# 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_email hmc@fjirsm.ac.cn _publ_contact_author_name 'Wei Wei' loop_ _publ_author_name 'Wei Wei' 'Hongtao Yu' 'Feilong Jiang' 'Bing Liu' 'Jie Ma' 'Maochun Hong' data_complex1a _database_code_depnum_ccdc_archive 'CCDC 699856' #TrackingRef '- 1a-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Ag2 B2 F8 N8 O5 S6' _chemical_formula_weight 1144.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.164(2) _cell_length_b 14.237(2) _cell_length_c 8.9017(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.170(7) _cell_angle_gamma 90.00 _cell_volume 2174.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3712 _cell_measurement_theta_min 3.0269 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.9276 _exptl_absorpt_process_details 'CrystalClear (Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8334 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2545 _reflns_number_gt 2102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0703P)^2^+5.3738P] 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 2540 _refine_ls_number_parameters 158 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.008 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 0.0000 0.34652(2) -0.5000 0.06341(9) Uani 1 2 d S . . S1 S 0.15455(4) 0.29576(5) 0.37036(7) 0.06589(19) Uani 1 1 d . . . S2 S 0.19417(5) 0.5000 0.30724(12) 0.0672(3) Uani 1 2 d S . . N1 N 0.07780(14) 0.31099(17) -0.2553(2) 0.0611(6) Uani 1 1 d . . . N2 N 0.09166(11) 0.45170(15) 0.4286(2) 0.0490(5) Uani 1 1 d . . . C1 C 0.10328(18) 0.2343(2) -0.0056(3) 0.0709(9) Uani 1 1 d . . . H1 H 0.0896 0.1876 0.0533 0.085 Uiso 1 1 calc R . . C2 C 0.0609(2) 0.2449(2) -0.1646(3) 0.0731(9) Uani 1 1 d . . . H2 H 0.0192 0.2047 -0.2104 0.088 Uiso 1 1 calc R . . C3 C 0.13940(17) 0.3652(2) -0.1860(3) 0.0619(7) Uani 1 1 d . . . H3 H 0.1533 0.4101 -0.2476 0.074 Uiso 1 1 calc R . . C4 C 0.18339(17) 0.3582(2) -0.0279(3) 0.0656(8) Uani 1 1 d . . . H4 H 0.2254 0.3983 0.0156 0.079 Uiso 1 1 calc R . . C5 C 0.16480(14) 0.2913(2) 0.0659(3) 0.0627(7) Uani 1 1 d . . . C6 C 0.21167(16) 0.2798(2) 0.2390(3) 0.0730(8) Uani 1 1 d . . . H6A H 0.2540 0.3250 0.2668 0.088 Uiso 1 1 calc R . . H6B H 0.2345 0.2174 0.2554 0.088 Uiso 1 1 calc R . . C7 C 0.14253(13) 0.4170(2) 0.3696(2) 0.0511(6) Uani 1 1 d . . . F1 F 0.1538(3) 0.0752(3) 0.3352(5) 0.2139(19) Uani 1 1 d U . . B1 B 0.1607(4) 0.0000 0.2629(7) 0.0839(19) Uani 1 2 d S . . F3 F 0.2261(3) 0.0000 0.2479(10) 0.297(4) Uani 1 2 d SU . . F2 F 0.1105(6) 0.0000 0.1252(9) 0.300(5) Uani 1 2 d SU . . O1 O 0.3483(5) 0.5000 0.1877(12) 0.146(5) Uani 0.461(8) 2 d SPU A 1 O2 O 0.5000 0.4009(8) 0.5000 0.132(7) Uani 0.333(9) 2 d SPU B 1 O2' O 0.4276(9) 0.3986(10) 0.4519(15) 0.190(5) Uani 0.333(5) 1 d PU B 2 O1' O 0.3982(6) 0.5000 0.2584(19) 0.202(7) Uani 0.539(8) 2 d SPU A 2 O3 O 0.0000 0.5000 0.0000 0.382(11) Uiso 1 4 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.07628(16) 0.07961(19) 0.03470(13) 0.000 0.01870(11) 0.000 S1 0.0880(4) 0.0760(4) 0.0391(3) 0.0131(3) 0.0282(2) 0.0326(3) S2 0.0682(4) 0.0910(7) 0.0556(4) 0.000 0.0382(3) 0.000 N1 0.0849(13) 0.0649(12) 0.0334(9) 0.0067(9) 0.0193(9) 0.0167(11) N2 0.0588(9) 0.0549(10) 0.0376(9) 0.0012(8) 0.0217(7) 0.0033(8) C1 0.1024(18) 0.0693(16) 0.0450(12) 0.0179(12) 0.0296(12) 0.0213(15) C2 0.106(2) 0.0648(16) 0.0477(14) 0.0084(12) 0.0240(13) 0.0102(15) C3 0.0867(15) 0.0625(14) 0.0419(12) 0.0077(10) 0.0285(10) 0.0174(13) C4 0.0729(14) 0.0831(18) 0.0422(12) -0.0022(12) 0.0210(10) 0.0178(13) C5 0.0713(12) 0.0798(15) 0.0396(11) 0.0085(11) 0.0221(9) 0.0402(12) C6 0.0787(14) 0.0998(19) 0.0413(13) 0.0112(13) 0.0207(10) 0.0467(14) C7 0.0527(10) 0.0750(15) 0.0270(9) 0.0029(10) 0.0153(8) 0.0097(11) F1 0.365(5) 0.103(2) 0.207(3) -0.016(2) 0.139(3) 0.006(3) B1 0.097(3) 0.079(3) 0.070(3) 0.000 0.020(3) 0.000 F3 0.187(3) 0.385(12) 0.388(7) 0.000 0.187(4) 0.000 F2 0.378(10) 0.204(7) 0.194(6) 0.000 -0.075(7) 0.000 O1 0.085(5) 0.251(14) 0.115(6) 0.000 0.049(4) 0.000 O2 0.265(17) 0.068(6) 0.054(6) 0.000 0.040(8) 0.000 O2' 0.317(11) 0.140(9) 0.179(8) -0.030(7) 0.170(7) -0.052(9) O1' 0.131(7) 0.107(7) 0.373(18) 0.000 0.089(9) 0.000 _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 2.2304(19) 2_554 ? Ag1 N1 2.2304(19) . ? Ag1 N2 2.473(2) 1_554 ? Ag1 N2 2.473(2) 2 ? S1 C7 1.739(3) . ? S1 C6 1.815(3) . ? S2 C7 1.711(3) . ? S2 C7 1.711(3) 6_565 ? N1 C3 1.333(4) . ? N1 C2 1.340(4) . ? N2 C7 1.301(3) . ? N2 N2 1.375(4) 6_565 ? N2 Ag1 2.473(2) 1_556 ? C1 C5 1.358(4) . ? C1 C2 1.379(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.375(4) . ? C3 H3 0.9300 . ? C4 C5 1.380(4) . ? C4 H4 0.9300 . ? C5 C6 1.504(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? F1 B1 1.277(5) . ? B1 F3 1.238(9) . ? B1 F2 1.265(9) . ? B1 F1 1.277(5) 6 ? 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 153.78(13) 2_554 . ? N1 Ag1 N2 98.66(8) 2_554 1_554 ? N1 Ag1 N2 97.13(8) . 1_554 ? N1 Ag1 N2 97.13(8) 2_554 2 ? N1 Ag1 N2 98.66(8) . 2 ? N2 Ag1 N2 105.45(10) 1_554 2 ? C7 S1 C6 102.68(14) . . ? C7 S2 C7 87.40(18) . 6_565 ? C3 N1 C2 116.8(2) . . ? C3 N1 Ag1 119.16(18) . . ? C2 N1 Ag1 123.44(19) . . ? C7 N2 N2 112.32(15) . 6_565 ? C7 N2 Ag1 120.08(17) . 1_556 ? N2 N2 Ag1 127.27(5) 6_565 1_556 ? C5 C1 C2 120.8(3) . . ? C5 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? N1 C2 C1 122.3(3) . . ? N1 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? N1 C3 C4 123.3(3) . . ? N1 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C1 C5 C4 117.1(2) . . ? C1 C5 C6 121.1(3) . . ? C4 C5 C6 121.7(3) . . ? C5 C6 S1 113.28(19) . . ? C5 C6 H6A 108.9 . . ? S1 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? S1 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 S2 114.0(2) . . ? N2 C7 S1 118.7(2) . . ? S2 C7 S1 127.26(15) . . ? F3 B1 F2 107.9(8) . . ? F3 B1 F1 108.2(4) . . ? F2 B1 F1 109.3(4) . . ? F3 B1 F1 108.2(4) . 6 ? F2 B1 F1 109.3(4) . 6 ? F1 B1 F1 114.0(7) . 6 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C3 144.2(2) 2_554 . . . ? N2 Ag1 N1 C3 17.5(2) 1_554 . . . ? N2 Ag1 N1 C3 -89.4(2) 2 . . . ? N1 Ag1 N1 C2 -44.7(2) 2_554 . . . ? N2 Ag1 N1 C2 -171.4(2) 1_554 . . . ? N2 Ag1 N1 C2 81.7(2) 2 . . . ? C3 N1 C2 C1 1.9(5) . . . . ? Ag1 N1 C2 C1 -169.4(3) . . . . ? C5 C1 C2 N1 -0.2(5) . . . . ? C2 N1 C3 C4 -2.3(4) . . . . ? Ag1 N1 C3 C4 169.4(2) . . . . ? N1 C3 C4 C5 1.0(5) . . . . ? C2 C1 C5 C4 -1.2(5) . . . . ? C2 C1 C5 C6 -179.6(3) . . . . ? C3 C4 C5 C1 0.8(4) . . . . ? C3 C4 C5 C6 179.2(3) . . . . ? C1 C5 C6 S1 -60.8(4) . . . . ? C4 C5 C6 S1 120.9(3) . . . . ? C7 S1 C6 C5 -75.3(2) . . . . ? N2 N2 C7 S2 -0.56(16) 6_565 . . . ? Ag1 N2 C7 S2 173.38(9) 1_556 . . . ? N2 N2 C7 S1 176.42(9) 6_565 . . . ? Ag1 N2 C7 S1 -9.6(2) 1_556 . . . ? C7 S2 C7 N2 0.7(2) 6_565 . . . ? C7 S2 C7 S1 -175.96(7) 6_565 . . . ? C6 S1 C7 N2 167.25(17) . . . . ? C6 S1 C7 S2 -16.23(18) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.561 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.087 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 699859' #TrackingRef '- 1a-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Ag N5 O2 S3' _chemical_formula_weight 486.34 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 29.96(3) _cell_length_b 5.629(4) _cell_length_c 20.905(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.337(14) _cell_angle_gamma 90.00 _cell_volume 3416(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3100 _cell_measurement_theta_min 2.0109 _cell_measurement_theta_max 27.4427 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6509 _exptl_absorpt_correction_T_max 0.8983 _exptl_absorpt_process_details 'CrystalClear (Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12231 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.58 _reflns_number_total 3847 _reflns_number_gt 2589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0482P)^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 3847 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.124477(13) 0.12703(6) 0.530515(19) 0.05130(15) Uani 1 1 d . . . S1 S 0.29808(4) 0.4971(2) 0.35287(6) 0.0438(3) Uani 1 1 d . . . S2 S 0.37165(4) 0.7119(2) 0.29379(6) 0.0464(3) Uani 1 1 d . . . S3 S 0.43566(4) 0.6296(2) 0.20550(7) 0.0536(3) Uani 1 1 d . . . O1 O 0.14646(15) -0.4435(7) 0.5747(2) 0.0731(11) Uani 1 1 d . . . O2 O 0.09370(15) -0.4429(7) 0.4861(2) 0.0717(11) Uani 1 1 d . . . N1 N 0.12189(17) -0.3302(7) 0.5283(3) 0.0603(12) Uani 1 1 d . . . N2 N 0.17004(14) 0.1517(6) 0.45349(19) 0.0458(9) Uani 1 1 d . . . N3 N 0.33456(13) 0.3050(6) 0.25845(19) 0.0490(10) Uani 1 1 d . . . N4 N 0.36811(13) 0.3357(6) 0.22318(19) 0.0488(10) Uani 1 1 d . . . N5 N 0.56050(13) 0.4047(6) 0.0779(2) 0.0481(10) Uani 1 1 d . . . C1 C 0.23528(18) 0.0158(8) 0.4164(2) 0.0534(13) Uani 1 1 d . . . H1 H 0.2584 -0.0971 0.4197 0.064 Uiso 1 1 calc R . . C2 C 0.20402(18) -0.0016(8) 0.4551(3) 0.0556(13) Uani 1 1 d . . . H2 H 0.2070 -0.1291 0.4841 0.067 Uiso 1 1 calc R . . C3 C 0.16707(16) 0.3359(7) 0.4117(2) 0.0453(11) Uani 1 1 d . . . H3 H 0.1440 0.4479 0.4102 0.054 Uiso 1 1 calc R . . C4 C 0.19655(16) 0.3675(7) 0.3710(2) 0.0443(11) Uani 1 1 d . . . H4 H 0.1929 0.4974 0.3426 0.053 Uiso 1 1 calc R . . C5 C 0.23163(15) 0.2045(7) 0.3725(2) 0.0412(10) Uani 1 1 d . . . C6 C 0.26388(16) 0.2290(8) 0.3283(2) 0.0473(11) Uani 1 1 d . . . H6A H 0.2466 0.2412 0.2826 0.057 Uiso 1 1 calc R . . H6B H 0.2839 0.0912 0.3327 0.057 Uiso 1 1 calc R . . C7 C 0.33370(15) 0.4834(7) 0.2983(2) 0.0375(9) Uani 1 1 d . . . C8 C 0.38973(15) 0.5346(8) 0.2368(2) 0.0410(10) Uani 1 1 d . . . C9 C 0.43862(19) 0.3767(8) 0.1529(3) 0.0605(14) Uani 1 1 d . . . H9A H 0.4389 0.2305 0.1775 0.073 Uiso 1 1 calc R . . H9B H 0.4118 0.3749 0.1157 0.073 Uiso 1 1 calc R . . C10 C 0.48180(17) 0.3939(8) 0.1284(2) 0.0458(11) Uani 1 1 d . . . C11 C 0.49075(17) 0.5829(8) 0.0917(2) 0.0496(12) Uani 1 1 d . . . H11 H 0.4704 0.7102 0.0828 0.060 Uiso 1 1 calc R . . C12 C 0.52996(17) 0.5844(8) 0.0681(2) 0.0484(12) Uani 1 1 d . . . H12 H 0.5355 0.7160 0.0443 0.058 Uiso 1 1 calc R . . C13 C 0.55181(17) 0.2254(9) 0.1144(2) 0.0543(12) Uani 1 1 d . . . H13 H 0.5727 0.1002 0.1226 0.065 Uiso 1 1 calc R . . C14 C 0.51447(18) 0.2117(9) 0.1406(3) 0.0574(13) Uani 1 1 d . . . H14 H 0.5108 0.0821 0.1664 0.069 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 0.0561(3) 0.0461(2) 0.0626(3) 0.00184(18) 0.0353(2) -0.00206(18) S1 0.0434(7) 0.0453(6) 0.0485(6) -0.0058(5) 0.0227(6) -0.0046(5) S2 0.0502(8) 0.0430(6) 0.0524(7) -0.0086(5) 0.0248(6) -0.0072(5) S3 0.0503(8) 0.0565(7) 0.0641(8) -0.0125(6) 0.0333(7) -0.0125(6) O1 0.072(3) 0.059(2) 0.086(3) 0.004(2) 0.014(2) -0.002(2) O2 0.073(3) 0.075(3) 0.069(2) 0.001(2) 0.020(2) 0.006(2) N1 0.063(3) 0.053(3) 0.078(3) -0.005(2) 0.042(3) -0.001(2) N2 0.049(2) 0.045(2) 0.050(2) 0.0054(18) 0.0257(19) 0.0039(18) N3 0.051(3) 0.047(2) 0.059(2) -0.0120(18) 0.033(2) -0.0112(18) N4 0.046(2) 0.049(2) 0.059(2) -0.0116(19) 0.027(2) -0.0070(18) N5 0.040(2) 0.048(2) 0.060(2) 0.0001(19) 0.021(2) 0.0000(18) C1 0.054(3) 0.044(2) 0.068(3) 0.005(2) 0.026(3) 0.015(2) C2 0.064(4) 0.046(3) 0.065(3) 0.014(2) 0.032(3) 0.011(3) C3 0.043(3) 0.047(2) 0.049(3) 0.003(2) 0.019(2) 0.009(2) C4 0.050(3) 0.043(2) 0.043(2) 0.011(2) 0.016(2) 0.001(2) C5 0.039(3) 0.042(2) 0.044(2) -0.005(2) 0.013(2) -0.004(2) C6 0.049(3) 0.045(2) 0.053(3) -0.009(2) 0.021(2) -0.009(2) C7 0.030(2) 0.040(2) 0.044(2) -0.0006(19) 0.013(2) -0.0003(19) C8 0.034(3) 0.048(2) 0.043(2) -0.001(2) 0.012(2) 0.002(2) C9 0.059(3) 0.057(3) 0.077(4) -0.017(3) 0.039(3) -0.010(3) C10 0.047(3) 0.048(2) 0.050(3) -0.010(2) 0.025(2) -0.007(2) C11 0.045(3) 0.049(3) 0.058(3) -0.003(2) 0.019(2) 0.007(2) C12 0.053(3) 0.048(3) 0.048(3) 0.001(2) 0.021(2) -0.002(2) C13 0.050(3) 0.051(3) 0.068(3) 0.003(3) 0.025(3) 0.006(2) C14 0.062(3) 0.050(3) 0.068(3) 0.006(3) 0.032(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.359(4) . ? Ag1 N5 2.372(4) 8_456 ? Ag1 N1 2.575(5) . ? S1 C7 1.746(4) . ? S1 C6 1.826(5) . ? S2 C7 1.735(4) . ? S2 C8 1.740(4) . ? S3 C8 1.748(5) . ? S3 C9 1.815(5) . ? O1 N1 1.240(6) . ? O2 N1 1.235(6) . ? N2 C2 1.329(6) . ? N2 C3 1.344(5) . ? N3 C7 1.309(5) . ? N3 N4 1.397(5) . ? N4 C8 1.290(5) . ? N5 C13 1.329(6) . ? N5 C12 1.346(6) . ? N5 Ag1 2.372(4) 8 ? C1 C2 1.385(6) . ? C1 C5 1.389(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C4 C5 1.390(6) . ? C4 H4 0.9300 . ? C5 C6 1.500(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C9 C10 1.508(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.376(6) . ? C10 C14 1.397(7) . ? C11 C12 1.383(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.365(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N5 162.46(14) . 8_456 ? N2 Ag1 N1 93.81(12) . . ? N5 Ag1 N1 84.75(13) 8_456 . ? C7 S1 C6 99.8(2) . . ? C7 S2 C8 86.1(2) . . ? C8 S3 C9 98.5(2) . . ? O2 N1 O1 117.6(4) . . ? O2 N1 Ag1 122.6(4) . . ? O1 N1 Ag1 119.4(4) . . ? C2 N2 C3 116.4(4) . . ? C2 N2 Ag1 120.9(3) . . ? C3 N2 Ag1 122.1(3) . . ? C7 N3 N4 111.8(3) . . ? C8 N4 N3 112.2(4) . . ? C13 N5 C12 115.8(4) . . ? C13 N5 Ag1 118.4(3) . 8 ? C12 N5 Ag1 125.6(3) . 8 ? C2 C1 C5 119.1(4) . . ? C2 C1 H1 120.5 . . ? C5 C1 H1 120.5 . . ? N2 C2 C1 124.4(4) . . ? N2 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? N2 C3 C4 123.4(4) . . ? N2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C1 C5 C4 117.1(4) . . ? C1 C5 C6 121.3(4) . . ? C4 C5 C6 121.6(4) . . ? C5 C6 S1 107.7(3) . . ? C5 C6 H6A 110.2 . . ? S1 C6 H6A 110.2 . . ? C5 C6 H6B 110.2 . . ? S1 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? N3 C7 S2 114.7(3) . . ? N3 C7 S1 124.2(3) . . ? S2 C7 S1 121.2(2) . . ? N4 C8 S2 115.1(3) . . ? N4 C8 S3 125.6(3) . . ? S2 C8 S3 119.2(3) . . ? C10 C9 S3 109.3(3) . . ? C10 C9 H9A 109.8 . . ? S3 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? S3 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C14 116.4(4) . . ? C11 C10 C9 122.7(4) . . ? C14 C10 C9 120.8(4) . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? N5 C12 C11 123.2(4) . . ? N5 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N5 C13 C14 124.8(5) . . ? N5 C13 H13 117.6 . . ? C14 C13 H13 117.6 . . ? C13 C14 C10 119.5(5) . . ? C13 C14 H14 120.3 . . ? C10 C14 H14 120.3 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.535 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.093 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 822100' #TrackingRef '- 1a-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 Ag4 N20 O12 S12' _chemical_formula_weight 2009.34 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, 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' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 26.283(6) _cell_length_b 26.418(6) _cell_length_c 10.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7378(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4580 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 20.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.23 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 1.457 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5518 _exptl_absorpt_correction_T_max 0.6836 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19162 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.16 _reflns_number_total 7271 _reflns_number_gt 3519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(6) _refine_ls_number_reflns 7282 _refine_ls_number_parameters 484 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2111 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 0.70449(7) 0.73327(18) 0.0956(6) Uani 1 2 d S . . S1 S 0.73210(13) 0.73699(16) 0.9136(4) 0.0822(10) Uani 1 1 d . . . O1 O 0.5000 0.6275(10) 0.640(3) 0.174(12) Uani 1 2 d SU . . N1 N 0.9192(3) 0.7193(4) 0.7387(13) 0.075(3) Uani 1 1 d . . . C1 C 0.8886(6) 0.6918(6) 0.6602(15) 0.089(4) Uani 1 1 d . . . H1 H 0.9022 0.6693 0.6018 0.107 Uiso 1 1 calc R . . Ag2 Ag 1.0000 0.52096(7) 0.79349(18) 0.0960(6) Uani 1 2 d S . . S2 S 0.72542(17) 0.62622(17) 0.8227(4) 0.0883(11) Uani 1 1 d . . . O2 O 0.5408(7) 0.6559(9) 0.4785(16) 0.184(8) Uani 1 1 d DU . . N2 N 0.9181(3) 0.5168(4) 0.7929(12) 0.073(3) Uani 1 1 d . . . C2 C 0.8345(4) 0.6990(6) 0.6716(13) 0.077(4) Uani 1 1 d . . . H2 H 0.8126 0.6795 0.6231 0.093 Uiso 1 1 calc R . . Ag3 Ag 0.58223(4) 0.62866(3) 0.76203(12) 0.0804(3) Uani 1 1 d . . . S3 S 0.72539(12) 0.51661(14) 0.9204(4) 0.0781(9) Uani 1 1 d . . . O3 O 0.7709(9) 0.6104(9) 0.512(3) 0.262(15) Uani 1 1 d DU . . N3 N 0.7401(5) 0.6552(5) 1.0410(15) 0.094(4) Uani 1 1 d . . . C3 C 0.8154(4) 0.7335(4) 0.7508(13) 0.065(3) Uani 1 1 d . . . S4 S 0.6123(3) 0.8920(2) 0.5505(8) 0.166(3) Uani 1 1 d . . . O4 O 0.7354(8) 0.6335(11) 0.361(2) 0.264(15) Uani 1 1 d DU . . N4 N 0.7399(6) 0.6009(6) 1.0458(14) 0.096(4) Uani 1 1 d . . . C4 C 0.8506(5) 0.7617(5) 0.8260(12) 0.065(3) Uani 1 1 d . . . H4 H 0.8392 0.7870 0.8803 0.078 Uiso 1 1 calc R . . S5 S 0.5000 0.9024(4) 0.6445(11) 0.164(4) Uani 1 2 d S . . O5 O 0.6898(7) 0.6327(7) 0.5114(14) 0.171(8) Uani 1 1 d DU . . N5 N 0.5953(3) 0.5475(3) 0.7626(11) 0.062(2) Uani 1 1 d . . . C5 C 0.8987(5) 0.7512(5) 0.8164(14) 0.074(3) Uani 1 1 d . . . H5 H 0.9206 0.7682 0.8706 0.089 Uiso 1 1 calc R . . S6 S 0.61086(11) 0.35767(12) 0.5932(3) 0.0659(8) Uani 1 1 d . . . O6 O 1.0000 0.6121(10) 0.631(2) 0.196(12) Uani 1 2 d SDU . . N6 N 0.5979(4) 0.7092(4) 0.7463(12) 0.069(3) Uani 1 1 d . . . C6 C 0.7583(4) 0.7456(5) 0.7472(18) 0.091(5) Uani 1 1 d . . . H6A H 0.7410 0.7230 0.6893 0.110 Uiso 1 1 calc R . . H6B H 0.7530 0.7801 0.7191 0.110 Uiso 1 1 calc R . . S7 S 0.5000 0.3603(2) 0.6908(4) 0.0705(13) Uani 1 2 d S . . O7 O 1.0000 0.5528(7) 0.501(2) 0.133(7) Uani 1 2 d SDU . . N7 N 0.5286(10) 0.8693(8) 0.443(2) 0.180(12) Uani 1 1 d . . . C7 C 0.7344(4) 0.6710(5) 0.9326(12) 0.065(3) Uani 1 1 d . . . O8 O 1.0000 0.6284(12) 0.438(3) 0.51(5) Uani 1 2 d SDU . . N8 N 0.5254(3) 0.3645(4) 0.4598(8) 0.053(2) Uani 1 1 d . . . C8 C 0.7349(4) 0.5811(6) 0.9426(12) 0.071(4) Uani 1 1 d . . . N9 N 0.5000 0.6441(8) 0.5344(17) 0.081(5) Uani 1 2 d SDU . . C9 C 0.7562(4) 0.5038(5) 0.7764(13) 0.073(3) Uani 1 1 d . . . H9A H 0.7480 0.4694 0.7511 0.088 Uiso 1 1 calc R . . H9B H 0.7427 0.5264 0.7127 0.088 Uiso 1 1 calc R . . N10 N 0.7323(5) 0.6244(5) 0.4711(12) 0.079(4) Uani 1 1 d DU . . C10 C 0.8137(4) 0.5094(5) 0.7794(13) 0.069(3) Uani 1 1 d . . . N11 N 1.0000 0.5989(6) 0.5249(16) 0.080(4) Uani 1 2 d SDU . . C11 C 0.8419(4) 0.4814(5) 0.8652(14) 0.072(3) Uani 1 1 d . . . H11 H 0.8265 0.4587 0.9202 0.086 Uiso 1 1 calc R . . C12 C 0.8917(5) 0.4885(5) 0.8652(15) 0.075(4) Uani 1 1 d . . . H12 H 0.9099 0.4705 0.9257 0.090 Uiso 1 1 calc R . . C13 C 0.8906(7) 0.5453(7) 0.7164(17) 0.110(6) Uani 1 1 d . . . H13 H 0.9078 0.5694 0.6689 0.132 Uiso 1 1 calc R . . C14 C 0.8411(4) 0.5426(6) 0.7020(19) 0.102(6) Uani 1 1 d . . . H14 H 0.8246 0.5622 0.6418 0.122 Uiso 1 1 calc R . . C15 C 0.5444(4) 0.3621(4) 0.5723(11) 0.052(3) Uani 1 1 d . . . C16 C 0.6196(5) 0.3856(4) 0.7492(13) 0.067(3) Uani 1 1 d . . . H16A H 0.5965 0.3693 0.8077 0.080 Uiso 1 1 calc R . . H16B H 0.6540 0.3789 0.7775 0.080 Uiso 1 1 calc R . . C17 C 0.6102(3) 0.4432(4) 0.7522(11) 0.054(2) Uani 1 1 d . . . C18 C 0.5815(5) 0.4638(5) 0.8361(13) 0.074(3) Uani 1 1 d . . . H18 H 0.5646 0.4430 0.8931 0.088 Uiso 1 1 calc R . . C19 C 0.5747(5) 0.5172(5) 0.8448(15) 0.081(4) Uani 1 1 d . . . H19 H 0.5552 0.5306 0.9099 0.098 Uiso 1 1 calc R . . C20 C 0.6238(5) 0.5272(5) 0.6753(15) 0.082(4) Uani 1 1 d . . . H20 H 0.6400 0.5483 0.6178 0.098 Uiso 1 1 calc R . . C21 C 0.6309(5) 0.4739(4) 0.6651(12) 0.065(3) Uani 1 1 d . . . H21 H 0.6497 0.4604 0.5989 0.078 Uiso 1 1 calc R . . C22 C 0.6271(5) 0.7275(5) 0.6585(12) 0.070(3) Uani 1 1 d . . . H22 H 0.6418 0.7045 0.6033 0.083 Uiso 1 1 calc R . . C23 C 0.6379(5) 0.7770(5) 0.6403(14) 0.076(4) Uani 1 1 d . . . H23 H 0.6595 0.7866 0.5752 0.091 Uiso 1 1 calc R . . C24 C 0.6178(6) 0.8116(5) 0.7151(15) 0.087(4) Uani 1 1 d . . . C25 C 0.5780(9) 0.7935(6) 0.801(2) 0.138(9) Uani 1 1 d . . . H25 H 0.5553 0.8153 0.8408 0.166 Uiso 1 1 calc R . . C26 C 0.5769(7) 0.7417(8) 0.8185(19) 0.112(6) Uani 1 1 d . . . H26 H 0.5594 0.7295 0.8884 0.135 Uiso 1 1 calc R . . C27 C 0.6255(11) 0.8682(5) 0.7110(18) 0.141(9) Uani 1 1 d . . . H27A H 0.6602 0.8763 0.7344 0.169 Uiso 1 1 calc R . . H27B H 0.6028 0.8844 0.7707 0.169 Uiso 1 1 calc R . . C28 C 0.5447(6) 0.8857(5) 0.5387(16) 0.079(4) 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 0.0578(7) 0.1086(13) 0.1204(15) 0.0186(11) 0.000 0.000 S1 0.073(2) 0.090(3) 0.084(2) -0.0065(19) 0.0216(18) 0.0009(17) O1 0.097(13) 0.24(3) 0.18(2) 0.14(2) 0.000 0.000 N1 0.049(5) 0.065(6) 0.112(10) 0.010(7) 0.006(6) -0.009(4) C1 0.091(9) 0.076(10) 0.100(10) -0.023(8) -0.017(9) 0.016(8) Ag2 0.0507(7) 0.1117(13) 0.1257(15) -0.0251(11) 0.000 0.000 S2 0.109(3) 0.097(3) 0.0583(18) -0.0004(18) 0.000(2) 0.011(2) O2 0.176(16) 0.26(2) 0.118(11) 0.024(13) -0.029(11) -0.069(15) N2 0.054(5) 0.066(6) 0.101(9) -0.012(6) -0.013(6) 0.010(5) C2 0.058(6) 0.104(11) 0.070(8) -0.014(8) 0.009(6) 0.007(7) Ag3 0.0862(6) 0.0529(5) 0.1021(8) 0.0067(6) -0.0035(7) 0.0000(4) S3 0.0681(18) 0.077(2) 0.089(2) 0.0079(18) 0.0187(17) 0.0022(16) O3 0.32(3) 0.22(2) 0.24(3) -0.09(2) -0.14(3) 0.12(2) N3 0.092(8) 0.081(9) 0.108(11) 0.003(8) 0.010(8) -0.007(7) C3 0.066(6) 0.064(6) 0.064(7) 0.001(7) -0.011(6) -0.005(5) S4 0.211(7) 0.089(4) 0.199(7) 0.067(4) 0.049(6) 0.025(4) O4 0.140(14) 0.46(5) 0.20(2) -0.03(2) -0.053(16) 0.023(18) N4 0.109(10) 0.091(10) 0.088(10) 0.017(8) -0.015(8) -0.011(8) C4 0.081(8) 0.050(7) 0.064(7) -0.005(5) 0.009(6) -0.018(6) S5 0.220(11) 0.104(7) 0.168(9) -0.015(6) 0.000 0.000 O5 0.188(16) 0.217(19) 0.108(11) 0.009(11) 0.028(11) 0.090(14) N5 0.064(5) 0.050(5) 0.074(6) 0.002(6) 0.009(5) 0.004(4) C5 0.073(8) 0.067(9) 0.082(9) -0.002(7) 0.008(7) -0.017(6) S6 0.0517(14) 0.0646(19) 0.082(2) -0.0130(15) -0.0069(15) 0.0067(13) O6 0.27(4) 0.18(3) 0.14(2) -0.022(18) 0.000 0.000 N6 0.065(5) 0.056(5) 0.084(8) -0.001(6) 0.004(6) 0.016(4) C6 0.060(6) 0.086(9) 0.128(14) -0.030(10) 0.007(8) 0.006(6) S7 0.055(2) 0.097(4) 0.059(3) -0.007(2) 0.000 0.000 O7 0.079(10) 0.135(17) 0.18(2) -0.050(15) 0.000 0.000 N7 0.29(4) 0.095(13) 0.155(17) -0.012(12) 0.012(18) -0.032(13) C7 0.050(6) 0.088(10) 0.058(8) 0.004(7) 0.013(5) 0.008(6) O8 0.64(9) 0.22(5) 0.68(10) 0.02(6) 0.000 0.000 N8 0.051(4) 0.066(6) 0.043(5) -0.011(4) 0.005(4) -0.003(4) C8 0.043(6) 0.118(12) 0.053(7) -0.003(7) 0.012(5) -0.015(6) N9 0.060(9) 0.115(15) 0.069(11) 0.008(10) 0.000 0.000 C9 0.052(5) 0.096(9) 0.071(8) -0.023(7) -0.009(6) 0.013(5) N10 0.095(9) 0.080(8) 0.063(7) -0.020(6) -0.033(7) 0.041(7) C10 0.045(5) 0.080(8) 0.083(9) -0.021(7) 0.004(6) -0.009(5) N11 0.097(12) 0.082(12) 0.061(10) 0.015(9) 0.000 0.000 C11 0.065(7) 0.051(7) 0.099(10) -0.001(7) -0.011(7) 0.006(5) C12 0.061(7) 0.061(8) 0.102(11) -0.017(7) -0.005(7) 0.010(6) C13 0.107(11) 0.120(14) 0.102(12) 0.057(11) 0.033(10) 0.006(10) C14 0.047(6) 0.104(12) 0.154(15) 0.058(11) 0.003(8) 0.008(6) C15 0.049(5) 0.038(6) 0.069(7) -0.001(5) -0.003(5) 0.008(4) C16 0.084(7) 0.050(6) 0.066(7) 0.000(6) -0.012(7) 0.006(5) C17 0.043(4) 0.054(6) 0.066(7) -0.013(6) -0.008(5) 0.001(4) C18 0.083(8) 0.064(8) 0.073(8) -0.018(6) 0.016(7) -0.015(6) C19 0.096(9) 0.061(9) 0.087(10) -0.016(7) 0.014(8) 0.004(7) C20 0.075(8) 0.070(9) 0.100(10) 0.005(8) 0.011(8) -0.013(7) C21 0.077(7) 0.034(6) 0.085(8) -0.003(6) 0.021(7) 0.001(5) C22 0.087(8) 0.057(8) 0.065(7) -0.001(6) 0.024(7) 0.014(6) C23 0.074(8) 0.065(9) 0.089(10) 0.022(7) 0.023(7) 0.018(6) C24 0.114(10) 0.046(7) 0.100(11) 0.019(7) -0.035(9) -0.013(7) C25 0.22(2) 0.052(9) 0.144(17) -0.020(10) 0.072(16) 0.032(12) C26 0.130(14) 0.101(14) 0.106(13) 0.024(10) 0.019(12) -0.007(11) C27 0.28(3) 0.019(6) 0.125(14) 0.008(7) 0.005(16) -0.009(10) C28 0.107(11) 0.044(7) 0.086(10) 0.012(7) -0.002(9) 0.012(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 Ag1 N1 2.161(9) . ? Ag1 N1 2.161(9) 3_755 ? S1 C7 1.756(14) . ? S1 C6 1.911(19) . ? O1 N9 1.20(3) . ? O1 Ag3 2.522(14) . ? O1 Ag3 2.522(14) 3_655 ? N1 C5 1.297(18) . ? N1 C1 1.367(18) . ? C1 C2 1.438(19) . ? C1 H1 0.9300 . ? Ag2 N2 2.157(9) 3_755 ? Ag2 N2 2.157(9) . ? S2 C7 1.679(14) . ? S2 C8 1.763(15) . ? O2 N9 1.265(14) . ? N2 C12 1.277(18) . ? N2 C13 1.323(19) . ? C2 C3 1.338(18) . ? C2 H2 0.9300 . ? Ag3 N5 2.173(9) . ? Ag3 N6 2.174(10) . ? Ag3 N8 2.583(9) 4_565 ? S3 C8 1.737(16) . ? S3 C9 1.764(13) . ? O3 N10 1.166(16) . ? N3 C7 1.233(19) . ? N3 N4 1.437(19) . ? C3 C4 1.432(16) . ? C3 C6 1.535(16) . ? S4 C28 1.788(18) . ? S4 C27 1.85(2) . ? O4 N10 1.200(17) . ? N4 C8 1.222(19) . ? C4 C5 1.300(18) . ? C4 H4 0.9300 . ? S5 C28 1.686(18) 3_655 ? S5 C28 1.686(18) . ? O5 N10 1.214(14) . ? N5 C19 1.302(18) . ? N5 C20 1.307(17) . ? C5 H5 0.9300 . ? S6 C15 1.764(10) . ? S6 C16 1.829(14) . ? O6 N11 1.177(15) . ? N6 C26 1.28(2) . ? N6 C22 1.302(16) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? S7 C15 1.718(12) 3_655 ? S7 C15 1.718(12) . ? O7 N11 1.244(15) . ? N7 C28 1.19(3) . ? N7 N7 1.51(5) 3_655 ? O8 N11 1.207(16) . ? N8 C15 1.297(15) . ? N8 N8 1.338(17) 3_655 ? N8 Ag3 2.583(9) 4_564 ? N9 O2 1.265(14) 3_655 ? C9 C10 1.519(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.389(18) . ? C10 C14 1.40(2) . ? C11 C12 1.322(16) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.31(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.541(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.289(16) . ? C17 C21 1.346(16) . ? C18 C19 1.425(19) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.426(18) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.350(19) . ? C22 H22 0.9300 . ? C23 C24 1.32(2) . ? C23 H23 0.9300 . ? C24 C25 1.47(2) . ? C24 C27 1.507(18) . ? C25 C26 1.38(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? 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 158.9(6) . 3_755 ? C7 S1 C6 102.2(6) . . ? N9 O1 Ag3 118.4(5) . . ? N9 O1 Ag3 118.4(5) . 3_655 ? Ag3 O1 Ag3 117.9(11) . 3_655 ? C5 N1 C1 119.3(11) . . ? C5 N1 Ag1 122.9(10) . . ? C1 N1 Ag1 117.8(10) . . ? N1 C1 C2 117.4(13) . . ? N1 C1 H1 121.3 . . ? C2 C1 H1 121.3 . . ? N2 Ag2 N2 174.1(6) 3_755 . ? C7 S2 C8 87.4(7) . . ? C12 N2 C13 114.1(11) . . ? C12 N2 Ag2 124.7(9) . . ? C13 N2 Ag2 121.2(11) . . ? C3 C2 C1 120.9(13) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? N5 Ag3 N6 159.5(3) . . ? N5 Ag3 O1 97.2(7) . . ? N6 Ag3 O1 97.7(6) . . ? N5 Ag3 N8 99.1(4) . 4_565 ? N6 Ag3 N8 95.9(4) . 4_565 ? O1 Ag3 N8 85.7(6) . 4_565 ? C8 S3 C9 103.9(6) . . ? C7 N3 N4 111.7(14) . . ? C2 C3 C4 117.6(11) . . ? C2 C3 C6 119.6(12) . . ? C4 C3 C6 122.4(12) . . ? C28 S4 C27 102.6(11) . . ? C8 N4 N3 113.4(14) . . ? C5 C4 C3 118.2(12) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C28 S5 C28 88.5(13) 3_655 . ? C19 N5 C20 117.6(12) . . ? C19 N5 Ag3 122.8(9) . . ? C20 N5 Ag3 119.5(9) . . ? N1 C5 C4 126.4(13) . . ? N1 C5 H5 116.8 . . ? C4 C5 H5 116.8 . . ? C15 S6 C16 102.2(6) . . ? C26 N6 C22 115.8(13) . . ? C26 N6 Ag3 122.0(11) . . ? C22 N6 Ag3 122.1(9) . . ? C3 C6 S1 107.7(11) . . ? C3 C6 H6A 110.2 . . ? S1 C6 H6A 110.2 . . ? C3 C6 H6B 110.2 . . ? S1 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C15 S7 C15 85.6(8) 3_655 . ? C28 N7 N7 110.9(16) . 3_655 ? N3 C7 S2 115.4(12) . . ? N3 C7 S1 116.5(11) . . ? S2 C7 S1 127.9(8) . . ? C15 N8 N8 112.6(6) . 3_655 ? C15 N8 Ag3 122.1(7) . 4_564 ? N8 N8 Ag3 125.3(2) 3_655 4_564 ? N4 C8 S3 123.8(12) . . ? N4 C8 S2 111.9(13) . . ? S3 C8 S2 123.0(8) . . ? O1 N9 O2 121.8(11) . 3_655 ? O1 N9 O2 121.8(11) . . ? O2 N9 O2 116(2) 3_655 . ? C10 C9 S3 114.8(9) . . ? C10 C9 H9A 108.6 . . ? S3 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S3 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? O3 N10 O4 112(2) . . ? O3 N10 O5 136(2) . . ? O4 N10 O5 111.7(17) . . ? C11 C10 C14 116.3(10) . . ? C11 C10 C9 119.6(12) . . ? C14 C10 C9 124.1(13) . . ? O6 N11 O8 122.5(19) . . ? O6 N11 O7 119.0(16) . . ? O8 N11 O7 118.5(18) . . ? C12 C11 C10 117.0(13) . . ? C12 C11 H11 121.5 . . ? C10 C11 H11 121.5 . . ? N2 C12 C11 128.3(14) . . ? N2 C12 H12 115.9 . . ? C11 C12 H12 115.9 . . ? C14 C13 N2 125.6(15) . . ? C14 C13 H13 117.2 . . ? N2 C13 H13 117.2 . . ? C13 C14 C10 118.4(14) . . ? C13 C14 H14 120.8 . . ? C10 C14 H14 120.8 . . ? N8 C15 S7 114.6(8) . . ? N8 C15 S6 120.0(9) . . ? S7 C15 S6 125.4(7) . . ? C17 C16 S6 113.4(9) . . ? C17 C16 H16A 108.9 . . ? S6 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? S6 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C21 117.3(12) . . ? C18 C17 C16 121.7(12) . . ? C21 C17 C16 121.0(11) . . ? C17 C18 C19 122.5(13) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? N5 C19 C18 120.8(13) . . ? N5 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? N5 C20 C21 122.2(12) . . ? N5 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C17 C21 C20 119.4(11) . . ? C17 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N6 C22 C23 126.0(12) . . ? N6 C22 H22 117.0 . . ? C23 C22 H22 117.0 . . ? C24 C23 C22 119.9(13) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 115.6(12) . . ? C23 C24 C27 128.0(16) . . ? C25 C24 C27 115.8(16) . . ? C26 C25 C24 114.8(15) . . ? C26 C25 H25 122.6 . . ? C24 C25 H25 122.6 . . ? N6 C26 C25 125.3(17) . . ? N6 C26 H26 117.4 . . ? C25 C26 H26 117.4 . . ? C24 C27 S4 109.8(13) . . ? C24 C27 H27A 109.7 . . ? S4 C27 H27A 109.7 . . ? C24 C27 H27B 109.7 . . ? S4 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N7 C28 S5 114.9(18) . . ? N7 C28 S4 116.6(18) . . ? S5 C28 S4 128.4(11) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.222 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.143