# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wanzhi Chen' _publ_contact_author_address ; Department of Chemistry Zhejiang University Tianmushan Road 148 Hangzhou 310028 CHINA ; _publ_contact_author_email CHENWZZ@ZJU.EDU.CN _publ_section_title ; Mononuclear, Dinuclear, Hexanuclear, and One-dimensional Polymeric Silver Complexes Having Ligand-Supported and Unsupported Argentophilic Interactions Stabilized by Pincer-like 2,6-Bis(5-pyrazolyl)pyridine Ligands ; loop_ _publ_author_name 'Wanzhi Chen' 'DaQi Wang' 'Yongbo Zhou' data_ligand_1 _database_code_depnum_ccdc_archive 'CCDC 655894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H14 N5 O0.50' _chemical_formula_sum 'C13 H14 N5 O0.50' _chemical_formula_weight 248.29 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z' 'x-1/2, -y, z' _cell_length_a 8.226(2) _cell_length_b 24.045(6) _cell_length_c 6.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1281.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1413 _cell_measurement_theta_min 2.541 _cell_measurement_theta_max 21.8 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9595 _exptl_absorpt_correction_T_max 0.9700 _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 'Bruker SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6085 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1146 _reflns_number_gt 593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+0.4485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1146 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2132 _refine_ls_wR_factor_gt 0.1724 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.7500 0.11147(15) 0.5000 0.0676(11) Uani 1 2 d S . . N2 N 0.5967(3) 0.17179(12) 0.7985(4) 0.0703(9) Uani 1 1 d . . . H6 H 0.6413 0.1910 0.7019 0.084 Uiso 1 1 calc R . . N3 N 0.5189(3) 0.19312(15) 0.9637(5) 0.0821(11) Uani 1 1 d . . . C1 C 0.6737(4) 0.08333(15) 0.6495(7) 0.0853(13) Uani 1 1 d . . . C6 C 0.5942(4) 0.11679(17) 0.8072(6) 0.0782(11) Uani 1 1 d . . . C7 C 0.5097(5) 0.1021(3) 0.9836(9) 0.1089(17) Uani 1 1 d . . . H7 H 0.4873 0.0663 1.0292 0.131 Uiso 1 1 calc R . . C8 C 0.4652(5) 0.1512(3) 1.0787(7) 0.1019(17) Uani 1 1 d . . . C9 C 0.3781(6) 0.1608(3) 1.2748(7) 0.144(2) Uani 1 1 d . . . H9A H 0.3231 0.1960 1.2692 0.216 Uiso 1 1 calc R . . H9B H 0.4545 0.1610 1.3868 0.216 Uiso 1 1 calc R . . H9C H 0.3001 0.1316 1.2959 0.216 Uiso 1 1 calc R . . O1 O 0.7500 0.2500 0.5000 0.0762(14) Uani 1 4 d S . . C2 C 0.6716(7) 0.02566(18) 0.6518(12) 0.154(3) Uani 1 1 d . . . H2 H 0.6172 0.0066 0.7559 0.185 Uiso 1 1 calc R . . C3 C 0.7500 -0.0026(3) 0.5000 0.202(6) Uani 1 2 d S . . H3 H 0.7500 -0.0413 0.5000 0.243 Uiso 1 2 calc SR . . 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 0.055(2) 0.048(2) 0.100(3) 0.000 -0.008(2) 0.000 N2 0.0634(19) 0.079(2) 0.068(2) 0.0168(15) -0.0016(15) -0.0095(15) N3 0.0607(18) 0.132(3) 0.0534(17) 0.0083(18) 0.0012(16) -0.0118(18) C1 0.060(2) 0.058(2) 0.138(4) 0.023(2) -0.007(2) -0.0058(19) C6 0.059(2) 0.073(3) 0.103(3) 0.031(2) -0.011(2) -0.009(2) C7 0.075(3) 0.134(4) 0.118(4) 0.072(4) -0.011(3) -0.031(3) C8 0.058(2) 0.178(5) 0.070(3) 0.045(3) -0.010(2) -0.025(3) C9 0.077(3) 0.284(8) 0.070(3) 0.039(3) 0.005(3) -0.031(4) O1 0.103(4) 0.052(2) 0.073(3) 0.000 0.000 0.000 C2 0.117(4) 0.053(3) 0.293(8) 0.045(4) 0.039(5) -0.002(3) C3 0.148(8) 0.041(4) 0.418(18) 0.000 0.042(11) 0.000 _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 1.338(4) 4_656 ? N1 C1 1.338(4) . ? N2 C6 1.324(5) . ? N2 N3 1.349(4) . ? N2 H6 0.8600 . ? N3 C8 1.328(5) . ? C1 C2 1.387(6) . ? C1 C6 1.455(6) . ? C6 C7 1.383(6) . ? C7 C8 1.381(7) . ? C7 H7 0.9300 . ? C8 C9 1.476(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C2 C3 1.358(6) . ? C2 H2 0.9300 . ? C3 C2 1.358(6) 4_656 ? C3 H3 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C1 119.2(5) 4_656 . ? C6 N2 N3 109.8(3) . . ? C6 N2 H6 125.1 . . ? N3 N2 H6 125.1 . . ? C8 N3 N2 108.3(4) . . ? N1 C1 C2 121.3(5) . . ? N1 C1 C6 116.1(3) . . ? C2 C1 C6 122.7(5) . . ? N2 C6 C7 107.3(4) . . ? N2 C6 C1 121.0(3) . . ? C7 C6 C1 131.7(4) . . ? C8 C7 C6 106.5(4) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? N3 C8 C7 108.1(4) . . ? N3 C8 C9 121.7(6) . . ? C7 C8 C9 130.2(5) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C2 119.9(6) . 4_656 ? C2 C3 H3 120.1 . . ? C2 C3 H3 120.1 4_656 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.301 _refine_diff_density_min -0.146 _refine_diff_density_rms 0.051 #===END data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 655895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 Ag N8 O4' _chemical_formula_weight 585.38 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.038(4) _cell_length_b 11.111(4) _cell_length_c 12.541(4) _cell_angle_alpha 78.493(5) _cell_angle_beta 71.280(5) _cell_angle_gamma 86.839(6) _cell_volume 1298.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1699 _cell_measurement_theta_min 2.296 _cell_measurement_theta_max 20.577 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7456 _exptl_absorpt_correction_T_max 0.7968 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6827 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4510 _reflns_number_gt 2423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4510 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.69936(5) 0.70041(4) 0.66833(3) 0.0896(3) Uani 1 1 d . . . N1 N 0.7700(5) 0.7567(3) 0.4645(3) 0.0525(10) Uani 1 1 d . . . N2 N 0.9463(5) 0.6473(4) 0.5816(3) 0.0628(11) Uani 1 1 d . . . N3 N 1.0577(5) 0.5974(4) 0.6118(4) 0.0697(12) Uani 1 1 d . . . H3 H 1.0538 0.5692 0.6817 0.084 Uiso 1 1 calc R . . N4 N 0.5002(5) 0.8044(4) 0.5932(3) 0.0678(12) Uani 1 1 d . . . N5 N 0.3634(5) 0.8373(4) 0.6274(4) 0.0710(13) Uani 1 1 d . . . H5 H 0.3134 0.8307 0.6983 0.085 Uiso 1 1 calc R . . N6 N 0.5745(5) 0.5325(4) 0.7889(3) 0.0674(12) Uani 1 1 d . . . N7 N 0.7223(6) 0.8399(4) 0.7778(3) 0.0700(12) Uani 1 1 d . . . N8 N 0.1682(6) 0.7560(5) 0.9212(5) 0.0880(15) Uani 1 1 d . . . O1 O 0.1170(6) 0.7233(5) 1.0219(4) 0.144(2) Uani 1 1 d . . . O2 O 0.2501(7) 0.8429(5) 0.8811(4) 0.1347(19) Uani 1 1 d . . . O3 O 0.1475(6) 0.7053(5) 0.8524(5) 0.146(2) Uani 1 1 d . . . O4 O 0.9995(6) 0.4936(4) 0.1504(4) 0.1330(18) Uani 1 1 d . . . H24 H 1.0199 0.5602 0.1013 0.160 Uiso 1 1 d R . . H25 H 0.9767 0.4427 0.1167 0.160 Uiso 1 1 d R . . C1 C 0.6817(6) 0.8067(4) 0.4101(4) 0.0553(13) Uani 1 1 d . . . C2 C 0.7212(7) 0.8385(5) 0.2913(4) 0.0771(17) Uani 1 1 d . . . H2 H 0.6580 0.8751 0.2545 0.093 Uiso 1 1 calc R . . C3 C 0.8575(8) 0.8139(6) 0.2297(5) 0.0890(19) Uani 1 1 d . . . H3A H 0.8870 0.8326 0.1499 0.107 Uiso 1 1 calc R . . C4 C 0.9479(6) 0.7627(5) 0.2853(4) 0.0747(16) Uani 1 1 d . . . H4 H 1.0400 0.7459 0.2446 0.090 Uiso 1 1 calc R . . C5 C 0.9010(6) 0.7354(4) 0.4047(4) 0.0584(14) Uani 1 1 d . . . C6 C 0.9955(6) 0.6787(4) 0.4686(4) 0.0581(14) Uani 1 1 d . . . C7 C 1.1384(6) 0.6472(5) 0.4294(5) 0.0700(16) Uani 1 1 d . . . H7 H 1.1966 0.6596 0.3536 0.084 Uiso 1 1 calc R . . C8 C 1.1747(7) 0.5958(5) 0.5230(5) 0.0680(16) Uani 1 1 d . . . C9 C 1.3095(6) 0.5436(5) 0.5380(6) 0.0888(18) Uani 1 1 d . . . H9A H 1.2960 0.5136 0.6181 0.133 Uiso 1 1 calc R . . H9B H 1.3810 0.6065 0.5086 0.133 Uiso 1 1 calc R . . H9C H 1.3380 0.4773 0.4970 0.133 Uiso 1 1 calc R . . C10 C 0.5376(6) 0.8292(4) 0.4794(4) 0.0576(14) Uani 1 1 d . . . C11 C 0.4243(6) 0.8761(5) 0.4448(5) 0.0667(15) Uani 1 1 d . . . H11 H 0.4236 0.9000 0.3695 0.080 Uiso 1 1 calc R . . C12 C 0.3141(6) 0.8805(5) 0.5415(5) 0.0670(15) Uani 1 1 d . . . C13 C 0.1657(6) 0.9241(5) 0.5595(5) 0.0852(18) Uani 1 1 d . . . H13A H 0.1157 0.9120 0.6402 0.128 Uiso 1 1 calc R . . H13B H 0.1201 0.8782 0.5236 0.128 Uiso 1 1 calc R . . H13C H 0.1664 1.0098 0.5262 0.128 Uiso 1 1 calc R . . C14 C 0.6291(7) 0.4514(6) 0.8540(5) 0.0804(17) Uani 1 1 d . . . H14 H 0.7219 0.4625 0.8499 0.096 Uiso 1 1 calc R . . C15 C 0.5556(9) 0.3507(6) 0.9281(6) 0.102(2) Uani 1 1 d . . . H15 H 0.5971 0.2952 0.9738 0.122 Uiso 1 1 calc R . . C16 C 0.4214(10) 0.3352(7) 0.9323(7) 0.117(3) Uani 1 1 d . . . H16 H 0.3692 0.2672 0.9800 0.140 Uiso 1 1 calc R . . C17 C 0.3647(8) 0.4175(7) 0.8680(6) 0.110(2) Uani 1 1 d . . . H17 H 0.2717 0.4086 0.8715 0.132 Uiso 1 1 calc R . . C18 C 0.4424(8) 0.5141(6) 0.7975(5) 0.0847(18) Uani 1 1 d . . . H18 H 0.4010 0.5707 0.7526 0.102 Uiso 1 1 calc R . . C19 C 0.6225(8) 0.9197(6) 0.8093(5) 0.0887(18) Uani 1 1 d . . . H19 H 0.5399 0.9155 0.7916 0.106 Uiso 1 1 calc R . . C20 C 0.6354(10) 1.0089(6) 0.8671(6) 0.109(2) Uani 1 1 d . . . H20 H 0.5644 1.0658 0.8862 0.131 Uiso 1 1 calc R . . C21 C 0.7549(11) 1.0119(7) 0.8958(6) 0.112(3) Uani 1 1 d . . . H21 H 0.7658 1.0705 0.9360 0.134 Uiso 1 1 calc R . . C22 C 0.8567(8) 0.9303(8) 0.8659(6) 0.107(2) Uani 1 1 d . . . H22 H 0.9385 0.9302 0.8855 0.128 Uiso 1 1 calc R . . C23 C 0.8359(7) 0.8471(6) 0.8057(5) 0.0877(18) Uani 1 1 d . . . H23 H 0.9076 0.7919 0.7830 0.105 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 0.1165(5) 0.0944(4) 0.0491(3) -0.0064(2) -0.0126(3) -0.0361(3) N1 0.060(3) 0.051(2) 0.045(2) -0.0061(18) -0.013(2) -0.014(2) N2 0.071(3) 0.066(3) 0.052(2) -0.007(2) -0.021(2) -0.011(2) N3 0.084(4) 0.065(3) 0.063(3) -0.006(2) -0.029(3) -0.009(3) N4 0.070(3) 0.077(3) 0.047(2) -0.007(2) -0.008(2) -0.006(3) N5 0.074(4) 0.074(3) 0.054(3) -0.005(2) -0.007(3) -0.007(3) N6 0.078(4) 0.070(3) 0.051(2) 0.001(2) -0.020(2) -0.016(3) N7 0.077(4) 0.081(3) 0.053(2) -0.014(2) -0.020(3) -0.007(3) N8 0.102(4) 0.090(4) 0.061(3) -0.007(3) -0.015(3) -0.009(3) O1 0.172(5) 0.150(5) 0.069(3) 0.001(3) 0.008(3) -0.022(4) O2 0.172(5) 0.123(4) 0.097(3) -0.017(3) -0.020(3) -0.045(4) O3 0.160(5) 0.173(5) 0.114(4) -0.057(4) -0.032(4) -0.040(4) O4 0.189(5) 0.135(4) 0.085(3) 0.003(3) -0.064(3) -0.039(4) C1 0.065(4) 0.051(3) 0.046(3) -0.006(2) -0.011(3) -0.017(3) C2 0.084(5) 0.098(4) 0.047(3) -0.009(3) -0.020(3) 0.002(4) C3 0.097(5) 0.117(5) 0.040(3) 0.000(3) -0.012(4) -0.005(4) C4 0.065(4) 0.101(4) 0.053(3) -0.017(3) -0.010(3) -0.005(3) C5 0.071(4) 0.053(3) 0.049(3) -0.010(2) -0.013(3) -0.017(3) C6 0.071(4) 0.052(3) 0.052(3) -0.014(2) -0.016(3) -0.017(3) C7 0.074(5) 0.070(4) 0.065(3) -0.027(3) -0.010(3) -0.009(3) C8 0.082(5) 0.052(3) 0.077(4) -0.025(3) -0.025(4) -0.013(3) C9 0.081(5) 0.076(4) 0.116(5) -0.020(4) -0.039(4) -0.001(4) C10 0.070(4) 0.047(3) 0.053(3) -0.003(2) -0.015(3) -0.019(3) C11 0.070(4) 0.065(3) 0.060(3) -0.006(3) -0.015(3) -0.015(3) C12 0.071(4) 0.048(3) 0.081(4) -0.012(3) -0.022(4) -0.011(3) C13 0.079(5) 0.074(4) 0.103(4) -0.020(3) -0.027(4) -0.006(3) C14 0.077(4) 0.079(4) 0.087(4) -0.015(4) -0.030(4) 0.002(4) C15 0.141(7) 0.064(4) 0.102(5) 0.011(4) -0.059(5) 0.004(5) C16 0.135(8) 0.092(6) 0.102(5) 0.017(4) -0.023(5) -0.041(5) C17 0.088(5) 0.108(6) 0.119(6) 0.016(5) -0.029(5) -0.031(5) C18 0.089(5) 0.084(4) 0.084(4) 0.004(3) -0.043(4) -0.013(4) C19 0.107(6) 0.081(5) 0.083(4) -0.011(4) -0.041(4) 0.003(4) C20 0.141(8) 0.088(5) 0.100(5) -0.034(4) -0.036(5) 0.029(5) C21 0.155(8) 0.095(6) 0.099(5) -0.041(4) -0.043(6) -0.011(6) C22 0.102(6) 0.121(6) 0.108(5) -0.033(5) -0.036(5) -0.031(5) C23 0.073(5) 0.101(5) 0.088(4) -0.026(4) -0.015(4) -0.014(4) _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 N6 2.292(4) . ? Ag1 N7 2.330(5) . ? Ag1 N1 2.382(4) . ? Ag1 N2 2.457(5) . ? Ag1 N4 2.595(5) . ? N1 C1 1.319(6) . ? N1 C5 1.323(6) . ? N2 C6 1.322(6) . ? N2 N3 1.350(6) . ? N3 C8 1.336(6) . ? N3 H3 0.8600 . ? N4 C10 1.328(6) . ? N4 N5 1.354(6) . ? N5 C12 1.321(7) . ? N5 H5 0.8600 . ? N6 C14 1.311(7) . ? N6 C18 1.319(7) . ? N7 C23 1.307(7) . ? N7 C19 1.316(7) . ? N8 O1 1.188(6) . ? N8 O3 1.195(6) . ? N8 O2 1.221(6) . ? O4 H24 0.8500 . ? O4 H25 0.8503 . ? C1 C2 1.389(7) . ? C1 C10 1.467(7) . ? C2 C3 1.381(8) . ? C2 H2 0.9300 . ? C3 C4 1.352(8) . ? C3 H3A 0.9300 . ? C4 C5 1.392(7) . ? C4 H4 0.9300 . ? C5 C6 1.469(7) . ? C6 C7 1.408(7) . ? C7 C8 1.349(7) . ? C7 H7 0.9300 . ? C8 C9 1.496(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.384(7) . ? C11 C12 1.362(7) . ? C11 H11 0.9300 . ? C12 C13 1.501(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.377(8) . ? C14 H14 0.9300 . ? C15 C16 1.351(10) . ? C15 H15 0.9300 . ? C16 C17 1.324(10) . ? C16 H16 0.9300 . ? C17 C18 1.347(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.374(9) . ? C19 H19 0.9300 . ? C20 C21 1.362(10) . ? C20 H20 0.9300 . ? C21 C22 1.339(9) . ? C21 H21 0.9300 . ? C22 C23 1.367(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N7 108.76(15) . . ? N6 Ag1 N1 130.21(14) . . ? N7 Ag1 N1 120.34(13) . . ? N6 Ag1 N2 110.77(16) . . ? N7 Ag1 N2 101.28(17) . . ? N1 Ag1 N2 68.81(15) . . ? N6 Ag1 N4 98.12(17) . . ? N7 Ag1 N4 99.95(17) . . ? N1 Ag1 N4 67.07(15) . . ? N2 Ag1 N4 135.88(14) . . ? C1 N1 C5 119.5(4) . . ? C1 N1 Ag1 121.8(3) . . ? C5 N1 Ag1 118.7(3) . . ? C6 N2 N3 104.2(4) . . ? C6 N2 Ag1 115.2(4) . . ? N3 N2 Ag1 140.6(3) . . ? C8 N3 N2 113.9(5) . . ? C8 N3 H3 123.1 . . ? N2 N3 H3 123.1 . . ? C10 N4 N5 104.2(4) . . ? C10 N4 Ag1 112.6(4) . . ? N5 N4 Ag1 143.0(3) . . ? C12 N5 N4 113.6(4) . . ? C12 N5 H5 123.2 . . ? N4 N5 H5 123.2 . . ? C14 N6 C18 116.7(5) . . ? C14 N6 Ag1 122.1(4) . . ? C18 N6 Ag1 121.2(4) . . ? C23 N7 C19 117.0(6) . . ? C23 N7 Ag1 122.2(5) . . ? C19 N7 Ag1 120.7(5) . . ? O1 N8 O3 123.3(7) . . ? O1 N8 O2 121.5(7) . . ? O3 N8 O2 115.2(6) . . ? H24 O4 H25 105.8 . . ? N1 C1 C2 122.3(5) . . ? N1 C1 C10 117.8(4) . . ? C2 C1 C10 119.9(5) . . ? C3 C2 C1 117.7(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 118.8(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.6(5) . . ? N1 C5 C6 117.7(4) . . ? C4 C5 C6 120.6(5) . . ? N2 C6 C7 109.9(5) . . ? N2 C6 C5 119.5(5) . . ? C7 C6 C5 130.6(5) . . ? C8 C7 C6 106.9(5) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? N3 C8 C7 105.2(5) . . ? N3 C8 C9 122.2(6) . . ? C7 C8 C9 132.6(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 109.9(5) . . ? N4 C10 C1 120.5(5) . . ? C11 C10 C1 129.6(5) . . ? C12 C11 C10 107.1(5) . . ? C12 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? N5 C12 C11 105.2(5) . . ? N5 C12 C13 122.7(5) . . ? C11 C12 C13 132.1(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 C15 123.1(6) . . ? N6 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C16 C15 C14 117.8(7) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.7(7) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? N6 C18 C17 123.2(6) . . ? N6 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? N7 C19 C20 122.7(7) . . ? N7 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C21 C20 C19 118.2(7) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 119.9(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 117.6(8) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? N7 C23 C22 124.5(7) . . ? N7 C23 H23 117.7 . . ? C22 C23 H23 117.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C1 78.5(4) . . . . ? N7 Ag1 N1 C1 -90.7(4) . . . . ? N2 Ag1 N1 C1 178.3(4) . . . . ? N4 Ag1 N1 C1 -2.5(3) . . . . ? N6 Ag1 N1 C5 -100.5(4) . . . . ? N7 Ag1 N1 C5 90.2(4) . . . . ? N2 Ag1 N1 C5 -0.7(3) . . . . ? N4 Ag1 N1 C5 178.5(4) . . . . ? N6 Ag1 N2 C6 128.3(3) . . . . ? N7 Ag1 N2 C6 -116.5(3) . . . . ? N1 Ag1 N2 C6 1.9(3) . . . . ? N4 Ag1 N2 C6 0.8(4) . . . . ? N6 Ag1 N2 N3 -54.8(5) . . . . ? N7 Ag1 N2 N3 60.4(5) . . . . ? N1 Ag1 N2 N3 178.8(5) . . . . ? N4 Ag1 N2 N3 177.7(4) . . . . ? C6 N2 N3 C8 -0.1(5) . . . . ? Ag1 N2 N3 C8 -177.2(3) . . . . ? N6 Ag1 N4 C10 -126.8(3) . . . . ? N7 Ag1 N4 C10 122.4(3) . . . . ? N1 Ag1 N4 C10 3.6(3) . . . . ? N2 Ag1 N4 C10 4.6(4) . . . . ? N6 Ag1 N4 N5 46.8(5) . . . . ? N7 Ag1 N4 N5 -63.9(5) . . . . ? N1 Ag1 N4 N5 177.2(6) . . . . ? N2 Ag1 N4 N5 178.3(5) . . . . ? C10 N4 N5 C12 0.3(6) . . . . ? Ag1 N4 N5 C12 -173.7(4) . . . . ? N7 Ag1 N6 C14 -73.0(4) . . . . ? N1 Ag1 N6 C14 116.7(4) . . . . ? N2 Ag1 N6 C14 37.4(4) . . . . ? N4 Ag1 N6 C14 -176.5(4) . . . . ? N7 Ag1 N6 C18 105.8(4) . . . . ? N1 Ag1 N6 C18 -64.4(5) . . . . ? N2 Ag1 N6 C18 -143.7(4) . . . . ? N4 Ag1 N6 C18 2.3(4) . . . . ? N6 Ag1 N7 C23 98.4(5) . . . . ? N1 Ag1 N7 C23 -90.2(5) . . . . ? N2 Ag1 N7 C23 -18.3(5) . . . . ? N4 Ag1 N7 C23 -159.4(4) . . . . ? N6 Ag1 N7 C19 -85.1(4) . . . . ? N1 Ag1 N7 C19 86.3(4) . . . . ? N2 Ag1 N7 C19 158.2(4) . . . . ? N4 Ag1 N7 C19 17.1(4) . . . . ? C5 N1 C1 C2 -0.1(7) . . . . ? Ag1 N1 C1 C2 -179.2(4) . . . . ? C5 N1 C1 C10 -179.8(4) . . . . ? Ag1 N1 C1 C10 1.2(5) . . . . ? N1 C1 C2 C3 1.2(8) . . . . ? C10 C1 C2 C3 -179.1(5) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? C1 N1 C5 C4 -1.0(7) . . . . ? Ag1 N1 C5 C4 178.1(4) . . . . ? C1 N1 C5 C6 -179.5(4) . . . . ? Ag1 N1 C5 C6 -0.4(5) . . . . ? C3 C4 C5 N1 1.0(8) . . . . ? C3 C4 C5 C6 179.5(5) . . . . ? N3 N2 C6 C7 0.2(5) . . . . ? Ag1 N2 C6 C7 178.1(3) . . . . ? N3 N2 C6 C5 179.1(4) . . . . ? Ag1 N2 C6 C5 -2.9(5) . . . . ? N1 C5 C6 N2 2.3(6) . . . . ? C4 C5 C6 N2 -176.2(5) . . . . ? N1 C5 C6 C7 -179.0(5) . . . . ? C4 C5 C6 C7 2.5(8) . . . . ? N2 C6 C7 C8 -0.2(6) . . . . ? C5 C6 C7 C8 -179.0(5) . . . . ? N2 N3 C8 C7 0.0(6) . . . . ? N2 N3 C8 C9 -179.6(4) . . . . ? C6 C7 C8 N3 0.1(5) . . . . ? C6 C7 C8 C9 179.7(5) . . . . ? N5 N4 C10 C11 -0.4(5) . . . . ? Ag1 N4 C10 C11 175.6(3) . . . . ? N5 N4 C10 C1 179.4(4) . . . . ? Ag1 N4 C10 C1 -4.6(5) . . . . ? N1 C1 C10 N4 2.7(7) . . . . ? C2 C1 C10 N4 -177.0(5) . . . . ? N1 C1 C10 C11 -177.6(5) . . . . ? C2 C1 C10 C11 2.8(8) . . . . ? N4 C10 C11 C12 0.4(6) . . . . ? C1 C10 C11 C12 -179.3(5) . . . . ? N4 N5 C12 C11 0.0(6) . . . . ? N4 N5 C12 C13 -179.2(4) . . . . ? C10 C11 C12 N5 -0.3(6) . . . . ? C10 C11 C12 C13 178.8(5) . . . . ? C18 N6 C14 C15 0.3(8) . . . . ? Ag1 N6 C14 C15 179.2(4) . . . . ? N6 C14 C15 C16 0.7(10) . . . . ? C14 C15 C16 C17 -1.5(12) . . . . ? C15 C16 C17 C18 1.4(12) . . . . ? C14 N6 C18 C17 -0.4(9) . . . . ? Ag1 N6 C18 C17 -179.3(5) . . . . ? C16 C17 C18 N6 -0.4(11) . . . . ? C23 N7 C19 C20 1.1(8) . . . . ? Ag1 N7 C19 C20 -175.5(5) . . . . ? N7 C19 C20 C21 -2.0(10) . . . . ? C19 C20 C21 C22 1.0(11) . . . . ? C20 C21 C22 C23 0.8(11) . . . . ? C19 N7 C23 C22 0.8(9) . . . . ? Ag1 N7 C23 C22 177.4(5) . . . . ? C21 C22 C23 N7 -1.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.605 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.069 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 655896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 Ag N6 O3' _chemical_formula_sum 'C19 H25 Ag N6 O3' _chemical_formula_weight 493.32 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 23.981(4) _cell_length_b 9.1046(17) _cell_length_c 21.983(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.224(3) _cell_angle_gamma 90.00 _cell_volume 4268.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2214 _cell_measurement_theta_min 2.467 _cell_measurement_theta_max 19.562 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8438 _exptl_absorpt_correction_T_max 0.9260 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21593 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.1701 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7455 _reflns_number_gt 3108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.1914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7455 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.2201 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.40991(4) 0.41391(9) 0.35429(4) 0.0709(3) Uani 1 1 d . . . Ag2 Ag 0.08220(4) 0.90782(9) 0.42958(5) 0.0737(3) Uani 1 1 d . . . N1 N 0.5045(3) 0.5306(8) 0.4149(4) 0.0458(18) Uani 1 1 d . . . N2 N 0.4992(3) 0.2787(9) 0.3417(4) 0.056(2) Uani 1 1 d . . . N3 N 0.5132(4) 0.1700(9) 0.3089(4) 0.059(2) Uani 1 1 d . . . N4 N 0.3927(4) 0.6670(9) 0.3884(4) 0.062(2) Uani 1 1 d . . . N5 N 0.3467(3) 0.7499(9) 0.3930(4) 0.065(2) Uani 1 1 d . . . N6 N 0.3015(5) 0.2254(13) 0.2952(6) 0.081(3) Uani 1 1 d . . . N7 N -0.0105(3) 1.0252(8) 0.4063(4) 0.0463(18) Uani 1 1 d . . . N8 N 0.1026(4) 1.1648(9) 0.4829(5) 0.071(2) Uani 1 1 d . . . N9 N 0.1497(4) 1.2509(10) 0.5284(5) 0.073(2) Uani 1 1 d . . . N10 N -0.0103(3) 0.7681(9) 0.3366(4) 0.057(2) Uani 1 1 d . . . N11 N -0.0280(4) 0.6530(9) 0.2934(4) 0.062(2) Uani 1 1 d . . . N12 N 0.1944(4) 0.7322(11) 0.4778(5) 0.066(2) Uani 1 1 d . . . O1 O 0.3471(4) 0.2137(9) 0.3490(4) 0.092(2) Uani 1 1 d . . . O2 O 0.2982(5) 0.3249(13) 0.2568(5) 0.131(4) Uani 1 1 d . . . O3 O 0.2583(4) 0.1355(13) 0.2793(6) 0.149(4) Uani 1 1 d . . . O4 O 0.1829(4) 0.8251(10) 0.4329(5) 0.099(3) Uani 1 1 d . . . O5 O 0.1535(4) 0.7096(10) 0.4957(5) 0.109(3) Uani 1 1 d . . . O6 O 0.2436(4) 0.6620(11) 0.5032(5) 0.115(3) Uani 1 1 d . . . C1 C 0.5062(4) 0.6524(10) 0.4511(4) 0.045(2) Uani 1 1 d . . . C2 C 0.5631(4) 0.7129(11) 0.4978(5) 0.062(3) Uani 1 1 d . . . H2 H 0.5640 0.7954 0.5232 0.074 Uiso 1 1 calc R . . C3 C 0.6176(4) 0.6490(12) 0.5058(5) 0.061(3) Uani 1 1 d . . . H3 H 0.6561 0.6891 0.5360 0.074 Uiso 1 1 calc R . . C4 C 0.6154(4) 0.5270(11) 0.4696(5) 0.058(3) Uani 1 1 d . . . H4 H 0.6525 0.4807 0.4770 0.070 Uiso 1 1 calc R . . C5 C 0.5589(4) 0.4706(10) 0.4218(4) 0.047(2) Uani 1 1 d . . . C6 C 0.5540(4) 0.3425(10) 0.3794(5) 0.049(2) Uani 1 1 d . . . C7 C 0.6016(4) 0.2749(11) 0.3715(5) 0.062(3) Uani 1 1 d . . . H7 H 0.6439 0.2996 0.3933 0.074 Uiso 1 1 calc R . . C8 C 0.5749(6) 0.1662(12) 0.3259(6) 0.070(3) Uani 1 1 d . . . C9 C 0.6034(6) 0.0587(13) 0.2959(7) 0.102(4) Uani 1 1 d . . . H9A H 0.5713 -0.0046 0.2641 0.152 Uiso 1 1 calc R . . H9B H 0.6346 0.0008 0.3319 0.152 Uiso 1 1 calc R . . H9C H 0.6226 0.1115 0.2726 0.152 Uiso 1 1 calc R . . C10 C 0.4463(4) 0.7132(9) 0.4391(5) 0.049(2) Uani 1 1 d . . . C11 C 0.4342(4) 0.8281(10) 0.4746(5) 0.052(2) Uani 1 1 d . . . H11 H 0.4636 0.8811 0.5115 0.062 Uiso 1 1 calc R . . C12 C 0.3714(4) 0.8455(11) 0.4444(5) 0.059(3) Uani 1 1 d . . . C13 C 0.3318(5) 0.9501(11) 0.4598(6) 0.075(3) Uani 1 1 d . . . H13A H 0.2885 0.9342 0.4284 0.112 Uiso 1 1 calc R . . H13B H 0.3433 1.0490 0.4553 0.112 Uiso 1 1 calc R . . H13C H 0.3382 0.9344 0.5058 0.112 Uiso 1 1 calc R . . C14 C 0.4646(5) 0.0638(12) 0.2695(6) 0.073(3) Uani 1 1 d . . . H14 H 0.4821 -0.0008 0.2468 0.087 Uiso 1 1 calc R . . C15 C 0.4084(6) 0.1320(14) 0.2152(7) 0.099(4) Uani 1 1 d . . . H15A H 0.4200 0.1896 0.1862 0.148 Uiso 1 1 calc R . . H15B H 0.3890 0.1942 0.2354 0.148 Uiso 1 1 calc R . . H15C H 0.3794 0.0569 0.1886 0.148 Uiso 1 1 calc R . . C16 C 0.4479(7) -0.0329(13) 0.3147(7) 0.115(5) Uani 1 1 d . . . H16A H 0.4852 -0.0788 0.3487 0.172 Uiso 1 1 calc R . . H16B H 0.4188 -0.1071 0.2873 0.172 Uiso 1 1 calc R . . H16C H 0.4291 0.0258 0.3367 0.172 Uiso 1 1 calc R . . C17 C 0.2809(5) 0.7282(14) 0.3408(7) 0.093(4) Uani 1 1 d . . . H17 H 0.2554 0.8031 0.3484 0.111 Uiso 1 1 calc R . . C18 C 0.2745(6) 0.7512(19) 0.2696(6) 0.135(6) Uani 1 1 d . . . H18A H 0.2888 0.8481 0.2663 0.203 Uiso 1 1 calc R . . H18B H 0.2314 0.7406 0.2364 0.203 Uiso 1 1 calc R . . H18C H 0.2994 0.6797 0.2609 0.203 Uiso 1 1 calc R . . C19 C 0.2583(6) 0.5819(15) 0.3502(7) 0.108(4) Uani 1 1 d . . . H19A H 0.2625 0.5748 0.3957 0.162 Uiso 1 1 calc R . . H19B H 0.2827 0.5062 0.3433 0.162 Uiso 1 1 calc R . . H19C H 0.2150 0.5704 0.3176 0.162 Uiso 1 1 calc R . . C20 C -0.0652(4) 0.9645(11) 0.3649(5) 0.053(2) Uani 1 1 d . . . C21 C -0.1217(4) 1.0206(12) 0.3577(5) 0.063(3) Uani 1 1 d . . . H21 H -0.1596 0.9765 0.3286 0.076 Uiso 1 1 calc R . . C22 C -0.1198(5) 1.1422(13) 0.3945(6) 0.071(3) Uani 1 1 d . . . H22 H -0.1571 1.1834 0.3897 0.086 Uiso 1 1 calc R . . C23 C -0.0638(4) 1.2053(11) 0.4386(5) 0.060(3) Uani 1 1 d . . . H23 H -0.0625 1.2859 0.4652 0.071 Uiso 1 1 calc R . . C24 C -0.0085(4) 1.1450(10) 0.4425(5) 0.050(2) Uani 1 1 d . . . C25 C 0.0523(4) 1.2126(11) 0.4867(5) 0.056(2) Uani 1 1 d . . . C26 C 0.0660(5) 1.3250(11) 0.5343(5) 0.059(3) Uani 1 1 d . . . H26 H 0.0383 1.3740 0.5461 0.071 Uiso 1 1 calc R . . C27 C 0.1297(5) 1.3479(12) 0.5600(6) 0.068(3) Uani 1 1 d . . . C28 C 0.1710(6) 1.4537(12) 0.6130(6) 0.092(4) Uani 1 1 d . . . H28A H 0.2134 1.4421 0.6202 0.138 Uiso 1 1 calc R . . H28B H 0.1692 1.4352 0.6550 0.138 Uiso 1 1 calc R . . H28C H 0.1571 1.5521 0.5980 0.138 Uiso 1 1 calc R . . C29 C -0.0641(4) 0.8342(11) 0.3266(5) 0.053(2) Uani 1 1 d . . . C30 C -0.1147(5) 0.7558(13) 0.2775(5) 0.073(3) Uani 1 1 d . . . H30 H -0.1570 0.7778 0.2613 0.088 Uiso 1 1 calc R . . C31 C -0.0909(5) 0.6437(13) 0.2582(6) 0.073(3) Uani 1 1 d . . . C32 C -0.1236(6) 0.5226(15) 0.2066(7) 0.119(5) Uani 1 1 d . . . H32A H -0.0929 0.4570 0.2053 0.178 Uiso 1 1 calc R . . H32B H -0.1478 0.5650 0.1622 0.178 Uiso 1 1 calc R . . H32C H -0.1509 0.4693 0.2198 0.178 Uiso 1 1 calc R . . C33 C 0.2140(5) 1.2412(19) 0.5349(10) 0.127(6) Uani 1 1 d . . . H33 H 0.2382 1.3247 0.5625 0.152 Uiso 1 1 calc R . . C34 C 0.2120(6) 1.253(2) 0.4658(10) 0.157(7) Uani 1 1 d . . . H34A H 0.1942 1.3453 0.4454 0.236 Uiso 1 1 calc R . . H34B H 0.1869 1.1744 0.4371 0.236 Uiso 1 1 calc R . . H34C H 0.2538 1.2453 0.4707 0.236 Uiso 1 1 calc R . . C35 C 0.2440(6) 1.1028(19) 0.5731(8) 0.138(6) Uani 1 1 d . . . H35A H 0.2438 1.1034 0.6167 0.208 Uiso 1 1 calc R . . H35B H 0.2864 1.0973 0.5799 0.208 Uiso 1 1 calc R . . H35C H 0.2209 1.0193 0.5471 0.208 Uiso 1 1 calc R . . C36 C 0.0199(5) 0.5494(11) 0.2961(6) 0.069(3) Uani 1 1 d . . . H36 H -0.0006 0.4856 0.2559 0.083 Uiso 1 1 calc R . . C37 C 0.0722(5) 0.6248(13) 0.2897(7) 0.097(4) Uani 1 1 d . . . H37A H 0.0555 0.6820 0.2484 0.146 Uiso 1 1 calc R . . H37B H 0.1008 0.5528 0.2882 0.146 Uiso 1 1 calc R . . H37C H 0.0940 0.6882 0.3283 0.146 Uiso 1 1 calc R . . C38 C 0.0399(7) 0.4520(15) 0.3578(7) 0.125(6) Uani 1 1 d . . . H38A H 0.0036 0.4071 0.3576 0.187 Uiso 1 1 calc R . . H38B H 0.0613 0.5096 0.3986 0.187 Uiso 1 1 calc R . . H38C H 0.0675 0.3770 0.3566 0.187 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 0.0585(5) 0.0746(6) 0.0691(6) -0.0134(4) 0.0200(4) -0.0175(4) Ag2 0.0560(5) 0.0780(7) 0.0875(7) 0.0028(5) 0.0332(5) 0.0180(4) N1 0.044(4) 0.045(4) 0.048(5) -0.010(4) 0.021(4) -0.005(3) N2 0.058(5) 0.057(5) 0.049(5) -0.012(4) 0.022(4) -0.004(4) N3 0.073(6) 0.053(5) 0.060(5) -0.004(4) 0.037(5) 0.000(4) N4 0.050(5) 0.060(5) 0.070(6) -0.007(4) 0.022(5) 0.007(4) N5 0.045(5) 0.070(6) 0.077(6) -0.018(5) 0.023(4) -0.002(4) N6 0.056(6) 0.088(8) 0.077(8) -0.024(6) 0.013(6) 0.010(6) N7 0.049(5) 0.043(5) 0.043(4) 0.008(4) 0.018(4) 0.005(4) N8 0.055(5) 0.064(6) 0.085(7) -0.008(5) 0.024(5) 0.005(5) N9 0.052(5) 0.060(6) 0.097(7) -0.009(5) 0.026(5) -0.006(5) N10 0.058(5) 0.053(5) 0.057(5) 0.001(4) 0.024(4) 0.003(4) N11 0.064(6) 0.048(5) 0.064(5) -0.006(4) 0.022(5) -0.001(4) N12 0.059(6) 0.080(7) 0.054(6) -0.001(5) 0.022(5) 0.004(5) O1 0.068(5) 0.116(7) 0.073(5) -0.007(5) 0.014(5) -0.021(5) O2 0.152(10) 0.119(9) 0.096(7) 0.022(7) 0.035(7) 0.050(7) O3 0.054(6) 0.146(9) 0.189(11) -0.040(8) 0.006(6) -0.043(6) O4 0.080(6) 0.102(7) 0.112(7) 0.026(6) 0.042(5) 0.001(5) O5 0.088(6) 0.154(9) 0.109(7) 0.039(6) 0.067(6) 0.029(6) O6 0.053(5) 0.133(8) 0.140(8) 0.013(6) 0.029(5) 0.034(5) C1 0.044(5) 0.049(6) 0.039(5) -0.001(4) 0.016(4) -0.008(4) C2 0.057(6) 0.067(7) 0.064(7) -0.018(5) 0.032(5) -0.011(5) C3 0.048(6) 0.076(7) 0.058(7) -0.011(6) 0.022(5) -0.009(5) C4 0.053(6) 0.057(7) 0.071(7) -0.002(5) 0.035(6) -0.002(5) C5 0.036(5) 0.051(6) 0.048(6) -0.011(5) 0.013(4) -0.006(4) C6 0.056(6) 0.050(6) 0.049(6) 0.010(5) 0.030(5) 0.006(5) C7 0.057(6) 0.068(7) 0.052(6) -0.007(5) 0.017(5) -0.003(5) C8 0.096(9) 0.057(7) 0.062(7) 0.009(6) 0.041(7) 0.022(6) C9 0.132(11) 0.081(9) 0.101(10) -0.019(7) 0.062(9) 0.021(8) C10 0.051(6) 0.041(6) 0.057(6) -0.001(5) 0.026(5) -0.002(4) C11 0.052(6) 0.050(6) 0.051(6) 0.002(5) 0.022(5) 0.002(5) C12 0.053(6) 0.060(6) 0.072(7) -0.007(6) 0.036(6) 0.001(5) C13 0.070(7) 0.063(7) 0.105(9) -0.008(6) 0.053(7) 0.013(5) C14 0.073(8) 0.077(8) 0.065(7) -0.015(6) 0.029(6) 0.003(6) C15 0.102(10) 0.088(9) 0.111(11) -0.042(8) 0.052(9) -0.011(8) C16 0.157(14) 0.061(8) 0.129(12) -0.001(8) 0.068(11) -0.044(8) C17 0.045(6) 0.083(9) 0.111(11) -0.040(8) 0.003(7) 0.003(6) C18 0.091(10) 0.187(17) 0.070(10) 0.026(10) -0.012(8) -0.001(10) C19 0.074(9) 0.129(13) 0.111(11) -0.014(9) 0.035(8) -0.017(8) C20 0.047(6) 0.067(7) 0.044(6) 0.003(5) 0.020(5) 0.004(5) C21 0.039(6) 0.082(8) 0.068(7) 0.009(6) 0.024(5) 0.017(5) C22 0.056(7) 0.097(9) 0.069(7) 0.008(7) 0.036(6) 0.024(6) C23 0.051(6) 0.071(7) 0.055(6) 0.003(5) 0.023(5) 0.007(5) C24 0.055(6) 0.046(6) 0.051(6) 0.006(5) 0.025(5) 0.011(5) C25 0.050(6) 0.054(6) 0.056(6) 0.009(5) 0.018(5) 0.003(5) C26 0.064(7) 0.052(7) 0.068(7) 0.002(5) 0.035(6) 0.005(5) C27 0.072(8) 0.051(7) 0.070(7) 0.006(6) 0.022(6) -0.007(6) C28 0.095(9) 0.063(8) 0.095(9) -0.004(7) 0.024(8) -0.011(7) C29 0.049(6) 0.062(7) 0.048(6) 0.006(5) 0.023(5) 0.007(5) C30 0.055(7) 0.098(9) 0.066(7) -0.012(7) 0.028(6) 0.008(6) C31 0.070(8) 0.064(7) 0.074(8) -0.006(6) 0.023(7) 0.006(6) C32 0.085(9) 0.118(12) 0.111(11) -0.052(9) 0.008(8) 0.000(8) C33 0.050(8) 0.119(13) 0.177(17) -0.042(12) 0.022(10) -0.007(8) C34 0.094(12) 0.22(2) 0.193(19) 0.027(16) 0.092(13) 0.008(12) C35 0.070(9) 0.196(19) 0.128(13) 0.007(12) 0.027(9) 0.035(10) C36 0.072(7) 0.053(7) 0.078(8) -0.013(6) 0.030(6) 0.009(5) C37 0.094(9) 0.099(10) 0.121(11) -0.045(8) 0.069(9) -0.027(7) C38 0.159(14) 0.112(12) 0.109(11) 0.059(9) 0.067(11) 0.078(10) _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 2.299(7) . ? Ag1 O1 2.333(8) . ? Ag1 N4 2.515(8) . ? Ag1 N2 2.592(7) . ? Ag1 O2 2.678(11) . ? Ag2 N7 2.304(7) . ? Ag2 O5 2.454(8) . ? Ag2 O4 2.499(8) . ? Ag2 N10 2.563(8) . ? Ag2 N8 2.561(9) . ? N1 C5 1.356(10) . ? N1 C1 1.356(11) . ? N2 C6 1.326(10) . ? N2 N3 1.354(10) . ? N3 C8 1.349(12) . ? N3 C14 1.456(12) . ? N4 C10 1.328(11) . ? N4 N5 1.377(9) . ? N5 C12 1.331(11) . ? N5 C17 1.479(12) . ? N6 O1 1.193(11) . ? N6 O2 1.216(13) . ? N6 O3 1.239(12) . ? N7 C20 1.327(11) . ? N7 C24 1.338(11) . ? N8 C25 1.319(11) . ? N8 N9 1.363(11) . ? N9 C27 1.340(12) . ? N9 C33 1.485(14) . ? N10 C29 1.347(10) . ? N10 N11 1.346(10) . ? N11 C31 1.348(12) . ? N11 C36 1.467(12) . ? N12 O4 1.232(10) . ? N12 O5 1.228(10) . ? N12 O6 1.230(10) . ? C1 C2 1.392(11) . ? C1 C10 1.446(11) . ? C2 C3 1.367(12) . ? C2 H2 0.9300 . ? C3 C4 1.354(13) . ? C3 H3 0.9300 . ? C4 C5 1.380(12) . ? C4 H4 0.9300 . ? C5 C6 1.463(12) . ? C6 C7 1.375(12) . ? C7 C8 1.344(14) . ? C7 H7 0.9300 . ? C8 C9 1.508(14) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.413(12) . ? C11 C12 1.347(12) . ? C11 H11 0.9300 . ? C12 C13 1.491(12) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.468(15) . ? C14 C16 1.513(15) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.488(16) . ? C17 C18 1.518(17) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.387(12) . ? C20 C29 1.463(13) . ? C21 C22 1.360(14) . ? C21 H21 0.9300 . ? C22 C23 1.372(13) . ? C22 H22 0.9300 . ? C23 C24 1.400(12) . ? C23 H23 0.9300 . ? C24 C25 1.467(12) . ? C25 C26 1.391(13) . ? C26 C27 1.381(13) . ? C26 H26 0.9300 . ? C27 C28 1.487(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.396(13) . ? C30 C31 1.329(14) . ? C30 H30 0.9300 . ? C31 C32 1.517(15) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C35 1.50(2) . ? C33 C34 1.502(19) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.504(15) . ? C36 C37 1.492(14) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? 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 O1 146.4(3) . . ? N1 Ag1 N4 70.0(2) . . ? O1 Ag1 N4 122.7(3) . . ? N1 Ag1 N2 68.7(2) . . ? O1 Ag1 N2 99.7(3) . . ? N4 Ag1 N2 136.4(2) . . ? N1 Ag1 O2 164.6(3) . . ? O1 Ag1 O2 48.5(3) . . ? N4 Ag1 O2 106.0(3) . . ? N2 Ag1 O2 110.1(3) . . ? N7 Ag2 O5 144.4(3) . . ? N7 Ag2 O4 165.5(3) . . ? O5 Ag2 O4 50.1(3) . . ? N7 Ag2 N10 70.0(3) . . ? O5 Ag2 N10 102.8(3) . . ? O4 Ag2 N10 110.2(3) . . ? N7 Ag2 N8 68.9(3) . . ? O5 Ag2 N8 117.7(3) . . ? O4 Ag2 N8 106.4(3) . . ? N10 Ag2 N8 137.1(3) . . ? C5 N1 C1 119.7(7) . . ? C5 N1 Ag1 121.4(5) . . ? C1 N1 Ag1 118.3(5) . . ? C6 N2 N3 103.7(7) . . ? C6 N2 Ag1 110.9(6) . . ? N3 N2 Ag1 145.4(6) . . ? C8 N3 N2 112.3(8) . . ? C8 N3 C14 128.7(9) . . ? N2 N3 C14 118.4(8) . . ? C10 N4 N5 105.4(7) . . ? C10 N4 Ag1 108.2(6) . . ? N5 N4 Ag1 140.4(6) . . ? C12 N5 N4 111.1(7) . . ? C12 N5 C17 130.4(8) . . ? N4 N5 C17 118.4(8) . . ? O1 N6 O2 119.6(12) . . ? O1 N6 O3 119.4(13) . . ? O2 N6 O3 121.0(12) . . ? C20 N7 C24 120.2(8) . . ? C20 N7 Ag2 120.6(6) . . ? C24 N7 Ag2 118.5(6) . . ? C25 N8 N9 103.8(8) . . ? C25 N8 Ag2 110.0(7) . . ? N9 N8 Ag2 141.4(6) . . ? C27 N9 N8 112.8(8) . . ? C27 N9 C33 126.2(10) . . ? N8 N9 C33 120.8(10) . . ? C29 N10 N11 105.3(8) . . ? C29 N10 Ag2 108.9(6) . . ? N11 N10 Ag2 145.9(6) . . ? N10 N11 C31 111.3(8) . . ? N10 N11 C36 119.0(8) . . ? C31 N11 C36 129.3(9) . . ? O4 N12 O5 117.0(9) . . ? O4 N12 O6 122.3(10) . . ? O5 N12 O6 120.6(10) . . ? N6 O1 Ag1 104.9(8) . . ? N6 O2 Ag1 86.9(7) . . ? N12 O4 Ag2 95.0(6) . . ? N12 O5 Ag2 97.4(7) . . ? N1 C1 C2 120.8(8) . . ? N1 C1 C10 116.5(7) . . ? C2 C1 C10 122.7(9) . . ? C3 C2 C1 118.9(9) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 119.8(9) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.9(9) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 119.7(8) . . ? N1 C5 C6 117.2(7) . . ? C4 C5 C6 123.1(8) . . ? N2 C6 C7 111.5(9) . . ? N2 C6 C5 121.0(8) . . ? C7 C6 C5 127.5(9) . . ? C8 C7 C6 106.5(9) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N3 C8 C7 106.0(9) . . ? N3 C8 C9 123.7(11) . . ? C7 C8 C9 130.3(12) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 109.5(8) . . ? N4 C10 C1 122.1(8) . . ? C11 C10 C1 128.4(9) . . ? C12 C11 C10 106.3(8) . . ? C12 C11 H11 126.9 . . ? C10 C11 H11 126.9 . . ? N5 C12 C11 107.8(8) . . ? N5 C12 C13 121.9(9) . . ? C11 C12 C13 130.3(10) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 113.0(10) . . ? N3 C14 C16 112.0(9) . . ? C15 C14 C16 111.0(11) . . ? N3 C14 H14 106.8 . . ? C15 C14 H14 106.8 . . ? C16 C14 H14 106.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 N5 109.9(11) . . ? C19 C17 C18 113.3(11) . . ? N5 C17 C18 110.4(10) . . ? C19 C17 H17 107.7 . . ? N5 C17 H17 107.7 . . ? C18 C17 H17 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N7 C20 C21 122.1(9) . . ? N7 C20 C29 117.4(8) . . ? C21 C20 C29 120.5(9) . . ? C22 C21 C20 117.8(10) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C21 C22 C23 121.1(9) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 118.2(10) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N7 C24 C23 120.5(9) . . ? N7 C24 C25 119.3(8) . . ? C23 C24 C25 120.2(9) . . ? N8 C25 C26 112.5(9) . . ? N8 C25 C24 118.7(9) . . ? C26 C25 C24 128.8(9) . . ? C27 C26 C25 104.8(9) . . ? C27 C26 H26 127.6 . . ? C25 C26 H26 127.6 . . ? N9 C27 C26 106.2(9) . . ? N9 C27 C28 124.4(10) . . ? C26 C27 C28 129.3(11) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N10 C29 C30 109.0(9) . . ? N10 C29 C20 122.5(9) . . ? C30 C29 C20 128.5(9) . . ? C31 C30 C29 107.0(9) . . ? C31 C30 H30 126.5 . . ? C29 C30 H30 126.5 . . ? C30 C31 N11 107.4(10) . . ? C30 C31 C32 130.2(11) . . ? N11 C31 C32 122.4(10) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N9 C33 C35 108.3(14) . . ? N9 C33 C34 110.4(12) . . ? C35 C33 C34 114.1(14) . . ? N9 C33 H33 107.9 . . ? C35 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N11 C36 C38 109.7(9) . . ? N11 C36 C37 112.1(9) . . ? C38 C36 C37 114.9(11) . . ? N11 C36 H36 106.5 . . ? C38 C36 H36 106.5 . . ? C37 C36 H36 106.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.526 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.096 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 655897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H54 Ag2 N16 O4' _chemical_formula_weight 1471.09 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.8634(19) _cell_length_b 21.723(3) _cell_length_c 12.7742(19) _cell_angle_alpha 90.00 _cell_angle_beta 115.749(2) _cell_angle_gamma 90.00 _cell_volume 3215.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5045 _cell_measurement_theta_min 2.571 _cell_measurement_theta_max 25.532 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7880 _exptl_absorpt_correction_T_max 0.9172 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16888 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5660 _reflns_number_gt 3958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+1.8127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5660 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.004 _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 0.47243(2) 1.029056(13) 0.88261(2) 0.05496(11) Uani 1 1 d . . . N1 N 0.2688(2) 1.02615(12) 0.8001(2) 0.0422(6) Uani 1 1 d . . . N2 N 0.4114(2) 1.08234(12) 1.0024(2) 0.0452(7) Uani 1 1 d . . . N3 N 0.4591(2) 1.11717(12) 1.1000(2) 0.0450(7) Uani 1 1 d . . . H3 H 0.5317 1.1178 1.1460 0.054 Uiso 1 1 calc R . . N4 N 0.4950(2) 0.91099(12) 0.5135(2) 0.0469(7) Uani 1 1 d . . . N5 N 0.5536(2) 0.97869(13) 0.7097(2) 0.0482(7) Uani 1 1 d . . . H5 H 0.4844 0.9645 0.6769 0.058 Uiso 1 1 calc R . . N6 N 0.5951(2) 1.01218(13) 0.8084(2) 0.0473(7) Uani 1 1 d . . . N7 N 0.2653(2) 0.86624(14) 0.4005(2) 0.0551(8) Uani 1 1 d . . . H7 H 0.2764 0.8909 0.4571 0.066 Uiso 1 1 calc R . . N8 N 0.1644(2) 0.83729(15) 0.3379(3) 0.0591(8) Uani 1 1 d . . . O1 O 0.35818(19) 0.93359(12) 0.7179(2) 0.0568(6) Uani 1 1 d . . . O2 O 0.2073(2) 0.94323(14) 0.5458(2) 0.0698(8) Uani 1 1 d . . . C1 C 0.2599(3) 0.95299(16) 0.6512(3) 0.0487(8) Uani 1 1 d . . . C2 C 0.2008(3) 0.99468(16) 0.7048(3) 0.0449(8) Uani 1 1 d . . . C3 C 0.0821(3) 1.00012(18) 0.6552(3) 0.0551(9) Uani 1 1 d . . . H3A H 0.0366 0.9769 0.5902 0.066 Uiso 1 1 calc R . . C4 C 0.0317(3) 1.04022(18) 0.7028(3) 0.0615(10) Uani 1 1 d . . . H4 H -0.0479 1.0455 0.6691 0.074 Uiso 1 1 calc R . . C5 C 0.1012(3) 1.07229(18) 0.8011(3) 0.0586(10) Uani 1 1 d . . . H5A H 0.0691 1.0993 0.8355 0.070 Uiso 1 1 calc R . . C6 C 0.2194(3) 1.06395(15) 0.8485(3) 0.0442(8) Uani 1 1 d . . . C7 C 0.2987(3) 1.09494(15) 0.9559(3) 0.0434(8) Uani 1 1 d . . . C8 C 0.2753(3) 1.13772(15) 1.0245(3) 0.0497(8) Uani 1 1 d . . . H8 H 0.2036 1.1541 1.0105 0.060 Uiso 1 1 calc R . . C9 C 0.3789(3) 1.15081(15) 1.1164(3) 0.0460(8) Uani 1 1 d . . . C10 C 0.4082(3) 1.19249(16) 1.2160(3) 0.0513(9) Uani 1 1 d . . . C11 C 0.5196(4) 1.19902(17) 1.3014(3) 0.0608(10) Uani 1 1 d . . . H11 H 0.5790 1.1763 1.2973 0.073 Uiso 1 1 calc R . . C12 C 0.5434(4) 1.23910(18) 1.3930(3) 0.0696(11) Uani 1 1 d . . . H12 H 0.6187 1.2433 1.4502 0.083 Uiso 1 1 calc R . . C13 C 0.4568(5) 1.2723(2) 1.3993(4) 0.0852(15) Uani 1 1 d . . . H13 H 0.4729 1.2988 1.4617 0.102 Uiso 1 1 calc R . . C14 C 0.3460(5) 1.2672(2) 1.3144(5) 0.0968(16) Uani 1 1 d . . . H14 H 0.2876 1.2909 1.3184 0.116 Uiso 1 1 calc R . . C15 C 0.3207(4) 1.2271(2) 1.2231(4) 0.0791(13) Uani 1 1 d . . . H15 H 0.2452 1.2233 1.1662 0.095 Uiso 1 1 calc R . . C16 C 0.4634(3) 0.87779(16) 0.4166(3) 0.0487(8) Uani 1 1 d . . . C17 C 0.5372(3) 0.86765(18) 0.3648(3) 0.0585(10) Uani 1 1 d . . . H17 H 0.5137 0.8436 0.2982 0.070 Uiso 1 1 calc R . . C18 C 0.6445(3) 0.8934(2) 0.4130(3) 0.0651(11) Uani 1 1 d . . . H18 H 0.6938 0.8881 0.3778 0.078 Uiso 1 1 calc R . . C19 C 0.6799(3) 0.92722(18) 0.5139(3) 0.0586(10) Uani 1 1 d . . . H19 H 0.7535 0.9442 0.5492 0.070 Uiso 1 1 calc R . . C20 C 0.6016(3) 0.93503(17) 0.5610(3) 0.0490(8) Uani 1 1 d . . . C21 C 0.6319(3) 0.96999(16) 0.6682(3) 0.0476(8) Uani 1 1 d . . . C22 C 0.7294(3) 0.99986(18) 0.7438(3) 0.0543(9) Uani 1 1 d . . . H22 H 0.7993 1.0023 0.7389 0.065 Uiso 1 1 calc R . . C23 C 0.7040(3) 1.02583(16) 0.8294(3) 0.0484(8) Uani 1 1 d . . . C24 C 0.7790(3) 1.06238(18) 0.9313(3) 0.0571(9) Uani 1 1 d . . . C25 C 0.8960(4) 1.0631(3) 0.9649(4) 0.0941(15) Uani 1 1 d . . . H25 H 0.9262 1.0406 0.9226 0.113 Uiso 1 1 calc R . . C26 C 0.9693(5) 1.0964(3) 1.0602(5) 0.123(2) Uani 1 1 d . . . H26 H 1.0481 1.0968 1.0809 0.148 Uiso 1 1 calc R . . C27 C 0.9266(6) 1.1288(3) 1.1243(5) 0.116(2) Uani 1 1 d . . . H27 H 0.9763 1.1507 1.1893 0.139 Uiso 1 1 calc R . . C28 C 0.8115(6) 1.1288(3) 1.0927(5) 0.122(2) Uani 1 1 d . . . H28 H 0.7818 1.1505 1.1363 0.146 Uiso 1 1 calc R . . C29 C 0.7386(4) 1.0963(2) 0.9955(4) 0.0973(16) Uani 1 1 d . . . H29 H 0.6595 1.0977 0.9731 0.117 Uiso 1 1 calc R . . C30 C 0.3471(3) 0.85210(17) 0.3644(3) 0.0499(9) Uani 1 1 d . . . C31 C 0.2961(3) 0.81136(17) 0.2746(3) 0.0554(9) Uani 1 1 d . . . H31 H 0.3300 0.7928 0.2314 0.066 Uiso 1 1 calc R . . C32 C 0.1834(3) 0.80318(16) 0.2606(3) 0.0527(9) Uani 1 1 d . . . C33 C 0.0925(3) 0.76342(18) 0.1771(3) 0.0580(9) Uani 1 1 d . . . C34 C 0.1152(4) 0.7284(2) 0.0979(4) 0.0839(14) Uani 1 1 d . . . H34 H 0.1870 0.7315 0.0971 0.101 Uiso 1 1 calc R . . C35 C 0.0332(4) 0.6895(2) 0.0208(4) 0.0962(16) Uani 1 1 d . . . H35 H 0.0500 0.6662 -0.0311 0.115 Uiso 1 1 calc R . . C36 C -0.0724(4) 0.6851(2) 0.0207(4) 0.0895(15) Uani 1 1 d . . . H36 H -0.1280 0.6588 -0.0312 0.107 Uiso 1 1 calc R . . C37 C -0.0967(4) 0.7194(2) 0.0967(4) 0.0832(13) Uani 1 1 d . . . H37 H -0.1693 0.7165 0.0957 0.100 Uiso 1 1 calc R . . C38 C -0.0154(3) 0.75832(19) 0.1752(4) 0.0673(11) Uani 1 1 d . . . H38 H -0.0332 0.7811 0.2268 0.081 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 0.04725(17) 0.0613(2) 0.05986(18) -0.00540(14) 0.02656(13) 0.00666(13) N1 0.0399(15) 0.0458(16) 0.0412(14) 0.0001(13) 0.0180(12) 0.0037(13) N2 0.0469(17) 0.0430(17) 0.0461(15) -0.0050(13) 0.0206(13) 0.0024(13) N3 0.0461(16) 0.0421(17) 0.0461(16) -0.0062(13) 0.0195(13) -0.0005(13) N4 0.0434(16) 0.0494(17) 0.0503(16) 0.0008(14) 0.0227(13) 0.0027(13) N5 0.0378(15) 0.0555(19) 0.0466(16) -0.0032(14) 0.0140(13) 0.0002(13) N6 0.0449(17) 0.0493(18) 0.0465(16) 0.0031(13) 0.0188(13) 0.0030(13) N7 0.0526(18) 0.060(2) 0.0539(17) -0.0112(15) 0.0241(15) 0.0003(15) N8 0.0506(19) 0.068(2) 0.0599(19) -0.0070(16) 0.0249(15) -0.0013(15) O1 0.0389(13) 0.0684(17) 0.0573(14) -0.0073(13) 0.0156(11) 0.0079(12) O2 0.0494(15) 0.097(2) 0.0538(16) -0.0266(14) 0.0137(12) 0.0033(14) C1 0.0383(19) 0.055(2) 0.052(2) -0.0072(17) 0.0189(17) -0.0048(16) C2 0.0385(18) 0.052(2) 0.0425(18) 0.0013(16) 0.0161(15) 0.0016(15) C3 0.040(2) 0.073(3) 0.0464(19) -0.0030(18) 0.0132(16) 0.0007(18) C4 0.0367(19) 0.081(3) 0.063(2) -0.001(2) 0.0183(18) 0.0080(18) C5 0.050(2) 0.065(3) 0.062(2) -0.003(2) 0.0252(19) 0.0119(18) C6 0.049(2) 0.040(2) 0.0456(19) 0.0059(15) 0.0226(16) 0.0083(15) C7 0.047(2) 0.0403(19) 0.0459(18) 0.0067(15) 0.0231(16) 0.0065(15) C8 0.051(2) 0.046(2) 0.058(2) 0.0035(17) 0.0296(18) 0.0094(16) C9 0.060(2) 0.0351(19) 0.050(2) 0.0034(15) 0.0306(18) 0.0059(16) C10 0.069(3) 0.041(2) 0.055(2) -0.0003(17) 0.037(2) 0.0024(17) C11 0.081(3) 0.046(2) 0.061(2) -0.0054(19) 0.036(2) 0.0027(19) C12 0.102(3) 0.049(3) 0.059(2) -0.0071(19) 0.035(2) -0.007(2) C13 0.135(5) 0.067(3) 0.077(3) -0.028(2) 0.068(3) -0.013(3) C14 0.112(4) 0.094(4) 0.113(4) -0.036(3) 0.076(4) 0.001(3) C15 0.082(3) 0.079(3) 0.088(3) -0.023(3) 0.047(3) 0.005(2) C16 0.050(2) 0.048(2) 0.050(2) 0.0045(17) 0.0237(17) 0.0084(16) C17 0.057(2) 0.068(3) 0.056(2) -0.0033(19) 0.0289(19) 0.0070(19) C18 0.058(2) 0.087(3) 0.061(2) 0.002(2) 0.035(2) 0.010(2) C19 0.044(2) 0.076(3) 0.058(2) -0.002(2) 0.0245(17) 0.0032(18) C20 0.044(2) 0.054(2) 0.051(2) 0.0051(17) 0.0223(16) 0.0050(17) C21 0.0420(19) 0.052(2) 0.051(2) 0.0090(17) 0.0227(16) 0.0054(16) C22 0.041(2) 0.065(2) 0.061(2) 0.0050(19) 0.0260(18) 0.0006(17) C23 0.044(2) 0.051(2) 0.0480(19) 0.0046(17) 0.0176(16) -0.0007(16) C24 0.053(2) 0.055(2) 0.056(2) 0.0044(19) 0.0176(18) -0.0081(18) C25 0.062(3) 0.116(4) 0.088(3) -0.030(3) 0.017(2) -0.020(3) C26 0.075(4) 0.140(6) 0.118(5) -0.038(4) 0.008(3) -0.031(4) C27 0.126(5) 0.109(5) 0.084(4) -0.031(3) 0.019(4) -0.043(4) C28 0.131(5) 0.124(5) 0.117(5) -0.059(4) 0.061(4) -0.045(4) C29 0.082(3) 0.117(4) 0.096(4) -0.044(3) 0.041(3) -0.032(3) C30 0.051(2) 0.054(2) 0.050(2) 0.0022(17) 0.0265(17) 0.0080(17) C31 0.058(2) 0.061(3) 0.052(2) -0.0085(18) 0.0294(18) 0.0012(18) C32 0.056(2) 0.050(2) 0.055(2) 0.0001(18) 0.0259(18) 0.0047(17) C33 0.057(2) 0.057(2) 0.059(2) 0.0007(19) 0.0243(19) 0.0013(18) C34 0.067(3) 0.105(4) 0.086(3) -0.031(3) 0.039(2) -0.017(3) C35 0.079(3) 0.119(4) 0.089(3) -0.045(3) 0.035(3) -0.024(3) C36 0.066(3) 0.093(4) 0.092(3) -0.026(3) 0.017(3) -0.020(3) C37 0.055(3) 0.084(3) 0.106(4) -0.006(3) 0.031(3) -0.006(2) C38 0.061(3) 0.061(3) 0.083(3) -0.001(2) 0.034(2) 0.005(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 N6 2.196(3) . ? Ag1 N2 2.311(3) . ? Ag1 N1 2.362(3) . ? Ag1 O1 2.864(2) . ? Ag1 Ag1 3.0403(7) 3_677 ? N1 C2 1.338(4) . ? N1 C6 1.341(4) . ? N2 C7 1.335(4) . ? N2 N3 1.356(3) . ? N3 C9 1.353(4) . ? N3 H3 0.8600 . ? N4 C16 1.335(4) . ? N4 C20 1.340(4) . ? N5 C21 1.339(4) . ? N5 N6 1.349(4) . ? N5 H5 0.8600 . ? N6 C23 1.341(4) . ? N7 N8 1.348(4) . ? N7 C30 1.355(4) . ? N7 H7 0.8600 . ? N8 C32 1.338(4) . ? O1 C1 1.251(4) . ? O2 C1 1.235(4) . ? C1 C2 1.522(5) . ? C2 C3 1.381(4) . ? C3 C4 1.375(5) . ? C3 H3A 0.9300 . ? C4 C5 1.373(5) . ? C4 H4 0.9300 . ? C5 C6 1.383(4) . ? C5 H5A 0.9300 . ? C6 C7 1.469(4) . ? C7 C8 1.397(4) . ? C8 C9 1.370(5) . ? C8 H8 0.9300 . ? C9 C10 1.471(5) . ? C10 C11 1.380(5) . ? C10 C15 1.389(5) . ? C11 C12 1.382(5) . ? C11 H11 0.9300 . ? C12 C13 1.359(6) . ? C12 H12 0.9300 . ? C13 C14 1.371(6) . ? C13 H13 0.9300 . ? C14 C15 1.376(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.390(5) . ? C16 C30 1.459(5) . ? C17 C18 1.363(5) . ? C17 H17 0.9300 . ? C18 C19 1.377(5) . ? C18 H18 0.9300 . ? C19 C20 1.391(5) . ? C19 H19 0.9300 . ? C20 C21 1.463(5) . ? C21 C22 1.369(5) . ? C22 C23 1.389(5) . ? C22 H22 0.9300 . ? C23 C24 1.471(5) . ? C24 C29 1.362(6) . ? C24 C25 1.374(5) . ? C25 C26 1.378(7) . ? C25 H25 0.9300 . ? C26 C27 1.362(8) . ? C26 H26 0.9300 . ? C27 C28 1.356(7) . ? C27 H27 0.9300 . ? C28 C29 1.381(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.370(5) . ? C31 C32 1.393(5) . ? C31 H31 0.9300 . ? C32 C33 1.473(5) . ? C33 C38 1.382(5) . ? C33 C34 1.394(5) . ? C34 C35 1.377(6) . ? C34 H34 0.9300 . ? C35 C36 1.362(6) . ? C35 H35 0.9300 . ? C36 C37 1.364(6) . ? C36 H36 0.9300 . ? C37 C38 1.379(6) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N2 152.11(10) . . ? N6 Ag1 N1 131.96(9) . . ? N2 Ag1 N1 71.27(9) . . ? N6 Ag1 O1 78.32(9) . . ? N2 Ag1 O1 129.47(8) . . ? N1 Ag1 O1 62.43(8) . . ? N6 Ag1 Ag1 116.94(7) . 3_677 ? N2 Ag1 Ag1 63.61(7) . 3_677 ? N1 Ag1 Ag1 99.63(6) . 3_677 ? O1 Ag1 Ag1 104.45(5) . 3_677 ? C2 N1 C6 118.6(3) . . ? C2 N1 Ag1 125.4(2) . . ? C6 N1 Ag1 115.7(2) . . ? C7 N2 N3 105.4(3) . . ? C7 N2 Ag1 115.0(2) . . ? N3 N2 Ag1 137.7(2) . . ? C9 N3 N2 111.9(3) . . ? C9 N3 H3 124.1 . . ? N2 N3 H3 124.1 . . ? C16 N4 C20 118.0(3) . . ? C21 N5 N6 112.7(3) . . ? C21 N5 H5 123.6 . . ? N6 N5 H5 123.6 . . ? C23 N6 N5 105.1(3) . . ? C23 N6 Ag1 139.6(2) . . ? N5 N6 Ag1 115.3(2) . . ? N8 N7 C30 112.4(3) . . ? N8 N7 H7 123.8 . . ? C30 N7 H7 123.8 . . ? C32 N8 N7 105.0(3) . . ? C1 O1 Ag1 107.5(2) . . ? O2 C1 O1 126.7(3) . . ? O2 C1 C2 116.7(3) . . ? O1 C1 C2 116.6(3) . . ? N1 C2 C3 122.0(3) . . ? N1 C2 C1 117.2(3) . . ? C3 C2 C1 120.8(3) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N1 C6 C5 122.0(3) . . ? N1 C6 C7 115.8(3) . . ? C5 C6 C7 122.2(3) . . ? N2 C7 C8 110.2(3) . . ? N2 C7 C6 120.0(3) . . ? C8 C7 C6 129.8(3) . . ? C9 C8 C7 106.4(3) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? N3 C9 C8 106.2(3) . . ? N3 C9 C10 122.7(3) . . ? C8 C9 C10 131.1(3) . . ? C11 C10 C15 119.0(4) . . ? C11 C10 C9 122.3(3) . . ? C15 C10 C9 118.6(4) . . ? C10 C11 C12 120.4(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 119.9(4) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? N4 C16 C17 122.1(3) . . ? N4 C16 C30 117.9(3) . . ? C17 C16 C30 120.0(3) . . ? C18 C17 C16 119.1(4) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 117.5(3) . . ? C18 C19 H19 121.2 . . ? C20 C19 H19 121.2 . . ? N4 C20 C19 123.2(3) . . ? N4 C20 C21 115.5(3) . . ? C19 C20 C21 121.3(3) . . ? N5 C21 C22 105.7(3) . . ? N5 C21 C20 120.2(3) . . ? C22 C21 C20 134.2(3) . . ? C21 C22 C23 106.9(3) . . ? C21 C22 H22 126.5 . . ? C23 C22 H22 126.5 . . ? N6 C23 C22 109.6(3) . . ? N6 C23 C24 121.5(3) . . ? C22 C23 C24 128.9(3) . . ? C29 C24 C25 117.3(4) . . ? C29 C24 C23 123.4(4) . . ? C25 C24 C23 119.3(4) . . ? C24 C25 C26 121.2(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.7(5) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.7(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C24 C29 C28 122.0(5) . . ? C24 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? N7 C30 C31 105.8(3) . . ? N7 C30 C16 123.5(3) . . ? C31 C30 C16 130.7(3) . . ? C30 C31 C32 106.4(3) . . ? C30 C31 H31 126.8 . . ? C32 C31 H31 126.8 . . ? N8 C32 C31 110.4(3) . . ? N8 C32 C33 121.2(3) . . ? C31 C32 C33 128.5(3) . . ? C38 C33 C34 118.0(4) . . ? C38 C33 C32 122.4(4) . . ? C34 C33 C32 119.6(4) . . ? C35 C34 C33 121.1(4) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C36 C35 C34 119.8(5) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 119.9(4) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 121.1(4) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C38 C33 120.1(4) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 N1 C2 23.1(3) . . . . ? N2 Ag1 N1 C2 -175.1(3) . . . . ? O1 Ag1 N1 C2 -16.0(2) . . . . ? Ag1 Ag1 N1 C2 -117.3(3) 3_677 . . . ? N6 Ag1 N1 C6 -150.6(2) . . . . ? N2 Ag1 N1 C6 11.3(2) . . . . ? O1 Ag1 N1 C6 170.4(2) . . . . ? Ag1 Ag1 N1 C6 69.0(2) 3_677 . . . ? N6 Ag1 N2 C7 137.6(2) . . . . ? N1 Ag1 N2 C7 -12.7(2) . . . . ? O1 Ag1 N2 C7 -36.9(3) . . . . ? Ag1 Ag1 N2 C7 -124.2(2) 3_677 . . . ? N6 Ag1 N2 N3 -24.1(4) . . . . ? N1 Ag1 N2 N3 -174.4(3) . . . . ? O1 Ag1 N2 N3 161.4(3) . . . . ? Ag1 Ag1 N2 N3 74.1(3) 3_677 . . . ? C7 N2 N3 C9 0.7(3) . . . . ? Ag1 N2 N3 C9 163.5(2) . . . . ? C21 N5 N6 C23 0.7(4) . . . . ? C21 N5 N6 Ag1 179.8(2) . . . . ? N2 Ag1 N6 C23 17.0(5) . . . . ? N1 Ag1 N6 C23 157.9(3) . . . . ? O1 Ag1 N6 C23 -167.4(3) . . . . ? Ag1 Ag1 N6 C23 -67.0(3) 3_677 . . . ? N2 Ag1 N6 N5 -161.7(2) . . . . ? N1 Ag1 N6 N5 -20.8(3) . . . . ? O1 Ag1 N6 N5 14.0(2) . . . . ? Ag1 Ag1 N6 N5 114.39(19) 3_677 . . . ? C30 N7 N8 C32 0.8(4) . . . . ? N6 Ag1 O1 C1 -124.3(2) . . . . ? N2 Ag1 O1 C1 53.1(3) . . . . ? N1 Ag1 O1 C1 27.1(2) . . . . ? Ag1 Ag1 O1 C1 120.6(2) 3_677 . . . ? Ag1 O1 C1 O2 142.8(3) . . . . ? Ag1 O1 C1 C2 -34.9(3) . . . . ? C6 N1 C2 C3 0.1(5) . . . . ? Ag1 N1 C2 C3 -173.4(2) . . . . ? C6 N1 C2 C1 179.1(3) . . . . ? Ag1 N1 C2 C1 5.6(4) . . . . ? O2 C1 C2 N1 -152.8(3) . . . . ? O1 C1 C2 N1 25.1(5) . . . . ? O2 C1 C2 C3 26.2(5) . . . . ? O1 C1 C2 C3 -155.9(3) . . . . ? N1 C2 C3 C4 1.8(5) . . . . ? C1 C2 C3 C4 -177.2(3) . . . . ? C2 C3 C4 C5 -2.2(6) . . . . ? C3 C4 C5 C6 0.8(6) . . . . ? C2 N1 C6 C5 -1.5(5) . . . . ? Ag1 N1 C6 C5 172.5(3) . . . . ? C2 N1 C6 C7 177.3(3) . . . . ? Ag1 N1 C6 C7 -8.6(4) . . . . ? C4 C5 C6 N1 1.1(5) . . . . ? C4 C5 C6 C7 -177.7(3) . . . . ? N3 N2 C7 C8 -0.1(3) . . . . ? Ag1 N2 C7 C8 -167.5(2) . . . . ? N3 N2 C7 C6 -179.0(3) . . . . ? Ag1 N2 C7 C6 13.6(4) . . . . ? N1 C6 C7 N2 -3.3(4) . . . . ? C5 C6 C7 N2 175.6(3) . . . . ? N1 C6 C7 C8 178.0(3) . . . . ? C5 C6 C7 C8 -3.1(5) . . . . ? N2 C7 C8 C9 -0.4(4) . . . . ? C6 C7 C8 C9 178.3(3) . . . . ? N2 N3 C9 C8 -0.9(4) . . . . ? N2 N3 C9 C10 -180.0(3) . . . . ? C7 C8 C9 N3 0.8(4) . . . . ? C7 C8 C9 C10 179.7(3) . . . . ? N3 C9 C10 C11 -1.6(5) . . . . ? C8 C9 C10 C11 179.5(4) . . . . ? N3 C9 C10 C15 177.3(3) . . . . ? C8 C9 C10 C15 -1.5(6) . . . . ? C15 C10 C11 C12 0.5(6) . . . . ? C9 C10 C11 C12 179.5(3) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C14 -1.1(7) . . . . ? C12 C13 C14 C15 1.6(8) . . . . ? C13 C14 C15 C10 -1.0(7) . . . . ? C11 C10 C15 C14 0.0(6) . . . . ? C9 C10 C15 C14 -179.0(4) . . . . ? C20 N4 C16 C17 0.2(5) . . . . ? C20 N4 C16 C30 -179.5(3) . . . . ? N4 C16 C17 C18 -1.4(6) . . . . ? C30 C16 C17 C18 178.2(3) . . . . ? C16 C17 C18 C19 2.2(6) . . . . ? C17 C18 C19 C20 -1.7(6) . . . . ? C16 N4 C20 C19 0.3(5) . . . . ? C16 N4 C20 C21 -178.9(3) . . . . ? C18 C19 C20 N4 0.5(6) . . . . ? C18 C19 C20 C21 179.7(3) . . . . ? N6 N5 C21 C22 -0.4(4) . . . . ? N6 N5 C21 C20 -179.5(3) . . . . ? N4 C20 C21 N5 -3.1(5) . . . . ? C19 C20 C21 N5 177.7(3) . . . . ? N4 C20 C21 C22 178.1(4) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? N5 C21 C22 C23 -0.1(4) . . . . ? C20 C21 C22 C23 178.8(4) . . . . ? N5 N6 C23 C22 -0.8(4) . . . . ? Ag1 N6 C23 C22 -179.5(3) . . . . ? N5 N6 C23 C24 -179.9(3) . . . . ? Ag1 N6 C23 C24 1.4(5) . . . . ? C21 C22 C23 N6 0.5(4) . . . . ? C21 C22 C23 C24 179.6(3) . . . . ? N6 C23 C24 C29 -15.5(6) . . . . ? C22 C23 C24 C29 165.5(4) . . . . ? N6 C23 C24 C25 164.6(4) . . . . ? C22 C23 C24 C25 -14.3(6) . . . . ? C29 C24 C25 C26 0.5(8) . . . . ? C23 C24 C25 C26 -179.6(5) . . . . ? C24 C25 C26 C27 1.0(9) . . . . ? C25 C26 C27 C28 -1.0(10) . . . . ? C26 C27 C28 C29 -0.5(10) . . . . ? C25 C24 C29 C28 -2.0(8) . . . . ? C23 C24 C29 C28 178.1(5) . . . . ? C27 C28 C29 C24 2.1(9) . . . . ? N8 N7 C30 C31 -0.7(4) . . . . ? N8 N7 C30 C16 179.2(3) . . . . ? N4 C16 C30 N7 8.4(5) . . . . ? C17 C16 C30 N7 -171.2(3) . . . . ? N4 C16 C30 C31 -171.8(4) . . . . ? C17 C16 C30 C31 8.6(6) . . . . ? N7 C30 C31 C32 0.3(4) . . . . ? C16 C30 C31 C32 -179.6(4) . . . . ? N7 N8 C32 C31 -0.6(4) . . . . ? N7 N8 C32 C33 178.8(3) . . . . ? C30 C31 C32 N8 0.2(4) . . . . ? C30 C31 C32 C33 -179.1(4) . . . . ? N8 C32 C33 C38 -1.2(6) . . . . ? C31 C32 C33 C38 178.0(4) . . . . ? N8 C32 C33 C34 -179.9(4) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C38 C33 C34 C35 -0.6(7) . . . . ? C32 C33 C34 C35 178.1(4) . . . . ? C33 C34 C35 C36 0.5(8) . . . . ? C34 C35 C36 C37 0.1(8) . . . . ? C35 C36 C37 C38 -0.6(8) . . . . ? C36 C37 C38 C33 0.5(7) . . . . ? C34 C33 C38 C37 0.1(6) . . . . ? C32 C33 C38 C37 -178.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.537 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.057 #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 655898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Ag2 N10, 2(N O3), H2 O' _chemical_formula_sum 'C26 H28 Ag2 N12 O7' _chemical_formula_weight 836.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 13.179(2) _cell_length_b 10.5389(16) _cell_length_c 22.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.296(2) _cell_angle_gamma 90.00 _cell_volume 3052.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6585 _cell_measurement_theta_min 2.483 _cell_measurement_theta_max 27.182 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6280 _exptl_absorpt_correction_T_max 0.8882 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15613 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5371 _reflns_number_gt 4297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+5.4399P] 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 5371 _refine_ls_number_parameters 430 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.75334(2) 0.08258(3) 0.727091(16) 0.05279(12) Uani 1 1 d . . . Ag2 Ag 0.81840(3) 0.34492(3) 0.729006(15) 0.06376(13) Uani 1 1 d . . . N1 N 0.7398(2) 0.2287(3) 0.82940(15) 0.0431(8) Uani 1 1 d . . . N2 N 0.9306(2) 0.2999(3) 0.80445(14) 0.0445(8) Uani 1 1 d . . . N3 N 1.0328(3) 0.3024(3) 0.80438(16) 0.0496(8) Uani 1 1 d . . . H29 H 1.0622 0.3182 0.7727 0.060 Uiso 1 1 calc R . . N4 N 0.6013(2) 0.1399(3) 0.73570(17) 0.0495(9) Uani 1 1 d . . . N5 N 0.5150(3) 0.1219(4) 0.69646(19) 0.0583(10) Uani 1 1 d . . . H5 H 0.5144 0.0987 0.6592 0.070 Uiso 1 1 calc R . . N6 N 0.6099(2) 0.4512(3) 0.67769(13) 0.0367(7) Uani 1 1 d . . . N7 N 0.7946(2) 0.3886(3) 0.63465(14) 0.0425(8) Uani 1 1 d . . . N8 N 0.8696(2) 0.3726(3) 0.59945(15) 0.0475(8) Uani 1 1 d . . . H8 H 0.9325 0.3594 0.6136 0.057 Uiso 1 1 calc R . . N9 N 0.6033(2) 0.5273(3) 0.79807(14) 0.0419(7) Uani 1 1 d . . . N10 N 0.5751(2) 0.5477(3) 0.85377(15) 0.0470(8) Uani 1 1 d . . . H10 H 0.6169 0.5694 0.8850 0.056 Uiso 1 1 calc R . . N11 N 0.7174(4) 0.0820(4) 0.5405(3) 0.0802(15) Uani 1 1 d . . . N12 N 0.1315(3) 0.3889(4) 0.6702(2) 0.0619(10) Uani 1 1 d . . . O1 O 0.7070(3) 0.0889(4) 0.5939(2) 0.0992(14) Uani 1 1 d . . . O2 O 0.6420(4) 0.0897(5) 0.5018(2) 0.126(2) Uani 1 1 d . . . O3 O 0.8054(4) 0.0724(4) 0.5260(2) 0.1002(14) Uani 1 1 d . . . O4 O 0.1962(3) 0.4046(4) 0.71456(19) 0.0900(13) Uani 1 1 d . . . O5 O 0.0487(2) 0.3403(4) 0.67866(15) 0.0692(9) Uani 1 1 d . . . O6 O 0.1471(4) 0.4172(6) 0.6193(2) 0.129(2) Uani 1 1 d . . . O7 O 0.5296(4) 0.9047(5) 0.4298(2) 0.1092(15) Uani 1 1 d D . . C1 C 0.6438(3) 0.2069(4) 0.8405(2) 0.0507(10) Uani 1 1 d . . . C2 C 0.6165(4) 0.2125(5) 0.8990(2) 0.0708(14) Uani 1 1 d . . . H2 H 0.5493 0.1976 0.9058 0.085 Uiso 1 1 calc R . . C3 C 0.6899(5) 0.2401(6) 0.9465(2) 0.0787(16) Uani 1 1 d . . . H3 H 0.6733 0.2440 0.9860 0.094 Uiso 1 1 calc R . . C4 C 0.7884(4) 0.2619(5) 0.9352(2) 0.0631(12) Uani 1 1 d . . . H4 H 0.8391 0.2814 0.9670 0.076 Uiso 1 1 calc R . . C5 C 0.8115(3) 0.2547(4) 0.87629(18) 0.0449(9) Uani 1 1 d . . . C6 C 0.9156(3) 0.2721(4) 0.86131(17) 0.0430(9) Uani 1 1 d . . . C7 C 1.0092(3) 0.2587(4) 0.89729(19) 0.0536(11) Uani 1 1 d . . . H7 H 1.0200 0.2406 0.9387 0.064 Uiso 1 1 calc R . . C8 C 1.0831(3) 0.2776(4) 0.8593(2) 0.0526(11) Uani 1 1 d . . . C9 C 1.1973(4) 0.2701(6) 0.8696(3) 0.0743(15) Uani 1 1 d . . . H9A H 1.2242 0.2884 0.8323 0.111 Uiso 1 1 calc R . . H9B H 1.2178 0.1862 0.8831 0.111 Uiso 1 1 calc R . . H9C H 1.2233 0.3307 0.9000 0.111 Uiso 1 1 calc R . . C10 C 0.5689(3) 0.1747(4) 0.7882(2) 0.0503(11) Uani 1 1 d . . . C11 C 0.4625(3) 0.1773(5) 0.7809(3) 0.0662(14) Uani 1 1 d . . . H11 H 0.4211 0.1976 0.8105 0.079 Uiso 1 1 calc R . . C12 C 0.4309(3) 0.1447(4) 0.7227(3) 0.0654(14) Uani 1 1 d . . . C13 C 0.3262(4) 0.1333(6) 0.6870(3) 0.090(2) Uani 1 1 d . . . H13A H 0.3326 0.1066 0.6463 0.135 Uiso 1 1 calc R . . H13B H 0.2925 0.2142 0.6860 0.135 Uiso 1 1 calc R . . H13C H 0.2868 0.0720 0.7061 0.135 Uiso 1 1 calc R . . C14 C 0.5184(3) 0.4638(3) 0.69834(17) 0.0378(8) Uani 1 1 d . . . C15 C 0.4262(3) 0.4473(4) 0.66124(18) 0.0458(10) Uani 1 1 d . . . H15 H 0.3643 0.4570 0.6767 0.055 Uiso 1 1 calc R . . C16 C 0.4282(3) 0.4164(4) 0.60112(19) 0.0506(10) Uani 1 1 d . . . H16 H 0.3675 0.4038 0.5755 0.061 Uiso 1 1 calc R . . C17 C 0.5203(3) 0.4045(4) 0.57931(18) 0.0468(10) Uani 1 1 d . . . H17 H 0.5227 0.3846 0.5386 0.056 Uiso 1 1 calc R . . C18 C 0.6102(3) 0.4223(3) 0.61867(17) 0.0374(8) Uani 1 1 d . . . C19 C 0.7096(3) 0.4059(4) 0.59627(17) 0.0391(8) Uani 1 1 d . . . C20 C 0.7329(3) 0.4011(4) 0.53633(18) 0.0484(10) Uani 1 1 d . . . H20 H 0.6875 0.4106 0.5009 0.058 Uiso 1 1 calc R . . C21 C 0.8359(3) 0.3795(4) 0.54027(19) 0.0480(10) Uani 1 1 d . . . C22 C 0.9060(4) 0.3599(5) 0.4928(2) 0.0679(14) Uani 1 1 d . . . H22A H 0.9745 0.3469 0.5123 0.102 Uiso 1 1 calc R . . H22B H 0.9042 0.4334 0.4671 0.102 Uiso 1 1 calc R . . H22C H 0.8842 0.2869 0.4687 0.102 Uiso 1 1 calc R . . C23 C 0.5185(3) 0.4964(4) 0.76288(17) 0.0386(8) Uani 1 1 d . . . C24 C 0.4358(3) 0.4966(4) 0.79709(19) 0.0502(10) Uani 1 1 d . . . H24 H 0.3679 0.4777 0.7832 0.060 Uiso 1 1 calc R . . C25 C 0.4753(3) 0.5304(4) 0.85488(19) 0.0502(10) Uani 1 1 d . . . C26 C 0.4273(4) 0.5502(6) 0.9120(2) 0.0795(17) Uani 1 1 d . . . H26A H 0.4790 0.5740 0.9445 0.119 Uiso 1 1 calc R . . H26B H 0.3951 0.4730 0.9225 0.119 Uiso 1 1 calc R . . H26C H 0.3769 0.6163 0.9056 0.119 Uiso 1 1 calc R . . H28 H 0.4697(19) 0.913(5) 0.441(2) 0.080 Uiso 1 1 d D . . H27 H 0.565(3) 0.963(4) 0.449(2) 0.080 Uiso 1 1 d 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 0.03758(17) 0.0520(2) 0.0710(2) 0.00237(16) 0.01553(15) 0.00149(14) Ag2 0.0936(3) 0.0516(2) 0.04111(19) -0.00315(15) -0.01090(17) 0.00604(19) N1 0.0482(19) 0.0389(18) 0.0444(19) 0.0000(15) 0.0143(15) 0.0031(15) N2 0.0467(19) 0.050(2) 0.0374(18) 0.0007(15) 0.0057(14) -0.0059(16) N3 0.048(2) 0.056(2) 0.046(2) 0.0016(16) 0.0080(16) -0.0090(17) N4 0.0353(17) 0.046(2) 0.066(2) -0.0015(18) 0.0022(16) 0.0003(15) N5 0.045(2) 0.049(2) 0.079(3) 0.0019(19) -0.0030(19) -0.0004(17) N6 0.0354(16) 0.0377(17) 0.0360(17) 0.0008(13) 0.0005(13) -0.0031(13) N7 0.0383(17) 0.049(2) 0.0396(18) -0.0044(15) 0.0029(14) 0.0025(15) N8 0.0358(17) 0.059(2) 0.048(2) -0.0060(17) 0.0057(15) 0.0014(16) N9 0.0416(17) 0.049(2) 0.0355(17) -0.0018(15) 0.0049(14) -0.0038(15) N10 0.0447(19) 0.058(2) 0.0377(18) -0.0038(16) 0.0027(15) -0.0049(16) N11 0.090(4) 0.056(3) 0.082(4) 0.011(2) -0.038(3) -0.012(3) N12 0.048(2) 0.073(3) 0.066(3) 0.009(2) 0.012(2) 0.005(2) O1 0.104(3) 0.113(4) 0.072(3) 0.008(3) -0.021(2) 0.012(3) O2 0.128(4) 0.140(4) 0.092(3) 0.030(3) -0.059(3) -0.044(3) O3 0.101(3) 0.098(3) 0.099(3) 0.011(3) 0.002(3) 0.008(3) O4 0.0469(19) 0.124(4) 0.096(3) -0.023(3) -0.0055(19) -0.001(2) O5 0.0464(18) 0.094(3) 0.067(2) 0.0093(19) 0.0052(15) -0.0158(17) O6 0.110(4) 0.190(6) 0.091(3) 0.051(3) 0.032(3) -0.023(4) O7 0.117(4) 0.094(3) 0.115(4) -0.033(3) 0.005(3) -0.022(3) C1 0.058(3) 0.039(2) 0.059(3) 0.004(2) 0.024(2) 0.0088(19) C2 0.071(3) 0.076(4) 0.074(4) 0.005(3) 0.042(3) 0.002(3) C3 0.104(4) 0.086(4) 0.055(3) 0.000(3) 0.042(3) 0.003(3) C4 0.087(3) 0.061(3) 0.043(2) -0.004(2) 0.015(2) -0.005(3) C5 0.062(2) 0.034(2) 0.041(2) 0.0019(17) 0.0134(19) 0.0019(19) C6 0.056(2) 0.035(2) 0.037(2) 0.0012(17) 0.0049(18) -0.0035(18) C7 0.066(3) 0.053(3) 0.040(2) 0.005(2) -0.003(2) -0.001(2) C8 0.055(3) 0.046(2) 0.054(3) 0.002(2) -0.003(2) -0.005(2) C9 0.056(3) 0.083(4) 0.080(4) 0.009(3) -0.007(3) -0.002(3) C10 0.039(2) 0.039(2) 0.076(3) 0.009(2) 0.023(2) 0.0069(18) C11 0.043(2) 0.052(3) 0.108(4) 0.012(3) 0.029(3) 0.010(2) C12 0.037(2) 0.044(3) 0.115(5) 0.012(3) 0.006(3) 0.0003(19) C13 0.040(3) 0.077(4) 0.149(6) 0.014(4) -0.006(3) -0.003(3) C14 0.038(2) 0.034(2) 0.041(2) 0.0045(16) 0.0005(16) -0.0053(16) C15 0.034(2) 0.053(2) 0.049(2) 0.0022(19) 0.0003(17) -0.0045(18) C16 0.039(2) 0.061(3) 0.048(2) -0.004(2) -0.0097(18) -0.006(2) C17 0.047(2) 0.055(3) 0.036(2) -0.0057(18) -0.0052(17) 0.001(2) C18 0.040(2) 0.0337(19) 0.037(2) 0.0013(16) -0.0014(16) -0.0015(16) C19 0.041(2) 0.037(2) 0.038(2) 0.0001(17) 0.0005(16) -0.0009(17) C20 0.052(2) 0.055(3) 0.037(2) 0.0022(19) 0.0007(18) -0.001(2) C21 0.053(2) 0.048(2) 0.044(2) -0.0013(19) 0.0113(19) -0.004(2) C22 0.061(3) 0.090(4) 0.056(3) -0.006(3) 0.022(2) -0.007(3) C23 0.0361(19) 0.039(2) 0.040(2) 0.0032(17) 0.0033(16) -0.0024(16) C24 0.038(2) 0.059(3) 0.054(3) -0.005(2) 0.0060(18) -0.0090(19) C25 0.047(2) 0.056(3) 0.050(2) 0.002(2) 0.0135(19) 0.000(2) C26 0.066(3) 0.123(5) 0.054(3) -0.010(3) 0.024(2) -0.009(3) _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 N9 2.118(3) 2_646 ? Ag1 N4 2.125(3) . ? Ag1 Ag2 2.8891(6) 2_646 ? Ag1 Ag2 2.8933(6) . ? Ag2 N7 2.125(3) . ? Ag2 N2 2.139(3) . ? Ag2 Ag1 2.8891(6) 2_656 ? N1 C1 1.340(5) . ? N1 C5 1.341(5) . ? N2 C6 1.332(5) . ? N2 N3 1.347(4) . ? N3 C8 1.336(5) . ? N3 H29 0.8600 . ? N4 C10 1.340(5) . ? N4 N5 1.354(5) . ? N5 C12 1.337(6) . ? N5 H5 0.8600 . ? N6 C18 1.343(5) . ? N6 C14 1.349(5) . ? N7 C19 1.330(5) . ? N7 N8 1.345(4) . ? N8 C21 1.332(5) . ? N8 H8 0.8600 . ? N9 C23 1.320(5) . ? N9 N10 1.350(4) . ? N9 Ag1 2.118(3) 2_656 ? N10 C25 1.331(5) . ? N10 H10 0.8600 . ? N11 O1 1.209(6) . ? N11 O2 1.231(6) . ? N11 O3 1.247(7) . ? N12 O6 1.209(5) . ? N12 O4 1.228(5) . ? N12 O5 1.242(5) . ? O7 H28 0.861(19) . ? O7 H28 0.861(19) . ? O7 H27 0.852(19) . ? C1 C2 1.391(6) . ? C1 C10 1.462(6) . ? C2 C3 1.366(8) . ? C2 H2 0.9300 . ? C3 C4 1.372(7) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 C6 1.463(6) . ? C6 C7 1.389(6) . ? C7 C8 1.379(6) . ? C7 H7 0.9300 . ? C8 C9 1.496(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.392(6) . ? C11 C12 1.349(7) . ? C11 H11 0.9300 . ? C12 C13 1.504(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.388(5) . ? C14 C23 1.470(5) . ? C15 C16 1.375(6) . ? C15 H15 0.9300 . ? C16 C17 1.367(6) . ? C16 H16 0.9300 . ? C17 C18 1.392(5) . ? C17 H17 0.9300 . ? C18 C19 1.468(5) . ? C19 C20 1.402(6) . ? C20 C21 1.367(6) . ? C20 H20 0.9300 . ? C21 C22 1.499(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.405(5) . ? C24 C25 1.366(6) . ? C24 H24 0.9300 . ? C25 C26 1.500(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 N9 Ag1 N4 169.97(13) 2_646 . ? N9 Ag1 Ag2 101.02(9) 2_646 2_646 ? N4 Ag1 Ag2 82.16(10) . 2_646 ? N9 Ag1 Ag2 89.66(9) 2_646 . ? N4 Ag1 Ag2 90.47(9) . . ? Ag2 Ag1 Ag2 158.828(15) 2_646 . ? N7 Ag2 N2 144.87(12) . . ? N7 Ag2 Ag1 97.45(9) . 2_656 ? N2 Ag2 Ag1 98.78(9) . 2_656 ? N7 Ag2 Ag1 100.73(9) . . ? N2 Ag2 Ag1 88.48(9) . . ? Ag1 Ag2 Ag1 136.413(18) 2_656 . ? C1 N1 C5 118.8(3) . . ? C6 N2 N3 105.9(3) . . ? C6 N2 Ag2 128.1(3) . . ? N3 N2 Ag2 125.9(2) . . ? C8 N3 N2 112.1(3) . . ? C8 N3 H29 124.0 . . ? N2 N3 H29 124.0 . . ? C10 N4 N5 105.2(3) . . ? C10 N4 Ag1 124.3(3) . . ? N5 N4 Ag1 128.8(3) . . ? C12 N5 N4 111.7(4) . . ? C12 N5 H5 124.1 . . ? N4 N5 H5 124.1 . . ? C18 N6 C14 117.8(3) . . ? C19 N7 N8 105.5(3) . . ? C19 N7 Ag2 131.7(3) . . ? N8 N7 Ag2 121.0(2) . . ? C21 N8 N7 112.7(3) . . ? C21 N8 H8 123.7 . . ? N7 N8 H8 123.7 . . ? C23 N9 N10 105.6(3) . . ? C23 N9 Ag1 129.0(3) . 2_656 ? N10 N9 Ag1 123.7(2) . 2_656 ? C25 N10 N9 112.5(3) . . ? C25 N10 H10 123.8 . . ? N9 N10 H10 123.8 . . ? O1 N11 O2 119.8(7) . . ? O1 N11 O3 118.8(5) . . ? O2 N11 O3 121.4(6) . . ? O6 N12 O4 122.1(5) . . ? O6 N12 O5 120.0(5) . . ? O4 N12 O5 117.9(4) . . ? H28 O7 H28 0(6) . . ? H28 O7 H27 105(3) . . ? H28 O7 H27 105(3) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 C10 116.9(4) . . ? C2 C1 C10 121.4(4) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.3(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 122.3(4) . . ? N2 C6 C7 109.7(4) . . ? N2 C6 C5 119.9(3) . . ? C7 C6 C5 130.3(4) . . ? C8 C7 C6 106.3(4) . . ? C8 C7 H7 126.9 . . ? C6 C7 H7 126.9 . . ? N3 C8 C7 106.1(4) . . ? N3 C8 C9 121.5(4) . . ? C7 C8 C9 132.4(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 109.4(4) . . ? N4 C10 C1 119.6(3) . . ? C11 C10 C1 131.0(4) . . ? C12 C11 C10 106.9(4) . . ? C12 C11 H11 126.6 . . ? C10 C11 H11 126.6 . . ? N5 C12 C11 106.8(4) . . ? N5 C12 C13 120.9(6) . . ? C11 C12 C13 132.3(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 C15 122.6(4) . . ? N6 C14 C23 117.5(3) . . ? C15 C14 C23 119.9(3) . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.3(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N6 C18 C17 122.2(4) . . ? N6 C18 C19 118.0(3) . . ? C17 C18 C19 119.8(3) . . ? N7 C19 C20 109.4(3) . . ? N7 C19 C18 121.0(3) . . ? C20 C19 C18 129.6(3) . . ? C21 C20 C19 106.3(4) . . ? C21 C20 H20 126.8 . . ? C19 C20 H20 126.8 . . ? N8 C21 C20 106.1(4) . . ? N8 C21 C22 121.6(4) . . ? C20 C21 C22 132.3(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C24 109.7(3) . . ? N9 C23 C14 121.9(3) . . ? C24 C23 C14 128.3(3) . . ? C25 C24 C23 106.0(3) . . ? C25 C24 H24 127.0 . . ? C23 C24 H24 127.0 . . ? N10 C25 C24 106.2(4) . . ? N10 C25 C26 121.4(4) . . ? C24 C25 C26 132.5(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.468 _refine_diff_density_min -1.564 _refine_diff_density_rms 0.074 #===END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 655899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H54 Ag6 N22 O7' _chemical_formula_weight 1782.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.032(3) _cell_length_b 12.0127(18) _cell_length_c 22.495(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6224.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3696 _cell_measurement_theta_min 2.531 _cell_measurement_theta_max 19.276 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7117 _exptl_absorpt_correction_T_max 0.8935 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31135 _diffrn_reflns_av_R_equivalents 0.1079 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5497 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5497 _refine_ls_number_parameters 408 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.038 _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 N8 N 0.4029(4) 0.5119(7) 0.2189(4) 0.049(2) Uani 1 1 d . . . N7 N 0.4182(4) 0.5422(8) 0.2753(4) 0.047(2) Uani 1 1 d . . . Ag1 Ag 0.46254(4) 0.68979(7) 0.30108(4) 0.0400(3) Uani 1 1 d . . . Ag2 Ag 0.38032(4) 0.79194(8) 0.21952(4) 0.0493(3) Uani 1 1 d . . . Ag3 Ag 0.55936(4) 0.57753(9) 0.35809(4) 0.0614(3) Uani 1 1 d . . . N1 N 0.3807(4) 0.8185(7) 0.3543(4) 0.040(2) Uani 1 1 d . . . N2 N 0.3071(4) 0.7312(8) 0.2660(4) 0.048(2) Uani 1 1 d . . . N3 N 0.2660(4) 0.6679(8) 0.2397(4) 0.058(3) Uani 1 1 d . . . H3 H 0.2652 0.6543 0.2022 0.070 Uiso 1 1 calc R . . N4 N 0.5009(4) 0.8340(7) 0.3370(4) 0.041(2) Uani 1 1 d . . . N5 N 0.5585(4) 0.8608(8) 0.3377(4) 0.046(2) Uani 1 1 d . . . N6 N 0.4355(4) 0.5638(8) 0.3976(4) 0.048(2) Uani 1 1 d . . . N9 N 0.5396(5) 0.6441(9) 0.4425(5) 0.060(3) Uani 1 1 d . . . N10 N 0.5803(4) 0.6970(9) 0.4746(5) 0.063(3) Uani 1 1 d . . . H10 H 0.6154 0.7071 0.4627 0.076 Uiso 1 1 calc R . . N11 N 0.7175(5) 0.6867(10) 0.4145(5) 0.066(3) Uani 1 1 d . . . O1 O 0.6766(5) 0.6866(11) 0.3818(5) 0.118(5) Uani 1 1 d . . . O2 O 0.7649(5) 0.6602(11) 0.3946(5) 0.126(5) Uani 1 1 d . . . O3 O 0.7106(5) 0.7103(10) 0.4664(4) 0.110(4) Uani 1 1 d . . . O4 O 0.5000 0.0924(14) 0.2500 0.180(7) Uani 1 2 d SDU . . C1 C 0.4132(5) 0.8695(10) 0.3949(5) 0.045(3) Uani 1 1 d . . . C2 C 0.3904(5) 0.8981(10) 0.4503(5) 0.053(3) Uani 1 1 d . . . H2 H 0.4132 0.9368 0.4775 0.064 Uiso 1 1 calc R . . C3 C 0.3348(6) 0.8696(12) 0.4649(5) 0.069(4) Uani 1 1 d . . . H3A H 0.3199 0.8863 0.5023 0.083 Uiso 1 1 calc R . . C4 C 0.3014(5) 0.8159(10) 0.4232(5) 0.052(3) Uani 1 1 d . . . H4 H 0.2631 0.7964 0.4312 0.063 Uiso 1 1 calc R . . C5 C 0.3268(5) 0.7917(9) 0.3690(4) 0.037(3) Uani 1 1 d . . . C6 C 0.2914(4) 0.7337(9) 0.3247(5) 0.043(3) Uani 1 1 d . . . C7 C 0.2409(5) 0.6693(10) 0.3320(5) 0.054(3) Uani 1 1 d . . . H7 H 0.2211 0.6569 0.3674 0.064 Uiso 1 1 calc R . . C8 C 0.2268(5) 0.6288(10) 0.2781(6) 0.058(3) Uani 1 1 d . . . C9 C 0.1775(6) 0.5527(14) 0.2577(6) 0.103(6) Uani 1 1 d . . . H9A H 0.1776 0.5480 0.2150 0.154 Uiso 1 1 calc R . . H9B H 0.1411 0.5824 0.2709 0.154 Uiso 1 1 calc R . . H9C H 0.1829 0.4797 0.2742 0.154 Uiso 1 1 calc R . . C10 C 0.4747(5) 0.8906(9) 0.3827(5) 0.041(3) Uani 1 1 d . . . C11 C 0.5154(5) 0.9541(10) 0.4109(5) 0.052(3) Uani 1 1 d . . . H11 H 0.5093 1.0007 0.4434 0.063 Uiso 1 1 calc R . . C12 C 0.5669(5) 0.9356(10) 0.3820(5) 0.050(3) Uani 1 1 d . . . C13 C 0.6262(5) 0.9757(12) 0.3954(6) 0.076(5) Uani 1 1 d . . . H13A H 0.6527 0.9479 0.3660 0.113 Uiso 1 1 calc R . . H13B H 0.6377 0.9496 0.4339 0.113 Uiso 1 1 calc R . . H13C H 0.6266 1.0556 0.3949 0.113 Uiso 1 1 calc R . . C14 C 0.4384(5) 0.5921(10) 0.4547(5) 0.047(3) Uani 1 1 d . . . C15 C 0.3910(6) 0.5778(12) 0.4928(6) 0.066(4) Uani 1 1 d . . . H15 H 0.3929 0.6024 0.5319 0.080 Uiso 1 1 calc R . . C16 C 0.3411(6) 0.5268(13) 0.4718(6) 0.074(4) Uani 1 1 d . . . H16 H 0.3098 0.5140 0.4970 0.088 Uiso 1 1 calc R . . C17 C 0.3387(6) 0.4957(12) 0.4137(6) 0.070(4) Uani 1 1 d . . . H17 H 0.3056 0.4617 0.3988 0.084 Uiso 1 1 calc R . . C18 C 0.3866(5) 0.5152(9) 0.3765(5) 0.049(3) Uani 1 1 d . . . C19 C 0.3836(5) 0.4920(10) 0.3129(5) 0.051(3) Uani 1 1 d . . . C20 C 0.3456(5) 0.4237(11) 0.2809(6) 0.063(4) Uani 1 1 d . . . H20 H 0.3175 0.3766 0.2966 0.075 Uiso 1 1 calc R . . C21 C 0.3576(6) 0.4391(11) 0.2230(6) 0.067(4) Uani 1 1 d . . . C22 C 0.3308(6) 0.3933(13) 0.1672(6) 0.097(6) Uani 1 1 d . . . H22A H 0.3504 0.4238 0.1332 0.145 Uiso 1 1 calc R . . H22B H 0.2905 0.4132 0.1658 0.145 Uiso 1 1 calc R . . H22C H 0.3345 0.3137 0.1669 0.145 Uiso 1 1 calc R . . C23 C 0.4913(6) 0.6455(11) 0.4758(5) 0.056(3) Uani 1 1 d . . . C24 C 0.5025(6) 0.6975(10) 0.5304(5) 0.057(3) Uani 1 1 d . . . H24 H 0.4769 0.7066 0.5620 0.068 Uiso 1 1 calc R . . C25 C 0.5599(6) 0.7327(11) 0.5275(6) 0.065(4) Uani 1 1 d . . . C26 C 0.5972(7) 0.7871(12) 0.5720(6) 0.091(5) Uani 1 1 d . . . H26A H 0.6351 0.7993 0.5554 0.137 Uiso 1 1 calc R . . H26B H 0.6004 0.7403 0.6065 0.137 Uiso 1 1 calc R . . H26C H 0.5805 0.8573 0.5832 0.137 Uiso 1 1 calc R . . C27 C 0.5000 0.2010(15) 0.2500 0.120(7) Uani 1 2 d SDU . . C28 C 0.4773(8) 0.2595(14) 0.1985(5) 0.170(7) Uani 1 1 d DU . . H28A H 0.4649 0.2065 0.1692 0.255 Uiso 1 1 calc R . . H28B H 0.5071 0.3061 0.1820 0.255 Uiso 1 1 calc R . . H28C H 0.4449 0.3047 0.2103 0.255 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 N8 0.053(6) 0.034(6) 0.060(7) -0.007(5) -0.006(5) -0.008(5) N7 0.050(6) 0.044(6) 0.045(6) -0.001(5) -0.007(5) -0.015(5) Ag1 0.0418(5) 0.0402(5) 0.0382(5) -0.0023(4) -0.0013(4) -0.0053(4) Ag2 0.0432(5) 0.0589(6) 0.0458(5) 0.0086(4) 0.0050(4) 0.0042(4) Ag3 0.0667(7) 0.0692(7) 0.0484(6) 0.0066(5) -0.0017(5) 0.0158(5) N1 0.035(5) 0.047(6) 0.040(5) 0.001(4) 0.004(4) 0.001(4) N2 0.043(6) 0.054(6) 0.046(6) -0.004(5) 0.002(5) 0.005(5) N3 0.051(7) 0.066(7) 0.057(6) 0.000(6) -0.008(6) -0.016(6) N4 0.036(5) 0.043(6) 0.043(6) -0.004(4) 0.005(5) -0.013(4) N5 0.041(6) 0.058(6) 0.039(5) -0.012(5) -0.006(4) -0.016(5) N6 0.050(6) 0.040(6) 0.054(6) 0.012(5) -0.003(5) -0.001(5) N9 0.054(7) 0.067(7) 0.060(7) 0.004(6) -0.014(6) -0.007(6) N10 0.055(7) 0.073(8) 0.062(7) 0.009(6) -0.011(6) 0.005(6) N11 0.051(8) 0.101(10) 0.046(7) 0.014(7) -0.002(6) 0.016(7) O1 0.077(8) 0.190(14) 0.087(8) 0.031(8) -0.033(7) -0.002(8) O2 0.081(8) 0.188(13) 0.109(9) 0.058(9) 0.017(7) 0.039(9) O3 0.124(10) 0.170(12) 0.036(6) 0.003(7) -0.003(6) -0.004(8) O4 0.174(14) 0.108(12) 0.258(17) 0.000 0.055(14) 0.000 C1 0.031(7) 0.051(8) 0.052(7) -0.008(6) 0.011(6) 0.000(6) C2 0.058(9) 0.055(8) 0.046(7) -0.019(6) 0.006(6) -0.008(6) C3 0.061(9) 0.100(12) 0.046(8) -0.020(8) 0.021(7) -0.017(8) C4 0.048(7) 0.063(9) 0.046(7) -0.006(6) 0.008(6) -0.008(6) C5 0.041(7) 0.047(7) 0.022(5) 0.000(5) 0.003(5) 0.006(5) C6 0.023(6) 0.051(7) 0.056(8) 0.007(6) 0.005(6) 0.001(5) C7 0.060(8) 0.049(8) 0.052(8) 0.003(6) -0.011(7) -0.007(6) C8 0.043(8) 0.062(9) 0.068(9) 0.013(7) -0.005(7) -0.016(6) C9 0.094(12) 0.129(15) 0.086(11) -0.008(10) -0.016(9) -0.081(11) C10 0.043(7) 0.040(7) 0.039(6) 0.003(5) 0.000(6) -0.002(5) C11 0.057(8) 0.061(8) 0.038(7) -0.019(6) 0.003(6) -0.003(6) C12 0.039(7) 0.070(9) 0.040(7) -0.009(6) 0.008(6) -0.016(6) C13 0.058(9) 0.100(12) 0.069(9) -0.045(8) 0.009(7) -0.036(8) C14 0.041(7) 0.056(8) 0.043(7) 0.011(6) 0.000(6) 0.003(6) C15 0.066(10) 0.081(10) 0.052(8) 0.019(7) 0.008(8) 0.005(8) C16 0.059(10) 0.103(13) 0.059(9) -0.002(9) 0.011(8) 0.002(8) C17 0.063(9) 0.068(10) 0.080(11) 0.015(8) 0.001(8) -0.010(8) C18 0.054(8) 0.033(7) 0.060(8) 0.015(6) -0.007(7) -0.004(6) C19 0.060(8) 0.041(7) 0.052(8) 0.012(6) -0.002(7) -0.013(6) C20 0.056(9) 0.062(9) 0.070(9) 0.015(8) 0.001(7) -0.021(7) C21 0.072(9) 0.064(10) 0.064(9) -0.014(7) 0.012(8) -0.028(8) C22 0.102(12) 0.111(14) 0.077(10) -0.030(10) -0.014(9) -0.058(10) C23 0.050(8) 0.070(9) 0.047(8) 0.020(7) -0.001(7) 0.021(7) C24 0.068(9) 0.064(9) 0.039(7) 0.002(6) -0.009(7) -0.004(7) C25 0.079(11) 0.063(9) 0.053(9) -0.003(7) -0.008(8) 0.012(8) C26 0.106(13) 0.068(11) 0.099(12) -0.013(9) -0.039(10) 0.004(9) C27 0.131(15) 0.026(10) 0.202(19) 0.000 0.062(15) 0.000 C28 0.160(14) 0.077(11) 0.274(19) 0.033(11) 0.078(14) 0.034(10) _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 N8 C21 1.364(14) . ? N8 N7 1.365(11) . ? N8 Ag3 2.092(9) 3_655 ? N7 C19 1.311(13) . ? N7 Ag1 2.126(9) . ? Ag1 N4 2.105(8) . ? Ag1 Ag1 2.8736(16) 3_655 ? Ag1 Ag3 2.9046(13) . ? Ag1 Ag2 2.9082(12) . ? Ag2 N5 2.081(9) 3_655 ? Ag2 N2 2.114(9) . ? Ag3 N8 2.092(9) 3_655 ? Ag3 N9 2.110(11) . ? N1 C5 1.325(12) . ? N1 C1 1.332(13) . ? N2 N3 1.351(12) . ? N2 C6 1.369(13) . ? N3 C8 1.336(13) . ? N3 H3 0.8600 . ? N4 N5 1.365(11) . ? N4 C10 1.372(12) . ? N5 C12 1.356(13) . ? N5 Ag2 2.081(9) 3_655 ? N6 C14 1.331(14) . ? N6 C18 1.355(13) . ? N9 C23 1.342(14) . ? N9 N10 1.342(13) . ? N10 C25 1.350(15) . ? N10 H10 0.8600 . ? N11 O1 1.194(12) . ? N11 O3 1.213(12) . ? N11 O2 1.221(13) . ? O4 C27 1.305(15) . ? C1 C2 1.396(14) . ? C1 C10 1.465(14) . ? C2 C3 1.366(15) . ? C2 H2 0.9300 . ? C3 C4 1.374(15) . ? C3 H3A 0.9300 . ? C4 C5 1.383(13) . ? C4 H4 0.9300 . ? C5 C6 1.465(14) . ? C6 C7 1.406(15) . ? C7 C8 1.347(15) . ? C7 H7 0.9300 . ? C8 C9 1.528(15) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.364(14) . ? C11 C12 1.372(14) . ? C11 H11 0.9300 . ? C12 C13 1.478(14) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.399(15) . ? C14 C23 1.455(16) . ? C15 C16 1.384(17) . ? C15 H15 0.9300 . ? C16 C17 1.359(17) . ? C16 H16 0.9300 . ? C17 C18 1.403(16) . ? C17 H17 0.9300 . ? C18 C19 1.458(16) . ? C19 C20 1.399(16) . ? C20 C21 1.344(15) . ? C20 H20 0.9300 . ? C21 C22 1.504(16) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.403(16) . ? C24 C25 1.388(17) . ? C24 H24 0.9300 . ? C25 C26 1.474(17) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.452(10) 3_655 ? C27 C28 1.452(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 C21 N8 N7 107.8(9) . . ? C21 N8 Ag3 127.9(8) . 3_655 ? N7 N8 Ag3 124.1(7) . 3_655 ? C19 N7 N8 108.7(9) . . ? C19 N7 Ag1 120.0(8) . . ? N8 N7 Ag1 126.8(7) . . ? N4 Ag1 N7 172.7(3) . . ? N4 Ag1 Ag1 93.1(2) . 3_655 ? N7 Ag1 Ag1 94.0(3) . 3_655 ? N4 Ag1 Ag3 83.7(2) . . ? N7 Ag1 Ag3 95.8(3) . . ? Ag1 Ag1 Ag3 83.81(4) 3_655 . ? N4 Ag1 Ag2 99.6(2) . . ? N7 Ag1 Ag2 82.4(2) . . ? Ag1 Ag1 Ag2 83.49(4) 3_655 . ? Ag3 Ag1 Ag2 167.01(4) . . ? N5 Ag2 N2 169.6(3) 3_655 . ? N5 Ag2 Ag1 96.7(2) 3_655 . ? N2 Ag2 Ag1 93.5(2) . . ? N8 Ag3 N9 167.8(4) 3_655 . ? N8 Ag3 Ag1 97.4(2) 3_655 . ? N9 Ag3 Ag1 93.2(3) . . ? C5 N1 C1 117.9(9) . . ? N3 N2 C6 104.4(9) . . ? N3 N2 Ag2 122.4(7) . . ? C6 N2 Ag2 132.9(8) . . ? C8 N3 N2 112.9(10) . . ? C8 N3 H3 123.6 . . ? N2 N3 H3 123.6 . . ? N5 N4 C10 107.5(8) . . ? N5 N4 Ag1 127.3(7) . . ? C10 N4 Ag1 120.8(7) . . ? C12 N5 N4 107.7(8) . . ? C12 N5 Ag2 128.4(7) . 3_655 ? N4 N5 Ag2 123.9(7) . 3_655 ? C14 N6 C18 119.4(10) . . ? C23 N9 N10 105.9(10) . . ? C23 N9 Ag3 133.3(9) . . ? N10 N9 Ag3 120.8(8) . . ? N9 N10 C25 112.4(11) . . ? N9 N10 H10 123.8 . . ? C25 N10 H10 123.8 . . ? O1 N11 O3 119.3(13) . . ? O1 N11 O2 118.5(13) . . ? O3 N11 O2 122.1(13) . . ? N1 C1 C2 120.9(10) . . ? N1 C1 C10 119.7(10) . . ? C2 C1 C10 119.3(11) . . ? C3 C2 C1 120.4(11) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 118.6(11) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C3 C4 C5 117.7(11) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 124.4(10) . . ? N1 C5 C6 117.8(9) . . ? C4 C5 C6 117.8(10) . . ? N2 C6 C7 108.7(10) . . ? N2 C6 C5 121.3(9) . . ? C7 C6 C5 129.9(11) . . ? C8 C7 C6 107.0(11) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? N3 C8 C7 107.0(11) . . ? N3 C8 C9 121.2(12) . . ? C7 C8 C9 131.8(12) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N4 109.0(9) . . ? C11 C10 C1 132.3(10) . . ? N4 C10 C1 118.6(10) . . ? C10 C11 C12 106.4(10) . . ? C10 C11 H11 126.8 . . ? C12 C11 H11 126.8 . . ? N5 C12 C11 109.3(9) . . ? N5 C12 C13 119.9(10) . . ? C11 C12 C13 130.6(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 C15 121.4(11) . . ? N6 C14 C23 118.0(11) . . ? C15 C14 C23 120.5(12) . . ? C16 C15 C14 119.5(13) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 118.9(13) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 119.7(13) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? N6 C18 C17 121.0(11) . . ? N6 C18 C19 117.7(11) . . ? C17 C18 C19 121.1(12) . . ? N7 C19 C20 108.5(10) . . ? N7 C19 C18 121.1(11) . . ? C20 C19 C18 130.3(11) . . ? C21 C20 C19 106.8(11) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? C20 C21 N8 108.1(11) . . ? C20 C21 C22 132.4(12) . . ? N8 C21 C22 119.4(12) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C24 109.9(12) . . ? N9 C23 C14 120.5(12) . . ? C24 C23 C14 129.5(12) . . ? C25 C24 C23 105.7(12) . . ? C25 C24 H24 127.2 . . ? C23 C24 H24 127.2 . . ? N10 C25 C24 106.1(12) . . ? N10 C25 C26 122.5(14) . . ? C24 C25 C26 131.2(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 C27 C28 119.0(8) . 3_655 ? O4 C27 C28 119.0(8) . . ? C28 C27 C28 122.1(15) 3_655 . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.449 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.157 #===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 655900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H47 Ag6 B2 F8 N20' _chemical_formula_weight 1772.94 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' Ag Ag -0.8971 1.1015 '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' F F 0.0171 0.0103 '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 17.219(5) _cell_length_b 23.494(7) _cell_length_c 17.751(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.124(4) _cell_angle_gamma 90.00 _cell_volume 6785(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4237 _cell_measurement_theta_min 2.429 _cell_measurement_theta_max 24.141 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3452 _exptl_absorpt_coefficient_mu 1.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5032 _exptl_absorpt_correction_T_max 0.7650 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17448 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5968 _reflns_number_gt 3243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5968 _refine_ls_number_parameters 398 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.102 _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 0.50707(3) 0.76087(2) 0.33347(3) 0.0538(2) Uani 1 1 d . . . Ag2 Ag 0.58233(4) 0.65060(3) 0.33565(4) 0.0712(2) Uani 1 1 d . . . Ag3 Ag 0.42824(4) 0.87190(3) 0.29420(4) 0.0732(2) Uani 1 1 d . . . N1 N 0.6078(4) 0.7296(3) 0.4747(4) 0.0573(17) Uani 1 1 d . . . N2 N 0.6151(3) 0.8113(2) 0.3651(4) 0.0529(15) Uani 1 1 d . . . N3 N 0.6358(4) 0.8544(3) 0.3251(4) 0.0632(18) Uani 1 1 d . . . N4 N 0.5343(4) 0.6233(3) 0.4247(4) 0.071(2) Uani 1 1 d . . . N5 N 0.4784(5) 0.5800(3) 0.4139(5) 0.079(2) Uani 1 1 d . . . H5 H 0.4619 0.5590 0.3719 0.095 Uiso 0.75 1 calc PR . . N6 N 0.4200(4) 0.7964(3) 0.4235(4) 0.0616(17) Uani 1 1 d . . . N7 N 0.3977(4) 0.7114(3) 0.3087(4) 0.0566(16) Uani 1 1 d . . . N8 N 0.3696(4) 0.6680(3) 0.2553(4) 0.0656(19) Uani 1 1 d . . . N9 N 0.4898(4) 0.9020(3) 0.4111(5) 0.0690(19) Uani 1 1 d . . . N10 N 0.5437(5) 0.9462(3) 0.4270(5) 0.077(2) Uani 1 1 d . . . H10 H 0.5532 0.9672 0.3913 0.093 Uiso 0.75 1 calc PR . . C1 C 0.7319(6) 0.9357(4) 0.3482(6) 0.112(4) Uani 1 1 d . . . H1A H 0.7797 0.9255 0.3346 0.169 Uiso 1 1 calc R . . H1B H 0.7464 0.9637 0.3898 0.169 Uiso 1 1 calc R . . H1C H 0.6907 0.9510 0.3020 0.169 Uiso 1 1 calc R . . C2 C 0.6991(5) 0.8845(3) 0.3760(6) 0.076(3) Uani 1 1 d . . . C3 C 0.7173(5) 0.8612(3) 0.4508(6) 0.071(2) Uani 1 1 d . . . H3 H 0.7564 0.8739 0.4975 0.085 Uiso 1 1 calc R . . C4 C 0.6646(4) 0.8143(3) 0.4422(5) 0.056(2) Uani 1 1 d . . . C5 C 0.6569(4) 0.7739(3) 0.5013(4) 0.053(2) Uani 1 1 d . . . C6 C 0.6944(5) 0.7845(4) 0.5813(5) 0.077(3) Uani 1 1 d . . . H6 H 0.7269 0.8167 0.5977 0.092 Uiso 1 1 calc R . . C7 C 0.6840(6) 0.7480(5) 0.6357(6) 0.094(3) Uani 1 1 d . . . H7 H 0.7111 0.7539 0.6897 0.113 Uiso 1 1 calc R . . C8 C 0.6320(6) 0.7011(4) 0.6100(5) 0.079(3) Uani 1 1 d . . . H8 H 0.6217 0.6759 0.6461 0.094 Uiso 1 1 calc R . . C9 C 0.5968(5) 0.6938(4) 0.5290(5) 0.060(2) Uani 1 1 d . . . C10 C 0.5424(5) 0.6446(4) 0.4970(5) 0.065(2) Uani 1 1 d . . . C11 C 0.4923(6) 0.6147(4) 0.5304(5) 0.082(3) Uani 1 1 d . . . H11 H 0.4868 0.6208 0.5802 0.098 Uiso 1 1 calc R . . C12 C 0.4529(6) 0.5748(4) 0.4760(6) 0.082(3) Uani 1 1 d . . . C13 C 0.3877(7) 0.5322(4) 0.4757(6) 0.119(4) Uani 1 1 d . . . H13A H 0.4002 0.5157 0.5278 0.179 Uiso 1 1 calc R . . H13B H 0.3860 0.5028 0.4376 0.179 Uiso 1 1 calc R . . H13C H 0.3353 0.5509 0.4613 0.179 Uiso 1 1 calc R . . C14 C 0.2644(6) 0.5907(4) 0.2286(5) 0.100(3) Uani 1 1 d . . . H14A H 0.2754 0.5869 0.1792 0.151 Uiso 1 1 calc R . . H14B H 0.2064 0.5951 0.2179 0.151 Uiso 1 1 calc R . . H14C H 0.2832 0.5572 0.2605 0.151 Uiso 1 1 calc R . . C15 C 0.3083(5) 0.6415(3) 0.2724(5) 0.067(2) Uani 1 1 d . . . C16 C 0.2992(5) 0.6665(4) 0.3385(6) 0.076(3) Uani 1 1 d . . . H16 H 0.2622 0.6561 0.3643 0.092 Uiso 1 1 calc R . . C17 C 0.3563(5) 0.7108(3) 0.3597(5) 0.061(2) Uani 1 1 d . . . C18 C 0.3743(5) 0.7515(4) 0.4269(5) 0.059(2) Uani 1 1 d . . . C19 C 0.3513(6) 0.7393(4) 0.4923(7) 0.088(3) Uani 1 1 d . . . H19 H 0.3217 0.7064 0.4938 0.105 Uiso 1 1 calc R . . C20 C 0.3725(7) 0.7760(6) 0.5548(7) 0.111(4) Uani 1 1 d . . . H20 H 0.3557 0.7694 0.5988 0.133 Uiso 1 1 calc R . . C21 C 0.4201(6) 0.8239(5) 0.5522(6) 0.090(3) Uani 1 1 d . . . H21 H 0.4353 0.8497 0.5942 0.108 Uiso 1 1 calc R . . C22 C 0.4434(5) 0.8319(4) 0.4867(6) 0.072(3) Uani 1 1 d . . . C23 C 0.4936(6) 0.8812(4) 0.4811(6) 0.068(2) Uani 1 1 d . . . C24 C 0.5489(6) 0.9118(4) 0.5416(6) 0.077(3) Uani 1 1 d . . . H24 H 0.5621 0.9055 0.5961 0.092 Uiso 1 1 calc R . . C25 C 0.5803(6) 0.9527(4) 0.5064(6) 0.075(3) Uani 1 1 d . . . C26 C 0.6422(6) 0.9973(4) 0.5378(6) 0.106(3) Uani 1 1 d . . . H26A H 0.6961 0.9809 0.5522 0.160 Uiso 1 1 calc R . . H26B H 0.6344 1.0142 0.5840 0.160 Uiso 1 1 calc R . . H26C H 0.6365 1.0259 0.4977 0.160 Uiso 1 1 calc R . . F3 F 0.0569(13) 0.9728(8) 0.3106(8) 0.544(19) Uani 1 1 d D . . F4 F 0.0434(12) 1.0160(7) 0.2239(10) 0.367(11) Uani 1 1 d D . . B2 B 0.0000 0.9824(10) 0.2500 0.39(6) Uani 1 2 d SD . . F1 F 0.5480(10) 0.0259(6) 0.3059(10) 0.339(9) Uani 1 1 d D . . B1 B 0.5000 0.0666(12) 0.2500 0.22(2) Uani 1 2 d SD . . F2 F 0.4468(10) 0.0528(8) 0.2792(9) 0.481(16) Uani 1 1 d 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 0.0410(3) 0.0507(4) 0.0575(4) -0.0042(3) -0.0007(3) -0.0047(3) Ag2 0.0764(5) 0.0645(4) 0.0549(4) -0.0024(3) -0.0028(3) 0.0162(3) Ag3 0.0670(5) 0.0644(4) 0.0775(5) -0.0009(4) 0.0088(4) 0.0144(3) N1 0.046(4) 0.068(5) 0.046(4) -0.012(4) -0.002(3) 0.008(3) N2 0.040(4) 0.047(4) 0.066(4) -0.012(3) 0.010(3) -0.005(3) N3 0.050(4) 0.059(4) 0.069(5) -0.001(4) 0.004(4) -0.002(3) N4 0.068(5) 0.060(4) 0.055(5) -0.003(4) -0.019(4) 0.008(4) N5 0.091(6) 0.054(5) 0.067(5) -0.008(4) -0.011(5) -0.002(4) N6 0.049(4) 0.069(5) 0.064(5) 0.007(4) 0.014(4) 0.012(4) N7 0.039(4) 0.060(4) 0.054(4) 0.005(3) -0.008(3) -0.012(3) N8 0.046(4) 0.070(5) 0.056(4) 0.009(4) -0.016(3) -0.014(3) N9 0.064(5) 0.054(4) 0.084(5) -0.009(4) 0.018(4) 0.004(4) N10 0.079(6) 0.053(5) 0.097(6) -0.001(4) 0.025(5) 0.003(4) C1 0.083(8) 0.091(8) 0.138(9) -0.003(7) 0.001(7) -0.037(6) C2 0.056(6) 0.054(6) 0.097(7) -0.015(5) -0.002(5) -0.018(4) C3 0.041(5) 0.071(6) 0.089(7) -0.031(5) 0.006(5) -0.007(4) C4 0.037(4) 0.054(5) 0.064(5) -0.020(4) 0.000(4) 0.007(4) C5 0.042(5) 0.077(6) 0.025(4) -0.017(4) -0.008(3) 0.006(4) C6 0.070(6) 0.081(6) 0.067(6) -0.006(5) 0.005(5) -0.008(5) C7 0.081(7) 0.109(9) 0.064(7) -0.049(6) -0.013(5) 0.002(6) C8 0.090(7) 0.080(7) 0.060(6) -0.009(5) 0.017(5) 0.009(5) C9 0.050(5) 0.071(6) 0.042(5) -0.014(5) -0.006(4) 0.016(4) C10 0.066(6) 0.063(6) 0.050(5) 0.002(5) -0.003(5) 0.014(5) C11 0.086(7) 0.088(7) 0.057(6) -0.002(5) 0.003(5) 0.000(6) C12 0.074(7) 0.083(7) 0.077(7) -0.008(6) 0.007(6) 0.009(6) C13 0.129(10) 0.091(8) 0.116(9) 0.016(7) 0.011(8) -0.025(7) C14 0.091(7) 0.085(7) 0.102(7) 0.007(6) -0.001(6) -0.038(6) C15 0.051(5) 0.058(5) 0.070(6) 0.005(5) -0.008(5) -0.017(4) C16 0.054(6) 0.077(6) 0.087(7) 0.022(6) 0.010(5) -0.013(5) C17 0.048(5) 0.063(5) 0.066(6) 0.014(5) 0.012(4) 0.002(4) C18 0.054(5) 0.069(6) 0.060(6) 0.005(5) 0.026(4) 0.008(4) C19 0.075(7) 0.105(8) 0.089(7) 0.009(7) 0.035(6) -0.008(6) C20 0.099(9) 0.147(12) 0.098(9) -0.001(8) 0.047(8) 0.008(8) C21 0.092(8) 0.102(8) 0.076(7) -0.011(6) 0.027(6) 0.012(6) C22 0.066(6) 0.088(7) 0.058(6) -0.009(5) 0.015(5) 0.024(5) C23 0.065(6) 0.063(6) 0.072(7) -0.009(5) 0.014(5) 0.012(5) C24 0.069(6) 0.082(7) 0.076(6) -0.007(6) 0.020(6) 0.016(5) C25 0.065(6) 0.061(6) 0.087(7) -0.021(6) 0.009(6) 0.013(5) C26 0.102(8) 0.060(6) 0.135(9) -0.020(6) 0.009(7) 0.003(6) F3 0.79(5) 0.61(3) 0.327(18) 0.309(19) 0.31(3) 0.48(3) F4 0.37(2) 0.37(2) 0.30(2) 0.20(2) 0.030(16) -0.053(19) B2 0.38(8) 0.053(16) 0.43(10) 0.000 -0.27(7) 0.000 F1 0.33(2) 0.349(17) 0.38(2) 0.233(15) 0.172(15) 0.125(13) B1 0.18(3) 0.45(7) 0.063(18) 0.000 0.086(19) 0.000 F2 0.37(3) 0.89(4) 0.159(12) -0.052(16) 0.061(13) 0.31(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.120(6) . ? Ag1 N7 2.133(6) . ? Ag1 Ag2 2.8913(11) . ? Ag1 Ag1 2.8928(15) 2_655 ? Ag1 Ag3 2.9176(11) . ? Ag2 N8 2.082(7) 2_655 ? Ag2 N4 2.110(7) . ? Ag3 N3 2.084(6) 2_655 ? Ag3 N9 2.119(7) . ? Ag3 Ag3 3.3332(16) 2_655 ? N1 C5 1.326(9) . ? N1 C9 1.339(9) . ? N2 N3 1.349(8) . ? N2 C4 1.357(9) . ? N3 C2 1.364(9) . ? N3 Ag3 2.084(6) 2_655 ? N4 C10 1.342(9) . ? N4 N5 1.369(9) . ? N5 C12 1.320(11) . ? N5 H5 0.8600 . ? N6 C18 1.329(9) . ? N6 C22 1.348(10) . ? N7 C17 1.323(9) . ? N7 N8 1.369(8) . ? N8 C15 1.344(10) . ? N8 Ag2 2.082(7) 2_655 ? N9 C23 1.316(10) . ? N9 N10 1.360(9) . ? N10 C25 1.351(10) . ? N10 H10 0.8600 . ? C1 C2 1.479(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(11) . ? C3 C4 1.402(10) . ? C3 H3 0.9300 . ? C4 C5 1.452(10) . ? C5 C6 1.376(10) . ? C6 C7 1.347(12) . ? C6 H6 0.9300 . ? C7 C8 1.398(12) . ? C7 H7 0.9300 . ? C8 C9 1.376(10) . ? C8 H8 0.9300 . ? C9 C10 1.478(11) . ? C10 C11 1.387(11) . ? C11 C12 1.359(12) . ? C11 H11 0.9300 . ? C12 C13 1.502(13) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.488(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.367(11) . ? C16 C17 1.396(11) . ? C16 H16 0.9300 . ? C17 C18 1.480(11) . ? C18 C19 1.375(11) . ? C19 C20 1.358(13) . ? C19 H19 0.9300 . ? C20 C21 1.402(14) . ? C20 H20 0.9300 . ? C21 C22 1.362(12) . ? C21 H21 0.9300 . ? C22 C23 1.468(12) . ? C23 C24 1.382(11) . ? C24 C25 1.352(12) . ? C24 H24 0.9300 . ? C25 C26 1.467(12) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? F3 B2 1.215(14) . ? F4 B2 1.274(14) . ? B2 F3 1.215(14) 2 ? B2 F4 1.274(14) 2 ? F1 B1 1.429(17) . ? F1 F2 1.668(15) 2_655 ? B1 F2 1.235(16) 2_655 ? B1 F2 1.235(16) . ? B1 F1 1.429(17) 2_655 ? F2 F1 1.668(15) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N7 176.4(3) . . ? N2 Ag1 Ag2 98.44(16) . . ? N7 Ag1 Ag2 82.91(17) . . ? N2 Ag1 Ag1 92.48(17) . 2_655 ? N7 Ag1 Ag1 90.96(18) . 2_655 ? Ag2 Ag1 Ag1 84.296(19) . 2_655 ? N2 Ag1 Ag3 82.10(16) . . ? N7 Ag1 Ag3 97.31(17) . . ? Ag2 Ag1 Ag3 167.34(3) . . ? Ag1 Ag1 Ag3 83.04(2) 2_655 . ? N8 Ag2 N4 173.6(3) 2_655 . ? N8 Ag2 Ag1 95.96(18) 2_655 . ? N4 Ag2 Ag1 89.94(18) . . ? N3 Ag3 N9 171.9(3) 2_655 . ? N3 Ag3 Ag1 96.66(18) 2_655 . ? N9 Ag3 Ag1 91.13(18) . . ? N3 Ag3 Ag3 75.45(18) 2_655 2_655 ? N9 Ag3 Ag3 104.6(2) . 2_655 ? Ag1 Ag3 Ag3 75.75(2) . 2_655 ? C5 N1 C9 117.5(6) . . ? N3 N2 C4 107.7(6) . . ? N3 N2 Ag1 129.8(5) . . ? C4 N2 Ag1 120.2(5) . . ? N2 N3 C2 109.5(7) . . ? N2 N3 Ag3 122.7(5) . 2_655 ? C2 N3 Ag3 127.7(6) . 2_655 ? C10 N4 N5 105.1(7) . . ? C10 N4 Ag2 131.2(6) . . ? N5 N4 Ag2 123.4(6) . . ? C12 N5 N4 111.3(7) . . ? C12 N5 H5 124.4 . . ? N4 N5 H5 124.4 . . ? C18 N6 C22 118.3(7) . . ? C17 N7 N8 108.5(6) . . ? C17 N7 Ag1 120.2(5) . . ? N8 N7 Ag1 129.5(5) . . ? C15 N8 N7 108.3(7) . . ? C15 N8 Ag2 128.7(6) . 2_655 ? N7 N8 Ag2 123.0(5) . 2_655 ? C23 N9 N10 105.5(7) . . ? C23 N9 Ag3 131.0(6) . . ? N10 N9 Ag3 123.1(6) . . ? C25 N10 N9 110.9(8) . . ? C25 N10 H10 124.6 . . ? N9 N10 H10 124.6 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C2 C3 108.2(7) . . ? N3 C2 C1 120.7(9) . . ? C3 C2 C1 130.9(8) . . ? C2 C3 C4 105.9(7) . . ? C2 C3 H3 127.1 . . ? C4 C3 H3 127.1 . . ? N2 C4 C3 108.7(8) . . ? N2 C4 C5 121.2(7) . . ? C3 C4 C5 130.0(8) . . ? N1 C5 C6 122.5(8) . . ? N1 C5 C4 117.0(6) . . ? C6 C5 C4 120.2(8) . . ? C7 C6 C5 119.8(9) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 119.3(9) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 117.0(9) . . ? C9 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? N1 C9 C8 123.8(8) . . ? N1 C9 C10 115.9(7) . . ? C8 C9 C10 120.3(9) . . ? N4 C10 C11 109.6(8) . . ? N4 C10 C9 120.9(9) . . ? C11 C10 C9 129.5(9) . . ? C12 C11 C10 106.4(9) . . ? C12 C11 H11 126.8 . . ? C10 C11 H11 126.8 . . ? N5 C12 C11 107.7(10) . . ? N5 C12 C13 120.8(10) . . ? C11 C12 C13 131.5(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N8 C15 C16 108.3(7) . . ? N8 C15 C14 123.8(9) . . ? C16 C15 C14 127.7(9) . . ? C15 C16 C17 106.4(8) . . ? C15 C16 H16 126.8 . . ? C17 C16 H16 126.8 . . ? N7 C17 C16 108.4(8) . . ? N7 C17 C18 121.7(7) . . ? C16 C17 C18 129.9(9) . . ? N6 C18 C19 122.8(8) . . ? N6 C18 C17 116.6(7) . . ? C19 C18 C17 120.2(9) . . ? C20 C19 C18 118.9(10) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 119.1(10) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 118.6(10) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? N6 C22 C21 122.2(10) . . ? N6 C22 C23 117.1(8) . . ? C21 C22 C23 120.7(9) . . ? N9 C23 C24 110.5(9) . . ? N9 C23 C22 120.5(8) . . ? C24 C23 C22 129.0(10) . . ? C25 C24 C23 106.8(9) . . ? C25 C24 H24 126.6 . . ? C23 C24 H24 126.6 . . ? N10 C25 C24 106.3(9) . . ? N10 C25 C26 120.7(10) . . ? C24 C25 C26 133.0(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F3 B2 F3 159(3) . 2 ? F3 B2 F4 101.0(13) . 2 ? F3 B2 F4 92.2(14) 2 2 ? F3 B2 F4 92.2(14) . . ? F3 B2 F4 101.0(13) 2 . ? F4 B2 F4 104(3) 2 . ? B1 F1 F2 46.2(7) . 2_655 ? F2 B1 F2 150(3) 2_655 . ? F2 B1 F1 82.7(14) 2_655 2_655 ? F2 B1 F1 77.2(13) . 2_655 ? F2 B1 F1 77.2(13) 2_655 . ? F2 B1 F1 82.7(14) . . ? F1 B1 F1 96(2) 2_655 . ? B1 F2 F1 56.6(9) . 2_655 ? 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 N2 Ag1 Ag2 N8 -62.3(2) . . . 2_655 ? N7 Ag1 Ag2 N8 121.0(2) . . . 2_655 ? Ag1 Ag1 Ag2 N8 29.36(16) 2_655 . . 2_655 ? Ag3 Ag1 Ag2 N8 29.2(2) . . . 2_655 ? N2 Ag1 Ag2 N4 120.2(3) . . . . ? N7 Ag1 Ag2 N4 -56.5(3) . . . . ? Ag1 Ag1 Ag2 N4 -148.17(18) 2_655 . . . ? Ag3 Ag1 Ag2 N4 -148.3(2) . . . . ? N2 Ag1 Ag3 N3 122.0(2) . . . 2_655 ? N7 Ag1 Ag3 N3 -61.5(3) . . . 2_655 ? Ag2 Ag1 Ag3 N3 28.7(2) . . . 2_655 ? Ag1 Ag1 Ag3 N3 28.55(18) 2_655 . . 2_655 ? N2 Ag1 Ag3 N9 -55.8(3) . . . . ? N7 Ag1 Ag3 N9 120.6(3) . . . . ? Ag2 Ag1 Ag3 N9 -149.2(2) . . . . ? Ag1 Ag1 Ag3 N9 -149.3(2) 2_655 . . . ? N2 Ag1 Ag3 Ag3 48.94(17) . . . 2_655 ? N7 Ag1 Ag3 Ag3 -134.63(19) . . . 2_655 ? Ag2 Ag1 Ag3 Ag3 -44.43(13) . . . 2_655 ? Ag1 Ag1 Ag3 Ag3 -44.55(3) 2_655 . . 2_655 ? N7 Ag1 N2 N3 -127(4) . . . . ? Ag2 Ag1 N2 N3 120.9(6) . . . . ? Ag1 Ag1 N2 N3 36.3(6) 2_655 . . . ? Ag3 Ag1 N2 N3 -46.3(6) . . . . ? N7 Ag1 N2 C4 33(4) . . . . ? Ag2 Ag1 N2 C4 -78.5(5) . . . . ? Ag1 Ag1 N2 C4 -163.0(5) 2_655 . . . ? Ag3 Ag1 N2 C4 114.3(5) . . . . ? C4 N2 N3 C2 0.8(8) . . . . ? C4 N2 N3 Ag3 -175.4(5) . . . 2_655 ? N8 Ag2 N4 C10 146.2(19) 2_655 . . . ? Ag1 Ag2 N4 C10 -56.4(7) . . . . ? N8 Ag2 N4 N5 -41(2) 2_655 . . . ? Ag1 Ag2 N4 N5 116.4(6) . . . . ? C10 N4 N5 C12 0.0(9) . . . . ? Ag2 N4 N5 C12 -174.4(6) . . . . ? N2 Ag1 N7 C17 4(4) . . . . ? Ag2 Ag1 N7 C17 116.4(6) . . . . ? Ag1 Ag1 N7 C17 -159.4(5) 2_655 . . . ? Ag3 Ag1 N7 C17 -76.3(5) . . . . ? N2 Ag1 N7 N8 -159(3) . . . . ? Ag2 Ag1 N7 N8 -46.7(5) . . . . ? Ag1 Ag1 N7 N8 37.4(6) 2_655 . . . ? Ag3 Ag1 N7 N8 120.5(5) . . . . ? C17 N7 N8 C15 1.9(8) . . . . ? Ag1 N7 N8 C15 166.6(5) . . . . ? C17 N7 N8 Ag2 -178.7(5) . . . 2_655 ? Ag1 N7 N8 Ag2 -14.0(8) . . . 2_655 ? N3 Ag3 N9 C23 141.6(17) 2_655 . . . ? Ag1 Ag3 N9 C23 -53.9(7) . . . . ? Ag3 Ag3 N9 C23 -129.4(7) 2_655 . . . ? N3 Ag3 N9 N10 -47(2) 2_655 . . . ? Ag1 Ag3 N9 N10 117.8(6) . . . . ? Ag3 Ag3 N9 N10 42.2(6) 2_655 . . . ? C23 N9 N10 C25 -0.2(9) . . . . ? Ag3 N9 N10 C25 -173.6(5) . . . . ? N2 N3 C2 C3 -2.0(9) . . . . ? Ag3 N3 C2 C3 173.9(5) 2_655 . . . ? N2 N3 C2 C1 -177.6(8) . . . . ? Ag3 N3 C2 C1 -1.6(12) 2_655 . . . ? N3 C2 C3 C4 2.4(9) . . . . ? C1 C2 C3 C4 177.3(10) . . . . ? N3 N2 C4 C3 0.7(8) . . . . ? Ag1 N2 C4 C3 -163.8(5) . . . . ? N3 N2 C4 C5 179.3(6) . . . . ? Ag1 N2 C4 C5 14.8(9) . . . . ? C2 C3 C4 N2 -1.9(9) . . . . ? C2 C3 C4 C5 179.7(8) . . . . ? C9 N1 C5 C6 -1.5(11) . . . . ? C9 N1 C5 C4 -176.4(6) . . . . ? N2 C4 C5 N1 9.1(10) . . . . ? C3 C4 C5 N1 -172.7(7) . . . . ? N2 C4 C5 C6 -165.9(7) . . . . ? C3 C4 C5 C6 12.3(12) . . . . ? N1 C5 C6 C7 2.4(13) . . . . ? C4 C5 C6 C7 177.1(8) . . . . ? C5 C6 C7 C8 -2.9(14) . . . . ? C6 C7 C8 C9 2.7(14) . . . . ? C5 N1 C9 C8 1.4(11) . . . . ? C5 N1 C9 C10 -179.3(7) . . . . ? C7 C8 C9 N1 -2.0(12) . . . . ? C7 C8 C9 C10 178.8(8) . . . . ? N5 N4 C10 C11 0.3(9) . . . . ? Ag2 N4 C10 C11 174.1(6) . . . . ? N5 N4 C10 C9 -178.2(7) . . . . ? Ag2 N4 C10 C9 -4.5(11) . . . . ? N1 C9 C10 N4 27.9(10) . . . . ? C8 C9 C10 N4 -152.7(8) . . . . ? N1 C9 C10 C11 -150.3(8) . . . . ? C8 C9 C10 C11 29.0(13) . . . . ? N4 C10 C11 C12 -0.5(10) . . . . ? C9 C10 C11 C12 177.9(8) . . . . ? N4 N5 C12 C11 -0.3(10) . . . . ? N4 N5 C12 C13 176.5(8) . . . . ? C10 C11 C12 N5 0.5(10) . . . . ? C10 C11 C12 C13 -175.9(10) . . . . ? N7 N8 C15 C16 -2.3(9) . . . . ? Ag2 N8 C15 C16 178.4(5) 2_655 . . . ? N7 N8 C15 C14 -177.8(7) . . . . ? Ag2 N8 C15 C14 2.9(11) 2_655 . . . ? N8 C15 C16 C17 1.7(9) . . . . ? C14 C15 C16 C17 177.1(8) . . . . ? N8 N7 C17 C16 -0.8(8) . . . . ? Ag1 N7 C17 C16 -167.2(5) . . . . ? N8 N7 C17 C18 177.9(6) . . . . ? Ag1 N7 C17 C18 11.5(9) . . . . ? C15 C16 C17 N7 -0.6(9) . . . . ? C15 C16 C17 C18 -179.1(8) . . . . ? C22 N6 C18 C19 -1.1(12) . . . . ? C22 N6 C18 C17 -174.5(7) . . . . ? N7 C17 C18 N6 14.9(11) . . . . ? C16 C17 C18 N6 -166.7(8) . . . . ? N7 C17 C18 C19 -158.7(8) . . . . ? C16 C17 C18 C19 19.7(13) . . . . ? N6 C18 C19 C20 3.4(14) . . . . ? C17 C18 C19 C20 176.5(9) . . . . ? C18 C19 C20 C21 -2.7(16) . . . . ? C19 C20 C21 C22 0.0(16) . . . . ? C18 N6 C22 C21 -1.8(12) . . . . ? C18 N6 C22 C23 -179.8(7) . . . . ? C20 C21 C22 N6 2.4(14) . . . . ? C20 C21 C22 C23 -179.7(9) . . . . ? N10 N9 C23 C24 0.3(9) . . . . ? Ag3 N9 C23 C24 173.1(5) . . . . ? N10 N9 C23 C22 -179.2(7) . . . . ? Ag3 N9 C23 C22 -6.5(12) . . . . ? N6 C22 C23 N9 25.0(11) . . . . ? C21 C22 C23 N9 -153.0(8) . . . . ? N6 C22 C23 C24 -154.5(8) . . . . ? C21 C22 C23 C24 27.5(14) . . . . ? N9 C23 C24 C25 -0.4(10) . . . . ? C22 C23 C24 C25 179.1(8) . . . . ? N9 N10 C25 C24 -0.1(9) . . . . ? N9 N10 C25 C26 178.9(7) . . . . ? C23 C24 C25 N10 0.3(10) . . . . ? C23 C24 C25 C26 -178.5(9) . . . . ? F2 F1 B1 F2 157(2) 2_655 . . . ? F2 F1 B1 F1 81.1(13) 2_655 . . 2_655 ? F2 B1 F2 F1 -49.6(11) 2_655 . . 2_655 ? F1 B1 F2 F1 -98(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.055 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.123 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.829 0.250 272.8 40.8 2 0.000 0.171 0.750 273.2 38.6 3 0.186 0.575 0.400 9.1 -0.6 4 0.186 0.425 0.900 9.4 -0.6 5 0.501 0.329 0.251 271.9 40.8 6 0.501 0.671 0.751 272.4 38.6 7 0.317 0.073 0.105 8.9 -0.5 8 0.317 0.927 0.605 9.1 -0.6 9 0.683 0.073 0.395 8.3 -0.5 10 0.683 0.927 0.895 8.5 -0.6 11 0.817 0.573 0.105 8.9 -0.5 12 0.817 0.427 0.605 9.1 -0.6 _platon_squeeze_details ; ; #===END data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 655901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Ag6 N20, 2(Cl O4)' _chemical_formula_sum 'C52 H48 Ag6 Cl2 N20 O8' _chemical_formula_weight 1799.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.165(6) _cell_length_b 11.793(3) _cell_length_c 22.190(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6323(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3312 _cell_measurement_theta_min 2.493 _cell_measurement_theta_max 19.462 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5708 _exptl_absorpt_correction_T_max 0.7562 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31057 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.1615 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5507 _reflns_number_gt 2991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5507 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _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 0.46307(3) 0.22309(6) 0.19857(3) 0.0465(2) Uani 1 1 d . . . Ag2 Ag 0.38681(3) 0.32839(7) 0.28517(3) 0.0609(3) Uani 1 1 d . . . Ag3 Ag 0.55253(3) 0.10064(7) 0.13907(3) 0.0672(3) Uani 1 1 d . . . Cl1 Cl 0.71984(13) 0.2385(3) 0.06759(14) 0.0884(9) Uani 1 1 d . . . N1 N 0.3850(3) 0.3513(6) 0.1464(3) 0.0490(18) Uani 1 1 d . . . N2 N 0.4986(3) 0.3671(5) 0.1587(3) 0.0449(16) Uani 1 1 d . . . N3 N 0.5529(3) 0.3999(6) 0.1596(3) 0.0506(18) Uani 1 1 d . . . N4 N 0.3164(3) 0.2635(6) 0.2393(3) 0.0568(19) Uani 1 1 d . . . N5 N 0.2794(3) 0.1950(7) 0.2665(4) 0.076(2) Uani 1 1 d . . . H5 H 0.2811 0.1775 0.3041 0.091 Uiso 1 1 calc R . . N6 N 0.4377(3) 0.0869(6) 0.0987(3) 0.0497(18) Uani 1 1 d . . . N7 N 0.4214(3) 0.0740(6) 0.2266(3) 0.0473(17) Uani 1 1 d . . . N8 N 0.4087(3) 0.0399(6) 0.2834(3) 0.0536(18) Uani 1 1 d . . . N9 N 0.5375(3) 0.1571(6) 0.0492(3) 0.058(2) Uani 1 1 d . . . N10 N 0.5777(4) 0.1906(7) 0.0112(3) 0.071(2) Uani 1 1 d . . . H10 H 0.6118 0.1977 0.0216 0.085 Uiso 1 1 calc R . . O1 O 0.6760(4) 0.2213(12) 0.1059(5) 0.174(5) Uani 1 1 d . . . O2 O 0.7333(7) 0.3484(14) 0.0698(7) 0.237(7) Uani 1 1 d . . . O3 O 0.7040(4) 0.2067(15) 0.0111(5) 0.220(8) Uani 1 1 d . . . O4 O 0.7660(6) 0.1918(15) 0.0863(7) 0.238(8) Uani 1 1 d . . . C1 C 0.6132(4) 0.5380(11) 0.1083(4) 0.089(4) Uani 1 1 d . . . H1A H 0.6394 0.4813 0.0961 0.134 Uiso 1 1 calc R . . H1B H 0.6254 0.5728 0.1450 0.134 Uiso 1 1 calc R . . H1C H 0.6102 0.5947 0.0774 0.134 Uiso 1 1 calc R . . C2 C 0.5583(4) 0.4844(9) 0.1180(4) 0.059(3) Uani 1 1 d . . . C3 C 0.5101(4) 0.5006(9) 0.0898(4) 0.067(3) Uani 1 1 d . . . H3 H 0.5032 0.5507 0.0583 0.080 Uiso 1 1 calc R . . C4 C 0.4727(4) 0.4283(7) 0.1165(4) 0.052(2) Uani 1 1 d . . . C5 C 0.4122(4) 0.4097(7) 0.1064(3) 0.049(2) Uani 1 1 d . . . C6 C 0.3881(5) 0.4546(10) 0.0536(4) 0.081(3) Uani 1 1 d . . . H6 H 0.4088 0.4969 0.0264 0.097 Uiso 1 1 calc R . . C7 C 0.3331(5) 0.4335(12) 0.0440(4) 0.094(4) Uani 1 1 d . . . H7 H 0.3158 0.4611 0.0095 0.113 Uiso 1 1 calc R . . C8 C 0.3038(4) 0.3727(10) 0.0845(4) 0.078(3) Uani 1 1 d . . . H8 H 0.2665 0.3575 0.0783 0.094 Uiso 1 1 calc R . . C9 C 0.3314(4) 0.3325(7) 0.1370(4) 0.055(2) Uani 1 1 d . . . C10 C 0.2999(4) 0.2689(8) 0.1823(4) 0.055(2) Uani 1 1 d . . . C11 C 0.2521(4) 0.2028(9) 0.1733(6) 0.080(3) Uani 1 1 d . . . H11 H 0.2328 0.1923 0.1375 0.096 Uiso 1 1 calc R . . C12 C 0.2398(5) 0.1565(11) 0.2294(6) 0.097(4) Uani 1 1 d . . . C13 C 0.1967(5) 0.0774(14) 0.2499(7) 0.163(8) Uani 1 1 d . . . H13A H 0.2076 0.0011 0.2406 0.245 Uiso 1 1 calc R . . H13B H 0.1625 0.0945 0.2298 0.245 Uiso 1 1 calc R . . H13C H 0.1919 0.0850 0.2927 0.245 Uiso 1 1 calc R . . C14 C 0.3421(5) -0.0871(10) 0.3333(4) 0.104(4) Uani 1 1 d . . . H14A H 0.3028 -0.0935 0.3279 0.156 Uiso 1 1 calc R . . H14B H 0.3496 -0.0415 0.3681 0.156 Uiso 1 1 calc R . . H14C H 0.3577 -0.1612 0.3387 0.156 Uiso 1 1 calc R . . C15 C 0.3668(4) -0.0333(9) 0.2796(4) 0.069(3) Uani 1 1 d . . . C16 C 0.3524(4) -0.0462(8) 0.2205(4) 0.061(2) Uani 1 1 d . . . H16 H 0.3245 -0.0924 0.2053 0.073 Uiso 1 1 calc R . . C17 C 0.3872(3) 0.0225(8) 0.1877(4) 0.050(2) Uani 1 1 d . . . C18 C 0.3905(4) 0.0468(7) 0.1226(4) 0.050(2) Uani 1 1 d . . . C19 C 0.3429(4) 0.0326(8) 0.0879(4) 0.066(3) Uani 1 1 d . . . H19 H 0.3109 0.0027 0.1050 0.080 Uiso 1 1 calc R . . C20 C 0.3439(5) 0.0626(9) 0.0293(4) 0.074(3) Uani 1 1 d . . . H20 H 0.3123 0.0562 0.0056 0.089 Uiso 1 1 calc R . . C21 C 0.3932(4) 0.1033(8) 0.0048(4) 0.066(3) Uani 1 1 d . . . H21 H 0.3952 0.1245 -0.0355 0.079 Uiso 1 1 calc R . . C22 C 0.4384(4) 0.1114(8) 0.0412(4) 0.054(2) Uani 1 1 d . . . C23 C 0.4921(4) 0.1521(8) 0.0160(4) 0.061(3) Uani 1 1 d . . . C24 C 0.5032(5) 0.1883(8) -0.0412(4) 0.068(3) Uani 1 1 d . . . H24 H 0.4779 0.1960 -0.0725 0.082 Uiso 1 1 calc R . . C25 C 0.5595(5) 0.2114(8) -0.0439(4) 0.073(3) Uani 1 1 d . . . C26 C 0.5962(5) 0.2548(9) -0.0931(4) 0.092(4) Uani 1 1 d . . . H26A H 0.6306 0.2801 -0.0762 0.139 Uiso 1 1 calc R . . H26B H 0.5783 0.3169 -0.1132 0.139 Uiso 1 1 calc R . . H26C H 0.6031 0.1952 -0.1216 0.139 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 0.0488(4) 0.0432(4) 0.0474(4) 0.0020(3) -0.0007(3) -0.0071(3) Ag2 0.0539(5) 0.0683(6) 0.0604(5) -0.0070(3) -0.0040(3) 0.0076(4) Ag3 0.0830(6) 0.0712(6) 0.0473(4) -0.0019(3) -0.0005(3) 0.0160(4) Cl1 0.074(2) 0.109(3) 0.082(2) -0.0154(17) 0.0149(16) -0.0146(19) N1 0.047(5) 0.052(5) 0.049(4) -0.004(3) -0.005(3) -0.008(4) N2 0.057(5) 0.041(4) 0.037(3) 0.006(3) 0.003(3) -0.007(3) N3 0.043(4) 0.055(5) 0.053(4) 0.008(4) 0.000(3) -0.009(4) N4 0.054(5) 0.051(5) 0.065(5) -0.004(4) 0.010(4) -0.007(4) N5 0.061(6) 0.078(6) 0.089(6) -0.004(5) 0.030(5) -0.012(5) N6 0.048(5) 0.040(4) 0.061(5) -0.007(3) -0.004(4) 0.003(3) N7 0.057(5) 0.042(4) 0.042(4) -0.003(3) 0.001(3) -0.005(3) N8 0.057(5) 0.055(5) 0.049(4) 0.004(3) 0.007(3) -0.012(4) N9 0.062(5) 0.061(5) 0.052(4) 0.001(4) 0.006(4) -0.006(4) N10 0.078(6) 0.076(6) 0.058(5) 0.017(4) 0.011(4) 0.001(5) O1 0.115(8) 0.281(17) 0.127(8) 0.019(9) 0.057(7) -0.025(9) O2 0.250(18) 0.159(14) 0.302(18) 0.039(12) -0.018(14) -0.073(13) O3 0.124(10) 0.41(2) 0.128(9) -0.121(12) 0.032(7) -0.062(11) O4 0.157(12) 0.289(19) 0.268(17) -0.089(14) -0.065(12) 0.133(13) C1 0.087(8) 0.117(10) 0.064(6) 0.022(6) -0.002(6) -0.043(7) C2 0.049(6) 0.084(8) 0.043(5) 0.007(5) -0.006(4) -0.016(5) C3 0.087(8) 0.062(7) 0.052(5) 0.009(5) -0.007(5) -0.015(6) C4 0.053(6) 0.051(6) 0.051(5) 0.007(4) -0.013(4) 0.000(4) C5 0.048(5) 0.059(6) 0.038(4) 0.007(4) -0.016(4) 0.025(4) C6 0.074(8) 0.102(9) 0.067(6) 0.020(6) -0.013(5) 0.005(7) C7 0.070(8) 0.155(12) 0.057(7) 0.022(7) -0.027(6) 0.022(8) C8 0.060(7) 0.102(9) 0.072(7) -0.007(6) -0.036(6) -0.002(6) C9 0.059(6) 0.046(6) 0.060(5) -0.012(4) -0.005(5) 0.006(5) C10 0.042(6) 0.067(7) 0.057(6) -0.019(5) 0.002(4) -0.002(5) C11 0.060(7) 0.077(8) 0.102(9) -0.016(7) 0.001(7) -0.002(6) C12 0.064(8) 0.101(10) 0.125(11) -0.044(8) 0.021(7) -0.035(7) C13 0.105(12) 0.186(17) 0.200(16) -0.071(13) 0.073(11) -0.095(11) C14 0.134(11) 0.101(10) 0.078(7) 0.013(6) 0.030(7) -0.059(8) C15 0.083(8) 0.065(7) 0.058(6) -0.002(5) 0.013(5) -0.029(6) C16 0.058(6) 0.042(6) 0.083(7) -0.015(5) 0.002(5) -0.014(5) C17 0.045(5) 0.051(6) 0.055(5) -0.002(4) 0.005(4) -0.006(4) C18 0.053(6) 0.050(5) 0.046(5) -0.002(4) -0.018(4) -0.006(5) C19 0.061(7) 0.068(7) 0.070(6) -0.005(5) -0.002(5) -0.023(5) C20 0.079(8) 0.069(7) 0.074(7) -0.010(5) -0.026(6) -0.006(6) C21 0.099(8) 0.064(7) 0.035(5) 0.004(4) -0.002(5) -0.013(6) C22 0.063(6) 0.062(6) 0.037(5) -0.003(4) -0.009(4) 0.000(5) C23 0.082(8) 0.062(7) 0.039(5) -0.006(4) -0.010(5) 0.016(6) C24 0.104(9) 0.057(6) 0.043(5) 0.015(4) 0.002(5) 0.003(6) C25 0.110(10) 0.044(6) 0.064(7) 0.009(5) 0.032(6) -0.004(6) C26 0.123(10) 0.084(9) 0.071(7) 0.006(6) 0.042(7) -0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.098(6) . ? Ag1 N7 2.119(7) . ? Ag1 Ag1 2.8974(13) 3_655 ? Ag1 Ag3 2.9159(11) . ? Ag1 Ag2 2.9377(10) . ? Ag2 N3 2.081(7) 3_655 ? Ag2 N4 2.124(7) . ? Ag3 N8 2.087(7) 3_655 ? Ag3 N9 2.134(7) . ? Cl1 O4 1.312(11) . ? Cl1 O2 1.338(15) . ? Cl1 O3 1.363(10) . ? Cl1 O1 1.373(9) . ? N1 C5 1.302(10) . ? N1 C9 1.329(10) . ? N2 C4 1.337(10) . ? N2 N3 1.370(8) . ? N3 C2 1.365(11) . ? N3 Ag2 2.081(7) 3_655 ? N4 C10 1.328(11) . ? N4 N5 1.347(10) . ? N5 C12 1.341(13) . ? N5 H5 0.8600 . ? N6 C22 1.307(10) . ? N6 C18 1.343(10) . ? N7 C17 1.342(10) . ? N7 N8 1.358(8) . ? N8 C15 1.333(11) . ? N8 Ag3 2.087(7) 3_655 ? N9 C23 1.323(11) . ? N9 N10 1.347(10) . ? N10 C25 1.322(12) . ? N10 H10 0.8600 . ? C1 C2 1.484(12) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.336(12) . ? C3 C4 1.378(12) . ? C3 H3 0.9300 . ? C4 C5 1.495(12) . ? C5 C6 1.410(11) . ? C6 C7 1.369(14) . ? C6 H6 0.9300 . ? C7 C8 1.349(14) . ? C7 H7 0.9300 . ? C8 C9 1.424(12) . ? C8 H8 0.9300 . ? C9 C10 1.466(12) . ? C10 C11 1.409(13) . ? C11 C12 1.391(16) . ? C11 H11 0.9300 . ? C12 C13 1.470(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.476(12) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.365(11) . ? C16 C17 1.375(11) . ? C16 H16 0.9300 . ? C17 C18 1.474(11) . ? C18 C19 1.395(11) . ? C19 C20 1.348(12) . ? C19 H19 0.9300 . ? C20 C21 1.394(13) . ? C20 H20 0.9300 . ? C21 C22 1.361(12) . ? C21 H21 0.9300 . ? C22 C23 1.492(13) . ? C23 C24 1.367(11) . ? C24 C25 1.389(15) . ? C24 H24 0.9300 . ? C25 C26 1.496(13) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N7 171.6(2) . . ? N2 Ag1 Ag1 94.63(18) . 3_655 ? N7 Ag1 Ag1 93.51(18) . 3_655 ? N2 Ag1 Ag3 84.64(18) . . ? N7 Ag1 Ag3 94.24(18) . . ? Ag1 Ag1 Ag3 84.26(3) 3_655 . ? N2 Ag1 Ag2 100.98(18) . . ? N7 Ag1 Ag2 82.00(18) . . ? Ag1 Ag1 Ag2 82.60(3) 3_655 . ? Ag3 Ag1 Ag2 166.07(3) . . ? N3 Ag2 N4 171.1(3) 3_655 . ? N3 Ag2 Ag1 96.75(19) 3_655 . ? N4 Ag2 Ag1 92.1(2) . . ? N8 Ag3 N9 162.7(3) 3_655 . ? N8 Ag3 Ag1 97.45(19) 3_655 . ? N9 Ag3 Ag1 98.2(2) . . ? O4 Cl1 O2 100.8(10) . . ? O4 Cl1 O3 114.5(8) . . ? O2 Cl1 O3 111.6(10) . . ? O4 Cl1 O1 113.5(10) . . ? O2 Cl1 O1 107.9(9) . . ? O3 Cl1 O1 108.2(7) . . ? C5 N1 C9 118.2(7) . . ? C4 N2 N3 107.9(6) . . ? C4 N2 Ag1 122.7(6) . . ? N3 N2 Ag1 127.9(5) . . ? C2 N3 N2 106.7(6) . . ? C2 N3 Ag2 128.9(6) . 3_655 ? N2 N3 Ag2 124.4(5) . 3_655 ? C10 N4 N5 104.8(8) . . ? C10 N4 Ag2 132.8(6) . . ? N5 N4 Ag2 122.2(6) . . ? C12 N5 N4 113.7(9) . . ? C12 N5 H5 123.1 . . ? N4 N5 H5 123.1 . . ? C22 N6 C18 118.4(7) . . ? C17 N7 N8 108.8(7) . . ? C17 N7 Ag1 118.7(5) . . ? N8 N7 Ag1 128.8(5) . . ? C15 N8 N7 107.8(7) . . ? C15 N8 Ag3 128.0(6) . 3_655 ? N7 N8 Ag3 124.1(5) . 3_655 ? C23 N9 N10 105.3(8) . . ? C23 N9 Ag3 130.3(6) . . ? N10 N9 Ag3 123.6(6) . . ? C25 N10 N9 113.1(9) . . ? C25 N10 H10 123.4 . . ? N9 N10 H10 123.4 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N3 109.8(8) . . ? C3 C2 C1 130.5(9) . . ? N3 C2 C1 119.6(8) . . ? C2 C3 C4 106.4(8) . . ? C2 C3 H3 126.8 . . ? C4 C3 H3 126.8 . . ? N2 C4 C3 109.1(8) . . ? N2 C4 C5 119.0(8) . . ? C3 C4 C5 131.9(8) . . ? N1 C5 C6 123.8(9) . . ? N1 C5 C4 117.9(7) . . ? C6 C5 C4 118.3(8) . . ? C7 C6 C5 117.5(10) . . ? C7 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? C8 C7 C6 120.1(9) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 118.4(9) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? N1 C9 C8 121.9(9) . . ? N1 C9 C10 118.9(8) . . ? C8 C9 C10 119.2(9) . . ? N4 C10 C11 110.8(9) . . ? N4 C10 C9 121.4(8) . . ? C11 C10 C9 127.7(9) . . ? C12 C11 C10 105.4(10) . . ? C12 C11 H11 127.3 . . ? C10 C11 H11 127.3 . . ? N5 C12 C11 105.3(10) . . ? N5 C12 C13 122.0(13) . . ? C11 C12 C13 132.6(13) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N8 C15 C16 109.0(8) . . ? N8 C15 C14 122.3(9) . . ? C16 C15 C14 128.7(9) . . ? C15 C16 C17 106.7(8) . . ? C15 C16 H16 126.7 . . ? C17 C16 H16 126.7 . . ? N7 C17 C16 107.7(7) . . ? N7 C17 C18 120.5(7) . . ? C16 C17 C18 131.7(8) . . ? N6 C18 C19 121.5(8) . . ? N6 C18 C17 120.2(7) . . ? C19 C18 C17 118.2(8) . . ? C20 C19 C18 119.2(9) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 118.7(9) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 118.6(8) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? N6 C22 C21 123.5(9) . . ? N6 C22 C23 116.6(8) . . ? C21 C22 C23 119.9(8) . . ? N9 C23 C24 109.8(10) . . ? N9 C23 C22 121.8(8) . . ? C24 C23 C22 128.3(9) . . ? C23 C24 C25 107.1(9) . . ? C23 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? N10 C25 C24 104.5(8) . . ? N10 C25 C26 122.8(11) . . ? C24 C25 C26 132.7(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 Ag2 N3 -66.5(3) . . . 3_655 ? N7 Ag1 Ag2 N3 121.4(3) . . . 3_655 ? Ag1 Ag1 Ag2 N3 26.75(19) 3_655 . . 3_655 ? Ag3 Ag1 Ag2 N3 46.2(2) . . . 3_655 ? N2 Ag1 Ag2 N4 114.7(3) . . . . ? N7 Ag1 Ag2 N4 -57.4(3) . . . . ? Ag1 Ag1 Ag2 N4 -152.0(2) 3_655 . . . ? Ag3 Ag1 Ag2 N4 -132.6(2) . . . . ? N2 Ag1 Ag3 N8 117.4(3) . . . 3_655 ? N7 Ag1 Ag3 N8 -70.9(3) . . . 3_655 ? Ag1 Ag1 Ag3 N8 22.2(2) 3_655 . . 3_655 ? Ag2 Ag1 Ag3 N8 2.8(3) . . . 3_655 ? N2 Ag1 Ag3 N9 -55.1(3) . . . . ? N7 Ag1 Ag3 N9 116.6(3) . . . . ? Ag1 Ag1 Ag3 N9 -150.3(2) 3_655 . . . ? Ag2 Ag1 Ag3 N9 -169.7(2) . . . . ? Ag1 Ag1 N2 C4 -161.6(6) 3_655 . . . ? Ag3 Ag1 N2 C4 114.6(6) . . . . ? Ag2 Ag1 N2 C4 -78.3(6) . . . . ? Ag1 Ag1 N2 N3 33.9(6) 3_655 . . . ? Ag3 Ag1 N2 N3 -49.9(6) . . . . ? Ag2 Ag1 N2 N3 117.3(6) . . . . ? C4 N2 N3 C2 1.6(9) . . . . ? Ag1 N2 N3 C2 167.8(5) . . . . ? C4 N2 N3 Ag2 -177.8(5) . . . 3_655 ? Ag1 N2 N3 Ag2 -11.5(9) . . . 3_655 ? Ag1 Ag2 N4 C10 -53.2(8) . . . . ? Ag1 Ag2 N4 N5 121.0(7) . . . . ? C10 N4 N5 C12 -0.2(11) . . . . ? Ag2 N4 N5 C12 -175.8(7) . . . . ? Ag1 Ag1 N7 C17 -168.4(6) 3_655 . . . ? Ag3 Ag1 N7 C17 -83.9(6) . . . . ? Ag2 Ag1 N7 C17 109.6(6) . . . . ? Ag1 Ag1 N7 N8 36.1(7) 3_655 . . . ? Ag3 Ag1 N7 N8 120.6(7) . . . . ? Ag2 Ag1 N7 N8 -45.9(7) . . . . ? C17 N7 N8 C15 0.4(10) . . . . ? Ag1 N7 N8 C15 157.8(7) . . . . ? C17 N7 N8 Ag3 -177.2(6) . . . 3_655 ? Ag1 N7 N8 Ag3 -19.7(10) . . . 3_655 ? N8 Ag3 N9 C23 150.8(9) 3_655 . . . ? Ag1 Ag3 N9 C23 -54.9(8) . . . . ? N8 Ag3 N9 N10 -18.1(14) 3_655 . . . ? Ag1 Ag3 N9 N10 136.2(7) . . . . ? C23 N9 N10 C25 2.5(11) . . . . ? Ag3 N9 N10 C25 173.8(6) . . . . ? N2 N3 C2 C3 -2.9(10) . . . . ? Ag2 N3 C2 C3 176.4(6) 3_655 . . . ? N2 N3 C2 C1 -179.8(8) . . . . ? Ag2 N3 C2 C1 -0.5(13) 3_655 . . . ? N3 C2 C3 C4 3.1(11) . . . . ? C1 C2 C3 C4 179.6(11) . . . . ? N3 N2 C4 C3 0.3(10) . . . . ? Ag1 N2 C4 C3 -166.8(6) . . . . ? N3 N2 C4 C5 -179.5(7) . . . . ? Ag1 N2 C4 C5 13.3(11) . . . . ? C2 C3 C4 N2 -2.1(11) . . . . ? C2 C3 C4 C5 177.7(9) . . . . ? C9 N1 C5 C6 0.2(13) . . . . ? C9 N1 C5 C4 -178.6(7) . . . . ? N2 C4 C5 N1 13.1(12) . . . . ? C3 C4 C5 N1 -166.7(10) . . . . ? N2 C4 C5 C6 -165.8(9) . . . . ? C3 C4 C5 C6 14.4(15) . . . . ? N1 C5 C6 C7 -1.0(15) . . . . ? C4 C5 C6 C7 177.8(10) . . . . ? C5 C6 C7 C8 0.6(18) . . . . ? C6 C7 C8 C9 0.4(18) . . . . ? C5 N1 C9 C8 0.9(13) . . . . ? C5 N1 C9 C10 -178.7(8) . . . . ? C7 C8 C9 N1 -1.3(15) . . . . ? C7 C8 C9 C10 178.4(11) . . . . ? N5 N4 C10 C11 -0.2(10) . . . . ? Ag2 N4 C10 C11 174.8(7) . . . . ? N5 N4 C10 C9 -177.3(8) . . . . ? Ag2 N4 C10 C9 -2.3(13) . . . . ? N1 C9 C10 N4 23.4(13) . . . . ? C8 C9 C10 N4 -156.3(9) . . . . ? N1 C9 C10 C11 -153.2(9) . . . . ? C8 C9 C10 C11 27.2(14) . . . . ? N4 C10 C11 C12 0.5(12) . . . . ? C9 C10 C11 C12 177.4(10) . . . . ? N4 N5 C12 C11 0.5(13) . . . . ? N4 N5 C12 C13 177.8(11) . . . . ? C10 C11 C12 N5 -0.6(13) . . . . ? C10 C11 C12 C13 -177.4(14) . . . . ? N7 N8 C15 C16 -0.1(11) . . . . ? Ag3 N8 C15 C16 177.3(6) 3_655 . . . ? N7 N8 C15 C14 -179.7(10) . . . . ? Ag3 N8 C15 C14 -2.3(15) 3_655 . . . ? N8 C15 C16 C17 -0.1(12) . . . . ? C14 C15 C16 C17 179.4(11) . . . . ? N8 N7 C17 C16 -0.4(10) . . . . ? Ag1 N7 C17 C16 -160.5(6) . . . . ? N8 N7 C17 C18 178.0(7) . . . . ? Ag1 N7 C17 C18 17.9(10) . . . . ? C15 C16 C17 N7 0.4(11) . . . . ? C15 C16 C17 C18 -177.9(10) . . . . ? C22 N6 C18 C19 -0.7(13) . . . . ? C22 N6 C18 C17 -177.5(8) . . . . ? N7 C17 C18 N6 23.4(13) . . . . ? C16 C17 C18 N6 -158.6(9) . . . . ? N7 C17 C18 C19 -153.5(8) . . . . ? C16 C17 C18 C19 24.6(15) . . . . ? N6 C18 C19 C20 -1.8(14) . . . . ? C17 C18 C19 C20 175.0(9) . . . . ? C18 C19 C20 C21 2.2(14) . . . . ? C19 C20 C21 C22 -0.2(14) . . . . ? C18 N6 C22 C21 2.9(13) . . . . ? C18 N6 C22 C23 -178.1(8) . . . . ? C20 C21 C22 N6 -2.5(15) . . . . ? C20 C21 C22 C23 178.5(9) . . . . ? N10 N9 C23 C24 -3.4(10) . . . . ? Ag3 N9 C23 C24 -173.8(6) . . . . ? N10 N9 C23 C22 176.5(8) . . . . ? Ag3 N9 C23 C22 6.1(13) . . . . ? N6 C22 C23 N9 3.6(13) . . . . ? C21 C22 C23 N9 -177.3(9) . . . . ? N6 C22 C23 C24 -176.5(9) . . . . ? C21 C22 C23 C24 2.5(15) . . . . ? N9 C23 C24 C25 3.1(11) . . . . ? C22 C23 C24 C25 -176.8(9) . . . . ? N9 N10 C25 C24 -0.6(11) . . . . ? N9 N10 C25 C26 177.1(9) . . . . ? C23 C24 C25 N10 -1.5(11) . . . . ? C23 C24 C25 C26 -178.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.859 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.128 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.220 0.250 119.4 38.4 2 0.500 0.280 0.750 119.4 37.3 3 0.500 0.720 0.250 119.4 37.1 4 0.000 0.780 0.750 119.4 38.6 _platon_squeeze_details ; ; #===END