# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- p1 and 1.cif' _audit_update_record ; 2010-03-06 # Formatted by publCIF ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Huang, Rongbin State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; _publ_contact_author_phone 86-592-2185191 _publ_contact_author_fax 86-592-2183047 _publ_contact_author_email rbhuang@xmu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) # 3. TITLE AND AUTHOR LIST _publ_section_title ; An unprecedented (4, 24)-connected metal-organic framework sustained by nanosized Ag12 cuboctahedral nodes ; loop_ _publ_author_name _publ_author_address 'Di Sun' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; 'Yun-Hua Li' ; Insitute of Materials Physical Chemistry, Huaqiao University, Quanzhou, Fujian 362021, China ; 'Rong-Bin Huang' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; 'Lan-Sun Zheng' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; _publ_section_exptl_refinement ; All H atoms were placed geometrically with C---H distances of 0.93 \%A, N---H distances of 0.86\%A and refined using a riding atom model with their isotropic displacement factors, J~iso~ fixed at 1.2 time the U~eq~ of the parent C and N atom. ; _publ_contact_author_name 'Huang, Rongbin' data_p1 _database_code_depnum_ccdc_archive 'CCDC 843436' #TrackingRef '- p1 and 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H16 Ag2 N8 O7' _chemical_formula_sum 'C7 H16 Ag2 N8 O7' _chemical_formula_weight 540.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 trigonal _symmetry_space_group_name_H-M 'R -3 m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 22.274(3) _cell_length_b 22.274(3) _cell_length_c 16.940(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7279(2) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5860 _cell_measurement_theta_min 6.08 _cell_measurement_theta_max 54.91 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 2.446 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 0.8099 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _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 11659 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1551 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+37.9459P] 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 SHELXL _refine_ls_extinction_coef 0.000226(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1551 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 0.088697(8) 0.177394(16) 0.698303(18) 0.02078(13) Uani 1 2 d S . . Ag2 Ag 0.277164(14) 0.277164(14) 1.0000 0.01923(12) Uani 1 2 d S . . C1 C 0.31550(13) 0.41857(13) 1.09322(14) 0.0150(5) Uani 1 1 d . . . C2 C 0.3333 0.4629(2) 1.1667 0.0349(11) Uani 1 2 d S . . H2A H 0.2947 0.4691 1.1790 0.042 Uiso 1 1 d R . . C3 C 0.17743(13) 0.25166(13) 0.84663(13) 0.0132(5) Uani 1 1 d . . . C4 C 0.13913(10) 0.2783(2) 0.9593(2) 0.0169(8) Uani 1 2 d S . . C5 C -0.03437(10) 0.03437(10) 0.6460(2) 0.0148(7) Uani 1 2 d S . . N1 N 0.12024(8) 0.24047(16) 0.80625(17) 0.0144(6) Uani 1 2 d S . . N2 N 0.18843(11) 0.26975(12) 0.92371(12) 0.0158(5) Uani 1 1 d . . . N3 N 0.22577(12) 0.24458(12) 0.80855(13) 0.0184(5) Uani 1 1 d . . . H3A H 0.2641 0.2516 0.8342 0.022 Uiso 1 1 d R . . H3B H 0.2201 0.2328 0.7571 0.022 Uiso 1 1 d R . . N4 N 0.14830(11) 0.2966(2) 1.03468(19) 0.0270(8) Uani 1 2 d S . . H4A H 0.1864 0.3027 1.0603 0.032 Uiso 1 1 d R . . N5 N 0.03585(8) 0.07170(16) 0.64600(18) 0.0153(6) Uani 1 2 d S . . N6 N -0.06875(8) 0.06875(8) 0.6463(2) 0.0192(7) Uani 1 2 d S . . H6A H -0.0454 0.1154 0.6465 0.023 Uiso 1 1 d R . . O1 O 0.32803(10) 0.44931(10) 1.02791(10) 0.0195(4) Uani 1 1 d . . . O2 O 0.28698(11) 0.35426(10) 1.10192(11) 0.0254(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01804(15) 0.02229(19) 0.02342(19) -0.01140(11) -0.00570(6) 0.01115(10) Ag2 0.02357(16) 0.02357(16) 0.01637(18) 0.00149(5) -0.00149(5) 0.01615(14) C1 0.0154(13) 0.0181(14) 0.0149(12) -0.0001(10) -0.0037(10) 0.0110(11) C2 0.071(4) 0.0308(16) 0.0160(19) -0.0037(10) -0.007(2) 0.0357(18) C3 0.0153(13) 0.0139(13) 0.0117(12) 0.0000(9) 0.0003(10) 0.0081(11) C4 0.0179(14) 0.0189(19) 0.0141(17) -0.0013(14) -0.0006(7) 0.0095(10) C5 0.0151(13) 0.0151(13) 0.0146(17) 0.0012(7) -0.0012(7) 0.0078(16) N1 0.0142(11) 0.0165(16) 0.0133(14) -0.0017(12) -0.0009(6) 0.0082(8) N2 0.0158(11) 0.0204(12) 0.0134(10) -0.0025(9) -0.0025(8) 0.0106(10) N3 0.0174(12) 0.0297(13) 0.0121(10) -0.0046(9) -0.0019(9) 0.0148(10) N4 0.0247(13) 0.053(2) 0.0128(15) -0.0108(16) -0.0054(8) 0.0265(12) N5 0.0134(11) 0.0136(16) 0.0189(15) 0.0002(12) 0.0001(6) 0.0068(8) N6 0.0109(11) 0.0109(11) 0.0359(18) 0.0011(7) -0.0011(7) 0.0056(13) O1 0.0281(11) 0.0190(10) 0.0128(8) 0.0009(7) -0.0027(8) 0.0129(9) O2 0.0342(12) 0.0133(10) 0.0214(10) -0.0008(8) -0.0106(8) 0.0064(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.197(3) . y Ag1 N5 2.223(3) . y Ag2 N2 2.297(2) . y Ag2 N2 2.297(2) 4_557 y Ag2 O2 2.367(2) . y Ag2 O2 2.367(2) 4_557 y C1 O2 1.252(3) . ? C1 O1 1.257(3) . ? C1 C2 1.513(3) . ? C2 C1 1.513(3) 12_557 ? C2 H2A 0.9597 . ? C3 N3 1.330(3) . ? C3 N2 1.352(3) . ? C3 N1 1.355(3) . ? C4 N4 1.325(5) . ? C4 N2 1.347(3) . ? C4 N2 1.347(3) 23 ? C5 N6 1.326(5) . ? C5 N5 1.355(2) . ? C5 N5 1.355(2) 2 ? N1 C3 1.355(3) 23 ? N3 H3A 0.8999 . ? N3 H3B 0.9001 . ? N4 H4A 0.9009 . ? N5 C5 1.355(2) 3 ? N6 H6A 0.9007 . ? 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 N5 147.13(11) . . y N2 Ag2 N2 124.44(11) . 4_557 y N2 Ag2 O2 103.10(7) . . y N2 Ag2 O2 98.89(7) 4_557 . y N2 Ag2 O2 98.89(7) . 4_557 y N2 Ag2 O2 103.10(7) 4_557 4_557 y O2 Ag2 O2 131.72(11) . 4_557 y O2 C1 O1 125.0(2) . . ? O2 C1 C2 117.9(2) . . ? O1 C1 C2 117.0(2) . . ? C1 C2 C1 117.1(3) 12_557 . ? C1 C2 H2A 107.8 12_557 . ? C1 C2 H2A 108.2 . . ? N3 C3 N2 117.8(2) . . ? N3 C3 N1 118.4(2) . . ? N2 C3 N1 123.8(2) . . ? N4 C4 N2 117.64(16) . . ? N4 C4 N2 117.64(16) . 23 ? N2 C4 N2 124.7(3) . 23 ? N6 C5 N5 117.91(18) . . ? N6 C5 N5 117.91(18) . 2 ? N5 C5 N5 124.2(4) . 2 ? C3 N1 C3 116.1(3) 23 . ? C3 N1 Ag1 120.57(15) 23 . ? C3 N1 Ag1 120.57(15) . . ? C4 N2 C3 115.8(2) . . ? C4 N2 Ag2 118.09(18) . . ? C3 N2 Ag2 125.87(17) . . ? C3 N3 H3A 120.0 . . ? C3 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C4 N4 H4A 119.9 . . ? C5 N5 C5 115.8(4) 3 . ? C5 N5 Ag1 119.17(19) 3 . ? C5 N5 Ag1 119.17(19) . . ? C5 N6 H6A 120.0 . . ? C1 O2 Ag2 123.66(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O2 0.90 2.06 2.946(3) 168.4 4_557 N3 H3B O1 0.90 2.03 2.924(3) 173.7 17_556 N4 H4A O2 0.90 2.06 2.919(3) 157.9 . N6 H6A O1 0.90 1.97 2.870(3) 176.1 31_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.656 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.087 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.052 -0.055 -0.006 2033 265 ' ' _platon_squeeze_details ; ; #===================================== data_p1'-dehydration _database_code_depnum_ccdc_archive 'CCDC 843435' #TrackingRef '- p1 and 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H10 Ag2 N8 O4' _chemical_formula_weight 485.97 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 22.1713(16) _cell_length_b 22.1713(16) _cell_length_c 16.947(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7214.6(13) _cell_formula_units_Z 18 _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 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 2.468 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7993 _exptl_absorpt_correction_T_max 0.8084 _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 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _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 12124 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1547 _reflns_number_gt 1515 _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^)+(0.0413P)^2^+48.1251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000132(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1547 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.243078(11) 0.48616(2) -0.02800(2) 0.03517(17) Uani 1 2 d S . . Ag2 Ag 0.27741(2) 0.27741(2) 0.0000 0.03561(17) Uani 1 2 d S . . C1 C 0.25035(18) 0.17663(17) 0.15372(18) 0.0247(7) Uani 1 1 d . . . C2 C 0.2763(3) 0.13813(14) 0.0417(3) 0.0299(11) Uani 1 2 d S . . C3 C 0.31387(19) 0.41731(18) 0.0938(2) 0.0286(8) Uani 1 1 d . . . C4 C 0.3333 0.4619(3) 0.1667 0.072(3) Uani 1 2 d S . . H4A H 0.2948 0.4684 0.1801 0.087 Uiso 1 1 d R . . C5 C 0.2644(3) 0.63220(13) 0.0179(3) 0.0273(10) Uani 1 2 d S . . N1 N 0.24421(17) 0.22545(16) 0.19207(18) 0.0334(7) Uani 1 1 d . . . H1A H 0.2517 0.2642 0.1665 0.040 Uiso 1 1 d R . . H1B H 0.2325 0.2199 0.2435 0.040 Uiso 1 1 d R . . N2 N 0.26792(16) 0.18761(15) 0.07698(16) 0.0289(6) Uani 1 1 d . . . N3 N 0.2391(2) 0.11957(11) 0.1939(2) 0.0252(8) Uani 1 2 d S . . N4 N 0.29755(11) 0.5951(2) 0.0181(2) 0.0270(9) Uani 1 2 d S . . N5 N 0.1961(2) 0.59803(11) 0.0182(3) 0.0349(10) Uani 1 2 d S . . H5A H 0.1726 0.5509 0.0185 0.042 Uiso 1 1 d R . . N6 N 0.2940(3) 0.14702(16) -0.0339(3) 0.0488(14) Uani 1 2 d S . . H6A H 0.3002 0.1855 -0.0595 0.059 Uiso 1 1 d R . . O1 O 0.32525(15) 0.44788(14) 0.02942(15) 0.0374(6) Uani 1 1 d . . . O2 O 0.28578(16) 0.35354(14) 0.10260(16) 0.0428(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0332(2) 0.0386(3) 0.0355(3) -0.01568(17) -0.00784(8) 0.01932(13) Ag2 0.0444(2) 0.0444(2) 0.0275(2) 0.00226(8) -0.00226(8) 0.0293(2) C1 0.0282(17) 0.0278(17) 0.0200(16) 0.0012(13) 0.0012(13) 0.0153(15) C2 0.039(3) 0.0312(19) 0.022(2) 0.0025(10) 0.005(2) 0.0197(14) C3 0.0363(19) 0.0311(19) 0.0252(18) -0.0034(15) -0.0084(15) 0.0220(16) C4 0.159(9) 0.061(3) 0.030(3) -0.014(2) -0.028(4) 0.079(4) C5 0.028(3) 0.0290(18) 0.025(2) 0.0010(10) 0.002(2) 0.0140(13) N1 0.054(2) 0.0301(16) 0.0254(15) 0.0044(13) 0.0078(14) 0.0278(15) N2 0.0399(17) 0.0298(15) 0.0221(14) 0.0036(12) 0.0053(12) 0.0213(14) N3 0.032(2) 0.0262(15) 0.0197(19) 0.0021(8) 0.0043(16) 0.0158(11) N4 0.0254(15) 0.025(2) 0.031(2) 0.0004(17) 0.0002(8) 0.0125(11) N5 0.022(2) 0.0250(16) 0.057(3) 0.0024(10) 0.005(2) 0.0108(11) N6 0.092(4) 0.0466(19) 0.023(2) 0.0105(13) 0.021(3) 0.046(2) O1 0.0548(17) 0.0356(14) 0.0248(13) 0.0007(11) -0.0054(12) 0.0248(13) O2 0.0567(18) 0.0313(15) 0.0331(14) -0.0006(11) -0.0137(13) 0.0165(13) _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 N3 2.198(4) 15_554 ? Ag1 N4 2.233(4) . ? Ag1 O1 2.556(3) . ? Ag1 O1 2.556(3) 23 ? Ag2 N2 2.300(3) 4 ? Ag2 N2 2.300(3) . ? Ag2 O2 2.365(3) 4 ? Ag2 O2 2.365(3) . ? C1 N1 1.327(4) . ? C1 N2 1.344(4) . ? C1 N3 1.346(4) . ? C2 N6 1.325(7) . ? C2 N2 1.341(4) 24 ? C2 N2 1.341(4) . ? C3 O2 1.236(4) . ? C3 O1 1.242(4) . ? C3 C4 1.504(5) . ? C4 C3 1.504(5) 12 ? C4 H4A 0.9599 . ? C5 N5 1.312(7) . ? C5 N4 1.350(3) 3_565 ? C5 N4 1.350(3) . ? N1 H1A 0.9001 . ? N1 H1B 0.9001 . ? N3 C1 1.346(4) 24 ? N3 Ag1 2.198(4) 8 ? N4 C5 1.350(3) 2_665 ? N5 H5A 0.9046 . ? N6 H6A 0.9038 . ? 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 N3 Ag1 N4 141.30(15) 15_554 . ? N3 Ag1 O1 100.35(8) 15_554 . ? N4 Ag1 O1 97.82(8) . . ? N3 Ag1 O1 100.36(8) 15_554 23 ? N4 Ag1 O1 97.82(8) . 23 ? O1 Ag1 O1 123.01(12) . 23 ? N2 Ag2 N2 122.83(16) 4 . ? N2 Ag2 O2 98.13(10) 4 4 ? N2 Ag2 O2 103.75(10) . 4 ? N2 Ag2 O2 103.75(10) 4 . ? N2 Ag2 O2 98.13(10) . . ? O2 Ag2 O2 133.33(15) 4 . ? N1 C1 N2 117.7(3) . . ? N1 C1 N3 118.2(3) . . ? N2 C1 N3 124.1(3) . . ? N6 C2 N2 117.5(2) . 24 ? N6 C2 N2 117.5(2) . . ? N2 C2 N2 125.0(4) 24 . ? O2 C3 O1 125.3(3) . . ? O2 C3 C4 117.9(3) . . ? O1 C3 C4 116.7(3) . . ? C3 C4 C3 118.1(5) 12 . ? C3 C4 H4A 107.6 12 . ? C3 C4 H4A 107.9 . . ? N5 C5 N4 118.1(2) . 3_565 ? N5 C5 N4 118.1(2) . . ? N4 C5 N4 123.7(5) 3_565 . ? C1 N1 H1A 119.8 . . ? C1 N1 H1B 120.2 . . ? H1A N1 H1B 120.0 . . ? C2 N2 C1 115.4(3) . . ? C2 N2 Ag2 117.7(2) . . ? C1 N2 Ag2 126.7(2) . . ? C1 N3 C1 115.8(4) 24 . ? C1 N3 Ag1 121.1(2) 24 8 ? C1 N3 Ag1 121.1(2) . 8 ? C5 N4 C5 116.3(5) 2_665 . ? C5 N4 Ag1 119.6(3) 2_665 . ? C5 N4 Ag1 119.6(3) . . ? C5 N5 H5A 119.8 . . ? C2 N6 H6A 119.9 . . ? C3 O1 Ag1 122.1(2) . . ? C3 O2 Ag2 122.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.576 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.112