) O8 0.0155(9) 0.0179(10) 0.0164(10) -0.0049(8) -0.0031(8) -0.0021(8) O9 0.0202(9) 0.0105(9) 0.0190(10) -0.0017(8) 0.0050(8) 0.0048(8) O10 0.0159(9) 0.0117(9) 0.0212(10) 0.0034(8) -0.0024(8) 0.0030(8) O11 0.0348(11) 0.0118(10) 0.0262(11) 0.0016(9) -0.0041(9) -0.0050(9) O12 0.0161(10) 0.0241(11) 0.0298(11) 0.0049(9) -0.0080(9) -0.0002(9) C1 0.0149(13) 0.0167(14) 0.0187(14) 0.0036(12) 0.0061(11) 0.0013(11) C2 0.0200(13) 0.0135(14) 0.0213(14) 0.0039(12) 0.0067(12) 0.0037(11) C3 0.0246(14) 0.0131(14) 0.0248(15) -0.0010(12) 0.0081(12) -0.0044(12) C4 0.0139(13) 0.0156(14) 0.0190(14) -0.0020(12) 0.0011(11) -0.0018(11) C5 0.0153(12) 0.0123(13) 0.0155(13) 0.0014(11) 0.0075(11) 0.0012(11) C6 0.0131(12) 0.0165(14) 0.0134(13) 0.0015(12) 0.0020(11) -0.0024(11) C7 0.0167(13) 0.0137(14) 0.0152(13) -0.0007(11) 0.0048(11) -0.0013(11) C8 0.0251(15) 0.0140(15) 0.0255(16) -0.0052(13) -0.0094(13) -0.0014(12) C9 0.0277(16) 0.0174(15) 0.0249(16) 0.0007(13) -0.0139(13) 0.0026(13) C10 0.0179(13) 0.0133(14) 0.0189(14) -0.0016(12) -0.0006(11) 0.0021(11) C11 0.0173(13) 0.0139(14) 0.0102(13) -0.0045(11) 0.0001(11) -0.0028(11) C12 0.0175(13) 0.0168(14) 0.0113(13) 0.0003(11) 0.0018(11) -0.0021(11) C13 0.0158(13) 0.0183(15) 0.0198(15) 0.0010(13) -0.0003(12) 0.0011(12) C14 0.0250(15) 0.0164(15) 0.0271(16) 0.0077(13) 0.0026(13) 0.0036(12) C15 0.0111(12) 0.0162(14) 0.0171(14) 0.0039(12) 0.0018(11) 0.0008(11) C16 0.0186(13) 0.0142(14) 0.0235(15) 0.0050(12) 0.0068(12) 0.0041(11) C17 0.0229(14) 0.0112(14) 0.0203(14) -0.0010(12) 0.0075(12) -0.0004(11) C18 0.0144(12) 0.0144(14) 0.0156(13) 0.0004(11) 0.0041(11) -0.0007(11) C19 0.0142(12) 0.0134(13) 0.0131(13) 0.0041(11) 0.0051(11) 0.0015(11) C20 0.0154(13) 0.0177(14) 0.0152(14) 0.0026(12) 0.0031(11) -0.0007(11) C21 0.0122(12) 0.0147(14) 0.0163(13) 0.0017(11) 0.0037(11) 0.0004(11) C22 0.0263(15) 0.0134(14) 0.0264(16) -0.0019(13) -0.0071(13) -0.0035(12) C23 0.0248(15) 0.0199(16) 0.0252(16) 0.0010(13) -0.0090(13) 0.0010(13) C24 0.0135(12) 0.0136(14) 0.0180(14) 0.0032(11) 0.0065(11) 0.0006(11) C25 0.0195(14) 0.0150(14) 0.0171(14) 0.0002(12) -0.0031(11) -0.0026(11) C26 0.0162(13) 0.0207(15) 0.0188(14) 0.0058(12) -0.0035(11) 0.0025(12) C27 0.0148(13) 0.0187(15) 0.0148(13) 0.0023(12) 0.0052(11) 0.0029(11) C28 0.0234(14) 0.0168(15) 0.0226(15) 0.0046(12) 0.0035(12) 0.0047(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.196(2) . ? Ag1 O10 2.3652(17) . ? Ag1 O7 2.3724(18) . ? Ag2 N3 2.242(2) . ? Ag2 O10 2.2458(17) . ? Ag2 O8 2.5896(17) 2_735 ? Ag2 Ag2 3.2251(4) 2_635 ? N1 C1 1.350(3) . ? N1 C5 1.352(3) . ? N2 C6 1.373(3) . ? N2 C5 1.401(3) . ? N2 H2A 0.8600 . ? N3 C15 1.344(3) . ? N3 C19 1.352(3) . ? N4 C20 1.374(3) . ? N4 C19 1.402(3) . ? N4 H4A 0.8600 . ? N5 O8 1.248(2) . ? N5 O7 1.258(2) . ? N5 O9 1.260(3) . ? N6 O11 1.230(3) . ? N6 O12 1.231(3) . ? N6 O10 1.305(3) . ? O1 C6 1.218(3) . ? O2 C13 1.193(3) . ? O3 C13 1.349(3) . ? O3 C14 1.442(3) . ? O4 C20 1.209(3) . ? O5 C27 1.205(3) . ? O6 C27 1.339(3) . ? O6 C28 1.444(3) . ? O8 Ag2 2.5896(17) 2_735 ? C1 C2 1.365(3) . ? C1 H1A 0.9300 . ? C2 C3 1.388(4) . ? C2 H2B 0.9300 . ? C3 C4 1.373(4) . ? C3 H3A 0.9300 . ? C4 C5 1.388(3) . ? C4 H4B 0.9300 . ? C6 C7 1.503(4) . ? C7 C8 1.394(4) . ? C7 C12 1.400(3) . ? C8 C9 1.377(4) . ? C8 H8A 0.9300 . ? C9 C10 1.388(4) . ? C9 H9A 0.9300 . ? C10 C11 1.384(3) . ? C10 C13 1.493(4) . ? C11 C12 1.385(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.377(3) . ? C15 H15A 0.9300 . ? C16 C17 1.387(4) . ? C16 H16A 0.9300 . ? C17 C18 1.372(3) . ? C17 H17A 0.9300 . ? C18 C19 1.386(3) . ? C18 H18A 0.9300 . ? C20 C21 1.502(4) . ? C21 C26 1.381(3) . ? C21 C22 1.389(4) . ? C22 C23 1.375(4) . ? C22 H22A 0.9300 . ? C23 C24 1.375(4) . ? C23 H23A 0.9300 . ? C24 C25 1.384(3) . ? C24 C27 1.499(4) . ? C25 C26 1.379(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 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 O10 139.60(7) . . ? N1 Ag1 O7 129.07(7) . . ? O10 Ag1 O7 84.19(6) . . ? N3 Ag2 O10 172.95(7) . . ? N3 Ag2 O8 92.79(6) . 2_735 ? O10 Ag2 O8 90.23(6) . 2_735 ? N3 Ag2 Ag2 123.11(5) . 2_635 ? O10 Ag2 Ag2 63.70(5) . 2_635 ? O8 Ag2 Ag2 80.36(4) 2_735 2_635 ? C1 N1 C5 117.8(2) . . ? C1 N1 Ag1 115.96(16) . . ? C5 N1 Ag1 126.12(17) . . ? C6 N2 C5 127.3(2) . . ? C6 N2 H2A 116.4 . . ? C5 N2 H2A 116.4 . . ? C15 N3 C19 117.4(2) . . ? C15 N3 Ag2 116.40(16) . . ? C19 N3 Ag2 125.72(16) . . ? C20 N4 C19 127.6(2) . . ? C20 N4 H4A 116.2 . . ? C19 N4 H4A 116.2 . . ? O8 N5 O7 120.2(2) . . ? O8 N5 O9 121.2(2) . . ? O7 N5 O9 118.6(2) . . ? O11 N6 O12 123.9(2) . . ? O11 N6 O10 117.2(2) . . ? O12 N6 O10 118.9(2) . . ? C13 O3 C14 115.3(2) . . ? C27 O6 C28 114.7(2) . . ? N5 O7 Ag1 116.37(14) . . ? N5 O8 Ag2 119.35(15) . 2_735 ? N6 O10 Ag2 118.23(14) . . ? N6 O10 Ag1 105.51(13) . . ? Ag2 O10 Ag1 135.85(8) . . ? N1 C1 C2 123.2(2) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 118.2(2) . . ? C1 C2 H2B 120.9 . . ? C3 C2 H2B 120.9 . . ? C4 C3 C2 120.0(2) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 118.5(2) . . ? C3 C4 H4B 120.8 . . ? C5 C4 H4B 120.8 . . ? N1 C5 C4 122.2(2) . . ? N1 C5 N2 113.9(2) . . ? C4 C5 N2 123.8(2) . . ? O1 C6 N2 123.4(2) . . ? O1 C6 C7 120.9(2) . . ? N2 C6 C7 115.6(2) . . ? C8 C7 C12 118.5(2) . . ? C8 C7 C6 117.0(2) . . ? C12 C7 C6 124.5(2) . . ? C9 C8 C7 120.5(2) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.8(2) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 119.2(2) . . ? C11 C10 C13 118.8(2) . . ? C9 C10 C13 121.9(2) . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.5(2) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? O2 C13 O3 123.9(2) . . ? O2 C13 C10 124.8(2) . . ? O3 C13 C10 111.3(2) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 123.5(2) . . ? N3 C15 H15A 118.2 . . ? C16 C15 H15A 118.2 . . ? C15 C16 C17 117.7(2) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C19 118.0(2) . . ? C17 C18 H18A 121.0 . . ? C19 C18 H18A 121.0 . . ? N3 C19 C18 122.9(2) . . ? N3 C19 N4 113.3(2) . . ? C18 C19 N4 123.8(2) . . ? O4 C20 N4 123.6(2) . . ? O4 C20 C21 122.3(2) . . ? N4 C20 C21 114.2(2) . . ? C26 C21 C22 118.8(2) . . ? C26 C21 C20 123.5(2) . . ? C22 C21 C20 117.7(2) . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C25 119.2(2) . . ? C23 C24 C27 121.9(2) . . ? C25 C24 C27 118.8(2) . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C21 120.9(2) . . ? C25 C26 H26A 119.5 . . ? C21 C26 H26A 119.5 . . ? O5 C27 O6 124.3(2) . . ? O5 C27 C24 123.9(2) . . ? O6 C27 C24 111.8(2) . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.622 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.116 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 888036' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag2 N6 O12' _chemical_formula_weight 852.27 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.28700(10) _cell_length_b 9.2477(2) _cell_length_c 15.5312(3) _cell_angle_alpha 76.3060(10) _cell_angle_beta 85.8970(10) _cell_angle_gamma 89.3840(10) _cell_volume 735.87(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8704 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8013 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12889 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3618 _reflns_number_gt 3148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0290P)^2^+0.2118P] 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 3618 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 1.0000 0.0000 0.04635(8) Uani 1 2 d S . . Ag2 Ag 1.0000 0.5000 0.0000 0.0813(15) Uani 0.50 2 d SP . 1 Ag2' Ag 0.9930(11) 0.5109(7) 0.0171(5) 0.0819(10) Uani 0.25 1 d P . 2 O1 O -0.4121(2) 0.48522(15) 0.27219(11) 0.0528(4) Uani 1 1 d . . . O2 O -0.1462(3) -0.25368(18) 0.47081(13) 0.0750(5) Uani 1 1 d . . . O3 O 0.2314(3) -0.22457(15) 0.39572(10) 0.0578(4) Uani 1 1 d . . . N1 N 0.1926(3) 0.90118(15) 0.09769(10) 0.0360(3) Uani 1 1 d . . . N2 N 0.0051(3) 0.53625(16) 0.23515(11) 0.0413(4) Uani 1 1 d . . . H2A H 0.1542 0.4980 0.2371 0.050 Uiso 1 1 calc R . . C1 C -0.0016(3) 0.98573(19) 0.11707(12) 0.0382(4) Uani 1 1 d . . . H1A H -0.0004 1.0867 0.0896 0.046 Uiso 1 1 calc R . . C2 C -0.2014(3) 0.9282(2) 0.17601(13) 0.0400(4) Uani 1 1 d . . . H2B H -0.3319 0.9902 0.1882 0.048 Uiso 1 1 calc R . . C3 C -0.2095(3) 0.7789(2) 0.21714(12) 0.0395(4) Uani 1 1 d . . . H3A H -0.3437 0.7388 0.2574 0.047 Uiso 1 1 calc R . . C4 C -0.0114(3) 0.68970(18) 0.19676(12) 0.0345(4) Uani 1 1 d . . . C5 C 0.1856(3) 0.75532(18) 0.13716(12) 0.0357(4) Uani 1 1 d . . . H5A H 0.3187 0.6958 0.1239 0.043 Uiso 1 1 calc R . . C6 C -0.1927(3) 0.44309(19) 0.26935(12) 0.0376(4) Uani 1 1 d . . . C7 C -0.1259(3) 0.28340(19) 0.30625(12) 0.0363(4) Uani 1 1 d . . . C8 C -0.3020(4) 0.1969(2) 0.36697(14) 0.0474(5) Uani 1 1 d . . . H8A H -0.4525 0.2392 0.3836 0.057 Uiso 1 1 calc R . . C9 C -0.2552(4) 0.0488(2) 0.40276(14) 0.0504(5) Uani 1 1 d . . . H9A H -0.3748 -0.0082 0.4432 0.060 Uiso 1 1 calc R . . C10 C -0.0321(4) -0.0158(2) 0.37909(12) 0.0392(4) Uani 1 1 d . . . C11 C 0.1427(4) 0.0693(2) 0.31823(13) 0.0435(4) Uani 1 1 d . . . H11A H 0.2924 0.0263 0.3015 0.052 Uiso 1 1 calc R . . C12 C 0.0967(4) 0.2180(2) 0.28201(13) 0.0437(4) Uani 1 1 d . . . H12A H 0.2158 0.2745 0.2412 0.052 Uiso 1 1 calc R . . C13 C 0.0061(4) -0.1767(2) 0.42037(13) 0.0463(4) Uani 1 1 d . . . C14 C 0.2860(5) -0.3787(2) 0.43547(17) 0.0662(7) Uani 1 1 d . . . H14A H 0.4519 -0.4029 0.4138 0.099 Uiso 1 1 calc R . . H14B H 0.1622 -0.4417 0.4201 0.099 Uiso 1 1 calc R . . H14C H 0.2803 -0.3937 0.4989 0.099 Uiso 1 1 calc R . . N3 N 1.4238(3) 0.32815(17) 0.05839(12) 0.0471(4) Uani 1 1 d . . . O4 O 1.3347(3) 0.43564(15) 0.08695(10) 0.0541(4) Uani 1 1 d . . . O5 O 1.3077(3) 0.28507(17) 0.00176(12) 0.0637(4) Uani 1 1 d . . . O6 O 1.6225(4) 0.2695(2) 0.08409(14) 0.0839(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04152(13) 0.03286(11) 0.05850(15) -0.00373(9) 0.01486(9) -0.00479(8) Ag2 0.0397(13) 0.084(2) 0.109(3) 0.005(2) -0.0209(13) 0.0079(14) Ag2' 0.0617(18) 0.093(2) 0.0984(19) -0.0334(19) -0.0225(13) 0.0313(15) O1 0.0336(7) 0.0405(7) 0.0798(10) -0.0075(7) 0.0031(7) -0.0018(6) O2 0.0619(10) 0.0469(9) 0.0952(13) 0.0194(9) 0.0148(10) -0.0079(7) O3 0.0620(10) 0.0355(7) 0.0651(9) 0.0057(7) 0.0089(8) 0.0032(7) N1 0.0328(7) 0.0286(7) 0.0441(8) -0.0051(6) 0.0022(6) -0.0011(6) N2 0.0307(7) 0.0306(7) 0.0560(9) 0.0000(7) 0.0058(7) 0.0015(6) C1 0.0376(9) 0.0285(8) 0.0475(10) -0.0073(7) -0.0032(8) 0.0036(7) C2 0.0327(9) 0.0365(9) 0.0504(10) -0.0116(8) 0.0019(8) 0.0066(7) C3 0.0323(9) 0.0385(9) 0.0452(10) -0.0073(8) 0.0061(8) -0.0004(7) C4 0.0329(8) 0.0292(8) 0.0393(9) -0.0041(7) -0.0007(7) -0.0001(7) C5 0.0303(8) 0.0292(8) 0.0467(10) -0.0087(7) 0.0028(7) 0.0011(7) C6 0.0364(9) 0.0339(9) 0.0411(9) -0.0075(7) 0.0010(7) -0.0023(7) C7 0.0363(9) 0.0333(8) 0.0372(9) -0.0043(7) -0.0006(7) -0.0047(7) C8 0.0395(10) 0.0439(10) 0.0538(11) -0.0053(9) 0.0102(9) -0.0030(8) C9 0.0481(11) 0.0418(10) 0.0513(11) 0.0045(9) 0.0122(9) -0.0086(9) C10 0.0425(10) 0.0338(9) 0.0376(9) -0.0009(7) -0.0024(8) -0.0058(7) C11 0.0414(10) 0.0352(9) 0.0489(11) -0.0025(8) 0.0056(8) -0.0008(8) C12 0.0422(10) 0.0356(9) 0.0461(10) 0.0010(8) 0.0095(8) -0.0051(8) C13 0.0491(11) 0.0374(10) 0.0473(11) 0.0006(8) -0.0051(9) -0.0069(8) C14 0.0803(17) 0.0335(10) 0.0743(16) 0.0043(10) 0.0051(13) 0.0090(11) N3 0.0465(9) 0.0292(7) 0.0580(10) 0.0003(7) 0.0100(8) 0.0060(7) O4 0.0640(10) 0.0403(7) 0.0570(9) -0.0127(7) 0.0051(7) 0.0134(7) O5 0.0623(10) 0.0475(8) 0.0852(12) -0.0254(8) 0.0015(9) -0.0058(7) O6 0.0697(12) 0.0710(12) 0.1044(15) -0.0063(11) -0.0174(11) 0.0377(10) _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 2.1911(14) 2_675 ? Ag1 N1 2.1911(14) . ? Ag2 O4 2.2909(16) 2_765 ? Ag2 O4 2.2909(16) . ? Ag2 O5 2.5513(15) 2_765 ? Ag2 O5 2.5513(15) . ? Ag2' Ag2' 0.610(14) 2_765 ? Ag2' O4 2.196(7) . ? Ag2' O4 2.421(8) 2_765 ? Ag2' O5 2.432(6) 2_765 ? O1 C6 1.221(2) . ? O2 C13 1.195(2) . ? O3 C13 1.329(3) . ? O3 C14 1.448(2) . ? N1 C5 1.343(2) . ? N1 C1 1.344(2) . ? N2 C6 1.357(2) . ? N2 C4 1.407(2) . ? N2 H2A 0.8600 . ? C1 C2 1.371(3) . ? C1 H1A 0.9300 . ? C2 C3 1.377(2) . ? C2 H2B 0.9300 . ? C3 C4 1.391(2) . ? C3 H3A 0.9300 . ? C4 C5 1.386(2) . ? C5 H5A 0.9300 . ? C6 C7 1.500(2) . ? C7 C12 1.386(3) . ? C7 C8 1.389(3) . ? C8 C9 1.378(3) . ? C8 H8A 0.9300 . ? C9 C10 1.382(3) . ? C9 H9A 0.9300 . ? C10 C11 1.380(2) . ? C10 C13 1.492(3) . ? C11 C12 1.383(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N3 O6 1.226(2) . ? N3 O5 1.248(2) . ? N3 O4 1.255(2) . ? O4 Ag2' 2.421(8) 2_765 ? O5 Ag2' 2.432(6) 2_765 ? 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 180.0 2_675 . ? O4 Ag2 O4 180.00(11) 2_765 . ? O4 Ag2 O5 52.33(5) 2_765 2_765 ? O4 Ag2 O5 127.67(5) . 2_765 ? O4 Ag2 O5 127.67(5) 2_765 . ? O4 Ag2 O5 52.33(5) . . ? O5 Ag2 O5 180.0 2_765 . ? Ag2' Ag2' O4 104.4(12) 2_765 . ? Ag2' Ag2' O4 61.4(12) 2_765 2_765 ? O4 Ag2' O4 165.9(3) . 2_765 ? Ag2' Ag2' O5 109.8(14) 2_765 2_765 ? O4 Ag2' O5 139.9(3) . 2_765 ? O4 Ag2' O5 52.54(15) 2_765 2_765 ? C13 O3 C14 115.53(17) . . ? C5 N1 C1 117.97(15) . . ? C5 N1 Ag1 121.89(11) . . ? C1 N1 Ag1 120.09(11) . . ? C6 N2 C4 125.98(15) . . ? C6 N2 H2A 117.0 . . ? C4 N2 H2A 117.0 . . ? N1 C1 C2 122.22(16) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 120.21(16) . . ? C1 C2 H2B 119.9 . . ? C3 C2 H2B 119.9 . . ? C2 C3 C4 118.16(16) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C5 C4 C3 118.63(15) . . ? C5 C4 N2 117.55(15) . . ? C3 C4 N2 123.79(15) . . ? N1 C5 C4 122.80(15) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O1 C6 N2 122.89(17) . . ? O1 C6 C7 121.20(16) . . ? N2 C6 C7 115.89(15) . . ? C12 C7 C8 118.88(17) . . ? C12 C7 C6 123.91(16) . . ? C8 C7 C6 117.20(16) . . ? C9 C8 C7 120.46(18) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.53(17) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 119.28(17) . . ? C11 C10 C13 123.02(18) . . ? C9 C10 C13 117.70(17) . . ? C10 C11 C12 120.45(18) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.39(17) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? O2 C13 O3 123.55(19) . . ? O2 C13 C10 124.2(2) . . ? O3 C13 C10 112.26(16) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 N3 O5 121.04(18) . . ? O6 N3 O4 120.7(2) . . ? O5 N3 O4 118.21(17) . . ? N3 O4 Ag2' 107.6(2) . . ? N3 O4 Ag2 100.78(13) . . ? Ag2' O4 Ag2 7.41(17) . . ? N3 O4 Ag2' 94.55(18) . 2_765 ? Ag2' O4 Ag2' 14.1(3) . 2_765 ? Ag2 O4 Ag2' 6.71(14) . 2_765 ? N3 O5 Ag2' 94.2(2) . 2_765 ? N3 O5 Ag2 88.50(10) . . ? Ag2' O5 Ag2 6.46(19) 2_765 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.305 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.051 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 888037' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag Cl N4 O10' _chemical_formula_weight 719.83 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.2148(4) _cell_length_b 5.56930(10) _cell_length_c 16.1812(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.6650(10) _cell_angle_gamma 90.00 _cell_volume 2773.09(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6853 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8960 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12383 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 28.32 _reflns_number_total 3454 _reflns_number_gt 2634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0497P)^2^+1.8228P] 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 0.00049(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3454 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.5000 0.0000 0.0000 0.06997(13) Uani 1 2 d S . . O1 O 0.62890(6) -0.2146(3) 0.23386(10) 0.0641(4) Uani 1 1 d . . . O2 O 0.73210(8) -0.6072(4) 0.62853(12) 0.0906(6) Uani 1 1 d . . . O3 O 0.69680(6) -0.9539(3) 0.60307(9) 0.0613(4) Uani 1 1 d . . . N1 N 0.54426(6) -0.3007(3) 0.01678(11) 0.0527(4) Uani 1 1 d . . . N2 N 0.61083(6) -0.5975(4) 0.19645(10) 0.0528(4) Uani 1 1 d . . . H2A H 0.6127 -0.7447 0.2127 0.063 Uiso 1 1 calc R . . C1 C 0.54900(7) -0.4557(4) -0.04451(13) 0.0544(5) Uani 1 1 d . . . H1A H 0.5355 -0.4224 -0.0990 0.065 Uiso 1 1 calc R . . C2 C 0.57308(7) -0.6606(4) -0.02952(12) 0.0559(5) Uani 1 1 d . . . H2B H 0.5754 -0.7663 -0.0731 0.067 Uiso 1 1 calc R . . C3 C 0.59402(7) -0.7097(4) 0.05096(12) 0.0527(5) Uani 1 1 d . . . H3A H 0.6106 -0.8482 0.0623 0.063 Uiso 1 1 calc R . . C4 C 0.58985(7) -0.5493(4) 0.11409(12) 0.0464(4) Uani 1 1 d . . . C5 C 0.56443(7) -0.3479(4) 0.09485(13) 0.0516(5) Uani 1 1 d . . . H5A H 0.5612 -0.2411 0.1376 0.062 Uiso 1 1 calc R . . C6 C 0.62832(6) -0.4264(4) 0.25186(12) 0.0468(4) Uani 1 1 d . . . C7 C 0.64826(7) -0.5173(3) 0.33688(12) 0.0443(4) Uani 1 1 d . . . C8 C 0.67835(7) -0.3717(4) 0.38636(13) 0.0521(5) Uani 1 1 d . . . H8A H 0.6861 -0.2251 0.3656 0.063 Uiso 1 1 calc R . . C9 C 0.69677(8) -0.4426(4) 0.46586(14) 0.0548(5) Uani 1 1 d . . . H9A H 0.7165 -0.3425 0.4988 0.066 Uiso 1 1 calc R . . C10 C 0.68616(6) -0.6613(4) 0.49701(11) 0.0477(4) Uani 1 1 d . . . C11 C 0.65577(7) -0.8071(4) 0.44824(12) 0.0526(5) Uani 1 1 d . . . H11A H 0.6481 -0.9534 0.4692 0.063 Uiso 1 1 calc R . . C12 C 0.63698(7) -0.7351(4) 0.36860(12) 0.0521(5) Uani 1 1 d . . . H12A H 0.6167 -0.8334 0.3362 0.063 Uiso 1 1 calc R . . C13 C 0.70739(7) -0.7323(4) 0.58327(13) 0.0553(5) Uani 1 1 d . . . C14 C 0.71628(10) -1.0368(5) 0.68544(15) 0.0673(7) Uani 1 1 d . . . H14A H 0.7082 -1.2010 0.6923 0.101 Uiso 1 1 calc R . . H14B H 0.7063 -0.9394 0.7273 0.101 Uiso 1 1 calc R . . H14C H 0.7473 -1.0252 0.6915 0.101 Uiso 1 1 calc R . . Cl Cl 0.5000 -0.00756(14) 0.2500 0.0564(2) Uani 1 2 d S . . O4 O 0.5138(5) -0.2371(12) 0.2701(7) 0.217(8) Uani 0.50 1 d P . . O5 O 0.4883(5) 0.0895(16) 0.3193(4) 0.164(6) Uani 0.50 1 d P . . O6 O 0.4650(4) -0.0104(16) 0.1953(8) 0.198(5) Uani 0.50 1 d P . . O7 O 0.5289(3) 0.122(2) 0.2131(10) 0.197(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.05881(18) 0.06124(19) 0.0839(2) 0.00418(12) -0.00520(14) 0.00777(11) O1 0.0745(10) 0.0502(9) 0.0615(9) 0.0004(7) -0.0058(8) -0.0081(8) O2 0.1190(16) 0.0694(12) 0.0658(10) -0.0081(9) -0.0354(11) -0.0131(12) O3 0.0740(11) 0.0613(10) 0.0427(7) -0.0016(6) -0.0071(7) -0.0009(8) N1 0.0502(9) 0.0532(10) 0.0527(9) 0.0026(8) 0.0026(7) -0.0033(8) N2 0.0683(11) 0.0466(9) 0.0408(8) -0.0024(7) 0.0011(7) -0.0006(9) C1 0.0529(12) 0.0676(14) 0.0418(10) 0.0033(9) 0.0054(9) -0.0095(10) C2 0.0636(13) 0.0622(13) 0.0421(10) -0.0087(9) 0.0095(9) -0.0039(10) C3 0.0606(12) 0.0508(11) 0.0459(10) -0.0049(8) 0.0071(9) 0.0002(9) C4 0.0496(10) 0.0482(11) 0.0410(9) -0.0024(8) 0.0066(8) -0.0052(8) C5 0.0533(11) 0.0534(12) 0.0470(10) -0.0056(9) 0.0053(8) 0.0010(9) C6 0.0441(10) 0.0506(10) 0.0458(10) -0.0042(9) 0.0075(8) -0.0039(9) C7 0.0431(9) 0.0483(11) 0.0413(9) -0.0071(7) 0.0070(8) -0.0008(8) C8 0.0549(11) 0.0493(11) 0.0510(10) -0.0049(9) 0.0058(9) -0.0118(9) C9 0.0547(12) 0.0548(12) 0.0517(11) -0.0123(9) -0.0004(9) -0.0121(10) C10 0.0493(10) 0.0504(11) 0.0415(9) -0.0095(8) 0.0028(8) 0.0010(8) C11 0.0621(12) 0.0483(11) 0.0454(10) -0.0048(8) 0.0031(9) -0.0098(9) C12 0.0567(11) 0.0523(11) 0.0441(10) -0.0068(8) -0.0009(8) -0.0137(9) C13 0.0630(13) 0.0543(12) 0.0448(10) -0.0114(9) -0.0022(9) 0.0052(10) C14 0.0791(17) 0.0722(16) 0.0461(11) 0.0041(10) -0.0027(11) 0.0133(13) Cl 0.0604(4) 0.0713(5) 0.0359(3) 0.000 0.0036(3) 0.000 O4 0.37(2) 0.122(4) 0.193(13) 0.105(8) 0.150(13) 0.138(10) O5 0.353(17) 0.101(5) 0.045(2) -0.027(3) 0.056(5) -0.049(7) O6 0.166(8) 0.189(10) 0.188(9) -0.031(7) -0.120(7) -0.008(7) O7 0.135(6) 0.149(7) 0.350(16) 0.042(10) 0.167(9) -0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.1591(18) 5_655 ? Ag N1 2.1591(18) . ? O1 C6 1.216(3) . ? O2 C13 1.195(3) . ? O3 C13 1.331(3) . ? O3 C14 1.445(3) . ? N1 C5 1.339(3) . ? N1 C1 1.341(3) . ? N2 C6 1.359(3) . ? N2 C4 1.409(3) . ? N2 H2A 0.8600 . ? C1 C2 1.366(3) . ? C1 H1A 0.9300 . ? C2 C3 1.383(3) . ? C2 H2B 0.9300 . ? C3 C4 1.379(3) . ? C3 H3A 0.9300 . ? C4 C5 1.379(3) . ? C5 H5A 0.9300 . ? C6 C7 1.500(3) . ? C7 C12 1.385(3) . ? C7 C8 1.389(3) . ? C8 C9 1.376(3) . ? C8 H8A 0.9300 . ? C9 C10 1.379(3) . ? C9 H9A 0.9300 . ? C10 C11 1.389(3) . ? C10 C13 1.494(3) . ? C11 C12 1.383(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? Cl O6 1.285(6) 2_655 ? Cl O6 1.285(6) . ? Cl O5 1.349(7) . ? Cl O5 1.349(7) 2_655 ? Cl O7 1.369(6) 2_655 ? Cl O7 1.369(6) . ? Cl O4 1.371(6) 2_655 ? Cl O4 1.371(6) . ? O4 O4 0.99(3) 2_655 ? O4 O6 1.489(11) 2_655 ? O5 O7 0.708(16) 2_655 ? O5 O6 1.613(16) 2_655 ? O6 O4 1.489(11) 2_655 ? O6 O5 1.613(16) 2_655 ? O6 O7 1.639(15) 2_655 ? O7 O5 0.708(16) 2_655 ? O7 O6 1.639(15) 2_655 ? 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 N1 180.0 5_655 . ? C13 O3 C14 115.82(18) . . ? C5 N1 C1 118.59(19) . . ? C5 N1 Ag 117.39(14) . . ? C1 N1 Ag 123.62(15) . . ? C6 N2 C4 124.21(19) . . ? C6 N2 H2A 117.9 . . ? C4 N2 H2A 117.9 . . ? N1 C1 C2 122.1(2) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2B 120.3 . . ? C3 C2 H2B 120.3 . . ? C4 C3 C2 118.8(2) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C5 C4 C3 118.80(19) . . ? C5 C4 N2 121.80(18) . . ? C3 C4 N2 119.38(19) . . ? N1 C5 C4 122.26(19) . . ? N1 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? O1 C6 N2 122.9(2) . . ? O1 C6 C7 121.78(19) . . ? N2 C6 C7 115.31(19) . . ? C12 C7 C8 119.15(19) . . ? C12 C7 C6 122.91(18) . . ? C8 C7 C6 117.91(18) . . ? C9 C8 C7 120.5(2) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.44(19) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C11 119.42(19) . . ? C9 C10 C13 118.61(18) . . ? C11 C10 C13 121.95(19) . . ? C12 C11 C10 120.2(2) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C7 120.30(19) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? O2 C13 O3 123.7(2) . . ? O2 C13 C10 123.9(2) . . ? O3 C13 C10 112.42(18) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 Cl O6 178.6(8) 2_655 . ? O6 Cl O5 75.5(8) 2_655 . ? O6 Cl O5 105.1(8) . . ? O6 Cl O5 105.1(8) 2_655 2_655 ? O6 Cl O5 75.5(8) . 2_655 ? O5 Cl O5 132.7(7) . 2_655 ? O6 Cl O7 104.6(8) 2_655 2_655 ? O6 Cl O7 76.2(8) . 2_655 ? O5 Cl O7 30.2(7) . 2_655 ? O5 Cl O7 116.1(5) 2_655 2_655 ? O6 Cl O7 76.2(8) 2_655 . ? O6 Cl O7 104.6(8) . . ? O5 Cl O7 116.1(5) . . ? O5 Cl O7 30.2(7) 2_655 . ? O7 Cl O7 116.1(10) 2_655 . ? O6 Cl O4 110.5(8) 2_655 2_655 ? O6 Cl O4 68.1(6) . 2_655 ? O5 Cl O4 116.9(7) . 2_655 ? O5 Cl O4 107.1(7) 2_655 2_655 ? O7 Cl O4 113.1(8) 2_655 2_655 ? O7 Cl O4 126.4(9) . 2_655 ? O6 Cl O4 68.1(6) 2_655 . ? O6 Cl O4 110.5(8) . . ? O5 Cl O4 107.1(7) . . ? O5 Cl O4 116.9(7) 2_655 . ? O7 Cl O4 126.4(9) 2_655 . ? O7 Cl O4 113.1(8) . . ? O4 Cl O4 42.4(12) 2_655 . ? O4 O4 Cl 68.8(6) 2_655 . ? O4 O4 O6 121.9(5) 2_655 2_655 ? Cl O4 O6 53.2(3) . 2_655 ? O7 O5 Cl 76.4(9) 2_655 . ? O7 O5 O6 124.8(11) 2_655 2_655 ? Cl O5 O6 50.4(5) . 2_655 ? Cl O6 O4 58.7(5) . 2_655 ? Cl O6 O5 54.1(5) . 2_655 ? O4 O6 O5 89.6(9) 2_655 2_655 ? Cl O6 O7 54.2(4) . 2_655 ? O4 O6 O7 93.8(7) 2_655 2_655 ? O5 O6 O7 90.4(5) 2_655 2_655 ? O5 O7 Cl 73.4(10) 2_655 . ? O5 O7 O6 120.7(13) 2_655 2_655 ? Cl O7 O6 49.6(5) . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.413 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.050 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 888038' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Ag Cl N6 O10' _chemical_formula_weight 801.94 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 7.38710(10) _cell_length_b 11.65940(10) _cell_length_c 20.3813(3) _cell_angle_alpha 88.7040(10) _cell_angle_beta 79.7520(10) _cell_angle_gamma 79.0920(10) _cell_volume 1696.10(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.61 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8574 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30731 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8379 _reflns_number_gt 4494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0480P)^2^+0.4706P] 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 8379 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.63507(4) 0.58527(2) 0.515440(13) 0.07357(10) Uani 1 1 d . . . N1 N 0.4812(3) 0.74161(19) 0.47650(11) 0.0522(6) Uani 1 1 d . . . N2 N 0.3858(3) 0.85272(18) 0.31344(10) 0.0490(6) Uani 1 1 d . . . H2A H 0.2902 0.8967 0.3015 0.059 Uiso 1 1 calc R . . N3 N 0.8134(3) 0.43983(19) 0.55528(12) 0.0554(6) Uani 1 1 d . . . N4 N 0.9201(3) 0.34877(19) 0.72005(11) 0.0559(6) Uani 1 1 d . . . H4A H 1.0105 0.3017 0.7333 0.067 Uiso 1 1 calc R . . O1 O 0.6600(3) 0.73051(18) 0.27491(9) 0.0635(6) Uani 1 1 d . . . O2 O 0.2672(3) 0.94487(19) -0.01700(10) 0.0721(6) Uani 1 1 d . . . O3 O 0.4800(4) 0.7870(2) -0.05106(11) 0.0936(8) Uani 1 1 d . . . O4 O 0.6610(4) 0.4809(3) 0.75438(13) 0.1114(10) Uani 1 1 d . . . O5 O 1.0176(3) 0.2849(2) 1.05350(10) 0.0805(7) Uani 1 1 d . . . O6 O 0.7929(4) 0.4398(2) 1.08518(13) 0.1006(9) Uani 1 1 d . . . C1 C 0.3849(4) 0.8304(3) 0.51600(15) 0.0615(8) Uani 1 1 d . . . H1A H 0.3830 0.8253 0.5617 0.074 Uiso 1 1 calc R . . C2 C 0.2892(5) 0.9282(3) 0.49098(15) 0.0708(9) Uani 1 1 d . . . H2B H 0.2231 0.9888 0.5196 0.085 Uiso 1 1 calc R . . C3 C 0.2899(4) 0.9376(2) 0.42399(15) 0.0622(8) Uani 1 1 d . . . H3A H 0.2243 1.0040 0.4067 0.075 Uiso 1 1 calc R . . C4 C 0.3898(3) 0.8465(2) 0.38223(13) 0.0445(6) Uani 1 1 d . . . C5 C 0.4818(4) 0.7498(2) 0.41083(13) 0.0478(7) Uani 1 1 d . . . H5A H 0.5473 0.6874 0.3834 0.057 Uiso 1 1 calc R . . C6 C 0.5185(4) 0.7960(2) 0.26428(13) 0.0466(7) Uani 1 1 d . . . C7 C 0.4813(3) 0.8165(2) 0.19431(13) 0.0456(6) Uani 1 1 d . . . C8 C 0.3602(4) 0.9130(2) 0.17617(14) 0.0528(7) Uani 1 1 d . . . H8B H 0.2968 0.9689 0.2082 0.063 Uiso 1 1 calc R . . C9 C 0.3329(4) 0.9270(2) 0.11106(14) 0.0566(8) Uani 1 1 d . . . H9A H 0.2510 0.9920 0.0994 0.068 Uiso 1 1 calc R . . C10 C 0.4272(4) 0.8445(2) 0.06296(13) 0.0497(7) Uani 1 1 d . . . C11 C 0.5484(4) 0.7494(3) 0.08082(14) 0.0568(8) Uani 1 1 d . . . H11A H 0.6132 0.6942 0.0486 0.068 Uiso 1 1 calc R . . C12 C 0.5750(4) 0.7348(2) 0.14585(14) 0.0532(7) Uani 1 1 d . . . H12A H 0.6566 0.6695 0.1573 0.064 Uiso 1 1 calc R . . C13 C 0.3985(4) 0.8542(3) -0.00800(15) 0.0594(8) Uani 1 1 d . . . C14 C 0.2228(5) 0.9595(3) -0.08343(16) 0.0836(11) Uani 1 1 d . . . H14A H 0.0987 1.0046 -0.0810 0.125 Uiso 1 1 calc R . . H14B H 0.2290 0.8843 -0.1028 0.125 Uiso 1 1 calc R . . H14C H 0.3111 0.9994 -0.1105 0.125 Uiso 1 1 calc R . . C15 C 0.9276(4) 0.3554(2) 0.51729(15) 0.0573(8) Uani 1 1 d . . . H15A H 0.9289 0.3557 0.4716 0.069 Uiso 1 1 calc R . . C16 C 1.0443(4) 0.2673(2) 0.54412(15) 0.0594(8) Uani 1 1 d . . . H16A H 1.1249 0.2101 0.5165 0.071 Uiso 1 1 calc R . . C17 C 1.0414(4) 0.2643(2) 0.61153(14) 0.0535(7) Uani 1 1 d . . . H17A H 1.1183 0.2048 0.6302 0.064 Uiso 1 1 calc R . . C18 C 0.9218(4) 0.3515(2) 0.65124(14) 0.0487(7) Uani 1 1 d . . . C19 C 0.8106(4) 0.4376(2) 0.62100(15) 0.0554(8) Uani 1 1 d . . . H19A H 0.7304 0.4966 0.6475 0.066 Uiso 1 1 calc R . . C20 C 0.7924(4) 0.4119(3) 0.76801(16) 0.0593(8) Uani 1 1 d . . . C21 C 0.8212(4) 0.3943(2) 0.83803(15) 0.0525(7) Uani 1 1 d . . . C22 C 0.9446(4) 0.3029(2) 0.85930(15) 0.0569(8) Uani 1 1 d . . . H22A H 1.0154 0.2466 0.8287 0.068 Uiso 1 1 calc R . . C23 C 0.9642(4) 0.2939(3) 0.92539(14) 0.0589(8) Uani 1 1 d . . . H23A H 1.0470 0.2314 0.9391 0.071 Uiso 1 1 calc R . . C24 C 0.8606(4) 0.3777(3) 0.97159(15) 0.0582(8) Uani 1 1 d . . . C25 C 0.7354(4) 0.4678(3) 0.95081(18) 0.0714(10) Uani 1 1 d . . . H25A H 0.6645 0.5237 0.9815 0.086 Uiso 1 1 calc R . . C26 C 0.7136(4) 0.4762(3) 0.88509(17) 0.0674(9) Uani 1 1 d . . . H26A H 0.6266 0.5368 0.8720 0.081 Uiso 1 1 calc R . . C27 C 0.8827(5) 0.3729(3) 1.04296(17) 0.0691(9) Uani 1 1 d . . . C28 C 1.0560(6) 0.2729(4) 1.12063(17) 0.0981(13) Uani 1 1 d . . . H28A H 1.1733 0.2206 1.1204 0.147 Uiso 1 1 calc R . . H28B H 0.9577 0.2422 1.1486 0.147 Uiso 1 1 calc R . . H28C H 1.0625 0.3480 1.1375 0.147 Uiso 1 1 calc R . . Cl Cl 0.12962(11) -0.03464(7) 0.71343(4) 0.0659(2) Uani 1 1 d . . . O7 O 0.2865(6) -0.0152(4) 0.6641(2) 0.1012(16) Uani 0.60 1 d P A 1 O8 O -0.0219(6) -0.0089(5) 0.6836(3) 0.109(2) Uani 0.60 1 d P A 1 O9 O 0.1242(14) -0.1370(6) 0.7426(5) 0.262(4) Uani 0.60 1 d P A 1 O10 O 0.1302(12) 0.0403(9) 0.7649(3) 0.213(4) Uani 0.60 1 d P A 1 O7' O 0.278(2) -0.0763(12) 0.6717(7) 0.184(6) Uiso 0.40 1 d P A 2 O8' O 0.018(2) -0.0936(14) 0.6896(9) 0.285(8) Uani 0.40 1 d P A 2 O9' O 0.1735(17) -0.1018(12) 0.7626(6) 0.157(4) Uiso 0.40 1 d P A 2 O10' O 0.0292(14) 0.0764(5) 0.7281(6) 0.159(5) Uani 0.40 1 d P A 2 N5 N 0.6728(18) 0.4512(12) 0.3919(6) 0.106(5) Uani 0.50 1 d P B 1 N5' N 0.704(2) 0.4657(11) 0.3927(6) 0.088(4) Uani 0.50 1 d P B 2 C29 C 0.7272(5) 0.4443(3) 0.3382(2) 0.0686(9) Uani 1 1 d . . . C30 C 0.795(2) 0.4242(12) 0.2656(6) 0.098(5) Uani 0.50 1 d P B 1 H30A H 0.9294 0.4121 0.2565 0.147 Uiso 0.50 1 calc PR B 1 H30B H 0.7448 0.4910 0.2416 0.147 Uiso 0.50 1 calc PR B 1 H30C H 0.7549 0.3564 0.2516 0.147 Uiso 0.50 1 calc PR B 1 C30' C 0.762(2) 0.4280(13) 0.2694(8) 0.091(5) Uani 0.50 1 d P B 2 H30D H 0.8286 0.3500 0.2585 0.137 Uiso 0.50 1 calc PR B 2 H30E H 0.8356 0.4829 0.2488 0.137 Uiso 0.50 1 calc PR B 2 H30F H 0.6450 0.4400 0.2534 0.137 Uiso 0.50 1 calc PR B 2 N6 N 0.733(2) 0.7309(13) 0.6223(8) 0.166(8) Uani 0.50 1 d P C 1 C31 C 0.678(2) 0.7524(11) 0.6738(6) 0.101(6) Uani 0.50 1 d P C 1 C32 C 0.643(3) 0.7726(16) 0.7426(9) 0.142(8) Uani 0.50 1 d P C 1 H32A H 0.7096 0.7078 0.7640 0.214 Uiso 0.50 1 calc PR C 1 H32B H 0.5115 0.7812 0.7592 0.214 Uiso 0.50 1 calc PR C 1 H32C H 0.6852 0.8426 0.7519 0.214 Uiso 0.50 1 calc PR C 1 N6' N 0.689(2) 0.7378(12) 0.6208(6) 0.106(4) Uani 0.50 1 d P D 2 C31' C 0.6721(17) 0.7587(12) 0.6756(9) 0.089(5) Uani 0.50 1 d P D 2 C32' C 0.631(2) 0.7877(14) 0.7459(7) 0.091(5) Uani 0.50 1 d P D 2 H32D H 0.7430 0.8000 0.7602 0.137 Uiso 0.50 1 calc PR D 2 H32E H 0.5855 0.7248 0.7706 0.137 Uiso 0.50 1 calc PR D 2 H32F H 0.5375 0.8577 0.7536 0.137 Uiso 0.50 1 calc PR D 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 0.07548(18) 0.06782(16) 0.06872(16) 0.01913(12) -0.01664(13) 0.00976(12) N1 0.0524(13) 0.0539(14) 0.0461(13) 0.0038(11) -0.0084(11) 0.0000(11) N2 0.0438(12) 0.0526(13) 0.0450(12) 0.0022(10) -0.0068(10) 0.0038(10) N3 0.0546(14) 0.0491(13) 0.0599(15) 0.0072(11) -0.0120(12) -0.0018(11) N4 0.0514(14) 0.0550(14) 0.0569(14) -0.0008(11) -0.0139(11) 0.0049(11) O1 0.0513(11) 0.0747(13) 0.0548(12) -0.0011(10) -0.0074(9) 0.0110(10) O2 0.0811(15) 0.0829(15) 0.0531(12) 0.0049(11) -0.0206(11) -0.0096(12) O3 0.1112(19) 0.1079(19) 0.0506(13) -0.0183(13) -0.0131(13) 0.0084(16) O4 0.0841(17) 0.133(2) 0.0809(17) 0.0210(16) 0.0035(14) 0.0509(16) O5 0.1009(18) 0.0874(16) 0.0477(12) -0.0117(11) -0.0021(12) -0.0125(14) O6 0.0968(18) 0.121(2) 0.0743(16) -0.0469(16) 0.0024(14) -0.0069(16) C1 0.073(2) 0.0628(19) 0.0472(16) -0.0019(14) -0.0159(15) -0.0027(16) C2 0.099(2) 0.0511(18) 0.0543(18) -0.0119(15) -0.0153(17) 0.0094(17) C3 0.077(2) 0.0481(17) 0.0560(18) -0.0011(14) -0.0174(16) 0.0072(15) C4 0.0444(15) 0.0447(14) 0.0444(15) 0.0010(12) -0.0086(12) -0.0079(12) C5 0.0453(15) 0.0438(15) 0.0498(16) 0.0000(12) -0.0045(12) -0.0010(12) C6 0.0441(15) 0.0465(15) 0.0497(16) 0.0019(12) -0.0098(13) -0.0087(13) C7 0.0420(14) 0.0457(15) 0.0490(15) -0.0003(12) -0.0043(12) -0.0116(12) C8 0.0590(17) 0.0483(16) 0.0476(16) -0.0038(13) -0.0084(13) -0.0020(13) C9 0.0594(18) 0.0539(17) 0.0538(17) -0.0008(14) -0.0122(14) -0.0013(14) C10 0.0490(16) 0.0554(16) 0.0479(16) 0.0005(13) -0.0071(13) -0.0194(13) C11 0.0585(18) 0.0559(17) 0.0512(17) -0.0103(14) -0.0012(14) -0.0054(14) C12 0.0513(16) 0.0502(16) 0.0545(17) -0.0027(13) -0.0062(14) -0.0033(13) C13 0.0601(19) 0.069(2) 0.0517(18) 0.0019(15) -0.0070(15) -0.0212(16) C14 0.096(3) 0.102(3) 0.062(2) 0.0164(19) -0.0331(19) -0.026(2) C15 0.0571(17) 0.0568(17) 0.0571(17) 0.0081(14) -0.0085(14) -0.0106(14) C16 0.0568(18) 0.0500(17) 0.0645(19) 0.0006(14) -0.0046(15) 0.0011(14) C17 0.0477(16) 0.0454(15) 0.0643(18) 0.0081(14) -0.0110(14) -0.0010(13) C18 0.0434(15) 0.0441(15) 0.0603(17) 0.0030(13) -0.0123(13) -0.0097(12) C19 0.0551(17) 0.0446(15) 0.0633(19) 0.0028(14) -0.0123(14) -0.0001(13) C20 0.0460(16) 0.0554(17) 0.070(2) 0.0085(15) -0.0046(15) -0.0006(14) C21 0.0421(15) 0.0486(16) 0.0630(18) -0.0057(14) 0.0030(13) -0.0095(13) C22 0.0524(17) 0.0529(17) 0.0579(18) -0.0080(14) 0.0026(14) -0.0020(14) C23 0.0589(18) 0.0615(18) 0.0505(17) -0.0041(14) 0.0009(14) -0.0061(15) C24 0.0527(17) 0.0579(18) 0.0621(19) -0.0178(15) 0.0070(15) -0.0198(15) C25 0.0586(19) 0.064(2) 0.082(2) -0.0292(18) 0.0080(17) -0.0040(16) C26 0.0557(18) 0.0551(18) 0.084(2) -0.0104(17) -0.0019(17) -0.0006(15) C27 0.068(2) 0.080(2) 0.060(2) -0.0192(18) 0.0070(17) -0.0308(18) C28 0.139(4) 0.104(3) 0.052(2) -0.005(2) -0.012(2) -0.028(3) Cl 0.0627(5) 0.0687(5) 0.0592(5) 0.0109(4) -0.0103(4) 0.0041(4) O7 0.090(3) 0.087(3) 0.101(3) -0.008(3) 0.056(2) -0.020(3) O8 0.069(3) 0.146(5) 0.096(3) -0.008(3) -0.033(2) 0.039(3) O9 0.352(10) 0.158(5) 0.373(10) 0.204(6) -0.236(8) -0.153(6) O10 0.225(8) 0.306(10) 0.121(5) -0.131(6) -0.022(5) -0.078(7) O8' 0.365(16) 0.243(15) 0.354(19) -0.001(14) -0.209(16) -0.191(13) O10' 0.166(8) 0.035(3) 0.206(10) 0.011(5) 0.108(7) 0.022(4) N5 0.092(6) 0.116(9) 0.085(8) 0.009(6) 0.010(5) 0.015(6) N5' 0.132(9) 0.071(6) 0.058(6) -0.004(4) -0.028(6) 0.000(5) C29 0.066(2) 0.061(2) 0.069(2) -0.0013(18) -0.0033(19) 0.0039(16) C30 0.123(9) 0.108(9) 0.054(6) -0.036(6) 0.019(6) -0.033(7) C30' 0.067(6) 0.089(8) 0.102(11) -0.001(7) -0.001(6) 0.013(6) N6 0.222(15) 0.090(8) 0.149(13) -0.002(8) 0.010(10) 0.023(9) C31 0.172(12) 0.050(7) 0.055(7) -0.002(5) 0.006(7) 0.017(7) C32 0.177(16) 0.094(10) 0.146(15) -0.013(10) -0.024(12) -0.002(10) N6' 0.148(8) 0.091(7) 0.078(7) -0.027(5) -0.061(6) 0.023(6) C31' 0.080(7) 0.066(8) 0.135(13) -0.027(8) -0.070(8) 0.004(6) C32' 0.106(9) 0.096(9) 0.082(8) -0.020(6) -0.056(7) -0.004(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 2.172(2) . ? Ag N3 2.178(2) . ? Ag Ag 3.2152(6) 2_666 ? N1 C1 1.334(3) . ? N1 C5 1.339(3) . ? N2 C6 1.356(3) . ? N2 C4 1.408(3) . ? N2 H2A 0.8600 . ? N3 C15 1.330(3) . ? N3 C19 1.336(3) . ? N4 C20 1.352(4) . ? N4 C18 1.400(3) . ? N4 H4A 0.8600 . ? O1 C6 1.222(3) . ? O2 C13 1.326(4) . ? O2 C14 1.448(4) . ? O3 C13 1.188(3) . ? O4 C20 1.207(3) . ? O5 C27 1.330(4) . ? O5 C28 1.444(4) . ? O6 C27 1.192(4) . ? C1 C2 1.363(4) . ? C1 H1A 0.9300 . ? C2 C3 1.366(4) . ? C2 H2B 0.9300 . ? C3 C4 1.385(4) . ? C3 H3A 0.9300 . ? C4 C5 1.376(3) . ? C5 H5A 0.9300 . ? C6 C7 1.505(4) . ? C7 C12 1.383(4) . ? C7 C8 1.386(4) . ? C8 C9 1.379(4) . ? C8 H8B 0.9300 . ? C9 C10 1.385(4) . ? C9 H9A 0.9300 . ? C10 C11 1.373(4) . ? C10 C13 1.497(4) . ? C11 C12 1.376(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.380(4) . ? C15 H15A 0.9300 . ? C16 C17 1.370(4) . ? C16 H16A 0.9300 . ? C17 C18 1.383(4) . ? C17 H17A 0.9300 . ? C18 C19 1.379(4) . ? C19 H19A 0.9300 . ? C20 C21 1.484(4) . ? C21 C22 1.381(4) . ? C21 C26 1.396(4) . ? C22 C23 1.380(4) . ? C22 H22A 0.9300 . ? C23 C24 1.389(4) . ? C23 H23A 0.9300 . ? C24 C25 1.374(4) . ? C24 C27 1.491(4) . ? C25 C26 1.377(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Cl O7' 1.281(14) . ? Cl O9' 1.306(14) . ? Cl O8' 1.324(12) . ? Cl O9 1.326(6) . ? Cl O8 1.349(5) . ? Cl O10' 1.375(6) . ? Cl O10 1.382(6) . ? Cl O7 1.442(4) . ? N5 C29 1.097(13) . ? N5' C29 1.120(12) . ? C29 C30' 1.390(15) . ? C29 C30 1.485(13) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? N6 C31 1.07(2) . ? C31 C32 1.40(2) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N6' C31' 1.13(2) . ? C31' C32' 1.44(2) . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 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 N3 173.60(9) . . ? N1 Ag Ag 95.74(6) . 2_666 ? N3 Ag Ag 90.58(6) . 2_666 ? C1 N1 C5 118.5(2) . . ? C1 N1 Ag 122.11(18) . . ? C5 N1 Ag 119.34(17) . . ? C6 N2 C4 126.1(2) . . ? C6 N2 H2A 116.9 . . ? C4 N2 H2A 116.9 . . ? C15 N3 C19 118.7(2) . . ? C15 N3 Ag 123.27(19) . . ? C19 N3 Ag 117.97(18) . . ? C20 N4 C18 127.3(2) . . ? C20 N4 H4A 116.3 . . ? C18 N4 H4A 116.3 . . ? C13 O2 C14 116.7(3) . . ? C27 O5 C28 116.6(3) . . ? N1 C1 C2 121.6(3) . . ? N1 C1 H1A 119.2 . . ? C2 C1 H1A 119.2 . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2B 119.9 . . ? C3 C2 H2B 119.9 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 117.8(2) . . ? C5 C4 N2 122.5(2) . . ? C3 C4 N2 119.6(2) . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O1 C6 N2 123.1(2) . . ? O1 C6 C7 120.8(2) . . ? N2 C6 C7 116.0(2) . . ? C12 C7 C8 118.8(3) . . ? C12 C7 C6 117.7(2) . . ? C8 C7 C6 123.5(2) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8B 119.7 . . ? C7 C8 H8B 119.7 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.3(3) . . ? C11 C10 C13 118.6(3) . . ? C9 C10 C13 122.1(3) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? O3 C13 O2 123.6(3) . . ? O3 C13 C10 124.2(3) . . ? O2 C13 C10 112.2(3) . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 121.5(3) . . ? N3 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 118.6(2) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? C19 C18 C17 118.3(3) . . ? C19 C18 N4 123.1(2) . . ? C17 C18 N4 118.5(2) . . ? N3 C19 C18 122.8(3) . . ? N3 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? O4 C20 N4 121.3(3) . . ? O4 C20 C21 121.2(3) . . ? N4 C20 C21 117.5(2) . . ? C22 C21 C26 118.6(3) . . ? C22 C21 C20 124.6(3) . . ? C26 C21 C20 116.8(3) . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 119.1(3) . . ? C25 C24 C27 119.2(3) . . ? C23 C24 C27 121.7(3) . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C21 120.4(3) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? O6 C27 O5 124.1(3) . . ? O6 C27 C24 124.6(3) . . ? O5 C27 C24 111.3(3) . . ? O5 C28 H28A 109.5 . . ? O5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7' Cl O9' 95.5(8) . . ? O7' Cl O8' 95.7(10) . . ? O9' Cl O8' 100.5(9) . . ? O7' Cl O9 92.6(7) . . ? O9' Cl O9 33.8(7) . . ? O8' Cl O9 67.4(8) . . ? O7' Cl O8 111.5(7) . . ? O9' Cl O8 134.7(6) . . ? O8' Cl O8 43.4(8) . . ? O9 Cl O8 106.9(5) . . ? O7' Cl O10' 133.6(7) . . ? O9' Cl O10' 118.5(7) . . ? O8' Cl O10' 106.9(9) . . ? O9 Cl O10' 133.3(6) . . ? O8 Cl O10' 67.0(6) . . ? O7' Cl O10 122.7(7) . . ? O9' Cl O10 74.5(6) . . ? O8' Cl O10 141.4(9) . . ? O9 Cl O10 104.3(6) . . ? O8 Cl O10 114.7(4) . . ? O10' Cl O10 50.1(6) . . ? O7' Cl O7 30.7(6) . . ? O9' Cl O7 115.0(6) . . ? O8' Cl O7 112.9(9) . . ? O9 Cl O7 122.2(5) . . ? O8 Cl O7 105.9(3) . . ? O10' Cl O7 103.1(4) . . ? O10 Cl O7 103.3(4) . . ? N5 C29 N5' 16.3(14) . . ? N5 C29 C30' 168.2(11) . . ? N5' C29 C30' 174.4(11) . . ? N5 C29 C30 174.6(10) . . ? N5' C29 C30 168.1(11) . . ? C30' C29 C30 8.8(11) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C30' H30D 109.5 . . ? C29 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C29 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? N6 C31 C32 168.6(19) . . ? N6' C31' C32' 174.5(13) . . ? C31' C32' H32D 109.5 . . ? C31' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C31' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.435 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.054 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 888039' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag N5 O9' _chemical_formula_weight 682.39 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.17570(10) _cell_length_b 9.9244(2) _cell_length_c 18.2818(4) _cell_angle_alpha 84.1830(10) _cell_angle_beta 87.7800(10) _cell_angle_gamma 67.1820(10) _cell_volume 1360.24(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6560 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.58 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6772 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24503 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6720 _reflns_number_gt 4480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0456P)^2^+0.1313P] 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 6720 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.67811(3) -0.02589(2) -0.051510(12) 0.05091(7) Uani 1 1 d . . . O1 O 0.2482(3) 0.5748(2) -0.32311(12) 0.0753(6) Uani 1 1 d . . . O2 O 0.2159(4) 1.2238(3) -0.52314(13) 0.0979(8) Uani 1 1 d . . . O3 O 0.3660(3) 1.2547(2) -0.43220(11) 0.0712(6) Uani 1 1 d . . . O4 O 1.1791(2) -0.63736(19) 0.20472(11) 0.0565(5) Uani 1 1 d . . . O5 O 1.2128(3) -1.2871(2) 0.40925(13) 0.0985(8) Uani 1 1 d . . . O6 O 1.0660(3) -1.32119(19) 0.31808(11) 0.0624(5) Uani 1 1 d . . . N1 N 0.5995(2) 0.1760(2) -0.12058(11) 0.0417(5) Uani 1 1 d . . . N2 N 0.4777(3) 0.5678(2) -0.25649(11) 0.0458(5) Uani 1 1 d . . . H2A H 0.5457 0.6136 -0.2504 0.055 Uiso 1 1 calc R . . N3 N 0.7807(2) -0.2359(2) 0.01065(11) 0.0425(5) Uani 1 1 d . . . N4 N 0.9381(2) -0.6324(2) 0.14422(11) 0.0413(5) Uani 1 1 d . . . H4A H 0.8732 -0.6816 0.1396 0.050 Uiso 1 1 calc R . . C1 C 0.4983(3) 0.2030(3) -0.18077(15) 0.0467(6) Uani 1 1 d . . . H1A H 0.4560 0.1325 -0.1911 0.056 Uiso 1 1 calc R . . C2 C 0.4537(3) 0.3285(3) -0.22789(15) 0.0464(6) Uani 1 1 d . . . H2B H 0.3840 0.3412 -0.2691 0.056 Uiso 1 1 calc R . . C3 C 0.5134(3) 0.4358(2) -0.21350(14) 0.0395(6) Uani 1 1 d . . . C4 C 0.6198(3) 0.4084(3) -0.15177(14) 0.0443(6) Uani 1 1 d . . . H4B H 0.6642 0.4770 -0.1404 0.053 Uiso 1 1 calc R . . C5 C 0.6584(3) 0.2797(3) -0.10795(14) 0.0450(6) Uani 1 1 d . . . H5A H 0.7298 0.2635 -0.0670 0.054 Uiso 1 1 calc R . . C6 C 0.3456(3) 0.6323(3) -0.30747(15) 0.0465(6) Uani 1 1 d . . . C7 C 0.3305(3) 0.7798(3) -0.34377(14) 0.0432(6) Uani 1 1 d . . . C8 C 0.2411(4) 0.8250(3) -0.41014(16) 0.0598(8) Uani 1 1 d . . . H8A H 0.1911 0.7664 -0.4293 0.072 Uiso 1 1 calc R . . C9 C 0.2259(4) 0.9566(3) -0.44790(16) 0.0618(8) Uani 1 1 d . . . H9A H 0.1659 0.9860 -0.4926 0.074 Uiso 1 1 calc R . . C10 C 0.2987(3) 1.0454(3) -0.42025(15) 0.0484(6) Uani 1 1 d . . . C11 C 0.3809(4) 1.0030(3) -0.35239(15) 0.0549(7) Uani 1 1 d . . . H11A H 0.4255 1.0640 -0.3321 0.066 Uiso 1 1 calc R . . C12 C 0.3974(4) 0.8701(3) -0.31420(15) 0.0535(7) Uani 1 1 d . . . H12A H 0.4537 0.8421 -0.2687 0.064 Uiso 1 1 calc R . . C13 C 0.2864(4) 1.1831(3) -0.46463(16) 0.0568(7) Uani 1 1 d . . . C14 C 0.3688(5) 1.3877(3) -0.47275(19) 0.0840(10) Uani 1 1 d . . . H14A H 0.4426 1.4232 -0.4474 0.126 Uiso 1 1 calc R . . H14B H 0.2503 1.4612 -0.4764 0.126 Uiso 1 1 calc R . . H14C H 0.4153 1.3665 -0.5212 0.126 Uiso 1 1 calc R . . C15 C 0.7322(3) -0.3460(3) -0.00245(14) 0.0426(6) Uani 1 1 d . . . H15A H 0.6605 -0.3330 -0.0430 0.051 Uiso 1 1 calc R . . C16 C 0.7827(3) -0.4761(2) 0.04072(13) 0.0414(6) Uani 1 1 d . . . H16A H 0.7447 -0.5487 0.0296 0.050 Uiso 1 1 calc R . . C17 C 0.8911(3) -0.4996(2) 0.10136(13) 0.0365(5) Uani 1 1 d . . . C18 C 0.9412(3) -0.3857(3) 0.11582(14) 0.0433(6) Uani 1 1 d . . . H18A H 1.0127 -0.3959 0.1560 0.052 Uiso 1 1 calc R . . C19 C 0.8835(3) -0.2586(3) 0.06986(15) 0.0464(6) Uani 1 1 d . . . H19A H 0.9175 -0.1834 0.0803 0.056 Uiso 1 1 calc R . . C20 C 1.0761(3) -0.6946(3) 0.19307(13) 0.0409(6) Uani 1 1 d . . . C21 C 1.0925(3) -0.8404(2) 0.23122(14) 0.0396(6) Uani 1 1 d . . . C22 C 1.0341(3) -0.9349(3) 0.20040(14) 0.0430(6) Uani 1 1 d . . . H22A H 0.9855 -0.9101 0.1534 0.052 Uiso 1 1 calc R . . C23 C 1.0470(3) -1.0657(3) 0.23854(14) 0.0452(6) Uani 1 1 d . . . H23A H 1.0037 -1.1270 0.2177 0.054 Uiso 1 1 calc R . . C24 C 1.1233(3) -1.1063(3) 0.30721(14) 0.0431(6) Uani 1 1 d . . . C25 C 1.1866(4) -1.0138(3) 0.33707(15) 0.0575(7) Uani 1 1 d . . . H25A H 1.2412 -1.0414 0.3829 0.069 Uiso 1 1 calc R . . C26 C 1.1704(4) -0.8814(3) 0.30021(15) 0.0534(7) Uani 1 1 d . . . H26A H 1.2117 -0.8195 0.3216 0.064 Uiso 1 1 calc R . . C27 C 1.1401(4) -1.2467(3) 0.35091(16) 0.0527(7) Uani 1 1 d . . . C28 C 1.0747(4) -1.4589(3) 0.35763(19) 0.0729(9) Uani 1 1 d . . . H28A H 0.9984 -1.4946 0.3342 0.109 Uiso 1 1 calc R . . H28B H 1.0370 -1.4429 0.4075 0.109 Uiso 1 1 calc R . . H28C H 1.1946 -1.5300 0.3572 0.109 Uiso 1 1 calc R . . N5 N 0.6775(3) 0.1514(2) 0.09578(13) 0.0529(6) Uani 1 1 d . . . O7 O 0.5911(3) 0.0780(2) 0.11256(16) 0.0983(8) Uani 1 1 d . . . O8 O 0.8039(3) 0.1083(3) 0.05149(12) 0.0826(7) Uani 1 1 d . . . O9 O 0.6437(3) 0.2682(2) 0.12281(13) 0.0713(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.06200(13) 0.03200(10) 0.05930(14) 0.00724(8) -0.00339(10) -0.02125(9) O1 0.0825(12) 0.0560(12) 0.1012(17) 0.0190(11) -0.0372(12) -0.0447(10) O2 0.153(2) 0.0800(15) 0.0749(16) 0.0381(12) -0.0494(15) -0.0673(15) O3 0.1022(14) 0.0549(11) 0.0658(13) 0.0183(10) -0.0132(11) -0.0449(11) O4 0.0568(10) 0.0509(10) 0.0723(13) 0.0129(9) -0.0188(9) -0.0352(9) O5 0.1554(19) 0.0803(15) 0.0828(16) 0.0415(12) -0.0575(15) -0.0771(14) O6 0.0845(12) 0.0435(10) 0.0695(13) 0.0097(9) -0.0158(11) -0.0379(10) N1 0.0455(10) 0.0319(10) 0.0512(13) 0.0008(9) 0.0014(10) -0.0200(9) N2 0.0540(11) 0.0359(10) 0.0544(13) 0.0070(9) -0.0093(10) -0.0267(9) N3 0.0448(10) 0.0309(10) 0.0541(13) -0.0015(9) -0.0013(10) -0.0175(9) N4 0.0473(10) 0.0334(10) 0.0498(12) 0.0037(9) -0.0064(9) -0.0240(9) C1 0.0537(14) 0.0366(13) 0.0586(17) -0.0034(11) -0.0029(13) -0.0269(11) C2 0.0532(14) 0.0385(13) 0.0529(16) -0.0006(11) -0.0076(12) -0.0239(11) C3 0.0404(12) 0.0317(12) 0.0477(15) -0.0019(10) 0.0041(11) -0.0162(10) C4 0.0503(13) 0.0338(12) 0.0560(16) 0.0003(11) -0.0054(12) -0.0246(11) C5 0.0502(13) 0.0354(13) 0.0523(16) 0.0030(11) -0.0075(12) -0.0209(11) C6 0.0501(14) 0.0404(14) 0.0515(16) -0.0019(11) -0.0007(12) -0.0208(12) C7 0.0483(13) 0.0367(13) 0.0460(15) 0.0005(11) -0.0003(11) -0.0189(11) C8 0.0773(18) 0.0519(16) 0.0596(18) 0.0046(13) -0.0189(15) -0.0358(14) C9 0.0795(18) 0.0557(17) 0.0537(18) 0.0100(13) -0.0222(15) -0.0315(15) C10 0.0550(14) 0.0406(14) 0.0496(15) 0.0052(11) -0.0025(12) -0.0206(12) C11 0.0768(17) 0.0435(14) 0.0543(17) 0.0056(12) -0.0155(14) -0.0349(13) C12 0.0724(17) 0.0435(14) 0.0496(16) 0.0094(12) -0.0142(14) -0.0298(13) C13 0.0714(17) 0.0462(15) 0.0532(18) 0.0101(13) -0.0053(15) -0.0263(14) C14 0.118(3) 0.0577(18) 0.086(2) 0.0229(17) -0.007(2) -0.0517(18) C15 0.0461(13) 0.0347(13) 0.0466(15) 0.0000(11) -0.0059(11) -0.0155(11) C16 0.0458(13) 0.0336(12) 0.0489(15) -0.0034(11) -0.0015(11) -0.0197(10) C17 0.0334(11) 0.0322(12) 0.0445(14) -0.0001(10) 0.0032(10) -0.0142(9) C18 0.0440(13) 0.0368(13) 0.0526(15) -0.0027(11) -0.0094(11) -0.0189(11) C19 0.0489(13) 0.0352(13) 0.0603(17) -0.0005(11) -0.0071(13) -0.0222(11) C20 0.0416(12) 0.0375(13) 0.0438(14) 0.0029(11) -0.0030(11) -0.0167(11) C21 0.0418(12) 0.0331(12) 0.0466(14) -0.0013(10) -0.0014(11) -0.0178(10) C22 0.0455(13) 0.0379(13) 0.0429(14) 0.0010(11) -0.0110(11) -0.0135(11) C23 0.0500(13) 0.0328(12) 0.0559(16) -0.0030(11) -0.0089(12) -0.0190(11) C24 0.0465(13) 0.0380(13) 0.0479(15) 0.0013(11) -0.0035(12) -0.0207(11) C25 0.0759(17) 0.0568(16) 0.0461(16) 0.0120(13) -0.0214(14) -0.0345(14) C26 0.0711(16) 0.0462(14) 0.0543(17) 0.0045(12) -0.0162(14) -0.0359(13) C27 0.0578(15) 0.0463(15) 0.0578(18) 0.0065(13) -0.0064(14) -0.0266(13) C28 0.096(2) 0.0503(17) 0.085(2) 0.0102(15) -0.0100(18) -0.0452(16) N5 0.0639(13) 0.0406(12) 0.0598(15) 0.0067(10) -0.0261(12) -0.0265(11) O7 0.1036(14) 0.0749(14) 0.145(2) 0.0170(14) -0.0345(15) -0.0697(12) O8 0.0980(16) 0.0891(17) 0.0614(14) -0.0162(12) -0.0102(13) -0.0338(13) O9 0.0709(12) 0.0411(11) 0.1114(18) -0.0231(11) -0.0075(12) -0.0275(9) _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 2.1384(19) . ? Ag N3 2.1390(19) . ? Ag Ag 3.3020(4) 2_655 ? O1 C6 1.202(3) . ? O2 C13 1.191(3) . ? O3 C13 1.323(3) . ? O3 C14 1.455(3) . ? O4 C20 1.220(3) . ? O5 C27 1.195(3) . ? O6 C27 1.319(3) . ? O6 C28 1.458(3) . ? N1 C5 1.336(3) . ? N1 C1 1.344(3) . ? N2 C6 1.366(3) . ? N2 C3 1.390(3) . ? N2 H2A 0.8600 . ? N3 C19 1.342(3) . ? N3 C15 1.345(3) . ? N4 C20 1.370(3) . ? N4 C17 1.386(3) . ? N4 H4A 0.8600 . ? C1 C2 1.371(3) . ? C1 H1A 0.9300 . ? C2 C3 1.384(3) . ? C2 H2B 0.9300 . ? C3 C4 1.390(3) . ? C4 C5 1.368(3) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.506(3) . ? C7 C12 1.377(4) . ? C7 C8 1.383(4) . ? C8 C9 1.376(4) . ? C8 H8A 0.9300 . ? C9 C10 1.382(4) . ? C9 H9A 0.9300 . ? C10 C11 1.381(4) . ? C10 C13 1.487(3) . ? C11 C12 1.388(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.366(3) . ? C15 H15A 0.9300 . ? C16 C17 1.390(3) . ? C16 H16A 0.9300 . ? C17 C18 1.394(3) . ? C18 C19 1.369(3) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.500(3) . ? C21 C22 1.378(3) . ? C21 C26 1.385(3) . ? C22 C23 1.378(3) . ? C22 H22A 0.9300 . ? C23 C24 1.375(3) . ? C23 H23A 0.9300 . ? C24 C25 1.379(4) . ? C24 C27 1.494(3) . ? C25 C26 1.375(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N5 O7 1.209(3) . ? N5 O9 1.233(3) . ? N5 O8 1.253(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 N3 174.07(7) . . ? N1 Ag Ag 101.90(5) . 2_655 ? N3 Ag Ag 83.98(5) . 2_655 ? C13 O3 C14 116.5(2) . . ? C27 O6 C28 116.1(2) . . ? C5 N1 C1 116.2(2) . . ? C5 N1 Ag 120.85(16) . . ? C1 N1 Ag 122.85(16) . . ? C6 N2 C3 126.7(2) . . ? C6 N2 H2A 116.7 . . ? C3 N2 H2A 116.7 . . ? C19 N3 C15 116.6(2) . . ? C19 N3 Ag 120.79(16) . . ? C15 N3 Ag 122.32(16) . . ? C20 N4 C17 127.6(2) . . ? C20 N4 H4A 116.2 . . ? C17 N4 H4A 116.2 . . ? N1 C1 C2 123.9(2) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2B 120.4 . . ? C3 C2 H2B 120.4 . . ? C2 C3 N2 125.1(2) . . ? C2 C3 C4 117.4(2) . . ? N2 C3 C4 117.5(2) . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4B 120.3 . . ? C3 C4 H4B 120.3 . . ? N1 C5 C4 123.9(2) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? O1 C6 N2 122.4(2) . . ? O1 C6 C7 121.8(2) . . ? N2 C6 C7 115.8(2) . . ? C12 C7 C8 119.6(2) . . ? C12 C7 C6 123.9(2) . . ? C8 C7 C6 116.6(2) . . ? C9 C8 C7 120.2(3) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 118.8(2) . . ? C11 C10 C13 122.3(2) . . ? C9 C10 C13 118.9(2) . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C7 C12 C11 119.9(2) . . ? C7 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? O2 C13 O3 123.6(3) . . ? O2 C13 C10 124.2(3) . . ? O3 C13 C10 112.2(2) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 123.4(2) . . ? N3 C15 H15A 118.3 . . ? C16 C15 H15A 118.3 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? N4 C17 C16 118.1(2) . . ? N4 C17 C18 124.5(2) . . ? C16 C17 C18 117.4(2) . . ? C19 C18 C17 118.9(2) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? N3 C19 C18 124.0(2) . . ? N3 C19 H19A 118.0 . . ? C18 C19 H19A 118.0 . . ? O4 C20 N4 123.1(2) . . ? O4 C20 C21 122.0(2) . . ? N4 C20 C21 114.8(2) . . ? C22 C21 C26 118.9(2) . . ? C22 C21 C20 122.8(2) . . ? C26 C21 C20 118.3(2) . . ? C23 C22 C21 120.7(2) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 118.8(2) . . ? C23 C24 C27 122.6(2) . . ? C25 C24 C27 118.6(2) . . ? C26 C25 C24 121.1(2) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C21 120.0(2) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? O5 C27 O6 123.7(3) . . ? O5 C27 C24 123.7(3) . . ? O6 C27 C24 112.6(2) . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 N5 O9 120.4(3) . . ? O7 N5 O8 120.2(3) . . ? O9 N5 O8 119.4(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.450 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.067 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 888040' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Ag Cl N5 O10' _chemical_formula_weight 760.89 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 8.5792(2) _cell_length_b 10.5968(2) _cell_length_c 17.2908(4) _cell_angle_alpha 82.5200(10) _cell_angle_beta 89.7910(10) _cell_angle_gamma 89.6930(10) _cell_volume 1558.54(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6342 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26001 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7668 _reflns_number_gt 5824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0445P)^2^+0.8333P] 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 7668 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.78738(2) 0.51183(2) -0.025715(11) 0.05891(9) Uani 1 1 d . . . O1 O 0.3067(3) 0.50329(17) 0.30932(12) 0.0715(6) Uani 1 1 d . . . O2 O -0.1014(2) 0.76832(18) 0.58742(10) 0.0577(5) Uani 1 1 d . . . O3 O -0.1705(2) 0.93734(18) 0.50341(12) 0.0603(5) Uani 1 1 d . . . O4 O 1.2882(2) 0.16811(15) -0.26145(9) 0.0484(4) Uani 1 1 d . . . O5 O 1.6469(2) 0.14211(15) -0.61954(10) 0.0538(5) Uani 1 1 d . . . O6 O 1.6661(2) 0.35293(15) -0.63754(10) 0.0548(5) Uani 1 1 d . . . N1 N 0.6251(2) 0.5730(2) 0.05626(11) 0.0438(4) Uani 1 1 d . . . N2 N 0.3325(2) 0.68747(18) 0.22902(10) 0.0394(4) Uani 1 1 d . . . H2A H 0.3067 0.7667 0.2223 0.047 Uiso 1 1 calc R . . N3 N 0.9456(2) 0.46720(19) -0.11440(11) 0.0424(4) Uani 1 1 d . . . N4 N 1.2421(2) 0.37962(16) -0.29259(10) 0.0370(4) Uani 1 1 d . . . H4A H 1.2682 0.4447 -0.3250 0.044 Uiso 1 1 calc R . . C1 C 0.5676(3) 0.4889(2) 0.11231(14) 0.0484(6) Uani 1 1 d . . . H1A H 0.5957 0.4039 0.1125 0.058 Uiso 1 1 calc R . . C2 C 0.4691(3) 0.5185(2) 0.17037(14) 0.0472(6) Uani 1 1 d . . . H2B H 0.4311 0.4551 0.2078 0.057 Uiso 1 1 calc R . . C3 C 0.4276(2) 0.6449(2) 0.17195(12) 0.0370(5) Uani 1 1 d . . . C4 C 0.4838(3) 0.7331(2) 0.11262(14) 0.0479(6) Uani 1 1 d . . . H4B H 0.4564 0.8185 0.1106 0.057 Uiso 1 1 calc R . . C5 C 0.5799(3) 0.6942(3) 0.05688(14) 0.0514(6) Uani 1 1 d . . . H5A H 0.6158 0.7551 0.0173 0.062 Uiso 1 1 calc R . . C6 C 0.2763(3) 0.6157(2) 0.29454(12) 0.0385(5) Uani 1 1 d . . . C7 C 0.1774(2) 0.6809(2) 0.34893(12) 0.0343(4) Uani 1 1 d . . . C8 C 0.1494(3) 0.6113(2) 0.42140(13) 0.0419(5) Uani 1 1 d . . . H8A H 0.1891 0.5291 0.4322 0.050 Uiso 1 1 calc R . . C9 C 0.0635(3) 0.6624(2) 0.47753(13) 0.0435(5) Uani 1 1 d . . . H9A H 0.0487 0.6161 0.5265 0.052 Uiso 1 1 calc R . . C10 C -0.0003(2) 0.7829(2) 0.46063(12) 0.0358(4) Uani 1 1 d . . . C11 C 0.0244(3) 0.8512(2) 0.38801(13) 0.0415(5) Uani 1 1 d . . . H11A H -0.0198 0.9318 0.3764 0.050 Uiso 1 1 calc R . . C12 C 0.1137(3) 0.8017(2) 0.33235(13) 0.0402(5) Uani 1 1 d . . . H12A H 0.1309 0.8492 0.2840 0.048 Uiso 1 1 calc R . . C13 C -0.1000(3) 0.8399(2) 0.51827(14) 0.0418(5) Uani 1 1 d . . . C14 C -0.2004(4) 0.8100(3) 0.64655(17) 0.0650(8) Uani 1 1 d . . . H14A H -0.2233 0.7391 0.6853 0.098 Uiso 1 1 calc R . . H14B H -0.2956 0.8439 0.6232 0.098 Uiso 1 1 calc R . . H14C H -0.1482 0.8747 0.6706 0.098 Uiso 1 1 calc R . . C15 C 0.9919(3) 0.3472(2) -0.11772(14) 0.0480(6) Uani 1 1 d . . . H15A H 0.9561 0.2843 -0.0793 0.058 Uiso 1 1 calc R . . C16 C 1.0890(3) 0.3112(2) -0.17422(13) 0.0436(5) Uani 1 1 d . . . H16A H 1.1177 0.2263 -0.1737 0.052 Uiso 1 1 calc R . . C17 C 1.1437(2) 0.4033(2) -0.23207(12) 0.0338(4) Uani 1 1 d . . . C18 C 1.0948(3) 0.5278(2) -0.22931(14) 0.0480(6) Uani 1 1 d . . . H18A H 1.1282 0.5926 -0.2671 0.058 Uiso 1 1 calc R . . C19 C 0.9967(3) 0.5548(2) -0.17048(14) 0.0482(6) Uani 1 1 d . . . H19A H 0.9647 0.6386 -0.1700 0.058 Uiso 1 1 calc R . . C20 C 1.3028(2) 0.26429(19) -0.30675(12) 0.0335(4) Uani 1 1 d . . . C21 C 1.3862(2) 0.26510(19) -0.38282(12) 0.0313(4) Uani 1 1 d . . . C22 C 1.4825(2) 0.16180(19) -0.39241(13) 0.0361(4) Uani 1 1 d . . . H22A H 1.4961 0.0969 -0.3513 0.043 Uiso 1 1 calc R . . C23 C 1.5580(2) 0.15527(19) -0.46276(13) 0.0367(5) Uani 1 1 d . . . H23A H 1.6203 0.0853 -0.4692 0.044 Uiso 1 1 calc R . . C24 C 1.5403(2) 0.25303(19) -0.52321(12) 0.0329(4) Uani 1 1 d . . . C25 C 1.4442(3) 0.3561(2) -0.51445(12) 0.0376(5) Uani 1 1 d . . . H25A H 1.4320 0.4215 -0.5554 0.045 Uiso 1 1 calc R . . C26 C 1.3666(3) 0.3610(2) -0.44475(12) 0.0371(5) Uani 1 1 d . . . H26A H 1.3006 0.4292 -0.4393 0.045 Uiso 1 1 calc R . . C27 C 1.6246(2) 0.2563(2) -0.59883(13) 0.0365(5) Uani 1 1 d . . . C28 C 1.7282(4) 0.1372(3) -0.69235(17) 0.0703(9) Uani 1 1 d . . . H28A H 1.7335 0.0507 -0.7032 0.105 Uiso 1 1 calc R . . H28B H 1.8318 0.1697 -0.6887 0.105 Uiso 1 1 calc R . . H28C H 1.6733 0.1881 -0.7336 0.105 Uiso 1 1 calc R . . Cl Cl 0.2602(2) 0.07256(11) 0.14827(6) 0.1177(5) Uani 1 1 d . . . O7 O 0.3359(11) -0.0101(5) 0.2026(5) 0.094(2) Uani 0.50 1 d P A 1 O8 O 0.3097(18) 0.1987(6) 0.1482(6) 0.167(4) Uani 0.50 1 d P A 1 O9 O 0.220(2) 0.057(2) 0.0797(7) 0.277(9) Uani 0.50 1 d P A 1 O10 O 0.0927(8) 0.0831(7) 0.1879(3) 0.1061(19) Uani 0.50 1 d P A 1 O7' O 0.361(2) 0.071(3) 0.2098(10) 0.360(16) Uani 0.50 1 d P A 2 O8' O 0.1861(16) 0.1607(11) 0.1281(12) 0.236(8) Uani 0.50 1 d P A 2 O9' O 0.3714(14) 0.0577(7) 0.0816(4) 0.162(4) Uani 0.50 1 d P A 2 O10' O 0.1990(15) -0.0491(8) 0.1439(9) 0.196(5) Uani 0.50 1 d P A 2 N5 N 0.7940(4) 0.2674(3) 0.04941(18) 0.0863(9) Uani 1 1 d . B . C29 C 0.7826(4) 0.1640(3) 0.06958(18) 0.0698(8) Uani 1 1 d . . . C30 C 0.775(4) 0.029(2) 0.101(2) 0.114(8) Uani 0.50 1 d P B 1 H30A H 0.7599 -0.0211 0.0590 0.170 Uiso 0.50 1 calc PR B 1 H30B H 0.6905 0.0149 0.1372 0.170 Uiso 0.50 1 calc PR B 1 H30C H 0.8714 0.0034 0.1270 0.170 Uiso 0.50 1 calc PR B 1 C30' C 0.765(5) 0.031(3) 0.089(2) 0.160(13) Uani 0.50 1 d P B 2 H30D H 0.8339 -0.0127 0.0576 0.239 Uiso 0.50 1 calc PR B 2 H30E H 0.6595 0.0076 0.0806 0.239 Uiso 0.50 1 calc PR B 2 H30F H 0.7909 0.0074 0.1434 0.239 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.05201(13) 0.08237(17) 0.04722(13) -0.02747(10) 0.02120(9) 0.00055(10) O1 0.1099(17) 0.0450(11) 0.0568(11) 0.0021(9) 0.0421(11) 0.0237(10) O2 0.0646(12) 0.0650(11) 0.0446(10) -0.0120(8) 0.0218(8) 0.0115(9) O3 0.0605(11) 0.0541(11) 0.0682(12) -0.0165(9) 0.0175(9) 0.0187(9) O4 0.0667(11) 0.0364(8) 0.0406(9) 0.0002(7) 0.0195(8) 0.0080(7) O5 0.0787(12) 0.0334(8) 0.0513(10) -0.0136(7) 0.0312(9) -0.0016(8) O6 0.0738(12) 0.0352(9) 0.0554(10) -0.0068(8) 0.0348(9) -0.0010(8) N1 0.0428(11) 0.0577(12) 0.0333(9) -0.0149(9) 0.0104(8) 0.0027(9) N2 0.0442(10) 0.0386(10) 0.0353(9) -0.0052(8) 0.0116(8) 0.0075(8) N3 0.0413(10) 0.0522(11) 0.0353(9) -0.0118(8) 0.0136(8) 0.0011(8) N4 0.0444(10) 0.0310(9) 0.0356(9) -0.0049(7) 0.0160(8) 0.0011(7) C1 0.0529(14) 0.0499(14) 0.0446(13) -0.0157(11) 0.0161(11) 0.0072(11) C2 0.0573(15) 0.0439(13) 0.0409(12) -0.0075(10) 0.0186(11) 0.0041(11) C3 0.0327(11) 0.0488(12) 0.0306(10) -0.0096(9) 0.0047(8) 0.0046(9) C4 0.0556(14) 0.0454(13) 0.0418(12) -0.0035(10) 0.0135(11) 0.0088(11) C5 0.0575(15) 0.0585(15) 0.0373(12) -0.0037(11) 0.0183(11) 0.0030(12) C6 0.0406(12) 0.0425(12) 0.0324(11) -0.0057(9) 0.0088(9) 0.0051(9) C7 0.0316(10) 0.0386(11) 0.0334(10) -0.0076(8) 0.0050(8) 0.0012(8) C8 0.0433(12) 0.0402(12) 0.0410(12) -0.0014(9) 0.0120(9) 0.0120(9) C9 0.0444(13) 0.0481(13) 0.0366(11) -0.0008(10) 0.0118(9) 0.0078(10) C10 0.0305(10) 0.0403(11) 0.0387(11) -0.0132(9) 0.0060(8) 0.0003(8) C11 0.0447(12) 0.0356(11) 0.0447(12) -0.0073(9) 0.0069(10) 0.0068(9) C12 0.0448(12) 0.0387(12) 0.0366(11) -0.0031(9) 0.0064(9) 0.0038(9) C13 0.0359(11) 0.0468(13) 0.0460(13) -0.0184(10) 0.0109(9) -0.0025(10) C14 0.0681(18) 0.0768(19) 0.0544(16) -0.0253(14) 0.0293(14) -0.0030(15) C15 0.0541(14) 0.0507(14) 0.0385(12) -0.0035(10) 0.0167(10) -0.0011(11) C16 0.0503(13) 0.0405(12) 0.0399(12) -0.0054(10) 0.0143(10) 0.0028(10) C17 0.0333(10) 0.0374(11) 0.0320(10) -0.0090(8) 0.0084(8) -0.0007(8) C18 0.0591(15) 0.0384(12) 0.0458(13) -0.0040(10) 0.0254(11) 0.0038(10) C19 0.0544(14) 0.0420(13) 0.0496(14) -0.0118(10) 0.0191(11) 0.0057(10) C20 0.0334(10) 0.0336(11) 0.0346(10) -0.0087(9) 0.0062(8) -0.0001(8) C21 0.0309(10) 0.0307(10) 0.0335(10) -0.0089(8) 0.0066(8) -0.0008(8) C22 0.0398(11) 0.0291(10) 0.0388(11) -0.0029(8) 0.0083(9) 0.0032(8) C23 0.0373(11) 0.0286(10) 0.0446(12) -0.0071(9) 0.0106(9) 0.0055(8) C24 0.0342(10) 0.0299(10) 0.0361(10) -0.0102(8) 0.0104(8) -0.0021(8) C25 0.0449(12) 0.0330(11) 0.0348(11) -0.0039(8) 0.0088(9) 0.0068(9) C26 0.0415(12) 0.0334(11) 0.0369(11) -0.0071(9) 0.0093(9) 0.0095(9) C27 0.0370(11) 0.0321(11) 0.0415(11) -0.0097(9) 0.0116(9) 0.0015(8) C28 0.103(2) 0.0479(15) 0.0628(18) -0.0212(13) 0.0435(16) 0.0027(15) Cl 0.2103(15) 0.0779(7) 0.0615(6) 0.0015(5) 0.0241(7) 0.0372(8) O7 0.126(6) 0.059(3) 0.088(5) 0.028(3) 0.019(4) 0.018(3) O8 0.283(14) 0.056(4) 0.157(8) 0.005(4) 0.053(9) -0.017(6) O9 0.34(2) 0.40(3) 0.105(8) -0.073(11) 0.088(11) -0.016(19) O10 0.104(4) 0.138(6) 0.075(3) -0.014(3) 0.003(3) 0.028(4) O7' 0.225(16) 0.73(5) 0.156(13) -0.18(2) -0.041(11) 0.13(2) O8' 0.182(12) 0.100(8) 0.43(3) -0.046(11) -0.041(14) 0.072(8) O9' 0.293(12) 0.099(4) 0.085(4) 0.024(3) 0.101(7) 0.057(6) O10' 0.246(12) 0.091(6) 0.237(12) 0.027(6) 0.114(11) 0.039(6) N5 0.118(3) 0.0585(17) 0.080(2) -0.0003(14) 0.0331(17) 0.0089(16) C29 0.098(2) 0.0592(19) 0.0514(16) -0.0056(14) 0.0183(16) 0.0035(16) C30 0.184(19) 0.055(10) 0.099(15) -0.001(8) 0.015(11) 0.006(10) C30' 0.31(3) 0.075(13) 0.085(11) 0.017(8) -0.013(15) -0.061(15) _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 2.1405(18) . ? Ag N3 2.1408(17) . ? O1 C6 1.213(3) . ? O2 C13 1.330(3) . ? O2 C14 1.438(3) . ? O3 C13 1.193(3) . ? O4 C20 1.209(3) . ? O5 C27 1.319(3) . ? O5 C28 1.443(3) . ? O6 C27 1.202(3) . ? N1 C1 1.324(3) . ? N1 C5 1.342(3) . ? N2 C6 1.367(3) . ? N2 C3 1.396(3) . ? N2 H2A 0.8600 . ? N3 C19 1.327(3) . ? N3 C15 1.338(3) . ? N4 C20 1.376(3) . ? N4 C17 1.389(2) . ? N4 H4A 0.8600 . ? C1 C2 1.376(3) . ? C1 H1A 0.9300 . ? C2 C3 1.388(3) . ? C2 H2B 0.9300 . ? C3 C4 1.382(3) . ? C4 C5 1.368(3) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.496(3) . ? C7 C12 1.385(3) . ? C7 C8 1.389(3) . ? C8 C9 1.381(3) . ? C8 H8A 0.9300 . ? C9 C10 1.383(3) . ? C9 H9A 0.9300 . ? C10 C11 1.382(3) . ? C10 C13 1.495(3) . ? C11 C12 1.383(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.372(3) . ? C15 H15A 0.9300 . ? C16 C17 1.386(3) . ? C16 H16A 0.9300 . ? C17 C18 1.389(3) . ? C18 C19 1.375(3) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.494(3) . ? C21 C26 1.387(3) . ? C21 C22 1.395(3) . ? C22 C23 1.386(3) . ? C22 H22A 0.9300 . ? C23 C24 1.381(3) . ? C23 H23A 0.9300 . ? C24 C25 1.388(3) . ? C24 C27 1.489(3) . ? C25 C26 1.382(3) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Cl O8' 1.144(9) . ? Cl O9 1.270(13) . ? Cl O7 1.363(7) . ? Cl O7' 1.373(16) . ? Cl O8 1.405(8) . ? Cl O10' 1.405(11) . ? Cl O9' 1.517(7) . ? Cl O10 1.599(6) . ? N5 C29 1.110(4) . ? C29 C30' 1.42(3) . ? C29 C30 1.47(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 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 N3 174.64(8) . . ? C13 O2 C14 116.9(2) . . ? C27 O5 C28 116.21(18) . . ? C1 N1 C5 116.25(19) . . ? C1 N1 Ag 119.54(16) . . ? C5 N1 Ag 124.17(16) . . ? C6 N2 C3 126.47(19) . . ? C6 N2 H2A 116.8 . . ? C3 N2 H2A 116.8 . . ? C19 N3 C15 116.71(19) . . ? C19 N3 Ag 122.26(16) . . ? C15 N3 Ag 120.95(15) . . ? C20 N4 C17 127.62(18) . . ? C20 N4 H4A 116.2 . . ? C17 N4 H4A 116.2 . . ? N1 C1 C2 124.5(2) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 118.7(2) . . ? C1 C2 H2B 120.6 . . ? C3 C2 H2B 120.6 . . ? C4 C3 C2 117.3(2) . . ? C4 C3 N2 118.6(2) . . ? C2 C3 N2 124.1(2) . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4B 120.1 . . ? C3 C4 H4B 120.1 . . ? N1 C5 C4 123.5(2) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? O1 C6 N2 121.7(2) . . ? O1 C6 C7 120.5(2) . . ? N2 C6 C7 117.84(19) . . ? C12 C7 C8 119.16(19) . . ? C12 C7 C6 125.39(19) . . ? C8 C7 C6 115.45(19) . . ? C9 C8 C7 121.0(2) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 119.7(2) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 119.51(19) . . ? C11 C10 C13 118.9(2) . . ? C9 C10 C13 121.6(2) . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 119.7(2) . . ? C11 C12 H12A 120.2 . . ? C7 C12 H12A 120.2 . . ? O3 C13 O2 124.4(2) . . ? O3 C13 C10 123.8(2) . . ? O2 C13 C10 111.8(2) . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 124.1(2) . . ? N3 C15 H15A 118.0 . . ? C16 C15 H15A 118.0 . . ? C15 C16 C17 119.0(2) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C16 C17 C18 117.18(19) . . ? C16 C17 N4 124.74(19) . . ? C18 C17 N4 118.07(19) . . ? C19 C18 C17 119.7(2) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? N3 C19 C18 123.3(2) . . ? N3 C19 H19A 118.3 . . ? C18 C19 H19A 118.3 . . ? O4 C20 N4 122.58(19) . . ? O4 C20 C21 121.91(18) . . ? N4 C20 C21 115.49(18) . . ? C26 C21 C22 119.10(18) . . ? C26 C21 C20 122.83(18) . . ? C22 C21 C20 118.01(18) . . ? C23 C22 C21 120.46(19) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 119.72(18) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 120.32(18) . . ? C23 C24 C27 122.82(18) . . ? C25 C24 C27 116.84(19) . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C25 C26 C21 120.60(19) . . ? C25 C26 H26A 119.7 . . ? C21 C26 H26A 119.7 . . ? O6 C27 O5 123.52(19) . . ? O6 C27 C24 123.65(19) . . ? O5 C27 C24 112.83(18) . . ? O5 C28 H28A 109.5 . . ? O5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8' Cl O9 76.3(11) . . ? O8' Cl O7 154.0(11) . . ? O9 Cl O7 128.8(11) . . ? O8' Cl O7' 120.9(13) . . ? O9 Cl O7' 155.6(10) . . ? O7 Cl O7' 39.0(13) . . ? O8' Cl O8 55.3(7) . . ? O9 Cl O8 109.0(10) . . ? O7 Cl O8 112.4(7) . . ? O7' Cl O8 73.8(13) . . ? O8' Cl O10' 119.5(9) . . ? O9 Cl O10' 67.1(10) . . ? O7 Cl O10' 72.9(6) . . ? O7' Cl O10' 111.3(13) . . ? O8 Cl O10' 174.6(8) . . ? O8' Cl O9' 106.0(11) . . ? O9 Cl O9' 54.9(8) . . ? O7 Cl O9' 96.1(5) . . ? O7' Cl O9' 101.6(8) . . ? O8 Cl O9' 90.0(5) . . ? O10' Cl O9' 90.5(5) . . ? O8' Cl O10 62.3(9) . . ? O9 Cl O10 100.1(8) . . ? O7 Cl O10 101.8(4) . . ? O7' Cl O10 103.4(8) . . ? O8 Cl O10 99.0(6) . . ? O10' Cl O10 78.4(5) . . ? O9' Cl O10 155.0(5) . . ? N5 C29 C30' 175.6(17) . . ? N5 C29 C30 175.8(16) . . ? C30' C29 C30 8(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C30' H30D 109.5 . . ? C29 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C29 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.614 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.057 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 888041' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Ag Cl N6 O10' _chemical_formula_weight 721.82 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 10.9516(12) _cell_length_b 11.4924(15) _cell_length_c 12.3178(12) _cell_angle_alpha 97.684(10) _cell_angle_beta 115.890(7) _cell_angle_gamma 91.832(10) _cell_volume 1375.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.99 _cell_measurement_theta_max 12.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9477 _exptl_absorpt_correction_T_max 0.9889 _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_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5668 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4836 _reflns_number_gt 3974 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+1.0146P] 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 0.0018(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4836 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.53377(3) 0.62587(2) 0.47655(2) 0.06562(12) Uani 1 1 d . . . C1 C 0.3264(3) 0.4898(3) 0.2211(3) 0.0544(8) Uani 1 1 d . . . H1A H 0.2713 0.5292 0.2504 0.065 Uiso 1 1 calc R . . C2 C 0.2705(3) 0.4390(3) 0.1021(3) 0.0602(9) Uani 1 1 d . . . H2A H 0.1791 0.4426 0.0497 0.072 Uiso 1 1 calc R . . C3 C 0.3555(4) 0.3821(4) 0.0631(3) 0.0790(12) Uani 1 1 d . . . H3A H 0.3206 0.3467 -0.0184 0.095 Uiso 1 1 calc R . . C4 C 0.5308(3) 0.4272(2) 0.2523(2) 0.0416(6) Uani 1 1 d . . . C5 C 0.7436(3) 0.4344(2) 0.4484(2) 0.0389(6) Uani 1 1 d . . . C6 C 0.8800(3) 0.3885(2) 0.4979(2) 0.0378(6) Uani 1 1 d . . . C11 C 0.9634(3) 0.4200(3) 0.6228(3) 0.0453(7) Uani 1 1 d . . . H11A H 0.9332 0.4687 0.6708 0.054 Uiso 1 1 calc R . . C10 C 1.0908(3) 0.3797(3) 0.6763(3) 0.0453(7) Uani 1 1 d . . . H10A H 1.1456 0.4012 0.7599 0.054 Uiso 1 1 calc R . . C9 C 1.1368(3) 0.3077(2) 0.6062(3) 0.0418(6) Uani 1 1 d . . . C8 C 1.0548(3) 0.2781(3) 0.4807(3) 0.0513(7) Uani 1 1 d . . . H8A H 1.0863 0.2315 0.4324 0.062 Uiso 1 1 calc R . . C7 C 0.9278(3) 0.3172(3) 0.4276(3) 0.0471(7) Uani 1 1 d . . . H7A H 0.8734 0.2956 0.3439 0.056 Uiso 1 1 calc R . . C12 C 1.2715(3) 0.2591(3) 0.6588(3) 0.0482(7) Uani 1 1 d . . . C13 C 1.4810(3) 0.2597(3) 0.8338(3) 0.0661(9) Uani 1 1 d . . . H13A H 1.5269 0.2970 0.9179 0.099 Uiso 1 1 calc R . . H13B H 1.5340 0.2780 0.7924 0.099 Uiso 1 1 calc R . . H13C H 1.4700 0.1758 0.8298 0.099 Uiso 1 1 calc R . . C14 C 0.7243(3) 0.7964(3) 0.7089(3) 0.0587(8) Uani 1 1 d . . . H14A H 0.7738 0.7325 0.7070 0.070 Uiso 1 1 calc R . . C15 C 0.7840(3) 0.8881(3) 0.8028(3) 0.0595(8) Uani 1 1 d . . . H15A H 0.8722 0.8883 0.8640 0.071 Uiso 1 1 calc R . . C16 C 0.7071(3) 0.9808(3) 0.8027(3) 0.0569(8) Uani 1 1 d . . . H16A H 0.7437 1.0441 0.8668 0.068 Uiso 1 1 calc R . . C17 C 0.5337(3) 0.8881(3) 0.6260(3) 0.0451(7) Uani 1 1 d . . . C18 C 0.3168(3) 0.8299(3) 0.4291(3) 0.0475(7) Uani 1 1 d . . . C19 C 0.1786(3) 0.8682(2) 0.3626(3) 0.0436(6) Uani 1 1 d . . . C24 C 0.1022(3) 0.8170(3) 0.2415(3) 0.0529(7) Uani 1 1 d . . . H24A H 0.1383 0.7609 0.2052 0.063 Uiso 1 1 calc R . . C23 C -0.0268(3) 0.8483(3) 0.1738(3) 0.0523(7) Uani 1 1 d . . . H23A H -0.0767 0.8141 0.0922 0.063 Uiso 1 1 calc R . . C22 C -0.0817(3) 0.9303(3) 0.2276(3) 0.0467(7) Uani 1 1 d . . . C21 C -0.0059(3) 0.9802(3) 0.3489(3) 0.0631(9) Uani 1 1 d . . . H21A H -0.0423 1.0353 0.3858 0.076 Uiso 1 1 calc R . . C20 C 0.1226(3) 0.9491(3) 0.4154(3) 0.0622(9) Uani 1 1 d . . . H20A H 0.1723 0.9831 0.4971 0.075 Uiso 1 1 calc R . . C25 C -0.2204(3) 0.9645(3) 0.1535(3) 0.0518(7) Uani 1 1 d . . . C26 C -0.3837(3) 1.0946(3) 0.1507(4) 0.0698(10) Uani 1 1 d . . . H26A H -0.4008 1.1520 0.2054 0.105 Uiso 1 1 calc R . . H26B H -0.4573 1.0325 0.1141 0.105 Uiso 1 1 calc R . . H26C H -0.3772 1.1317 0.0879 0.105 Uiso 1 1 calc R . . N1 N 0.4583(2) 0.4859(2) 0.2991(2) 0.0468(6) Uani 1 1 d . . . N2 N 0.4864(3) 0.3754(3) 0.1372(2) 0.0703(9) Uani 1 1 d . . . N3 N 0.6676(2) 0.4124(2) 0.3244(2) 0.0436(5) Uani 1 1 d . . . H3B H 0.7106 0.3850 0.2841 0.052 Uiso 1 1 calc R . . N4 N 0.5968(3) 0.7932(2) 0.6183(2) 0.0506(6) Uani 1 1 d . . . N5 N 0.5824(3) 0.9824(2) 0.7137(2) 0.0540(6) Uani 1 1 d . . . N6 N 0.4012(2) 0.8985(2) 0.5383(2) 0.0523(6) Uani 1 1 d . . . H6A H 0.3664 0.9597 0.5565 0.063 Uiso 1 1 calc R . . O1 O 0.7030(2) 0.4858(2) 0.51764(19) 0.0583(6) Uani 1 1 d . . . O2 O 1.3085(3) 0.1883(3) 0.6012(2) 0.0858(9) Uani 1 1 d . . . O3 O 1.3474(2) 0.3025(2) 0.77532(19) 0.0602(6) Uani 1 1 d . . . O4 O 0.3508(3) 0.7438(2) 0.3854(2) 0.0808(8) Uani 1 1 d . . . O5 O -0.2908(2) 0.9233(3) 0.0480(2) 0.0739(7) Uani 1 1 d . . . O6 O -0.2575(2) 1.0460(2) 0.2180(2) 0.0629(6) Uani 1 1 d . . . O7 O 0.7887(3) 0.3618(3) 0.1327(2) 0.0803(8) Uani 1 1 d . . . O8 O 0.9537(14) 0.2398(14) 0.1790(9) 0.142(7) Uani 0.50 1 d P . . O8' O 1.0092(11) 0.3640(15) 0.1572(18) 0.185(9) Uani 0.50 1 d P . . O9 O 0.8045(11) 0.2488(12) -0.0226(10) 0.133(7) Uani 0.50 1 d P . . O9' O 0.8934(16) 0.1915(10) 0.106(2) 0.188(8) Uani 0.50 1 d P . . O10 O 0.9635(12) 0.3912(13) 0.0866(15) 0.149(6) Uani 0.50 1 d P . . O10' O 0.842(3) 0.310(2) -0.0230(11) 0.244(12) Uani 0.50 1 d P . . Cl Cl 0.88109(8) 0.30708(7) 0.09356(7) 0.0540(2) 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 0.05690(17) 0.06281(18) 0.06402(18) -0.00737(12) 0.01849(13) 0.02754(12) C1 0.0370(15) 0.067(2) 0.0547(18) 0.0050(15) 0.0168(14) 0.0195(14) C2 0.0334(15) 0.081(2) 0.0524(19) 0.0056(16) 0.0075(14) 0.0150(15) C3 0.0479(19) 0.126(3) 0.0419(18) -0.0106(19) 0.0064(15) 0.026(2) C4 0.0332(14) 0.0480(15) 0.0386(14) 0.0037(12) 0.0118(12) 0.0119(12) C5 0.0356(14) 0.0412(14) 0.0383(14) 0.0055(11) 0.0151(12) 0.0095(11) C6 0.0341(14) 0.0398(14) 0.0382(14) 0.0074(11) 0.0143(11) 0.0082(11) C11 0.0399(15) 0.0530(16) 0.0392(15) 0.0024(12) 0.0153(12) 0.0127(13) C10 0.0375(15) 0.0516(16) 0.0370(14) 0.0061(12) 0.0076(12) 0.0082(13) C9 0.0349(14) 0.0466(15) 0.0431(15) 0.0117(12) 0.0151(12) 0.0101(12) C8 0.0427(16) 0.0661(19) 0.0447(16) 0.0081(14) 0.0182(13) 0.0233(14) C7 0.0391(15) 0.0598(18) 0.0348(14) 0.0044(13) 0.0099(12) 0.0165(13) C12 0.0377(15) 0.0577(18) 0.0509(17) 0.0150(14) 0.0191(14) 0.0134(13) C13 0.0401(17) 0.085(2) 0.060(2) 0.0195(18) 0.0074(15) 0.0255(17) C14 0.0464(17) 0.060(2) 0.065(2) 0.0149(16) 0.0188(16) 0.0192(15) C15 0.0414(17) 0.074(2) 0.0540(19) 0.0160(17) 0.0110(15) 0.0118(16) C16 0.0500(18) 0.065(2) 0.0456(17) 0.0036(15) 0.0135(15) 0.0039(15) C17 0.0412(15) 0.0507(16) 0.0432(15) 0.0089(13) 0.0179(13) 0.0092(13) C18 0.0442(16) 0.0440(16) 0.0505(17) 0.0086(13) 0.0169(14) 0.0134(13) C19 0.0428(15) 0.0433(15) 0.0431(15) 0.0090(12) 0.0166(13) 0.0097(12) C24 0.0508(18) 0.0532(17) 0.0498(17) 0.0016(14) 0.0192(14) 0.0143(14) C23 0.0474(17) 0.0607(19) 0.0409(16) 0.0039(14) 0.0134(13) 0.0089(14) C22 0.0437(16) 0.0505(16) 0.0427(15) 0.0110(13) 0.0149(13) 0.0090(13) C21 0.0525(19) 0.074(2) 0.0501(18) -0.0048(16) 0.0138(15) 0.0273(17) C20 0.0523(19) 0.074(2) 0.0411(16) -0.0050(15) 0.0066(14) 0.0198(16) C25 0.0419(16) 0.0619(19) 0.0510(18) 0.0154(15) 0.0180(15) 0.0111(14) C26 0.0430(18) 0.077(2) 0.084(3) 0.020(2) 0.0203(18) 0.0219(17) N1 0.0359(12) 0.0545(14) 0.0439(13) 0.0017(11) 0.0132(10) 0.0147(11) N2 0.0411(14) 0.110(2) 0.0427(15) -0.0106(15) 0.0082(12) 0.0267(15) N3 0.0315(11) 0.0561(14) 0.0388(12) 0.0010(10) 0.0128(10) 0.0155(10) N4 0.0442(14) 0.0540(15) 0.0511(14) 0.0098(12) 0.0180(12) 0.0142(11) N5 0.0479(15) 0.0566(15) 0.0495(15) 0.0041(12) 0.0153(12) 0.0124(12) N6 0.0428(13) 0.0515(14) 0.0485(14) 0.0006(11) 0.0089(11) 0.0171(11) O1 0.0487(12) 0.0829(16) 0.0419(11) 0.0055(10) 0.0188(10) 0.0296(11) O2 0.0539(15) 0.121(2) 0.0643(15) -0.0031(15) 0.0130(12) 0.0445(15) O3 0.0400(11) 0.0781(15) 0.0481(12) 0.0090(11) 0.0056(10) 0.0252(11) O4 0.0635(15) 0.0680(16) 0.0763(17) -0.0125(13) 0.0047(13) 0.0317(13) O5 0.0512(14) 0.0940(19) 0.0536(15) 0.0042(13) 0.0040(12) 0.0185(13) O6 0.0455(12) 0.0738(15) 0.0607(14) 0.0103(12) 0.0149(11) 0.0221(11) O7 0.0668(16) 0.109(2) 0.0677(16) 0.0079(15) 0.0327(13) 0.0348(15) O8 0.150(11) 0.250(18) 0.096(6) 0.106(8) 0.087(7) 0.162(12) O8' 0.063(6) 0.201(14) 0.229(15) -0.141(13) 0.060(8) -0.045(7) O9 0.086(5) 0.164(11) 0.092(8) -0.091(9) 0.019(5) -0.005(7) O9' 0.153(12) 0.076(6) 0.40(2) 0.102(11) 0.166(15) 0.054(6) O10 0.091(8) 0.190(11) 0.194(14) 0.079(11) 0.078(9) -0.022(7) O10' 0.36(3) 0.36(2) 0.074(8) 0.094(12) 0.122(13) 0.28(2) Cl 0.0456(4) 0.0686(5) 0.0441(4) 0.0038(3) 0.0178(3) 0.0130(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 Ag N4 2.277(3) . ? Ag N1 2.334(2) . ? Ag O4 2.394(2) . ? Ag O1 2.423(2) . ? Ag Ag 3.1518(7) 2_666 ? C1 N1 1.347(4) . ? C1 C2 1.352(5) . ? C1 H1A 0.9300 . ? C2 C3 1.369(5) . ? C2 H2A 0.9300 . ? C3 N2 1.333(4) . ? C3 H3A 0.9300 . ? C4 N1 1.321(4) . ? C4 N2 1.325(4) . ? C4 N3 1.399(3) . ? C5 O1 1.220(3) . ? C5 N3 1.365(3) . ? C5 C6 1.491(4) . ? C6 C7 1.389(4) . ? C6 C11 1.391(4) . ? C11 C10 1.385(4) . ? C11 H11A 0.9300 . ? C10 C9 1.378(4) . ? C10 H10A 0.9300 . ? C9 C8 1.393(4) . ? C9 C12 1.491(4) . ? C8 C7 1.374(4) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C12 O2 1.203(4) . ? C12 O3 1.319(4) . ? C13 O3 1.456(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N4 1.349(4) . ? C14 C15 1.359(5) . ? C14 H14A 0.9300 . ? C15 C16 1.378(5) . ? C15 H15A 0.9300 . ? C16 N5 1.330(4) . ? C16 H16A 0.9300 . ? C17 N4 1.324(4) . ? C17 N5 1.332(4) . ? C17 N6 1.402(4) . ? C18 O4 1.209(4) . ? C18 N6 1.367(4) . ? C18 C19 1.488(4) . ? C19 C20 1.373(4) . ? C19 C24 1.384(4) . ? C24 C23 1.380(4) . ? C24 H24A 0.9300 . ? C23 C22 1.380(4) . ? C23 H23A 0.9300 . ? C22 C21 1.381(4) . ? C22 C25 1.490(4) . ? C21 C20 1.372(4) . ? C21 H21A 0.9300 . ? C20 H20A 0.9300 . ? C25 O5 1.201(4) . ? C25 O6 1.335(4) . ? C26 O6 1.443(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N3 H3B 0.8600 . ? N6 H6A 0.8600 . ? O7 Cl 1.427(3) . ? O8 O9' 0.936(19) . ? O8 Cl 1.365(8) . ? O8 O8' 1.63(2) . ? O8' O10 0.90(2) . ? O8' Cl 1.362(9) . ? O9 O10' 0.81(3) . ? O9 Cl 1.363(8) . ? O9 O9' 1.69(2) . ? O9' Cl 1.362(9) . ? O10 Cl 1.338(9) . ? O10 O10' 1.57(2) . ? O10' Cl 1.312(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 N4 Ag N1 166.45(9) . . ? N4 Ag O4 77.35(8) . . ? N1 Ag O4 93.07(8) . . ? N4 Ag O1 114.98(8) . . ? N1 Ag O1 73.63(8) . . ? O4 Ag O1 166.07(8) . . ? N4 Ag Ag 124.26(7) . 2_666 ? N1 Ag Ag 68.72(7) . 2_666 ? O4 Ag Ag 118.83(8) . 2_666 ? O1 Ag Ag 60.77(6) . 2_666 ? N1 C1 C2 123.1(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 116.4(3) . . ? C1 C2 H2A 121.8 . . ? C3 C2 H2A 121.8 . . ? N2 C3 C2 122.6(3) . . ? N2 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? N1 C4 N2 126.1(2) . . ? N1 C4 N3 121.5(2) . . ? N2 C4 N3 112.4(2) . . ? O1 C5 N3 123.0(2) . . ? O1 C5 C6 120.3(2) . . ? N3 C5 C6 116.6(2) . . ? C7 C6 C11 118.7(2) . . ? C7 C6 C5 124.3(2) . . ? C11 C6 C5 117.0(2) . . ? C10 C11 C6 120.6(3) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C9 C8 119.2(2) . . ? C10 C9 C12 122.9(3) . . ? C8 C9 C12 117.9(3) . . ? C7 C8 C9 120.5(3) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? O2 C12 O3 123.1(3) . . ? O2 C12 C9 123.8(3) . . ? O3 C12 C9 113.1(3) . . ? 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 123.3(3) . . ? N4 C14 H14A 118.3 . . ? C15 C14 H14A 118.3 . . ? C14 C15 C16 116.6(3) . . ? C14 C15 H15A 121.7 . . ? C16 C15 H15A 121.7 . . ? N5 C16 C15 122.0(3) . . ? N5 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? N4 C17 N5 126.7(3) . . ? N4 C17 N6 121.7(3) . . ? N5 C17 N6 111.6(3) . . ? O4 C18 N6 123.3(3) . . ? O4 C18 C19 120.4(3) . . ? N6 C18 C19 116.3(3) . . ? C20 C19 C24 118.8(3) . . ? C20 C19 C18 123.7(3) . . ? C24 C19 C18 117.5(3) . . ? C23 C24 C19 120.8(3) . . ? C23 C24 H24A 119.6 . . ? C19 C24 H24A 119.6 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C22 C21 119.2(3) . . ? C23 C22 C25 119.5(3) . . ? C21 C22 C25 121.3(3) . . ? C20 C21 C22 120.6(3) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? O5 C25 O6 124.0(3) . . ? O5 C25 C22 123.9(3) . . ? O6 C25 C22 112.1(3) . . ? 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 . . ? C4 N1 C1 115.6(2) . . ? C4 N1 Ag 128.95(18) . . ? C1 N1 Ag 113.05(19) . . ? C4 N2 C3 116.3(3) . . ? C5 N3 C4 130.3(2) . . ? C5 N3 H3B 114.8 . . ? C4 N3 H3B 114.8 . . ? C17 N4 C14 114.9(3) . . ? C17 N4 Ag 132.1(2) . . ? C14 N4 Ag 113.0(2) . . ? C16 N5 C17 116.4(3) . . ? C18 N6 C17 132.1(3) . . ? C18 N6 H6A 113.9 . . ? C17 N6 H6A 113.9 . . ? C5 O1 Ag 128.75(18) . . ? C12 O3 C13 116.7(3) . . ? C18 O4 Ag 131.0(2) . . ? C25 O6 C26 116.2(3) . . ? O9' O8 Cl 69.7(9) . . ? O9' O8 O8' 113.1(13) . . ? Cl O8 O8' 53.1(6) . . ? O10 O8' Cl 69.1(10) . . ? O10 O8' O8 120.4(13) . . ? Cl O8' O8 53.3(6) . . ? O10' O9 Cl 69.0(11) . . ? O10' O9 O9' 112.4(17) . . ? Cl O9 O9' 51.6(6) . . ? O8 O9' Cl 70.1(10) . . ? O8 O9' O9 121.2(13) . . ? Cl O9' O9 51.6(6) . . ? O8' O10 Cl 72.0(12) . . ? O8' O10 O10' 119.4(16) . . ? Cl O10 O10' 52.8(8) . . ? O9 O10' Cl 76.0(16) . . ? O9 O10' O10 128.4(18) . . ? Cl O10' O10 54.3(7) . . ? O10' Cl O10 72.9(12) . . ? O10' Cl O9' 105.8(11) . . ? O10 Cl O9' 132.5(8) . . ? O10' Cl O8' 108.0(13) . . ? O10 Cl O8' 38.9(9) . . ? O9' Cl O8' 106.2(9) . . ? O10' Cl O9 35.0(14) . . ? O10 Cl O9 106.8(9) . . ? O9' Cl O9 76.8(10) . . ? O8' Cl O9 135.8(9) . . ? O10' Cl O8 138.9(8) . . ? O10 Cl O8 110.9(8) . . ? O9' Cl O8 40.2(8) . . ? O8' Cl O8 73.6(9) . . ? O9 Cl O8 116.5(9) . . ? O10' Cl O7 110.3(7) . . ? O10 Cl O7 108.9(7) . . ? O9' Cl O7 115.3(6) . . ? O8' Cl O7 110.9(5) . . ? O9 Cl O7 106.7(6) . . ? O8 Cl O7 106.9(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.288 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.053 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 888042' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Ag B F4 N6 O6' _chemical_formula_weight 709.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8318(16) _cell_length_b 11.5968(12) _cell_length_c 12.2368(15) _cell_angle_alpha 98.530(9) _cell_angle_beta 115.595(9) _cell_angle_gamma 91.721(9) _cell_volume 1363.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.70 _cell_measurement_theta_max 12.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8891 _exptl_absorpt_correction_T_max 0.9911 _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_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5570 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4752 _reflns_number_gt 2652 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.9763P] 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 4752 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.53642(5) 0.62413(5) -0.01934(5) 0.0673(2) Uani 1 1 d . . . C4 C 0.5321(5) 0.4274(5) -0.2491(5) 0.0425(14) Uani 1 1 d . . . C3 C 0.3562(7) 0.3844(8) -0.4391(6) 0.097(3) Uani 1 1 d . . . H3A H 0.3208 0.3495 -0.5216 0.116 Uiso 1 1 calc R . . C2 C 0.2708(6) 0.4403(6) -0.3992(6) 0.0664(19) Uani 1 1 d . . . H2A H 0.1792 0.4448 -0.4521 0.080 Uiso 1 1 calc R . . C1 C 0.3262(6) 0.4890(5) -0.2783(6) 0.0550(17) Uani 1 1 d . . . H1A H 0.2702 0.5274 -0.2480 0.066 Uiso 1 1 calc R . . C5 C 0.7454(5) 0.4326(4) -0.0529(5) 0.0402(14) Uani 1 1 d . . . C6 C 0.8835(5) 0.3869(4) -0.0030(5) 0.0412(14) Uani 1 1 d . . . C11 C 0.9677(5) 0.4202(5) 0.1222(5) 0.0438(14) Uani 1 1 d . . . H11A H 0.9377 0.4706 0.1702 0.053 Uiso 1 1 calc R . . C10 C 1.0947(6) 0.3800(5) 0.1767(5) 0.0459(14) Uani 1 1 d . . . H10A H 1.1495 0.4026 0.2609 0.055 Uiso 1 1 calc R . . C9 C 1.1408(5) 0.3059(4) 0.1060(5) 0.0418(14) Uani 1 1 d . . . C8 C 1.0580(6) 0.2754(5) -0.0195(5) 0.0561(17) Uani 1 1 d . . . H8A H 1.0898 0.2277 -0.0679 0.067 Uiso 1 1 calc R . . C7 C 0.9313(6) 0.3133(5) -0.0740(5) 0.0515(16) Uani 1 1 d . . . H7A H 0.8769 0.2903 -0.1582 0.062 Uiso 1 1 calc R . . C12 C 1.2757(6) 0.2565(5) 0.1600(6) 0.0517(16) Uani 1 1 d . . . C13 C 1.4878(6) 0.2595(6) 0.3354(6) 0.0681(19) Uani 1 1 d . . . H13A H 1.5351 0.2993 0.4194 0.102 Uiso 1 1 calc R . . H13B H 1.5412 0.2739 0.2925 0.102 Uiso 1 1 calc R . . H13C H 1.4753 0.1768 0.3334 0.102 Uiso 1 1 calc R . . C17 C 0.5376(6) 0.8886(5) 0.1278(5) 0.0454(14) Uani 1 1 d . . . C16 C 0.7130(6) 0.9822(6) 0.3050(6) 0.0584(17) Uani 1 1 d . . . H16A H 0.7504 1.0468 0.3685 0.070 Uiso 1 1 calc R . . C15 C 0.7899(6) 0.8907(6) 0.3076(6) 0.0588(17) Uani 1 1 d . . . H15A H 0.8784 0.8915 0.3698 0.071 Uiso 1 1 calc R . . C14 C 0.7283(7) 0.7973(6) 0.2122(6) 0.0637(18) Uani 1 1 d . . . H14A H 0.7783 0.7339 0.2101 0.076 Uiso 1 1 calc R . . C18 C 0.3213(6) 0.8285(5) -0.0689(5) 0.0504(15) Uani 1 1 d . . . C19 C 0.1809(5) 0.8648(5) -0.1371(5) 0.0433(14) Uani 1 1 d . . . C24 C 0.1038(6) 0.8135(5) -0.2598(5) 0.0505(16) Uani 1 1 d . . . H24A H 0.1399 0.7575 -0.2972 0.061 Uiso 1 1 calc R . . C23 C -0.0252(6) 0.8447(5) -0.3264(5) 0.0531(16) Uani 1 1 d . . . H23A H -0.0755 0.8095 -0.4085 0.064 Uiso 1 1 calc R . . C22 C -0.0813(6) 0.9273(5) -0.2736(5) 0.0495(15) Uani 1 1 d . . . C21 C -0.0047(6) 0.9776(6) -0.1515(6) 0.0644(18) Uani 1 1 d . . . H21A H -0.0412 1.0332 -0.1142 0.077 Uiso 1 1 calc R . . C20 C 0.1252(6) 0.9467(5) -0.0838(5) 0.0619(18) Uani 1 1 d . . . H20A H 0.1753 0.9817 -0.0016 0.074 Uiso 1 1 calc R . . C25 C -0.2200(6) 0.9616(6) -0.3475(6) 0.0552(16) Uani 1 1 d . . . C26 C -0.3811(6) 1.0958(6) -0.3498(6) 0.075(2) Uani 1 1 d . . . H26A H -0.3965 1.1549 -0.2945 0.112 Uiso 1 1 calc R . . H26B H -0.4569 1.0353 -0.3861 0.112 Uiso 1 1 calc R . . H26C H -0.3733 1.1303 -0.4134 0.112 Uiso 1 1 calc R . . N2 N 0.4879(5) 0.3772(5) -0.3661(5) 0.0756(18) Uani 1 1 d . . . N1 N 0.4585(4) 0.4845(4) -0.1999(4) 0.0497(13) Uani 1 1 d . . . N3 N 0.6703(4) 0.4111(4) -0.1772(4) 0.0445(12) Uani 1 1 d . . . H3B H 0.7137 0.3834 -0.2181 0.053 Uiso 1 1 calc R . . N5 N 0.5872(5) 0.9835(4) 0.2164(5) 0.0539(13) Uani 1 1 d . . . N4 N 0.6011(5) 0.7924(4) 0.1226(4) 0.0521(13) Uani 1 1 d . . . N6 N 0.4051(4) 0.8993(4) 0.0388(4) 0.0495(13) Uani 1 1 d . . . H6A H 0.3710 0.9617 0.0555 0.059 Uiso 1 1 calc R . . O1 O 0.7044(4) 0.4847(4) 0.0180(4) 0.0617(12) Uani 1 1 d . . . O2 O 1.3110(4) 0.1830(5) 0.1027(4) 0.0883(16) Uani 1 1 d . . . O3 O 1.3536(4) 0.3029(4) 0.2760(4) 0.0624(12) Uani 1 1 d . . . O4 O 0.3546(4) 0.7412(4) -0.1138(4) 0.0817(15) Uani 1 1 d . . . O5 O -0.2911(4) 0.9200(4) -0.4525(4) 0.0785(14) Uani 1 1 d . . . O6 O -0.2546(4) 1.0455(4) -0.2820(4) 0.0663(12) Uani 1 1 d . . . B B 0.1187(9) 0.6923(8) -0.5954(8) 0.060(2) Uani 1 1 d . . . F1 F 0.2051(4) 0.6438(4) -0.6388(3) 0.0898(13) Uani 1 1 d . . . F2 F 0.0247(18) 0.6129(14) -0.6066(19) 0.150(5) Uani 0.60 1 d P . . F2' F -0.0146(13) 0.660(2) -0.685(2) 0.115(8) Uani 0.40 1 d P . . F3 F 0.1936(11) 0.7406(16) -0.4785(11) 0.123(5) Uani 0.60 1 d P . . F3' F 0.128(4) 0.656(3) -0.494(2) 0.167(11) Uani 0.40 1 d P . . F4 F 0.060(2) 0.7731(18) -0.6654(17) 0.137(5) Uani 0.60 1 d P . . F4' F 0.129(2) 0.8135(13) -0.568(3) 0.135(7) Uani 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0599(3) 0.0629(3) 0.0662(4) -0.0069(2) 0.0207(3) 0.0240(2) C4 0.038(3) 0.045(3) 0.040(3) 0.001(3) 0.014(3) 0.007(3) C3 0.056(5) 0.164(8) 0.044(4) -0.011(4) 0.006(4) 0.034(5) C2 0.035(4) 0.092(5) 0.055(4) 0.004(4) 0.006(3) 0.022(3) C1 0.033(3) 0.065(4) 0.057(4) 0.003(3) 0.012(3) 0.017(3) C5 0.033(3) 0.042(3) 0.042(4) 0.005(3) 0.013(3) 0.005(3) C6 0.037(3) 0.043(3) 0.041(3) 0.007(3) 0.016(3) 0.002(3) C11 0.041(3) 0.053(4) 0.034(3) 0.004(3) 0.014(3) 0.015(3) C10 0.047(4) 0.049(3) 0.038(3) 0.003(3) 0.016(3) 0.005(3) C9 0.033(3) 0.040(3) 0.049(4) 0.012(3) 0.014(3) 0.010(3) C8 0.049(4) 0.075(4) 0.050(4) 0.010(3) 0.027(3) 0.023(3) C7 0.042(4) 0.064(4) 0.038(3) -0.001(3) 0.011(3) 0.016(3) C12 0.043(4) 0.061(4) 0.050(4) 0.015(3) 0.018(3) 0.013(3) C13 0.042(4) 0.088(5) 0.062(4) 0.019(4) 0.009(3) 0.025(3) C17 0.044(4) 0.044(4) 0.051(4) 0.015(3) 0.021(3) 0.017(3) C16 0.050(4) 0.063(4) 0.053(4) 0.008(3) 0.016(4) 0.000(3) C15 0.046(4) 0.070(4) 0.050(4) 0.012(3) 0.011(3) 0.010(3) C14 0.051(4) 0.066(4) 0.076(5) 0.017(4) 0.027(4) 0.023(3) C18 0.050(4) 0.048(4) 0.049(4) 0.006(3) 0.018(3) 0.004(3) C19 0.037(3) 0.042(3) 0.045(4) 0.010(3) 0.013(3) 0.006(3) C24 0.050(4) 0.050(4) 0.044(4) 0.003(3) 0.015(3) 0.015(3) C23 0.048(4) 0.058(4) 0.041(3) 0.001(3) 0.011(3) 0.007(3) C22 0.051(4) 0.054(4) 0.040(4) 0.011(3) 0.016(3) 0.007(3) C21 0.060(4) 0.071(4) 0.054(4) -0.002(3) 0.021(4) 0.023(3) C20 0.052(4) 0.070(4) 0.042(4) -0.005(3) 0.005(3) 0.018(3) C25 0.042(4) 0.070(4) 0.052(4) 0.016(4) 0.018(4) 0.008(3) C26 0.049(4) 0.090(5) 0.075(5) 0.015(4) 0.016(4) 0.029(4) N2 0.047(3) 0.123(5) 0.042(3) -0.011(3) 0.013(3) 0.031(3) N1 0.036(3) 0.058(3) 0.046(3) -0.004(2) 0.013(2) 0.014(2) N3 0.035(3) 0.058(3) 0.037(3) -0.001(2) 0.015(2) 0.014(2) N5 0.049(3) 0.052(3) 0.052(3) 0.007(3) 0.014(3) 0.012(2) N4 0.045(3) 0.056(3) 0.049(3) 0.012(2) 0.013(3) 0.021(3) N6 0.041(3) 0.042(3) 0.049(3) -0.003(2) 0.008(2) 0.026(2) O1 0.049(3) 0.089(3) 0.046(2) 0.005(2) 0.021(2) 0.030(2) O2 0.058(3) 0.116(4) 0.070(3) -0.008(3) 0.014(2) 0.045(3) O3 0.044(3) 0.081(3) 0.046(3) 0.006(2) 0.006(2) 0.027(2) O4 0.069(3) 0.066(3) 0.076(3) -0.011(3) 0.007(3) 0.031(2) O5 0.052(3) 0.104(4) 0.055(3) 0.001(3) 0.004(2) 0.017(3) O6 0.050(3) 0.073(3) 0.064(3) 0.007(2) 0.015(2) 0.021(2) B 0.044(5) 0.082(6) 0.056(6) 0.013(5) 0.023(4) 0.017(5) F1 0.069(3) 0.126(3) 0.075(3) 0.004(2) 0.036(2) 0.033(2) F2 0.112(11) 0.210(14) 0.135(13) -0.007(12) 0.077(10) -0.057(10) F2' 0.035(7) 0.17(2) 0.092(12) -0.049(12) 0.007(8) 0.009(9) F3 0.110(8) 0.159(12) 0.061(7) -0.038(9) 0.019(5) 0.031(8) F3' 0.30(4) 0.17(2) 0.095(17) 0.072(16) 0.13(2) 0.11(2) F4 0.145(12) 0.189(16) 0.135(10) 0.088(11) 0.091(10) 0.115(12) F4' 0.154(17) 0.069(9) 0.164(18) -0.004(13) 0.064(16) -0.008(10) _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 N4 2.275(5) . ? Ag N1 2.337(4) . ? Ag O4 2.391(4) . ? Ag O1 2.411(4) . ? Ag Ag 3.1186(12) 2_665 ? C4 N2 1.327(7) . ? C4 N1 1.328(6) . ? C4 N3 1.406(6) . ? C3 N2 1.330(8) . ? C3 C2 1.359(8) . ? C3 H3A 0.9300 . ? C2 C1 1.354(8) . ? C2 H2A 0.9300 . ? C1 N1 1.345(6) . ? C1 H1A 0.9300 . ? C5 O1 1.228(6) . ? C5 N3 1.358(6) . ? C5 C6 1.499(7) . ? C6 C11 1.387(7) . ? C6 C7 1.395(7) . ? C11 C10 1.376(7) . ? C11 H11A 0.9300 . ? C10 C9 1.384(7) . ? C10 H10A 0.9300 . ? C9 C8 1.385(7) . ? C9 C12 1.492(7) . ? C8 C7 1.361(7) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C12 O2 1.199(7) . ? C12 O3 1.314(7) . ? C13 O3 1.461(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C17 N4 1.336(6) . ? C17 N5 1.336(7) . ? C17 N6 1.400(6) . ? C16 N5 1.327(7) . ? C16 C15 1.365(8) . ? C16 H16A 0.9300 . ? C15 C14 1.374(8) . ? C15 H15A 0.9300 . ? C14 N4 1.332(7) . ? C14 H14A 0.9300 . ? C18 O4 1.219(6) . ? C18 N6 1.355(7) . ? C18 C19 1.494(8) . ? C19 C20 1.372(7) . ? C19 C24 1.389(7) . ? C24 C23 1.371(7) . ? C24 H24A 0.9300 . ? C23 C22 1.376(7) . ? C23 H23A 0.9300 . ? C22 C21 1.379(8) . ? C22 C25 1.484(8) . ? C21 C20 1.381(8) . ? C21 H21A 0.9300 . ? C20 H20A 0.9300 . ? C25 O5 1.189(7) . ? C25 O6 1.334(7) . ? C26 O6 1.454(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N3 H3B 0.8600 . ? N6 H6A 0.8600 . ? B F2 1.299(14) . ? B F3 1.323(12) . ? B F3' 1.328(19) . ? B F4 1.349(13) . ? B F1 1.360(8) . ? B F2' 1.381(17) . ? B F4' 1.386(17) . ? F2 F2' 1.10(2) . ? F2 F3' 1.35(3) . ? F2' F4 1.45(2) . ? F3 F3' 1.13(3) . ? F3 F4' 1.44(2) . ? F4 F4' 1.110(18) . ? 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 N4 Ag N1 165.44(17) . . ? N4 Ag O4 77.68(15) . . ? N1 Ag O4 91.82(15) . . ? N4 Ag O1 115.70(15) . . ? N1 Ag O1 73.46(14) . . ? O4 Ag O1 164.28(14) . . ? N4 Ag Ag 126.18(13) . 2_665 ? N1 Ag Ag 67.75(12) . 2_665 ? O4 Ag Ag 119.05(13) . 2_665 ? O1 Ag Ag 60.96(11) . 2_665 ? N2 C4 N1 126.3(5) . . ? N2 C4 N3 112.0(4) . . ? N1 C4 N3 121.6(5) . . ? N2 C3 C2 123.2(6) . . ? N2 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C1 C2 C3 116.4(6) . . ? C1 C2 H2A 121.8 . . ? C3 C2 H2A 121.8 . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? O1 C5 N3 123.3(5) . . ? O1 C5 C6 120.0(5) . . ? N3 C5 C6 116.7(5) . . ? C11 C6 C7 118.7(5) . . ? C11 C6 C5 117.0(5) . . ? C7 C6 C5 124.3(5) . . ? C10 C11 C6 121.1(5) . . ? C10 C11 H11A 119.4 . . ? C6 C11 H11A 119.4 . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C9 C8 118.8(5) . . ? C10 C9 C12 122.5(5) . . ? C8 C9 C12 118.7(5) . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C7 C6 119.7(5) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? O2 C12 O3 123.0(5) . . ? O2 C12 C9 123.4(6) . . ? O3 C12 C9 113.6(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 C17 N5 126.0(5) . . ? N4 C17 N6 122.4(5) . . ? N5 C17 N6 111.6(4) . . ? N5 C16 C15 123.2(6) . . ? N5 C16 H16A 118.4 . . ? C15 C16 H16A 118.4 . . ? C16 C15 C14 115.7(6) . . ? C16 C15 H15A 122.2 . . ? C14 C15 H15A 122.2 . . ? N4 C14 C15 123.8(6) . . ? N4 C14 H14A 118.1 . . ? C15 C14 H14A 118.1 . . ? O4 C18 N6 124.4(5) . . ? O4 C18 C19 119.3(5) . . ? N6 C18 C19 116.3(5) . . ? C20 C19 C24 118.7(5) . . ? C20 C19 C18 122.9(5) . . ? C24 C19 C18 118.4(5) . . ? C23 C24 C19 120.5(5) . . ? C23 C24 H24A 119.7 . . ? C19 C24 H24A 119.7 . . ? C24 C23 C22 121.1(5) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C22 C21 118.2(5) . . ? C23 C22 C25 120.4(5) . . ? C21 C22 C25 121.4(5) . . ? C22 C21 C20 121.1(5) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C19 C20 C21 120.4(5) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? O5 C25 O6 124.2(6) . . ? O5 C25 C22 124.2(6) . . ? O6 C25 C22 111.7(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 . . ? C4 N2 C3 115.7(5) . . ? C4 N1 C1 115.3(5) . . ? C4 N1 Ag 128.5(4) . . ? C1 N1 Ag 113.3(3) . . ? C5 N3 C4 129.7(4) . . ? C5 N3 H3B 115.2 . . ? C4 N3 H3B 115.2 . . ? C16 N5 C17 116.2(5) . . ? C14 N4 C17 115.0(5) . . ? C14 N4 Ag 113.4(4) . . ? C17 N4 Ag 131.5(4) . . ? C18 N6 C17 131.3(4) . . ? C18 N6 H6A 114.4 . . ? C17 N6 H6A 114.4 . . ? C5 O1 Ag 129.1(4) . . ? C12 O3 C13 116.9(4) . . ? C18 O4 Ag 130.1(4) . . ? C25 O6 C26 116.1(5) . . ? F2 B F3 111.0(12) . . ? F2 B F3' 61.9(15) . . ? F3 B F3' 50.6(13) . . ? F2 B F4 110.0(11) . . ? F3 B F4 111.8(12) . . ? F3' B F4 140.1(11) . . ? F2 B F1 110.4(9) . . ? F3 B F1 107.7(8) . . ? F3' B F1 113.5(11) . . ? F4 B F1 105.9(8) . . ? F2 B F2' 48.4(11) . . ? F3 B F2' 143.7(11) . . ? F3' B F2' 107.2(19) . . ? F4 B F2' 64.4(11) . . ? F1 B F2' 107.9(9) . . ? F2 B F4' 131.0(11) . . ? F3 B F4' 64.0(11) . . ? F3' B F4' 105.3(14) . . ? F4 B F4' 47.9(10) . . ? F1 B F4' 117.5(11) . . ? F2' B F4' 104.7(13) . . ? F2' F2 B 69.7(14) . . ? F2' F2 F3' 125(2) . . ? B F2 F3' 60.1(12) . . ? F2 F2' B 61.9(11) . . ? F2 F2' F4 115.5(16) . . ? B F2' F4 56.8(9) . . ? F3' F3 B 64.9(12) . . ? F3' F3 F4' 113.5(18) . . ? B F3 F4' 60.1(9) . . ? F3 F3' B 64.5(14) . . ? F3 F3' F2 120.6(19) . . ? B F3' F2 58.0(10) . . ? F4' F4 B 67.8(12) . . ? F4' F4 F2' 116.7(17) . . ? B F4 F2' 58.9(9) . . ? F4 F4' B 64.3(11) . . ? F4 F4' F3 120.1(16) . . ? B F4' F3 55.9(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.643 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.092 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 888043' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Ag F6 N6 O6 P' _chemical_formula_weight 767.34 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' _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 11.1676(15) _cell_length_b 11.3893(18) _cell_length_c 12.6805(12) _cell_angle_alpha 80.868(10) _cell_angle_beta 63.900(9) _cell_angle_gamma 88.796(12) _cell_volume 1427.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.94 _cell_measurement_theta_max 12.30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8993 _exptl_absorpt_correction_T_max 0.9973 _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_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5831 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4997 _reflns_number_gt 3342 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.3590P] 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 4997 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.94190(4) 0.63362(3) 0.52529(3) 0.07112(16) Uani 1 1 d . . . C4 C 0.7308(4) 0.4250(3) 0.7365(3) 0.0444(9) Uani 1 1 d . . . C3 C 0.7220(5) 0.3722(4) 0.9188(4) 0.0769(14) Uani 1 1 d . . . H3A H 0.6786 0.3326 0.9969 0.092 Uiso 1 1 calc R . . C2 C 0.8405(4) 0.4323(4) 0.8832(4) 0.0586(11) Uani 1 1 d . . . H2A H 0.8797 0.4335 0.9344 0.070 Uiso 1 1 calc R . . C1 C 0.8987(4) 0.4902(4) 0.7699(4) 0.0570(10) Uani 1 1 d . . . H1A H 0.9791 0.5335 0.7436 0.068 Uiso 1 1 calc R . . C5 C 0.7116(4) 0.4374(3) 0.5449(3) 0.0410(8) Uani 1 1 d . . . C6 C 0.6258(3) 0.3913(3) 0.4964(3) 0.0382(8) Uani 1 1 d . . . C11 C 0.6653(4) 0.4209(3) 0.3757(3) 0.0482(9) Uani 1 1 d . . . H11A H 0.7432 0.4683 0.3285 0.058 Uiso 1 1 calc R . . C10 C 0.5917(4) 0.3816(3) 0.3235(3) 0.0490(9) Uani 1 1 d . . . H10A H 0.6209 0.4016 0.2417 0.059 Uiso 1 1 calc R . . C9 C 0.4751(3) 0.3128(3) 0.3923(3) 0.0423(9) Uani 1 1 d . . . C8 C 0.4325(4) 0.2857(4) 0.5137(3) 0.0543(10) Uani 1 1 d . . . H8A H 0.3524 0.2413 0.5611 0.065 Uiso 1 1 calc R . . C7 C 0.5067(4) 0.3234(3) 0.5657(3) 0.0512(10) Uani 1 1 d . . . H7A H 0.4772 0.3034 0.6476 0.061 Uiso 1 1 calc R . . C12 C 0.3914(4) 0.2672(3) 0.3416(4) 0.0502(10) Uani 1 1 d . . . C13 C 0.3600(5) 0.2674(4) 0.1686(4) 0.0737(13) Uani 1 1 d . . . H13A H 0.4012 0.3018 0.0857 0.111 Uiso 1 1 calc R . . H13B H 0.2703 0.2925 0.2055 0.111 Uiso 1 1 calc R . . H13C H 0.3584 0.1822 0.1767 0.111 Uiso 1 1 calc R . . C17 C 1.0967(4) 0.8972(3) 0.3785(3) 0.0460(9) Uani 1 1 d . . . C16 C 1.1021(4) 0.9888(4) 0.2052(4) 0.0639(12) Uani 1 1 d . . . H16A H 1.1299 1.0526 0.1425 0.077 Uiso 1 1 calc R . . C15 C 1.0280(5) 0.8967(4) 0.2038(4) 0.0663(12) Uani 1 1 d . . . H15A H 1.0031 0.8967 0.1428 0.080 Uiso 1 1 calc R . . C14 C 0.9921(4) 0.8049(4) 0.2955(4) 0.0636(12) Uani 1 1 d . . . H14A H 0.9417 0.7405 0.2962 0.076 Uiso 1 1 calc R . . C18 C 1.1212(4) 0.8364(3) 0.5682(3) 0.0498(10) Uani 1 1 d . . . C19 C 1.1913(4) 0.8738(3) 0.6347(3) 0.0447(9) Uani 1 1 d . . . C24 C 1.1492(4) 0.8204(3) 0.7518(3) 0.0541(10) Uani 1 1 d . . . H24A H 1.0782 0.7636 0.7867 0.065 Uiso 1 1 calc R . . C23 C 1.2110(4) 0.8503(3) 0.8172(3) 0.0539(10) Uani 1 1 d . . . H23A H 1.1805 0.8145 0.8963 0.065 Uiso 1 1 calc R . . C22 C 1.3177(4) 0.9327(3) 0.7666(3) 0.0456(9) Uani 1 1 d . . . C21 C 1.3590(4) 0.9848(4) 0.6504(4) 0.0692(13) Uani 1 1 d . . . H21A H 1.4311 1.0405 0.6150 0.083 Uiso 1 1 calc R . . C20 C 1.2969(4) 0.9569(4) 0.5848(3) 0.0668(12) Uani 1 1 d . . . H20A H 1.3263 0.9943 0.5063 0.080 Uiso 1 1 calc R . . C25 C 1.3833(4) 0.9625(4) 0.8398(4) 0.0513(10) Uani 1 1 d . . . C26 C 1.5444(5) 1.0875(4) 0.8471(4) 0.0771(14) Uani 1 1 d . . . H26A H 1.6153 1.1456 0.7956 0.116 Uiso 1 1 calc R . . H26B H 1.5798 1.0221 0.8802 0.116 Uiso 1 1 calc R . . H26C H 1.4784 1.1232 0.9103 0.116 Uiso 1 1 calc R . . N2 N 0.6648(4) 0.3674(3) 0.8461(3) 0.0729(11) Uani 1 1 d . . . N1 N 0.8459(3) 0.4882(3) 0.6927(3) 0.0490(8) Uani 1 1 d . . . N3 N 0.6678(3) 0.4114(3) 0.6652(3) 0.0501(8) Uani 1 1 d . . . H3B H 0.5872 0.3813 0.7039 0.060 Uiso 1 1 calc R . . N5 N 1.1363(3) 0.9915(3) 0.2929(3) 0.0585(9) Uani 1 1 d . . . N4 N 1.0253(3) 0.8015(3) 0.3860(3) 0.0530(8) Uani 1 1 d . . . N6 N 1.1414(3) 0.9076(3) 0.4642(3) 0.0539(8) Uani 1 1 d . . . H6A H 1.1910 0.9710 0.4480 0.065 Uiso 1 1 calc R . . O1 O 0.8164(3) 0.4933(3) 0.4793(2) 0.0625(8) Uani 1 1 d . . . O2 O 0.2937(3) 0.2017(3) 0.3984(3) 0.0879(10) Uani 1 1 d . . . O3 O 0.4359(3) 0.3067(3) 0.2262(2) 0.0651(8) Uani 1 1 d . . . O4 O 1.0493(4) 0.7460(3) 0.6081(3) 0.0871(11) Uani 1 1 d . . . O5 O 1.3507(3) 0.9173(3) 0.9413(3) 0.0719(8) Uani 1 1 d . . . O6 O 1.4833(3) 1.0444(2) 0.7793(2) 0.0637(8) Uani 1 1 d . . . P P 0.80604(10) 0.69960(10) 0.08562(9) 0.0531(3) Uani 1 1 d . . . F1 F 0.6514(7) 0.6655(10) 0.1389(10) 0.098(3) Uani 0.70 1 d P A 1 F2 F 0.8292(9) 0.6952(8) -0.0441(7) 0.084(3) Uani 0.70 1 d P A 1 F3 F 0.7841(9) 0.6992(10) 0.2182(8) 0.082(3) Uani 0.70 1 d P A 1 F4 F 0.9583(6) 0.7263(6) 0.0399(6) 0.082(2) Uani 0.70 1 d P A 1 F5 F 0.8331(7) 0.5598(4) 0.1021(4) 0.0910(18) Uani 0.70 1 d P A 1 F6 F 0.7840(8) 0.8340(5) 0.0718(6) 0.1035(18) Uani 0.70 1 d P A 1 F1' F 0.691(3) 0.615(3) 0.127(3) 0.178(16) Uani 0.30 1 d P A 2 F2' F 0.787(3) 0.740(3) -0.028(2) 0.200(16) Uani 0.30 1 d P A 2 F3' F 0.832(3) 0.660(3) 0.194(2) 0.133(10) Uani 0.30 1 d P A 2 F4' F 0.925(2) 0.801(2) 0.0297(13) 0.130(8) Uani 0.30 1 d P A 2 F5' F 0.908(4) 0.620(3) 0.022(3) 0.261(14) Uani 0.30 1 d P A 2 F6' F 0.717(2) 0.794(2) 0.148(2) 0.216(12) Uani 0.30 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 0.0797(3) 0.0705(2) 0.0690(2) 0.00698(16) -0.0425(2) -0.03854(18) C4 0.051(2) 0.045(2) 0.045(2) -0.0054(17) -0.0278(19) -0.0061(18) C3 0.089(3) 0.099(4) 0.054(3) 0.014(2) -0.050(3) -0.032(3) C2 0.075(3) 0.063(3) 0.061(3) -0.009(2) -0.051(2) -0.001(2) C1 0.059(3) 0.062(2) 0.062(3) -0.011(2) -0.038(2) -0.011(2) C5 0.042(2) 0.045(2) 0.043(2) -0.0087(16) -0.0238(19) -0.0036(17) C6 0.036(2) 0.0424(19) 0.042(2) -0.0096(16) -0.0221(17) 0.0000(16) C11 0.049(2) 0.051(2) 0.046(2) 0.0008(17) -0.0240(19) -0.0162(18) C10 0.057(2) 0.054(2) 0.042(2) -0.0036(17) -0.0276(19) -0.0093(19) C9 0.042(2) 0.045(2) 0.050(2) -0.0155(17) -0.0271(19) 0.0035(17) C8 0.047(2) 0.071(3) 0.047(2) -0.0087(19) -0.023(2) -0.019(2) C7 0.050(2) 0.064(2) 0.039(2) -0.0037(18) -0.0203(19) -0.0149(19) C12 0.049(2) 0.057(2) 0.058(3) -0.015(2) -0.034(2) -0.001(2) C13 0.086(3) 0.092(3) 0.073(3) -0.026(3) -0.058(3) -0.004(3) C17 0.046(2) 0.050(2) 0.048(2) -0.0121(19) -0.0239(19) 0.0002(18) C16 0.075(3) 0.067(3) 0.057(3) 0.001(2) -0.038(2) -0.004(2) C15 0.082(3) 0.075(3) 0.060(3) -0.015(2) -0.047(3) 0.006(3) C14 0.071(3) 0.070(3) 0.072(3) -0.020(2) -0.049(3) -0.001(2) C18 0.058(2) 0.046(2) 0.052(2) -0.0082(18) -0.030(2) -0.0080(19) C19 0.049(2) 0.044(2) 0.044(2) -0.0069(17) -0.0234(19) -0.0056(18) C24 0.054(2) 0.059(2) 0.049(2) 0.0033(19) -0.026(2) -0.020(2) C23 0.056(2) 0.066(3) 0.041(2) 0.0009(19) -0.025(2) -0.013(2) C22 0.054(2) 0.047(2) 0.041(2) -0.0096(17) -0.0253(19) -0.0007(18) C21 0.075(3) 0.073(3) 0.063(3) 0.008(2) -0.037(2) -0.038(2) C20 0.079(3) 0.078(3) 0.046(2) 0.007(2) -0.035(2) -0.034(2) C25 0.052(3) 0.056(2) 0.051(2) -0.015(2) -0.025(2) 0.003(2) C26 0.077(3) 0.088(3) 0.094(3) -0.029(3) -0.058(3) -0.008(3) N2 0.076(3) 0.094(3) 0.054(2) 0.0165(19) -0.042(2) -0.038(2) N1 0.0478(19) 0.0580(19) 0.0500(18) -0.0064(15) -0.0299(16) -0.0098(15) N3 0.0491(19) 0.063(2) 0.0429(18) 0.0013(15) -0.0271(15) -0.0193(15) N5 0.071(2) 0.060(2) 0.053(2) -0.0017(17) -0.0369(18) -0.0102(18) N4 0.060(2) 0.0549(19) 0.0540(19) -0.0100(15) -0.0335(17) -0.0049(16) N6 0.060(2) 0.0570(19) 0.0523(19) -0.0011(16) -0.0339(17) -0.0193(16) O1 0.0530(17) 0.087(2) 0.0475(15) -0.0055(14) -0.0233(14) -0.0271(15) O2 0.075(2) 0.129(3) 0.070(2) -0.0056(19) -0.0416(18) -0.043(2) O3 0.075(2) 0.081(2) 0.0566(18) -0.0082(15) -0.0449(16) -0.0170(15) O4 0.128(3) 0.068(2) 0.090(2) 0.0179(17) -0.079(2) -0.046(2) O5 0.091(2) 0.079(2) 0.0601(19) -0.0014(16) -0.0499(18) -0.0136(17) O6 0.0633(18) 0.0731(19) 0.0656(18) -0.0132(15) -0.0372(15) -0.0128(15) P 0.0506(7) 0.0685(8) 0.0423(6) -0.0039(5) -0.0235(5) -0.0107(6) F1 0.042(2) 0.166(10) 0.080(4) -0.011(5) -0.024(2) -0.013(4) F2 0.095(4) 0.120(5) 0.041(3) -0.017(4) -0.032(3) -0.019(3) F3 0.072(4) 0.129(8) 0.042(2) -0.022(4) -0.019(3) -0.025(4) F4 0.046(2) 0.118(5) 0.068(3) 0.005(3) -0.017(2) -0.017(3) F5 0.128(5) 0.060(3) 0.069(3) 0.006(2) -0.034(3) -0.004(3) F6 0.122(6) 0.060(3) 0.101(4) 0.000(3) -0.029(4) 0.008(3) F1' 0.23(3) 0.18(3) 0.14(2) 0.083(17) -0.13(2) -0.17(2) F2' 0.21(3) 0.26(3) 0.15(2) 0.150(19) -0.16(2) -0.16(2) F3' 0.17(3) 0.14(2) 0.12(2) 0.050(15) -0.11(2) -0.051(16) F4' 0.15(2) 0.166(16) 0.062(7) 0.007(11) -0.040(10) -0.115(15) F5' 0.34(4) 0.21(3) 0.30(4) -0.18(3) -0.18(3) 0.18(3) F6' 0.141(18) 0.145(18) 0.26(3) -0.042(18) 0.005(18) 0.079(16) _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 N4 2.280(3) . ? Ag N1 2.314(3) . ? Ag O4 2.404(3) . ? Ag O1 2.443(2) . ? Ag Ag 3.3287(9) 2_766 ? C4 N2 1.317(5) . ? C4 N1 1.328(4) . ? C4 N3 1.395(4) . ? C3 N2 1.340(5) . ? C3 C2 1.356(6) . ? C3 H3A 0.9300 . ? C2 C1 1.348(5) . ? C2 H2A 0.9300 . ? C1 N1 1.349(4) . ? C1 H1A 0.9300 . ? C5 O1 1.214(4) . ? C5 N3 1.364(4) . ? C5 C6 1.488(4) . ? C6 C11 1.378(5) . ? C6 C7 1.392(5) . ? C11 C10 1.379(5) . ? C11 H11A 0.9300 . ? C10 C9 1.378(5) . ? C10 H10A 0.9300 . ? C9 C8 1.379(5) . ? C9 C12 1.488(5) . ? C8 C7 1.375(5) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C12 O2 1.199(4) . ? C12 O3 1.323(5) . ? C13 O3 1.455(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C17 N5 1.325(5) . ? C17 N4 1.331(4) . ? C17 N6 1.400(4) . ? C16 N5 1.330(5) . ? C16 C15 1.357(6) . ? C16 H16A 0.9300 . ? C15 C14 1.352(6) . ? C15 H15A 0.9300 . ? C14 N4 1.347(5) . ? C14 H14A 0.9300 . ? C18 O4 1.214(4) . ? C18 N6 1.362(5) . ? C18 C19 1.488(5) . ? C19 C20 1.374(5) . ? C19 C24 1.381(5) . ? C24 C23 1.371(5) . ? C24 H24A 0.9300 . ? C23 C22 1.377(5) . ? C23 H23A 0.9300 . ? C22 C21 1.369(5) . ? C22 C25 1.490(5) . ? C21 C20 1.368(5) . ? C21 H21A 0.9300 . ? C20 H20A 0.9300 . ? C25 O5 1.200(4) . ? C25 O6 1.329(5) . ? C26 O6 1.453(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N3 H3B 0.8600 . ? N6 H6A 0.8600 . ? P F5' 1.464(19) . ? P F1' 1.468(19) . ? P F6' 1.517(17) . ? P F3' 1.52(3) . ? P F6 1.539(5) . ? P F2' 1.54(2) . ? P F4 1.555(6) . ? P F2 1.558(7) . ? P F1 1.583(8) . ? P F3 1.588(9) . ? P F4' 1.602(13) . ? P F5 1.612(5) . ? 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 N4 Ag N1 168.95(11) . . ? N4 Ag O4 76.91(10) . . ? N1 Ag O4 94.79(10) . . ? N4 Ag O1 114.36(10) . . ? N1 Ag O1 73.83(9) . . ? O4 Ag O1 168.62(9) . . ? N4 Ag Ag 122.69(8) . 2_766 ? N1 Ag Ag 67.34(8) . 2_766 ? O4 Ag Ag 115.39(9) . 2_766 ? O1 Ag Ag 60.76(7) . 2_766 ? N2 C4 N1 126.4(3) . . ? N2 C4 N3 112.5(3) . . ? N1 C4 N3 121.2(3) . . ? N2 C3 C2 122.8(4) . . ? N2 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C1 C2 C3 116.6(4) . . ? C1 C2 H2A 121.7 . . ? C3 C2 H2A 121.7 . . ? C2 C1 N1 123.2(4) . . ? C2 C1 H1A 118.4 . . ? N1 C1 H1A 118.4 . . ? O1 C5 N3 122.4(3) . . ? O1 C5 C6 120.9(3) . . ? N3 C5 C6 116.7(3) . . ? C11 C6 C7 118.3(3) . . ? C11 C6 C5 117.6(3) . . ? C7 C6 C5 124.1(3) . . ? C6 C11 C10 121.3(3) . . ? C6 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C9 C8 119.0(3) . . ? C10 C9 C12 122.8(3) . . ? C8 C9 C12 118.1(3) . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? O2 C12 O3 123.1(3) . . ? O2 C12 C9 124.1(4) . . ? O3 C12 C9 112.8(3) . . ? 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 . . ? N5 C17 N4 126.6(3) . . ? N5 C17 N6 111.5(3) . . ? N4 C17 N6 121.9(3) . . ? N5 C16 C15 122.5(4) . . ? N5 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? C14 C15 C16 116.7(4) . . ? C14 C15 H15A 121.6 . . ? C16 C15 H15A 121.6 . . ? N4 C14 C15 123.6(4) . . ? N4 C14 H14A 118.2 . . ? C15 C14 H14A 118.2 . . ? O4 C18 N6 123.2(3) . . ? O4 C18 C19 119.6(3) . . ? N6 C18 C19 117.2(3) . . ? C20 C19 C24 118.6(3) . . ? C20 C19 C18 123.3(3) . . ? C24 C19 C18 118.1(3) . . ? C23 C24 C19 120.7(3) . . ? C23 C24 H24A 119.7 . . ? C19 C24 H24A 119.7 . . ? C24 C23 C22 120.6(3) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C21 C22 C23 118.2(3) . . ? C21 C22 C25 122.5(3) . . ? C23 C22 C25 119.3(3) . . ? C20 C21 C22 121.7(4) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C21 C20 C19 120.2(4) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? O5 C25 O6 123.7(4) . . ? O5 C25 C22 124.1(4) . . ? O6 C25 C22 112.2(3) . . ? 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 . . ? C4 N2 C3 116.0(3) . . ? C4 N1 C1 115.1(3) . . ? C4 N1 Ag 129.6(2) . . ? C1 N1 Ag 113.2(2) . . ? C5 N3 C4 131.3(3) . . ? C5 N3 H3B 114.3 . . ? C4 N3 H3B 114.3 . . ? C17 N5 C16 116.2(3) . . ? C17 N4 C14 114.4(3) . . ? C17 N4 Ag 132.6(2) . . ? C14 N4 Ag 113.0(3) . . ? C18 N6 C17 132.2(3) . . ? C18 N6 H6A 113.9 . . ? C17 N6 H6A 113.9 . . ? C5 O1 Ag 129.0(2) . . ? C12 O3 C13 116.9(3) . . ? C18 O4 Ag 132.5(3) . . ? C25 O6 C26 115.9(3) . . ? F5' P F1' 96.6(18) . . ? F5' P F6' 171.8(16) . . ? F1' P F6' 91.6(16) . . ? F5' P F3' 88.8(15) . . ? F1' P F3' 94.3(16) . . ? F6' P F3' 89.6(13) . . ? F5' P F6 137.0(16) . . ? F1' P F6 118.9(15) . . ? F6' P F6 37.0(9) . . ? F3' P F6 110.3(11) . . ? F5' P F2' 89.4(15) . . ? F1' P F2' 87.6(14) . . ? F6' P F2' 91.9(17) . . ? F3' P F2' 177.6(15) . . ? F6 P F2' 70.1(13) . . ? F5' P F4 56.6(14) . . ? F1' P F4 150.7(15) . . ? F6' P F4 115.2(11) . . ? F3' P F4 75.3(11) . . ? F6 P F4 90.4(3) . . ? F2' P F4 102.3(11) . . ? F5' P F2 64.2(12) . . ? F1' P F2 87.8(12) . . ? F6' P F2 117.3(12) . . ? F3' P F2 152.9(11) . . ? F6 P F2 92.0(4) . . ? F2' P F2 25.4(14) . . ? F4 P F2 89.8(4) . . ? F5' P F1 122.1(15) . . ? F1' P F1 26.6(16) . . ? F6' P F1 66.2(11) . . ? F3' P F1 101.2(12) . . ? F6 P F1 92.5(5) . . ? F2' P F1 81.1(11) . . ? F4 P F1 176.1(5) . . ? F2 P F1 92.7(6) . . ? F5' P F3 114.0(12) . . ? F1' P F3 91.4(13) . . ? F6' P F3 64.7(12) . . ? F3' P F3 25.2(11) . . ? F6 P F3 90.1(5) . . ? F2' P F3 156.5(14) . . ? F4 P F3 89.8(4) . . ? F2 P F3 177.9(5) . . ? F1 P F3 87.5(5) . . ? F5' P F4' 85.8(15) . . ? F1' P F4' 172.9(14) . . ? F6' P F4' 86.2(12) . . ? F3' P F4' 92.5(13) . . ? F6 P F4' 56.3(9) . . ? F2' P F4' 85.8(11) . . ? F4 P F4' 34.4(9) . . ? F2 P F4' 87.2(6) . . ? F1 P F4' 148.8(11) . . ? F3 P F4' 93.7(6) . . ? F5' P F5 42.6(15) . . ? F1' P F5 62.9(14) . . ? F6' P F5 143.1(10) . . ? F3' P F5 67.9(12) . . ? F6 P F5 177.8(4) . . ? F2' P F5 111.7(13) . . ? F4 P F5 88.0(4) . . ? F2 P F5 89.5(4) . . ? F1 P F5 89.1(4) . . ? F3 P F5 88.5(4) . . ? F4' P F5 122.1(11) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.282 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.074 #===END