Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Ivan Lin' _publ_contact_author_address ; Department of Chemistry National Dong Hwa University Hualien 974 TAIWAN ; _publ_contact_author_email IJBLIN@MAIL.NDHU.EDU.TW _publ_section_title ; Liquid Crystals of Silver Complexes Derived from Simple 1-Alkylimidazoles ; loop_ _publ_author_name I.J.B.Lin H.Kuang-Mei L.K.Chung L.K.Ching T.Chun-Hsien data_[Ag(C16-bim)2(NO3)] _database_code_depnum_ccdc_archive 'CCDC 224068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag(C16-bim)2(NO3)]' _chemical_formula_sum 'C46 H76 Ag N5 O3' _chemical_formula_weight 854.99 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.592(8) _cell_length_b 8.7170(17) _cell_length_c 13.483(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.23(3) _cell_angle_gamma 90.00 _cell_volume 4758.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.04 _cell_measurement_theta_max 12.53 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 0.290 _exptl_absorpt_process_details ? _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.71 _diffrn_reflns_number 5006 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4191 _reflns_number_gt 2541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker 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^)+(0.0500P)^2^+4.7000P] 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_number_reflns 4191 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.5000 0.57489(8) 0.7500 0.0711(3) Uani 1 2 d S . . N1 N 0.52658(9) 0.4736(5) 0.6428(3) 0.0550(10) Uani 1 1 d . . . N2 N 0.54571(9) 0.2844(5) 0.5608(3) 0.0571(10) Uani 1 1 d . . . N3 N 0.5000 0.9283(10) 0.7500 0.089(2) Uani 1 2 d S . . O1 O 0.47601(18) 0.8527(9) 0.7305(6) 0.197(3) Uani 1 1 d . . . O2 O 0.5000 1.0584(10) 0.7500 0.199(5) Uani 1 2 d S . . C1 C 0.53082(12) 0.3265(6) 0.6366(3) 0.0596(12) Uani 1 1 d . . . H1A H 0.5243 0.2563 0.6800 0.072 Uiso 1 1 calc R . . C2 C 0.53901(10) 0.5364(5) 0.5650(3) 0.0504(12) Uani 1 1 d . . . C3 C 0.54105(12) 0.6873(6) 0.5350(3) 0.0629(13) Uani 1 1 d . . . H3A H 0.5332 0.7675 0.5685 0.075 Uiso 1 1 calc R . . C4 C 0.55506(13) 0.7136(7) 0.4538(4) 0.0770(16) Uani 1 1 d . . . H4A H 0.5565 0.8139 0.4318 0.092 Uiso 1 1 calc R . . C5 C 0.56706(13) 0.5965(8) 0.4038(4) 0.0757(16) Uani 1 1 d . . . H5A H 0.5765 0.6202 0.3495 0.091 Uiso 1 1 calc R . . C6 C 0.56543(11) 0.4475(7) 0.4317(3) 0.0650(13) Uani 1 1 d . . . H6A H 0.5733 0.3683 0.3974 0.078 Uiso 1 1 calc R . . C7 C 0.55141(10) 0.4198(6) 0.5144(3) 0.0530(11) Uani 1 1 d . . . C8 C 0.55646(14) 0.1305(6) 0.5420(4) 0.0748(15) Uani 1 1 d . . . H8A H 0.5524 0.1135 0.4691 0.090 Uiso 1 1 calc R . . H8B H 0.5435 0.0563 0.5698 0.090 Uiso 1 1 calc R . . C9 C 0.59291(13) 0.1045(6) 0.5892(4) 0.0797(16) Uani 1 1 d . . . H9A H 0.5993 0.0047 0.5682 0.096 Uiso 1 1 calc R . . H9B H 0.6057 0.1813 0.5633 0.096 Uiso 1 1 calc R . . C10 C 0.60113(13) 0.1120(7) 0.7043(4) 0.0869(18) Uani 1 1 d . . . H10A H 0.5928 0.2080 0.7246 0.104 Uiso 1 1 calc R . . H10B H 0.5895 0.0296 0.7296 0.104 Uiso 1 1 calc R . . C11 C 0.63705(13) 0.1005(7) 0.7547(4) 0.0834(17) Uani 1 1 d . . . H11A H 0.6488 0.1828 0.7299 0.100 Uiso 1 1 calc R . . H11B H 0.6456 0.0041 0.7354 0.100 Uiso 1 1 calc R . . C12 C 0.64386(13) 0.1093(8) 0.8694(4) 0.0875(18) Uani 1 1 d . . . H12A H 0.6339 0.2025 0.8881 0.105 Uiso 1 1 calc R . . H12B H 0.6331 0.0233 0.8940 0.105 Uiso 1 1 calc R . . C13 C 0.67978(13) 0.1080(8) 0.9229(4) 0.0903(19) Uani 1 1 d . . . H13A H 0.6905 0.1950 0.8994 0.108 Uiso 1 1 calc R . . H13B H 0.6898 0.0157 0.9034 0.108 Uiso 1 1 calc R . . C14 C 0.68642(13) 0.1141(8) 1.0379(4) 0.0901(19) Uani 1 1 d . . . H14A H 0.6761 0.2058 1.0570 0.108 Uiso 1 1 calc R . . H14B H 0.6757 0.0266 1.0611 0.108 Uiso 1 1 calc R . . C15 C 0.72199(13) 0.1143(8) 1.0934(4) 0.0930(19) Uani 1 1 d . . . H15A H 0.7325 0.0241 1.0727 0.112 Uiso 1 1 calc R . . H15B H 0.7325 0.2034 1.0716 0.112 Uiso 1 1 calc R . . C16 C 0.72861(13) 0.1159(8) 1.2064(4) 0.0924(19) Uani 1 1 d . . . H16A H 0.7179 0.2058 1.2266 0.111 Uiso 1 1 calc R . . H16B H 0.7180 0.0267 1.2277 0.111 Uiso 1 1 calc R . . C17 C 0.76361(14) 0.1166(9) 1.2638(4) 0.098(2) Uani 1 1 d . . . H17A H 0.7744 0.0279 1.2427 0.118 Uiso 1 1 calc R . . H17B H 0.7741 0.2071 1.2439 0.118 Uiso 1 1 calc R . . C18 C 0.76980(13) 0.1148(8) 1.3766(4) 0.096(2) Uani 1 1 d . . . H18A H 0.7587 0.2030 1.3973 0.115 Uiso 1 1 calc R . . H18B H 0.7593 0.0240 1.3962 0.115 Uiso 1 1 calc R . . C19 C 0.80449(14) 0.1166(8) 1.4360(4) 0.094(2) Uani 1 1 d . . . H19A H 0.8158 0.0296 1.4146 0.113 Uiso 1 1 calc R . . H19B H 0.8149 0.2087 1.4179 0.113 Uiso 1 1 calc R . . C20 C 0.81001(14) 0.1116(8) 1.5481(4) 0.098(2) Uani 1 1 d . . . H20A H 0.7997 0.0189 1.5657 0.118 Uiso 1 1 calc R . . H20B H 0.7983 0.1976 1.5689 0.118 Uiso 1 1 calc R . . C21 C 0.84425(14) 0.1152(8) 1.6104(4) 0.098(2) Uani 1 1 d . . . H21A H 0.8546 0.2085 1.5941 0.117 Uiso 1 1 calc R . . H21B H 0.8562 0.0296 1.5899 0.117 Uiso 1 1 calc R . . C22 C 0.84850(16) 0.1083(10) 1.7230(4) 0.125(3) Uani 1 1 d . . . H22A H 0.8360 0.1922 1.7426 0.150 Uiso 1 1 calc R . . H22B H 0.8384 0.0138 1.7388 0.150 Uiso 1 1 calc R . . C23 C 0.88138(16) 0.1149(10) 1.7871(5) 0.139(3) Uani 1 1 d . . . H23A H 0.8802 0.1070 1.8573 0.208 Uiso 1 1 calc R . . H23B H 0.8915 0.2105 1.7764 0.208 Uiso 1 1 calc R . . H23C H 0.8943 0.0315 1.7704 0.208 Uiso 1 1 calc R . . 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 0.0755(4) 0.0781(5) 0.0680(4) 0.000 0.0334(3) 0.000 N1 0.050(2) 0.063(3) 0.053(2) 0.0025(19) 0.0149(18) 0.001(2) N2 0.056(2) 0.063(3) 0.051(2) -0.008(2) 0.0078(18) 0.007(2) N3 0.113(6) 0.046(5) 0.112(5) 0.000 0.037(5) 0.000 O1 0.181(6) 0.150(6) 0.238(8) 0.016(6) 0.003(6) -0.036(5) O2 0.298(13) 0.060(5) 0.300(12) 0.000 0.193(11) 0.000 C1 0.059(3) 0.064(4) 0.055(3) 0.006(3) 0.012(2) 0.000(3) C2 0.042(2) 0.062(3) 0.046(2) 0.001(2) 0.008(2) 0.002(2) C3 0.065(3) 0.068(4) 0.054(3) -0.001(3) 0.011(2) -0.003(3) C4 0.086(4) 0.079(4) 0.064(3) 0.011(3) 0.012(3) -0.015(3) C5 0.073(3) 0.104(5) 0.053(3) 0.004(3) 0.018(3) -0.017(4) C6 0.055(3) 0.086(4) 0.056(3) -0.013(3) 0.016(2) 0.005(3) C7 0.045(2) 0.062(3) 0.049(2) 0.002(3) 0.004(2) 0.000(3) C8 0.089(4) 0.060(3) 0.069(3) -0.006(3) 0.004(3) 0.011(3) C9 0.085(4) 0.081(4) 0.071(3) -0.012(3) 0.012(3) 0.026(3) C10 0.081(4) 0.107(5) 0.067(3) -0.002(3) 0.006(3) 0.028(4) C11 0.078(4) 0.105(5) 0.065(3) -0.001(3) 0.013(3) 0.021(4) C12 0.075(4) 0.117(5) 0.068(3) 0.003(3) 0.013(3) 0.017(4) C13 0.079(4) 0.121(5) 0.071(3) 0.008(3) 0.017(3) 0.012(4) C14 0.075(4) 0.128(6) 0.066(3) 0.006(3) 0.012(3) 0.018(4) C15 0.074(4) 0.131(6) 0.074(4) 0.009(4) 0.018(3) 0.011(4) C16 0.076(4) 0.133(6) 0.067(3) 0.004(4) 0.013(3) 0.014(4) C17 0.074(4) 0.143(6) 0.075(4) 0.006(4) 0.013(3) 0.009(4) C18 0.067(4) 0.146(6) 0.072(4) 0.004(4) 0.012(3) 0.009(4) C19 0.075(4) 0.126(6) 0.079(4) -0.001(4) 0.014(3) 0.006(4) C20 0.074(4) 0.145(6) 0.072(4) -0.001(4) 0.011(3) 0.004(4) C21 0.070(4) 0.135(6) 0.084(4) -0.003(4) 0.008(3) 0.002(4) C22 0.088(5) 0.199(9) 0.081(4) -0.010(5) 0.007(4) 0.016(5) C23 0.092(5) 0.201(9) 0.109(5) -0.019(6) -0.006(4) 0.026(6) _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 2.196(4) 2_656 ? Ag1 N1 2.196(4) . ? N1 C1 1.299(6) . ? N1 C2 1.384(5) . ? N2 C1 1.362(6) . ? N2 C7 1.380(6) . ? N2 C8 1.455(6) . ? N3 O2 1.134(9) . ? N3 O1 1.174(7) . ? N3 O1 1.174(7) 2_656 ? C2 C3 1.385(7) . ? C2 C7 1.388(6) . ? C3 C4 1.372(7) . ? C4 C5 1.378(7) . ? C5 C6 1.358(7) . ? C6 C7 1.393(6) . ? C8 C9 1.521(7) . ? C9 C10 1.512(7) . ? C10 C11 1.496(7) . ? C11 C12 1.510(7) . ? C12 C13 1.503(7) . ? C13 C14 1.512(7) . ? C14 C15 1.497(7) . ? C15 C16 1.485(7) . ? C16 C17 1.484(7) . ? C17 C18 1.483(7) . ? C18 C19 1.481(7) . ? C19 C20 1.476(7) . ? C20 C21 1.479(7) . ? C21 C22 1.489(8) . ? C22 C23 1.442(8) . ? 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 132.6(2) 2_656 . ? C1 N1 C2 105.1(4) . . ? C1 N1 Ag1 122.4(3) . . ? C2 N1 Ag1 132.2(3) . . ? C1 N2 C7 105.3(4) . . ? C1 N2 C8 126.1(4) . . ? C7 N2 C8 128.2(4) . . ? O2 N3 O1 124.1(5) . . ? O2 N3 O1 124.1(5) . 2_656 ? O1 N3 O1 111.7(11) . 2_656 ? N1 C1 N2 114.0(5) . . ? N1 C2 C3 131.0(4) . . ? N1 C2 C7 109.2(4) . . ? C3 C2 C7 119.8(4) . . ? C4 C3 C2 117.2(5) . . ? C3 C4 C5 122.3(5) . . ? C6 C5 C4 121.8(5) . . ? C5 C6 C7 116.4(5) . . ? N2 C7 C2 106.4(4) . . ? N2 C7 C6 131.1(5) . . ? C2 C7 C6 122.5(5) . . ? N2 C8 C9 112.4(4) . . ? C10 C9 C8 113.1(4) . . ? C11 C10 C9 115.5(5) . . ? C10 C11 C12 113.3(4) . . ? C13 C12 C11 115.1(5) . . ? C12 C13 C14 114.8(5) . . ? C15 C14 C13 116.1(5) . . ? C16 C15 C14 116.3(5) . . ? C17 C16 C15 117.7(5) . . ? C18 C17 C16 117.0(5) . . ? C19 C18 C17 118.3(5) . . ? C20 C19 C18 117.2(5) . . ? C19 C20 C21 119.0(5) . . ? C20 C21 C22 116.9(5) . . ? C23 C22 C21 119.0(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.689 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.059 data_[Ag(C16-bim)2][BF4] _database_code_depnum_ccdc_archive 'CCDC 224069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag(C16-bim)2][BF4]' _chemical_formula_sum 'C46 H76 Ag B F4 N4' _chemical_formula_weight 879.79 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5750(10) _cell_length_b 9.5010(10) _cell_length_c 19.3300(10) _cell_angle_alpha 82.240(10) _cell_angle_beta 87.990(10) _cell_angle_gamma 89.320(10) _cell_volume 1195.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 4.84 _cell_measurement_theta_max 12.57 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7886 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.94 _diffrn_reflns_number 4968 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3932 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker 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^)+(0.0487P)^2^+0.3119P] 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_number_reflns 3932 _refine_ls_number_parameters 274 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 0.5000 1.5000 1.0000 0.0824(2) Uani 1 2 d S . . N1 N 0.2458(4) 1.4643(4) 0.94244(15) 0.0611(8) Uani 1 1 d . . . N2 N 0.0020(4) 1.3473(3) 0.89942(15) 0.0535(7) Uani 1 1 d . . . C1 C 0.1802(6) 1.3404(5) 0.93157(19) 0.0622(10) Uani 1 1 d . . . H1A H 0.2499 1.2558 0.9448 0.075 Uiso 1 1 calc R . . C2 C -0.0528(5) 1.4880(4) 0.88849(17) 0.0493(8) Uani 1 1 d . . . C3 C -0.2229(6) 1.5562(5) 0.8593(2) 0.0662(11) Uani 1 1 d . . . H3A H -0.3249 1.5068 0.8409 0.079 Uiso 1 1 calc R . . C4 C -0.2325(7) 1.7008(5) 0.8589(2) 0.0855(13) Uani 1 1 d . . . H4A H -0.3445 1.7508 0.8401 0.103 Uiso 1 1 calc R . . C5 C -0.0805(9) 1.7736(5) 0.8858(3) 0.0894(14) Uani 1 1 d . . . H5A H -0.0928 1.8716 0.8844 0.107 Uiso 1 1 calc R . . C6 C 0.0885(7) 1.7063(5) 0.9147(2) 0.0759(12) Uani 1 1 d . . . H6A H 0.1908 1.7566 0.9323 0.091 Uiso 1 1 calc R . . C7 C 0.1002(5) 1.5612(4) 0.91638(18) 0.0543(9) Uani 1 1 d . . . C8 C -0.1086(6) 1.2273(4) 0.8794(2) 0.0697(11) Uani 1 1 d . . . H8A H -0.2534 1.2470 0.8826 0.084 Uiso 1 1 calc R . . H8B H -0.0808 1.1434 0.9123 0.084 Uiso 1 1 calc R . . C9 C -0.0526(5) 1.1963(4) 0.8061(2) 0.0669(10) Uani 1 1 d . . . H9A H -0.1455 1.1258 0.7939 0.080 Uiso 1 1 calc R . . H9B H -0.0715 1.2824 0.7738 0.080 Uiso 1 1 calc R . . C10 C 0.1625(5) 1.1435(4) 0.7969(2) 0.0630(10) Uani 1 1 d . . . H10A H 0.1877 1.0652 0.8334 0.076 Uiso 1 1 calc R . . H10B H 0.2558 1.2191 0.8025 0.076 Uiso 1 1 calc R . . C11 C 0.2065(6) 1.0941(4) 0.7263(2) 0.0691(11) Uani 1 1 d . . . H11A H 0.1092 1.0213 0.7200 0.083 Uiso 1 1 calc R . . H11B H 0.1854 1.1735 0.6900 0.083 Uiso 1 1 calc R . . C12 C 0.4180(6) 1.0358(4) 0.7166(2) 0.0669(10) Uani 1 1 d . . . H12A H 0.4393 0.9566 0.7529 0.080 Uiso 1 1 calc R . . H12B H 0.5153 1.1087 0.7226 0.080 Uiso 1 1 calc R . . C13 C 0.4613(6) 0.9860(4) 0.6462(2) 0.0685(10) Uani 1 1 d . . . H13A H 0.3598 0.9164 0.6393 0.082 Uiso 1 1 calc R . . H13B H 0.4459 1.0664 0.6100 0.082 Uiso 1 1 calc R . . C14 C 0.6697(6) 0.9213(4) 0.6370(2) 0.0684(10) Uani 1 1 d . . . H14A H 0.6852 0.8402 0.6728 0.082 Uiso 1 1 calc R . . H14B H 0.7716 0.9905 0.6441 0.082 Uiso 1 1 calc R . . C15 C 0.7100(5) 0.8734(4) 0.5661(2) 0.0672(10) Uani 1 1 d . . . H15A H 0.6979 0.9551 0.5305 0.081 Uiso 1 1 calc R . . H15B H 0.6055 0.8064 0.5586 0.081 Uiso 1 1 calc R . . C16 C 0.9160(6) 0.8047(4) 0.5569(2) 0.0673(10) Uani 1 1 d . . . H16A H 1.0205 0.8715 0.5647 0.081 Uiso 1 1 calc R . . H16B H 0.9278 0.7226 0.5923 0.081 Uiso 1 1 calc R . . C17 C 0.9564(5) 0.7577(4) 0.4858(2) 0.0647(10) Uani 1 1 d . . . H17A H 0.8517 0.6913 0.4778 0.078 Uiso 1 1 calc R . . H17B H 0.9454 0.8399 0.4504 0.078 Uiso 1 1 calc R . . C18 C 1.1606(5) 0.6890(4) 0.4769(2) 0.0657(10) Uani 1 1 d . . . H18A H 1.1705 0.6064 0.5121 0.079 Uiso 1 1 calc R . . H18B H 1.2649 0.7552 0.4857 0.079 Uiso 1 1 calc R . . C19 C 1.2057(5) 0.6429(4) 0.4057(2) 0.0640(10) Uani 1 1 d . . . H19A H 1.1016 0.5770 0.3966 0.077 Uiso 1 1 calc R . . H19B H 1.1975 0.7255 0.3704 0.077 Uiso 1 1 calc R . . C20 C 1.4111(6) 0.5735(4) 0.3985(2) 0.0684(10) Uani 1 1 d . . . H20A H 1.4197 0.4924 0.4347 0.082 Uiso 1 1 calc R . . H20B H 1.5147 0.6404 0.4071 0.082 Uiso 1 1 calc R . . C21 C 1.4603(6) 0.5237(4) 0.3289(2) 0.0688(10) Uani 1 1 d . . . H21A H 1.4534 0.6043 0.2924 0.083 Uiso 1 1 calc R . . H21B H 1.3582 0.4560 0.3201 0.083 Uiso 1 1 calc R . . C22 C 1.6683(6) 0.4549(5) 0.3251(2) 0.0826(12) Uani 1 1 d . . . H22A H 1.7699 0.5231 0.3337 0.099 Uiso 1 1 calc R . . H22B H 1.6751 0.3753 0.3621 0.099 Uiso 1 1 calc R . . C23 C 1.7207(8) 0.4033(6) 0.2571(3) 0.1067(17) Uani 1 1 d . . . H23A H 1.8540 0.3610 0.2589 0.160 Uiso 1 1 calc R . . H23B H 1.7188 0.4818 0.2202 0.160 Uiso 1 1 calc R . . H23C H 1.6230 0.3340 0.2485 0.160 Uiso 1 1 calc R . . B B 0.5000 1.0000 1.0000 0.143(7) Uani 0.80 2 d SPD . . F3 F 0.5291(8) 1.1527(6) 0.9992(4) 0.1048(18) Uani 0.50 1 d PD . . F4 F 0.7192(8) 0.9892(5) 1.0103(3) 0.0961(16) Uani 0.50 1 d PD . . F2 F 0.4942(14) 0.9582(12) 1.0713(4) 0.169(5) Uani 0.50 1 d PD . . F1 F 0.571(3) 0.9622(17) 0.9385(8) 0.340(16) Uani 0.50 1 d PD . . 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 0.0506(3) 0.1391(5) 0.0643(3) -0.0374(3) -0.0089(2) 0.0068(3) N1 0.0504(17) 0.085(2) 0.0507(18) -0.0193(17) -0.0039(14) 0.0066(18) N2 0.0502(17) 0.058(2) 0.0535(17) -0.0121(14) 0.0013(13) 0.0047(15) C1 0.059(2) 0.072(3) 0.056(2) -0.010(2) -0.0010(18) 0.019(2) C2 0.0469(19) 0.057(2) 0.0435(18) -0.0092(16) 0.0055(15) 0.0069(17) C3 0.054(2) 0.083(3) 0.062(2) -0.011(2) -0.0020(18) 0.012(2) C4 0.087(3) 0.083(4) 0.084(3) -0.005(3) -0.008(3) 0.032(3) C5 0.115(4) 0.058(3) 0.093(3) -0.009(3) 0.010(3) 0.009(3) C6 0.082(3) 0.076(3) 0.072(3) -0.022(2) 0.010(2) -0.013(3) C7 0.053(2) 0.062(3) 0.048(2) -0.0127(18) 0.0044(16) 0.0001(19) C8 0.063(2) 0.064(3) 0.084(3) -0.018(2) 0.012(2) -0.009(2) C9 0.060(2) 0.070(3) 0.076(3) -0.031(2) -0.0035(19) -0.0020(19) C10 0.061(2) 0.070(3) 0.062(2) -0.020(2) -0.0037(18) 0.0015(19) C11 0.062(2) 0.081(3) 0.069(3) -0.028(2) -0.0084(19) 0.008(2) C12 0.064(2) 0.074(3) 0.067(2) -0.021(2) -0.0080(19) 0.008(2) C13 0.066(2) 0.074(3) 0.069(3) -0.023(2) -0.0057(19) 0.008(2) C14 0.061(2) 0.078(3) 0.069(3) -0.019(2) -0.0031(19) 0.006(2) C15 0.062(2) 0.074(3) 0.068(2) -0.018(2) -0.0037(19) 0.007(2) C16 0.061(2) 0.074(3) 0.068(3) -0.017(2) -0.0038(19) 0.007(2) C17 0.057(2) 0.071(3) 0.068(2) -0.016(2) -0.0041(18) 0.0060(19) C18 0.060(2) 0.071(3) 0.067(2) -0.015(2) -0.0029(18) 0.0036(19) C19 0.058(2) 0.072(3) 0.064(2) -0.015(2) -0.0046(18) 0.0052(19) C20 0.062(2) 0.083(3) 0.063(2) -0.018(2) -0.0050(18) 0.007(2) C21 0.067(2) 0.078(3) 0.062(2) -0.012(2) 0.0044(19) 0.003(2) C22 0.072(3) 0.106(3) 0.073(3) -0.022(3) 0.002(2) 0.011(2) C23 0.099(4) 0.135(5) 0.086(4) -0.024(3) 0.022(3) 0.017(3) B 0.175(16) 0.109(13) 0.113(10) 0.068(9) 0.075(10) 0.106(11) F3 0.073(3) 0.087(4) 0.150(6) 0.002(4) -0.005(3) 0.009(3) F4 0.102(4) 0.063(3) 0.117(4) 0.012(3) -0.010(3) 0.009(3) F2 0.113(7) 0.145(9) 0.235(12) 0.035(8) -0.063(8) 0.005(6) F1 0.215(17) 0.188(15) 0.65(5) -0.20(2) 0.12(2) 0.002(11) _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 2.096(3) 2_687 ? Ag1 N1 2.096(3) . ? N1 C1 1.304(5) . ? N1 C7 1.381(5) . ? N2 C1 1.342(5) . ? N2 C2 1.371(4) . ? N2 C8 1.461(5) . ? C2 C3 1.385(5) . ? C2 C7 1.394(5) . ? C3 C4 1.374(6) . ? C4 C5 1.377(7) . ? C5 C6 1.373(6) . ? C6 C7 1.375(5) . ? C8 C9 1.518(5) . ? C9 C10 1.508(5) . ? C10 C11 1.520(5) . ? C11 C12 1.506(5) . ? C12 C13 1.516(5) . ? C13 C14 1.510(5) . ? C14 C15 1.515(5) . ? C15 C16 1.513(5) . ? C16 C17 1.515(5) . ? C17 C18 1.500(5) . ? C18 C19 1.518(5) . ? C19 C20 1.507(5) . ? C20 C21 1.509(5) . ? C21 C22 1.512(5) . ? C22 C23 1.491(6) . ? B F1 1.354(10) 2_677 ? B F1 1.354(10) . ? B F2 1.381(8) 2_677 ? B F2 1.381(8) . ? B F3 1.464(5) . ? B F3 1.464(5) 2_677 ? B F4 1.462(5) . ? B F4 1.462(5) 2_677 ? F3 F1 1.637(17) 2_677 ? F4 F1 1.772(19) . ? F2 F1 0.866(15) 2_677 ? F1 F2 0.866(15) 2_677 ? F1 F3 1.637(17) 2_677 ? 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 180.000(1) 2_687 . ? C1 N1 C7 105.7(3) . . ? C1 N1 Ag1 125.7(3) . . ? C7 N1 Ag1 128.1(3) . . ? C1 N2 C2 106.5(3) . . ? C1 N2 C8 126.1(3) . . ? C2 N2 C8 127.3(3) . . ? N1 C1 N2 113.2(3) . . ? N2 C2 C3 131.7(3) . . ? N2 C2 C7 106.1(3) . . ? C3 C2 C7 122.2(4) . . ? C4 C3 C2 116.3(4) . . ? C3 C4 C5 121.7(4) . . ? C6 C5 C4 122.2(4) . . ? C5 C6 C7 117.2(4) . . ? C6 C7 N1 131.1(4) . . ? C6 C7 C2 120.5(4) . . ? N1 C7 C2 108.4(3) . . ? N2 C8 C9 113.3(3) . . ? C10 C9 C8 114.4(3) . . ? C9 C10 C11 113.5(3) . . ? C12 C11 C10 114.6(3) . . ? C11 C12 C13 114.5(3) . . ? C14 C13 C12 115.0(3) . . ? C13 C14 C15 114.1(3) . . ? C14 C15 C16 114.7(3) . . ? C17 C16 C15 114.6(3) . . ? C18 C17 C16 114.4(3) . . ? C17 C18 C19 115.4(3) . . ? C20 C19 C18 114.1(3) . . ? C19 C20 C21 115.8(3) . . ? C20 C21 C22 113.2(3) . . ? C23 C22 C21 114.5(4) . . ? F1 B F1 180.000(14) 2_677 . ? F1 B F2 143.1(7) 2_677 2_677 ? F1 B F2 36.9(7) . 2_677 ? F1 B F2 36.9(7) 2_677 . ? F1 B F2 143.1(7) . . ? F2 B F2 180.000(7) 2_677 . ? F1 B F3 70.9(7) 2_677 . ? F1 B F3 109.1(7) . . ? F2 B F3 80.8(5) 2_677 . ? F2 B F3 99.2(5) . . ? F1 B F3 109.1(7) 2_677 2_677 ? F1 B F3 70.9(7) . 2_677 ? F2 B F3 99.2(5) 2_677 2_677 ? F2 B F3 80.8(5) . 2_677 ? F3 B F3 180.000(3) . 2_677 ? F1 B F4 102.1(9) 2_677 . ? F1 B F4 77.9(9) . . ? F2 B F4 98.4(5) 2_677 . ? F2 B F4 81.6(5) . . ? F3 B F4 85.0(3) . . ? F3 B F4 95.0(3) 2_677 . ? F1 B F4 77.9(9) 2_677 2_677 ? F1 B F4 102.1(9) . 2_677 ? F2 B F4 81.6(5) 2_677 2_677 ? F2 B F4 98.4(5) . 2_677 ? F3 B F4 95.0(3) . 2_677 ? F3 B F4 85.0(3) 2_677 2_677 ? F4 B F4 180.000(2) . 2_677 ? B F3 F1 51.4(4) . 2_677 ? B F4 F1 48.3(4) . . ? F1 F2 B 69.8(10) 2_677 . ? F2 F1 B 73.3(9) 2_677 . ? F2 F1 F3 116.6(16) 2_677 2_677 ? B F1 F3 57.7(6) . 2_677 ? F2 F1 F4 104.0(15) 2_677 . ? B F1 F4 53.8(6) . . ? F3 F1 F4 78.4(8) 2_677 . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.293 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.048 data_[Ag(C12H25-im)2][NO3] _database_code_depnum_ccdc_archive 'CCDC 224070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag(C12H25-im)2][NO3]' _chemical_formula_sum 'C30 H56 Ag N5 O3' _chemical_formula_weight 642.67 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9813(9) _cell_length_b 15.392(2) _cell_length_c 19.218(3) _cell_angle_alpha 81.747(3) _cell_angle_beta 81.902(3) _cell_angle_gamma 83.315(3) _cell_volume 1725.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7303 _exptl_absorpt_correction_T_max 0.8187 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 17156 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.1192 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 28.18 _reflns_number_total 7644 _reflns_number_gt 3362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0450P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7644 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 0.72633(6) 0.73744(2) 0.569421(19) 0.07056(16) Uani 1 1 d . . . N1 N 0.7864(6) 0.5970(2) 0.58079(18) 0.0654(10) Uani 1 1 d . . . N2 N 0.9396(7) 0.4605(2) 0.60046(19) 0.0693(10) Uani 1 1 d . . . N3 N 0.6479(6) 0.8745(2) 0.57886(17) 0.0561(9) Uani 1 1 d . . . N4 N 0.4701(6) 1.0036(2) 0.59839(17) 0.0554(9) Uani 1 1 d . . . N5 N 0.2568(8) -0.2484(2) 0.4903(3) 0.0686(10) Uani 1 1 d . . . O1 O 0.2303(6) -0.2627(3) 0.5554(3) 0.1209(15) Uani 1 1 d . . . O2 O 0.4437(6) -0.2657(2) 0.4571(2) 0.1014(12) Uani 1 1 d . . . O3 O 0.0923(6) -0.2170(2) 0.4601(2) 0.1004(11) Uani 1 1 d . . . C1 C 0.9622(8) 0.5452(3) 0.6015(2) 0.0738(13) Uani 1 1 d . . . H1A H 1.0877 0.5655 0.6152 0.089 Uiso 1 1 calc R . . C2 C 0.7393(9) 0.4570(3) 0.5781(3) 0.0827(14) Uani 1 1 d . . . H2A H 0.6758 0.4064 0.5726 0.099 Uiso 1 1 calc R . . C3 C 0.6467(8) 0.5415(3) 0.5650(3) 0.0805(14) Uani 1 1 d . . . H3A H 0.5084 0.5587 0.5478 0.097 Uiso 1 1 calc R . . C4 C 1.1017(9) 0.3848(3) 0.6207(3) 0.1002(17) Uani 1 1 d . . . H4A H 1.2365 0.4059 0.6325 0.120 Uiso 1 1 calc R . . H4B H 1.1466 0.3516 0.5809 0.120 Uiso 1 1 calc R . . C5 C 0.9994(16) 0.3256(5) 0.6830(5) 0.178(4) Uani 1 1 d . . . H5A H 1.1026 0.2724 0.6893 0.214 Uiso 1 1 calc R . . H5B H 0.8602 0.3085 0.6709 0.214 Uiso 1 1 calc R . . C6 C 0.9451(14) 0.3607(5) 0.7534(5) 0.147(3) Uani 1 1 d . . . H6A H 0.8886 0.4224 0.7447 0.176 Uiso 1 1 calc R . . H6B H 0.8229 0.3297 0.7809 0.176 Uiso 1 1 calc R . . C7 C 1.1289(16) 0.3536(5) 0.7960(5) 0.175(3) Uani 1 1 d . . . H7A H 1.1895 0.2921 0.8019 0.209 Uiso 1 1 calc R . . H7B H 1.2477 0.3864 0.7684 0.209 Uiso 1 1 calc R . . C8 C 1.0902(14) 0.3819(5) 0.8649(4) 0.142(3) Uani 1 1 d . . . H8A H 1.0549 0.4454 0.8581 0.171 Uiso 1 1 calc R . . H8B H 0.9543 0.3572 0.8895 0.171 Uiso 1 1 calc R . . C9 C 1.2596(15) 0.3630(5) 0.9120(5) 0.156(3) Uani 1 1 d . . . H9A H 1.2910 0.2993 0.9190 0.187 Uiso 1 1 calc R . . H9B H 1.3960 0.3859 0.8861 0.187 Uiso 1 1 calc R . . C10 C 1.2371(14) 0.3903(5) 0.9798(5) 0.140(2) Uani 1 1 d . . . H10A H 1.0985 0.3688 1.0053 0.168 Uiso 1 1 calc R . . H10B H 1.2097 0.4542 0.9726 0.168 Uiso 1 1 calc R . . C11 C 1.4058(15) 0.3695(5) 1.0277(4) 0.145(3) Uani 1 1 d . . . H11A H 1.4391 0.3059 1.0332 0.174 Uiso 1 1 calc R . . H11B H 1.5424 0.3938 1.0033 0.174 Uiso 1 1 calc R . . C12 C 1.3747(14) 0.3948(5) 1.0976(5) 0.144(3) Uani 1 1 d . . . H12A H 1.2345 0.3729 1.1215 0.172 Uiso 1 1 calc R . . H12B H 1.3490 0.4587 1.0922 0.172 Uiso 1 1 calc R . . C13 C 1.5451(14) 0.3696(5) 1.1466(4) 0.148(3) Uani 1 1 d . . . H13A H 1.5781 0.3061 1.1500 0.177 Uiso 1 1 calc R . . H13B H 1.6827 0.3949 1.1242 0.177 Uiso 1 1 calc R . . C14 C 1.5045(16) 0.3917(6) 1.2184(5) 0.175(3) Uani 1 1 d . . . H14A H 1.4770 0.4553 1.2157 0.210 Uiso 1 1 calc R . . H14B H 1.3657 0.3676 1.2412 0.210 Uiso 1 1 calc R . . C15 C 1.6780(16) 0.3627(6) 1.2641(4) 0.197(4) Uani 1 1 d . . . H15A H 1.6301 0.3822 1.3096 0.295 Uiso 1 1 calc R . . H15B H 1.8164 0.3871 1.2435 0.295 Uiso 1 1 calc R . . H15C H 1.7029 0.2994 1.2697 0.295 Uiso 1 1 calc R . . C16 C 0.7964(7) 0.9370(3) 0.5629(2) 0.0594(11) Uani 1 1 d . . . H16A H 0.9493 0.9264 0.5461 0.071 Uiso 1 1 calc R . . C17 C 0.6895(8) 1.0169(3) 0.5750(2) 0.0634(12) Uani 1 1 d . . . H17A H 0.7537 1.0701 0.5686 0.076 Uiso 1 1 calc R . . C18 C 0.4536(8) 0.9173(3) 0.5999(2) 0.0604(11) Uani 1 1 d . . . H18A H 0.3197 0.8908 0.6143 0.072 Uiso 1 1 calc R . . C19 C 0.2905(7) 1.0702(3) 0.6211(2) 0.0717(13) Uani 1 1 d . . . H19A H 0.1484 1.0580 0.6074 0.086 Uiso 1 1 calc R . . H19B H 0.3256 1.1277 0.5971 0.086 Uiso 1 1 calc R . . C20 C 0.2622(8) 1.0723(3) 0.6996(3) 0.0857(15) Uani 1 1 d . . . H20A H 0.1286 1.1119 0.7120 0.103 Uiso 1 1 calc R . . H20B H 0.2334 1.0138 0.7230 0.103 Uiso 1 1 calc R . . C21 C 0.4574(8) 1.1004(3) 0.7289(2) 0.0804(14) Uani 1 1 d . . . H21A H 0.5940 1.0647 0.7127 0.096 Uiso 1 1 calc R . . H21B H 0.4764 1.1611 0.7092 0.096 Uiso 1 1 calc R . . C22 C 0.4378(9) 1.0941(4) 0.8077(3) 0.0936(16) Uani 1 1 d . . . H22A H 0.2992 1.1289 0.8238 0.112 Uiso 1 1 calc R . . H22B H 0.4207 1.0332 0.8272 0.112 Uiso 1 1 calc R . . C23 C 0.6254(9) 1.1227(4) 0.8383(3) 0.0942(16) Uani 1 1 d . . . H23A H 0.6321 1.1853 0.8230 0.113 Uiso 1 1 calc R . . H23B H 0.7662 1.0925 0.8184 0.113 Uiso 1 1 calc R . . C24 C 0.6149(10) 1.1076(4) 0.9175(3) 0.1000(17) Uani 1 1 d . . . H24A H 0.4729 1.1372 0.9372 0.120 Uiso 1 1 calc R . . H24B H 0.6091 1.0449 0.9325 0.120 Uiso 1 1 calc R . . C25 C 0.7995(10) 1.1363(4) 0.9497(3) 0.1002(17) Uani 1 1 d . . . H25A H 0.8012 1.1995 0.9365 0.120 Uiso 1 1 calc R . . H25B H 0.9422 1.1086 0.9286 0.120 Uiso 1 1 calc R . . C26 C 0.7919(10) 1.1175(4) 1.0278(3) 0.1028(18) Uani 1 1 d . . . H26A H 0.6472 1.1438 1.0488 0.123 Uiso 1 1 calc R . . H26B H 0.7938 1.0542 1.0408 0.123 Uiso 1 1 calc R . . C27 C 0.9715(10) 1.1476(4) 1.0609(3) 0.1106(19) Uani 1 1 d . . . H27A H 1.1160 1.1220 1.0393 0.133 Uiso 1 1 calc R . . H27B H 0.9680 1.2110 1.0483 0.133 Uiso 1 1 calc R . . C28 C 0.9678(11) 1.1285(4) 1.1382(3) 0.1073(18) Uani 1 1 d . . . H28A H 0.8237 1.1542 1.1599 0.129 Uiso 1 1 calc R . . H28B H 0.9714 1.0650 1.1509 0.129 Uiso 1 1 calc R . . C29 C 1.1480(13) 1.1588(5) 1.1699(3) 0.141(3) Uani 1 1 d . . . H29A H 1.1456 1.2220 1.1562 0.170 Uiso 1 1 calc R . . H29B H 1.2915 1.1323 1.1483 0.170 Uiso 1 1 calc R . . C30 C 1.1483(12) 1.1420(5) 1.2474(4) 0.145(2) Uiso 1 1 d . . . H30A H 1.2767 1.1656 1.2599 0.217 Uiso 1 1 calc R . . H30B H 1.1573 1.0796 1.2625 0.217 Uiso 1 1 calc R . . H30C H 1.0112 1.1698 1.2704 0.217 Uiso 1 1 calc R . . 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 0.0810(3) 0.0436(2) 0.0890(3) -0.01329(16) -0.01501(19) -0.00282(16) N1 0.062(2) 0.047(2) 0.089(3) -0.0107(19) -0.013(2) -0.008(2) N2 0.068(3) 0.048(2) 0.089(3) -0.0064(19) -0.012(2) 0.007(2) N3 0.056(2) 0.048(2) 0.067(2) -0.0097(17) -0.0126(19) -0.007(2) N4 0.052(2) 0.050(2) 0.066(2) -0.0131(17) -0.0117(18) -0.0013(18) N5 0.062(3) 0.045(2) 0.103(4) -0.011(2) -0.021(3) -0.010(2) O1 0.088(3) 0.172(4) 0.107(3) -0.003(3) -0.026(3) -0.031(3) O2 0.064(2) 0.095(3) 0.144(3) -0.034(2) 0.002(2) 0.002(2) O3 0.077(2) 0.092(3) 0.133(3) 0.000(2) -0.041(2) 0.004(2) C1 0.063(3) 0.058(3) 0.106(4) -0.014(3) -0.024(3) -0.008(3) C2 0.088(4) 0.051(3) 0.118(4) -0.020(3) -0.025(3) -0.014(3) C3 0.068(3) 0.059(3) 0.125(4) -0.026(3) -0.034(3) -0.005(3) C4 0.110(4) 0.062(3) 0.122(5) -0.010(3) -0.021(4) 0.024(3) C5 0.265(11) 0.091(6) 0.172(8) -0.006(6) -0.071(7) 0.048(6) C6 0.176(8) 0.102(6) 0.155(7) 0.002(5) -0.024(6) 0.000(5) C7 0.211(10) 0.131(7) 0.193(9) -0.041(6) -0.076(8) 0.021(6) C8 0.189(8) 0.116(6) 0.120(6) -0.013(5) -0.020(6) -0.008(5) C9 0.210(9) 0.123(6) 0.135(7) -0.015(5) -0.033(7) -0.005(6) C10 0.177(8) 0.115(6) 0.124(6) -0.003(5) -0.015(6) -0.019(5) C11 0.190(8) 0.123(6) 0.116(6) -0.005(5) -0.005(6) -0.014(5) C12 0.172(8) 0.123(6) 0.134(7) -0.010(5) -0.011(6) -0.022(5) C13 0.182(8) 0.132(7) 0.125(7) -0.025(5) 0.001(6) -0.014(6) C14 0.199(10) 0.175(9) 0.153(8) -0.038(7) -0.008(7) -0.018(7) C15 0.196(9) 0.258(12) 0.138(7) -0.040(7) -0.027(7) -0.004(8) C16 0.054(3) 0.059(3) 0.066(3) -0.013(2) -0.003(2) -0.004(2) C17 0.075(4) 0.048(3) 0.069(3) -0.010(2) -0.006(3) -0.014(2) C18 0.055(3) 0.056(3) 0.075(3) -0.012(2) -0.014(2) -0.008(2) C19 0.062(3) 0.066(3) 0.087(4) -0.016(2) -0.016(3) 0.012(2) C20 0.073(4) 0.080(4) 0.100(4) -0.027(3) 0.006(3) 0.012(3) C21 0.085(4) 0.071(3) 0.085(4) -0.024(3) -0.009(3) 0.001(3) C22 0.104(4) 0.095(4) 0.081(4) -0.024(3) 0.000(3) -0.004(3) C23 0.101(4) 0.101(4) 0.080(4) -0.024(3) -0.002(3) -0.002(3) C24 0.113(5) 0.107(5) 0.080(4) -0.023(3) 0.001(3) -0.011(4) C25 0.106(5) 0.112(5) 0.081(4) -0.017(3) -0.004(3) -0.013(4) C26 0.120(5) 0.107(5) 0.081(4) -0.019(3) -0.009(4) -0.008(4) C27 0.118(5) 0.123(5) 0.092(5) -0.014(4) -0.011(4) -0.019(4) C28 0.125(5) 0.110(5) 0.088(5) -0.010(3) -0.021(4) -0.011(4) C29 0.163(7) 0.163(7) 0.098(5) -0.005(4) -0.018(5) -0.033(5) _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 2.134(3) . ? Ag1 N3 2.135(3) . ? N1 C1 1.315(5) . ? N1 C3 1.354(5) . ? N2 C1 1.330(5) . ? N2 C2 1.338(5) . ? N2 C4 1.471(6) . ? N3 C18 1.309(5) . ? N3 C16 1.359(5) . ? N4 C18 1.340(5) . ? N4 C17 1.355(5) . ? N4 C19 1.461(5) . ? N5 O2 1.227(5) . ? N5 O3 1.228(4) . ? N5 O1 1.230(4) . ? C2 C3 1.356(6) . ? C4 C5 1.499(9) . ? C5 C6 1.506(9) . ? C6 C7 1.446(9) . ? C7 C8 1.434(9) . ? C8 C9 1.430(9) . ? C9 C10 1.409(9) . ? C10 C11 1.439(9) . ? C11 C12 1.434(9) . ? C12 C13 1.466(9) . ? C13 C14 1.448(9) . ? C14 C15 1.444(9) . ? C16 C17 1.353(5) . ? C19 C20 1.499(6) . ? C20 C21 1.497(6) . ? C21 C22 1.492(6) . ? C22 C23 1.474(7) . ? C23 C24 1.499(6) . ? C24 C25 1.478(7) . ? C25 C26 1.483(6) . ? C26 C27 1.471(7) . ? C27 C28 1.470(7) . ? C28 C29 1.461(8) . ? C29 C30 1.476(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 N3 169.33(13) . . ? C1 N1 C3 104.7(4) . . ? C1 N1 Ag1 129.7(3) . . ? C3 N1 Ag1 125.6(3) . . ? C1 N2 C2 106.9(4) . . ? C1 N2 C4 126.8(5) . . ? C2 N2 C4 126.3(4) . . ? C18 N3 C16 104.9(4) . . ? C18 N3 Ag1 129.3(3) . . ? C16 N3 Ag1 125.8(3) . . ? C18 N4 C17 106.7(4) . . ? C18 N4 C19 127.0(4) . . ? C17 N4 C19 126.2(4) . . ? O2 N5 O3 121.6(5) . . ? O2 N5 O1 120.1(5) . . ? O3 N5 O1 118.3(5) . . ? N1 C1 N2 112.1(4) . . ? N2 C2 C3 106.7(4) . . ? N1 C3 C2 109.6(4) . . ? N2 C4 C5 111.1(5) . . ? C4 C5 C6 118.2(7) . . ? C7 C6 C5 116.7(8) . . ? C8 C7 C6 120.4(9) . . ? C9 C8 C7 121.1(8) . . ? C10 C9 C8 124.6(8) . . ? C9 C10 C11 124.4(8) . . ? C12 C11 C10 123.4(8) . . ? C11 C12 C13 122.4(8) . . ? C14 C13 C12 121.4(8) . . ? C15 C14 C13 118.2(8) . . ? C17 C16 N3 110.2(4) . . ? C16 C17 N4 106.1(4) . . ? N3 C18 N4 112.1(4) . . ? N4 C19 C20 112.4(4) . . ? C21 C20 C19 116.3(4) . . ? C22 C21 C20 116.1(4) . . ? C23 C22 C21 117.4(5) . . ? C22 C23 C24 116.9(5) . . ? C25 C24 C23 118.1(5) . . ? C24 C25 C26 117.5(5) . . ? C27 C26 C25 118.2(5) . . ? C28 C27 C26 118.8(5) . . ? C29 C28 C27 117.9(5) . . ? C28 C29 C30 119.5(6) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.507 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.116