# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jonathan Steed' 'Peter Byrne' 'Nigel Clarke' 'Gareth O Lloyd' _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_section_title ; Anion Hydrogen Bond Control in the Formation of Planar or Quintuple Helical Coordination Polymers ; # Attachment 'BF4.CIF' data_BF4.CIF _database_code_depnum_ccdc_archive 'CCDC 684397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'AgBF4 Helix' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H26 Ag B F4 N6 O3' _chemical_formula_weight 581.14 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 15.4790(17) _cell_length_b 7.3940(8) _cell_length_c 21.154(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.132(4) _cell_angle_gamma 90.00 _cell_volume 2407.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 0.8919 _exptl_absorpt_process_details ? _exptl_special_details ; The structures was determined twice but all samples proved to be twinned and the problems with poor R factor and residual peaks near the Ag atom stem from this issue. Space group P21 was also investigated since the reflections for the n-glide absence are weakly observed. The R value proved better in P21 but the refinement was poorly behaved and the disorder impossible to model. We concluded that the P21/n solution is probably correct. The BF4 is disordered and the disorder correlated to whether the O1S site is a thf molecule or a water molecule. Occupancy refined to 50 % each and then fixed. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22311 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4204 _reflns_number_gt 3735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (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^)+(0.0000P)^2^+96.3287P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4204 _refine_ls_number_parameters 351 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.1264 _refine_ls_wR_factor_ref 0.2973 _refine_ls_wR_factor_gt 0.2940 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.213 _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 0.12987(7) 0.21555(16) 0.04426(6) 0.0386(4) Uani 1 1 d . . . F1 F 0.6701(7) -0.5362(18) 0.1084(6) 0.077(4) Uani 1 1 d U . . O1 O 0.2335(7) -0.4574(17) 0.1063(6) 0.057(4) Uani 1 1 d . . . N1 N 0.2390(7) 0.0632(18) 0.0227(6) 0.038(3) Uani 1 1 d . . . C1 C 0.2947(10) 0.145(3) -0.0141(10) 0.059(5) Uani 1 1 d . . . H1 H 0.2833 0.2644 -0.0291 0.071 Uiso 1 1 calc R . . B1 B 0.578(3) -0.530(7) 0.118(2) 0.050(11) Uiso 0.50 1 d P A 1 F2 F 0.5409(16) -0.365(4) 0.1051(17) 0.083(8) Uani 0.50 1 d PU A 1 O2 O 0.4141(7) -1.6040(14) 0.3840(6) 0.047(3) Uani 1 1 d . . . N2 N 0.3564(9) -0.3637(18) 0.0629(7) 0.046(3) Uani 1 1 d . . . H2 H 0.4065 -0.4062 0.0534 0.055 Uiso 1 1 calc R . . C2 C 0.3671(13) 0.055(3) -0.0296(12) 0.089(9) Uani 1 1 d . . . H2A H 0.4032 0.1061 -0.0585 0.107 Uiso 1 1 calc R . . F3 F 0.574(3) -0.556(7) 0.1885(17) 0.072(12) Uani 0.50 1 d PU A 1 N3 N 0.3603(9) -0.6087(18) 0.1323(6) 0.044(3) Uani 1 1 d . . . H3 H 0.4160 -0.6111 0.1271 0.053 Uiso 1 1 calc R . . C3 C 0.3862(9) -0.113(3) -0.0018(9) 0.058(5) Uani 1 1 d . . . H3A H 0.4377 -0.1747 -0.0100 0.069 Uiso 1 1 calc R . . F4 F 0.5248(16) -0.665(5) 0.0949(18) 0.123(12) Uani 0.50 1 d PU A 1 N4 N 0.4694(9) -1.4809(17) 0.2973(6) 0.042(3) Uani 1 1 d . . . H4 H 0.5128 -1.4840 0.2736 0.051 Uiso 1 1 calc R . . C4 C 0.3308(10) -0.192(2) 0.0376(8) 0.044(4) Uani 1 1 d . . . N5 N 0.5388(9) -1.7232(19) 0.3528(7) 0.054(4) Uani 1 1 d . . . H5 H 0.5841 -1.6937 0.3331 0.065 Uiso 1 1 calc R . . C5 C 0.2565(10) -0.103(2) 0.0470(7) 0.038(4) Uani 1 1 d . . . H5A H 0.2157 -0.1596 0.0711 0.045 Uiso 1 1 calc R . . N6 N 0.4819(8) -2.1367(16) 0.4350(5) 0.034(3) Uani 1 1 d . . . C6 C 0.3093(12) -0.473(2) 0.1015(7) 0.044(4) Uani 1 1 d . . . C7 C 0.3269(11) -0.7482(19) 0.1729(8) 0.043(4) Uani 1 1 d . . . H7A H 0.2733 -0.8017 0.1508 0.052 Uiso 1 1 calc R . . H7B H 0.3121 -0.6924 0.2129 0.052 Uiso 1 1 calc R . . C8 C 0.3930(10) -0.893(2) 0.1877(7) 0.039(4) Uani 1 1 d . . . H8A H 0.4458 -0.8387 0.2108 0.047 Uiso 1 1 calc R . . H8B H 0.4094 -0.9439 0.1474 0.047 Uiso 1 1 calc R . . C9 C 0.3614(10) -1.0457(19) 0.2278(7) 0.034(3) Uani 1 1 d . . . H9A H 0.3101 -1.1041 0.2043 0.041 Uiso 1 1 calc R . . H9B H 0.3435 -0.9955 0.2677 0.041 Uiso 1 1 calc R . . C10 C 0.4328(11) -1.187(2) 0.2434(8) 0.044(4) Uani 1 1 d . . . H10A H 0.4518 -1.2341 0.2033 0.053 Uiso 1 1 calc R . . H10B H 0.4834 -1.1289 0.2677 0.053 Uiso 1 1 calc R . . C11 C 0.4020(10) -1.347(2) 0.2824(7) 0.040(4) Uani 1 1 d . . . H11A H 0.3829 -1.3000 0.3225 0.048 Uiso 1 1 calc R . . H11B H 0.3514 -1.4052 0.2580 0.048 Uiso 1 1 calc R . . C12 C 0.4697(11) -1.6035(19) 0.3462(8) 0.040(4) Uani 1 1 d . . . C13 C 0.5455(9) -1.8839(19) 0.3866(7) 0.034(3) Uani 1 1 d . . . C14 C 0.6264(10) -1.969(2) 0.3995(8) 0.042(4) Uani 1 1 d . . . H14 H 0.6770 -1.9106 0.3877 0.050 Uiso 1 1 calc R . . C15 C 0.6335(10) -2.132(3) 0.4287(8) 0.051(4) Uani 1 1 d . . . H15 H 0.6887 -2.1890 0.4364 0.062 Uiso 1 1 calc R . . C16 C 0.5617(11) -2.215(2) 0.4471(7) 0.048(4) Uani 1 1 d . . . H16 H 0.5672 -2.3285 0.4683 0.058 Uiso 1 1 calc R . . C17 C 0.4755(9) -1.9731(18) 0.4059(7) 0.030(3) Uani 1 1 d . . . H17 H 0.4199 -1.9180 0.3985 0.035 Uiso 1 1 calc R . . F2A F 0.5498(16) -0.444(4) 0.0655(13) 0.078(8) Uani 0.50 1 d PU A 2 F3A F 0.561(3) -0.586(7) 0.163(2) 0.096(16) Uani 0.50 1 d PU A 2 F4A F 0.625(2) -0.302(4) 0.1615(14) 0.109(10) Uani 0.50 1 d PU A 2 O1S O 0.6968(12) -1.625(3) 0.3063(10) 0.116(7) Uani 1 1 d U . . C1S C 0.735(4) -1.756(8) 0.264(3) 0.100(17) Uani 0.50 1 d PU . . H1S1 H 0.6954 -1.7791 0.2246 0.120 Uiso 0.50 1 calc PR . . H1S2 H 0.7503 -1.8715 0.2854 0.120 Uiso 0.50 1 calc PR . . C2S C 0.816(3) -1.654(9) 0.249(3) 0.11(2) Uani 0.50 1 d PU . . H2S1 H 0.8645 -1.7402 0.2483 0.138 Uiso 0.50 1 calc PR . . H2S2 H 0.8048 -1.5998 0.2058 0.138 Uiso 0.50 1 calc PR . . C3S C 0.841(3) -1.509(7) 0.295(2) 0.090(15) Uani 0.50 1 d PU . . H3S1 H 0.8699 -1.4071 0.2752 0.108 Uiso 0.50 1 calc PR . . H3S2 H 0.8802 -1.5549 0.3318 0.108 Uiso 0.50 1 calc PR . . C4S C 0.749(3) -1.453(6) 0.315(3) 0.095(16) Uani 0.50 1 d PU . . H4S1 H 0.7539 -1.4121 0.3598 0.114 Uiso 0.50 1 calc PR . . H4S2 H 0.7228 -1.3556 0.2873 0.114 Uiso 0.50 1 calc PR . . B1A B 0.601(4) -0.463(9) 0.131(3) 0.066(14) Uiso 0.50 1 d P A 2 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 0.0358(6) 0.0330(6) 0.0462(7) 0.0036(5) 0.0008(5) -0.0066(5) F1 0.059(7) 0.090(9) 0.089(8) -0.005(7) 0.038(6) -0.001(7) O1 0.017(5) 0.063(8) 0.091(9) 0.033(7) -0.002(5) -0.005(5) N1 0.018(6) 0.047(8) 0.049(8) 0.009(6) 0.001(5) -0.008(5) C1 0.026(8) 0.056(11) 0.098(15) 0.039(11) 0.019(9) 0.011(8) F2 0.047(13) 0.066(16) 0.14(2) 0.034(16) 0.024(15) 0.025(12) O2 0.051(7) 0.033(6) 0.061(7) 0.005(5) 0.027(6) 0.010(5) N2 0.040(8) 0.039(8) 0.061(9) 0.013(7) 0.018(6) 0.007(6) C2 0.038(11) 0.100(18) 0.13(2) 0.070(17) 0.016(12) -0.002(12) F3 0.046(19) 0.10(2) 0.07(2) -0.004(18) 0.042(17) 0.028(16) N3 0.038(7) 0.042(8) 0.053(8) 0.008(7) 0.008(6) 0.002(6) C3 0.012(7) 0.072(13) 0.091(14) 0.037(11) 0.015(8) 0.005(7) F4 0.048(13) 0.15(3) 0.18(3) -0.08(2) 0.061(17) -0.015(16) N4 0.042(7) 0.034(7) 0.051(8) 0.004(6) 0.010(6) 0.003(6) C4 0.038(8) 0.034(9) 0.056(10) 0.015(8) -0.006(7) -0.010(7) N5 0.046(8) 0.038(8) 0.077(10) 0.017(8) 0.002(7) 0.005(7) C5 0.034(8) 0.028(8) 0.048(9) 0.008(7) -0.009(7) -0.013(6) N6 0.041(7) 0.026(6) 0.034(7) -0.004(5) -0.001(5) 0.001(5) C6 0.059(11) 0.026(8) 0.041(9) 0.008(7) -0.012(8) -0.003(7) C7 0.056(10) 0.023(8) 0.049(9) 0.007(7) -0.002(7) -0.008(7) C8 0.047(9) 0.029(8) 0.042(9) 0.004(7) 0.004(7) 0.002(7) C9 0.038(8) 0.023(7) 0.042(8) 0.000(6) 0.001(6) 0.005(6) C10 0.058(10) 0.025(8) 0.049(9) 0.003(7) -0.006(8) 0.005(7) C11 0.045(9) 0.028(8) 0.046(9) -0.002(7) 0.004(7) 0.004(7) C12 0.049(9) 0.020(7) 0.050(9) 0.000(7) 0.002(8) -0.006(7) C13 0.030(7) 0.023(7) 0.049(9) -0.007(6) 0.003(6) 0.005(6) C14 0.035(8) 0.040(9) 0.049(9) 0.003(7) -0.001(7) 0.010(7) C15 0.028(8) 0.065(12) 0.061(11) 0.012(9) 0.001(7) 0.018(8) C16 0.060(10) 0.038(9) 0.045(9) 0.004(8) -0.006(8) 0.016(9) C17 0.027(7) 0.023(7) 0.037(8) 0.000(6) -0.003(6) 0.000(6) F2A 0.054(14) 0.10(2) 0.084(17) 0.022(15) 0.033(13) 0.038(14) F3A 0.047(16) 0.14(3) 0.11(3) 0.05(3) 0.03(2) -0.016(19) F4A 0.16(3) 0.082(19) 0.099(19) 0.022(16) 0.051(19) 0.018(19) O1S 0.094(13) 0.114(15) 0.148(17) 0.022(13) 0.046(12) 0.009(12) C1S 0.12(3) 0.09(3) 0.10(3) -0.02(3) 0.02(3) 0.02(3) C2S 0.07(3) 0.15(4) 0.13(3) 0.08(3) 0.05(3) -0.02(3) C3S 0.11(3) 0.09(3) 0.09(3) -0.01(2) 0.06(3) -0.01(3) C4S 0.09(3) 0.07(3) 0.13(3) 0.02(3) 0.02(3) -0.05(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.120(13) . ? Ag1 N6 2.131(12) 2_575 ? F1 B1 1.46(5) . ? F1 B1A 1.34(6) . ? O1 C6 1.19(2) . ? N1 C5 1.348(19) . ? N1 C1 1.363(19) . ? C1 C2 1.37(3) . ? B1 F2 1.36(5) . ? B1 F3 1.51(6) . ? B1 F4 1.35(6) . ? O2 C12 1.237(19) . ? N2 C6 1.41(2) . ? N2 C4 1.42(2) . ? C2 C3 1.39(3) . ? N3 C6 1.396(19) . ? N3 C7 1.471(19) . ? C3 C4 1.39(2) . ? N4 C12 1.375(19) . ? N4 C11 1.449(19) . ? C4 C5 1.36(2) . ? N5 C12 1.38(2) . ? N5 C13 1.385(19) . ? N6 C17 1.357(18) . ? N6 C16 1.364(19) . ? N6 Ag1 2.131(12) 2_525 ? C7 C8 1.49(2) . ? C8 C9 1.52(2) . ? C9 C10 1.53(2) . ? C10 C11 1.54(2) . ? C13 C17 1.37(2) . ? C13 C14 1.40(2) . ? C14 C15 1.36(2) . ? C15 C16 1.36(2) . ? F2A B1A 1.54(6) . ? F3A B1A 1.31(7) . ? F4A B1A 1.39(7) . ? O1S C4S 1.51(4) . ? O1S C1S 1.49(5) . ? C1S C2S 1.52(7) . ? C2S C3S 1.48(7) . ? C3S C4S 1.58(7) . ? 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 N6 178.6(5) . 2_575 ? B1 F1 B1A 27(3) . . ? C5 N1 C1 120.5(14) . . ? C5 N1 Ag1 122.4(10) . . ? C1 N1 Ag1 117.0(11) . . ? N1 C1 C2 120.3(17) . . ? F2 B1 F1 113(4) . . ? F2 B1 F3 105(4) . . ? F1 B1 F3 106(3) . . ? F2 B1 F4 111(4) . . ? F1 B1 F4 120(4) . . ? F3 B1 F4 100(4) . . ? C6 N2 C4 126.2(14) . . ? C1 C2 C3 118.2(18) . . ? C6 N3 C7 124.1(14) . . ? C2 C3 C4 120.7(17) . . ? C12 N4 C11 124.0(13) . . ? C5 C4 C3 118.3(15) . . ? C5 C4 N2 125.8(14) . . ? C3 C4 N2 115.9(15) . . ? C12 N5 C13 127.9(14) . . ? N1 C5 C4 121.6(14) . . ? C17 N6 C16 119.1(14) . . ? C17 N6 Ag1 121.9(10) . 2_525 ? C16 N6 Ag1 118.8(11) . 2_525 ? O1 C6 N3 122.7(15) . . ? O1 C6 N2 124.8(14) . . ? N3 C6 N2 112.5(15) . . ? N3 C7 C8 110.5(13) . . ? C7 C8 C9 113.3(13) . . ? C8 C9 C10 111.0(13) . . ? C11 C10 C9 112.4(13) . . ? N4 C11 C10 112.5(13) . . ? O2 C12 N4 122.8(15) . . ? O2 C12 N5 121.1(15) . . ? N4 C12 N5 116.0(15) . . ? C17 C13 N5 123.4(13) . . ? C17 C13 C14 116.5(14) . . ? N5 C13 C14 120.0(14) . . ? C15 C14 C13 121.0(16) . . ? C16 C15 C14 120.1(15) . . ? C15 C16 N6 120.3(15) . . ? N6 C17 C13 122.9(13) . . ? C4S O1S C1S 112(3) . . ? O1S C1S C2S 101(4) . . ? C3S C2S C1S 113(4) . . ? C2S C3S C4S 100(4) . . ? O1S C4S C3S 104(4) . . ? F4A B1A F3A 119(5) . . ? F4A B1A F1 109(5) . . ? F3A B1A F1 110(5) . . ? F4A B1A F2A 115(4) . . ? F3A B1A F2A 107(5) . . ? F1 B1A F2A 93(4) . . ? 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 N2 H2 F2A 0.88 2.22 3.05(3) 155.9 . N2 H2 F2 0.88 2.26 2.90(3) 129.0 . N3 H3 F4 0.88 1.92 2.78(3) 162.5 . N3 H3 F3A 0.88 2.30 3.11(5) 153.2 . N4 H4 F3 0.88 2.19 3.01(4) 154.1 1_545 N5 H5 O1S 0.88 1.96 2.83(2) 168.6 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.996 _refine_diff_density_min -4.332 _refine_diff_density_rms 0.203 # Attachment 'NO3.CIF' data_NO3.CIF _database_code_depnum_ccdc_archive 'CCDC 684398' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NO3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H29.50 Ag N8 O6.75' _chemical_formula_weight 585.88 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 34.975(3) _cell_length_b 12.5607(11) _cell_length_c 5.7537(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2527.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7726 _exptl_absorpt_correction_T_max 0.8902 _exptl_absorpt_process_details ? _exptl_special_details ; There is a strange disorder of water molecule O7 with two sites of occupancy approximately 50 % and 25 %. ; _diffrn_ambient_temperature 120(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 SMART6000 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14617 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5580 _reflns_number_gt 4842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (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^)+(0.0557P)^2^+0.2571P] 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 -0.03(3) _refine_ls_number_reflns 5580 _refine_ls_number_parameters 334 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.130313(7) 0.59275(2) 0.14403(8) 0.03438(9) Uani 1 1 d . . . O1 O 0.04410(7) 0.2256(2) -0.6907(5) 0.0351(6) Uani 1 1 d . . . N1 N 0.08930(8) 0.5072(2) -0.0673(5) 0.0304(6) Uani 1 1 d . . . C1 C 0.05298(10) 0.4950(3) 0.0054(7) 0.0324(8) Uani 1 1 d . . . H1 H 0.0447 0.5324 0.1399 0.039 Uiso 1 1 calc R . . O2 O 0.13640(7) -0.2181(2) -2.0732(5) 0.0320(6) Uani 1 1 d . . . N2 N 0.09246(8) 0.3386(2) -0.5778(5) 0.0295(7) Uani 1 1 d . . . H2 H 0.1155 0.3604 -0.6172 0.035 Uiso 1 1 calc R . . C2 C 0.02727(10) 0.4297(3) -0.1097(7) 0.0334(8) Uani 1 1 d . . . H2A H 0.0019 0.4220 -0.0526 0.040 Uiso 1 1 calc R . . O3 O 0.19032(8) 0.4279(3) -0.1795(5) 0.0468(8) Uani 1 1 d . . . N3 N 0.10111(8) 0.2249(2) -0.8775(7) 0.0320(7) Uani 1 1 d . . . H3 H 0.1243 0.2518 -0.8800 0.038 Uiso 1 1 calc R . . C3 C 0.03859(10) 0.3757(3) -0.3087(6) 0.0299(9) Uani 1 1 d . . . H3A H 0.0212 0.3317 -0.3915 0.036 Uiso 1 1 calc R . . O4 O 0.25119(8) 0.4283(2) -0.1180(6) 0.0426(7) Uani 1 1 d . . . N4 N 0.17289(7) -0.1121(2) -1.8474(8) 0.0310(6) Uani 1 1 d . . . H4 H 0.1955 -0.0834 -1.8226 0.037 Uiso 1 1 calc R . . C4 C 0.07629(9) 0.3881(3) -0.3832(8) 0.0273(7) Uani 1 1 d . . . O5 O 0.22831(9) 0.3649(3) -0.4404(5) 0.0449(8) Uani 1 1 d . . . N5 N 0.20165(8) -0.2140(2) -2.1240(5) 0.0307(7) Uani 1 1 d . . . H5 H 0.2229 -0.1891 -2.0633 0.037 Uiso 1 1 calc R . . C5 C 0.10030(10) 0.4548(3) -0.2583(6) 0.0287(7) Uani 1 1 d . . . H5A H 0.1258 0.4637 -0.3110 0.034 Uiso 1 1 calc R . . O6 O 0.16905(8) 0.3458(3) -0.7477(6) 0.0397(7) Uani 1 1 d . . . N6 N 0.18048(9) -0.3746(3) -2.6412(6) 0.0315(7) Uani 1 1 d . . . H6 H 0.1606 -0.3953 -2.7237 0.038 Uiso 1 1 calc R . . C6 C 0.07676(10) 0.2593(3) -0.7165(6) 0.0280(7) Uani 1 1 d . . . N7 N 0.22329(11) 0.4076(3) -0.2438(7) 0.0348(8) Uani 1 1 d . . . C7 C 0.09099(11) 0.1448(3) -1.0495(7) 0.0321(8) Uani 1 1 d . . . H7A H 0.0704 0.1722 -1.1510 0.039 Uiso 1 1 calc R . . H7B H 0.0815 0.0799 -0.9705 0.039 Uiso 1 1 calc R . . N8 N 0.07635(11) 0.6721(3) 0.4166(7) 0.0485(9) Uani 1 1 d . . . C8 C 0.12609(10) 0.1177(3) -1.1957(7) 0.0312(8) Uani 1 1 d . . . H8A H 0.1351 0.1826 -1.2767 0.037 Uiso 1 1 calc R . . H8B H 0.1469 0.0928 -1.0926 0.037 Uiso 1 1 calc R . . C9 C 0.11704(9) 0.0318(3) -1.3740(9) 0.0307(7) Uani 1 1 d . . . H9A H 0.0957 0.0564 -1.4735 0.037 Uiso 1 1 calc R . . H9B H 0.1084 -0.0331 -1.2917 0.037 Uiso 1 1 calc R . . C10 C 0.15119(10) 0.0036(3) -1.5284(6) 0.0324(8) Uani 1 1 d . . . H10A H 0.1599 0.0680 -1.6122 0.039 Uiso 1 1 calc R . . H10B H 0.1726 -0.0221 -1.4306 0.039 Uiso 1 1 calc R . . C11 C 0.14014(12) -0.0819(3) -1.7024(7) 0.0328(8) Uani 1 1 d . . . H11A H 0.1306 -0.1454 -1.6182 0.039 Uiso 1 1 calc R . . H11B H 0.1192 -0.0552 -1.8027 0.039 Uiso 1 1 calc R . . C12 C 0.16825(10) -0.1833(3) -2.0169(6) 0.0297(7) Uani 1 1 d . . . C13 C 0.20576(10) -0.2803(3) -2.3189(7) 0.0298(9) Uani 1 1 d . . . C14 C 0.24235(9) -0.3094(3) -2.3846(8) 0.0328(8) Uani 1 1 d . . . H14 H 0.2638 -0.2876 -2.2952 0.039 Uiso 1 1 calc R . . C15 C 0.24729(11) -0.3705(3) -2.5815(7) 0.0364(9) Uani 1 1 d . . . H15 H 0.2722 -0.3909 -2.6295 0.044 Uiso 1 1 calc R . . C16 C 0.21567(12) -0.4017(3) -2.7083(7) 0.0351(9) Uani 1 1 d . . . H16 H 0.2190 -0.4431 -2.8451 0.042 Uiso 1 1 calc R . . C17 C 0.17516(10) -0.3168(3) -2.4511(7) 0.0309(8) Uani 1 1 d . . . H17 H 0.1498 -0.2999 -2.4041 0.037 Uiso 1 1 calc R . . C18 C 0.06414(12) 0.7207(4) 0.5647(9) 0.0487(12) Uani 1 1 d . . . C19 C 0.04890(15) 0.7840(5) 0.7593(12) 0.081(2) Uani 1 1 d . . . H19A H 0.0245 0.7537 0.8103 0.121 Uiso 1 1 calc R . . H19B H 0.0449 0.8577 0.7085 0.121 Uiso 1 1 calc R . . H19C H 0.0671 0.7828 0.8886 0.121 Uiso 1 1 calc R . . H1O H 0.1777(14) 0.384(4) -0.858(12) 0.049(13) Uiso 1 1 d . . . H2O H 0.1860(16) 0.361(4) -0.620(10) 0.059(15) Uiso 1 1 d . . . O7 O 0.0166(3) 0.0190(7) -0.587(3) 0.100(5) Uani 0.50 1 d P A 1 O7A O 0.0138(7) -0.031(2) -0.707(5) 0.105(8) Uani 0.25 1 d P B 2 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 0.02688(13) 0.04418(15) 0.03207(14) -0.01011(16) -0.00266(15) -0.00604(11) O1 0.0223(13) 0.0414(15) 0.0415(15) -0.0084(13) 0.0019(11) -0.0071(11) N1 0.0228(14) 0.0389(17) 0.0294(15) -0.0047(13) -0.0033(12) -0.0005(13) C1 0.0277(18) 0.040(2) 0.0298(18) -0.0067(15) 0.0015(14) 0.0035(15) O2 0.0226(12) 0.0375(14) 0.0360(14) -0.0086(11) -0.0021(10) -0.0032(10) N2 0.0184(13) 0.0387(17) 0.0314(16) -0.0055(13) 0.0022(11) -0.0059(12) C2 0.0210(17) 0.046(2) 0.034(2) -0.0066(16) 0.0015(14) 0.0021(15) O3 0.0246(14) 0.077(2) 0.0390(17) -0.0064(15) 0.0055(12) 0.0114(14) N3 0.0269(14) 0.0350(14) 0.0341(17) -0.0070(17) 0.0019(16) -0.0038(11) C3 0.0193(16) 0.0373(17) 0.033(2) -0.0035(14) -0.0050(13) -0.0013(13) O4 0.0293(14) 0.0592(18) 0.0393(15) -0.0127(14) -0.0021(12) 0.0067(13) N4 0.0198(12) 0.0356(14) 0.0375(15) -0.011(2) 0.0023(19) -0.0029(10) C4 0.0228(14) 0.0290(15) 0.030(2) 0.0006(15) -0.0049(16) 0.0020(11) O5 0.0301(15) 0.066(2) 0.0385(16) -0.0198(16) 0.0002(12) 0.0108(15) N5 0.0212(15) 0.0389(17) 0.0319(16) -0.0098(14) -0.0009(12) -0.0005(12) C5 0.0198(17) 0.0370(19) 0.0292(16) -0.0020(16) 0.0028(13) 0.0020(14) O6 0.0266(14) 0.0546(18) 0.0378(15) -0.0033(15) 0.0017(12) -0.0062(13) N6 0.0216(14) 0.0388(17) 0.0342(17) -0.0026(14) -0.0033(12) -0.0023(13) C6 0.0222(17) 0.0323(18) 0.0295(18) -0.0023(15) -0.0015(13) 0.0005(14) N7 0.0290(19) 0.045(2) 0.0306(17) 0.0034(15) 0.0013(15) 0.0059(14) C7 0.0277(18) 0.0329(19) 0.036(2) -0.0077(16) 0.0000(15) -0.0025(15) N8 0.036(2) 0.055(2) 0.054(2) -0.012(2) 0.0039(17) -0.0040(17) C8 0.0278(19) 0.0332(18) 0.033(2) -0.0017(15) 0.0034(14) -0.0009(15) C9 0.0260(15) 0.0348(16) 0.0312(19) -0.0041(19) -0.0001(19) -0.0003(12) C10 0.0273(18) 0.040(2) 0.0303(18) -0.0050(16) 0.0006(14) -0.0027(15) C11 0.0293(19) 0.037(2) 0.032(2) -0.0059(15) 0.0012(15) 0.0009(15) C12 0.0228(17) 0.0339(18) 0.0325(19) 0.0002(15) -0.0002(14) -0.0002(14) C13 0.0243(16) 0.0284(15) 0.037(3) -0.0014(15) -0.0016(15) -0.0012(12) C14 0.0201(15) 0.0398(18) 0.039(2) -0.0069(18) -0.0028(16) -0.0015(13) C15 0.0224(18) 0.045(2) 0.042(2) -0.0085(19) 0.0009(16) 0.0022(16) C16 0.032(2) 0.039(2) 0.035(2) -0.0075(16) -0.0014(16) -0.0002(16) C17 0.0242(18) 0.0318(18) 0.0367(18) -0.0015(15) -0.0026(14) 0.0003(14) C18 0.0218(19) 0.044(2) 0.080(4) -0.007(2) 0.0012(18) -0.0112(17) C19 0.032(3) 0.083(4) 0.127(5) -0.059(4) 0.026(3) -0.011(3) O7 0.055(5) 0.037(4) 0.209(14) 0.051(6) -0.052(7) -0.021(4) O7A 0.061(14) 0.094(17) 0.16(2) -0.037(16) 0.010(13) 0.012(12) _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 2.166(3) . ? Ag1 N6 2.185(3) 1_568 ? O1 C6 1.227(4) . ? N1 C5 1.337(5) . ? N1 C1 1.346(5) . ? C1 C2 1.385(5) . ? C1 H1 0.9500 . ? O2 C12 1.240(4) . ? N2 C6 1.389(4) . ? N2 C4 1.400(5) . ? N2 H2 0.8800 . ? C2 C3 1.389(5) . ? C2 H2A 0.9500 . ? O3 N7 1.238(5) . ? N3 C6 1.330(5) . ? N3 C7 1.455(5) . ? N3 H3 0.8800 . ? C3 C4 1.395(5) . ? C3 H3A 0.9500 . ? O4 N7 1.242(5) . ? N4 C12 1.333(5) . ? N4 C11 1.467(5) . ? N4 H4 0.8800 . ? C4 C5 1.387(5) . ? O5 N7 1.264(4) . ? N5 C12 1.376(4) . ? N5 C13 1.404(5) . ? N5 H5 0.8800 . ? C5 H5A 0.9500 . ? O6 H1O 0.85(6) . ? O6 H2O 0.96(6) . ? N6 C17 1.326(5) . ? N6 C16 1.334(5) . ? N6 Ag1 2.185(3) 1_542 ? N6 H6 0.8800 . ? C7 C8 1.527(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N8 C18 1.132(6) . ? C8 C9 1.523(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.530(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.519(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.384(5) . ? C13 C17 1.391(5) . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.473(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 N6 160.47(12) . 1_568 ? C5 N1 C1 118.1(3) . . ? C5 N1 Ag1 121.0(2) . . ? C1 N1 Ag1 120.5(2) . . ? N1 C1 C2 122.1(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C6 N2 C4 128.2(3) . . ? C6 N2 H2 115.9 . . ? C4 N2 H2 115.9 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C6 N3 C7 122.8(3) . . ? C6 N3 H3 118.6 . . ? C7 N3 H3 118.6 . . ? C2 C3 C4 117.9(3) . . ? C2 C3 H3A 121.0 . . ? C4 C3 H3A 121.0 . . ? C12 N4 C11 119.6(3) . . ? C12 N4 H4 120.2 . . ? C11 N4 H4 120.2 . . ? C5 C4 C3 118.7(4) . . ? C5 C4 N2 116.0(3) . . ? C3 C4 N2 125.3(3) . . ? C12 N5 C13 127.6(3) . . ? C12 N5 H5 116.2 . . ? C13 N5 H5 116.2 . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? H1O O6 H2O 104(5) . . ? C17 N6 C16 120.5(3) . . ? C17 N6 Ag1 117.2(2) . 1_542 ? C16 N6 Ag1 122.0(3) . 1_542 ? C17 N6 H6 119.7 . . ? C16 N6 H6 119.7 . . ? Ag1 N6 H6 6.4 1_542 . ? O1 C6 N3 124.6(3) . . ? O1 C6 N2 123.1(3) . . ? N3 C6 N2 112.3(3) . . ? O3 N7 O4 121.0(4) . . ? O3 N7 O5 118.9(4) . . ? O4 N7 O5 120.1(4) . . ? N3 C7 C8 109.5(3) . . ? N3 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C7 111.2(3) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 113.1(3) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 110.3(3) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N4 C11 C10 111.1(3) . . ? N4 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N4 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O2 C12 N4 122.5(3) . . ? O2 C12 N5 123.2(3) . . ? N4 C12 N5 114.3(3) . . ? C14 C13 C17 118.3(4) . . ? C14 C13 N5 118.0(3) . . ? C17 C13 N5 123.6(3) . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? N6 C16 C15 120.9(4) . . ? N6 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? N6 C17 C13 121.6(3) . . ? N6 C17 H17 119.2 . . ? C13 C17 H17 119.2 . . ? N8 C18 C19 179.0(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C5 -56.2(5) 1_568 . . . ? N6 Ag1 N1 C1 115.8(4) 1_568 . . . ? C5 N1 C1 C2 0.6(6) . . . . ? Ag1 N1 C1 C2 -171.7(3) . . . . ? N1 C1 C2 C3 -1.0(6) . . . . ? C1 C2 C3 C4 1.2(6) . . . . ? C2 C3 C4 C5 -1.1(5) . . . . ? C2 C3 C4 N2 179.2(4) . . . . ? C6 N2 C4 C5 171.7(4) . . . . ? C6 N2 C4 C3 -8.6(6) . . . . ? C1 N1 C5 C4 -0.6(5) . . . . ? Ag1 N1 C5 C4 171.7(3) . . . . ? C3 C4 C5 N1 0.9(6) . . . . ? N2 C4 C5 N1 -179.4(3) . . . . ? C7 N3 C6 O1 2.4(6) . . . . ? C7 N3 C6 N2 -177.7(3) . . . . ? C4 N2 C6 O1 4.4(6) . . . . ? C4 N2 C6 N3 -175.5(3) . . . . ? C6 N3 C7 C8 -175.9(4) . . . . ? N3 C7 C8 C9 178.4(3) . . . . ? C7 C8 C9 C10 178.8(3) . . . . ? C8 C9 C10 C11 -179.7(3) . . . . ? C12 N4 C11 C10 -177.3(4) . . . . ? C9 C10 C11 N4 -178.3(3) . . . . ? C11 N4 C12 O2 7.1(6) . . . . ? C11 N4 C12 N5 -173.2(3) . . . . ? C13 N5 C12 O2 5.3(6) . . . . ? C13 N5 C12 N4 -174.4(3) . . . . ? C12 N5 C13 C14 -173.7(4) . . . . ? C12 N5 C13 C17 7.3(6) . . . . ? C17 C13 C14 C15 1.9(6) . . . . ? N5 C13 C14 C15 -177.1(4) . . . . ? C13 C14 C15 C16 -0.3(6) . . . . ? C17 N6 C16 C15 0.1(6) . . . . ? Ag1 N6 C16 C15 173.2(3) 1_542 . . . ? C14 C15 C16 N6 -0.8(6) . . . . ? C16 N6 C17 C13 1.6(6) . . . . ? Ag1 N6 C17 C13 -171.7(3) 1_542 . . . ? C14 C13 C17 N6 -2.7(6) . . . . ? N5 C13 C17 N6 176.3(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 N2 H2 O6 0.88 2.03 2.853(4) 155.9 . N3 H3 O6 0.88 2.10 2.917(4) 153.7 . N4 H4 O4 0.88 2.21 3.008(4) 150.6 3_543 N5 H5 O5 0.88 1.97 2.846(4) 177.5 3_543 O6 H1O O3 0.85(6) 1.98(7) 2.790(5) 159(5) 1_554 O6 H2O O5 0.96(6) 1.81(6) 2.735(4) 162(5) . O6 H2O N7 0.96(6) 2.60(6) 3.551(5) 172(4) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.139 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.080