Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #=========================================================================== _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bastida, Rufina' 'Fenton, David E.' 'Gonzalez, Sonia' 'Macias, Alejandro' 'Rodriguez, Adolfo' 'Valencia, Laura' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr Rufina Bastida' _publ_contact_author_address ; Facultad de Quimica Universidad de Santiago de Compostela Avenida de las Ciencias s/n Santiago de Compostela 15782 SPAIN ; _publ_contact_author_email QIBASTID@USC.ES _publ_requested_journal 'Chemical Communications' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of a New Tetra-Cyanomethylated Macrocyclic Ligand with a Nanotubular Structure. X-ray Crystal Structures of Mono-, Dinuclear and Polymeric Metal Complexes. ; data_L1 _database_code_CSD 185884 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C26H30N10 _chemical_formula_sum 'C13 H15 N5' _chemical_formula_weight 241.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 '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' _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 6.1800(3) _cell_length_b 8.3150(3) _cell_length_c 13.2140(9) _cell_angle_alpha 86.256(4) _cell_angle_beta 78.343(5) _cell_angle_gamma 80.581(4) _cell_volume 655.69(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 256 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7540 _exptl_absorpt_correction_T_max 0.8855 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MACH3 Enraf Nonius' _diffrn_measurement_method ?omega/2-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 2875 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 72.93 _reflns_number_total 2617 _reflns_number_gt 2251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software' _computing_cell_refinement 'CAD4-Express Software' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0708P)^2^+0.1416P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2617 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 N1 N 0.1871(2) 0.21220(19) 0.98138(9) 0.0583(4) Uani 1 1 d . . . N2 N 0.0043(2) 0.20486(16) 1.26255(9) 0.0541(3) Uani 1 1 d . . . N3 N 0.1927(2) 0.34508(16) 0.71662(9) 0.0518(3) Uani 1 1 d . . . N4 N 0.7335(3) 0.3243(3) 0.57957(14) 0.0896(6) Uani 1 1 d . . . N5 N 0.4505(4) 0.1175(3) 1.38453(14) 0.0906(6) Uani 1 1 d . . . C1 C 0.1047(2) 0.2339(2) 0.89485(11) 0.0538(4) Uani 1 1 d . . . C2 C -0.1216(3) 0.2504(2) 0.89526(12) 0.0598(4) Uani 1 1 d . . . H2 H -0.1750 0.2710 0.8340 0.072 Uiso 1 1 calc R . . C3 C -0.2661(3) 0.2356(2) 0.98799(13) 0.0646(5) Uani 1 1 d . . . H3 H -0.4188 0.2437 0.9902 0.077 Uiso 1 1 calc R . . C4 C -0.1824(2) 0.2086(2) 1.07781(12) 0.0581(4) Uani 1 1 d . . . H4 H -0.2769 0.1956 1.1411 0.070 Uiso 1 1 calc R . . C5 C 0.0446(2) 0.2013(2) 1.07181(11) 0.0540(4) Uani 1 1 d . . . C6 C 0.2743(3) 0.2317(2) 0.79466(12) 0.0626(4) Uani 1 1 d . . . H6A H 0.4117 0.2607 0.8077 0.075 Uiso 1 1 calc R . . H6B H 0.3077 0.1222 0.7686 0.075 Uiso 1 1 calc R . . C7A C 0.1887(4) 0.5105(3) 0.7484(2) 0.0508(7) Uani 0.790(8) 1 d P . 1 H7A1 H 0.3386 0.5383 0.7313 0.061 Uiso 0.790(8) 1 calc PR . 1 H7A2 H 0.1383 0.5162 0.8227 0.061 Uiso 0.790(8) 1 calc PR . 1 C8A C -0.0344(6) 0.3687(3) 1.3050(3) 0.0632(8) Uani 0.790(8) 1 d P . 1 H8A1 H 0.1078 0.4076 1.2978 0.076 Uiso 0.790(8) 1 calc PR . 1 H8A2 H -0.0987 0.3620 1.3782 0.076 Uiso 0.790(8) 1 calc PR . 1 C7B C 0.1754(19) 0.5307(12) 0.6899(14) 0.076(4) Uani 0.210(8) 1 d P . 2 H7B1 H 0.3053 0.5705 0.7036 0.091 Uiso 0.210(8) 1 calc PR . 2 H7B2 H 0.1717 0.5504 0.6171 0.091 Uiso 0.210(8) 1 calc PR . 2 C8B C 0.0282(13) 0.3822(9) 1.2476(10) 0.047(2) Uani 0.210(8) 1 d P . 2 H8B1 H 0.1598 0.4027 1.2711 0.056 Uiso 0.210(8) 1 calc PR . 2 H8B2 H 0.0405 0.4162 1.1753 0.056 Uiso 0.210(8) 1 calc PR . 2 C9 C 0.1541(3) 0.1741(3) 1.16476(12) 0.0735(6) Uani 1 1 d . . . H9A H 0.2287 0.0621 1.1660 0.088 Uiso 1 1 calc R . . H9B H 0.2679 0.2442 1.1569 0.088 Uiso 1 1 calc R . . C10 C 0.3070(3) 0.3026(2) 0.61350(11) 0.0608(4) Uani 1 1 d . . . H10A H 0.2358 0.3735 0.5645 0.073 Uiso 1 1 calc R . . H10B H 0.2903 0.1916 0.6022 0.073 Uiso 1 1 calc R . . C11 C 0.5483(3) 0.3155(2) 0.59233(12) 0.0654(5) Uani 1 1 d . . . C12 C 0.0612(3) 0.0906(3) 1.34305(14) 0.0726(5) Uani 1 1 d . . . H12A H 0.0641 -0.0192 1.3215 0.087 Uiso 1 1 calc R . . H12B H -0.0542 0.1092 1.4047 0.087 Uiso 1 1 calc R . . C13 C 0.2814(4) 0.1029(2) 1.36904(13) 0.0701(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0396(6) 0.0947(10) 0.0409(7) -0.0014(6) -0.0069(5) -0.0128(6) N2 0.0561(7) 0.0605(8) 0.0415(6) 0.0000(5) -0.0062(5) -0.0020(6) N3 0.0491(7) 0.0621(8) 0.0412(6) -0.0055(5) -0.0072(5) -0.0006(5) N4 0.0653(10) 0.1289(16) 0.0687(10) -0.0022(10) 0.0022(8) -0.0175(10) N5 0.0910(13) 0.1086(14) 0.0721(11) -0.0101(9) -0.0324(10) 0.0077(10) C1 0.0417(7) 0.0782(10) 0.0415(7) -0.0039(7) -0.0080(6) -0.0088(7) C2 0.0444(8) 0.0896(12) 0.0482(8) -0.0041(7) -0.0138(6) -0.0118(7) C3 0.0388(7) 0.0988(13) 0.0592(9) -0.0042(8) -0.0100(7) -0.0185(8) C4 0.0422(7) 0.0846(11) 0.0479(8) -0.0035(7) -0.0022(6) -0.0188(7) C5 0.0421(7) 0.0791(10) 0.0414(7) -0.0031(7) -0.0066(6) -0.0123(7) C6 0.0467(8) 0.0928(12) 0.0437(8) 0.0004(8) -0.0074(6) 0.0001(8) C7A 0.0506(10) 0.0610(12) 0.0397(13) -0.0014(10) -0.0108(9) -0.0025(8) C8A 0.0755(17) 0.0671(14) 0.0434(17) -0.0037(11) -0.0167(13) 0.0071(12) C7B 0.072(6) 0.069(6) 0.073(9) 0.005(5) 0.008(6) 0.000(5) C8B 0.044(4) 0.049(4) 0.043(6) 0.000(3) 0.000(3) -0.005(3) C9 0.0462(8) 0.1327(17) 0.0402(8) -0.0046(9) -0.0069(6) -0.0107(9) C10 0.0553(9) 0.0848(11) 0.0398(8) -0.0038(7) -0.0087(6) -0.0037(8) C11 0.0621(10) 0.0838(12) 0.0436(8) 0.0004(7) 0.0004(7) -0.0058(8) C12 0.0683(11) 0.0882(13) 0.0533(9) 0.0141(9) -0.0041(8) -0.0047(9) C13 0.0781(12) 0.0812(12) 0.0433(8) -0.0017(8) -0.0132(8) 0.0118(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.3331(19) . ? N1 C5 1.3410(19) . ? N2 C12 1.438(2) . ? N2 C9 1.4403(19) . ? N2 C8A 1.472(3) . ? N2 C8B 1.502(7) . ? N3 C10 1.4397(18) . ? N3 C7A 1.460(3) . ? N3 C6 1.461(2) . ? N3 C7B 1.552(11) . ? N4 C11 1.137(2) . ? N5 C13 1.131(3) . ? C1 C2 1.382(2) . ? C1 C6 1.512(2) . ? C2 C3 1.374(2) . ? C3 C4 1.379(2) . ? C4 C5 1.380(2) . ? C5 C9 1.506(2) . ? C7A C8A 1.511(4) 2_567 ? C8A C7A 1.511(4) 2_567 ? C7B C8B 1.466(15) 2_567 ? C8B C7B 1.466(15) 2_567 ? C10 C11 1.481(2) . ? C12 C13 1.490(3) . ? 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 C1 N1 C5 118.46(13) . . ? C12 N2 C9 112.59(14) . . ? C12 N2 C8A 106.97(17) . . ? C9 N2 C8A 119.2(2) . . ? C12 N2 C8B 129.2(4) . . ? C9 N2 C8B 89.1(5) . . ? C8A N2 C8B 30.7(4) . . ? C10 N3 C7A 117.81(17) . . ? C10 N3 C6 111.94(12) . . ? C7A N3 C6 107.88(16) . . ? C10 N3 C7B 92.7(6) . . ? C7A N3 C7B 30.5(6) . . ? C6 N3 C7B 137.1(7) . . ? N1 C1 C2 122.51(14) . . ? N1 C1 C6 116.18(13) . . ? C2 C1 C6 121.25(13) . . ? C3 C2 C1 118.65(14) . . ? C2 C3 C4 119.36(14) . . ? C3 C4 C5 118.66(14) . . ? N1 C5 C4 122.25(14) . . ? N1 C5 C9 114.42(13) . . ? C4 C5 C9 123.29(14) . . ? N3 C6 C1 111.76(13) . . ? N3 C7A C8A 110.61(19) . 2_567 ? N2 C8A C7A 112.40(19) . 2_567 ? C8B C7B N3 109.8(9) 2_567 . ? C7B C8B N2 105.2(8) 2_567 . ? N2 C9 C5 114.92(13) . . ? N3 C10 C11 114.08(14) . . ? N4 C11 C10 177.66(19) . . ? N2 C12 C13 113.18(16) . . ? N5 C13 C12 176.5(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 72.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.347 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.033 #===END data_[ZnL1(NO3)2].2H2O _database_code_CSD 185885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ZnL(NO3)2.H2O _chemical_formula_sum 'C26 H34 N12 O8 Zn' _chemical_formula_weight 708.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 15.486(3) _cell_length_b 12.804(3) _cell_length_c 16.421(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.097(4) _cell_angle_gamma 90.00 _cell_volume 3128.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 992 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 26.38 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6798 _exptl_absorpt_correction_T_max 0.8214 _exptl_absorpt_process_details 'Sadabs, Sheldrick 1996' _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 'Smart-CCD-1000 Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9159 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3214 _reflns_number_gt 2733 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0507P)^2^+1.3509P] 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 3214 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Zn1 Zn 0.0000 0.30367(2) 0.2500 0.03363(11) Uani 1 2 d S . . N1 N 0.12230(10) 0.30310(11) 0.22314(10) 0.0365(3) Uani 1 1 d . . . N2 N 0.07633(10) 0.43678(11) 0.32967(9) 0.0340(3) Uani 1 1 d . . . N3 N -0.01282(11) 0.17036(12) 0.15654(11) 0.0456(4) Uani 1 1 d . . . N4 N 0.14119(19) 0.6170(2) 0.48692(17) 0.1014(9) Uani 1 1 d . . . N5 N -0.1245(2) 0.0039(3) -0.0048(3) 0.169(2) Uani 1 1 d . . . C1 C 0.19150(12) 0.35673(14) 0.27159(12) 0.0388(4) Uani 1 1 d . . . C2 C 0.27463(14) 0.35471(17) 0.25641(15) 0.0530(5) Uani 1 1 d . . . H2 H 0.3222 0.3933 0.2899 0.064 Uiso 1 1 calc R . . C3 C 0.28599(16) 0.29447(19) 0.19065(16) 0.0596(6) Uani 1 1 d . . . H3 H 0.3417 0.2917 0.1797 0.072 Uiso 1 1 calc R . . C4 C 0.21464(15) 0.23836(18) 0.14120(14) 0.0527(5) Uani 1 1 d . . . H4 H 0.2216 0.1970 0.0969 0.063 Uiso 1 1 calc R . . C5 C 0.13321(13) 0.24487(15) 0.15864(12) 0.0426(4) Uani 1 1 d . . . C6 C 0.17352(12) 0.41524(15) 0.34496(12) 0.0413(4) Uani 1 1 d . . . H6A H 0.1948 0.3743 0.3963 0.050 Uiso 1 1 calc R . . H6B H 0.2064 0.4807 0.3530 0.050 Uiso 1 1 calc R . . C7 C 0.04974(12) 0.52725(13) 0.27153(11) 0.0380(4) Uani 1 1 d . . . H7A H 0.0824 0.5248 0.2289 0.046 Uiso 1 1 calc R . . H7B H 0.0659 0.5915 0.3034 0.046 Uiso 1 1 calc R . . C8 C 0.01907(15) 0.07878(15) 0.21266(16) 0.0582(6) Uani 1 1 d . . . H8A H 0.0842 0.0801 0.2327 0.070 Uiso 1 1 calc R . . H8B H 0.0015 0.0150 0.1804 0.070 Uiso 1 1 calc R . . C9 C 0.04939(15) 0.19302(17) 0.10531(14) 0.0542(5) Uani 1 1 d . . . H9A H 0.0201 0.2384 0.0585 0.065 Uiso 1 1 calc R . . H9B H 0.0652 0.1285 0.0819 0.065 Uiso 1 1 calc R . . C10 C 0.05446(14) 0.45588(16) 0.41041(11) 0.0447(4) Uani 1 1 d . . . H10A H -0.0097 0.4677 0.3990 0.054 Uiso 1 1 calc R . . H10B H 0.0696 0.3944 0.4460 0.054 Uiso 1 1 calc R . . C11 C 0.10324(17) 0.5464(2) 0.45599(14) 0.0607(6) Uani 1 1 d . . . C12 C -0.10567(14) 0.15558(18) 0.10237(15) 0.0581(6) Uani 1 1 d . . . H12A H -0.1449 0.1437 0.1384 0.070 Uiso 1 1 calc R . . H12B H -0.1252 0.2193 0.0707 0.070 Uiso 1 1 calc R . . C13 C -0.11566(18) 0.0681(3) 0.0423(2) 0.0976(12) Uani 1 1 d . . . N1N N 0.66688(13) 0.14325(15) 0.11125(11) 0.0514(4) Uani 1 1 d . . . O1N O 0.69615(12) 0.19030(16) 0.05849(11) 0.0764(6) Uani 1 1 d . . . O2N O 0.58373(12) 0.14199(15) 0.10082(12) 0.0741(5) Uani 1 1 d . . . O3N O 0.71825(13) 0.09917(16) 0.17202(11) 0.0790(5) Uani 1 1 d . . . O1W O 0.4951(2) 0.3135(2) 0.1528(2) 0.1365(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 Zn1 0.02755(17) 0.03226(16) 0.04053(18) 0.000 0.00849(12) 0.000 N1 0.0307(8) 0.0385(8) 0.0400(8) 0.0001(6) 0.0094(6) 0.0028(6) N2 0.0334(8) 0.0359(7) 0.0314(7) -0.0008(6) 0.0067(6) -0.0022(6) N3 0.0345(9) 0.0401(8) 0.0573(10) -0.0127(7) 0.0046(8) 0.0047(7) N4 0.104(2) 0.107(2) 0.0845(17) -0.0541(17) 0.0122(15) -0.0199(17) N5 0.0727(19) 0.171(3) 0.233(4) -0.160(3) -0.006(2) 0.0154(19) C1 0.0309(9) 0.0389(9) 0.0450(10) 0.0073(8) 0.0080(8) -0.0002(8) C2 0.0345(11) 0.0536(12) 0.0715(14) 0.0065(11) 0.0157(10) -0.0041(10) C3 0.0409(12) 0.0692(15) 0.0772(16) 0.0124(12) 0.0305(12) 0.0100(11) C4 0.0505(13) 0.0593(13) 0.0546(12) 0.0062(10) 0.0250(11) 0.0183(11) C5 0.0403(11) 0.0435(10) 0.0447(10) 0.0014(8) 0.0128(9) 0.0103(9) C6 0.0315(9) 0.0437(10) 0.0441(10) -0.0021(8) 0.0029(8) -0.0062(8) C7 0.0438(11) 0.0327(9) 0.0361(9) -0.0002(7) 0.0090(8) -0.0053(8) C8 0.0427(12) 0.0331(10) 0.0922(18) -0.0078(10) 0.0076(11) 0.0046(9) C9 0.0491(13) 0.0581(13) 0.0542(12) -0.0193(10) 0.0123(10) 0.0119(10) C10 0.0467(11) 0.0530(11) 0.0337(9) -0.0015(8) 0.0102(8) -0.0002(9) C11 0.0637(15) 0.0730(15) 0.0428(12) -0.0184(11) 0.0104(11) 0.0006(13) C12 0.0392(12) 0.0548(12) 0.0706(15) -0.0269(11) -0.0010(11) 0.0059(10) C13 0.0438(14) 0.099(2) 0.132(3) -0.071(2) -0.0056(16) 0.0108(14) N1N 0.0504(11) 0.0579(11) 0.0454(10) -0.0067(8) 0.0123(9) -0.0124(9) O1N 0.0522(10) 0.1162(16) 0.0576(10) 0.0240(10) 0.0100(8) -0.0215(10) O2N 0.0500(10) 0.0936(13) 0.0827(12) -0.0041(10) 0.0248(9) -0.0166(9) O3N 0.0824(13) 0.0893(13) 0.0609(11) 0.0190(10) 0.0124(10) 0.0072(11) O1W 0.093(2) 0.112(2) 0.212(3) -0.0112(19) 0.053(2) 0.0013(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 Zn1 N1 2.0603(15) . ? Zn1 N1 2.0603(15) 2 ? Zn1 N3 2.2671(16) . ? Zn1 N3 2.2671(16) 2 ? Zn1 N2 2.2706(15) . ? Zn1 N2 2.2706(14) 2 ? N1 C1 1.334(2) . ? N1 C5 1.344(2) . ? N2 C10 1.477(2) . ? N2 C6 1.482(2) . ? N2 C7 1.485(2) . ? N3 C9 1.473(3) . ? N3 C12 1.478(3) . ? N3 C8 1.489(3) . ? N4 C11 1.121(3) . ? N5 C13 1.111(4) . ? C1 C2 1.378(3) . ? C1 C6 1.509(3) . ? C2 C3 1.377(3) . ? C3 C4 1.378(3) . ? C4 C5 1.371(3) . ? C5 C9 1.504(3) . ? C7 C7 1.506(4) 2 ? C8 C8 1.502(5) 2 ? C10 C11 1.470(3) . ? C12 C13 1.472(3) . ? N1N O3N 1.228(2) . ? N1N O1N 1.240(2) . ? N1N O2N 1.251(2) . ? 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 Zn1 N1 179.59(8) . 2 ? N1 Zn1 N3 76.44(6) . . ? N1 Zn1 N3 103.24(6) 2 . ? N1 Zn1 N3 103.24(6) . 2 ? N1 Zn1 N3 76.44(6) 2 2 ? N3 Zn1 N3 82.31(9) . 2 ? N1 Zn1 N2 76.32(6) . . ? N1 Zn1 N2 104.00(6) 2 . ? N3 Zn1 N2 152.76(6) . . ? N3 Zn1 N2 103.96(6) 2 . ? N1 Zn1 N2 104.00(6) . 2 ? N1 Zn1 N2 76.32(6) 2 2 ? N3 Zn1 N2 103.96(6) . 2 ? N3 Zn1 N2 152.76(6) 2 2 ? N2 Zn1 N2 82.72(7) . 2 ? C1 N1 C5 120.00(16) . . ? C1 N1 Zn1 120.30(12) . . ? C5 N1 Zn1 119.65(13) . . ? C10 N2 C6 110.72(14) . . ? C10 N2 C7 110.87(14) . . ? C6 N2 C7 109.98(14) . . ? C10 N2 Zn1 115.42(11) . . ? C6 N2 Zn1 107.46(10) . . ? C7 N2 Zn1 102.00(10) . . ? C9 N3 C12 111.26(18) . . ? C9 N3 C8 110.58(16) . . ? C12 N3 C8 111.85(17) . . ? C9 N3 Zn1 106.86(12) . . ? C12 N3 Zn1 113.06(12) . . ? C8 N3 Zn1 102.84(12) . . ? N1 C1 C2 121.24(18) . . ? N1 C1 C6 115.87(16) . . ? C2 C1 C6 122.84(18) . . ? C1 C2 C3 118.8(2) . . ? C2 C3 C4 119.88(19) . . ? C5 C4 C3 118.6(2) . . ? N1 C5 C4 121.49(19) . . ? N1 C5 C9 115.28(16) . . ? C4 C5 C9 123.15(18) . . ? N2 C6 C1 111.15(14) . . ? N2 C7 C7 111.53(13) . 2 ? N3 C8 C8 111.56(15) . 2 ? N3 C9 C5 110.48(17) . . ? C11 C10 N2 111.97(17) . . ? N4 C11 C10 176.4(3) . . ? C13 C12 N3 113.87(18) . . ? N5 C13 C12 178.1(4) . . ? O3N N1N O1N 120.8(2) . . ? O3N N1N O2N 121.04(19) . . ? O1N N1N O2N 118.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.308 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.045 #===END data_[Ag2L1(NO3)2] _database_code_CSD 185886 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Ag2 N12 O6' _chemical_formula_weight 822.36 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 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 9.439(4) _cell_length_b 9.229(4) _cell_length_c 17.967(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.414(7) _cell_angle_gamma 90.00 _cell_volume 1516.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 858 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 26.345 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8436 _exptl_absorpt_correction_T_max 0.8764 _exptl_absorpt_process_details Sadabs _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 'SMART CCD-1000 Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11688 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.47 _reflns_number_total 3109 _reflns_number_gt 2335 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0622P)^2^+1.3215P] 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 3109 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.84916(4) 0.03257(4) 0.99075(2) 0.04425(15) Uani 1 1 d . . . C1 C 0.9423(4) 0.0953(6) 0.8256(2) 0.0417(10) Uani 1 1 d . . . C2 C 0.9380(6) 0.1752(7) 0.7602(3) 0.0584(14) Uani 1 1 d . . . H2 H 0.9549 0.1306 0.7168 0.070 Uiso 1 1 calc R . . C3 C 0.9090(6) 0.3197(7) 0.7595(3) 0.0654(16) Uani 1 1 d . . . H3 H 0.9078 0.3753 0.7162 0.079 Uiso 1 1 calc R . . C4 C 0.8816(5) 0.3812(6) 0.8232(3) 0.0581(14) Uani 1 1 d . . . H4 H 0.8603 0.4796 0.8236 0.070 Uiso 1 1 calc R . . C5 C 0.8856(5) 0.2969(5) 0.8880(3) 0.0446(11) Uani 1 1 d . . . C6 C 0.8555(5) 0.3598(5) 0.9594(3) 0.0497(12) Uani 1 1 d . . . H6A H 0.9455 0.3603 0.9998 0.060 Uiso 1 1 calc R . . H6B H 0.8239 0.4595 0.9494 0.060 Uiso 1 1 calc R . . C7 C 0.7409(5) 0.3221(6) 1.0646(3) 0.0519(12) Uani 1 1 d . . . H7A H 0.6511 0.2878 1.0757 0.062 Uiso 1 1 calc R . . H7B H 0.7412 0.4271 1.0677 0.062 Uiso 1 1 calc R . . C8 C 0.8700(5) 0.2634(6) 1.1248(3) 0.0512(12) Uani 1 1 d . . . H8A H 0.9591 0.3044 1.1161 0.061 Uiso 1 1 calc R . . H8B H 0.8621 0.2952 1.1750 0.061 Uiso 1 1 calc R . . C9 C 1.0272(5) 0.0642(5) 1.1730(3) 0.0420(11) Uani 1 1 d . . . H9A H 1.0350 0.0972 1.2251 0.050 Uiso 1 1 calc R . . H9B H 1.1013 0.1144 1.1538 0.050 Uiso 1 1 calc R . . C10 C 0.5977(5) 0.3001(6) 0.9348(3) 0.0488(12) Uani 1 1 d . . . H10A H 0.5237 0.2787 0.9623 0.059 Uiso 1 1 calc R . . H10B H 0.5868 0.4008 0.9189 0.059 Uiso 1 1 calc R . . C11 C 0.5743(5) 0.2080(6) 0.8669(3) 0.0482(12) Uani 1 1 d . . . C12 C 0.7641(5) 0.0316(6) 1.1513(3) 0.0541(13) Uani 1 1 d . . . H12A H 0.7746 -0.0725 1.1475 0.065 Uiso 1 1 calc R . . H12B H 0.6703 0.0589 1.1181 0.065 Uiso 1 1 calc R . . C13 C 0.7668(6) 0.0700(8) 1.2319(4) 0.0655(16) Uani 1 1 d . . . N1 N 0.9164(4) 0.1548(4) 0.8891(2) 0.0378(8) Uani 1 1 d . . . N1N N 0.6830(4) -0.2344(4) 0.9512(2) 0.0460(9) Uani 1 1 d . . . N2 N 0.7426(4) 0.2790(4) 0.9864(2) 0.0415(9) Uani 1 1 d . . . N3 N 0.8816(4) 0.1041(4) 1.1249(2) 0.0403(8) Uani 1 1 d . . . N4 N 0.5537(6) 0.1381(6) 0.8138(3) 0.0733(15) Uani 1 1 d . . . N5 N 0.7749(6) 0.0989(8) 1.2940(3) 0.0900(19) Uani 1 1 d . . . O1N O 0.8115(4) -0.2265(5) 0.9508(3) 0.0791(13) Uani 1 1 d . . . O2N O 0.6230(5) -0.1241(5) 0.9685(3) 0.0857(14) Uani 1 1 d . . . O3N O 0.6125(4) -0.3452(4) 0.9326(3) 0.0763(13) 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 0.0549(2) 0.0339(2) 0.0437(2) -0.00424(16) 0.01199(16) -0.00488(16) C1 0.035(2) 0.052(3) 0.037(2) 0.005(2) 0.0063(17) -0.004(2) C2 0.053(3) 0.074(4) 0.048(3) 0.019(3) 0.013(2) 0.001(3) C3 0.059(3) 0.075(5) 0.061(4) 0.031(3) 0.013(3) 0.000(3) C4 0.048(3) 0.040(3) 0.081(4) 0.024(3) 0.006(3) -0.003(2) C5 0.035(2) 0.036(3) 0.060(3) 0.008(2) 0.006(2) -0.0056(19) C6 0.044(2) 0.030(3) 0.072(3) -0.009(2) 0.009(2) -0.004(2) C7 0.052(3) 0.050(3) 0.050(3) -0.014(2) 0.006(2) 0.009(2) C8 0.053(3) 0.045(3) 0.050(3) -0.013(2) 0.003(2) 0.001(2) C9 0.034(2) 0.052(3) 0.038(2) -0.005(2) 0.0059(18) -0.0034(19) C10 0.038(2) 0.052(3) 0.054(3) -0.009(2) 0.005(2) 0.002(2) C11 0.039(2) 0.041(3) 0.058(3) 0.004(2) -0.002(2) -0.002(2) C12 0.036(2) 0.070(4) 0.055(3) -0.003(3) 0.010(2) -0.005(2) C13 0.046(3) 0.091(5) 0.064(4) -0.004(3) 0.022(3) -0.006(3) N1 0.0354(17) 0.035(2) 0.044(2) 0.0059(16) 0.0102(15) 0.0000(15) N1N 0.046(2) 0.039(2) 0.054(2) -0.0031(19) 0.0141(18) -0.0093(18) N2 0.0346(17) 0.040(2) 0.046(2) -0.0079(17) 0.0031(15) 0.0008(16) N3 0.0358(18) 0.043(2) 0.0408(19) -0.0059(17) 0.0067(15) 0.0007(16) N4 0.075(3) 0.062(4) 0.066(3) -0.015(3) -0.012(3) 0.004(3) N5 0.074(3) 0.135(6) 0.070(4) -0.013(4) 0.033(3) -0.017(4) O1N 0.047(2) 0.065(3) 0.128(4) 0.006(3) 0.027(2) -0.0061(19) O2N 0.082(3) 0.044(3) 0.143(4) -0.023(3) 0.051(3) -0.010(2) O3N 0.068(2) 0.048(2) 0.118(4) -0.027(2) 0.032(2) -0.022(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 2.363(4) . ? Ag1 N3 2.444(4) . ? Ag1 N2 2.480(4) . ? Ag1 O1N 2.496(5) . ? Ag1 O2N 2.527(4) . ? Ag1 Ag1 2.8476(14) 3_757 ? C1 N1 1.343(6) . ? C1 C2 1.379(7) . ? C1 C9 1.499(7) 3_757 ? C2 C3 1.360(9) . ? C2 H2 0.9300 . ? C3 C4 1.360(8) . ? C3 H3 0.9300 . ? C4 C5 1.392(7) . ? C4 H4 0.9300 . ? C5 N1 1.343(6) . ? C5 C6 1.498(7) . ? C6 N2 1.479(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.465(6) . ? C7 C8 1.513(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.475(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N3 1.476(5) . ? C9 C1 1.499(7) 3_757 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.458(7) . ? C10 N2 1.462(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.128(7) . ? C12 N3 1.471(6) . ? C12 C13 1.485(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N5 1.130(7) . ? N1N O1N 1.217(5) . ? N1N O3N 1.220(5) . ? N1N O2N 1.242(6) . ? 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 129.90(14) . . ? N1 Ag1 N2 73.92(13) . . ? N3 Ag1 N2 74.55(13) . . ? N1 Ag1 O1N 106.34(15) . . ? N3 Ag1 O1N 121.07(16) . . ? N2 Ag1 O1N 147.31(13) . . ? N1 Ag1 O2N 121.96(16) . . ? N3 Ag1 O2N 101.79(15) . . ? N2 Ag1 O2N 101.52(14) . . ? O1N Ag1 O2N 49.61(13) . . ? N1 Ag1 Ag1 74.81(9) . 3_757 ? N3 Ag1 Ag1 93.77(8) . 3_757 ? N2 Ag1 Ag1 125.68(9) . 3_757 ? O1N Ag1 Ag1 84.15(9) . 3_757 ? O2N Ag1 Ag1 132.74(11) . 3_757 ? N1 C1 C2 122.2(5) . . ? N1 C1 C9 117.4(4) . 3_757 ? C2 C1 C9 120.3(5) . 3_757 ? C3 C2 C1 119.6(6) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.8(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 121.3(5) . . ? N1 C5 C6 116.9(4) . . ? C4 C5 C6 121.8(5) . . ? N2 C6 C5 113.1(4) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 112.8(4) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C7 113.9(4) . . ? N3 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N3 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N3 C9 C1 113.7(4) . 3_757 ? N3 C9 H9A 108.8 . . ? C1 C9 H9A 108.8 3_757 . ? N3 C9 H9B 108.8 . . ? C1 C9 H9B 108.8 3_757 . ? H9A C9 H9B 107.7 . . ? C11 C10 N2 112.1(4) . . ? C11 C10 H10A 109.2 . . ? N2 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? N2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N4 C11 C10 178.6(6) . . ? N3 C12 C13 112.0(4) . . ? N3 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N3 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N5 C13 C12 177.2(6) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Ag1 127.1(3) . . ? C5 N1 Ag1 112.3(3) . . ? O1N N1N O3N 121.7(5) . . ? O1N N1N O2N 118.0(4) . . ? O3N N1N O2N 120.3(4) . . ? C10 N2 C7 109.9(4) . . ? C10 N2 C6 111.2(4) . . ? C7 N2 C6 111.0(4) . . ? C10 N2 Ag1 116.8(3) . . ? C7 N2 Ag1 108.7(3) . . ? C6 N2 Ag1 98.8(3) . . ? C9 N3 C8 107.9(4) . . ? C9 N3 C12 111.4(4) . . ? C8 N3 C12 113.1(4) . . ? C9 N3 Ag1 112.3(3) . . ? C8 N3 Ag1 106.0(3) . . ? C12 N3 Ag1 106.0(3) . . ? N1N O1N Ag1 97.3(3) . . ? N1N O2N Ag1 95.1(3) . . ? 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 C1 C2 C3 1.1(8) . . . . ? C9 C1 C2 C3 179.4(5) 3_757 . . . ? C1 C2 C3 C4 -1.4(8) . . . . ? C2 C3 C4 C5 0.8(8) . . . . ? C3 C4 C5 N1 0.2(7) . . . . ? C3 C4 C5 C6 -179.7(5) . . . . ? N1 C5 C6 N2 -52.1(5) . . . . ? C4 C5 C6 N2 127.7(5) . . . . ? N2 C7 C8 N3 -58.1(6) . . . . ? N2 C10 C11 N4 -175(100) . . . . ? N3 C12 C13 N5 -40(16) . . . . ? C2 C1 N1 C5 -0.1(6) . . . . ? C9 C1 N1 C5 -178.5(4) 3_757 . . . ? C2 C1 N1 Ag1 160.3(4) . . . . ? C9 C1 N1 Ag1 -18.1(5) 3_757 . . . ? C4 C5 N1 C1 -0.5(6) . . . . ? C6 C5 N1 C1 179.3(4) . . . . ? C4 C5 N1 Ag1 -163.7(3) . . . . ? C6 C5 N1 Ag1 16.2(5) . . . . ? N3 Ag1 N1 C1 155.6(3) . . . . ? N2 Ag1 N1 C1 -151.4(4) . . . . ? O1N Ag1 N1 C1 -5.5(4) . . . . ? O2N Ag1 N1 C1 -57.7(4) . . . . ? Ag1 Ag1 N1 C1 73.6(3) 3_757 . . . ? N3 Ag1 N1 C5 -43.1(3) . . . . ? N2 Ag1 N1 C5 9.9(3) . . . . ? O1N Ag1 N1 C5 155.8(3) . . . . ? O2N Ag1 N1 C5 103.6(3) . . . . ? Ag1 Ag1 N1 C5 -125.1(3) 3_757 . . . ? C11 C10 N2 C7 -156.4(4) . . . . ? C11 C10 N2 C6 80.3(5) . . . . ? C11 C10 N2 Ag1 -32.0(5) . . . . ? C8 C7 N2 C10 162.9(4) . . . . ? C8 C7 N2 C6 -73.6(5) . . . . ? C8 C7 N2 Ag1 34.0(5) . . . . ? C5 C6 N2 C10 -70.5(5) . . . . ? C5 C6 N2 C7 166.8(4) . . . . ? C5 C6 N2 Ag1 52.8(4) . . . . ? N1 Ag1 N2 C10 87.3(3) . . . . ? N3 Ag1 N2 C10 -132.1(3) . . . . ? O1N Ag1 N2 C10 -8.0(5) . . . . ? O2N Ag1 N2 C10 -32.9(3) . . . . ? Ag1 Ag1 N2 C10 144.5(3) 3_757 . . . ? N1 Ag1 N2 C7 -147.7(3) . . . . ? N3 Ag1 N2 C7 -7.2(3) . . . . ? O1N Ag1 N2 C7 116.9(3) . . . . ? O2N Ag1 N2 C7 92.0(3) . . . . ? Ag1 Ag1 N2 C7 -90.6(3) 3_757 . . . ? N1 Ag1 N2 C6 -31.9(3) . . . . ? N3 Ag1 N2 C6 108.7(3) . . . . ? O1N Ag1 N2 C6 -127.2(3) . . . . ? O2N Ag1 N2 C6 -152.1(3) . . . . ? Ag1 Ag1 N2 C6 25.3(3) 3_757 . . . ? C1 C9 N3 C8 -176.5(4) 3_757 . . . ? C1 C9 N3 C12 58.7(5) 3_757 . . . ? C1 C9 N3 Ag1 -60.0(4) 3_757 . . . ? C7 C8 N3 C9 167.4(4) . . . . ? C7 C8 N3 C12 -68.9(5) . . . . ? C7 C8 N3 Ag1 46.9(5) . . . . ? C13 C12 N3 C9 59.8(6) . . . . ? C13 C12 N3 C8 -62.0(6) . . . . ? C13 C12 N3 Ag1 -177.8(4) . . . . ? N1 Ag1 N3 C9 -84.9(3) . . . . ? N2 Ag1 N3 C9 -137.7(3) . . . . ? O1N Ag1 N3 C9 73.8(3) . . . . ? O2N Ag1 N3 C9 123.5(3) . . . . ? Ag1 Ag1 N3 C9 -11.6(3) 3_757 . . . ? N1 Ag1 N3 C8 32.7(3) . . . . ? N2 Ag1 N3 C8 -20.0(3) . . . . ? O1N Ag1 N3 C8 -168.6(3) . . . . ? O2N Ag1 N3 C8 -118.9(3) . . . . ? Ag1 Ag1 N3 C8 106.0(3) 3_757 . . . ? N1 Ag1 N3 C12 153.2(3) . . . . ? N2 Ag1 N3 C12 100.5(3) . . . . ? O1N Ag1 N3 C12 -48.1(3) . . . . ? O2N Ag1 N3 C12 1.6(3) . . . . ? Ag1 Ag1 N3 C12 -133.5(3) 3_757 . . . ? O3N N1N O1N Ag1 178.0(4) . . . . ? O2N N1N O1N Ag1 0.6(5) . . . . ? N1 Ag1 O1N N1N -118.7(3) . . . . ? N3 Ag1 O1N N1N 78.2(4) . . . . ? N2 Ag1 O1N N1N -33.1(5) . . . . ? O2N Ag1 O1N N1N -0.3(3) . . . . ? Ag1 Ag1 O1N N1N 169.0(3) 3_757 . . . ? O1N N1N O2N Ag1 -0.6(5) . . . . ? O3N N1N O2N Ag1 -178.1(4) . . . . ? N1 Ag1 O2N N1N 84.8(4) . . . . ? N3 Ag1 O2N N1N -120.7(3) . . . . ? N2 Ag1 O2N N1N 163.0(3) . . . . ? O1N Ag1 O2N N1N 0.3(3) . . . . ? Ag1 Ag1 O2N N1N -14.1(4) 3_757 . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.003 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.115 #===END data_[Ag2L1](ClO4)2.4CH3CN _database_code_CSD 185887 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Ag2 Cl2 N14 O8' _chemical_formula_weight 1061.46 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' 'Cl' 'Cl' 0.1484 0.1585 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.423(4) _cell_length_b 18.521(7) _cell_length_c 11.133(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.304(6) _cell_angle_gamma 90.00 _cell_volume 2179.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5866 _exptl_absorpt_correction_T_max 0.8370 _exptl_absorpt_process_details Sadabs _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 'Smart-CCD-1000-Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11781 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.47 _reflns_number_total 4420 _reflns_number_gt 3697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Shelxtl' _computing_structure_solution 'SIR-92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0285P)^2^+2.2469P] 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 4420 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C 0.1909(2) 0.01723(14) 0.4978(2) 0.0176(5) Uani 1 1 d . . . C1S C 0.7582(3) 0.08324(15) 0.8146(3) 0.0273(6) Uani 1 1 d . . . C2 C 0.0862(2) -0.00909(15) 0.3976(3) 0.0212(5) Uani 1 1 d . . . H2 H 0.0422 -0.0488 0.4100 0.025 Uiso 1 1 calc R . . C2S C 0.8748(3) 0.09717(18) 0.9236(3) 0.0360(7) Uani 1 1 d . . . H2S1 H 0.8619 0.1355 0.9754 0.054 Uiso 1 1 calc R . . H2S2 H 0.9392 0.1110 0.8924 0.054 Uiso 1 1 calc R . . H2S3 H 0.9008 0.0543 0.9754 0.054 Uiso 1 1 calc R . . C3 C 0.0478(3) 0.02479(15) 0.2780(3) 0.0246(6) Uani 1 1 d . . . H3 H -0.0233 0.0085 0.2092 0.030 Uiso 1 1 calc R . . C3S C 0.1130(4) 0.7732(2) 0.3656(5) 0.0605(11) Uani 1 1 d . . . C4 C 0.1158(3) 0.08277(15) 0.2617(2) 0.0230(6) Uani 1 1 d . . . H4 H 0.0920 0.1058 0.1817 0.028 Uiso 1 1 calc R . . C4S C 0.0765(5) 0.7402(2) 0.2371(4) 0.0708(13) Uani 1 1 d . . . H4S1 H 0.0646 0.6892 0.2435 0.106 Uiso 1 1 calc R . . H4S2 H 0.1419 0.7482 0.2042 0.106 Uiso 1 1 calc R . . H4S3 H -0.0010 0.7615 0.1791 0.106 Uiso 1 1 calc R . . C5 C 0.2201(2) 0.10611(13) 0.3662(2) 0.0170(5) Uani 1 1 d . . . C6 C 0.2952(2) 0.17181(14) 0.3601(2) 0.0190(5) Uani 1 1 d . . . H6A H 0.2686 0.1878 0.2707 0.023 Uiso 1 1 calc R . . H6B H 0.2785 0.2105 0.4101 0.023 Uiso 1 1 calc R . . C7 C 0.4630(2) 0.11043(13) 0.3191(2) 0.0169(5) Uani 1 1 d . . . H7A H 0.4404 0.1355 0.2369 0.020 Uiso 1 1 calc R . . H7B H 0.4140 0.0662 0.3038 0.020 Uiso 1 1 calc R . . C8 C 0.6026(2) 0.09208(14) 0.3709(2) 0.0177(5) Uani 1 1 d . . . H8A H 0.6489 0.1323 0.3546 0.021 Uiso 1 1 calc R . . H8B H 0.6323 0.0852 0.4641 0.021 Uiso 1 1 calc R . . C9 C 0.7659(2) 0.01218(14) 0.3656(2) 0.0197(5) Uani 1 1 d . . . H9A H 0.8111 0.0566 0.3661 0.024 Uiso 1 1 calc R . . H9B H 0.7864 -0.0223 0.3109 0.024 Uiso 1 1 calc R . . C10 C 0.5058(2) 0.22257(13) 0.4456(2) 0.0191(5) Uani 1 1 d . . . H10A H 0.5945 0.2102 0.4895 0.023 Uiso 1 1 calc R . . H10B H 0.4803 0.2501 0.5057 0.023 Uiso 1 1 calc R . . C11 C 0.4911(3) 0.26815(15) 0.3320(3) 0.0260(6) Uani 1 1 d . . . C12 C 0.5811(2) 0.03021(14) 0.1691(2) 0.0196(5) Uani 1 1 d . . . H12A H 0.4900 0.0364 0.1363 0.024 Uiso 1 1 calc R . . H12B H 0.5984 -0.0152 0.1358 0.024 Uiso 1 1 calc R . . C13 C 0.6369(3) 0.08985(16) 0.1192(3) 0.0271(6) Uani 1 1 d . . . N1 N 0.25669(19) 0.07345(11) 0.48187(19) 0.0174(4) Uani 1 1 d . . . N1S N 0.6670(2) 0.07247(15) 0.7300(3) 0.0366(6) Uani 1 1 d . . . N2 N 0.43175(19) 0.15633(11) 0.41148(19) 0.0156(4) Uani 1 1 d . . . N2S N 0.1402(4) 0.7978(2) 0.4637(5) 0.0909(14) Uani 1 1 d . . . N3 N 0.62922(19) 0.02642(11) 0.31078(19) 0.0164(4) Uani 1 1 d . . . N4 N 0.4764(3) 0.20030(14) 0.7404(3) 0.0399(7) Uani 1 1 d . . . N5 N 0.6815(3) 0.13625(16) 0.0857(3) 0.0391(6) Uani 1 1 d . . . O1 O 0.1840(2) 0.17418(13) 1.0112(2) 0.0458(6) Uani 1 1 d . . . O2 O 0.1413(2) 0.12064(14) 0.8100(2) 0.0454(6) Uani 1 1 d . . . O3 O 0.2151(3) 0.05026(13) 0.9969(3) 0.0538(7) Uani 1 1 d . . . O4 O 0.3504(2) 0.13207(13) 0.9583(2) 0.0426(6) Uani 1 1 d . . . Cl1 Cl 0.22285(6) 0.11954(4) 0.94402(6) 0.02285(14) Uani 1 1 d . . . Ag1 Ag 0.458683(19) 0.092083(11) 0.624928(18) 0.02143(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0153(12) 0.0193(13) 0.0204(12) 0.0002(10) 0.0092(10) 0.0040(10) C1S 0.0220(15) 0.0275(16) 0.0335(16) 0.0023(12) 0.0117(13) 0.0030(12) C2 0.0160(12) 0.0249(14) 0.0256(13) -0.0023(10) 0.0113(10) -0.0017(11) C2S 0.0249(16) 0.0413(19) 0.0366(17) -0.0002(14) 0.0059(13) -0.0083(14) C3 0.0164(13) 0.0335(16) 0.0225(13) -0.0066(11) 0.0058(11) -0.0016(11) C3S 0.049(2) 0.039(2) 0.077(3) 0.007(2) 0.006(2) -0.0052(19) C4 0.0207(13) 0.0304(15) 0.0171(12) 0.0013(10) 0.0061(10) 0.0037(11) C4S 0.075(3) 0.054(3) 0.073(3) 0.018(2) 0.017(2) 0.003(2) C5 0.0144(12) 0.0204(13) 0.0177(12) 0.0004(9) 0.0080(10) 0.0041(10) C6 0.0179(13) 0.0187(13) 0.0205(12) 0.0021(10) 0.0074(10) 0.0051(10) C7 0.0177(13) 0.0171(13) 0.0154(11) -0.0014(9) 0.0058(10) 0.0008(10) C8 0.0171(13) 0.0196(13) 0.0164(11) -0.0027(9) 0.0065(10) -0.0016(10) C9 0.0174(13) 0.0226(14) 0.0210(13) 0.0018(10) 0.0094(10) 0.0006(10) C10 0.0229(13) 0.0163(13) 0.0197(12) -0.0007(10) 0.0098(10) -0.0020(10) C11 0.0311(15) 0.0172(14) 0.0346(15) 0.0014(12) 0.0181(13) -0.0015(12) C12 0.0217(13) 0.0237(14) 0.0144(12) -0.0012(9) 0.0078(10) 0.0004(11) C13 0.0295(15) 0.0348(16) 0.0169(12) 0.0023(11) 0.0087(11) 0.0066(13) N1 0.0143(11) 0.0204(11) 0.0182(10) -0.0009(8) 0.0069(9) 0.0032(8) N1S 0.0215(14) 0.0398(16) 0.0406(15) 0.0010(12) 0.0030(12) 0.0047(11) N2 0.0179(11) 0.0136(10) 0.0160(10) -0.0009(8) 0.0072(8) 0.0002(8) N2S 0.087(3) 0.077(3) 0.084(3) -0.018(2) 0.004(3) -0.014(3) N3 0.0169(11) 0.0191(11) 0.0142(10) 0.0001(8) 0.0069(8) 0.0009(8) N4 0.0527(18) 0.0303(15) 0.0427(16) -0.0123(12) 0.0247(14) -0.0003(13) N5 0.0405(16) 0.0433(17) 0.0370(15) 0.0113(12) 0.0186(13) -0.0001(13) O1 0.0539(15) 0.0490(15) 0.0358(12) -0.0095(10) 0.0184(11) 0.0122(12) O2 0.0448(14) 0.0560(15) 0.0239(11) -0.0082(10) 0.0001(10) 0.0042(12) O3 0.0627(17) 0.0328(14) 0.0656(17) 0.0158(12) 0.0239(14) -0.0107(12) O4 0.0228(11) 0.0439(14) 0.0628(15) 0.0035(11) 0.0181(11) -0.0063(10) Cl1 0.0215(3) 0.0221(3) 0.0239(3) -0.0002(2) 0.0075(3) -0.0025(3) Ag1 0.01984(11) 0.02240(11) 0.01815(10) 0.00022(8) 0.00283(7) -0.00294(8) _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 C1 N1 1.335(3) . ? C1 C2 1.379(4) . ? C1 C9 1.511(3) 3_656 ? C1S N1S 1.126(4) . ? C1S C2S 1.444(4) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C3S N2S 1.113(6) . ? C3S C4S 1.464(7) . ? C4 C5 1.381(4) . ? C4 H4 0.9300 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C5 N1 1.338(3) . ? C5 C6 1.505(4) . ? C6 N2 1.472(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.479(3) . ? C7 C8 1.513(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.474(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N3 1.468(3) . ? C9 C1 1.511(3) 3_656 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.456(3) . ? C10 C11 1.476(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.131(4) 4_565 ? C12 N3 1.462(3) . ? C12 C13 1.485(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N5 1.132(4) . ? N1 Ag1 2.278(2) . ? N1S Ag1 2.248(3) . ? N2 Ag1 2.569(2) . ? N3 Ag1 2.624(2) 3_656 ? N4 C11 1.131(4) 4_566 ? N4 Ag1 2.348(3) . ? O1 Cl1 1.426(2) . ? O2 Cl1 1.428(2) . ? O3 Cl1 1.429(2) . ? O4 Cl1 1.424(2) . ? Ag1 N3 2.624(2) 3_656 ? 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 C1 C2 121.8(2) . . ? N1 C1 C9 115.5(2) . 3_656 ? C2 C1 C9 122.6(2) . 3_656 ? N1S C1S C2S 179.7(4) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? N2S C3S C4S 179.3(5) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N1 C5 C4 121.6(2) . . ? N1 C5 C6 115.7(2) . . ? C4 C5 C6 122.6(2) . . ? N2 C6 C5 111.3(2) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 111.2(2) . . ? N2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C7 112.4(2) . . ? N3 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N3 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N3 C9 C1 111.9(2) . 3_656 ? N3 C9 H9A 109.2 . . ? C1 C9 H9A 109.2 3_656 . ? N3 C9 H9B 109.2 . . ? C1 C9 H9B 109.2 3_656 . ? H9A C9 H9B 107.9 . . ? N2 C10 C11 113.1(2) . . ? N2 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N4 C11 C10 175.9(3) 4_565 . ? N3 C12 C13 113.6(2) . . ? N3 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N3 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N5 C13 C12 177.5(3) . . ? C1 N1 C5 119.6(2) . . ? C1 N1 Ag1 119.81(16) . . ? C5 N1 Ag1 117.91(16) . . ? C1S N1S Ag1 150.1(3) . . ? C10 N2 C6 111.3(2) . . ? C10 N2 C7 113.31(19) . . ? C6 N2 C7 110.01(19) . . ? C10 N2 Ag1 107.17(14) . . ? C6 N2 Ag1 100.77(14) . . ? C7 N2 Ag1 113.64(14) . . ? C12 N3 C9 111.25(19) . . ? C12 N3 C8 113.08(19) . . ? C9 N3 C8 109.25(19) . . ? C12 N3 Ag1 107.95(15) . 3_656 ? C9 N3 Ag1 101.13(14) . 3_656 ? C8 N3 Ag1 113.57(14) . 3_656 ? C11 N4 Ag1 152.5(3) 4_566 . ? O4 Cl1 O1 109.56(15) . . ? O4 Cl1 O3 108.76(15) . . ? O1 Cl1 O3 109.92(16) . . ? O4 Cl1 O2 110.38(15) . . ? O1 Cl1 O2 109.20(14) . . ? O3 Cl1 O2 109.00(16) . . ? N1S Ag1 N1 158.56(9) . . ? N1S Ag1 N4 89.95(10) . . ? N1 Ag1 N4 111.46(9) . . ? N1S Ag1 N2 106.70(9) . . ? N1 Ag1 N2 71.92(7) . . ? N4 Ag1 N2 93.79(9) . . ? N1S Ag1 N3 99.34(9) . 3_656 ? N1 Ag1 N3 70.91(7) . 3_656 ? N4 Ag1 N3 121.81(8) . 3_656 ? N2 Ag1 N3 135.71(6) . 3_656 ? 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 C1 C2 C3 -1.0(4) . . . . ? C9 C1 C2 C3 175.0(2) 3_656 . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C3 C4 C5 N1 0.6(4) . . . . ? C3 C4 C5 C6 -176.0(2) . . . . ? N1 C5 C6 N2 51.9(3) . . . . ? C4 C5 C6 N2 -131.4(2) . . . . ? N2 C7 C8 N3 157.78(19) . . . . ? N2 C10 C11 N4 -12(5) . . . 4_565 ? N3 C12 C13 N5 -9(7) . . . . ? C2 C1 N1 C5 0.8(4) . . . . ? C9 C1 N1 C5 -175.5(2) 3_656 . . . ? C2 C1 N1 Ag1 -160.46(19) . . . . ? C9 C1 N1 Ag1 23.2(3) 3_656 . . . ? C4 C5 N1 C1 -0.5(4) . . . . ? C6 C5 N1 C1 176.3(2) . . . . ? C4 C5 N1 Ag1 161.04(19) . . . . ? C6 C5 N1 Ag1 -22.2(3) . . . . ? C2S C1S N1S Ag1 21(92) . . . . ? C11 C10 N2 C6 -66.2(3) . . . . ? C11 C10 N2 C7 58.4(3) . . . . ? C11 C10 N2 Ag1 -175.46(17) . . . . ? C5 C6 N2 C10 -161.2(2) . . . . ? C5 C6 N2 C7 72.4(2) . . . . ? C5 C6 N2 Ag1 -47.9(2) . . . . ? C8 C7 N2 C10 56.1(3) . . . . ? C8 C7 N2 C6 -178.6(2) . . . . ? C8 C7 N2 Ag1 -66.5(2) . . . . ? C13 C12 N3 C9 -62.4(3) . . . . ? C13 C12 N3 C8 61.0(3) . . . . ? C13 C12 N3 Ag1 -172.48(18) . . . 3_656 ? C1 C9 N3 C12 -160.2(2) 3_656 . . . ? C1 C9 N3 C8 74.3(3) 3_656 . . . ? C1 C9 N3 Ag1 -45.7(2) 3_656 . . 3_656 ? C7 C8 N3 C12 55.5(3) . . . . ? C7 C8 N3 C9 180.0(2) . . . . ? C7 C8 N3 Ag1 -68.0(2) . . . 3_656 ? C1S N1S Ag1 N1 -163.4(4) . . . . ? C1S N1S Ag1 N4 19.7(5) . . . . ? C1S N1S Ag1 N2 113.6(5) . . . . ? C1S N1S Ag1 N3 -102.6(5) . . . 3_656 ? C1 N1 Ag1 N1S 67.9(3) . . . . ? C5 N1 Ag1 N1S -93.7(3) . . . . ? C1 N1 Ag1 N4 -115.46(19) . . . . ? C5 N1 Ag1 N4 83.01(19) . . . . ? C1 N1 Ag1 N2 157.62(19) . . . . ? C5 N1 Ag1 N2 -3.91(17) . . . . ? C1 N1 Ag1 N3 2.15(17) . . . 3_656 ? C5 N1 Ag1 N3 -159.39(19) . . . 3_656 ? C11 N4 Ag1 N1S -71.0(6) 4_566 . . . ? C11 N4 Ag1 N1 110.2(6) 4_566 . . . ? C11 N4 Ag1 N2 -177.7(6) 4_566 . . . ? C11 N4 Ag1 N3 30.0(6) 4_566 . . 3_656 ? C10 N2 Ag1 N1S -58.36(17) . . . . ? C6 N2 Ag1 N1S -174.78(15) . . . . ? C7 N2 Ag1 N1S 67.61(17) . . . . ? C10 N2 Ag1 N1 144.08(16) . . . . ? C6 N2 Ag1 N1 27.65(14) . . . . ? C7 N2 Ag1 N1 -89.95(16) . . . . ? C10 N2 Ag1 N4 32.73(16) . . . . ? C6 N2 Ag1 N4 -83.70(15) . . . . ? C7 N2 Ag1 N4 158.70(16) . . . . ? C10 N2 Ag1 N3 178.26(14) . . . 3_656 ? C6 N2 Ag1 N3 61.83(17) . . . 3_656 ? C7 N2 Ag1 N3 -55.77(19) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.553 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.075