Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_address ; Fujian Inst of Res on the Struct of Matter Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email YYG@FJIRSM.AC.CN _publ_section_title ; Polycatenated 3-connected hydrogen-bonding bilayer stabilized by ligand unsupported Ag...Ag interactions ; loop_ _publ_author_name 'Yuan-Gen Yao' 'Zhao-Ji Li' 'Ye-Yan Qin' 'Yi-Cheng Shen' 'Jian Zhang' data_a _database_code_depnum_ccdc_archive 'CCDC 638295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H8 Ag2 N7 O6' _chemical_formula_sum 'C11 H8 Ag2 N7 O6' _chemical_formula_weight 549.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7478(3) _cell_length_b 10.4917(3) _cell_length_c 11.4993(5) _cell_angle_alpha 64.7370(10) _cell_angle_beta 87.555(2) _cell_angle_gamma 73.999(2) _cell_volume 705.08(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 156 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 25.69 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .5100 _exptl_absorpt_correction_T_max .75100 _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 and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3913 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.69 _reflns_number_total 2589 _reflns_number_gt 2380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+1.7191P] 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 2589 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0281 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.86507(5) 0.20798(3) 0.55328(3) 0.03090(10) Uani 1 1 d . . . Ag2 Ag 0.74231(5) 0.03055(3) 0.43671(3) 0.03071(10) Uani 1 1 d . . . O1 O 0.7914(4) 0.1832(3) 0.8214(2) 0.0297(6) Uani 1 1 d . . . O2 O 0.7232(5) -0.2718(3) 1.0655(2) 0.0364(7) Uani 1 1 d . . . O3 O 0.7255(5) -0.1099(3) 0.6340(2) 0.0308(6) Uani 1 1 d . . . O4 O 0.7689(4) 0.3508(3) 0.3274(2) 0.0297(6) Uani 1 1 d . . . O5 O 0.7470(5) 0.5130(3) -0.1052(2) 0.0368(7) Uani 1 1 d . . . O6 O 0.7424(4) 0.0437(3) 0.1491(2) 0.0298(6) Uani 1 1 d . . . N1 N 1.1269(5) 0.3083(3) 0.5292(3) 0.0258(6) Uani 1 1 d . . . N2 N 0.7614(5) 0.0458(3) 0.7183(3) 0.0209(6) Uani 1 1 d . . . N3 N 0.7477(5) -0.0407(3) 0.9439(3) 0.0255(6) Uani 1 1 d . . . H3B H 0.7426 -0.0233 1.0107 0.031 Uiso 1 1 calc R . . N4 N 0.7366(5) -0.1918(3) 0.8485(3) 0.0231(6) Uani 1 1 d . . . H4A H 0.7352 -0.2758 0.8537 0.028 Uiso 1 1 calc R . . N5 N 0.7594(5) 0.4308(3) 0.1125(3) 0.0255(6) Uani 1 1 d . . . H5A H 0.7632 0.5151 0.1054 0.031 Uiso 1 1 calc R . . N6 N 0.7529(5) 0.2760(3) 0.0217(3) 0.0250(6) Uani 1 1 d . . . H6A H 0.7558 0.2582 -0.0448 0.030 Uiso 1 1 calc R . . N7 N 0.7535(5) 0.1895(3) 0.2472(3) 0.0217(6) Uani 1 1 d . . . C1 C 1.1787(6) 0.3914(4) 0.4142(4) 0.0284(8) Uani 1 1 d . . . H1A H 1.1146 0.3984 0.3408 0.034 Uiso 1 1 calc R . . C2 C 1.3227(6) 0.4678(4) 0.3982(3) 0.0242(7) Uani 1 1 d . . . H2A H 1.3529 0.5247 0.3157 0.029 Uiso 1 1 calc R . . C3 C 1.4229(5) 0.4593(3) 0.5062(3) 0.0191(7) Uani 1 1 d . . . C4 C 1.3680(6) 0.3723(4) 0.6259(3) 0.0246(7) Uani 1 1 d . . . H4B H 1.4296 0.3629 0.7010 0.029 Uiso 1 1 calc R . . C5 C 1.2220(6) 0.2999(4) 0.6332(4) 0.0283(8) Uani 1 1 d . . . H5B H 1.1881 0.2423 0.7143 0.034 Uiso 1 1 calc R . . C6 C 0.7686(5) 0.0686(4) 0.8266(3) 0.0222(7) Uani 1 1 d . . . C7 C 0.7346(6) -0.1748(4) 0.9603(3) 0.0239(7) Uani 1 1 d . . . C8 C 0.7406(5) -0.0821(4) 0.7285(3) 0.0215(7) Uani 1 1 d . . . C9 C 0.7610(5) 0.3228(4) 0.2351(3) 0.0215(7) Uani 1 1 d . . . C10 C 0.7489(5) 0.1626(4) 0.1414(3) 0.0222(7) Uani 1 1 d . . . C11 C 0.7525(6) 0.4139(4) 0.0021(3) 0.0232(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 0.04388(19) 0.02747(16) 0.02820(16) -0.01163(13) 0.01274(13) -0.02254(13) Ag2 0.04669(19) 0.02866(16) 0.01851(15) -0.00690(12) 0.00554(12) -0.01917(13) O1 0.0522(17) 0.0184(12) 0.0233(13) -0.0093(10) 0.0051(12) -0.0172(12) O2 0.070(2) 0.0256(14) 0.0190(13) -0.0084(11) 0.0096(13) -0.0252(14) O3 0.0546(17) 0.0281(13) 0.0185(12) -0.0115(11) 0.0062(12) -0.0230(12) O4 0.0469(16) 0.0268(13) 0.0213(13) -0.0128(11) 0.0024(11) -0.0152(12) O5 0.068(2) 0.0243(14) 0.0205(13) -0.0067(11) 0.0068(13) -0.0226(13) O6 0.0501(16) 0.0193(12) 0.0251(13) -0.0107(11) 0.0029(12) -0.0157(11) N1 0.0323(16) 0.0280(15) 0.0243(15) -0.0124(13) 0.0062(13) -0.0184(13) N2 0.0307(15) 0.0171(13) 0.0167(14) -0.0057(11) 0.0052(11) -0.0125(12) N3 0.0423(18) 0.0206(14) 0.0201(15) -0.0115(12) 0.0052(13) -0.0148(13) N4 0.0388(17) 0.0172(14) 0.0180(14) -0.0082(11) 0.0047(12) -0.0144(12) N5 0.0440(18) 0.0176(14) 0.0198(15) -0.0085(12) 0.0037(13) -0.0155(13) N6 0.0436(18) 0.0198(14) 0.0175(14) -0.0107(12) 0.0034(12) -0.0135(13) N7 0.0316(16) 0.0187(14) 0.0170(14) -0.0072(11) 0.0025(12) -0.0114(12) C1 0.036(2) 0.034(2) 0.0225(18) -0.0128(16) 0.0032(15) -0.0199(17) C2 0.0311(19) 0.0277(18) 0.0167(16) -0.0082(14) 0.0070(14) -0.0159(15) C3 0.0215(16) 0.0137(15) 0.0224(17) -0.0087(13) 0.0016(13) -0.0042(13) C4 0.0284(18) 0.0244(17) 0.0204(17) -0.0068(14) -0.0019(14) -0.0109(14) C5 0.036(2) 0.0304(19) 0.0200(17) -0.0070(15) 0.0053(15) -0.0189(16) C6 0.0279(18) 0.0197(17) 0.0197(16) -0.0081(14) 0.0037(13) -0.0090(14) C7 0.0324(19) 0.0210(17) 0.0198(17) -0.0074(14) 0.0032(14) -0.0122(14) C8 0.0251(17) 0.0214(17) 0.0201(17) -0.0086(14) 0.0055(13) -0.0106(14) C9 0.0245(17) 0.0178(16) 0.0231(17) -0.0085(14) 0.0022(13) -0.0079(13) C10 0.0263(17) 0.0194(17) 0.0207(17) -0.0076(14) 0.0010(13) -0.0082(13) C11 0.0314(18) 0.0193(16) 0.0210(17) -0.0079(14) 0.0035(14) -0.0122(14) _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 2.184(3) . ? Ag1 N1 2.246(3) . ? Ag1 O4 2.387(2) . ? Ag1 Ag2 3.0038(4) . ? Ag1 Ag2 3.0692(5) 2_756 ? Ag2 N7 2.119(3) . ? Ag2 O3 2.133(2) . ? Ag2 Ag1 3.0692(5) 2_756 ? Ag2 Ag2 3.6098(6) 2_756 ? Ag2 Ag2 3.6298(6) 2_656 ? O1 C6 1.230(4) . ? O2 C7 1.220(4) . ? O3 C8 1.254(4) . ? O4 C9 1.223(4) . ? O5 C11 1.222(4) . ? O6 C10 1.225(4) . ? N1 C1 1.333(5) . ? N1 C5 1.339(5) . ? N2 C8 1.343(4) . ? N2 C6 1.370(4) . ? N3 C7 1.365(4) . ? N3 C6 1.381(4) . ? N3 H3B 0.8600 . ? N4 C7 1.370(4) . ? N4 C8 1.374(4) . ? N4 H4A 0.8600 . ? N5 C11 1.360(4) . ? N5 C9 1.379(4) . ? N5 H5A 0.8600 . ? N6 C11 1.364(4) . ? N6 C10 1.389(4) . ? N6 H6A 0.8600 . ? N7 C9 1.360(4) . ? N7 C10 1.365(4) . ? C1 C2 1.380(5) . ? C1 H1A 0.9300 . ? C2 C3 1.397(5) . ? C2 H2A 0.9300 . ? C3 C4 1.392(5) . ? C3 C3 1.485(6) 2_866 ? C4 C5 1.380(5) . ? C4 H4B 0.9300 . ? C5 H5B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 133.55(11) . . ? N2 Ag1 O4 138.14(10) . . ? N1 Ag1 O4 88.30(10) . . ? N2 Ag1 Ag2 77.77(7) . . ? N1 Ag1 Ag2 133.85(8) . . ? O4 Ag1 Ag2 69.12(6) . . ? N2 Ag1 Ag2 90.30(8) . 2_756 ? N1 Ag1 Ag2 74.09(8) . 2_756 ? O4 Ag1 Ag2 103.22(7) . 2_756 ? Ag2 Ag1 Ag2 72.930(12) . 2_756 ? N7 Ag2 O3 173.54(10) . . ? N7 Ag2 Ag1 91.66(8) . . ? O3 Ag2 Ag1 82.44(7) . . ? N7 Ag2 Ag1 97.90(8) . 2_756 ? O3 Ag2 Ag1 86.40(8) . 2_756 ? Ag1 Ag2 Ag1 107.070(11) . 2_756 ? N7 Ag2 Ag2 98.11(8) . 2_756 ? O3 Ag2 Ag2 80.62(8) . 2_756 ? Ag1 Ag2 Ag2 54.369(9) . 2_756 ? Ag1 Ag2 Ag2 52.701(10) 2_756 2_756 ? N7 Ag2 Ag2 121.90(8) . 2_656 ? O3 Ag2 Ag2 57.97(8) . 2_656 ? Ag1 Ag2 Ag2 106.635(13) . 2_656 ? Ag1 Ag2 Ag2 125.959(13) 2_756 2_656 ? Ag2 Ag2 Ag2 137.518(16) 2_756 2_656 ? C8 O3 Ag2 126.1(2) . . ? C9 O4 Ag1 135.0(2) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Ag1 122.9(2) . . ? C5 N1 Ag1 119.5(2) . . ? C8 N2 C6 119.9(3) . . ? C8 N2 Ag1 126.5(2) . . ? C6 N2 Ag1 111.8(2) . . ? C7 N3 C6 124.1(3) . . ? C7 N3 H3B 118.0 . . ? C6 N3 H3B 118.0 . . ? C7 N4 C8 123.7(3) . . ? C7 N4 H4A 118.2 . . ? C8 N4 H4A 118.2 . . ? C11 N5 C9 124.8(3) . . ? C11 N5 H5A 117.6 . . ? C9 N5 H5A 117.6 . . ? C11 N6 C10 124.6(3) . . ? C11 N6 H6A 117.7 . . ? C10 N6 H6A 117.7 . . ? C9 N7 C10 121.0(3) . . ? C9 N7 Ag2 116.5(2) . . ? C10 N7 Ag2 122.5(2) . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 116.3(3) . . ? C4 C3 C3 121.8(4) . 2_866 ? C2 C3 C3 121.8(4) . 2_866 ? C5 C4 C3 120.1(3) . . ? C5 C4 H4B 120.0 . . ? C3 C4 H4B 120.0 . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5B 118.4 . . ? C4 C5 H5B 118.4 . . ? O1 C6 N2 121.8(3) . . ? O1 C6 N3 119.9(3) . . ? N2 C6 N3 118.3(3) . . ? O2 C7 N3 123.0(3) . . ? O2 C7 N4 122.7(3) . . ? N3 C7 N4 114.2(3) . . ? O3 C8 N2 123.9(3) . . ? O3 C8 N4 116.5(3) . . ? N2 C8 N4 119.5(3) . . ? O4 C9 N7 123.1(3) . . ? O4 C9 N5 118.9(3) . . ? N7 C9 N5 118.0(3) . . ? O6 C10 N7 122.5(3) . . ? O6 C10 N6 120.0(3) . . ? N7 C10 N6 117.4(3) . . ? O5 C11 N5 123.1(3) . . ? O5 C11 N6 122.9(3) . . ? N5 C11 N6 114.0(3) . . ? 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 N4 H4A O5 0.86 2.04 2.891(4) 171.3 1_546 N3 H3B O6 0.86 2.00 2.849(4) 171.6 1_556 N6 H6A O1 0.86 1.98 2.836(4) 170.3 1_554 N5 H5A O2 0.86 2.02 2.871(4) 169.1 1_564 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.812 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.090