# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Verma, Sandeep' _publ_contact_author_email sverma@iitk.ac.in _publ_section_title ; Probing structural consequences of N9-alkylation in silver-adenine frameworks ; loop_ _publ_author_name A.Mishra R.Prajapati S.Verma data_Complex-5 _database_code_depnum_ccdc_archive 'CCDC 767285' #TrackingRef 'Final-CIF-Merged.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '9-Bzadenine silver complex' _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Ag N11, N O3' _chemical_formula_sum 'C26 H22 Ag N12 O3' _chemical_formula_weight 658.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.072(5) _cell_length_b 19.976(5) _cell_length_c 6.025(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 2777(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2818 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description Cuboid _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type psi_scan _exptl_absorpt_correction_T_min 0.7062 _exptl_absorpt_correction_T_max 0.8473 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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-Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14489 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2818 _reflns_number_gt 2227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45 (Bruker, 2003)' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 3.1d' _computing_publication_material ? _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^)+(0.0700P)^2^+0.7106P] 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 2818 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 0.498552(16) 0.2500 0.59598(6) 0.01913(17) Uani 1 2 d S . . N6 N 0.49705(11) 0.11098(16) 0.8920(5) 0.0153(7) Uani 1 1 d . . . H6A H 0.5097 0.1507 0.9184 0.018 Uiso 1 1 calc R . . H6B H 0.5034 0.0793 0.9855 0.018 Uiso 1 1 calc R . . O1 O 0.52352(16) 0.2500 0.0451(6) 0.0214(8) Uani 1 2 d S . . N1 N 0.45807(12) 0.14921(14) 0.5612(5) 0.0163(6) Uani 1 1 d . . . N9 N 0.40097(12) -0.03666(14) 0.4370(5) 0.0158(6) Uani 1 1 d . . . N3 N 0.40603(12) 0.07857(13) 0.3057(5) 0.0161(6) Uani 1 1 d . . . O2 O 0.60442(11) 0.30438(11) 0.0819(4) 0.0206(6) Uani 1 1 d . . . N7 N 0.44907(12) -0.02641(13) 0.7584(5) 0.0162(6) Uani 1 1 d . . . C8 C 0.42165(15) -0.06769(17) 0.6236(6) 0.0170(7) Uani 1 1 d . . . H8 H 0.4169 -0.1131 0.6522 0.020 Uiso 1 1 calc R . . C2 C 0.42856(15) 0.13583(17) 0.3732(6) 0.0179(7) Uani 1 1 d . . . H2 H 0.4233 0.1719 0.2779 0.021 Uiso 1 1 calc R . . N1C N 0.57841(18) 0.2500 0.0701(6) 0.0171(9) Uani 1 2 d S . . C4 C 0.41662(14) 0.02907(17) 0.4541(6) 0.0151(7) Uani 1 1 d . . . C5 C 0.44603(14) 0.03500(16) 0.6511(6) 0.0145(7) Uani 1 1 d . . . C11 C 0.30627(14) -0.08149(16) 0.3029(6) 0.0169(7) Uani 1 1 d . . . C12 C 0.27912(15) -0.06147(16) 0.4953(6) 0.0202(8) Uani 1 1 d . . . H12 H 0.2998 -0.0381 0.6027 0.024 Uiso 1 1 calc R . . C10 C 0.36931(15) -0.06816(17) 0.2537(6) 0.0178(7) Uani 1 1 d . . . H10A H 0.3880 -0.1102 0.2171 0.021 Uiso 1 1 calc R . . H10B H 0.3719 -0.0394 0.1243 0.021 Uiso 1 1 calc R . . C6 C 0.46794(13) 0.09868(15) 0.7083(6) 0.0141(7) Uani 1 1 d . . . C15 C 0.21609(16) -0.13056(19) 0.1775(7) 0.0286(9) Uani 1 1 d . . . H15 H 0.1951 -0.1533 0.0693 0.034 Uiso 1 1 calc R . . N1S N 0.5987(2) 0.2500 0.5825(7) 0.0239(10) Uani 1 2 d S . . C17 C 0.6454(2) 0.2500 0.5212(9) 0.0216(11) Uani 1 2 d S . . C16 C 0.27439(16) -0.11649(18) 0.1433(6) 0.0227(8) Uani 1 1 d . . . H16 H 0.2924 -0.1305 0.0131 0.027 Uiso 1 1 calc R . . C14 C 0.18920(16) -0.11078(18) 0.3727(6) 0.0247(9) Uani 1 1 d . . . H14 H 0.1504 -0.1208 0.3973 0.030 Uiso 1 1 calc R . . C13 C 0.22053(16) -0.07609(18) 0.5300(7) 0.0242(8) Uani 1 1 d . . . H13 H 0.2025 -0.0623 0.6603 0.029 Uiso 1 1 calc R . . C18 C 0.7052(2) 0.2500 0.4343(9) 0.0240(12) Uani 1 2 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 0.0277(3) 0.0092(2) 0.0205(3) 0.000 -0.00198(16) 0.000 N6 0.0223(16) 0.0094(15) 0.0144(16) 0.0021(11) -0.0035(12) -0.0027(11) O1 0.0183(18) 0.0176(18) 0.028(2) 0.000 -0.0065(16) 0.000 N1 0.0165(14) 0.0134(14) 0.0189(16) 0.0012(12) 0.0001(12) 0.0002(11) N9 0.0156(15) 0.0146(14) 0.0171(16) 0.0000(11) 0.0004(11) -0.0030(12) N3 0.0169(14) 0.0134(13) 0.0180(16) 0.0022(12) 0.0006(12) 0.0010(11) O2 0.0291(14) 0.0106(12) 0.0222(15) 0.0007(10) -0.0029(11) -0.0056(11) N7 0.0160(15) 0.0129(13) 0.0198(16) 0.0025(12) 0.0013(12) -0.0012(11) C8 0.0170(17) 0.0123(17) 0.0216(19) 0.0005(14) 0.0007(14) -0.0008(14) C2 0.0198(17) 0.0172(18) 0.0165(18) 0.0048(14) -0.0036(14) 0.0004(14) N1C 0.026(2) 0.012(2) 0.013(2) 0.000 0.0019(17) 0.000 C4 0.0125(16) 0.0149(17) 0.0180(18) -0.0014(14) 0.0013(14) -0.0017(13) C5 0.0119(16) 0.0152(16) 0.0164(18) 0.0006(14) 0.0018(13) 0.0014(13) C11 0.0179(17) 0.0121(16) 0.0208(19) 0.0019(14) -0.0017(15) 0.0002(13) C12 0.0231(18) 0.0146(17) 0.023(2) -0.0021(15) 0.0001(16) -0.0032(14) C10 0.0217(18) 0.0146(16) 0.0171(19) -0.0052(14) -0.0006(14) -0.0026(14) C6 0.0122(16) 0.0124(16) 0.0178(19) -0.0022(14) 0.0037(14) 0.0008(13) C15 0.0231(19) 0.033(2) 0.029(2) 0.0013(18) -0.0099(17) -0.0075(17) N1S 0.027(3) 0.024(2) 0.021(3) 0.000 0.000(2) 0.000 C17 0.031(3) 0.018(3) 0.016(3) 0.000 -0.005(2) 0.000 C16 0.0255(19) 0.0245(19) 0.0180(19) -0.0008(15) -0.0023(16) -0.0037(16) C14 0.0153(18) 0.024(2) 0.035(2) 0.0055(16) -0.0031(16) -0.0023(16) C13 0.0209(18) 0.0191(18) 0.033(2) -0.0024(17) 0.0052(17) 0.0012(15) C18 0.019(3) 0.019(3) 0.034(3) 0.000 0.003(2) 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 2.229(3) . ? Ag1 N1 2.229(3) 8_565 ? Ag1 N1S 2.312(5) . ? N6 C6 1.318(4) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O1 N1C 1.275(5) . ? N1 C2 1.348(4) . ? N1 C6 1.363(4) . ? N9 C4 1.366(5) . ? N9 C8 1.369(4) . ? N9 C10 1.466(4) . ? N3 C2 1.321(4) . ? N3 C4 1.355(4) . ? O2 N1C 1.243(3) . ? N7 C8 1.319(4) . ? N7 C5 1.389(4) . ? C8 H8 0.9300 . ? C2 H2 0.9300 . ? N1C O2 1.243(3) 8_565 ? C4 C5 1.372(5) . ? C5 C6 1.411(4) . ? C11 C12 1.377(5) . ? C11 C16 1.398(5) . ? C11 C10 1.508(5) . ? C12 C13 1.399(5) . ? C12 H12 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C15 C14 1.387(6) . ? C15 C16 1.390(5) . ? C15 H15 0.9300 . ? N1S C17 1.140(7) . ? C17 C18 1.475(7) . ? C16 H16 0.9300 . ? C14 C13 1.379(5) . ? C14 H14 0.9300 . ? C13 H13 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 N1 Ag1 N1 129.15(14) . 8_565 ? N1 Ag1 N1S 114.54(7) . . ? N1 Ag1 N1S 114.54(7) 8_565 . ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C2 N1 C6 118.9(3) . . ? C2 N1 Ag1 118.0(2) . . ? C6 N1 Ag1 122.5(2) . . ? C4 N9 C8 106.3(3) . . ? C4 N9 C10 127.0(3) . . ? C8 N9 C10 126.7(3) . . ? C2 N3 C4 111.0(3) . . ? C8 N7 C5 104.0(3) . . ? N7 C8 N9 112.9(3) . . ? N7 C8 H8 123.5 . . ? N9 C8 H8 123.5 . . ? N3 C2 N1 129.0(3) . . ? N3 C2 H2 115.5 . . ? N1 C2 H2 115.5 . . ? O2 N1C O2 121.8(4) 8_565 . ? O2 N1C O1 119.1(2) 8_565 . ? O2 N1C O1 119.1(2) . . ? N3 C4 N9 127.2(3) . . ? N3 C4 C5 126.6(3) . . ? N9 C4 C5 106.2(3) . . ? C4 C5 N7 110.6(3) . . ? C4 C5 C6 117.8(3) . . ? N7 C5 C6 131.6(3) . . ? C12 C11 C16 119.0(3) . . ? C12 C11 C10 123.6(3) . . ? C16 C11 C10 117.4(3) . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N9 C10 C11 114.1(3) . . ? N9 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N9 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N6 C6 N1 119.6(3) . . ? N6 C6 C5 123.8(3) . . ? N1 C6 C5 116.7(3) . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 N1S Ag1 163.1(4) . . ? N1S C17 C18 178.1(6) . . ? C15 C16 C11 120.6(3) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C2 53.4(3) 8_565 . . . ? N1S Ag1 N1 C2 -110.4(3) . . . . ? N1 Ag1 N1 C6 -134.8(2) 8_565 . . . ? N1S Ag1 N1 C6 61.4(3) . . . . ? C5 N7 C8 N9 -0.3(4) . . . . ? C4 N9 C8 N7 0.3(4) . . . . ? C10 N9 C8 N7 179.2(3) . . . . ? C4 N3 C2 N1 -0.9(5) . . . . ? C6 N1 C2 N3 0.6(5) . . . . ? Ag1 N1 C2 N3 172.7(3) . . . . ? C2 N3 C4 N9 -178.5(3) . . . . ? C2 N3 C4 C5 0.6(5) . . . . ? C8 N9 C4 N3 179.1(3) . . . . ? C10 N9 C4 N3 0.2(5) . . . . ? C8 N9 C4 C5 -0.2(4) . . . . ? C10 N9 C4 C5 -179.1(3) . . . . ? N3 C4 C5 N7 -179.3(3) . . . . ? N9 C4 C5 N7 0.0(4) . . . . ? N3 C4 C5 C6 -0.1(5) . . . . ? N9 C4 C5 C6 179.2(3) . . . . ? C8 N7 C5 C4 0.2(4) . . . . ? C8 N7 C5 C6 -178.8(3) . . . . ? C16 C11 C12 C13 0.1(5) . . . . ? C10 C11 C12 C13 -179.5(3) . . . . ? C4 N9 C10 C11 -103.0(4) . . . . ? C8 N9 C10 C11 78.2(4) . . . . ? C12 C11 C10 N9 4.8(5) . . . . ? C16 C11 C10 N9 -174.8(3) . . . . ? C2 N1 C6 N6 179.6(3) . . . . ? Ag1 N1 C6 N6 7.9(4) . . . . ? C2 N1 C6 C5 0.0(4) . . . . ? Ag1 N1 C6 C5 -171.7(2) . . . . ? C4 C5 C6 N6 -179.8(3) . . . . ? N7 C5 C6 N6 -0.8(6) . . . . ? C4 C5 C6 N1 -0.2(4) . . . . ? N7 C5 C6 N1 178.7(3) . . . . ? N1 Ag1 N1S C17 83.13(9) . . . . ? N1 Ag1 N1S C17 -83.13(9) 8_565 . . . ? Ag1 N1S C17 C18 0.00(2) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? C12 C11 C16 C15 0.4(5) . . . . ? C10 C11 C16 C15 180.0(3) . . . . ? C16 C15 C14 C13 1.2(6) . . . . ? C15 C14 C13 C12 -0.8(6) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.131 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.184 data_Complex-3 _database_code_depnum_ccdc_archive 'CCDC 772587' #TrackingRef 'Final-CIF-Merged.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H34 Ag2 N12 O8' _chemical_formula_sum 'C22 H34 Ag2 N12 O8' _chemical_formula_weight 810.35 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 Monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 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 18.577(6) _cell_length_b 7.346(5) _cell_length_c 25.747(5) _cell_angle_alpha 90.000(8) _cell_angle_beta 103.013(5) _cell_angle_gamma 90.000(4) _cell_volume 3423(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8127 _exptl_absorpt_correction_T_max 0.8892 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21050 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8180 _reflns_number_gt 4028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1590P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8180 _refine_ls_number_parameters 413 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2827 _refine_ls_wR_factor_gt 0.2251 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.00567(4) 0.80249(9) 0.53317(3) 0.0531(3) Uani 1 1 d . . . Ag2 Ag 0.00701(4) 1.07197(10) 0.78642(3) 0.0552(3) Uani 1 1 d . . . N1' N -0.0244(4) 0.6105(11) 0.3919(3) 0.0478(18) Uani 1 1 d D . . N9' N -0.0726(5) 1.1211(10) 0.7140(3) 0.0498(19) Uani 1 1 d . . . C15' C 0.0913(5) 0.5575(12) 0.4558(3) 0.045(2) Uani 1 1 d . . . C1' C -0.0304(5) 0.9777(11) 0.6345(3) 0.0380(18) Uani 1 1 d . . . N6' N 0.0356(5) 0.9235(11) 0.6586(4) 0.052(2) Uani 1 1 d D . . N7' N -0.0583(4) 0.9441(10) 0.5818(3) 0.0499(19) Uani 1 1 d . . . N2' N 0.0724(5) 0.4728(10) 0.3664(3) 0.052(2) Uani 1 1 d . . . N4' N 0.0805(4) 0.6313(12) 0.5046(3) 0.054(2) Uani 1 1 d . . . N3' N 0.1888(4) 0.4078(10) 0.4253(3) 0.0508(19) Uani 1 1 d . . . C4' C -0.0790(5) 1.0700(11) 0.6606(3) 0.044(2) Uani 1 1 d . . . N10' N -0.1836(4) 1.1968(10) 0.6666(3) 0.0498(19) Uani 1 1 d . . . N8' N -0.1761(5) 1.0873(10) 0.5787(3) 0.052(2) Uani 1 1 d . . . C3' C -0.1505(6) 1.1154(12) 0.6313(4) 0.051(2) Uani 1 1 d . . . N5' N 0.1932(5) 0.5115(13) 0.5140(3) 0.065(2) Uani 1 1 d . . . C12' C 0.0428(5) 0.5518(11) 0.4037(3) 0.046(2) Uani 1 1 d . . . C17' C 0.2695(6) 0.4539(17) 0.5418(4) 0.073(3) Uani 1 1 d . . . H17A H 0.2665 0.3776 0.5719 0.088 Uiso 1 1 calc R . . H17B H 0.2909 0.3819 0.5175 0.088 Uiso 1 1 calc R . . C5' C -0.1375(6) 1.1970(13) 0.7135(4) 0.053(2) Uani 1 1 d . . . H5' H -0.1494 1.2462 0.7438 0.064 Uiso 1 1 calc R . . C6' C -0.2604(5) 1.2668(14) 0.6552(4) 0.060(3) Uani 1 1 d . . . H6'1 H -0.2741 1.3072 0.6184 0.072 Uiso 1 1 calc R . . H6'2 H -0.2629 1.3710 0.6778 0.072 Uiso 1 1 calc R . . C16' C 0.1443(6) 0.5976(16) 0.5367(4) 0.062(3) Uani 1 1 d . . . H16' H 0.1551 0.6307 0.5725 0.075 Uiso 1 1 calc R . . C18' C 0.3186(7) 0.612(2) 0.5608(8) 0.130(7) Uani 1 1 d . . . H18A H 0.2993 0.6695 0.5887 0.156 Uiso 1 1 calc R . . H18B H 0.3663 0.5614 0.5779 0.156 Uiso 1 1 calc R . . C7' C -0.3143(6) 1.1256(17) 0.6643(5) 0.072(3) Uani 1 1 d . . . H7'1 H -0.3622 1.1824 0.6609 0.086 Uiso 1 1 calc R . . H7'2 H -0.2986 1.0806 0.7005 0.086 Uiso 1 1 calc R . . C10' C -0.3850(9) 0.673(2) 0.5932(10) 0.159(9) Uani 1 1 d . . . H10A H -0.4037 0.7277 0.5585 0.191 Uiso 1 1 calc R . . H10B H -0.3374 0.6186 0.5932 0.191 Uiso 1 1 calc R . . C14' C 0.1603(5) 0.4869(13) 0.4619(4) 0.048(2) Uani 1 1 d . . . C2' C -0.1276(5) 0.9994(14) 0.5575(4) 0.055(2) Uani 1 1 d . . . H2' H -0.1427 0.9717 0.5215 0.066 Uiso 1 1 calc R . . C13' C 0.1429(6) 0.4092(12) 0.3782(4) 0.056(3) Uani 1 1 d . . . H13' H 0.1606 0.3616 0.3499 0.068 Uiso 1 1 calc R . . C11' C -0.4384(9) 0.525(3) 0.6028(14) 0.249(18) Uani 1 1 d . . . H11A H -0.4439 0.4350 0.5751 0.374 Uiso 1 1 calc R . . H11B H -0.4856 0.5785 0.6025 0.374 Uiso 1 1 calc R . . H11C H -0.4193 0.4685 0.6367 0.374 Uiso 1 1 calc R . . C20' C 0.3902(14) 0.887(4) 0.5428(12) 0.212(13) Uani 1 1 d D . . H20A H 0.4340 0.8293 0.5642 0.254 Uiso 1 1 calc R . . H20B H 0.4026 0.9286 0.5101 0.254 Uiso 1 1 calc R . . C8' C -0.3222(7) 0.9648(16) 0.6261(6) 0.085(4) Uani 1 1 d . . . H8'1 H -0.3392 1.0090 0.5899 0.102 Uiso 1 1 calc R . . H8'2 H -0.2741 0.9093 0.6289 0.102 Uiso 1 1 calc R . . C9' C -0.3757(7) 0.8211(18) 0.6369(8) 0.122(6) Uani 1 1 d . . . H9'1 H -0.4231 0.8764 0.6367 0.147 Uiso 1 1 calc R . . H9'2 H -0.3569 0.7668 0.6716 0.147 Uiso 1 1 calc R . . OW1 O 0.1670(5) 0.6617(13) 0.6648(3) 0.089(3) Uani 1 1 d . . . N1 N 0.1537(5) 0.2398(12) 0.7414(3) 0.055(2) Uani 1 1 d . . . N2 N -0.1531(5) 0.8861(12) 0.4173(3) 0.055(2) Uani 1 1 d . . . O4 O -0.1815(5) 0.8031(14) 0.3783(4) 0.108(3) Uani 1 1 d . . . O1 O 0.1424(9) 0.0846(13) 0.7539(4) 0.147(5) Uani 1 1 d . . . O5 O -0.1006(6) 0.840(2) 0.4493(4) 0.148(6) Uani 1 1 d . . . O2 O 0.1046(9) 0.300(2) 0.7133(5) 0.225(10) Uani 1 1 d . . . O3 O 0.2052(6) 0.3135(19) 0.7638(9) 0.221(10) Uani 1 1 d . . . O6 O -0.1752(13) 1.022(2) 0.4249(5) 0.290(15) Uani 1 1 d . . . C19' C 0.3315(9) 0.745(3) 0.5285(10) 0.169(10) Uani 1 1 d . . . H19A H 0.2853 0.8111 0.5176 0.203 Uiso 1 1 calc R . . H19B H 0.3399 0.6855 0.4968 0.203 Uiso 1 1 calc R . . C21' C 0.373(3) 1.045(5) 0.572(2) 0.46(5) Uani 1 1 d D . . H21A H 0.3645 1.0096 0.6061 0.555 Uiso 1 1 calc R . . H21B H 0.3290 1.1058 0.5516 0.555 Uiso 1 1 calc R . . C22' C 0.4400(15) 1.170(3) 0.5784(17) 0.34(3) Uani 1 1 d . . . H22A H 0.4241 1.2942 0.5753 0.509 Uiso 1 1 calc R . . H22B H 0.4664 1.1429 0.5512 0.509 Uiso 1 1 calc R . . H22C H 0.4719 1.1501 0.6128 0.509 Uiso 1 1 calc R . . OW2 O 0.282(2) 0.914(5) 0.7034(11) 0.44(2) Uani 1 1 d . . . H1N H -0.047(4) 0.620(12) 0.3574(12) 0.04(2) Uiso 1 1 d D . . H2N H -0.040(5) 0.670(10) 0.418(2) 0.05(3) Uiso 1 1 d D . . H1N' H 0.062(4) 0.898(11) 0.638(3) 0.02(2) Uiso 1 1 d . . . H2N' H 0.047(6) 0.977(15) 0.691(2) 0.09(4) Uiso 1 1 d 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 0.0736(5) 0.0407(4) 0.0415(4) -0.0007(3) 0.0017(3) -0.0093(3) Ag2 0.0797(6) 0.0428(4) 0.0383(4) 0.0003(3) 0.0032(3) 0.0011(4) N1' 0.048(5) 0.059(5) 0.033(4) 0.005(4) 0.001(4) -0.001(4) N9' 0.067(5) 0.039(4) 0.039(4) 0.001(3) 0.003(4) -0.005(4) C15' 0.060(6) 0.043(5) 0.030(4) 0.004(4) 0.003(4) -0.012(4) C1' 0.048(5) 0.039(4) 0.025(4) 0.006(3) 0.004(4) -0.009(4) N6' 0.071(6) 0.040(5) 0.049(5) -0.002(4) 0.018(5) -0.007(4) N7' 0.060(5) 0.038(4) 0.053(5) -0.002(3) 0.015(4) -0.011(4) N2' 0.069(5) 0.042(4) 0.038(4) 0.007(3) -0.002(4) -0.009(4) N4' 0.060(5) 0.063(5) 0.036(4) 0.001(4) 0.004(4) -0.002(4) N3' 0.059(5) 0.033(4) 0.057(5) 0.005(3) 0.008(4) -0.001(3) C4' 0.056(5) 0.033(4) 0.040(5) 0.005(4) 0.005(4) -0.011(4) N10' 0.059(5) 0.039(4) 0.048(5) 0.002(3) 0.005(4) 0.001(4) N8' 0.072(5) 0.040(4) 0.043(4) 0.007(3) 0.008(4) -0.004(4) C3' 0.076(7) 0.029(4) 0.046(5) 0.006(4) 0.012(5) -0.006(4) N5' 0.068(6) 0.072(6) 0.051(5) -0.001(5) 0.003(4) 0.001(5) C12' 0.065(6) 0.033(5) 0.035(5) -0.002(4) 0.003(4) -0.014(4) C17' 0.064(7) 0.083(8) 0.061(7) -0.003(6) -0.008(5) 0.011(6) C5' 0.069(6) 0.053(6) 0.040(5) 0.005(4) 0.015(5) -0.002(5) C6' 0.072(7) 0.042(5) 0.061(6) 0.012(5) 0.006(5) 0.004(5) C16' 0.071(7) 0.075(8) 0.037(5) -0.003(5) 0.006(5) -0.002(6) C18' 0.063(8) 0.101(12) 0.203(19) 0.062(13) -0.020(10) -0.009(8) C7' 0.072(7) 0.070(7) 0.073(7) 0.029(6) 0.013(6) 0.006(6) C10' 0.090(11) 0.068(11) 0.30(3) 0.006(14) 0.006(14) -0.007(8) C14' 0.057(6) 0.038(5) 0.046(5) 0.007(4) 0.003(5) -0.005(4) C2' 0.056(6) 0.055(6) 0.047(6) 0.001(5) -0.001(5) -0.006(5) C13' 0.088(8) 0.032(5) 0.046(6) 0.003(4) 0.009(5) -0.013(5) C11' 0.087(12) 0.078(12) 0.56(5) 0.04(2) 0.02(2) -0.017(10) C20' 0.143(18) 0.17(2) 0.27(3) 0.08(2) -0.08(2) -0.091(19) C8' 0.071(8) 0.057(7) 0.124(11) 0.017(7) 0.015(7) -0.001(6) C9' 0.071(8) 0.055(8) 0.23(2) 0.031(10) 0.017(10) -0.002(7) OW1 0.090(6) 0.109(7) 0.065(5) 0.005(5) 0.012(4) 0.005(5) N1 0.067(6) 0.047(5) 0.048(5) 0.004(4) 0.007(4) -0.001(4) N2 0.071(6) 0.050(5) 0.038(4) -0.011(4) 0.008(4) -0.004(4) O4 0.122(8) 0.107(8) 0.079(6) -0.028(6) -0.012(5) -0.024(6) O1 0.323(18) 0.058(6) 0.058(5) -0.001(4) 0.040(8) -0.040(8) O5 0.117(8) 0.251(16) 0.055(5) -0.050(7) -0.007(6) 0.081(9) O2 0.288(17) 0.209(16) 0.111(9) -0.097(10) -0.100(11) 0.191(15) O3 0.077(7) 0.139(13) 0.44(3) -0.156(16) 0.045(11) -0.031(7) O6 0.54(3) 0.129(11) 0.103(9) -0.056(8) -0.138(14) 0.193(17) C19' 0.103(13) 0.097(12) 0.27(3) 0.056(16) -0.043(15) -0.010(11) C21' 0.36(6) 0.17(4) 0.76(14) 0.09(6) -0.07(8) -0.002(4) C22' 0.19(2) 0.085(17) 0.62(7) -0.03(3) -0.17(3) 0.009(15) OW2 0.68(6) 0.43(4) 0.28(3) 0.14(3) 0.28(3) 0.31(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4' 2.125(8) . ? Ag1 N7' 2.176(8) . ? Ag1 O5 2.592(9) . ? Ag1 Ag1 3.350(2) 3_576 ? Ag2 N9' 2.135(7) . ? Ag2 N2' 2.167(7) 4_576 ? N1' C12' 1.291(12) . ? N9' C5' 1.326(12) . ? N9' C4' 1.404(11) . ? C15' C14' 1.358(13) . ? C15' N4' 1.424(12) . ? C15' C12' 1.438(11) . ? C1' N6' 1.306(12) . ? C1' N7' 1.360(10) . ? C1' C4' 1.412(12) . ? N7' C2' 1.361(12) . ? N2' C12' 1.342(12) . ? N2' C13' 1.359(13) . ? N2' Ag2 2.167(7) 4_575 ? N4' C16' 1.307(12) . ? N3' C14' 1.315(12) . ? N3' C13' 1.317(12) . ? C4' C3' 1.412(13) . ? N10' C5' 1.314(12) . ? N10' C3' 1.347(12) . ? N10' C6' 1.482(12) . ? N8' C2' 1.322(13) . ? N8' C3' 1.347(12) . ? N5' C16' 1.344(13) . ? N5' C14' 1.355(12) . ? N5' C17' 1.498(13) . ? C17' C18' 1.487(19) . ? C6' C7' 1.497(14) . ? C18' C19' 1.34(2) . ? C7' C8' 1.523(17) . ? C10' C11' 1.53(2) . ? C10' C9' 1.55(3) . ? C20' C21' 1.46(2) . ? C20' C19' 1.49(3) . ? C8' C9' 1.517(17) . ? N1 O2 1.119(12) . ? N1 O3 1.137(13) . ? N1 O1 1.216(12) . ? N2 O6 1.113(13) . ? N2 O5 1.176(11) . ? N2 O4 1.193(10) . ? C21' C22' 1.52(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4' Ag1 N7' 165.2(3) . . ? N4' Ag1 O5 102.1(3) . . ? N7' Ag1 O5 91.0(3) . . ? N4' Ag1 Ag1 107.9(2) . 3_576 ? N7' Ag1 Ag1 84.2(2) . 3_576 ? O5 Ag1 Ag1 62.3(4) . 3_576 ? N9' Ag2 N2' 170.4(3) . 4_576 ? C5' N9' C4' 103.2(8) . . ? C5' N9' Ag2 121.9(6) . . ? C4' N9' Ag2 134.4(7) . . ? C14' C15' N4' 111.1(8) . . ? C14' C15' C12' 118.3(8) . . ? N4' C15' C12' 130.6(9) . . ? N6' C1' N7' 121.6(8) . . ? N6' C1' C4' 123.5(8) . . ? N7' C1' C4' 114.9(7) . . ? C1' N7' C2' 120.8(8) . . ? C1' N7' Ag1 121.8(6) . . ? C2' N7' Ag1 117.4(6) . . ? C12' N2' C13' 121.3(8) . . ? C12' N2' Ag2 120.9(6) . 4_575 ? C13' N2' Ag2 117.8(7) . 4_575 ? C16' N4' C15' 101.4(8) . . ? C16' N4' Ag1 117.6(7) . . ? C15' N4' Ag1 139.8(6) . . ? C14' N3' C13' 112.0(9) . . ? N9' C4' C3' 108.7(8) . . ? N9' C4' C1' 132.2(8) . . ? C3' C4' C1' 119.0(8) . . ? C5' N10' C3' 108.6(8) . . ? C5' N10' C6' 125.5(8) . . ? C3' N10' C6' 125.9(8) . . ? C2' N8' C3' 111.7(8) . . ? N8' C3' N10' 129.4(9) . . ? N8' C3' C4' 125.3(9) . . ? N10' C3' C4' 105.2(8) . . ? C16' N5' C14' 107.2(9) . . ? C16' N5' C17' 125.7(9) . . ? C14' N5' C17' 127.0(9) . . ? N1' C12' N2' 120.5(8) . . ? N1' C12' C15' 125.4(9) . . ? N2' C12' C15' 114.1(9) . . ? C18' C17' N5' 112.4(10) . . ? N10' C5' N9' 114.3(8) . . ? N10' C6' C7' 112.1(8) . . ? N4' C16' N5' 114.8(9) . . ? C19' C18' C17' 123.2(18) . . ? C6' C7' C8' 114.0(10) . . ? C11' C10' C9' 111(2) . . ? N3' C14' N5' 127.1(9) . . ? N3' C14' C15' 127.4(9) . . ? N5' C14' C15' 105.4(9) . . ? N8' C2' N7' 128.2(9) . . ? N3' C13' N2' 126.9(10) . . ? C21' C20' C19' 117(3) . . ? C9' C8' C7' 113.2(12) . . ? C8' C9' C10' 109.2(15) . . ? O2 N1 O3 127.6(15) . . ? O2 N1 O1 112.1(15) . . ? O3 N1 O1 119.2(14) . . ? O6 N2 O5 114.8(12) . . ? O6 N2 O4 119.7(12) . . ? O5 N2 O4 125.6(11) . . ? N2 O5 Ag1 165.8(9) . . ? C18' C19' C20' 125(2) . . ? C20' C21' C22' 106(3) . . ? 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 N2' Ag2 N9' C5' 18(2) 4_576 . . . ? N2' Ag2 N9' C4' -152.0(15) 4_576 . . . ? N6' C1' N7' C2' 179.1(8) . . . . ? C4' C1' N7' C2' 0.7(11) . . . . ? N6' C1' N7' Ag1 -1.3(11) . . . . ? C4' C1' N7' Ag1 -179.7(5) . . . . ? N4' Ag1 N7' C1' 29.8(15) . . . . ? O5 Ag1 N7' C1' -178.0(7) . . . . ? Ag1 Ag1 N7' C1' -115.9(6) 3_576 . . . ? N4' Ag1 N7' C2' -150.5(11) . . . . ? O5 Ag1 N7' C2' 1.7(7) . . . . ? Ag1 Ag1 N7' C2' 63.7(6) 3_576 . . . ? C14' C15' N4' C16' -0.5(10) . . . . ? C12' C15' N4' C16' -178.9(9) . . . . ? C14' C15' N4' Ag1 166.2(8) . . . . ? C12' C15' N4' Ag1 -12.2(16) . . . . ? N7' Ag1 N4' C16' -34.0(16) . . . . ? O5 Ag1 N4' C16' 174.5(8) . . . . ? Ag1 Ag1 N4' C16' 110.0(8) 3_576 . . . ? N7' Ag1 N4' C15' 160.7(9) . . . . ? O5 Ag1 N4' C15' 9.3(10) . . . . ? Ag1 Ag1 N4' C15' -55.3(10) 3_576 . . . ? C5' N9' C4' C3' -1.9(9) . . . . ? Ag2 N9' C4' C3' 169.6(6) . . . . ? C5' N9' C4' C1' -177.7(9) . . . . ? Ag2 N9' C4' C1' -6.2(14) . . . . ? N6' C1' C4' N9' -1.8(15) . . . . ? N7' C1' C4' N9' 176.6(8) . . . . ? N6' C1' C4' C3' -177.2(8) . . . . ? N7' C1' C4' C3' 1.2(11) . . . . ? C2' N8' C3' N10' -178.9(9) . . . . ? C2' N8' C3' C4' 4.3(13) . . . . ? C5' N10' C3' N8' -178.9(9) . . . . ? C6' N10' C3' N8' 3.8(15) . . . . ? C5' N10' C3' C4' -1.5(10) . . . . ? C6' N10' C3' C4' -178.9(8) . . . . ? N9' C4' C3' N8' 179.6(8) . . . . ? C1' C4' C3' N8' -4.0(13) . . . . ? N9' C4' C3' N10' 2.1(9) . . . . ? C1' C4' C3' N10' 178.6(7) . . . . ? C13' N2' C12' N1' -179.6(8) . . . . ? Ag2 N2' C12' N1' -3.3(11) 4_575 . . . ? C13' N2' C12' C15' -1.4(12) . . . . ? Ag2 N2' C12' C15' 174.9(5) 4_575 . . . ? C14' C15' C12' N1' 178.8(9) . . . . ? N4' C15' C12' N1' -2.9(15) . . . . ? C14' C15' C12' N2' 0.7(11) . . . . ? N4' C15' C12' N2' 179.0(9) . . . . ? C16' N5' C17' C18' -65.7(17) . . . . ? C14' N5' C17' C18' 114.6(14) . . . . ? C3' N10' C5' N9' 0.4(11) . . . . ? C6' N10' C5' N9' 177.7(8) . . . . ? C4' N9' C5' N10' 0.9(10) . . . . ? Ag2 N9' C5' N10' -171.9(6) . . . . ? C5' N10' C6' C7' -86.8(12) . . . . ? C3' N10' C6' C7' 90.1(11) . . . . ? C15' N4' C16' N5' -0.3(12) . . . . ? Ag1 N4' C16' N5' -170.6(7) . . . . ? C14' N5' C16' N4' 0.9(13) . . . . ? C17' N5' C16' N4' -178.8(10) . . . . ? N5' C17' C18' C19' -56(2) . . . . ? N10' C6' C7' C8' -66.0(12) . . . . ? C13' N3' C14' N5' -178.7(9) . . . . ? C13' N3' C14' C15' 2.8(13) . . . . ? C16' N5' C14' N3' -179.9(9) . . . . ? C17' N5' C14' N3' -0.1(17) . . . . ? C16' N5' C14' C15' -1.2(11) . . . . ? C17' N5' C14' C15' 178.6(10) . . . . ? N4' C15' C14' N3' 179.8(9) . . . . ? C12' C15' C14' N3' -1.6(14) . . . . ? N4' C15' C14' N5' 1.0(10) . . . . ? C12' C15' C14' N5' 179.6(8) . . . . ? C3' N8' C2' N7' -2.2(14) . . . . ? C1' N7' C2' N8' -0.1(15) . . . . ? Ag1 N7' C2' N8' -179.8(8) . . . . ? C14' N3' C13' N2' -3.6(13) . . . . ? C12' N2' C13' N3' 3.1(14) . . . . ? Ag2 N2' C13' N3' -173.3(7) 4_575 . . . ? C6' C7' C8' C9' 178.6(10) . . . . ? C7' C8' C9' C10' 175.1(11) . . . . ? C11' C10' C9' C8' 179.8(13) . . . . ? O6 N2 O5 Ag1 14(6) . . . . ? O4 N2 O5 Ag1 -168(4) . . . . ? N4' Ag1 O5 N2 -165(5) . . . . ? N7' Ag1 O5 N2 22(5) . . . . ? Ag1 Ag1 O5 N2 -61(5) 3_576 . . . ? C17' C18' C19' C20' -168(2) . . . . ? C21' C20' C19' C18' -83(4) . . . . ? C19' C20' C21' C22' -177(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.319 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.205 data_Complex-4 _database_code_depnum_ccdc_archive 'CCDC 772589' #TrackingRef 'Final-CIF-Merged.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H50 Ag2 N12 O8' _chemical_formula_sum 'C30 H50 Ag2 N12 O8' _chemical_formula_weight 922.56 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 Monoclinic _symmetry_space_group_name_H-M P21/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 20.600(3) _cell_length_b 7.1530(11) _cell_length_c 25.954(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.326(2) _cell_angle_gamma 90.00 _cell_volume 3817.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8117 _exptl_absorpt_correction_T_max 0.8989 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23423 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9349 _reflns_number_gt 5802 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0472P)^2^+24.9886P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9349 _refine_ls_number_parameters 472 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _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 Ag2 Ag 0.00411(3) 0.78567(7) 0.965124(18) 0.03325(15) Uani 1 1 d . . . Ag1 Ag -0.00266(3) 1.03925(8) 0.713435(19) 0.03663(16) Uani 1 1 d . . . N6' N -0.0237(3) 0.6288(8) 1.09930(19) 0.0334(13) Uani 1 1 d . . . H6'1 H -0.0486 0.6205 1.1246 0.040 Uiso 1 1 calc R . . H6'2 H -0.0387 0.6713 1.0700 0.040 Uiso 1 1 calc R . . N1 N -0.0594(3) 0.9103(7) 0.9037(2) 0.0303(12) Uani 1 1 d . . . N3' N 0.1688(3) 0.4551(8) 1.1233(2) 0.0342(13) Uani 1 1 d . . . N7' N 0.0760(3) 0.6352(8) 1.0138(2) 0.0329(13) Uani 1 1 d . . . N7 N -0.0743(3) 1.0861(8) 0.7685(2) 0.0333(13) Uani 1 1 d . . . N9 N -0.1735(3) 1.1594(8) 0.7929(2) 0.0334(13) Uani 1 1 d . . . N9' N 0.1762(3) 0.5326(9) 1.0330(2) 0.0370(13) Uani 1 1 d . . . N3 N -0.1649(3) 1.0427(8) 0.8812(2) 0.0326(13) Uani 1 1 d . . . C5' C 0.0810(3) 0.5805(9) 1.0651(2) 0.0288(14) Uani 1 1 d . . . N1' N 0.0609(3) 0.5097(7) 1.1517(2) 0.0298(12) Uani 1 1 d . . . N6 N 0.0247(3) 0.9027(8) 0.8476(2) 0.0342(13) Uani 1 1 d . . . H6A H 0.0489 0.8482 0.8711 0.041 Uiso 1 1 calc R . . H6B H 0.0398 0.9270 0.8181 0.041 Uiso 1 1 calc R . . C12 C -0.2975(4) 0.9201(10) 0.8049(3) 0.0417(18) Uani 1 1 d . . . H12A H -0.3095 0.9681 0.8380 0.050 Uiso 1 1 calc R . . H12B H -0.2563 0.8552 0.8103 0.050 Uiso 1 1 calc R . . C6 C -0.0357(3) 0.9493(8) 0.8567(2) 0.0302(14) Uani 1 1 d . . . C2 C -0.1216(3) 0.9578(10) 0.9129(3) 0.0334(15) Uani 1 1 d . . . H2 H -0.1354 0.9270 0.9453 0.040 Uiso 1 1 calc R . . C4' C 0.1437(3) 0.5186(9) 1.0779(2) 0.0300(14) Uani 1 1 d . . . C10 C -0.2403(4) 1.2308(10) 0.7890(3) 0.0404(17) Uani 1 1 d . . . H10A H -0.2424 1.3385 0.7662 0.048 Uiso 1 1 calc R . . H10B H -0.2522 1.2716 0.8228 0.048 Uiso 1 1 calc R . . C14 C -0.3615(4) 0.6229(11) 0.8221(3) 0.0473(19) Uani 1 1 d . . . H14A H -0.3213 0.5551 0.8295 0.057 Uiso 1 1 calc R . . H14B H -0.3749 0.6754 0.8543 0.057 Uiso 1 1 calc R . . C4 C -0.1414(3) 1.0752(9) 0.8348(3) 0.0321(15) Uani 1 1 d . . . C13 C -0.3491(4) 0.7816(11) 0.7848(3) 0.0463(19) Uani 1 1 d . . . H13A H -0.3357 0.7285 0.7527 0.056 Uiso 1 1 calc R . . H13B H -0.3895 0.8484 0.7773 0.056 Uiso 1 1 calc R . . C5 C -0.0801(3) 1.0316(9) 0.8190(2) 0.0321(15) Uani 1 1 d . . . C15 C -0.4130(4) 0.4877(11) 0.8014(3) 0.051(2) Uani 1 1 d . . . H15A H -0.3998 0.4383 0.7688 0.061 Uiso 1 1 calc R . . H15B H -0.4532 0.5564 0.7944 0.061 Uiso 1 1 calc R . . C6' C 0.0375(3) 0.5765(8) 1.1054(2) 0.0292(14) Uani 1 1 d . . . C8 C -0.1314(4) 1.1610(9) 0.7548(3) 0.0369(16) Uani 1 1 d . . . H8 H -0.1416 1.2099 0.7221 0.044 Uiso 1 1 calc R . . C16 C -0.4267(4) 0.3245(11) 0.8367(3) 0.052(2) Uani 1 1 d . . . H16A H -0.4423 0.3727 0.8686 0.063 Uiso 1 1 calc R . . H16B H -0.3864 0.2581 0.8450 0.063 Uiso 1 1 calc R . . C11 C -0.2890(4) 1.0830(10) 0.7684(3) 0.0420(18) Uani 1 1 d . . . H11A H -0.3309 1.1424 0.7613 0.050 Uiso 1 1 calc R . . H11B H -0.2746 1.0349 0.7360 0.050 Uiso 1 1 calc R . . C8' C 0.1338(3) 0.6003(11) 0.9966(3) 0.0386(17) Uani 1 1 d . . . H8' H 0.1441 0.6207 0.9626 0.046 Uiso 1 1 calc R . . C19 C 0.2449(4) 0.4803(13) 1.0281(3) 0.051(2) Uani 1 1 d . . . H19A H 0.2517 0.4507 0.9923 0.061 Uiso 1 1 calc R . . H19B H 0.2547 0.3691 1.0485 0.061 Uiso 1 1 calc R . . C2' C 0.1238(4) 0.4564(9) 1.1587(2) 0.0330(15) Uani 1 1 d . . . H2' H 0.1374 0.4162 1.1916 0.040 Uiso 1 1 calc R . . C20 C 0.2908(5) 0.6351(17) 1.0458(4) 0.075(3) Uani 1 1 d . . . H20A H 0.2789 0.6778 1.0795 0.090 Uiso 1 1 calc R . . H20B H 0.3345 0.5846 1.0498 0.090 Uiso 1 1 calc R . . C21 C 0.2911(7) 0.7911(16) 1.0120(5) 0.097(4) Uani 1 1 d . . . H21A H 0.2496 0.8550 1.0120 0.116 Uiso 1 1 calc R . . H21B H 0.2972 0.7482 0.9771 0.116 Uiso 1 1 calc R . . C17 C -0.4767(5) 0.1873(13) 0.8130(4) 0.067(3) Uani 1 1 d . . . H17A H -0.4615 0.1398 0.7808 0.080 Uiso 1 1 calc R . . H17B H -0.5173 0.2527 0.8052 0.080 Uiso 1 1 calc R . . C18 C -0.4890(5) 0.0214(13) 0.8492(4) 0.076(3) Uani 1 1 d . . . H18A H -0.4486 -0.0407 0.8582 0.114 Uiso 1 1 calc R . . H18B H -0.5185 -0.0650 0.8319 0.114 Uiso 1 1 calc R . . H18C H -0.5075 0.0667 0.8799 0.114 Uiso 1 1 calc R . . O3 O 0.0985(3) 0.0992(11) 0.7765(2) 0.082(3) Uani 1 1 d . . . O4 O 0.0800(3) 0.0913(8) 0.9677(2) 0.0515(14) Uani 1 1 d . . . N10 N 0.1376(3) 0.2219(9) 0.7925(2) 0.0383(14) Uani 1 1 d . . . O1 O 0.1841(3) 0.2616(7) 0.7679(2) 0.0445(13) Uani 1 1 d . . . O2 O 0.1285(3) 0.3022(9) 0.8345(2) 0.0591(16) Uani 1 1 d . . . O6 O 0.1378(3) -0.0760(8) 0.9185(2) 0.0541(15) Uani 1 1 d . . . N11 N 0.1335(3) 0.0639(10) 0.9480(2) 0.0419(15) Uani 1 1 d . . . O5 O 0.1801(3) 0.1595(11) 0.9582(3) 0.085(2) Uani 1 1 d . . . C22 C 0.3491(10) 0.935(2) 1.0298(5) 0.155(8) Uani 1 1 d . . . H22A H 0.3370 1.0040 1.0600 0.186 Uiso 1 1 calc R . . H22B H 0.3884 0.8656 1.0391 0.186 Uiso 1 1 calc R . . C23 C 0.3613(9) 1.063(3) 0.9897(8) 0.174(9) Uani 1 1 d . . . H22C H 0.3211 1.1279 0.9801 0.209 Uiso 1 1 calc R . . H22D H 0.3733 0.9919 0.9599 0.209 Uiso 1 1 calc R . . O7 O 0.2262(4) 0.8751(10) 0.8416(3) 0.079(2) Uani 1 1 d . . . H233 H 0.2027 0.9122 0.8639 0.119 Uiso 1 1 calc R . . C28 C 0.2866(6) 0.978(2) 0.8451(5) 0.105(4) Uani 1 1 d . . . H32A H 0.2784 1.1044 0.8555 0.158 Uiso 1 1 calc R . . H32B H 0.3052 0.9786 0.8121 0.158 Uiso 1 1 calc R . . H32C H 0.3162 0.9200 0.8701 0.158 Uiso 1 1 calc R . . O8 O 0.2233(4) 0.5275(10) 0.8965(3) 0.082(2) Uani 1 1 d D . . C24 C 0.4109(9) 1.201(3) 1.0010(10) 0.185(10) Uani 1 1 d . . . H66A H 0.4540 1.1451 1.0025 0.221 Uiso 1 1 calc R . . H66B H 0.4044 1.2642 1.0333 0.221 Uiso 1 1 calc R . . C25 C 0.4006(12) 1.336(4) 0.9539(11) 0.266(17) Uani 1 1 d D . . H25A H 0.3959 1.2552 0.9238 0.319 Uiso 1 1 calc R . . H25B H 0.3582 1.3920 0.9575 0.319 Uiso 1 1 calc R . . C27 C 0.421(2) 1.590(4) 0.8898(18) 0.63(6) Uani 1 1 d D . . H27A H 0.4565 1.6677 0.8799 0.649 Uiso 1 1 calc R . . H27B H 0.3841 1.6668 0.8956 0.649 Uiso 1 1 calc R . . H27C H 0.4103 1.5019 0.8629 0.649 Uiso 1 1 calc R . . C26 C 0.4416(13) 1.486(4) 0.9390(18) 0.68(7) Uani 1 1 d D . . H26A H 0.4849 1.4363 0.9353 0.812 Uiso 1 1 calc R . . H26B H 0.4447 1.5762 0.9670 0.812 Uiso 1 1 calc R . . C29 C 0.1601(16) 0.592(10) 0.8697(14) 0.66(7) Uani 1 1 d 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 Ag2 0.0466(3) 0.0276(3) 0.0259(3) 0.0006(2) 0.0051(2) -0.0026(2) Ag1 0.0548(4) 0.0308(3) 0.0254(3) -0.0009(2) 0.0114(2) -0.0013(2) N6' 0.044(3) 0.041(3) 0.016(2) 0.008(2) 0.007(2) -0.001(3) N1 0.041(3) 0.023(3) 0.028(3) -0.004(2) 0.010(2) -0.005(2) N3' 0.044(3) 0.025(3) 0.034(3) -0.003(2) 0.006(3) -0.005(3) N7' 0.039(3) 0.029(3) 0.031(3) 0.003(2) 0.003(2) 0.000(3) N7 0.044(3) 0.027(3) 0.030(3) -0.004(2) 0.008(3) -0.002(3) N9 0.048(4) 0.028(3) 0.025(3) 0.001(2) 0.004(2) 0.003(3) N9' 0.031(3) 0.040(3) 0.040(3) -0.004(3) 0.009(3) -0.002(3) N3 0.046(3) 0.026(3) 0.028(3) -0.007(2) 0.014(3) -0.001(3) C5' 0.043(4) 0.022(3) 0.023(3) -0.001(2) 0.011(3) -0.008(3) N1' 0.045(3) 0.019(3) 0.026(3) 0.008(2) 0.004(2) -0.005(2) N6 0.045(3) 0.028(3) 0.030(3) 0.002(2) 0.008(3) 0.000(3) C12 0.039(4) 0.036(4) 0.050(4) -0.006(3) 0.001(3) 0.003(3) C6 0.049(4) 0.013(3) 0.029(3) -0.002(2) 0.009(3) -0.003(3) C2 0.047(4) 0.027(3) 0.027(3) -0.010(3) 0.013(3) -0.004(3) C4' 0.041(4) 0.020(3) 0.029(3) -0.001(3) 0.004(3) -0.008(3) C10 0.054(5) 0.028(4) 0.040(4) -0.001(3) 0.005(3) 0.004(3) C14 0.039(4) 0.035(4) 0.067(5) 0.000(4) -0.001(4) 0.001(3) C4 0.044(4) 0.022(3) 0.030(3) -0.004(3) 0.004(3) -0.009(3) C13 0.047(5) 0.040(4) 0.051(5) 0.000(4) -0.004(4) -0.002(4) C5 0.045(4) 0.027(3) 0.025(3) -0.003(3) 0.008(3) -0.004(3) C15 0.046(5) 0.038(5) 0.068(6) 0.004(4) -0.010(4) -0.005(4) C6' 0.042(4) 0.016(3) 0.030(3) -0.004(2) 0.005(3) -0.004(3) C8 0.058(5) 0.023(3) 0.029(3) -0.002(3) -0.002(3) 0.000(3) C16 0.050(5) 0.039(5) 0.068(6) 0.004(4) -0.007(4) 0.001(4) C11 0.047(4) 0.038(4) 0.040(4) -0.006(3) -0.002(3) 0.003(3) C8' 0.042(4) 0.043(4) 0.032(4) 0.004(3) 0.006(3) -0.005(3) C19 0.047(5) 0.064(6) 0.044(4) -0.003(4) 0.009(4) 0.002(4) C2' 0.053(4) 0.019(3) 0.026(3) -0.005(3) -0.001(3) -0.005(3) C20 0.060(6) 0.105(9) 0.063(6) -0.011(6) 0.021(5) -0.023(6) C21 0.149(12) 0.067(7) 0.075(7) -0.012(6) 0.016(8) -0.042(8) C17 0.062(6) 0.044(5) 0.093(7) 0.008(5) -0.006(5) -0.007(4) C18 0.072(7) 0.046(6) 0.110(9) 0.006(6) 0.003(6) -0.013(5) O3 0.097(5) 0.124(6) 0.026(3) 0.009(3) 0.003(3) -0.079(5) O4 0.067(4) 0.048(3) 0.040(3) 0.006(3) 0.011(3) 0.012(3) N10 0.047(4) 0.041(3) 0.027(3) -0.002(3) 0.002(3) 0.001(3) O1 0.048(3) 0.042(3) 0.045(3) -0.002(2) 0.020(3) -0.008(2) O2 0.060(4) 0.070(4) 0.049(3) -0.014(3) 0.018(3) 0.000(3) O6 0.071(4) 0.041(3) 0.051(3) -0.004(3) 0.010(3) 0.000(3) N11 0.042(4) 0.048(4) 0.037(3) 0.008(3) 0.007(3) 0.005(3) O5 0.071(5) 0.083(5) 0.101(6) -0.030(5) 0.015(4) -0.037(4) C22 0.27(2) 0.116(13) 0.082(9) -0.023(9) 0.042(12) -0.041(14) C23 0.154(16) 0.160(18) 0.21(2) -0.011(16) 0.027(15) -0.096(14) O7 0.111(6) 0.062(4) 0.069(5) -0.003(4) 0.032(4) -0.012(4) C28 0.096(9) 0.124(12) 0.097(9) 0.018(9) 0.020(7) -0.026(9) O8 0.115(6) 0.061(4) 0.070(5) -0.004(4) 0.009(4) -0.013(4) C24 0.134(15) 0.113(14) 0.33(3) 0.017(17) 0.083(18) -0.040(12) C25 0.25(3) 0.26(3) 0.30(3) 0.12(3) 0.18(3) 0.09(3) C27 0.92(10) 0.20(3) 0.96(11) 0.25(5) 0.78(9) 0.27(5) C26 0.87(6) 0.24(4) 1.15(19) 0.24(8) 0.75(10) 0.24(5) C29 0.49(7) 1.3(2) 0.18(3) -0.09(7) -0.02(4) -0.30(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 Ag2 N7' 2.175(6) . ? Ag2 N1 2.193(6) . ? Ag1 N7 2.140(5) . ? Ag1 N1' 2.156(5) 4_575 ? N6' C6' 1.315(8) . ? N1 C2 1.361(8) . ? N1 C6 1.369(8) . ? N3' C4' 1.337(8) . ? N3' C2' 1.342(8) . ? N7' C8' 1.320(9) . ? N7' C5' 1.386(8) . ? N7 C8 1.323(9) . ? N7 C5 1.377(8) . ? N9 C8 1.352(9) . ? N9 C4 1.379(9) . ? N9 C10 1.464(9) . ? N9' C8' 1.339(9) . ? N9' C4' 1.381(8) . ? N9' C19 1.478(9) . ? N3 C2 1.325(9) . ? N3 C4 1.344(8) . ? C5' C4' 1.388(10) . ? C5' C6' 1.415(8) . ? N1' C2' 1.354(9) . ? N1' C6' 1.356(8) . ? N1' Ag1 2.156(5) 4_576 ? N6 C6 1.324(8) . ? C12 C11 1.519(10) . ? C12 C13 1.522(10) . ? C6 C5 1.427(10) . ? C10 C11 1.533(10) . ? C14 C15 1.511(11) . ? C14 C13 1.523(11) . ? C4 C5 1.387(9) . ? C15 C16 1.520(11) . ? C16 C17 1.525(12) . ? C19 C20 1.510(13) . ? C20 C21 1.420(15) . ? C21 C22 1.626(17) . ? C17 C18 1.543(13) . ? O3 N10 1.245(8) . ? O4 N11 1.257(8) . ? N10 O1 1.214(7) . ? N10 O2 1.256(8) . ? O6 N11 1.266(8) . ? N11 O5 1.196(8) . ? C22 C23 1.42(2) . ? C23 C24 1.44(2) . ? O7 C28 1.444(13) . ? O8 C29 1.51(2) . ? C24 C25 1.57(3) . ? C25 C26 1.434(18) . ? C27 C26 1.51(2) . ? 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 N7' Ag2 N1 168.9(2) . . ? N7 Ag1 N1' 173.8(2) . 4_575 ? C2 N1 C6 119.6(6) . . ? C2 N1 Ag2 120.1(4) . . ? C6 N1 Ag2 120.1(5) . . ? C4' N3' C2' 110.8(6) . . ? C8' N7' C5' 104.8(6) . . ? C8' N7' Ag2 119.6(5) . . ? C5' N7' Ag2 135.0(4) . . ? C8 N7 C5 104.2(6) . . ? C8 N7 Ag1 121.4(5) . . ? C5 N7 Ag1 133.8(5) . . ? C8 N9 C4 106.3(6) . . ? C8 N9 C10 125.9(6) . . ? C4 N9 C10 127.7(6) . . ? C8' N9' C4' 107.1(6) . . ? C8' N9' C19 128.3(6) . . ? C4' N9' C19 124.6(6) . . ? C2 N3 C4 111.9(6) . . ? N7' C5' C4' 109.6(5) . . ? N7' C5' C6' 134.4(6) . . ? C4' C5' C6' 116.0(6) . . ? C2' N1' C6' 120.4(6) . . ? C2' N1' Ag1 118.2(4) . 4_576 ? C6' N1' Ag1 121.1(4) . 4_576 ? C11 C12 C13 112.9(6) . . ? N6 C6 N1 119.7(6) . . ? N6 C6 C5 123.6(6) . . ? N1 C6 C5 116.6(6) . . ? N3 C2 N1 127.7(6) . . ? N3' C4' N9' 125.9(6) . . ? N3' C4' C5' 128.7(6) . . ? N9' C4' C5' 105.4(6) . . ? N9 C10 C11 112.1(6) . . ? C15 C14 C13 113.0(7) . . ? N3 C4 N9 127.0(6) . . ? N3 C4 C5 127.4(7) . . ? N9 C4 C5 105.6(6) . . ? C12 C13 C14 114.0(6) . . ? N7 C5 C4 110.4(6) . . ? N7 C5 C6 133.0(6) . . ? C4 C5 C6 116.6(6) . . ? C14 C15 C16 115.4(7) . . ? N6' C6' N1' 119.7(6) . . ? N6' C6' C5' 123.3(6) . . ? N1' C6' C5' 117.0(6) . . ? N7 C8 N9 113.5(6) . . ? C15 C16 C17 113.4(7) . . ? C12 C11 C10 114.1(6) . . ? N7' C8' N9' 113.1(6) . . ? N9' C19 C20 111.9(7) . . ? N3' C2' N1' 127.1(6) . . ? C21 C20 C19 114.4(9) . . ? C20 C21 C22 110.7(11) . . ? C16 C17 C18 112.4(8) . . ? O1 N10 O3 120.3(6) . . ? O1 N10 O2 120.7(6) . . ? O3 N10 O2 119.0(6) . . ? O5 N11 O4 122.1(7) . . ? O5 N11 O6 120.1(7) . . ? O4 N11 O6 117.6(7) . . ? C23 C22 C21 111.0(13) . . ? C22 C23 C24 116.5(19) . . ? C23 C24 C25 102(2) . . ? C26 C25 C24 128(3) . . ? C25 C26 C27 117(3) . . ? 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 N7' Ag2 N1 C2 150.4(9) . . . . ? N7' Ag2 N1 C6 -32.9(13) . . . . ? N1 Ag2 N7' C8' 32.2(14) . . . . ? N1 Ag2 N7' C5' -158.3(9) . . . . ? N1' Ag1 N7 C8 -26(2) 4_575 . . . ? N1' Ag1 N7 C5 143.0(17) 4_575 . . . ? C8' N7' C5' C4' 1.9(7) . . . . ? Ag2 N7' C5' C4' -168.6(5) . . . . ? C8' N7' C5' C6' -178.7(7) . . . . ? Ag2 N7' C5' C6' 10.8(12) . . . . ? C2 N1 C6 N6 -179.8(6) . . . . ? Ag2 N1 C6 N6 3.5(8) . . . . ? C2 N1 C6 C5 -2.8(9) . . . . ? Ag2 N1 C6 C5 -179.5(4) . . . . ? C4 N3 C2 N1 2.3(10) . . . . ? C6 N1 C2 N3 -0.6(10) . . . . ? Ag2 N1 C2 N3 176.1(5) . . . . ? C2' N3' C4' N9' -178.7(6) . . . . ? C2' N3' C4' C5' 0.1(10) . . . . ? C8' N9' C4' N3' 179.3(6) . . . . ? C19 N9' C4' N3' -0.6(11) . . . . ? C8' N9' C4' C5' 0.3(7) . . . . ? C19 N9' C4' C5' -179.6(7) . . . . ? N7' C5' C4' N3' 179.6(6) . . . . ? C6' C5' C4' N3' 0.1(10) . . . . ? N7' C5' C4' N9' -1.4(7) . . . . ? C6' C5' C4' N9' 179.1(5) . . . . ? C8 N9 C10 C11 87.3(8) . . . . ? C4 N9 C10 C11 -91.4(8) . . . . ? C2 N3 C4 N9 179.5(6) . . . . ? C2 N3 C4 C5 -0.6(10) . . . . ? C8 N9 C4 N3 -179.6(6) . . . . ? C10 N9 C4 N3 -0.6(11) . . . . ? C8 N9 C4 C5 0.5(7) . . . . ? C10 N9 C4 C5 179.4(6) . . . . ? C11 C12 C13 C14 -176.5(6) . . . . ? C15 C14 C13 C12 179.8(7) . . . . ? C8 N7 C5 C4 0.1(7) . . . . ? Ag1 N7 C5 C4 -170.5(5) . . . . ? C8 N7 C5 C6 -177.1(7) . . . . ? Ag1 N7 C5 C6 12.3(11) . . . . ? N3 C4 C5 N7 179.7(6) . . . . ? N9 C4 C5 N7 -0.3(7) . . . . ? N3 C4 C5 C6 -2.6(10) . . . . ? N9 C4 C5 C6 177.3(6) . . . . ? N6 C6 C5 N7 -1.9(12) . . . . ? N1 C6 C5 N7 -178.8(7) . . . . ? N6 C6 C5 C4 -178.9(6) . . . . ? N1 C6 C5 C4 4.2(9) . . . . ? C13 C14 C15 C16 179.0(7) . . . . ? C2' N1' C6' N6' -179.6(6) . . . . ? Ag1 N1' C6' N6' 6.4(8) 4_576 . . . ? C2' N1' C6' C5' 2.3(9) . . . . ? Ag1 N1' C6' C5' -171.8(4) 4_576 . . . ? N7' C5' C6' N6' 1.3(11) . . . . ? C4' C5' C6' N6' -179.3(6) . . . . ? N7' C5' C6' N1' 179.4(7) . . . . ? C4' C5' C6' N1' -1.3(8) . . . . ? C5 N7 C8 N9 0.3(8) . . . . ? Ag1 N7 C8 N9 172.3(4) . . . . ? C4 N9 C8 N7 -0.5(8) . . . . ? C10 N9 C8 N7 -179.5(6) . . . . ? C14 C15 C16 C17 -177.3(8) . . . . ? C13 C12 C11 C10 176.6(6) . . . . ? N9 C10 C11 C12 67.6(8) . . . . ? C5' N7' C8' N9' -1.8(8) . . . . ? Ag2 N7' C8' N9' 170.5(5) . . . . ? C4' N9' C8' N7' 1.0(8) . . . . ? C19 N9' C8' N7' -179.1(7) . . . . ? C8' N9' C19 C20 97.0(9) . . . . ? C4' N9' C19 C20 -83.1(9) . . . . ? C4' N3' C2' N1' 1.0(9) . . . . ? C6' N1' C2' N3' -2.3(10) . . . . ? Ag1 N1' C2' N3' 171.9(5) 4_576 . . . ? N9' C19 C20 C21 -72.0(11) . . . . ? C19 C20 C21 C22 -171.7(10) . . . . ? C15 C16 C17 C18 179.2(8) . . . . ? C20 C21 C22 C23 164.3(16) . . . . ? C21 C22 C23 C24 179.0(16) . . . . ? C22 C23 C24 C25 -169.0(19) . . . . ? C23 C24 C25 C26 -170(3) . . . . ? C24 C25 C26 C27 177(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.358 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.174 data_Complex-2 _database_code_depnum_ccdc_archive 'CCDC 772591' #TrackingRef 'Final-CIF-Merged.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '9PAAgClO4 NH4OH' _chemical_melting_point ? _chemical_formula_moiety 'C32 H44 Ag4 Cl4 N20 O18' _chemical_formula_sum 'C32 H44 Ag4 Cl4 N20 O18' _chemical_formula_weight 1570.15 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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 25.146(5) _cell_length_b 25.516(5) _cell_length_c 7.849(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 5036(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description hexagonal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_correction_T_max 0.9219 _exptl_absorpt_process_details '(North et al., 1968)' _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 'CCD area Detector' _diffrn_measurement_method 'Phi-Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7959 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2683 _reflns_number_gt 2361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45 (Bruker, 2003)' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 3.1d' _computing_publication_material ? _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^)+(0.1056P)^2^+183.2561P] 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 -0.19(11) _refine_ls_number_reflns 2683 _refine_ls_number_parameters 178 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _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 0.79629(3) 1.07355(3) 1.49537(16) 0.0245(2) Uani 1 1 d . . . Cl1 Cl 0.74193(12) 0.87093(16) 1.3741(5) 0.0446(8) Uani 1 1 d . . . N1 N 0.7853(4) 0.9412(4) 1.8519(15) 0.031(2) Uani 1 1 d . . . N9 N 0.8998(3) 0.9660(3) 1.5038(16) 0.0270(19) Uani 1 1 d . . . C5 C 0.8659(4) 0.9213(4) 1.7145(15) 0.024(2) Uani 1 1 d . . . O4 O 0.7743(4) 0.8994(4) 1.2578(18) 0.058(3) Uani 1 1 d . . . N7 N 0.9128(3) 0.8954(4) 1.6667(13) 0.027(2) Uani 1 1 d . . . N6 N 0.8327(4) 0.8698(4) 1.9516(15) 0.036(3) Uani 1 1 d . . . H6A H 0.8085 0.8654 2.0278 0.043 Uiso 1 1 calc R . . H6B H 0.8595 0.8489 1.9472 0.043 Uiso 1 1 calc R . . C10 C 0.9100(4) 1.0036(5) 1.3645(16) 0.031(2) Uani 1 1 d U . . H10A H 0.9471 1.0015 1.3314 0.037 Uiso 1 1 calc R . . H10B H 0.9033 1.0389 1.4050 0.037 Uiso 1 1 calc R . . N3 N 0.8155(3) 0.9969(4) 1.6264(14) 0.028(2) Uani 1 1 d . . . O1 O 0.7678(5) 0.8564(9) 1.512(2) 0.113(8) Uani 1 1 d . . . C11 C 0.8752(5) 0.9927(6) 1.2101(17) 0.040(3) Uani 1 1 d U . . H11A H 0.8793 0.9563 1.1762 0.048 Uiso 1 1 calc R . . H11B H 0.8382 0.9984 1.2399 0.048 Uiso 1 1 calc R . . C6 C 0.8286(5) 0.9087(4) 1.8408(16) 0.028(2) Uani 1 1 d . . . C8 C 0.9308(5) 0.9243(5) 1.5401(16) 0.033(3) Uani 1 1 d . . . H8 H 0.9620 0.9166 1.4813 0.039 Uiso 1 1 calc R . . C4 C 0.8571(4) 0.9642(4) 1.6152(15) 0.025(2) Uani 1 1 d . . . C2 C 0.7821(4) 0.9820(4) 1.747(2) 0.036(3) Uani 1 1 d . . . H2 H 0.7521 1.0030 1.7599 0.044 Uiso 1 1 calc R . . C12 C 0.8901(6) 1.0279(6) 1.063(2) 0.050(4) Uani 1 1 d U . . H12A H 0.8890 1.0638 1.0998 0.075 Uiso 1 1 calc R . . H12B H 0.8655 1.0228 0.9715 0.075 Uiso 1 1 calc R . . H12C H 0.9254 1.0194 1.0254 0.075 Uiso 1 1 calc R . . O3 O 0.6930(5) 0.8925(8) 1.385(3) 0.119(8) Uani 1 1 d . . . O2 O 0.7314(9) 0.8178(7) 1.299(4) 0.142(12) Uani 1 1 d . . . O5 O 0.7500 0.7500 1.010(5) 0.151(13) Uani 1 2 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 0.0253(4) 0.0213(3) 0.0269(4) 0.0020(3) -0.0039(3) -0.0034(3) Cl1 0.0293(14) 0.062(2) 0.0424(18) 0.0228(16) -0.0007(12) -0.0009(13) N1 0.025(4) 0.033(5) 0.036(6) 0.010(5) 0.014(4) 0.013(4) N9 0.014(3) 0.026(4) 0.041(5) 0.013(5) 0.013(4) 0.002(3) C5 0.021(5) 0.023(4) 0.029(7) -0.007(4) 0.009(4) 0.001(3) O4 0.062(6) 0.053(6) 0.059(7) 0.023(6) 0.037(6) 0.014(5) N7 0.012(4) 0.028(4) 0.039(6) 0.011(4) 0.009(4) 0.004(3) N6 0.027(5) 0.037(5) 0.044(7) 0.011(5) 0.018(4) 0.013(4) C10 0.024(5) 0.041(6) 0.028(5) 0.022(5) 0.014(4) 0.001(4) N3 0.016(4) 0.029(5) 0.038(6) 0.011(4) 0.011(4) -0.005(3) O1 0.047(7) 0.22(2) 0.076(11) 0.082(14) 0.008(7) 0.019(10) C11 0.040(6) 0.049(7) 0.032(7) 0.000(5) 0.001(5) 0.004(5) C6 0.030(6) 0.024(5) 0.030(6) 0.010(5) 0.006(5) 0.002(4) C8 0.024(5) 0.038(6) 0.035(8) 0.003(5) 0.009(4) 0.008(4) C4 0.029(5) 0.019(5) 0.026(5) 0.000(4) 0.002(4) 0.007(4) C2 0.028(5) 0.016(4) 0.065(8) 0.022(6) 0.006(6) 0.007(4) C12 0.050(8) 0.048(8) 0.051(7) 0.021(7) -0.025(6) -0.016(6) O3 0.039(7) 0.139(16) 0.18(2) 0.082(15) 0.020(10) 0.026(8) O2 0.115(15) 0.072(10) 0.24(4) -0.046(15) 0.002(17) -0.012(10) O5 0.18(3) 0.17(3) 0.10(2) 0.000 0.000 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N7 2.192(9) 11_654 ? Ag1 N3 2.262(10) . ? Ag1 N1 2.370(10) 10_674 ? Cl1 O1 1.314(15) . ? Cl1 O3 1.349(14) . ? Cl1 O4 1.423(11) . ? Cl1 O2 1.50(2) . ? N1 C2 1.332(16) . ? N1 C6 1.371(14) . ? N1 Ag1 2.370(9) 10_675 ? N9 C8 1.350(14) . ? N9 C4 1.386(14) . ? N9 C10 1.477(14) . ? C5 C4 1.361(15) . ? C5 N7 1.402(13) . ? C5 C6 1.403(15) . ? N7 C8 1.317(15) . ? N7 Ag1 2.192(9) 15_645 ? N6 C6 1.324(15) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C10 C11 1.521(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N3 C2 1.320(17) . ? N3 C4 1.342(14) . ? C11 C12 1.51(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C8 H8 0.9300 . ? C2 H2 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 N7 Ag1 N3 138.7(3) 11_654 . ? N7 Ag1 N1 113.9(4) 11_654 10_674 ? N3 Ag1 N1 105.3(4) . 10_674 ? O1 Cl1 O3 121.0(14) . . ? O1 Cl1 O4 112.9(9) . . ? O3 Cl1 O4 110.6(9) . . ? O1 Cl1 O2 98.9(16) . . ? O3 Cl1 O2 103.4(14) . . ? O4 Cl1 O2 108.1(14) . . ? C2 N1 C6 118.8(10) . . ? C2 N1 Ag1 111.5(7) . 10_675 ? C6 N1 Ag1 128.5(8) . 10_675 ? C8 N9 C4 106.8(9) . . ? C8 N9 C10 124.6(10) . . ? C4 N9 C10 128.5(9) . . ? C4 C5 N7 111.3(9) . . ? C4 C5 C6 118.7(10) . . ? N7 C5 C6 130.1(10) . . ? C8 N7 C5 103.2(9) . . ? C8 N7 Ag1 121.2(7) . 15_645 ? C5 N7 Ag1 135.5(7) . 15_645 ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N9 C10 C11 111.7(10) . . ? N9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C2 N3 C4 111.4(10) . . ? C2 N3 Ag1 116.0(7) . . ? C4 N3 Ag1 132.4(7) . . ? C12 C11 C10 110.9(11) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N6 C6 N1 118.2(10) . . ? N6 C6 C5 125.7(11) . . ? N1 C6 C5 116.0(10) . . ? N7 C8 N9 113.6(10) . . ? N7 C8 H8 123.2 . . ? N9 C8 H8 123.2 . . ? N3 C4 C5 126.1(10) . . ? N3 C4 N9 128.7(10) . . ? C5 C4 N9 105.1(9) . . ? N3 C2 N1 129.1(10) . . ? N3 C2 H2 115.5 . . ? N1 C2 H2 115.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C5 N7 C8 0.6(13) . . . . ? C6 C5 N7 C8 178.8(13) . . . . ? C4 C5 N7 Ag1 -176.2(9) . . . 15_645 ? C6 C5 N7 Ag1 2(2) . . . 15_645 ? C8 N9 C10 C11 101.0(14) . . . . ? C4 N9 C10 C11 -75.6(16) . . . . ? N7 Ag1 N3 C2 134.0(10) 11_654 . . . ? N1 Ag1 N3 C2 -64.6(11) 10_674 . . . ? N7 Ag1 N3 C4 -40.4(15) 11_654 . . . ? N1 Ag1 N3 C4 121.1(11) 10_674 . . . ? N9 C10 C11 C12 -174.2(12) . . . . ? C2 N1 C6 N6 176.7(13) . . . . ? Ag1 N1 C6 N6 -17.4(19) 10_675 . . . ? C2 N1 C6 C5 -1.1(19) . . . . ? Ag1 N1 C6 C5 164.7(9) 10_675 . . . ? C4 C5 C6 N6 -177.1(12) . . . . ? N7 C5 C6 N6 5(2) . . . . ? C4 C5 C6 N1 0.6(17) . . . . ? N7 C5 C6 N1 -177.4(12) . . . . ? C5 N7 C8 N9 0.1(14) . . . . ? Ag1 N7 C8 N9 177.5(8) 15_645 . . . ? C4 N9 C8 N7 -0.8(15) . . . . ? C10 N9 C8 N7 -178.0(12) . . . . ? C2 N3 C4 C5 -1.2(19) . . . . ? Ag1 N3 C4 C5 173.3(9) . . . . ? C2 N3 C4 N9 178.9(13) . . . . ? Ag1 N3 C4 N9 -7(2) . . . . ? N7 C5 C4 N3 179.0(11) . . . . ? C6 C5 C4 N3 0.6(19) . . . . ? N7 C5 C4 N9 -1.0(13) . . . . ? C6 C5 C4 N9 -179.5(11) . . . . ? C8 N9 C4 N3 -179.0(12) . . . . ? C10 N9 C4 N3 -2(2) . . . . ? C8 N9 C4 C5 1.1(14) . . . . ? C10 N9 C4 C5 178.1(12) . . . . ? C4 N3 C2 N1 1(2) . . . . ? Ag1 N3 C2 N1 -174.8(14) . . . . ? C6 N1 C2 N3 0(3) . . . . ? Ag1 N1 C2 N3 -167.6(14) 10_675 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.337 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.255 # Attachment 'Final-CIF-Merged.cif.txt' data_Complex-1 _database_code_depnum_ccdc_archive 'CCDC 772592' #TrackingRef 'Final-CIF-Merged.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'adenine silver nitrate' _chemical_melting_point ? _chemical_formula_moiety 'C5 H6 Ag N7 O7' _chemical_formula_sum 'C5 H6 Ag N7 O7' _chemical_formula_weight 384.04 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 monoclinic _symmetry_space_group_name_H-M P21/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 6.5283(17) _cell_length_b 8.175(2) _cell_length_c 20.896(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.687(4) _cell_angle_gamma 90.00 _cell_volume 1109.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.4 _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.869 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.6132 _exptl_absorpt_correction_T_max 0.7541 _exptl_absorpt_process_details '(North et al., 1968)' _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 'CCD area Detector' _diffrn_measurement_method 'Phi-Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6942 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.38 _reflns_number_total 2727 _reflns_number_gt 2269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45 (Bruker, 2003)' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 3.1d' _computing_publication_material ? _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^)+(0.0931P)^2^+10.0960P] 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 2727 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _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 0.97019(7) 0.62177(6) 0.05475(2) 0.0171(2) Uani 1 1 d . . . O1W O 0.4171(8) 0.0976(6) 0.2013(3) 0.0230(11) Uani 1 1 d . . . O1 O 0.9181(8) 0.7068(7) 0.1732(2) 0.0244(11) Uani 1 1 d . . . O5 O 1.0911(8) 1.1492(6) 0.1061(2) 0.0207(10) Uani 1 1 d . . . O6 O 0.8876(8) 0.9721(6) 0.0564(2) 0.0212(10) Uani 1 1 d . . . O2 O 0.8828(9) 0.9414(7) 0.2209(3) 0.0281(12) Uani 1 1 d . . . O3 O 0.6329(7) 0.8445(6) 0.1558(2) 0.0207(10) Uani 1 1 d . . . O4 O 1.2066(8) 0.9118(6) 0.0810(3) 0.0223(10) Uani 1 1 d . . . N7 N 0.6097(8) 0.2300(7) 0.0430(3) 0.0149(10) Uani 1 1 d . . . H7 H 0.7182 0.1698 0.0452 0.018 Uiso 1 1 calc R . . N3 N 1.2615(8) 0.5166(7) 0.0970(3) 0.0170(11) Uani 1 1 d . . . N1 N 0.5271(9) 0.4913(7) 0.1807(3) 0.0189(11) Uani 1 1 d . . . H1 H 0.5698 0.5224 0.2190 0.023 Uiso 1 1 calc R . . C5 C 0.5528(9) 0.3360(8) 0.0894(3) 0.0151(12) Uani 1 1 d . . . N1A N 0.8114(9) 0.8306(8) 0.1836(3) 0.0186(11) Uani 1 1 d . . . N6 N 0.8194(9) 0.3304(8) 0.1781(3) 0.0209(12) Uani 1 1 d . . . H6A H 0.8653 0.3639 0.2158 0.025 Uiso 1 1 calc R . . H6B H 0.8898 0.2618 0.1580 0.025 Uiso 1 1 calc R . . N9 N 0.6857(9) 0.6550(7) -0.0047(3) 0.0171(11) Uani 1 1 d . . . N2A N 1.0641(9) 1.0113(7) 0.0812(3) 0.0179(11) Uani 1 1 d . . . C6 C 0.6435(10) 0.3836(8) 0.1513(3) 0.0153(12) Uani 1 1 d . . . C2 C 0.3456(10) 0.5537(8) 0.1531(3) 0.0172(12) Uani 1 1 d . . . H2 H 0.2776 0.6288 0.1769 0.021 Uiso 1 1 calc R . . C4 C 0.3683(11) 0.4053(8) 0.0643(3) 0.0180(13) Uani 1 1 d . . . C8 C 0.4616(9) 0.2397(8) -0.0061(3) 0.0152(12) Uani 1 1 d . . . H8 H 0.4622 0.1790 -0.0437 0.018 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 0.0139(3) 0.0198(3) 0.0169(3) -0.00080(17) -0.00245(19) 0.00217(16) O1W 0.022(3) 0.026(3) 0.021(2) 0.003(2) 0.001(2) -0.002(2) O1 0.024(3) 0.026(3) 0.023(2) 0.000(2) 0.002(2) 0.008(2) O5 0.017(2) 0.021(2) 0.023(2) -0.0043(19) -0.0005(19) -0.0021(18) O6 0.018(2) 0.021(2) 0.023(2) -0.0010(19) -0.0057(18) -0.0023(19) O2 0.029(3) 0.022(3) 0.031(3) -0.005(2) -0.006(2) 0.001(2) O3 0.015(2) 0.024(2) 0.021(2) -0.003(2) -0.0036(18) 0.0025(19) O4 0.016(2) 0.024(2) 0.026(3) -0.005(2) -0.0057(19) 0.0101(19) N7 0.012(2) 0.017(3) 0.016(2) -0.002(2) 0.0018(19) 0.008(2) N3 0.013(2) 0.017(3) 0.021(3) 0.002(2) -0.001(2) 0.005(2) N1 0.018(3) 0.019(3) 0.018(3) -0.002(2) -0.003(2) -0.002(2) C5 0.009(3) 0.016(3) 0.019(3) -0.004(2) -0.004(2) 0.001(2) N1A 0.017(3) 0.024(3) 0.016(3) -0.001(2) 0.004(2) 0.001(2) N6 0.020(3) 0.028(3) 0.012(2) -0.007(2) -0.010(2) 0.008(2) N9 0.016(3) 0.021(3) 0.014(2) -0.001(2) -0.003(2) -0.005(2) N2A 0.016(3) 0.011(2) 0.027(3) 0.001(2) 0.008(2) 0.000(2) C6 0.011(3) 0.017(3) 0.019(3) -0.002(2) 0.006(2) -0.002(2) C2 0.017(3) 0.021(3) 0.014(3) -0.004(2) 0.005(2) 0.000(2) C4 0.020(3) 0.018(3) 0.016(3) -0.004(2) 0.004(2) -0.003(2) C8 0.014(3) 0.014(3) 0.017(3) 0.000(2) 0.002(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N9 2.146(6) . ? Ag1 N3 2.192(5) . ? Ag1 Ag1 3.0864(11) 3_765 ? O1 N1A 1.259(8) . ? O5 N2A 1.247(7) . ? O6 N2A 1.257(8) . ? O2 N1A 1.254(8) . ? O3 N1A 1.255(7) . ? O4 N2A 1.236(7) . ? N7 C8 1.341(8) . ? N7 C5 1.379(8) . ? N7 H7 0.8600 . ? N3 C2 1.280(8) 1_655 ? N3 C4 1.370(9) 1_655 ? N1 C6 1.349(8) . ? N1 C2 1.364(9) . ? N1 H1 0.8600 . ? C5 C4 1.387(9) . ? C5 C6 1.422(9) . ? N6 C6 1.301(9) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N9 C8 1.326(8) 3_665 ? N9 C4 1.354(8) 3_665 ? C2 N3 1.280(8) 1_455 ? C2 H2 0.9300 . ? C4 N9 1.354(8) 3_665 ? C4 N3 1.370(9) 1_455 ? C8 N9 1.326(8) 3_665 ? C8 H8 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 N9 Ag1 N3 161.7(2) . . ? N9 Ag1 Ag1 79.54(16) . 3_765 ? N3 Ag1 Ag1 82.97(15) . 3_765 ? C8 N7 C5 106.1(5) . . ? C8 N7 H7 127.0 . . ? C5 N7 H7 127.0 . . ? C2 N3 C4 114.9(6) 1_655 1_655 ? C2 N3 Ag1 123.5(5) 1_655 . ? C4 N3 Ag1 121.6(4) 1_655 . ? C6 N1 C2 123.8(6) . . ? C6 N1 H1 118.1 . . ? C2 N1 H1 118.1 . . ? N7 C5 C4 106.0(5) . . ? N7 C5 C6 134.0(6) . . ? C4 C5 C6 120.0(6) . . ? O2 N1A O3 119.5(6) . . ? O2 N1A O1 120.6(6) . . ? O3 N1A O1 119.8(6) . . ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C8 N9 C4 105.4(6) 3_665 3_665 ? C8 N9 Ag1 125.8(4) 3_665 . ? C4 N9 Ag1 128.1(5) 3_665 . ? O4 N2A O5 121.4(6) . . ? O4 N2A O6 119.3(6) . . ? O5 N2A O6 119.3(5) . . ? N6 C6 N1 122.4(6) . . ? N6 C6 C5 124.7(6) . . ? N1 C6 C5 112.9(6) . . ? N3 C2 N1 125.0(6) 1_455 . ? N3 C2 H2 117.5 1_455 . ? N1 C2 H2 117.5 . . ? N9 C4 N3 127.1(6) 3_665 1_455 ? N9 C4 C5 109.7(6) 3_665 . ? N3 C4 C5 123.2(6) 1_455 . ? N9 C8 N7 112.9(6) 3_665 . ? N9 C8 H8 123.6 3_665 . ? N7 C8 H8 123.6 . . ? 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 N9 Ag1 N3 C2 -158.0(6) . . . 1_655 ? Ag1 Ag1 N3 C2 -175.4(6) 3_765 . . 1_655 ? N9 Ag1 N3 C4 22.4(10) . . . 1_655 ? Ag1 Ag1 N3 C4 5.0(5) 3_765 . . 1_655 ? C8 N7 C5 C4 -0.2(7) . . . . ? C8 N7 C5 C6 -178.7(7) . . . . ? N3 Ag1 N9 C8 164.9(6) . . . 3_665 ? Ag1 Ag1 N9 C8 -177.6(6) 3_765 . . 3_665 ? N3 Ag1 N9 C4 -26.2(11) . . . 3_665 ? Ag1 Ag1 N9 C4 -8.7(6) 3_765 . . 3_665 ? C2 N1 C6 N6 177.7(7) . . . . ? C2 N1 C6 C5 -2.6(9) . . . . ? N7 C5 C6 N6 1.0(12) . . . . ? C4 C5 C6 N6 -177.3(7) . . . . ? N7 C5 C6 N1 -178.7(7) . . . . ? C4 C5 C6 N1 2.9(9) . . . . ? C6 N1 C2 N3 1.2(11) . . . 1_455 ? N7 C5 C4 N9 -0.3(8) . . . 3_665 ? C6 C5 C4 N9 178.5(6) . . . 3_665 ? N7 C5 C4 N3 179.2(6) . . . 1_455 ? C6 C5 C4 N3 -2.0(10) . . . 1_455 ? C5 N7 C8 N9 0.6(8) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.402 _refine_diff_density_min -1.843 _refine_diff_density_rms 0.318