# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Wen, Ke' _publ_contact_author_email kwen@brain.ecnu.edu.cn _publ_section_title ; Silver-mediated self-assembly of metallosupramolecular networks based on pyrimidine-containing oxacalix[n]aromatics ; _publ_author_name 'Ke Wen' data_z_3 _database_code_depnum_ccdc_archive 'CCDC 757489' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H27 Ag2 N8 O10' _chemical_formula_weight 911.37 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 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 24.2508(6) _cell_length_b 12.6282(3) _cell_length_c 13.2061(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.7930(10) _cell_angle_gamma 90.00 _cell_volume 3509.74(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_T_max 0.8670 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_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 20484 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0125 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3226 _reflns_number_gt 2829 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0445P)^2^+27.8857P] 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 3226 _refine_ls_number_parameters 255 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.071 _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 0.285725(15) 0.25098(2) 0.39956(3) 0.02973(14) Uani 1 1 d . . . O1 O 0.39734(18) 0.2061(5) 0.7591(3) 0.0801(15) Uani 1 1 d . . . O2 O 0.3629(3) 0.2998(5) 0.6034(5) 0.0918(15) Uani 1 1 d U . . O3 O 0.31242(16) 0.1622(3) 0.6008(3) 0.0514(9) Uani 1 1 d . . . O4 O 0.15368(14) 0.1901(2) -0.2493(2) 0.0314(6) Uani 1 1 d . . . O5 O 0.19723(14) 0.1905(2) 0.1485(2) 0.0314(6) Uani 1 1 d . . . N1 N 0.35886(19) 0.2208(4) 0.6566(3) 0.0492(11) Uani 1 1 d . . . N2 N 0.24826(15) 0.0936(2) 0.3102(3) 0.0253(7) Uani 1 1 d . . . N3 N 0.19254(16) 0.0935(3) -0.3408(3) 0.0275(7) Uani 1 1 d . . . N01 N 0.3016(4) 0.0000 0.0128(12) 0.105(4) Uani 1 2 d S . . N02 N 0.0530(3) 0.0000 -0.1196(5) 0.0428(13) Uani 1 2 d S . . C1 C 0.2041(3) 0.0000 -0.3712(5) 0.0290(12) Uani 1 2 d S . . H1A H 0.2227 0.0000 -0.4198 0.035 Uiso 1 2 calc SR . . C2 C 0.16452(18) 0.0923(3) -0.2748(3) 0.0250(8) Uani 1 1 d U . . C3 C 0.1485(3) 0.0000 -0.2395(5) 0.0243(11) Uani 1 2 d S . . H3A H 0.1280 0.0000 -0.1942 0.029 Uiso 1 2 calc SR . . C4 C 0.13405(19) 0.2035(3) -0.1665(3) 0.0270(8) Uani 1 1 d . . . C5 C 0.17617(18) 0.1829(3) -0.0501(3) 0.0259(8) Uani 1 1 d . . . H5A H 0.2175 0.1557 -0.0250 0.031 Uiso 1 1 calc R . . C6 C 0.15522(19) 0.2039(3) 0.0276(3) 0.0267(8) Uani 1 1 d . . . C7 C 0.0963(2) 0.2449(3) -0.0052(4) 0.0329(10) Uani 1 1 d . . . H7A H 0.0837 0.2588 0.0511 0.040 Uiso 1 1 calc R . . C8 C 0.0554(2) 0.2656(4) -0.1230(4) 0.0377(10) Uani 1 1 d . . . H8A H 0.0145 0.2944 -0.1477 0.045 Uiso 1 1 calc R . . C9 C 0.0741(2) 0.2446(3) -0.2040(4) 0.0331(10) Uani 1 1 d . . . H9A H 0.0461 0.2582 -0.2844 0.040 Uiso 1 1 calc R . . C09 C -0.0678(4) 0.0000 -0.1952(8) 0.069(3) Uani 1 2 d S . . C10 C 0.1898(3) 0.0000 0.1302(5) 0.0239(11) Uani 1 2 d S . . H10A H 0.1624 0.0000 0.0480 0.029 Uiso 1 2 calc SR . . C11 C 0.21104(17) 0.0921(3) 0.1939(3) 0.0234(8) Uani 1 1 d . . . C12 C 0.2644(3) 0.0000 0.3625(5) 0.0269(12) Uani 1 2 d S . . H12A H 0.2900 0.0000 0.4451 0.032 Uiso 1 2 calc SR . . C01 C 0.3985(5) 0.0554(2) 0.3726(13) 0.240(11) Uani 1 1 d DU . . H01A H 0.3841 0.0907 0.3002 0.288 Uiso 1 1 calc R . . C02 C 0.4184(6) 0.1180(11) 0.4732(9) 0.174(8) Uani 1 1 d DU . . H02A H 0.4195 0.1932 0.4734 0.208 Uiso 1 1 calc R . . C03 C 0.4365(4) 0.0557(2) 0.5735(10) 0.151(5) Uani 1 1 d DU . . H03A H 0.4495 0.0911 0.6454 0.181 Uiso 1 1 calc R . . C04 C 0.0305(2) 0.0546(5) -0.5485(4) 0.0507(13) Uani 1 1 d . . . H04A H 0.0514 0.0926 -0.5818 0.061 Uiso 1 1 calc R . . C05 C 0.0000 0.1079(6) -0.5000 0.0503(18) Uani 1 2 d S . . H05A H 0.0000 0.1831 -0.5000 0.060 Uiso 1 2 calc SR . . C06 C 0.3576(5) 0.0000 -0.1282(10) 0.086(3) Uani 1 2 d SD . . C07 C 0.3269(5) 0.0000 -0.0503(10) 0.085(3) Uani 1 2 d SD . . C08 C 0.0009(3) 0.0000 -0.1523(5) 0.0357(14) 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 0.0435(2) 0.02026(19) 0.0275(2) -0.00168(11) 0.01917(16) -0.00431(12) O1 0.048(2) 0.160(5) 0.0242(18) -0.003(2) 0.0119(17) 0.000(3) O2 0.097(2) 0.091(2) 0.084(2) 0.0035(17) 0.0421(17) -0.0174(17) O3 0.0387(18) 0.060(2) 0.054(2) -0.0155(18) 0.0222(16) -0.0076(17) O4 0.0530(17) 0.0188(14) 0.0333(15) 0.0034(11) 0.0296(14) 0.0055(12) O5 0.0437(16) 0.0185(13) 0.0203(13) 0.0004(11) 0.0071(12) 0.0039(12) N1 0.041(2) 0.079(3) 0.030(2) 0.000(2) 0.0191(19) -0.009(2) N2 0.0309(17) 0.0205(16) 0.0222(16) -0.0014(13) 0.0116(14) 0.0005(13) N3 0.0365(18) 0.0212(17) 0.0289(17) 0.0022(13) 0.0194(15) -0.0004(14) N01 0.065(5) 0.067(6) 0.193(12) 0.000 0.070(7) 0.000 N02 0.038(3) 0.045(3) 0.045(3) 0.000 0.019(3) 0.000 C1 0.038(3) 0.025(3) 0.030(3) 0.000 0.022(3) 0.000 C2 0.0275(15) 0.0224(15) 0.0240(14) -0.0007(12) 0.0121(12) 0.0017(12) C3 0.028(3) 0.023(3) 0.023(3) 0.000 0.014(2) 0.000 C4 0.041(2) 0.0161(18) 0.0273(19) 0.0016(15) 0.0195(18) 0.0033(16) C5 0.0291(19) 0.0154(17) 0.030(2) 0.0008(15) 0.0127(17) 0.0036(15) C6 0.036(2) 0.0176(19) 0.0207(18) 0.0011(15) 0.0099(16) 0.0032(16) C7 0.041(2) 0.032(2) 0.030(2) 0.0018(16) 0.0202(19) 0.0099(18) C8 0.034(2) 0.042(3) 0.035(2) 0.0051(19) 0.015(2) 0.0162(19) C9 0.037(2) 0.033(2) 0.023(2) 0.0038(16) 0.0097(18) 0.0103(17) C09 0.032(4) 0.109(8) 0.065(5) 0.000 0.025(4) 0.000 C10 0.024(3) 0.025(3) 0.020(3) 0.000 0.009(2) 0.000 C11 0.0246(18) 0.0215(19) 0.0241(18) 0.0020(15) 0.0120(15) 0.0020(15) C12 0.031(3) 0.025(3) 0.022(3) 0.000 0.011(2) 0.000 C01 0.083(7) 0.197(15) 0.45(3) 0.230(17) 0.143(13) 0.053(8) C02 0.092(9) 0.095(9) 0.30(2) 0.058(11) 0.069(11) -0.010(7) C03 0.066(5) 0.160(10) 0.241(14) -0.098(10) 0.087(7) -0.038(6) C04 0.047(3) 0.068(3) 0.031(2) 0.003(2) 0.014(2) -0.015(2) C05 0.068(5) 0.036(4) 0.030(3) 0.000 0.012(3) 0.000 C06 0.059(6) 0.053(5) 0.130(10) 0.000 0.034(6) 0.000 C07 0.060(6) 0.056(6) 0.129(10) 0.000 0.039(6) 0.000 C08 0.040(4) 0.036(3) 0.034(3) 0.000 0.021(3) 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 N2 2.259(3) . ? Ag1 N3 2.268(3) 7 ? Ag1 O2 2.474(5) . ? O1 N1 1.217(5) . ? O2 N1 1.251(7) . ? O3 N1 1.239(5) . ? O4 C2 1.340(5) . ? O4 C4 1.403(5) . ? O5 C11 1.348(5) . ? O5 C6 1.414(4) . ? N2 C12 1.327(4) . ? N2 C11 1.340(5) . ? N3 C1 1.321(4) . ? N3 C2 1.346(5) . ? N3 Ag1 2.268(3) 7 ? N01 C07 1.257(15) . ? N02 C08 1.115(8) . ? C1 N3 1.321(4) 6 ? C1 H1A 0.9500 . ? C2 C3 1.380(5) . ? C3 C2 1.380(5) 6 ? C3 H3A 0.9500 . ? C4 C5 1.383(5) . ? C4 C9 1.384(6) . ? C5 C6 1.378(5) . ? C5 H5A 0.9500 . ? C6 C7 1.372(6) . ? C7 C8 1.393(6) . ? C7 H7A 0.9500 . ? C8 C9 1.377(7) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C09 C08 1.468(10) . ? C10 C11 1.377(5) . ? C10 C11 1.377(5) 6 ? C10 H10A 0.9500 . ? C12 N2 1.327(4) 6 ? C12 H12A 0.9500 . ? C01 C01 1.400(5) 6 ? C01 C02 1.409(5) . ? C01 H01A 0.9500 . ? C02 C03 1.410(5) . ? C02 H02A 0.9500 . ? C03 C03 1.408(5) 6 ? C03 H03A 0.9500 . ? C04 C05 1.371(7) . ? C04 C04 1.380(11) 6 ? C04 H04A 0.9500 . ? C05 C04 1.371(7) 2_554 ? C05 H05A 0.9500 . ? C06 C07 1.541(9) . ? 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 N3 133.20(11) . 7 ? N2 Ag1 O2 132.69(16) . . ? N3 Ag1 O2 88.74(15) 7 . ? N1 O2 Ag1 100.7(4) . . ? C2 O4 C4 119.4(3) . . ? C11 O5 C6 119.6(3) . . ? O1 N1 O3 122.6(5) . . ? O1 N1 O2 121.0(5) . . ? O3 N1 O2 116.3(4) . . ? C12 N2 C11 116.2(4) . . ? C12 N2 Ag1 125.0(3) . . ? C11 N2 Ag1 118.6(2) . . ? C1 N3 C2 116.0(4) . . ? C1 N3 Ag1 123.3(3) . 7 ? C2 N3 Ag1 120.6(3) . 7 ? N3 C1 N3 126.7(5) . 6 ? N3 C1 H1A 116.7 . . ? N3 C1 H1A 116.7 6 . ? O4 C2 N3 112.2(3) . . ? O4 C2 C3 124.8(3) . . ? N3 C2 C3 123.0(4) . . ? C2 C3 C2 115.2(5) 6 . ? C2 C3 H3A 122.4 6 . ? C2 C3 H3A 122.4 . . ? C5 C4 C9 122.2(4) . . ? C5 C4 O4 119.6(3) . . ? C9 C4 O4 118.0(3) . . ? C6 C5 C4 116.7(4) . . ? C6 C5 H5A 121.6 . . ? C4 C5 H5A 121.6 . . ? C7 C6 C5 123.3(4) . . ? C7 C6 O5 117.0(3) . . ? C5 C6 O5 119.5(3) . . ? C6 C7 C8 118.3(4) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C4 119.1(4) . . ? C8 C9 H9A 120.4 . . ? C4 C9 H9A 120.4 . . ? C11 C10 C11 115.3(5) . 6 ? C11 C10 H10A 122.3 . . ? C11 C10 H10A 122.3 6 . ? N2 C11 O5 111.9(3) . . ? N2 C11 C10 123.2(4) . . ? O5 C11 C10 124.9(3) . . ? N2 C12 N2 126.0(5) 6 . ? N2 C12 H12A 117.0 6 . ? N2 C12 H12A 117.0 . . ? C01 C01 C02 124.1(7) 6 . ? C01 C01 H01A 117.9 6 . ? C02 C01 H01A 117.9 . . ? C01 C02 C03 112.0(13) . . ? C01 C02 H02A 124.0 . . ? C03 C02 H02A 124.0 . . ? C03 C03 C02 123.9(7) 6 . ? C03 C03 H03A 118.0 6 . ? C02 C03 H03A 118.0 . . ? C05 C04 C04 119.4(4) . 6 ? C05 C04 H04A 120.3 . . ? C04 C04 H04A 120.3 6 . ? C04 C05 C04 121.3(7) . 2_554 ? C04 C05 H05A 119.4 . . ? C04 C05 H05A 119.4 2_554 . ? N01 C07 C06 179.7(11) . . ? N02 C08 C09 179.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 O2 N1 -24.7(5) . . . . ? N3 Ag1 O2 N1 179.6(4) 7 . . . ? Ag1 O2 N1 O1 168.0(4) . . . . ? Ag1 O2 N1 O3 -15.0(5) . . . . ? N3 Ag1 N2 C12 146.6(4) 7 . . . ? O2 Ag1 N2 C12 1.0(5) . . . . ? N3 Ag1 N2 C11 -27.4(3) 7 . . . ? O2 Ag1 N2 C11 -173.0(3) . . . . ? C2 N3 C1 N3 -1.9(8) . . . 6 ? Ag1 N3 C1 N3 -179.7(4) 7 . . 6 ? C4 O4 C2 N3 -170.0(3) . . . . ? C4 O4 C2 C3 10.7(6) . . . . ? C1 N3 C2 O4 -179.1(4) . . . . ? Ag1 N3 C2 O4 -1.3(4) 7 . . . ? C1 N3 C2 C3 0.2(6) . . . . ? Ag1 N3 C2 C3 178.0(3) 7 . . . ? O4 C2 C3 C2 -179.5(3) . . . 6 ? N3 C2 C3 C2 1.3(8) . . . 6 ? C2 O4 C4 C5 69.5(5) . . . . ? C2 O4 C4 C9 -115.3(4) . . . . ? C9 C4 C5 C6 1.0(6) . . . . ? O4 C4 C5 C6 176.1(3) . . . . ? C4 C5 C6 C7 -1.2(6) . . . . ? C4 C5 C6 O5 -176.3(3) . . . . ? C11 O5 C6 C7 109.1(4) . . . . ? C11 O5 C6 C5 -75.4(5) . . . . ? C5 C6 C7 C8 0.5(6) . . . . ? O5 C6 C7 C8 175.8(4) . . . . ? C6 C7 C8 C9 0.4(7) . . . . ? C7 C8 C9 C4 -0.5(7) . . . . ? C5 C4 C9 C8 -0.2(6) . . . . ? O4 C4 C9 C8 -175.4(4) . . . . ? C12 N2 C11 O5 -179.9(4) . . . . ? Ag1 N2 C11 O5 -5.4(4) . . . . ? C12 N2 C11 C10 0.3(6) . . . . ? Ag1 N2 C11 C10 174.8(3) . . . . ? C6 O5 C11 N2 -176.2(3) . . . . ? C6 O5 C11 C10 3.6(6) . . . . ? C11 C10 C11 N2 -1.9(7) 6 . . . ? C11 C10 C11 O5 178.3(3) 6 . . . ? C11 N2 C12 N2 1.5(8) . . . 6 ? Ag1 N2 C12 N2 -172.6(3) . . . 6 ? C01 C01 C02 C03 -1.9(16) 6 . . . ? C01 C02 C03 C03 1.9(16) . . . 6 ? C04 C04 C05 C04 0.000(2) 6 . . 2_554 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.842 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.101 # Attachment '- 4.cif' data_z_4 _database_code_depnum_ccdc_archive 'CCDC 757490' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H35 Ag2 N9 O13' _chemical_formula_weight 1113.55 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 Pna2(1) 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' _cell_length_a 24.0171(11) _cell_length_b 10.0687(5) _cell_length_c 18.5808(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4493.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6697 _exptl_absorpt_correction_T_max 0.8997 _exptl_absorpt_process_details ? _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 ? _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 48046 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7868 _reflns_number_gt 6210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0168P)^2^+13.3997P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 7868 _refine_ls_number_parameters 624 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.140 _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 0.28191(2) 1.72666(5) 0.32072(3) 0.04849(15) Uani 1 1 d . . . Ag2 Ag 0.25225(3) 0.72241(6) 0.00655(3) 0.05524(17) Uani 1 1 d . . . N1 N 0.2368(2) 0.8510(6) 0.2297(3) 0.0402(15) Uani 1 1 d . . . N2 N 0.2269(3) 0.8484(7) 0.1040(3) 0.0415(15) Uani 1 1 d . . . N3 N 0.2262(3) 1.3364(6) 0.4056(3) 0.0413(14) Uani 1 1 d . . . N4 N 0.2306(2) 1.5304(6) 0.3349(3) 0.0444(15) Uani 1 1 d . . . N5 N 0.2010(2) 1.3235(6) -0.0694(3) 0.0364(14) Uani 1 1 d . . . N6 N 0.2106(2) 1.5226(5) -0.0036(3) 0.0369(13) Uani 1 1 d . . . N7 N 0.0639(4) 1.5071(12) 0.4619(5) 0.087(3) Uani 1 1 d . . . N8 N 0.3887(3) 1.6401(10) 0.2385(5) 0.077(2) Uani 1 1 d DU . . O10 O 0.3936(8) 1.647(2) 0.3036(8) 0.133(6) Uani 0.50 1 d PDU A 1 O11 O 0.3416(6) 1.660(3) 0.2263(12) 0.116(7) Uani 0.50 1 d PDU A 1 O12 O 0.4269(17) 1.638(3) 0.197(3) 0.114(11) Uani 0.50 1 d PDU A 1 O10' O 0.3774(8) 1.5650(18) 0.2889(9) 0.114(6) Uani 0.50 1 d PDU A 2 O11' O 0.3637(8) 1.7384(15) 0.2224(13) 0.106(7) Uani 0.50 1 d PDU A 2 O12' O 0.4234(17) 1.586(4) 0.202(2) 0.132(14) Uani 0.50 1 d PDU A 2 N9 N 0.0724(3) 1.2287(6) 0.1818(4) 0.0518(16) Uani 1 1 d . . . O1 O 0.1562(2) 0.9393(5) 0.0452(2) 0.0445(13) Uani 1 1 d . . . O1W O 0.3563(3) 0.7563(10) 0.0543(5) 0.103(3) Uani 1 1 d . . . O2 O 0.1766(2) 0.9452(5) 0.3032(2) 0.0516(14) Uani 1 1 d . . . O3 O 0.1711(2) 1.1657(5) 0.3813(3) 0.0507(14) Uani 1 1 d . . . O4 O 0.17654(19) 1.5643(5) 0.2387(2) 0.0427(12) Uani 1 1 d . A . O5 O 0.1628(2) 1.5653(5) 0.0965(2) 0.0398(12) Uani 1 1 d . . . O6 O 0.1458(2) 1.1577(5) -0.0352(3) 0.0403(12) Uani 1 1 d . . . O7 O 0.0427(5) 1.4324(16) 0.5030(7) 0.210(7) Uani 1 1 d . . . O8 O 0.0407(5) 1.6036(11) 0.4395(8) 0.162(5) Uani 1 1 d . . . O9 O 0.1081(3) 1.4776(9) 0.4399(4) 0.107(3) Uani 1 1 d . . . C1 C 0.2537(3) 0.8200(7) 0.1637(4) 0.048(2) Uani 1 1 d . . . H1A H 0.2872 0.7744 0.1595 0.058 Uiso 1 1 calc R . . C2 C 0.1902(3) 0.9190(7) 0.2341(4) 0.0371(17) Uani 1 1 d . . . C3 C 0.1596(3) 0.9589(6) 0.1752(4) 0.0406(17) Uani 1 1 d . . . H3A H 0.1277 1.0107 0.1794 0.049 Uiso 1 1 calc R . . C4 C 0.1798(3) 0.9164(7) 0.1098(4) 0.0368(17) Uani 1 1 d . . . C5 C 0.1235(3) 0.9948(6) 0.3190(4) 0.0376(15) Uani 1 1 d . . . C6 C 0.0756(3) 0.9280(7) 0.3030(4) 0.051(2) Uani 1 1 d . . . H6A H 0.0774 0.8471 0.2790 0.061 Uiso 1 1 calc R . . C7 C 0.0253(3) 0.9791(9) 0.3219(6) 0.067(2) Uani 1 1 d . . . H7A H -0.0074 0.9353 0.3097 0.080 Uiso 1 1 calc R . . C8 C 0.0238(4) 1.0967(11) 0.3596(5) 0.071(3) Uani 1 1 d . . . H8A H -0.0105 1.1318 0.3728 0.085 Uiso 1 1 calc R . . C9 C 0.0715(4) 1.1640(9) 0.3783(4) 0.055(2) Uani 1 1 d . . . H9A H 0.0700 1.2428 0.4043 0.066 Uiso 1 1 calc R . . C10 C 0.1208(3) 1.1109(6) 0.3575(4) 0.0345(16) Uani 1 1 d . . . C11 C 0.1869(3) 1.2903(7) 0.3620(4) 0.0341(16) Uani 1 1 d . . . C12 C 0.2457(3) 1.4543(9) 0.3895(4) 0.048(2) Uani 1 1 d . . . H12A H 0.2732 1.4880 0.4197 0.058 Uiso 1 1 calc R A . C13 C 0.1904(3) 1.4813(7) 0.2941(3) 0.0355(17) Uani 1 1 d . . . C14 C 0.1675(3) 1.3579(7) 0.3039(3) 0.0342(16) Uani 1 1 d . A . H14A H 0.1407 1.3231 0.2732 0.041 Uiso 1 1 calc R . . C15 C 0.1219(3) 1.5608(7) 0.2125(3) 0.0323(16) Uani 1 1 d . . . C16 C 0.0768(3) 1.5701(7) 0.2573(4) 0.0434(18) Uani 1 1 d . A . H16A H 0.0817 1.5714 0.3070 0.052 Uiso 1 1 calc R . . C17 C 0.0248(3) 1.5776(8) 0.2287(4) 0.051(2) Uani 1 1 d . . . H17A H -0.0059 1.5864 0.2588 0.061 Uiso 1 1 calc R A . C18 C 0.0171(4) 1.5721(8) 0.1545(5) 0.052(2) Uani 1 1 d . A . H18A H -0.0186 1.5727 0.1353 0.063 Uiso 1 1 calc R . . C19 C 0.0621(3) 1.5659(8) 0.1101(4) 0.0392(18) Uani 1 1 d . . . H19A H 0.0573 1.5676 0.0604 0.047 Uiso 1 1 calc R A . C20 C 0.1148(3) 1.5570(7) 0.1387(4) 0.0323(16) Uani 1 1 d . A . C21 C 0.2226(3) 1.4425(7) -0.0579(4) 0.0373(17) Uani 1 1 d . . . H21A H 0.2487 1.4727 -0.0911 0.045 Uiso 1 1 calc R . . C22 C 0.1718(3) 1.4780(7) 0.0426(3) 0.0323(15) Uani 1 1 d . . . C23 C 0.1467(3) 1.3564(7) 0.0363(3) 0.0342(16) Uani 1 1 d . . . H23A H 0.1200 1.3267 0.0688 0.041 Uiso 1 1 calc R . . C24 C 0.1634(3) 1.2817(7) -0.0212(3) 0.0335(16) Uani 1 1 d . . . C25 C 0.0464(3) 1.1624(8) -0.0130(4) 0.0451(18) Uani 1 1 d . . . H25A H 0.0426 1.2389 -0.0407 0.054 Uiso 1 1 calc R . . C26 C 0.0007(3) 1.1041(9) 0.0160(5) 0.057(2) Uani 1 1 d . . . H26A H -0.0343 1.1407 0.0082 0.068 Uiso 1 1 calc R . . C27 C 0.0061(4) 0.9897(9) 0.0573(4) 0.055(2) Uani 1 1 d . . . H27A H -0.0253 0.9500 0.0774 0.065 Uiso 1 1 calc R . . C28 C 0.0570(3) 0.9364(7) 0.0682(4) 0.0459(19) Uani 1 1 d . . . H28A H 0.0604 0.8589 0.0951 0.055 Uiso 1 1 calc R . . C29 C 0.1035(3) 0.9951(6) 0.0402(3) 0.0313(15) Uani 1 1 d . . . C30 C 0.0982(3) 1.1087(6) -0.0017(4) 0.0330(15) Uani 1 1 d . . . C31 C 0.3168(7) 1.4330(11) 0.1001(11) 0.151(8) Uani 1 1 d G . . H31A H 0.3196 1.5196 0.1170 0.181 Uiso 1 1 calc R . . C32 C 0.3439(4) 1.3963(17) 0.0371(11) 0.140(7) Uani 1 1 d G . . H32A H 0.3649 1.4584 0.0119 0.167 Uiso 1 1 calc R . . C33 C 0.3397(5) 1.267(2) 0.0118(5) 0.139(6) Uani 1 1 d G . . H33A H 0.3579 1.2423 -0.0304 0.167 Uiso 1 1 calc R . . C34 C 0.3084(6) 1.1739(10) 0.0495(10) 0.148(7) Uani 1 1 d G . . H34A H 0.3055 1.0873 0.0325 0.178 Uiso 1 1 calc R . . C35 C 0.2812(4) 1.2106(18) 0.1125(10) 0.148(7) Uani 1 1 d G . . H35A H 0.2602 1.1485 0.1377 0.178 Uiso 1 1 calc R . . C36 C 0.2854(6) 1.340(2) 0.1378(5) 0.169(9) Uani 1 1 d G . . H36A H 0.2673 1.3646 0.1800 0.202 Uiso 1 1 calc R . . C37 C 0.0834(4) 0.5494(11) 0.8862(6) 0.123(5) Uani 1 1 d G . . H37A H 0.0593 0.4927 0.9107 0.148 Uiso 1 1 calc R . . C38 C 0.1133(5) 0.5030(8) 0.8273(7) 0.130(6) Uani 1 1 d G . . H38A H 0.1093 0.4154 0.8123 0.156 Uiso 1 1 calc R . . C39 C 0.1493(4) 0.5876(14) 0.7908(4) 0.141(8) Uani 1 1 d G . . H39A H 0.1693 0.5567 0.7514 0.169 Uiso 1 1 calc R . . C40 C 0.1554(3) 0.7186(13) 0.8133(5) 0.114(4) Uani 1 1 d G . . H40A H 0.1794 0.7752 0.7888 0.137 Uiso 1 1 calc R . . C41 C 0.1254(4) 0.7649(8) 0.8722(5) 0.097(4) Uani 1 1 d G . . H41A H 0.1295 0.8525 0.8872 0.116 Uiso 1 1 calc R . . C42 C 0.0895(3) 0.6803(12) 0.9087(4) 0.102(4) Uani 1 1 d G . . H42A H 0.0694 0.7113 0.9481 0.123 Uiso 1 1 calc R . . C43 C -0.0375(4) 1.2358(11) 0.1904(7) 0.094(3) Uani 1 1 d . . . C44 C 0.0242(4) 1.2324(7) 0.1853(4) 0.052(2) Uani 1 1 d . . . H1WB H 0.376(5) 0.759(11) 0.102(5) 0.11(4) Uiso 1 1 d D . . H1WA H 0.381(4) 0.806(9) 0.036(4) 0.07(3) 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 0.0553(3) 0.0467(3) 0.0434(3) -0.0024(4) -0.0133(3) 0.0006(3) Ag2 0.0721(4) 0.0452(3) 0.0484(3) -0.0075(4) 0.0256(3) -0.0094(3) N1 0.044(4) 0.045(4) 0.032(3) -0.001(3) -0.006(3) 0.013(3) N2 0.043(4) 0.048(4) 0.034(3) -0.003(3) 0.004(3) 0.016(3) N3 0.041(4) 0.036(3) 0.047(4) -0.001(3) -0.011(3) -0.001(3) N4 0.044(3) 0.044(4) 0.046(4) 0.001(3) -0.010(3) -0.009(3) N5 0.037(3) 0.046(4) 0.027(3) 0.000(3) 0.009(3) -0.001(3) N6 0.044(3) 0.032(3) 0.035(3) 0.001(3) 0.004(3) -0.006(3) N7 0.079(7) 0.111(9) 0.069(6) -0.022(6) 0.017(5) 0.017(6) N8 0.057(6) 0.094(7) 0.080(5) 0.008(5) -0.008(5) 0.029(5) O10 0.135(6) 0.135(6) 0.131(6) -0.001(2) 0.000(2) 0.002(2) O11 0.060(11) 0.185(19) 0.101(12) -0.023(15) -0.014(10) 0.056(12) O12 0.084(17) 0.14(2) 0.123(18) 0.008(19) 0.060(14) -0.005(17) O10' 0.115(6) 0.114(6) 0.115(6) 0.002(2) 0.000(2) -0.001(2) O11' 0.091(13) 0.088(13) 0.141(15) -0.009(12) -0.052(12) 0.011(10) O12' 0.10(2) 0.16(3) 0.13(2) -0.04(2) 0.022(15) 0.09(2) N9 0.056(5) 0.046(4) 0.054(4) -0.003(3) 0.008(4) 0.000(4) O1 0.051(3) 0.060(3) 0.022(2) 0.002(2) 0.000(2) 0.018(3) O1W 0.069(5) 0.149(8) 0.093(6) -0.004(6) 0.009(5) -0.018(5) O2 0.049(3) 0.071(4) 0.034(3) -0.015(2) -0.009(2) 0.023(3) O3 0.057(3) 0.032(3) 0.064(3) 0.002(2) -0.025(3) -0.004(3) O4 0.040(3) 0.055(3) 0.033(3) 0.011(2) -0.008(2) -0.016(2) O5 0.048(3) 0.039(3) 0.032(3) -0.013(2) 0.011(2) -0.014(2) O6 0.045(3) 0.031(3) 0.045(3) -0.003(2) 0.015(2) -0.004(2) O7 0.179(11) 0.330(19) 0.122(9) 0.043(12) 0.078(9) -0.020(11) O8 0.145(10) 0.107(8) 0.235(13) -0.051(8) -0.064(9) 0.062(7) O9 0.084(6) 0.126(7) 0.109(6) -0.032(5) 0.027(5) 0.016(5) C1 0.051(6) 0.056(4) 0.037(4) -0.004(4) 0.001(4) 0.020(4) C2 0.048(4) 0.028(4) 0.035(4) -0.005(3) -0.004(3) 0.016(3) C3 0.036(5) 0.044(4) 0.042(4) -0.005(4) 0.001(3) 0.010(3) C4 0.041(4) 0.032(4) 0.038(4) 0.002(3) 0.004(3) 0.010(3) C5 0.044(4) 0.038(4) 0.031(3) 0.002(4) -0.002(4) 0.002(3) C6 0.065(5) 0.032(4) 0.055(5) -0.005(3) -0.003(4) -0.013(4) C7 0.048(5) 0.083(6) 0.071(5) 0.002(6) -0.001(5) -0.027(4) C8 0.043(5) 0.096(8) 0.073(6) 0.009(6) 0.017(5) 0.008(5) C9 0.066(6) 0.050(5) 0.050(5) -0.014(4) 0.004(4) 0.015(4) C10 0.044(4) 0.020(4) 0.039(4) -0.002(3) -0.002(3) -0.005(3) C11 0.041(4) 0.028(4) 0.033(3) -0.003(3) -0.007(3) 0.002(3) C12 0.046(5) 0.054(5) 0.045(5) 0.003(4) -0.015(4) -0.006(4) C13 0.038(4) 0.043(4) 0.025(3) -0.001(3) -0.007(3) 0.000(3) C14 0.036(4) 0.035(4) 0.031(4) -0.005(3) -0.007(3) -0.005(3) C15 0.035(4) 0.031(4) 0.031(4) -0.002(3) -0.002(3) 0.001(3) C16 0.057(5) 0.043(4) 0.030(4) -0.006(3) 0.007(3) 0.001(4) C17 0.046(5) 0.054(5) 0.053(5) 0.004(4) 0.012(4) 0.011(4) C18 0.032(5) 0.053(5) 0.072(6) 0.006(4) -0.011(4) 0.001(4) C19 0.050(5) 0.033(4) 0.035(4) 0.007(3) -0.007(4) 0.001(4) C20 0.040(4) 0.022(4) 0.035(4) -0.005(3) 0.006(3) -0.002(3) C21 0.035(4) 0.037(5) 0.040(4) 0.001(3) 0.006(3) -0.003(3) C22 0.034(4) 0.032(4) 0.031(4) 0.007(3) -0.003(3) 0.002(3) C23 0.033(4) 0.038(4) 0.032(4) 0.003(3) 0.004(3) -0.003(3) C24 0.025(3) 0.039(4) 0.037(4) 0.003(3) 0.002(3) 0.004(3) C25 0.046(4) 0.045(4) 0.044(4) 0.004(3) -0.003(3) 0.006(4) C26 0.037(4) 0.068(6) 0.065(5) -0.003(5) -0.003(4) -0.002(4) C27 0.051(5) 0.055(5) 0.058(5) -0.008(4) 0.014(4) -0.023(4) C28 0.061(5) 0.033(4) 0.044(4) -0.002(3) 0.002(4) -0.001(4) C29 0.042(4) 0.025(4) 0.027(3) -0.003(3) -0.004(3) -0.001(3) C30 0.031(4) 0.033(4) 0.035(4) -0.012(3) 0.000(3) -0.002(3) C31 0.141(17) 0.151(17) 0.162(17) -0.043(15) -0.089(14) 0.066(14) C32 0.062(8) 0.132(15) 0.23(3) 0.051(13) -0.032(12) 0.015(9) C33 0.088(11) 0.193(19) 0.136(12) 0.016(17) 0.003(11) 0.049(12) C34 0.110(13) 0.137(15) 0.20(2) -0.024(15) -0.046(13) -0.006(12) C35 0.099(11) 0.157(18) 0.19(2) 0.042(14) 0.024(12) 0.013(12) C36 0.19(2) 0.21(2) 0.106(11) 0.011(15) -0.038(12) 0.122(19) C37 0.111(11) 0.104(12) 0.155(15) 0.038(10) -0.074(11) 0.022(9) C38 0.126(13) 0.107(11) 0.157(15) -0.036(13) -0.074(12) 0.061(10) C39 0.090(11) 0.22(2) 0.118(12) -0.057(14) -0.028(9) 0.065(12) C40 0.067(7) 0.185(15) 0.090(9) 0.014(11) -0.002(7) -0.003(8) C41 0.078(8) 0.120(10) 0.092(8) -0.009(8) -0.024(6) 0.004(8) C42 0.099(10) 0.122(11) 0.086(8) 0.032(8) -0.017(7) 0.032(8) C43 0.040(5) 0.120(9) 0.124(9) -0.025(8) 0.014(6) 0.001(6) C44 0.070(6) 0.039(4) 0.046(5) -0.008(4) 0.008(5) -0.003(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 N5 2.299(5) 4 ? Ag1 N4 2.344(6) . ? Ag1 O11 2.36(2) . ? Ag1 N1 2.366(6) 1_565 ? Ag2 N6 2.254(5) 1_545 ? Ag2 N3 2.259(6) 4_544 ? Ag2 N2 2.294(6) . ? N1 C2 1.316(9) . ? N1 C1 1.328(9) . ? N1 Ag1 2.366(6) 1_545 ? N2 C1 1.314(10) . ? N2 C4 1.327(9) . ? N3 C12 1.311(10) . ? N3 C11 1.328(9) . ? N3 Ag2 2.259(6) 4 ? N4 C12 1.322(10) . ? N4 C13 1.323(8) . ? N5 C21 1.323(9) . ? N5 C24 1.340(8) . ? N5 Ag1 2.299(5) 4_544 ? N6 C21 1.322(9) . ? N6 C22 1.346(8) . ? N6 Ag2 2.254(5) 1_565 ? N7 O9 1.176(10) . ? N7 O7 1.186(14) . ? N7 O8 1.195(13) . ? N8 O11 1.173(12) . ? N8 O11' 1.197(12) . ? N8 O12 1.203(14) . ? N8 O12' 1.206(14) . ? N8 O10 1.217(13) . ? N8 O10' 1.233(12) . ? N9 C44 1.160(9) . ? O1 C4 1.347(8) . ? O1 C29 1.388(8) . ? O1W H1WB 1.01(10) . ? O1W H1WA 0.84(9) . ? O2 C2 1.350(8) . ? O2 C5 1.401(8) . ? O3 C11 1.358(8) . ? O3 C10 1.400(8) . ? O4 C13 1.368(8) . ? O4 C15 1.399(8) . ? O5 C22 1.351(8) . ? O5 C20 1.397(8) . ? O6 C24 1.344(8) . ? O6 C30 1.392(8) . ? C1 H1A 0.9300 . ? C2 C3 1.377(10) . ? C3 C4 1.377(10) . ? C3 H3A 0.9300 . ? C5 C6 1.366(9) . ? C5 C10 1.373(9) . ? C6 C7 1.358(11) . ? C6 H6A 0.9300 . ? C7 C8 1.376(13) . ? C7 H7A 0.9300 . ? C8 C9 1.376(12) . ? C8 H8A 0.9300 . ? C9 C10 1.355(10) . ? C9 H9A 0.9300 . ? C11 C14 1.358(9) . ? C12 H12A 0.9300 . ? C13 C14 1.372(9) . ? C14 H14A 0.9300 . ? C15 C16 1.369(9) . ? C15 C20 1.382(9) . ? C16 C17 1.361(10) . ? C16 H16A 0.9300 . ? C17 C18 1.391(11) . ? C17 H17A 0.9300 . ? C18 C19 1.362(11) . ? C18 H18A 0.9300 . ? C19 C20 1.376(10) . ? C19 H19A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.369(10) . ? C23 C24 1.366(9) . ? C23 H23A 0.9300 . ? C25 C26 1.356(10) . ? C25 C30 1.372(9) . ? C25 H25A 0.9300 . ? C26 C27 1.391(12) . ? C26 H26A 0.9300 . ? C27 C28 1.350(12) . ? C27 H27A 0.9300 . ? C28 C29 1.368(10) . ? C28 H28A 0.9300 . ? C29 C30 1.389(9) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 H31A 0.9300 . ? C32 C33 1.3900 . ? C32 H32A 0.9300 . ? C33 C34 1.3900 . ? C33 H33A 0.9300 . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 H37A 0.9300 . ? C38 C39 1.3900 . ? C38 H38A 0.9300 . ? C39 C40 1.3900 . ? C39 H39A 0.9300 . ? C40 C41 1.3900 . ? C40 H40A 0.9300 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.484(12) . ? 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 N5 Ag1 N4 110.6(2) 4 . ? N5 Ag1 O11 132.2(5) 4 . ? N4 Ag1 O11 99.4(7) . . ? N5 Ag1 N1 119.5(2) 4 1_565 ? N4 Ag1 N1 106.6(2) . 1_565 ? O11 Ag1 N1 84.1(5) . 1_565 ? N6 Ag2 N3 119.0(2) 1_545 4_544 ? N6 Ag2 N2 116.3(2) 1_545 . ? N3 Ag2 N2 115.8(2) 4_544 . ? C2 N1 C1 116.1(6) . . ? C2 N1 Ag1 128.4(5) . 1_545 ? C1 N1 Ag1 113.3(5) . 1_545 ? C1 N2 C4 117.5(6) . . ? C1 N2 Ag2 114.6(5) . . ? C4 N2 Ag2 125.1(5) . . ? C12 N3 C11 115.6(6) . . ? C12 N3 Ag2 124.6(5) . 4 ? C11 N3 Ag2 119.5(5) . 4 ? C12 N4 C13 115.1(6) . . ? C12 N4 Ag1 115.5(5) . . ? C13 N4 Ag1 129.3(5) . . ? C21 N5 C24 116.1(6) . . ? C21 N5 Ag1 117.3(5) . 4_544 ? C24 N5 Ag1 125.5(5) . 4_544 ? C21 N6 C22 115.7(6) . . ? C21 N6 Ag2 120.8(5) . 1_565 ? C22 N6 Ag2 123.5(4) . 1_565 ? O9 N7 O7 116.8(13) . . ? O9 N7 O8 120.4(13) . . ? O7 N7 O8 122.7(13) . . ? O11 N8 O11' 47.4(13) . . ? O11 N8 O12 128(3) . . ? O11' N8 O12 104(3) . . ? O11 N8 O12' 129(3) . . ? O11' N8 O12' 125(3) . . ? O12 N8 O12' 26(3) . . ? O11 N8 O10 106.0(16) . . ? O11' N8 O10 104.5(17) . . ? O12 N8 O10 125(3) . . ? O12' N8 O10 122(3) . . ? O11 N8 O10' 92.2(17) . . ? O11' N8 O10' 125.9(17) . . ? O12 N8 O10' 130(2) . . ? O12' N8 O10' 108(2) . . ? O10 N8 O10' 45.8(11) . . ? N8 O11 Ag1 119.4(14) . . ? C4 O1 C29 120.9(5) . . ? H1WB O1W H1WA 91(6) . . ? C2 O2 C5 119.2(5) . . ? C11 O3 C10 121.4(5) . . ? C13 O4 C15 118.3(5) . . ? C22 O5 C20 120.6(5) . . ? C24 O6 C30 120.1(5) . . ? N2 C1 N1 125.4(7) . . ? N2 C1 H1A 117.3 . . ? N1 C1 H1A 117.3 . . ? N1 C2 O2 111.4(6) . . ? N1 C2 C3 123.8(6) . . ? O2 C2 C3 124.7(6) . . ? C2 C3 C4 115.0(6) . . ? C2 C3 H3A 122.5 . . ? C4 C3 H3A 122.5 . . ? N2 C4 O1 112.1(6) . . ? N2 C4 C3 122.2(7) . . ? O1 C4 C3 125.8(6) . . ? C6 C5 C10 119.5(7) . . ? C6 C5 O2 123.1(7) . . ? C10 C5 O2 117.2(6) . . ? C7 C6 C5 120.4(8) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C8 118.8(8) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? C9 C8 C7 122.0(8) . . ? C9 C8 H8A 119.0 . . ? C7 C8 H8A 119.0 . . ? C10 C9 C8 117.5(8) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? C9 C10 C5 121.7(7) . . ? C9 C10 O3 120.6(7) . . ? C5 C10 O3 117.3(6) . . ? N3 C11 C14 123.6(7) . . ? N3 C11 O3 111.1(6) . . ? C14 C11 O3 125.2(6) . . ? N3 C12 N4 127.0(7) . . ? N3 C12 H12A 116.5 . . ? N4 C12 H12A 116.5 . . ? N4 C13 O4 112.4(6) . . ? N4 C13 C14 123.7(6) . . ? O4 C13 C14 123.8(6) . . ? C11 C14 C13 115.0(6) . . ? C11 C14 H14A 122.5 . . ? C13 C14 H14A 122.5 . . ? C16 C15 C20 120.5(7) . . ? C16 C15 O4 121.9(6) . . ? C20 C15 O4 117.5(6) . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C19 C18 C17 119.9(8) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C15 119.7(7) . . ? C19 C20 O5 122.5(6) . . ? C15 C20 O5 117.0(6) . . ? N6 C21 N5 126.2(7) . . ? N6 C21 H21A 116.9 . . ? N5 C21 H21A 116.9 . . ? N6 C22 O5 111.5(6) . . ? N6 C22 C23 123.3(6) . . ? O5 C22 C23 125.1(6) . . ? C24 C23 C22 115.4(6) . . ? C24 C23 H23A 122.3 . . ? C22 C23 H23A 122.3 . . ? N5 C24 O6 112.0(6) . . ? N5 C24 C23 123.2(7) . . ? O6 C24 C23 124.7(6) . . ? C26 C25 C30 120.1(7) . . ? C26 C25 H25A 119.9 . . ? C30 C25 H25A 119.9 . . ? C25 C26 C27 120.2(8) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 119.8(7) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 120.7(7) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C28 C29 O1 122.9(6) . . ? C28 C29 C30 119.6(6) . . ? O1 C29 C30 117.1(6) . . ? C25 C30 C29 119.6(7) . . ? C25 C30 O6 122.4(6) . . ? C29 C30 O6 117.8(6) . . ? C32 C31 C36 120.0 . . ? C32 C31 H31A 120.0 . . ? C36 C31 H31A 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 H37A 120.0 . . ? C42 C37 H37A 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42A 120.0 . . ? C37 C42 H42A 120.0 . . ? N9 C44 C43 179.4(10) . . ? 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 N6 Ag2 N2 C1 83.6(6) 1_545 . . . ? N3 Ag2 N2 C1 -129.3(5) 4_544 . . . ? N6 Ag2 N2 C4 -77.0(7) 1_545 . . . ? N3 Ag2 N2 C4 70.2(7) 4_544 . . . ? N5 Ag1 N4 C12 -41.2(6) 4 . . . ? O11 Ag1 N4 C12 100.9(7) . . . . ? N1 Ag1 N4 C12 -172.5(5) 1_565 . . . ? N5 Ag1 N4 C13 142.5(6) 4 . . . ? O11 Ag1 N4 C13 -75.4(7) . . . . ? N1 Ag1 N4 C13 11.2(7) 1_565 . . . ? O11' N8 O11 Ag1 -88(3) . . . . ? O12 N8 O11 Ag1 -160(2) . . . . ? O12' N8 O11 Ag1 167(3) . . . . ? O10 N8 O11 Ag1 7(3) . . . . ? O10' N8 O11 Ag1 51(2) . . . . ? N5 Ag1 O11 N8 22(3) 4 . . . ? N4 Ag1 O11 N8 -108(2) . . . . ? N1 Ag1 O11 N8 146(2) 1_565 . . . ? C4 N2 C1 N1 1.7(11) . . . . ? Ag2 N2 C1 N1 -160.4(6) . . . . ? C2 N1 C1 N2 -2.0(11) . . . . ? Ag1 N1 C1 N2 162.3(6) 1_545 . . . ? C1 N1 C2 O2 179.9(6) . . . . ? Ag1 N1 C2 O2 18.3(9) 1_545 . . . ? C1 N1 C2 C3 -0.6(11) . . . . ? Ag1 N1 C2 C3 -162.2(5) 1_545 . . . ? C5 O2 C2 N1 -168.3(6) . . . . ? C5 O2 C2 C3 12.2(11) . . . . ? N1 C2 C3 C4 3.3(11) . . . . ? O2 C2 C3 C4 -177.3(7) . . . . ? C1 N2 C4 O1 -179.9(6) . . . . ? Ag2 N2 C4 O1 -19.9(9) . . . . ? C1 N2 C4 C3 1.4(11) . . . . ? Ag2 N2 C4 C3 161.4(5) . . . . ? C29 O1 C4 N2 172.4(6) . . . . ? C29 O1 C4 C3 -8.9(11) . . . . ? C2 C3 C4 N2 -3.6(11) . . . . ? C2 C3 C4 O1 177.8(7) . . . . ? C2 O2 C5 C6 59.9(10) . . . . ? C2 O2 C5 C10 -125.5(7) . . . . ? C10 C5 C6 C7 3.2(12) . . . . ? O2 C5 C6 C7 177.6(7) . . . . ? C5 C6 C7 C8 -2.2(13) . . . . ? C6 C7 C8 C9 0.2(14) . . . . ? C7 C8 C9 C10 0.8(14) . . . . ? C8 C9 C10 C5 0.3(12) . . . . ? C8 C9 C10 O3 -173.0(7) . . . . ? C6 C5 C10 C9 -2.2(11) . . . . ? O2 C5 C10 C9 -177.0(7) . . . . ? C6 C5 C10 O3 171.2(7) . . . . ? O2 C5 C10 O3 -3.5(9) . . . . ? C11 O3 C10 C9 -65.0(9) . . . . ? C11 O3 C10 C5 121.5(7) . . . . ? C12 N3 C11 C14 0.4(11) . . . . ? Ag2 N3 C11 C14 173.6(5) 4 . . . ? C12 N3 C11 O3 177.4(6) . . . . ? Ag2 N3 C11 O3 -9.4(8) 4 . . . ? C10 O3 C11 N3 161.8(6) . . . . ? C10 O3 C11 C14 -21.3(10) . . . . ? C11 N3 C12 N4 -0.3(12) . . . . ? Ag2 N3 C12 N4 -173.1(6) 4 . . . ? C13 N4 C12 N3 1.8(12) . . . . ? Ag1 N4 C12 N3 -175.0(6) . . . . ? C12 N4 C13 O4 179.9(6) . . . . ? Ag1 N4 C13 O4 -3.8(9) . . . . ? C12 N4 C13 C14 -3.5(11) . . . . ? Ag1 N4 C13 C14 172.8(5) . . . . ? C15 O4 C13 N4 -151.0(6) . . . . ? C15 O4 C13 C14 32.4(9) . . . . ? N3 C11 C14 C13 -1.9(10) . . . . ? O3 C11 C14 C13 -178.4(6) . . . . ? N4 C13 C14 C11 3.5(10) . . . . ? O4 C13 C14 C11 179.8(6) . . . . ? C13 O4 C15 C16 50.7(9) . . . . ? C13 O4 C15 C20 -133.9(7) . . . . ? C20 C15 C16 C17 -0.9(11) . . . . ? O4 C15 C16 C17 174.4(7) . . . . ? C15 C16 C17 C18 1.8(12) . . . . ? C16 C17 C18 C19 -3.3(13) . . . . ? C17 C18 C19 C20 3.9(12) . . . . ? C18 C19 C20 C15 -3.0(11) . . . . ? C18 C19 C20 O5 -172.6(7) . . . . ? C16 C15 C20 C19 1.6(11) . . . . ? O4 C15 C20 C19 -174.0(6) . . . . ? C16 C15 C20 O5 171.7(6) . . . . ? O4 C15 C20 O5 -3.8(10) . . . . ? C22 O5 C20 C19 -59.2(9) . . . . ? C22 O5 C20 C15 131.0(7) . . . . ? C22 N6 C21 N5 -1.7(11) . . . . ? Ag2 N6 C21 N5 179.9(5) 1_565 . . . ? C24 N5 C21 N6 0.2(11) . . . . ? Ag1 N5 C21 N6 168.8(6) 4_544 . . . ? C21 N6 C22 O5 179.3(6) . . . . ? Ag2 N6 C22 O5 -2.4(7) 1_565 . . . ? C21 N6 C22 C23 1.8(10) . . . . ? Ag2 N6 C22 C23 -179.9(5) 1_565 . . . ? C20 O5 C22 N6 162.7(6) . . . . ? C20 O5 C22 C23 -19.9(10) . . . . ? N6 C22 C23 C24 -0.5(9) . . . . ? O5 C22 C23 C24 -177.6(6) . . . . ? C21 N5 C24 O6 -177.0(6) . . . . ? Ag1 N5 C24 O6 15.5(8) 4_544 . . . ? C21 N5 C24 C23 1.2(10) . . . . ? Ag1 N5 C24 C23 -166.2(5) 4_544 . . . ? C30 O6 C24 N5 -165.3(6) . . . . ? C30 O6 C24 C23 16.4(10) . . . . ? C22 C23 C24 N5 -1.1(10) . . . . ? C22 C23 C24 O6 176.9(6) . . . . ? C30 C25 C26 C27 0.0(12) . . . . ? C25 C26 C27 C28 -0.3(12) . . . . ? C26 C27 C28 C29 1.2(12) . . . . ? C27 C28 C29 O1 -175.1(6) . . . . ? C27 C28 C29 C30 -1.8(10) . . . . ? C4 O1 C29 C28 -61.0(9) . . . . ? C4 O1 C29 C30 125.6(7) . . . . ? C26 C25 C30 C29 -0.6(10) . . . . ? C26 C25 C30 O6 174.3(7) . . . . ? C28 C29 C30 C25 1.5(10) . . . . ? O1 C29 C30 C25 175.1(6) . . . . ? C28 C29 C30 O6 -173.7(6) . . . . ? O1 C29 C30 O6 0.0(9) . . . . ? C24 O6 C30 C25 64.1(9) . . . . ? C24 O6 C30 C29 -120.9(7) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C42 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C37 0.0 . . . . ? C38 C37 C42 C41 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.996 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.082