# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;A New Infinite Inorganic [n]Catenane From Silver and Bis(2-methylimidazolyl)methane Ligand ; _publ_contact_author_name 'Prof. Chuan-Ming Jin' _publ_contact_author_email JINCM1999@YAHOO.COM loop_ _publ_author_name 'Chuan-Ming Jin' 'Jing Huang' 'Huan Lu' 'Ling-Yan Wu' # Attachment '613418.cif' data_051210cm _database_code_depnum_ccdc_archive 'CCDC 613418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Ag4 N20 O15' _chemical_formula_weight 1432.42 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 20.913(2) _cell_length_b 14.8336(15) _cell_length_c 18.2903(19) _cell_angle_alpha 90.00 _cell_angle_beta 118.808(2) _cell_angle_gamma 90.00 _cell_volume 4971.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 5993 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 21.85 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 1.638 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6392 _exptl_absorpt_correction_T_max 0.7353 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23676 _diffrn_reflns_av_R_equivalents 0.1191 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4483 _reflns_number_gt 2790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4483 _refine_ls_number_parameters 366 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2341 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.016 _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 0.69786(6) 0.5000 0.93718(6) 0.1312(5) Uani 1 2 d S . . Ag2 Ag 0.5000 0.87708(8) 0.5000 0.1881(9) Uani 1 2 d S . . Ag3 Ag 0.5000 0.63062(6) 0.5000 0.1131(4) Uani 1 2 d S . . Ag4 Ag 0.61766(7) 1.0000 0.18220(7) 0.1378(5) Uani 1 2 d S . . C1 C 0.7447(5) 0.6764(8) 0.8484(6) 0.133(3) Uani 1 1 d . . . H1A H 0.7855 0.6405 0.8861 0.199 Uiso 1 1 calc R . . H1B H 0.7620 0.7317 0.8369 0.199 Uiso 1 1 calc R . . H1C H 0.7167 0.6438 0.7974 0.199 Uiso 1 1 calc R . . C2 C 0.6967(4) 0.6975(5) 0.8879(4) 0.0874(17) Uani 1 1 d . . . C3 C 0.6414(4) 0.6854(6) 0.9581(4) 0.0955(19) Uani 1 1 d . . . H3 H 0.6216 0.6604 0.9894 0.115 Uiso 1 1 calc R . . C4 C 0.6338(4) 0.7675(6) 0.9346(5) 0.0948(19) Uani 1 1 d . . . H4 H 0.6097 0.8124 0.9473 0.114 Uiso 1 1 calc R . . C5 C 0.6688(5) 0.8618(5) 0.8457(5) 0.101(2) Uani 1 1 d . . . H5A H 0.6684 0.9126 0.8789 0.121 Uiso 1 1 calc R . . H5B H 0.7134 0.8649 0.8419 0.121 Uiso 1 1 calc R . . C6 C 0.6675(9) 0.8437(12) 0.6740(9) 0.204(7) Uani 1 1 d . . . H6A H 0.6583 0.8680 0.6211 0.306 Uiso 1 1 calc R . . H6B H 0.6752 0.7798 0.6746 0.306 Uiso 1 1 calc R . . H6C H 0.7102 0.8717 0.7178 0.306 Uiso 1 1 calc R . . C7 C 0.6044(8) 0.8616(6) 0.6868(6) 0.128(3) Uani 1 1 d . . . C8 C 0.5359(6) 0.8786(7) 0.7468(6) 0.134(4) Uani 1 1 d . . . H8 H 0.5189 0.8798 0.7853 0.161 Uiso 1 1 calc R . . C9 C 0.4979(8) 0.8863(7) 0.6665(6) 0.153(5) Uani 1 1 d . . . H9 H 0.4481 0.8985 0.6380 0.184 Uiso 1 1 calc R . . C10 C 0.6499(6) 0.6625(14) 0.4700(6) 0.215(8) Uani 1 1 d . . . H10A H 0.6461 0.7157 0.4975 0.323 Uiso 1 1 calc R . . H10B H 0.6871 0.6710 0.4541 0.323 Uiso 1 1 calc R . . H10C H 0.6624 0.6120 0.5072 0.323 Uiso 1 1 calc R . . C11 C 0.5799(4) 0.6453(6) 0.3954(4) 0.097(2) Uani 1 1 d . . . C12 C 0.4661(5) 0.6240(6) 0.3135(6) 0.117(3) Uani 1 1 d . . . H12 H 0.4165 0.6159 0.2947 0.141 Uiso 1 1 calc R . . C13 C 0.4957(5) 0.6262(6) 0.2654(5) 0.114(3) Uani 1 1 d . . . H13 H 0.4719 0.6211 0.2076 0.137 Uiso 1 1 calc R . . C14 C 0.6264(6) 0.6433(8) 0.2908(6) 0.142(4) Uani 1 1 d . . . H14A H 0.6739 0.6471 0.3401 0.171 Uiso 1 1 calc R . . H14B H 0.6254 0.5892 0.2605 0.171 Uiso 1 1 calc R . . C15 C 0.6885(7) 0.8331(12) 0.3462(6) 0.191(6) Uani 1 1 d . . . H15A H 0.7195 0.8819 0.3483 0.287 Uiso 1 1 calc R . . H15B H 0.7177 0.7809 0.3724 0.287 Uiso 1 1 calc R . . H15C H 0.6622 0.8501 0.3749 0.287 Uiso 1 1 calc R . . C16 C 0.6356(5) 0.8119(11) 0.2572(5) 0.129(4) Uani 1 1 d . . . C17 C 0.5691(5) 0.8027(10) 0.1229(5) 0.134(4) Uani 1 1 d . . . H17 H 0.5456 0.8213 0.0675 0.160 Uiso 1 1 calc R . . C18 C 0.5687(6) 0.7213(9) 0.1481(5) 0.132(3) Uani 1 1 d . . . H18 H 0.5435 0.6720 0.1154 0.158 Uiso 1 1 calc R . . N1 N 0.6829(4) 0.6388(4) 0.9305(4) 0.0998(18) Uani 1 1 d . . . N2 N 0.6677(3) 0.7773(4) 0.8872(3) 0.0842(14) Uani 1 1 d . . . N3 N 0.6067(4) 0.8681(3) 0.7630(3) 0.0927(17) Uani 1 1 d . . . N4 N 0.5397(6) 0.8745(4) 0.6292(4) 0.135(3) Uani 1 1 d . . . N5 N 0.5173(3) 0.6350(4) 0.3952(4) 0.0957(17) Uani 1 1 d . . . N6 N 0.5687(4) 0.6374(4) 0.3163(4) 0.1009(18) Uani 1 1 d . . . N7 N 0.6154(5) 0.7226(8) 0.2377(5) 0.130(3) Uani 1 1 d . . . N8 N 0.6105(4) 0.8591(6) 0.1918(5) 0.122(2) Uani 1 1 d . . . N9 N 0.6609(5) 0.5000 0.1222(7) 0.116(3) Uani 1 2 d SDU . . N10 N 0.6903(6) 1.0000 0.5292(7) 0.123(3) Uani 1 2 d SDU . . N11 N 0.3346(10) 0.5000 0.3468(12) 0.143(4) Uani 1 2 d SU . . N12 N 0.5983(5) 1.0000 0.9849(5) 0.081(2) Uani 1 2 d S . . O1 O 0.6810(12) 0.5000 0.1966(9) 0.318(12) Uani 1 2 d SDU . . O2 O 0.7053(8) 0.5000 0.0979(9) 0.199(5) Uani 1 2 d SDU . . O3 O 0.5961(7) 0.5000 0.0729(14) 0.47(2) Uani 1 2 d SDU . . O4 O 0.7522(6) 1.0000 0.5833(8) 0.177(4) Uani 1 2 d SDU . . O5 O 0.6240(7) 1.0000 0.4925(12) 0.234(7) Uani 1 2 d SDU . . O6 O 0.6783(8) 0.9194(6) 0.5104(7) 0.223(5) Uani 1 1 d DU . . O7 O 0.3849(9) 0.5000 0.4149(10) 0.194(5) Uani 1 2 d SU . . O8 O 0.2883(11) 0.5000 0.2785(13) 0.218(6) Uani 1 2 d SU . . O9 O 0.3335(9) 0.4044(11) 0.3505(8) 0.241(5) Uani 1 1 d U . . O13 O 0.4795(9) 0.5000 0.0870(9) 0.207(6) Uani 1 2 d S . . O11 O 0.6109(15) 1.0000 0.9351(11) 0.280(13) Uani 1 2 d S . . O12 O 0.6030(13) 0.9488(8) 1.0269(9) 0.330(11) 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 0.1342(8) 0.0886(6) 0.1006(7) 0.000 0.0007(6) 0.000 Ag2 0.336(2) 0.1278(9) 0.0614(6) 0.000 0.0651(9) 0.000 Ag3 0.1358(8) 0.1309(8) 0.1080(7) 0.000 0.0870(6) 0.000 Ag4 0.1358(9) 0.1868(11) 0.1308(9) 0.000 0.0961(8) 0.000 C1 0.125(7) 0.170(8) 0.114(6) -0.033(6) 0.066(6) 0.017(6) C2 0.086(4) 0.098(5) 0.061(3) -0.010(3) 0.022(3) -0.006(4) C3 0.097(5) 0.105(5) 0.083(4) 0.007(4) 0.043(4) 0.003(4) C4 0.093(5) 0.118(6) 0.080(4) 0.001(4) 0.047(4) 0.003(4) C5 0.120(6) 0.096(5) 0.083(5) -0.011(3) 0.045(4) -0.026(4) C6 0.239(16) 0.297(17) 0.155(11) -0.016(11) 0.158(12) -0.067(13) C7 0.204(11) 0.110(6) 0.079(6) -0.006(4) 0.076(7) -0.027(6) C8 0.136(8) 0.166(9) 0.091(6) 0.014(5) 0.046(5) 0.062(6) C9 0.184(11) 0.184(10) 0.067(5) 0.008(5) 0.040(6) 0.066(8) C10 0.116(7) 0.46(3) 0.062(5) 0.063(9) 0.035(5) 0.026(11) C11 0.078(4) 0.148(6) 0.062(4) 0.016(4) 0.032(3) 0.021(4) C12 0.102(6) 0.153(8) 0.089(6) 0.016(5) 0.040(5) -0.029(5) C13 0.121(7) 0.135(7) 0.066(4) 0.009(4) 0.029(5) -0.023(5) C14 0.140(7) 0.226(10) 0.090(5) 0.056(6) 0.078(6) 0.086(7) C15 0.131(8) 0.329(18) 0.076(6) -0.022(8) 0.020(6) -0.021(10) C16 0.084(5) 0.232(13) 0.075(5) -0.012(7) 0.041(4) 0.008(7) C17 0.097(6) 0.232(12) 0.055(4) 0.011(6) 0.023(4) -0.017(6) C18 0.128(7) 0.205(10) 0.065(5) 0.008(6) 0.047(5) -0.014(7) N1 0.095(4) 0.095(4) 0.078(4) 0.002(3) 0.017(3) -0.001(3) N2 0.097(4) 0.087(3) 0.064(3) -0.010(2) 0.035(3) -0.002(3) N3 0.128(5) 0.089(3) 0.057(3) -0.004(2) 0.041(3) -0.010(3) N4 0.215(9) 0.103(5) 0.051(4) 0.004(3) 0.036(5) 0.009(5) N5 0.089(4) 0.127(5) 0.071(4) 0.008(3) 0.038(3) 0.007(3) N6 0.107(5) 0.138(5) 0.064(3) 0.024(3) 0.046(3) 0.021(4) N7 0.120(5) 0.207(9) 0.086(5) 0.009(5) 0.069(4) 0.018(6) N8 0.109(5) 0.183(7) 0.096(5) 0.026(5) 0.067(5) 0.001(5) N9 0.094(5) 0.131(6) 0.114(6) 0.000 0.044(5) 0.000 N10 0.129(7) 0.154(7) 0.105(6) 0.000 0.072(6) 0.000 N11 0.141(8) 0.186(9) 0.136(8) 0.000 0.093(7) 0.000 N12 0.118(6) 0.080(5) 0.060(4) 0.000 0.056(4) 0.000 O1 0.34(2) 0.37(2) 0.272(17) 0.000 0.170(15) 0.000 O2 0.223(12) 0.229(12) 0.192(10) 0.000 0.138(10) 0.000 O3 0.45(3) 0.46(3) 0.48(3) 0.000 0.21(2) 0.000 O4 0.120(7) 0.204(10) 0.152(8) 0.000 0.023(7) 0.000 O5 0.225(10) 0.251(11) 0.225(10) 0.000 0.108(8) 0.000 O6 0.251(11) 0.274(11) 0.173(8) -0.033(8) 0.125(8) -0.049(9) O7 0.191(11) 0.226(12) 0.154(10) 0.000 0.074(9) 0.000 O8 0.202(12) 0.226(12) 0.205(13) 0.000 0.082(11) 0.000 O9 0.291(13) 0.278(11) 0.193(10) 0.007(9) 0.149(9) 0.003(10) O13 0.204(13) 0.272(17) 0.175(12) 0.000 0.115(11) 0.000 O11 0.64(4) 0.117(8) 0.260(18) 0.000 0.35(3) 0.000 O12 0.63(4) 0.223(12) 0.253(13) 0.077(9) 0.31(2) 0.136(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 N1 2.077(6) . ? Ag1 N1 2.077(6) 6_565 ? Ag2 N4 2.095(7) 2_656 ? Ag2 N4 2.095(7) . ? Ag3 N5 2.116(6) . ? Ag3 N5 2.116(6) 2_656 ? Ag4 N8 2.109(8) . ? Ag4 N8 2.109(8) 6_575 ? C1 C2 1.524(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.289(10) . ? C2 N2 1.327(9) . ? C3 C4 1.276(10) . ? C3 N1 1.383(10) . ? C3 H3 0.9300 . ? C4 N2 1.366(9) . ? C4 H4 0.9300 . ? C5 N3 1.445(10) . ? C5 N2 1.472(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.472(19) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N4 1.265(14) . ? C7 N3 1.373(10) . ? C8 C9 1.296(13) . ? C8 N3 1.372(13) . ? C8 H8 0.9300 . ? C9 N4 1.355(16) . ? C9 H9 0.9300 . ? C10 C11 1.464(13) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N5 1.316(9) . ? C11 N6 1.354(9) . ? C12 C13 1.296(14) . ? C12 N5 1.366(11) . ? C12 H12 0.9300 . ? C13 N6 1.361(11) . ? C13 H13 0.9300 . ? C14 N7 1.470(13) . ? C14 N6 1.492(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.495(13) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N8 1.261(13) . ? C16 N7 1.383(15) . ? C17 C18 1.295(15) . ? C17 N8 1.409(13) . ? C17 H17 0.9300 . ? C18 N7 1.448(12) . ? C18 H18 0.9300 . ? N9 O2 1.208(7) . ? N9 O3 1.213(8) . ? N9 O1 1.215(8) . ? N10 O4 1.192(8) . ? N10 O5 1.215(9) . ? N10 O6 1.235(8) 6_575 ? N10 O6 1.235(8) . ? N11 O8 1.15(2) . ? N11 O7 1.181(19) . ? N11 O9 1.421(16) 6_565 ? N11 O9 1.421(16) . ? N12 O12 1.050(11) . ? N12 O12 1.050(11) 6_575 ? N12 O11 1.063(12) . ? O5 O6 1.570(16) 6_575 ? O12 O12 1.52(2) 6_575 ? 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 164.8(4) . 6_565 ? N4 Ag2 N4 177.9(4) 2_656 . ? N5 Ag3 N5 176.5(3) . 2_656 ? N8 Ag4 N8 164.7(4) . 6_575 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 111.9(7) . . ? N1 C2 C1 122.5(8) . . ? N2 C2 C1 125.5(8) . . ? C4 C3 N1 110.6(7) . . ? C4 C3 H3 124.7 . . ? N1 C3 H3 124.7 . . ? C3 C4 N2 107.3(7) . . ? C3 C4 H4 126.4 . . ? N2 C4 H4 126.4 . . ? N3 C5 N2 111.4(5) . . ? N3 C5 H5A 109.4 . . ? N2 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? N2 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 N3 109.6(11) . . ? N4 C7 C6 125.1(10) . . ? N3 C7 C6 125.3(12) . . ? C9 C8 N3 105.3(11) . . ? C9 C8 H8 127.3 . . ? N3 C8 H8 127.3 . . ? C8 C9 N4 111.4(11) . . ? C8 C9 H9 124.3 . . ? N4 C9 H9 124.3 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 N6 109.0(6) . . ? N5 C11 C10 124.7(7) . . ? N6 C11 C10 126.3(8) . . ? C13 C12 N5 111.1(8) . . ? C13 C12 H12 124.4 . . ? N5 C12 H12 124.4 . . ? C12 C13 N6 106.5(8) . . ? C12 C13 H13 126.8 . . ? N6 C13 H13 126.8 . . ? N7 C14 N6 111.2(6) . . ? N7 C14 H14A 109.4 . . ? N6 C14 H14A 109.4 . . ? N7 C14 H14B 109.4 . . ? N6 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 N7 110.6(9) . . ? N8 C16 C15 131.8(15) . . ? N7 C16 C15 117.1(12) . . ? C18 C17 N8 110.0(8) . . ? C18 C17 H17 125.0 . . ? N8 C17 H17 125.0 . . ? C17 C18 N7 105.9(10) . . ? C17 C18 H18 127.1 . . ? N7 C18 H18 127.1 . . ? C2 N1 C3 104.2(6) . . ? C2 N1 Ag1 129.3(6) . . ? C3 N1 Ag1 125.2(6) . . ? C2 N2 C4 105.9(6) . . ? C2 N2 C5 130.1(6) . . ? C4 N2 C5 124.0(6) . . ? C8 N3 C7 106.3(8) . . ? C8 N3 C5 124.4(7) . . ? C7 N3 C5 129.2(9) . . ? C7 N4 C9 106.9(8) . . ? C7 N4 Ag2 128.7(9) . . ? C9 N4 Ag2 124.3(8) . . ? C11 N5 C12 105.7(7) . . ? C11 N5 Ag3 127.2(5) . . ? C12 N5 Ag3 127.0(6) . . ? C11 N6 C13 107.6(7) . . ? C11 N6 C14 125.4(7) . . ? C13 N6 C14 127.0(7) . . ? C16 N7 C18 105.1(9) . . ? C16 N7 C14 131.6(9) . . ? C18 N7 C14 122.8(11) . . ? C16 N8 C17 108.3(10) . . ? C16 N8 Ag4 128.0(9) . . ? C17 N8 Ag4 123.4(7) . . ? O2 N9 O3 120.4(9) . . ? O2 N9 O1 120.0(9) . . ? O3 N9 O1 119.6(9) . . ? O4 N10 O5 162.3(16) . . ? O4 N10 O6 103.0(9) . 6_575 ? O5 N10 O6 79.7(9) . 6_575 ? O4 N10 O6 103.0(9) . . ? O5 N10 O6 79.7(9) . . ? O6 N10 O6 150.6(17) 6_575 . ? O8 N11 O7 176.0(18) . . ? O8 N11 O9 91.6(11) . 6_565 ? O7 N11 O9 88.7(11) . 6_565 ? O8 N11 O9 91.6(11) . . ? O7 N11 O9 88.7(11) . . ? O9 N11 O9 173.4(15) 6_565 . ? O12 N12 O12 92.7(15) . 6_575 ? O12 N12 O11 130.6(10) . . ? O12 N12 O11 130.6(10) 6_575 . ? N10 O5 O6 50.7(5) . 6_575 ? N12 O12 O12 43.7(7) . 6_575 ? 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 C3 C4 N2 2.6(8) . . . . ? N3 C8 C9 N4 4.7(13) . . . . ? N5 C12 C13 N6 1.1(10) . . . . ? N8 C17 C18 N7 -3.3(11) . . . . ? N2 C2 N1 C3 0.5(8) . . . . ? C1 C2 N1 C3 177.2(7) . . . . ? N2 C2 N1 Ag1 168.3(4) . . . . ? C1 C2 N1 Ag1 -15.0(10) . . . . ? C4 C3 N1 C2 -2.0(8) . . . . ? C4 C3 N1 Ag1 -170.4(5) . . . . ? N1 Ag1 N1 C2 -117.2(15) 6_565 . . . ? N1 Ag1 N1 C3 48.3(18) 6_565 . . . ? N1 C2 N2 C4 1.0(7) . . . . ? C1 C2 N2 C4 -175.6(7) . . . . ? N1 C2 N2 C5 -178.8(6) . . . . ? C1 C2 N2 C5 4.5(11) . . . . ? C3 C4 N2 C2 -2.2(8) . . . . ? C3 C4 N2 C5 177.7(6) . . . . ? N3 C5 N2 C2 90.7(9) . . . . ? N3 C5 N2 C4 -89.1(8) . . . . ? C9 C8 N3 C7 -5.8(11) . . . . ? C9 C8 N3 C5 176.5(7) . . . . ? N4 C7 N3 C8 5.0(10) . . . . ? C6 C7 N3 C8 -175.7(11) . . . . ? N4 C7 N3 C5 -177.4(7) . . . . ? C6 C7 N3 C5 1.9(14) . . . . ? N2 C5 N3 C8 68.5(10) . . . . ? N2 C5 N3 C7 -108.7(8) . . . . ? N3 C7 N4 C9 -2.2(10) . . . . ? C6 C7 N4 C9 178.6(11) . . . . ? N3 C7 N4 Ag2 178.2(5) . . . . ? C6 C7 N4 Ag2 -1.0(15) . . . . ? C8 C9 N4 C7 -1.7(13) . . . . ? C8 C9 N4 Ag2 177.9(7) . . . . ? N4 Ag2 N4 C7 79.7(8) 2_656 . . . ? N4 Ag2 N4 C9 -99.8(8) 2_656 . . . ? N6 C11 N5 C12 -2.3(9) . . . . ? C10 C11 N5 C12 177.7(12) . . . . ? N6 C11 N5 Ag3 175.2(5) . . . . ? C10 C11 N5 Ag3 -4.8(15) . . . . ? C13 C12 N5 C11 0.8(10) . . . . ? C13 C12 N5 Ag3 -176.7(6) . . . . ? N5 Ag3 N5 C11 82.9(7) 2_656 . . . ? N5 Ag3 N5 C12 -100.1(7) 2_656 . . . ? N5 C11 N6 C13 3.0(9) . . . . ? C10 C11 N6 C13 -177.0(12) . . . . ? N5 C11 N6 C14 -178.9(8) . . . . ? C10 C11 N6 C14 1.0(15) . . . . ? C12 C13 N6 C11 -2.5(9) . . . . ? C12 C13 N6 C14 179.5(8) . . . . ? N7 C14 N6 C11 -114.7(9) . . . . ? N7 C14 N6 C13 63.0(13) . . . . ? N8 C16 N7 C18 -3.5(10) . . . . ? C15 C16 N7 C18 -176.3(9) . . . . ? N8 C16 N7 C14 -175.3(8) . . . . ? C15 C16 N7 C14 11.9(14) . . . . ? C17 C18 N7 C16 4.1(10) . . . . ? C17 C18 N7 C14 176.8(8) . . . . ? N6 C14 N7 C16 84.1(12) . . . . ? N6 C14 N7 C18 -86.4(11) . . . . ? N7 C16 N8 C17 1.6(10) . . . . ? C15 C16 N8 C17 173.0(11) . . . . ? N7 C16 N8 Ag4 176.0(5) . . . . ? C15 C16 N8 Ag4 -12.6(15) . . . . ? C18 C17 N8 C16 1.2(11) . . . . ? C18 C17 N8 Ag4 -173.5(7) . . . . ? N8 Ag4 N8 C16 -59(2) 6_575 . . . ? N8 Ag4 N8 C17 115.2(16) 6_575 . . . ? O4 N10 O5 O6 100.5(7) . . . 6_575 ? O6 N10 O5 O6 -158.9(14) . . . 6_575 ? O11 N12 O12 O12 154(4) . . . 6_575 ? 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 C1 H1A O12 0.96 2.48 3.43(2) 173.5 7_667 C1 H1C O8 0.96 2.52 3.342(15) 143.7 2_656 C1 H1C O9 0.96 2.49 3.409(17) 160.4 5_666 C5 H5B O2 0.97 2.51 3.095(14) 118.4 4_656 C10 H10C O9 0.96 2.57 3.283(15) 131.0 5_666 C12 H12 O9 0.93 2.42 3.185(18) 139.5 6_565 C15 H15A O9 0.96 2.39 3.18(2) 139.0 3 C17 H17 O12 0.93 2.54 3.080(18) 117.6 1_554 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.012 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.141 # Attachment '614245.cif' data_bt739 _database_code_depnum_ccdc_archive 'CCDC 614245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Bis(imidazolium)AgNO3.H2O)n _chemical_melting_point ? _chemical_formula_moiety 'C7 H8 Ag N4, N O3, H2 O' _chemical_formula_sum 'C7 H10 Ag N5 O4' _chemical_formula_weight 336.07 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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2469(4) _cell_length_b 7.9889(4) _cell_length_c 16.3187(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.750(1) _cell_angle_gamma 90.00 _cell_volume 1065.32(9) _cell_formula_units_Z 4 _cell_measurement_temperature 87(2) _cell_measurement_reflns_used 8159 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.29 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6175 _exptl_absorpt_correction_T_max 0.8782 _exptl_absorpt_process_details 'SADABS; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 87(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11833 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.30 _reflns_number_total 1939 _reflns_number_gt 1819 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45a' _computing_data_reduction 'Bruker SAINT+ v. 6.45a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0293P)^2^+0.7005P] 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 1939 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _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 0.511502(19) 0.260896(18) 0.516369(9) 0.01706(8) Uani 1 1 d . . . C1 C 0.6887(2) 0.0556(2) 0.39169(12) 0.0154(4) Uani 1 1 d . . . H1 H 0.7825 0.0338 0.4308 0.018 Uiso 1 1 calc R . . C3 C 0.4543(2) 0.1467(2) 0.33425(12) 0.0159(4) Uani 1 1 d . . . H3 H 0.3518 0.2028 0.3266 0.019 Uiso 1 1 calc R . . C4 C 0.5159(2) 0.0550(2) 0.27605(12) 0.0146(4) Uani 1 1 d . . . H4 H 0.4663 0.0341 0.2210 0.018 Uiso 1 1 calc R . . C6 C 0.7795(2) -0.1055(2) 0.27440(12) 0.0152(4) Uani 1 1 d . . . H6A H 0.7165 -0.1830 0.2348 0.018 Uiso 1 1 calc R . . H6B H 0.8459 -0.1736 0.3172 0.018 Uiso 1 1 calc R . . C8 C 1.0376(2) 0.0601(2) 0.26470(12) 0.0151(4) Uani 1 1 d . . . H8 H 1.0903 0.0466 0.3198 0.018 Uiso 1 1 calc R . . C9 C 1.0933(2) 0.1471(2) 0.20308(12) 0.0152(4) Uani 1 1 d . . . H9 H 1.1938 0.2066 0.2079 0.018 Uiso 1 1 calc R . . C11 C 0.8602(2) 0.0433(2) 0.15093(12) 0.0142(4) Uani 1 1 d . . . H11 H 0.7660 0.0143 0.1134 0.017 Uiso 1 1 calc R . . N1 N 0.6102(2) 0.1710(2) -0.06254(11) 0.0184(4) Uani 1 1 d . . . N2 N 0.5629(2) 0.1465(2) 0.40663(10) 0.0149(3) Uani 1 1 d . . . N5 N 0.6667(2) -0.00234(19) 0.31336(10) 0.0128(3) Uani 1 1 d . . . N7 N 0.8879(2) -0.00509(19) 0.23088(10) 0.0132(3) Uani 1 1 d . . . N10 N 0.9816(2) 0.1362(2) 0.13214(10) 0.0141(3) Uani 1 1 d . . . O1 O 0.46541(17) 0.1365(2) -0.08889(10) 0.0264(4) Uani 1 1 d . . . O2 O 0.72249(19) 0.0738(2) -0.07617(11) 0.0310(4) Uani 1 1 d . . . O3 O 0.6436(2) 0.3026(2) -0.02380(12) 0.0374(4) Uani 1 1 d . . . O4 O 0.3967(2) 0.26803(18) 0.09093(11) 0.0266(4) Uani 1 1 d . . . H1A H 0.3657 0.1610 0.0865 0.039 Uiso 1 1 d . . . H2A H 0.4479 0.2952 0.0475 0.058 Uiso 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 0.01800(12) 0.02195(11) 0.01149(12) -0.00225(5) 0.00294(7) -0.00179(6) C1 0.0140(10) 0.0174(9) 0.0138(10) 0.0035(8) -0.0011(8) -0.0011(8) C3 0.0115(9) 0.0192(10) 0.0160(10) 0.0008(8) -0.0012(8) -0.0002(8) C4 0.0114(10) 0.0189(10) 0.0127(9) -0.0002(8) -0.0016(8) -0.0001(8) C6 0.0151(10) 0.0128(9) 0.0185(11) 0.0014(7) 0.0047(8) 0.0004(7) C8 0.0122(9) 0.0176(9) 0.0149(10) 0.0005(8) -0.0008(8) -0.0002(8) C9 0.0112(9) 0.0184(10) 0.0156(10) 0.0005(8) 0.0005(8) -0.0007(8) C11 0.0121(10) 0.0156(9) 0.0147(9) -0.0035(8) 0.0010(8) 0.0018(8) N1 0.0171(9) 0.0224(9) 0.0157(9) -0.0011(7) 0.0022(7) -0.0039(7) N2 0.0150(8) 0.0169(8) 0.0129(8) 0.0005(7) 0.0020(7) -0.0012(7) N5 0.0121(8) 0.0134(8) 0.0127(8) 0.0011(7) 0.0008(6) -0.0005(6) N7 0.0114(8) 0.0133(8) 0.0148(8) -0.0006(7) 0.0014(6) 0.0009(6) N10 0.0139(8) 0.0179(8) 0.0103(8) -0.0003(6) 0.0013(6) 0.0024(7) O1 0.0129(7) 0.0357(9) 0.0290(9) -0.0052(7) -0.0030(6) -0.0040(6) O2 0.0189(8) 0.0274(9) 0.0480(11) -0.0046(7) 0.0096(7) 0.0006(7) O3 0.0354(10) 0.0316(9) 0.0448(12) -0.0203(9) 0.0039(9) -0.0118(8) O4 0.0343(10) 0.0254(8) 0.0204(9) -0.0033(6) 0.0052(8) -0.0017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.1038(16) . ? Ag1 N10 2.1050(16) 4_566 ? C1 N2 1.316(3) . ? C1 N5 1.349(3) . ? C1 H1 0.9500 . ? C3 C4 1.352(3) . ? C3 N2 1.383(3) . ? C3 H3 0.9500 . ? C4 N5 1.386(3) . ? C4 H4 0.9500 . ? C6 N5 1.452(2) . ? C6 N7 1.455(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.352(3) . ? C8 N7 1.385(3) . ? C8 H8 0.9500 . ? C9 N10 1.381(3) . ? C9 H9 0.9500 . ? C11 N10 1.316(3) . ? C11 N7 1.350(3) . ? C11 H11 0.9500 . ? N1 O3 1.238(3) . ? N1 O1 1.245(2) . ? N1 O2 1.251(2) . ? N10 Ag1 2.1050(16) 4_665 ? O4 H1A 0.8928 . ? O4 H2A 0.8989 . ? 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 N10 174.23(6) . 4_566 ? N2 C1 N5 110.86(17) . . ? N2 C1 H1 124.6 . . ? N5 C1 H1 124.6 . . ? C4 C3 N2 109.77(17) . . ? C4 C3 H3 125.1 . . ? N2 C3 H3 125.1 . . ? C3 C4 N5 105.68(17) . . ? C3 C4 H4 127.2 . . ? N5 C4 H4 127.2 . . ? N5 C6 N7 111.91(16) . . ? N5 C6 H6A 109.2 . . ? N7 C6 H6A 109.2 . . ? N5 C6 H6B 109.2 . . ? N7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C9 C8 N7 105.71(17) . . ? C9 C8 H8 127.1 . . ? N7 C8 H8 127.1 . . ? C8 C9 N10 109.64(17) . . ? C8 C9 H9 125.2 . . ? N10 C9 H9 125.2 . . ? N10 C11 N7 110.59(17) . . ? N10 C11 H11 124.7 . . ? N7 C11 H11 124.7 . . ? O3 N1 O1 120.08(18) . . ? O3 N1 O2 119.95(18) . . ? O1 N1 O2 119.96(18) . . ? C1 N2 C3 106.15(16) . . ? C1 N2 Ag1 130.68(14) . . ? C3 N2 Ag1 123.03(13) . . ? C1 N5 C4 107.54(16) . . ? C1 N5 C6 126.67(16) . . ? C4 N5 C6 125.79(16) . . ? C11 N7 C8 107.64(16) . . ? C11 N7 C6 126.47(17) . . ? C8 N7 C6 125.89(16) . . ? C11 N10 C9 106.41(16) . . ? C11 N10 Ag1 127.91(14) . 4_665 ? C9 N10 Ag1 125.60(13) . 4_665 ? H1A O4 H2A 109.0 . . ? 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 O4 H1A O2 0.89 2.01 2.902(2) 175.5 3_655 O4 H1A N1 0.89 2.69 3.538(2) 158.4 3_655 O4 H2A O3 0.90 2.11 2.959(3) 156.2 . O4 H2A N1 0.90 2.58 3.341(3) 143.1 . O4 H2A O1 0.90 2.58 3.238(2) 130.4 . C1 H1 O3 0.95 2.42 3.137(3) 132.5 2_645 C6 H6B O4 0.99 2.47 3.376(3) 151.6 2_645 C11 H11 O1 0.95 2.25 3.092(2) 147.8 3_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.547 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.073