# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Dr A R Kennedy' _publ_contact_author_address ; Dept. of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street GLASGOW G1 1XL UK ; _publ_contact_author_email A.R.KENNEDY@STRATH.AC.UK _publ_section_title ; Chromophore containing bipyridyl ligands: Part 1, supramolecular solid-state structure of Ag(I) complexes. ; _publ_contact_letter ; Updated after referee's comments, March 2005. Dear Sir, The following cif contains details of 9 crystal structures submitted as supplementary information for the ms by Kennedy, Brown, Graham, Kirkhouse, Kittner, Major, McHugh, Murdoch & Smith which we ask you to consider for publication. If there are any problems with the file or its transmission please contact me. Yours Sincerely, Dr Alan Kennedy P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL Scotland a.r.kennedy@strath.ac.uk ; loop_ _publ_author_name 'A. R. Kennedy' 'Karen G. Brown' 'Duncan Graham' 'Jennifer B. Kirkhouse' 'Madeleine Kittner' ; C.Major ; 'Callum J. McHugh' 'Paul Murdoch' 'W. Smith' data_ag2 _database_code_depnum_ccdc_archive 'CCDC 266716' #-------------------------------------------------------------------------- #--------------DATA FOR 1A - Ag(ligand1) BF4------------------------------- #------------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Ag B F4 N5' _chemical_formula_weight 445.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.0846(2) _cell_length_b 15.6681(4) _cell_length_c 8.6321(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.589(1) _cell_angle_gamma 90.00 _cell_volume 817.50(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6131 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.282 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6281 _exptl_absorpt_correction_T_max 0.9387 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8971 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 27.32 _reflns_number_total 1878 _reflns_number_gt 1448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.2630P] 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 1878 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.5000 0.0000 0.02214(12) Uani 1 d S . . F1 F 0.0467(4) 0.2500 0.1715(3) 0.0408(6) Uani 1 d S . . F2 F -0.0140(3) 0.32235(11) -0.0581(2) 0.0355(4) Uani 1 d . . . F3 F 0.3088(4) 0.2500 0.0022(3) 0.0381(6) Uani 1 d S . . N1 N 0.2725(4) 0.51203(13) -0.1352(3) 0.0187(5) Uani 1 d . . . N2 N 0.9111(4) 0.48478(14) -0.4624(3) 0.0216(5) Uani 1 d . . . N3 N 0.3466(7) 0.2500 -0.4295(5) 0.0442(10) Uani 1 d S . . C1 C 0.3535(5) 0.58926(16) -0.1623(3) 0.0227(6) Uani 1 d . . . H1 H 0.2863 0.6379 -0.1219 0.027 Uiso 1 calc R . . C2 C 0.5297(4) 0.60127(17) -0.2463(3) 0.0230(6) Uani 1 d . . . H2 H 0.5800 0.6574 -0.2645 0.028 Uiso 1 calc R . . C3 C 0.6342(4) 0.53140(18) -0.3044(3) 0.0186(5) Uani 1 d . . . C4 C 0.5491(4) 0.45045(17) -0.2762(3) 0.0205(6) Uani 1 d . . . H4 H 0.6136 0.4007 -0.3148 0.025 Uiso 1 calc R . . C5 C 0.3719(4) 0.44384(17) -0.1922(3) 0.0204(6) Uani 1 d . . . H5 H 0.3164 0.3886 -0.1733 0.025 Uiso 1 calc R . . C6 C 0.8217(4) 0.54556(16) -0.3908(3) 0.0199(6) Uani 1 d . . . H6 H 0.8808 0.6016 -0.3948 0.024 Uiso 1 calc R . . C7 C 0.1629(10) 0.2500 -0.4272(5) 0.0396(12) Uani 1 d S . . C8 C -0.0813(8) 0.2500 -0.4312(6) 0.0434(12) Uani 1 d S . . H8A H -0.1468 0.2173 -0.5218 0.065 Uiso 0.50 calc PR . . H8B H -0.1360 0.3089 -0.4390 0.065 Uiso 0.50 calc PR . . H8C H -0.1226 0.2238 -0.3356 0.065 Uiso 0.50 calc PR . . B1 B 0.0830(9) 0.2500 0.0151(6) 0.0274(10) Uani 1 d S . . 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 0.01768(17) 0.0283(2) 0.02246(18) 0.00048(12) 0.01092(11) -0.00052(11) F1 0.0465(16) 0.0435(15) 0.0352(14) 0.000 0.0174(12) 0.000 F2 0.0394(11) 0.0222(9) 0.0477(10) 0.0029(8) 0.0166(8) 0.0055(7) F3 0.0286(14) 0.0348(13) 0.0538(16) 0.000 0.0179(12) 0.000 N1 0.0141(11) 0.0265(13) 0.0170(11) 0.0001(9) 0.0088(9) -0.0008(8) N2 0.0154(11) 0.0306(14) 0.0206(11) 0.0026(9) 0.0087(10) -0.0014(9) N3 0.044(3) 0.037(2) 0.051(3) 0.000 0.003(2) 0.000 C1 0.0217(14) 0.0206(14) 0.0269(14) -0.0009(12) 0.0083(12) 0.0030(11) C2 0.0219(14) 0.0197(14) 0.0289(14) 0.0017(12) 0.0100(12) -0.0015(11) C3 0.0156(12) 0.0243(12) 0.0158(12) 0.0011(11) 0.0014(11) 0.0011(11) C4 0.0220(14) 0.0194(15) 0.0213(13) -0.0006(11) 0.0070(11) 0.0008(11) C5 0.0211(14) 0.0189(13) 0.0220(13) 0.0000(11) 0.0056(11) -0.0019(11) C6 0.0180(13) 0.0214(15) 0.0217(13) 0.0022(11) 0.0083(11) -0.0006(11) C7 0.070(4) 0.018(2) 0.031(3) 0.000 0.007(3) 0.000 C8 0.055(3) 0.032(3) 0.047(3) 0.000 0.021(3) 0.000 B1 0.030(2) 0.021(2) 0.034(3) 0.000 0.020(2) 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 Ag1 N1 2.143(2) 3_565 ? Ag1 N1 2.143(2) . ? F1 B1 1.393(5) . ? F2 B1 1.395(4) . ? F3 B1 1.391(6) . ? N1 C1 1.337(3) . ? N1 C5 1.348(3) . ? N2 C6 1.289(4) . ? N2 N2 1.407(5) 3_764 ? N3 C7 1.121(6) . ? C1 C2 1.374(4) . ? C1 H1 0.9500 . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? C3 C4 1.402(4) . ? C3 C6 1.450(4) . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.482(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? B1 F2 1.395(4) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.0 3_565 . ? C1 N1 C5 117.6(2) . . ? C1 N1 Ag1 119.91(17) . . ? C5 N1 Ag1 122.45(18) . . ? C6 N2 N2 111.1(3) . 3_764 ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 117.2(2) . . ? C2 C3 C6 119.0(3) . . ? C4 C3 C6 123.8(3) . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.1(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C3 122.2(2) . . ? N2 C6 H6 118.9 . . ? C3 C6 H6 118.9 . . ? N3 C7 C8 177.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F3 B1 F1 110.2(4) . . ? F3 B1 F2 109.5(2) . 4_565 ? F1 B1 F2 109.4(2) . 4_565 ? F3 B1 F2 109.5(2) . . ? F1 B1 F2 109.4(2) . . ? F2 B1 F2 108.7(4) 4_565 . ? 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 C5 N1 C1 C2 0.7(4) . . . . ? Ag1 N1 C1 C2 179.1(2) . . . . ? N1 C1 C2 C3 -1.3(4) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C1 C2 C3 C6 -179.2(2) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C6 C3 C4 C5 179.6(3) . . . . ? C1 N1 C5 C4 -0.3(4) . . . . ? Ag1 N1 C5 C4 -178.64(19) . . . . ? C3 C4 C5 N1 0.4(4) . . . . ? N2 N2 C6 C3 179.7(2) 3_764 . . . ? C2 C3 C6 N2 -172.2(2) . . . . ? C4 C3 C6 N2 7.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.934 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.102 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 1C - Ag(ligand1) SbF6------------------------------- #------------------------------------------------------------------------- data_agsb _database_code_depnum_ccdc_archive 'CCDC 266717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? #formula based on 1 MeCN and 1.75 H2O solvent molecules. _chemical_formula_sum 'C14 H16.50 Ag F6 N5 O1.75 Sb' _chemical_formula_weight 626.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sb Sb -0.5866 1.5461 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4959(15) _cell_length_b 11.9036(16) _cell_length_c 8.6632(12) _cell_angle_alpha 97.956(13) _cell_angle_beta 110.611(9) _cell_angle_gamma 92.935(13) _cell_volume 997.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.66 _cell_measurement_theta_max 18.62 _exptl_crystal_description fragment _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 603 _exptl_absorpt_coefficient_mu 2.409 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North et al' _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Diffractometer' _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.825 _diffrn_reflns_number 4841 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4589 _reflns_number_gt 4185 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/Rigaku diffractometer control software ; _computing_cell_refinement ' " ' _computing_data_reduction texsan _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The SbF6 ion was modelled as disordered over two sites whose occupancies were refined to total 1. The minor component atoms were refined isotropically. There is an area of electron density which is interpreted as badly disordered and possibly partially present solvent. From the closeness of the atom sites it is presumed that this may be a 2nd NCMe molecule but no satisfactory model was obtained. Eventually this area was treated by placing partial O atoms on each site. The formula given assumes that these correspond to water molecules. 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 w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+1.6811P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4589 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 1.44115(4) 0.78282(11) -0.31706(17) 0.02444(19) Uani 0.873(5) d P . . Sb2 Sb 1.4366(3) 0.7572(4) -0.3591(6) 0.0186(7) Uiso 0.127(5) d P . . Ag1 Ag 1.05609(3) 1.208291(19) -0.40913(3) 0.02468(8) Uani 1 d . . . F1 F 1.4972(4) 0.6651(3) -0.4361(7) 0.0681(12) Uani 0.873(5) d P . . F2 F 1.6106(3) 0.8012(4) -0.1419(4) 0.0556(10) Uani 0.873(5) d P . . F3 F 1.3846(3) 0.9016(4) -0.2003(4) 0.0520(8) Uani 0.873(5) d P . . F4 F 1.2682(2) 0.7659(2) -0.4919(3) 0.0466(6) Uani 1 d . . . F5 F 1.3723(3) 0.6794(3) -0.2143(5) 0.0550(11) Uani 0.873(5) d P . . F6 F 1.5058(3) 0.8891(2) -0.4178(3) 0.0444(6) Uani 1 d . . . F7 F 1.3737(15) 0.6267(13) -0.2988(19) 0.021(3) Uiso 0.127(5) d P . . F8 F 1.615(2) 0.7488(17) -0.218(3) 0.037(5) Uiso 0.127(5) d P . . F9 F 1.467(2) 0.6697(19) -0.530(3) 0.040(5) Uiso 0.127(5) d P . . F10 F 1.396(3) 0.850(2) -0.187(3) 0.047(6) Uiso 0.127(5) d P . . N1 N 1.0083(3) 1.0598(2) -0.3120(3) 0.0209(5) Uani 1 d . . . N2 N 1.0433(3) 0.7453(2) 0.0276(3) 0.0202(5) Uani 1 d . . . N3 N 1.0039(3) 0.6619(2) 0.1085(3) 0.0217(5) Uani 1 d . . . N4 N 1.0683(3) 0.3409(2) 0.4455(3) 0.0193(5) Uani 1 d . . . N5 N 1.3184(4) 1.2023(4) -0.2917(6) 0.0544(11) Uani 1 d . . . C1 C 0.8820(3) 1.0230(3) -0.3232(4) 0.0226(6) Uani 1 d . . . H1 H 0.8071 1.0596 -0.3859 0.027 Uiso 1 calc R . . C2 C 0.8557(3) 0.9339(3) -0.2473(4) 0.0223(6) Uani 1 d . . . H2 H 0.7645 0.9100 -0.2590 0.027 Uiso 1 calc R . . C3 C 0.9642(3) 0.8800(2) -0.1540(4) 0.0179(5) Uani 1 d . . . C4 C 1.0949(3) 0.9158(3) -0.1467(4) 0.0224(6) Uani 1 d . . . H4 H 1.1710 0.8788 -0.0880 0.027 Uiso 1 calc R . . C5 C 1.1134(3) 1.0054(3) -0.2253(4) 0.0237(6) Uani 1 d . . . H5 H 1.2033 1.0296 -0.2182 0.028 Uiso 1 calc R . . C6 C 0.9400(3) 0.7900(2) -0.0640(4) 0.0199(6) Uani 1 d . . . H6 H 0.8497 0.7653 -0.0733 0.024 Uiso 1 calc R . . C7 C 1.1046(3) 0.6079(2) 0.1790(4) 0.0201(6) Uani 1 d . . . H7 H 1.1914 0.6281 0.1733 0.024 Uiso 1 calc R . . C8 C 1.0891(3) 0.5153(2) 0.2688(4) 0.0182(5) Uani 1 d . . . C9 C 0.9620(3) 0.4698(2) 0.2625(4) 0.0188(5) Uani 1 d . . . H9 H 0.8804 0.4977 0.1974 0.023 Uiso 1 calc R . . C10 C 0.9562(3) 0.3833(2) 0.3524(4) 0.0202(6) Uani 1 d . . . H10 H 0.8693 0.3528 0.3479 0.024 Uiso 1 calc R . . C11 C 1.1907(3) 0.3834(2) 0.4504(4) 0.0216(6) Uani 1 d . . . H11 H 1.2705 0.3534 0.5160 0.026 Uiso 1 calc R . . C12 C 1.2052(3) 0.4697(3) 0.3630(4) 0.0224(6) Uani 1 d . . . H12 H 1.2932 0.4972 0.3675 0.027 Uiso 1 calc R . . C13 C 1.4270(4) 1.1800(4) -0.2466(5) 0.0373(8) Uani 1 d . . . C14 C 1.5666(4) 1.1511(4) -0.1857(5) 0.0431(9) Uani 1 d . . . H14A H 1.6291 1.2206 -0.1291 0.065 Uiso 1 calc R . . H14B H 1.5896 1.1154 -0.2802 0.065 Uiso 1 calc R . . H14C H 1.5755 1.0978 -0.1068 0.065 Uiso 1 calc R . . O1S O 0.5533(7) 0.4554(5) 0.8515(9) 0.0437(10) Uiso 0.50 d P . . O2S O 0.6059(8) 0.4811(7) 0.9286(10) 0.0437(10) Uiso 0.50 d P . . O3S O 0.6312(11) 0.5369(10) 0.9761(13) 0.0437(10) Uiso 0.301(9) d P . . O4S O 0.5439(12) 0.4881(10) 0.9705(15) 0.0437(10) Uiso 0.306(9) d P . . O5S O 0.455(3) 0.467(2) 0.959(3) 0.0437(10) Uiso 0.141(8) d P . . 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 Sb1 0.01780(15) 0.0281(3) 0.0299(3) 0.0142(3) 0.00805(14) 0.00368(13) Ag1 0.03185(14) 0.01946(12) 0.02896(13) 0.01471(9) 0.01441(11) 0.00459(9) F1 0.065(2) 0.0432(18) 0.104(4) -0.003(2) 0.045(3) 0.0139(16) F2 0.0190(13) 0.091(3) 0.053(2) 0.037(2) 0.0010(12) -0.0003(14) F3 0.0536(19) 0.056(2) 0.0557(19) 0.0048(17) 0.0318(15) 0.0135(17) F4 0.0338(12) 0.0489(14) 0.0448(13) 0.0218(11) -0.0049(10) -0.0036(10) F5 0.0280(14) 0.067(2) 0.077(2) 0.055(2) 0.0119(14) 0.0030(13) F6 0.0517(15) 0.0456(13) 0.0381(12) 0.0158(10) 0.0182(11) -0.0113(11) N1 0.0293(14) 0.0159(11) 0.0208(12) 0.0086(9) 0.0110(10) 0.0038(10) N2 0.0243(13) 0.0187(11) 0.0213(12) 0.0101(10) 0.0101(10) 0.0036(10) N3 0.0251(13) 0.0195(12) 0.0246(12) 0.0126(10) 0.0107(11) 0.0037(10) N4 0.0262(13) 0.0161(11) 0.0191(11) 0.0089(9) 0.0101(10) 0.0040(10) N5 0.0304(18) 0.066(3) 0.073(3) 0.048(2) 0.0125(18) 0.0058(17) C1 0.0235(15) 0.0202(14) 0.0241(14) 0.0113(11) 0.0055(12) 0.0046(11) C2 0.0222(15) 0.0192(13) 0.0267(15) 0.0088(12) 0.0084(12) 0.0032(11) C3 0.0226(14) 0.0157(12) 0.0168(12) 0.0064(10) 0.0072(11) 0.0030(11) C4 0.0212(15) 0.0236(14) 0.0274(15) 0.0148(12) 0.0103(12) 0.0069(12) C5 0.0244(15) 0.0239(15) 0.0278(15) 0.0135(12) 0.0118(13) 0.0056(12) C6 0.0240(15) 0.0167(13) 0.0219(13) 0.0072(11) 0.0103(12) 0.0020(11) C7 0.0223(14) 0.0202(14) 0.0203(13) 0.0079(11) 0.0093(11) 0.0005(11) C8 0.0253(15) 0.0156(13) 0.0162(12) 0.0063(10) 0.0089(11) 0.0032(11) C9 0.0206(14) 0.0184(13) 0.0187(13) 0.0070(11) 0.0070(11) 0.0048(11) C10 0.0235(15) 0.0171(13) 0.0223(14) 0.0052(11) 0.0108(12) 0.0010(11) C11 0.0256(15) 0.0181(13) 0.0251(14) 0.0111(11) 0.0107(12) 0.0066(11) C12 0.0205(14) 0.0222(14) 0.0282(15) 0.0103(12) 0.0112(12) 0.0029(11) C13 0.032(2) 0.046(2) 0.0343(18) 0.0237(17) 0.0066(15) 0.0006(16) C14 0.031(2) 0.058(3) 0.036(2) 0.0096(18) 0.0056(16) 0.0099(18) _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 Sb1 F10 1.52(3) . ? Sb1 F8 1.81(2) . ? Sb1 F6 1.859(2) . ? Sb1 F2 1.866(3) . ? Sb1 F1 1.866(3) . ? Sb1 F3 1.868(3) . ? Sb1 F5 1.870(3) . ? Sb1 F4 1.890(2) . ? Sb1 F7 2.001(15) . ? Sb1 F9 2.23(2) . ? Sb2 F1 1.490(6) . ? Sb2 F4 1.754(4) . ? Sb2 F9 1.82(2) . ? Sb2 F8 1.86(2) . ? Sb2 F7 1.867(15) . ? Sb2 F6 1.901(4) . ? Sb2 F10 1.91(2) . ? Sb2 F5 1.934(4) . ? Sb2 F2 2.088(5) . ? Sb2 F3 2.261(6) . ? Ag1 N1 2.168(3) . ? Ag1 N4 2.177(2) 1_564 ? Ag1 N5 2.586(4) . ? N1 C1 1.341(4) . ? N1 C5 1.351(4) . ? N2 C6 1.288(4) . ? N2 N3 1.415(3) . ? N3 C7 1.275(4) . ? N4 C10 1.339(4) . ? N4 C11 1.341(4) . ? N4 Ag1 2.177(2) 1_546 ? N5 C13 1.126(5) . ? C1 C2 1.387(4) . ? C1 H1 0.9500 . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.393(4) . ? C3 C6 1.471(4) . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.469(4) . ? C7 H7 0.9500 . ? C8 C12 1.391(4) . ? C8 C9 1.394(4) . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.449(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O1S O2S 0.715(8) . ? O1S O4S 1.091(14) . ? O1S O3S 1.335(12) . ? O1S O5S 1.61(3) . ? O1S O5S 1.81(3) 2_667 ? O2S O3S 0.714(10) . ? O2S O4S 0.852(12) . ? O2S O5S 1.44(3) 2_667 ? O2S O5S 1.70(3) . ? O3S O4S 1.042(15) . ? O3S O5S 1.23(3) 2_667 ? O4S O5S 0.75(2) 2_667 ? O4S O5S 0.92(2) . ? O4S O4S 1.23(3) 2_667 ? O5S O4S 0.75(2) 2_667 ? O5S O5S 1.15(5) 2_667 ? O5S O3S 1.23(3) 2_667 ? O5S O2S 1.44(3) 2_667 ? O5S O1S 1.81(3) 2_667 ? 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 F10 Sb1 F8 109.4(11) . . ? F10 Sb1 F6 106.7(10) . . ? F8 Sb1 F6 89.6(6) . . ? F10 Sb1 F2 83.6(10) . . ? F8 Sb1 F2 26.8(6) . . ? F6 Sb1 F2 90.31(13) . . ? F10 Sb1 F1 161.9(10) . . ? F8 Sb1 F1 64.0(7) . . ? F6 Sb1 F1 90.42(16) . . ? F2 Sb1 F1 90.77(19) . . ? F10 Sb1 F3 18.8(9) . . ? F8 Sb1 F3 116.4(7) . . ? F6 Sb1 F3 88.96(14) . . ? F2 Sb1 F3 89.64(17) . . ? F1 Sb1 F3 179.27(19) . . ? F10 Sb1 F5 71.6(10) . . ? F8 Sb1 F5 91.8(6) . . ? F6 Sb1 F5 178.10(14) . . ? F2 Sb1 F5 90.38(13) . . ? F1 Sb1 F5 91.34(19) . . ? F3 Sb1 F5 89.27(17) . . ? F10 Sb1 F4 95.4(10) . . ? F8 Sb1 F4 154.2(6) . . ? F6 Sb1 F4 89.91(11) . . ? F2 Sb1 F4 178.96(15) . . ? F1 Sb1 F4 90.25(17) . . ? F3 Sb1 F4 89.35(14) . . ? F5 Sb1 F4 89.37(12) . . ? F10 Sb1 F7 97.6(10) . . ? F8 Sb1 F7 88.4(8) . . ? F6 Sb1 F7 154.8(4) . . ? F2 Sb1 F7 99.0(4) . . ? F1 Sb1 F7 66.2(5) . . ? F3 Sb1 F7 114.3(4) . . ? F5 Sb1 F7 26.6(4) . . ? F4 Sb1 F7 81.2(4) . . ? F10 Sb1 F9 169.2(11) . . ? F8 Sb1 F9 79.5(8) . . ? F6 Sb1 F9 78.9(6) . . ? F2 Sb1 F9 105.9(6) . . ? F1 Sb1 F9 19.1(5) . . ? F3 Sb1 F9 160.2(6) . . ? F5 Sb1 F9 102.6(6) . . ? F4 Sb1 F9 75.2(6) . . ? F7 Sb1 F9 76.1(7) . . ? F1 Sb2 F4 110.0(3) . . ? F1 Sb2 F9 24.4(7) . . ? F4 Sb2 F9 90.0(7) . . ? F1 Sb2 F8 70.3(6) . . ? F4 Sb2 F8 179.7(7) . . ? F9 Sb2 F8 90.3(9) . . ? F1 Sb2 F7 77.3(5) . . ? F4 Sb2 F7 88.8(5) . . ? F9 Sb2 F7 90.3(8) . . ? F8 Sb2 F7 91.3(8) . . ? F1 Sb2 F6 101.8(2) . . ? F4 Sb2 F6 92.79(17) . . ? F9 Sb2 F6 89.3(7) . . ? F8 Sb2 F6 87.1(6) . . ? F7 Sb2 F6 178.4(5) . . ? F1 Sb2 F10 157.9(8) . . ? F4 Sb2 F10 87.2(8) . . ? F9 Sb2 F10 177.2(10) . . ? F8 Sb2 F10 92.5(10) . . ? F7 Sb2 F10 89.7(9) . . ? F6 Sb2 F10 90.8(7) . . ? F1 Sb2 F5 101.8(3) . . ? F4 Sb2 F5 91.45(17) . . ? F9 Sb2 F5 117.5(8) . . ? F8 Sb2 F5 88.5(6) . . ? F7 Sb2 F5 27.3(4) . . ? F6 Sb2 F5 152.9(3) . . ? F10 Sb2 F5 62.7(8) . . ? F1 Sb2 F2 94.4(2) . . ? F4 Sb2 F2 155.5(3) . . ? F9 Sb2 F2 113.9(7) . . ? F8 Sb2 F2 24.1(6) . . ? F7 Sb2 F2 96.0(5) . . ? F6 Sb2 F2 82.78(18) . . ? F10 Sb2 F2 68.9(8) . . ? F5 Sb2 F2 82.35(18) . . ? F1 Sb2 F3 168.8(3) . . ? F4 Sb2 F3 81.2(2) . . ? F9 Sb2 F3 163.4(7) . . ? F8 Sb2 F3 98.4(6) . . ? F7 Sb2 F3 103.5(5) . . ? F6 Sb2 F3 77.17(19) . . ? F10 Sb2 F3 15.2(7) . . ? F5 Sb2 F3 77.1(2) . . ? F2 Sb2 F3 74.4(2) . . ? N1 Ag1 N4 167.86(10) . 1_564 ? N1 Ag1 N5 95.42(11) . . ? N4 Ag1 N5 93.31(11) 1_564 . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ag1 124.1(2) . . ? C5 N1 Ag1 117.9(2) . . ? C6 N2 N3 112.2(3) . . ? C7 N3 N2 110.9(3) . . ? C10 N4 C11 118.5(3) . . ? C10 N4 Ag1 121.7(2) . 1_546 ? C11 N4 Ag1 119.8(2) . 1_546 ? C13 N5 Ag1 168.2(4) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.3(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 117.8(3) . . ? C2 C3 C6 120.3(3) . . ? C4 C3 C6 121.9(3) . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C3 118.9(3) . . ? N2 C6 H6 120.6 . . ? C3 C6 H6 120.6 . . ? N3 C7 C8 121.3(3) . . ? N3 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C12 C8 C9 118.2(3) . . ? C12 C8 C7 119.2(3) . . ? C9 C8 C7 122.6(3) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N4 C10 C9 122.7(3) . . ? N4 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N4 C11 C12 122.4(3) . . ? N4 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C8 119.1(3) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? N5 C13 C14 179.0(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 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 N4 Ag1 N1 C1 -49.2(6) 1_564 . . . ? N5 Ag1 N1 C1 175.0(3) . . . . ? N4 Ag1 N1 C5 135.3(4) 1_564 . . . ? N5 Ag1 N1 C5 -0.6(3) . . . . ? C6 N2 N3 C7 170.9(3) . . . . ? N1 Ag1 N5 C13 35.7(18) . . . . ? N4 Ag1 N5 C13 -135.9(18) 1_564 . . . ? C5 N1 C1 C2 1.4(5) . . . . ? Ag1 N1 C1 C2 -174.2(2) . . . . ? N1 C1 C2 C3 0.5(5) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C1 C2 C3 C6 176.3(3) . . . . ? C2 C3 C4 C5 2.6(4) . . . . ? C6 C3 C4 C5 -176.1(3) . . . . ? C1 N1 C5 C4 -1.2(5) . . . . ? Ag1 N1 C5 C4 174.6(2) . . . . ? C3 C4 C5 N1 -0.8(5) . . . . ? N3 N2 C6 C3 178.8(2) . . . . ? C2 C3 C6 N2 -176.8(3) . . . . ? C4 C3 C6 N2 1.9(4) . . . . ? N2 N3 C7 C8 -178.8(2) . . . . ? N3 C7 C8 C12 -171.2(3) . . . . ? N3 C7 C8 C9 9.5(4) . . . . ? C12 C8 C9 C10 1.4(4) . . . . ? C7 C8 C9 C10 -179.3(3) . . . . ? C11 N4 C10 C9 -0.6(4) . . . . ? Ag1 N4 C10 C9 178.2(2) 1_546 . . . ? C8 C9 C10 N4 -0.2(4) . . . . ? C10 N4 C11 C12 0.2(4) . . . . ? Ag1 N4 C11 C12 -178.7(2) 1_546 . . . ? N4 C11 C12 C8 1.0(5) . . . . ? C9 C8 C12 C11 -1.8(4) . . . . ? C7 C8 C12 C11 178.8(3) . . . . ? Ag1 N5 C13 C14 -84(28) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.633 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.116 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 1D Ag(ligand1) NO3------------------------------- #------------------------------------------------------------------------- data_agab _database_code_depnum_ccdc_archive 'CCDC 266718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Ag N5 O3' _chemical_formula_weight 380.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 6.7441(12) _cell_length_b 13.452(2) _cell_length_c 15.028(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.568(13) _cell_angle_gamma 90.00 _cell_volume 1351.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.74 _cell_measurement_theta_max 8.93 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Diffractometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3284 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3019 _reflns_number_gt 2565 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC-Rigaku diff control' _computing_cell_refinement ? _computing_data_reduction texsan _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+1.2435P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3019 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.75358(4) 0.13407(2) -0.237384(15) 0.02055(10) Uani 1 d . . . O1 O -0.3716(4) 0.1775(2) -0.26984(16) 0.0257(5) Uani 1 d . . . O2 O -0.3168(5) 0.0210(2) -0.28296(19) 0.0367(7) Uani 1 d . . . O3 O -0.1234(4) 0.1086(3) -0.18563(18) 0.0398(8) Uani 1 d . . . N1 N -0.6473(4) 0.1269(2) -0.09406(18) 0.0190(6) Uani 1 d . . . N2 N -0.2515(5) 0.1612(3) 0.21230(19) 0.0278(7) Uani 1 d . . . N3 N -0.2091(5) 0.1631(3) 0.30666(19) 0.0275(7) Uani 1 d . . . N4 N 0.1528(4) 0.1239(2) 0.61831(18) 0.0183(6) Uani 1 d . . . N5 N -0.2685(4) 0.1017(3) -0.24595(17) 0.0209(6) Uani 1 d . . . C1 C -0.4737(5) 0.1720(3) -0.0642(2) 0.0205(7) Uani 1 d . . . C2 C -0.3947(5) 0.1735(3) 0.0257(2) 0.0223(7) Uani 1 d . . . C3 C -0.5011(5) 0.1297(2) 0.0888(2) 0.0191(7) Uani 1 d . . . C4 C -0.6812(6) 0.0827(3) 0.0579(2) 0.0222(7) Uani 1 d . . . C5 C -0.7476(5) 0.0827(3) -0.0342(2) 0.0218(7) Uani 1 d . . . C6 C -0.4274(6) 0.1328(3) 0.1852(2) 0.0238(7) Uani 1 d . . . C7 C -0.0378(6) 0.1299(3) 0.3359(2) 0.0221(7) Uani 1 d . . . C8 C 0.0270(5) 0.1278(2) 0.4331(2) 0.0189(7) Uani 1 d . . . C9 C 0.2119(5) 0.0881(3) 0.4678(2) 0.0223(7) Uani 1 d . . . C10 C 0.2685(5) 0.0871(3) 0.5606(2) 0.0206(7) Uani 1 d . . . C11 C -0.0257(5) 0.1635(3) 0.5843(2) 0.0195(7) Uani 1 d . . . C12 C -0.0934(5) 0.1653(3) 0.4938(2) 0.0205(7) Uani 1 d . . . H1 H -0.407(6) 0.200(3) -0.106(3) 0.025(10) Uiso 1 d . . . H2 H -0.279(6) 0.203(3) 0.047(3) 0.028(11) Uiso 1 d . . . H3 H -0.757(5) 0.056(3) 0.095(2) 0.013(9) Uiso 1 d . . . H4 H -0.881(7) 0.050(3) -0.060(3) 0.036(12) Uiso 1 d . . . H5 H -0.523(8) 0.121(3) 0.222(3) 0.048(15) Uiso 1 d . . . H6 H 0.045(6) 0.107(3) 0.301(3) 0.019(10) Uiso 1 d . . . H7 H 0.301(6) 0.059(3) 0.431(2) 0.020(10) Uiso 1 d . . . H8 H 0.392(5) 0.064(3) 0.584(2) 0.007(8) Uiso 1 d . . . H9 H -0.101(5) 0.191(3) 0.625(2) 0.009(8) Uiso 1 d . . . H10 H -0.230(6) 0.193(3) 0.476(3) 0.029(11) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02177(15) 0.03035(16) 0.00779(14) 0.00015(9) -0.00458(9) 0.00017(11) O1 0.0273(13) 0.0275(14) 0.0220(12) 0.0054(10) 0.0021(10) 0.0032(11) O2 0.0473(17) 0.0265(15) 0.0364(16) -0.0045(12) 0.0063(13) 0.0008(14) O3 0.0190(13) 0.073(2) 0.0251(14) 0.0074(14) -0.0059(11) 0.0011(14) N1 0.0221(14) 0.0239(15) 0.0088(12) -0.0003(10) -0.0057(11) 0.0009(12) N2 0.0304(17) 0.0431(19) 0.0078(12) -0.0004(13) -0.0050(11) -0.0009(15) N3 0.0292(17) 0.0405(19) 0.0107(13) 0.0013(12) -0.0046(12) -0.0007(15) N4 0.0227(14) 0.0221(15) 0.0088(12) -0.0007(10) -0.0031(10) 0.0019(12) N5 0.0183(14) 0.0317(16) 0.0126(12) 0.0042(12) 0.0018(10) -0.0018(12) C1 0.0229(17) 0.0243(17) 0.0129(15) 0.0018(13) -0.0030(13) -0.0045(14) C2 0.0215(17) 0.0295(19) 0.0140(15) 0.0001(13) -0.0054(13) -0.0046(15) C3 0.0249(17) 0.0199(16) 0.0111(14) 0.0017(11) -0.0031(12) 0.0035(14) C4 0.0291(18) 0.0250(19) 0.0118(14) 0.0029(13) 0.0001(13) -0.0075(15) C5 0.0243(17) 0.0262(19) 0.0133(15) 0.0049(13) -0.0035(13) -0.0057(15) C6 0.0268(18) 0.0306(19) 0.0122(15) 0.0027(13) -0.0038(14) 0.0002(15) C7 0.0266(18) 0.0283(19) 0.0104(15) -0.0022(13) -0.0011(13) -0.0010(15) C8 0.0237(17) 0.0181(16) 0.0128(15) 0.0001(11) -0.0049(13) -0.0007(13) C9 0.0264(18) 0.0279(19) 0.0118(14) -0.0034(13) 0.0003(13) 0.0049(15) C10 0.0222(17) 0.0241(18) 0.0137(15) -0.0013(13) -0.0046(12) 0.0047(15) C11 0.0195(16) 0.0237(17) 0.0143(15) -0.0024(12) -0.0011(12) 0.0029(14) C12 0.0202(16) 0.0233(17) 0.0161(15) 0.0001(13) -0.0051(13) 0.0028(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.181(3) . ? Ag1 N4 2.182(3) 1_454 ? O1 N5 1.260(4) . ? O2 N5 1.243(4) . ? O3 N5 1.247(3) . ? N1 C5 1.334(4) . ? N1 C1 1.342(4) . ? N2 C6 1.262(5) . ? N2 N3 1.409(4) . ? N3 C7 1.262(5) . ? N4 C10 1.336(4) . ? N4 C11 1.354(4) . ? N4 Ag1 2.182(3) 1_656 ? C1 C2 1.386(4) . ? C1 H1 0.91(4) . ? C2 C3 1.393(5) . ? C2 H2 0.89(4) . ? C3 C4 1.393(5) . ? C3 C6 1.469(4) . ? C4 C5 1.398(4) . ? C4 H3 0.88(4) . ? C5 H4 1.03(4) . ? C6 H5 0.92(5) . ? C7 C8 1.469(4) . ? C7 H6 0.87(4) . ? C8 C9 1.393(5) . ? C8 C12 1.393(5) . ? C9 C10 1.396(4) . ? C9 H7 0.95(4) . ? C10 H8 0.92(3) . ? C11 C12 1.376(4) . ? C11 H9 0.92(3) . ? C12 H10 1.00(4) . ? 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 N4 173.45(11) . 1_454 ? C5 N1 C1 118.3(3) . . ? C5 N1 Ag1 123.7(2) . . ? C1 N1 Ag1 117.9(2) . . ? C6 N2 N3 112.8(3) . . ? C7 N3 N2 113.5(3) . . ? C10 N4 C11 117.8(3) . . ? C10 N4 Ag1 123.5(2) . 1_656 ? C11 N4 Ag1 118.5(2) . 1_656 ? O2 N5 O3 121.7(3) . . ? O2 N5 O1 118.5(3) . . ? O3 N5 O1 119.9(3) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1 117(2) . . ? C2 C1 H1 121(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2 124(3) . . ? C3 C2 H2 116(3) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 C6 120.6(3) . . ? C2 C3 C6 121.4(3) . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H3 122(2) . . ? C5 C4 H3 119(2) . . ? N1 C5 C4 122.8(3) . . ? N1 C5 H4 116(2) . . ? C4 C5 H4 122(2) . . ? N2 C6 C3 120.6(3) . . ? N2 C6 H5 125(3) . . ? C3 C6 H5 114(3) . . ? N3 C7 C8 119.5(3) . . ? N3 C7 H6 123(3) . . ? C8 C7 H6 118(3) . . ? C9 C8 C12 117.6(3) . . ? C9 C8 C7 121.0(3) . . ? C12 C8 C7 121.4(3) . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H7 123(2) . . ? C10 C9 H7 118(2) . . ? N4 C10 C9 122.6(3) . . ? N4 C10 H8 117(2) . . ? C9 C10 H8 120(2) . . ? N4 C11 C12 122.9(3) . . ? N4 C11 H9 116(2) . . ? C12 C11 H9 121(2) . . ? C11 C12 C8 119.6(3) . . ? C11 C12 H10 116(2) . . ? C8 C12 H10 124(2) . . ? 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 N4 Ag1 N1 C5 -80.3(10) 1_454 . . . ? N4 Ag1 N1 C1 101.5(9) 1_454 . . . ? C6 N2 N3 C7 138.1(4) . . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Ag1 N1 C1 C2 178.7(3) . . . . ? N1 C1 C2 C3 -2.1(6) . . . . ? C1 C2 C3 C4 2.1(5) . . . . ? C1 C2 C3 C6 -177.6(3) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? C6 C3 C4 C5 179.0(3) . . . . ? C1 N1 C5 C4 1.0(5) . . . . ? Ag1 N1 C5 C4 -177.1(3) . . . . ? C3 C4 C5 N1 -0.9(6) . . . . ? N3 N2 C6 C3 177.8(3) . . . . ? C4 C3 C6 N2 168.9(4) . . . . ? C2 C3 C6 N2 -11.4(6) . . . . ? N2 N3 C7 C8 179.7(3) . . . . ? N3 C7 C8 C9 177.5(4) . . . . ? N3 C7 C8 C12 -2.6(6) . . . . ? C12 C8 C9 C10 0.3(5) . . . . ? C7 C8 C9 C10 -179.8(3) . . . . ? C11 N4 C10 C9 0.0(5) . . . . ? Ag1 N4 C10 C9 -175.0(3) 1_656 . . . ? C8 C9 C10 N4 -0.8(6) . . . . ? C10 N4 C11 C12 1.4(5) . . . . ? Ag1 N4 C11 C12 176.6(3) 1_656 . . . ? N4 C11 C12 C8 -1.9(6) . . . . ? C9 C8 C12 C11 1.0(5) . . . . ? C7 C8 C12 C11 -178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.525 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.111 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 1B - Ag(ligand1) ClO4------------------------------ #------------------------------------------------------------------------- data_paul2 _database_code_depnum_ccdc_archive 'CCDC 266719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Ag Cl N5 O4' _chemical_formula_weight 458.61 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' 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' 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 monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.0509(2) _cell_length_b 15.8105(4) _cell_length_c 8.6688(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.244(1) _cell_angle_gamma 90.00 _cell_volume 822.71(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4533 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3719 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1935 _reflns_number_gt 1694 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0330P)^2^+0.4188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1935 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.0000 0.5000 0.5000 0.02010(12) Uani 1 2 d S . . Cl1 Cl 0.92201(13) 0.2500 0.49044(8) 0.02105(18) Uani 1 2 d S . . N1 N 0.2728(3) 0.48892(10) 0.3640(2) 0.0170(4) Uani 1 1 d . . . N2 N 0.9120(3) 0.51539(11) 0.0384(2) 0.0187(4) Uani 1 1 d . . . N3 N 0.3360(6) 0.7500 0.0710(4) 0.0417(8) Uani 1 2 d S . . O1 O 0.9598(4) 0.2500 0.3294(3) 0.0307(5) Uani 1 2 d S . . O2 O 0.6858(3) 0.2500 0.5011(3) 0.0290(5) Uani 1 2 d S . . O3 O 1.0228(3) 0.32429(9) 0.5667(2) 0.0280(4) Uani 1 1 d . . . C1 C 0.3522(3) 0.41197(13) 0.3352(2) 0.0211(4) Uani 1 1 d . . . H1 H 0.2841 0.3638 0.3746 0.025 Uiso 1 1 calc R . . C2 C 0.5283(3) 0.39995(13) 0.2508(2) 0.0205(4) Uani 1 1 d . . . H2 H 0.5777 0.3444 0.2315 0.025 Uiso 1 1 calc R . . C3 C 0.6332(3) 0.46973(13) 0.1942(2) 0.0169(4) Uani 1 1 d . . . C4 C 0.5510(3) 0.54988(13) 0.2246(2) 0.0188(4) Uani 1 1 d . . . H4 H 0.6172 0.5992 0.1878 0.023 Uiso 1 1 calc R . . C5 C 0.3735(3) 0.55668(13) 0.3084(2) 0.0188(4) Uani 1 1 d . . . H5 H 0.3192 0.6115 0.3281 0.023 Uiso 1 1 calc R . . C6 C 0.8214(3) 0.45523(12) 0.1068(2) 0.0184(4) Uani 1 1 d . . . H6 H 0.8781 0.3995 0.1007 0.022 Uiso 1 1 calc R . . C7 C 0.1474(7) 0.7500 0.0661(4) 0.0347(8) Uani 1 2 d S . . C8 C -0.0949(7) 0.7500 0.0566(5) 0.0372(8) Uani 1 2 d S . . H8A H -0.140(8) 0.7500 0.146(6) 0.056 Uiso 1 2 d S . . H8B H -0.153(5) 0.706(2) -0.002(4) 0.056 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01639(15) 0.02543(15) 0.02042(15) -0.00057(8) 0.00984(9) 0.00048(8) Cl1 0.0238(4) 0.0152(3) 0.0264(4) 0.000 0.0119(3) 0.000 N1 0.0140(8) 0.0221(9) 0.0161(8) -0.0008(6) 0.0063(7) 0.0004(6) N2 0.0128(8) 0.0255(9) 0.0194(9) -0.0028(7) 0.0083(7) 0.0021(7) N3 0.046(2) 0.0321(16) 0.0458(19) 0.000 0.0017(15) 0.000 O1 0.0375(13) 0.0313(12) 0.0263(12) 0.000 0.0155(10) 0.000 O2 0.0214(11) 0.0286(11) 0.0395(13) 0.000 0.0131(9) 0.000 O3 0.0323(9) 0.0173(7) 0.0363(9) -0.0027(7) 0.0120(7) -0.0056(6) C1 0.0213(10) 0.0189(9) 0.0248(10) 0.0021(8) 0.0096(8) -0.0022(8) C2 0.0215(10) 0.0169(9) 0.0245(10) -0.0004(8) 0.0080(8) 0.0015(8) C3 0.0144(9) 0.0212(9) 0.0155(9) -0.0011(8) 0.0032(7) -0.0006(8) C4 0.0190(9) 0.0194(10) 0.0194(9) -0.0002(8) 0.0078(8) -0.0017(8) C5 0.0184(9) 0.0174(9) 0.0218(10) -0.0001(8) 0.0074(8) 0.0005(8) C6 0.0165(9) 0.0195(10) 0.0201(10) -0.0013(8) 0.0058(7) 0.0009(8) C7 0.053(2) 0.0213(16) 0.0299(18) 0.000 0.0061(16) 0.000 C8 0.046(2) 0.0283(18) 0.038(2) 0.000 0.0102(17) 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 Ag1 N1 2.1532(18) 3_566 ? Ag1 N1 2.1532(18) . ? Cl1 O1 1.443(2) . ? Cl1 O2 1.444(2) . ? Cl1 O3 1.4447(15) . ? Cl1 O3 1.4447(15) 4_565 ? N1 C1 1.343(3) . ? N1 C5 1.351(3) . ? N2 C6 1.280(3) . ? N2 N2 1.413(4) 3_765 ? N3 C7 1.137(5) . ? C1 C2 1.379(3) . ? C1 H1 0.9500 . ? C2 C3 1.393(3) . ? C2 H2 0.9500 . ? C3 C4 1.399(3) . ? C3 C6 1.463(3) . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.458(6) . ? C8 H8A 0.85(5) . ? C8 H8B 0.91(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.0 3_566 . ? O1 Cl1 O2 109.93(14) . . ? O1 Cl1 O3 109.49(9) . . ? O2 Cl1 O3 109.56(9) . . ? O1 Cl1 O3 109.49(9) . 4_565 ? O2 Cl1 O3 109.56(9) . 4_565 ? O3 Cl1 O3 108.79(14) . 4_565 ? C1 N1 C5 117.65(18) . . ? C1 N1 Ag1 119.50(13) . . ? C5 N1 Ag1 122.83(13) . . ? C6 N2 N2 110.8(2) . 3_765 ? N1 C1 C2 122.80(19) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.66(19) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 117.51(18) . . ? C2 C3 C6 118.53(18) . . ? C4 C3 C6 123.95(19) . . ? C5 C4 C3 119.41(19) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.96(19) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C3 122.00(19) . . ? N2 C6 H6 119.0 . . ? C3 C6 H6 119.0 . . ? N3 C7 C8 178.9(4) . . ? C7 C8 H8A 113(3) . . ? C7 C8 H8B 110(2) . . ? H8A C8 H8B 112(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 -0.7(3) . . . . ? Ag1 N1 C1 C2 -179.12(16) . . . . ? N1 C1 C2 C3 1.1(3) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C1 C2 C3 C6 179.20(18) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C6 C3 C4 C5 -179.77(19) . . . . ? C1 N1 C5 C4 0.1(3) . . . . ? Ag1 N1 C5 C4 178.45(15) . . . . ? C3 C4 C5 N1 0.1(3) . . . . ? N2 N2 C6 C3 -179.5(2) 3_765 . . . ? C2 C3 C6 N2 173.0(2) . . . . ? C4 C3 C6 N2 -6.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.532 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.081 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 2A - Ag(ligand2) BF4------------------------------ #------------------------------------------------------------------------- data_jen2sort _database_code_depnum_ccdc_archive 'CCDC 266720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Ag B F4 N5' _chemical_formula_weight 445.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5292(2) _cell_length_b 9.7601(3) _cell_length_c 11.8669(4) _cell_angle_alpha 75.444(1) _cell_angle_beta 74.672(1) _cell_angle_gamma 83.659(2) _cell_volume 813.13(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14037 _cell_measurement_theta_min 0.34 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; Exptl_absorpt_process_details multi-scan from symmetry-related measurements (Blessing 1995) ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15331 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.32 _reflns_number_total 3634 _reflns_number_gt 3007 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.3124P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3634 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.78610(3) 0.01755(2) 0.525055(17) 0.02508(8) Uani 1 d . . . F1 F 0.5196(2) 0.46959(19) 0.2217(2) 0.0678(6) Uani 1 d . . . F2 F 0.8251(2) 0.49676(16) 0.17451(14) 0.0388(4) Uani 1 d . . . F3 F 0.7115(2) 0.31405(16) 0.13319(14) 0.0448(4) Uani 1 d . . . F4 F 0.6973(3) 0.3151(2) 0.32468(15) 0.0600(5) Uani 1 d . . . N1 N 0.6811(2) -0.0886(2) 0.41923(17) 0.0186(4) Uani 1 d . . . N2 N 0.8598(2) 0.1649(2) 0.61045(17) 0.0189(4) Uani 1 d . . . N3 N 0.5114(3) -0.0517(2) 0.05168(16) 0.0189(4) Uani 1 d . . . N4 N 0.9843(3) 0.0178(2) 0.94203(16) 0.0206(5) Uani 1 d . . . N5 N 0.8092(3) -0.2081(2) 0.6933(2) 0.0393(6) Uani 1 d . . . C1 C 0.6488(3) -0.0186(3) 0.3135(2) 0.0179(5) Uani 1 d . . . C2 C 0.5976(3) -0.0839(2) 0.2367(2) 0.0160(5) Uani 1 d . . . C3 C 0.5832(3) -0.2307(3) 0.2700(2) 0.0192(5) Uani 1 d . . . C4 C 0.6150(3) -0.3033(3) 0.3791(2) 0.0214(5) Uani 1 d . . . C5 C 0.6611(3) -0.2297(3) 0.4512(2) 0.0214(6) Uani 1 d . . . C6 C 0.5648(3) 0.0036(3) 0.1236(2) 0.0169(5) Uani 1 d . . . C7 C 0.8903(3) 0.1191(3) 0.7197(2) 0.0185(5) Uani 1 d . . . C8 C 0.9092(3) 0.2083(2) 0.7899(2) 0.0182(5) Uani 1 d . . . C9 C 0.8914(3) 0.3534(3) 0.7443(2) 0.0223(6) Uani 1 d . . . C10 C 0.8607(3) 0.4015(3) 0.6309(2) 0.0249(6) Uani 1 d . . . C11 C 0.8471(3) 0.3066(3) 0.5658(2) 0.0226(6) Uani 1 d . . . C12 C 0.9469(3) 0.1505(3) 0.9084(2) 0.0196(5) Uani 1 d . . . C13 C 0.7853(4) -0.2673(3) 0.7913(2) 0.0271(6) Uani 1 d . . . C14 C 0.7524(5) -0.3419(4) 0.9174(3) 0.0357(7) Uani 1 d . . . B1 B 0.6886(4) 0.3994(3) 0.2136(3) 0.0259(7) Uani 1 d . . . H1 H 0.666(3) 0.077(3) 0.291(2) 0.020(6) Uiso 1 d . . . H2 H 0.550(3) -0.274(3) 0.223(2) 0.021(7) Uiso 1 d . . . H3 H 0.607(3) -0.402(3) 0.402(2) 0.017(6) Uiso 1 d . . . H4 H 0.679(3) -0.273(2) 0.527(2) 0.010(6) Uiso 1 d . . . H5 H 0.586(3) 0.102(3) 0.106(2) 0.019(6) Uiso 1 d . . . H6 H 0.901(3) 0.024(3) 0.750(2) 0.014(6) Uiso 1 d . . . H7 H 0.904(3) 0.415(3) 0.790(2) 0.026(7) Uiso 1 d . . . H8 H 0.852(3) 0.493(3) 0.602(2) 0.016(6) Uiso 1 d . . . H9 H 0.826(3) 0.337(2) 0.489(2) 0.016(6) Uiso 1 d . . . H10 H 0.936(3) 0.211(2) 0.957(2) 0.015(6) Uiso 1 d . . . H11 H 0.657(4) -0.412(4) 0.938(3) 0.060(10) Uiso 1 d . . . H12 H 0.859(4) -0.387(3) 0.931(3) 0.051(10) Uiso 1 d . . . H13 H 0.704(5) -0.279(4) 0.967(3) 0.073(12) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02433(12) 0.03511(13) 0.02135(11) -0.01299(8) -0.00957(8) -0.00002(8) F1 0.0305(10) 0.0437(11) 0.142(2) -0.0457(12) -0.0233(11) 0.0044(8) F2 0.0350(9) 0.0364(9) 0.0469(10) -0.0109(8) -0.0079(8) -0.0119(7) F3 0.0749(12) 0.0318(9) 0.0325(9) -0.0165(7) -0.0099(9) -0.0092(9) F4 0.0942(15) 0.0598(12) 0.0301(10) 0.0034(9) -0.0246(10) -0.0299(11) N1 0.0180(10) 0.0245(11) 0.0154(11) -0.0050(9) -0.0075(8) 0.0000(8) N2 0.0170(10) 0.0240(11) 0.0167(11) -0.0039(9) -0.0060(8) -0.0016(9) N3 0.0228(11) 0.0196(11) 0.0146(10) -0.0013(8) -0.0069(9) -0.0026(9) N4 0.0223(11) 0.0288(12) 0.0122(10) -0.0048(9) -0.0068(9) -0.0010(9) N5 0.0584(17) 0.0297(14) 0.0320(15) -0.0022(11) -0.0186(12) -0.0046(12) C1 0.0171(12) 0.0192(14) 0.0173(13) -0.0037(10) -0.0050(10) 0.0006(10) C2 0.0123(11) 0.0200(13) 0.0148(12) -0.0037(10) -0.0025(9) -0.0004(9) C3 0.0165(12) 0.0230(14) 0.0205(13) -0.0075(11) -0.0061(10) -0.0019(10) C4 0.0226(13) 0.0155(13) 0.0251(14) -0.0013(11) -0.0079(11) -0.0002(11) C5 0.0213(13) 0.0248(14) 0.0159(13) -0.0002(11) -0.0066(11) 0.0031(11) C6 0.0142(12) 0.0185(13) 0.0178(13) -0.0040(10) -0.0033(10) -0.0018(10) C7 0.0186(12) 0.0197(14) 0.0177(13) -0.0024(10) -0.0067(10) -0.0017(10) C8 0.0136(11) 0.0231(13) 0.0178(12) -0.0036(10) -0.0039(9) -0.0031(10) C9 0.0223(13) 0.0231(14) 0.0232(14) -0.0090(11) -0.0047(11) -0.0012(11) C10 0.0242(14) 0.0195(14) 0.0276(15) 0.0005(12) -0.0065(11) -0.0008(11) C11 0.0206(13) 0.0279(15) 0.0167(13) 0.0018(11) -0.0073(11) -0.0006(11) C12 0.0200(13) 0.0250(14) 0.0158(13) -0.0088(11) -0.0039(10) -0.0015(11) C13 0.0346(15) 0.0213(14) 0.0310(16) -0.0098(12) -0.0155(13) 0.0021(12) C14 0.046(2) 0.0388(19) 0.0208(15) -0.0064(13) -0.0097(14) 0.0086(16) B1 0.0305(17) 0.0222(16) 0.0265(17) -0.0067(13) -0.0075(13) -0.0039(13) _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 2.1471(19) . ? Ag1 N1 2.1529(19) . ? Ag1 N5 2.600(2) . ? Ag1 Ag1 3.1131(4) 2_756 ? F1 B1 1.369(3) . ? F2 B1 1.385(3) . ? F3 B1 1.384(3) . ? F4 B1 1.381(3) . ? N1 C1 1.339(3) . ? N1 C5 1.347(3) . ? N2 C7 1.333(3) . ? N2 C11 1.354(3) . ? N3 C6 1.282(3) . ? N3 N3 1.415(4) 2_655 ? N4 C12 1.278(3) . ? N4 N4 1.409(4) 2_757 ? N5 C13 1.136(3) . ? C1 C2 1.385(3) . ? C1 H1 0.92(2) . ? C2 C3 1.396(3) . ? C2 C6 1.464(3) . ? C3 C4 1.378(3) . ? C3 H2 0.87(2) . ? C4 C5 1.375(3) . ? C4 H3 0.94(2) . ? C5 H4 0.93(2) . ? C6 H5 0.95(2) . ? C7 C8 1.388(3) . ? C7 H6 0.91(2) . ? C8 C9 1.389(3) . ? C8 C12 1.467(3) . ? C9 C10 1.381(3) . ? C9 H7 0.93(3) . ? C10 C11 1.374(4) . ? C10 H8 0.88(2) . ? C11 H9 0.94(2) . ? C12 H10 0.91(2) . ? C13 C14 1.458(4) . ? C14 H11 0.99(3) . ? C14 H12 0.91(3) . ? C14 H13 0.94(4) . ? 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 N1 167.03(7) . . ? N2 Ag1 N5 96.73(7) . . ? N1 Ag1 N5 95.03(7) . . ? N2 Ag1 Ag1 75.65(5) . 2_756 ? N1 Ag1 Ag1 111.57(5) . 2_756 ? N5 Ag1 Ag1 81.70(6) . 2_756 ? C1 N1 C5 117.4(2) . . ? C1 N1 Ag1 120.93(16) . . ? C5 N1 Ag1 121.43(16) . . ? C7 N2 C11 117.9(2) . . ? C7 N2 Ag1 119.59(16) . . ? C11 N2 Ag1 121.66(16) . . ? C6 N3 N3 111.2(2) . 2_655 ? C12 N4 N4 111.7(2) . 2_757 ? C13 N5 Ag1 152.4(2) . . ? N1 C1 C2 123.4(2) . . ? N1 C1 H1 117.0(15) . . ? C2 C1 H1 119.6(15) . . ? C1 C2 C3 118.2(2) . . ? C1 C2 C6 118.6(2) . . ? C3 C2 C6 123.2(2) . . ? C4 C3 C2 118.7(2) . . ? C4 C3 H2 121.3(16) . . ? C2 C3 H2 119.9(16) . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H3 121.3(14) . . ? C3 C4 H3 119.4(14) . . ? N1 C5 C4 123.0(2) . . ? N1 C5 H4 114.3(14) . . ? C4 C5 H4 122.7(14) . . ? N3 C6 C2 120.7(2) . . ? N3 C6 H5 122.1(14) . . ? C2 C6 H5 117.2(14) . . ? N2 C7 C8 123.7(2) . . ? N2 C7 H6 118.5(15) . . ? C8 C7 H6 117.8(15) . . ? C7 C8 C9 117.9(2) . . ? C7 C8 C12 120.8(2) . . ? C9 C8 C12 121.3(2) . . ? C10 C9 C8 118.6(2) . . ? C10 C9 H7 122.0(16) . . ? C8 C9 H7 119.3(16) . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H8 121.7(16) . . ? C9 C10 H8 118.2(16) . . ? N2 C11 C10 121.7(2) . . ? N2 C11 H9 116.6(14) . . ? C10 C11 H9 121.7(14) . . ? N4 C12 C8 119.9(2) . . ? N4 C12 H10 122.7(15) . . ? C8 C12 H10 117.4(15) . . ? N5 C13 C14 179.2(3) . . ? C13 C14 H11 111.2(18) . . ? C13 C14 H12 108.9(19) . . ? H11 C14 H12 110(3) . . ? C13 C14 H13 110(2) . . ? H11 C14 H13 104(3) . . ? H12 C14 H13 112(3) . . ? F1 B1 F4 109.6(2) . . ? F1 B1 F3 108.8(2) . . ? F4 B1 F3 108.8(2) . . ? F1 B1 F2 109.5(2) . . ? F4 B1 F2 109.9(2) . . ? F3 B1 F2 110.1(2) . . ? 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 N1 C1 27.5(4) . . . . ? N5 Ag1 N1 C1 -177.47(17) . . . . ? Ag1 Ag1 N1 C1 -94.41(17) 2_756 . . . ? N2 Ag1 N1 C5 -158.5(3) . . . . ? N5 Ag1 N1 C5 -3.45(18) . . . . ? Ag1 Ag1 N1 C5 79.60(17) 2_756 . . . ? N1 Ag1 N2 C7 152.2(3) . . . . ? N5 Ag1 N2 C7 -2.69(18) . . . . ? Ag1 Ag1 N2 C7 -82.31(16) 2_756 . . . ? N1 Ag1 N2 C11 -16.7(4) . . . . ? N5 Ag1 N2 C11 -171.62(17) . . . . ? Ag1 Ag1 N2 C11 108.76(17) 2_756 . . . ? N2 Ag1 N5 C13 42.1(5) . . . . ? N1 Ag1 N5 C13 -132.5(5) . . . . ? Ag1 Ag1 N5 C13 116.4(5) 2_756 . . . ? C5 N1 C1 C2 -0.4(3) . . . . ? Ag1 N1 C1 C2 173.87(17) . . . . ? N1 C1 C2 C3 -1.5(3) . . . . ? N1 C1 C2 C6 179.6(2) . . . . ? C1 C2 C3 C4 1.9(3) . . . . ? C6 C2 C3 C4 -179.3(2) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C1 N1 C5 C4 1.9(3) . . . . ? Ag1 N1 C5 C4 -172.28(18) . . . . ? C3 C4 C5 N1 -1.5(4) . . . . ? N3 N3 C6 C2 -179.9(2) 2_655 . . . ? C1 C2 C6 N3 -177.7(2) . . . . ? C3 C2 C6 N3 3.5(3) . . . . ? C11 N2 C7 C8 0.1(3) . . . . ? Ag1 N2 C7 C8 -169.22(17) . . . . ? N2 C7 C8 C9 1.4(3) . . . . ? N2 C7 C8 C12 -178.6(2) . . . . ? C7 C8 C9 C10 -1.6(3) . . . . ? C12 C8 C9 C10 178.3(2) . . . . ? C8 C9 C10 C11 0.4(4) . . . . ? C7 N2 C11 C10 -1.4(3) . . . . ? Ag1 N2 C11 C10 167.70(18) . . . . ? C9 C10 C11 N2 1.1(4) . . . . ? N4 N4 C12 C8 -179.8(2) 2_757 . . . ? C7 C8 C12 N4 8.3(3) . . . . ? C9 C8 C12 N4 -171.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.508 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.087 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 2B - Ag(ligand2)ClO4 ---------------------------- #------------------------------------------------------------------------- data_again _database_code_depnum_ccdc_archive 'CCDC 266721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Ag Cl N5 O4' _chemical_formula_weight 458.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3202(4) _cell_length_b 14.2960(6) _cell_length_c 13.2368(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.178(2) _cell_angle_gamma 90.00 _cell_volume 1655.45(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7401 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3781 _reflns_number_gt 2784 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0279P)^2^+1.2584P] 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 3781 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.20050(2) 0.002029(14) 0.105184(17) 0.02763(8) Uani 1 1 d . . . Cl1 Cl 0.85576(8) 0.13894(5) 0.17036(6) 0.02607(15) Uani 1 1 d . . . O1 O 0.8089(4) 0.14747(18) 0.2604(2) 0.0695(9) Uani 1 1 d . . . O2 O 0.7549(3) 0.07563(17) 0.0932(2) 0.0575(7) Uani 1 1 d . . . O3 O 1.0068(2) 0.10077(15) 0.20161(19) 0.0415(6) Uani 1 1 d . . . O4 O 0.8526(3) 0.22899(14) 0.12103(18) 0.0415(6) Uani 1 1 d . . . N1 N 0.2770(2) 0.13732(15) 0.07283(17) 0.0218(5) Uani 1 1 d . . . N2 N 0.2301(3) 0.47015(16) 0.09034(18) 0.0227(5) Uani 1 1 d . . . N3 N 0.1420(3) 0.53813(16) 0.11956(18) 0.0246(5) Uani 1 1 d . . . N4 N 0.1073(3) 0.87160(15) 0.13657(17) 0.0226(5) Uani 1 1 d . . . N5 N 0.5157(3) 0.07238(19) 0.8314(2) 0.0384(6) Uani 1 1 d . . . C1 C 0.3933(3) 0.14508(19) 0.0348(2) 0.0241(6) Uani 1 1 d . . . H1 H 0.4406 0.0897 0.0220 0.029 Uiso 1 1 calc R . . C2 C 0.4463(3) 0.2305(2) 0.0138(2) 0.0267(6) Uani 1 1 d . . . H2 H 0.5278 0.2332 -0.0137 0.032 Uiso 1 1 calc R . . C3 C 0.3802(3) 0.31201(18) 0.0330(2) 0.0227(6) Uani 1 1 d . . . H3 H 0.4151 0.3713 0.0187 0.027 Uiso 1 1 calc R . . C4 C 0.2611(3) 0.30540(17) 0.07399(19) 0.0183(5) Uani 1 1 d . . . C5 C 0.2132(3) 0.21715(18) 0.0915(2) 0.0203(6) Uani 1 1 d . . . H5 H 0.1310 0.2126 0.1182 0.024 Uiso 1 1 calc R . . C6 C 0.1860(3) 0.38697(18) 0.0995(2) 0.0200(6) Uani 1 1 d . . . H6 H 0.1021 0.3780 0.1236 0.024 Uiso 1 1 calc R . . C7 C 0.1936(3) 0.62039(18) 0.1144(2) 0.0218(6) Uani 1 1 d . . . H7 H 0.2822 0.6277 0.0952 0.026 Uiso 1 1 calc R . . C8 C 0.1179(3) 0.70356(18) 0.1377(2) 0.0205(6) Uani 1 1 d . . . C9 C -0.0058(3) 0.69932(19) 0.1740(2) 0.0222(6) Uani 1 1 d . . . H9 H -0.0443 0.6408 0.1870 0.027 Uiso 1 1 calc R . . C10 C -0.0715(3) 0.78253(18) 0.1907(2) 0.0226(6) Uani 1 1 d . . . H10 H -0.1555 0.7816 0.2158 0.027 Uiso 1 1 calc R . . C11 C -0.0136(3) 0.86610(19) 0.1707(2) 0.0233(6) Uani 1 1 d . . . H11 H -0.0605 0.9225 0.1812 0.028 Uiso 1 1 calc R . . C12 C 0.1715(3) 0.79082(19) 0.1218(2) 0.0228(6) Uani 1 1 d . . . H12 H 0.2579 0.7937 0.0994 0.027 Uiso 1 1 calc R . . C13 C 0.4095(4) 0.0650(2) 0.7571(2) 0.0283(7) Uani 1 1 d . . . C14 C 0.2747(4) 0.0565(2) 0.6602(2) 0.0360(7) Uani 1 1 d . . . H14A H 0.2308 0.1186 0.6378 0.054 Uiso 1 1 calc R . . H14B H 0.1988 0.0167 0.6752 0.054 Uiso 1 1 calc R . . H14C H 0.3037 0.0285 0.6025 0.054 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 0.03729(13) 0.01377(10) 0.03540(13) 0.00131(10) 0.01709(10) -0.00078(10) Cl1 0.0271(3) 0.0225(3) 0.0327(4) 0.0010(3) 0.0156(3) 0.0033(3) O1 0.121(3) 0.0478(16) 0.0752(18) 0.0080(14) 0.0797(19) 0.0193(16) O2 0.0357(14) 0.0429(15) 0.0799(18) -0.0175(13) 0.0022(13) -0.0080(11) O3 0.0287(12) 0.0332(12) 0.0624(15) 0.0044(11) 0.0152(11) 0.0058(10) O4 0.0484(14) 0.0268(12) 0.0506(14) 0.0116(10) 0.0186(12) 0.0062(10) N1 0.0259(12) 0.0165(11) 0.0231(11) 0.0018(9) 0.0087(10) 0.0017(9) N2 0.0278(13) 0.0158(11) 0.0251(12) -0.0007(9) 0.0098(10) -0.0002(9) N3 0.0281(13) 0.0176(11) 0.0280(13) 0.0000(10) 0.0095(11) 0.0026(10) N4 0.0296(13) 0.0145(11) 0.0247(12) -0.0001(9) 0.0108(10) -0.0007(9) N5 0.0378(16) 0.0410(16) 0.0389(16) 0.0014(13) 0.0164(14) 0.0055(13) C1 0.0236(14) 0.0215(14) 0.0298(15) -0.0018(12) 0.0126(12) 0.0025(12) C2 0.0237(14) 0.0287(16) 0.0306(15) 0.0010(12) 0.0131(13) 0.0010(12) C3 0.0245(14) 0.0181(13) 0.0259(14) 0.0009(11) 0.0092(12) -0.0019(11) C4 0.0202(13) 0.0152(12) 0.0181(13) 0.0005(10) 0.0047(11) 0.0017(10) C5 0.0197(14) 0.0179(13) 0.0224(14) -0.0002(11) 0.0064(11) 0.0019(11) C6 0.0231(15) 0.0170(13) 0.0197(13) -0.0002(10) 0.0071(11) -0.0005(11) C7 0.0258(15) 0.0171(13) 0.0215(14) 0.0016(11) 0.0069(12) 0.0028(11) C8 0.0253(14) 0.0155(13) 0.0179(13) 0.0002(10) 0.0039(11) -0.0005(11) C9 0.0279(15) 0.0171(13) 0.0194(13) -0.0011(11) 0.0055(11) -0.0019(11) C10 0.0235(14) 0.0229(14) 0.0224(13) -0.0021(11) 0.0092(12) -0.0003(11) C11 0.0293(15) 0.0183(13) 0.0237(14) 0.0001(11) 0.0109(12) 0.0048(12) C12 0.0283(15) 0.0184(13) 0.0222(14) -0.0004(11) 0.0092(12) 0.0023(11) C13 0.0393(18) 0.0208(14) 0.0331(17) -0.0003(13) 0.0231(15) 0.0028(13) C14 0.045(2) 0.0285(17) 0.0363(17) 0.0019(14) 0.0158(15) -0.0020(15) _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 2.155(2) . ? Ag1 N4 2.157(2) 1_545 ? Cl1 O1 1.409(2) . ? Cl1 O3 1.431(2) . ? Cl1 O4 1.439(2) . ? Cl1 O2 1.443(2) . ? N1 C1 1.348(3) . ? N1 C5 1.349(3) . ? N2 C6 1.278(3) . ? N2 N3 1.410(3) . ? N3 C7 1.281(3) . ? N4 C12 1.346(3) . ? N4 C11 1.353(3) . ? N4 Ag1 2.157(2) 1_565 ? N5 C13 1.135(4) . ? C1 C2 1.380(4) . ? C1 H1 0.9500 . ? C2 C3 1.382(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 C6 1.459(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.469(4) . ? C7 H7 0.9500 . ? C8 C12 1.386(4) . ? C8 C9 1.395(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.374(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.458(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N4 175.56(8) . 1_545 ? O1 Cl1 O3 110.43(17) . . ? O1 Cl1 O4 110.04(14) . . ? O3 Cl1 O4 109.65(13) . . ? O1 Cl1 O2 109.67(17) . . ? O3 Cl1 O2 107.52(14) . . ? O4 Cl1 O2 109.49(15) . . ? C1 N1 C5 117.5(2) . . ? C1 N1 Ag1 120.79(17) . . ? C5 N1 Ag1 121.74(17) . . ? C6 N2 N3 112.3(2) . . ? C7 N3 N2 110.7(2) . . ? C12 N4 C11 117.5(2) . . ? C12 N4 Ag1 119.02(18) . 1_565 ? C11 N4 Ag1 123.48(18) . 1_565 ? N1 C1 C2 122.5(2) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.6(2) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.2(2) . . ? C5 C4 C6 118.8(2) . . ? C3 C4 C6 123.0(2) . . ? N1 C5 C4 123.5(2) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C4 121.8(2) . . ? N2 C6 H6 119.1 . . ? C4 C6 H6 119.1 . . ? N3 C7 C8 121.0(3) . . ? N3 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C12 C8 C9 118.4(2) . . ? C12 C8 C7 118.2(2) . . ? C9 C8 C7 123.5(2) . . ? C10 C9 C8 118.7(2) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 119.3(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N4 C11 C10 122.9(2) . . ? N4 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N4 C12 C8 123.3(3) . . ? N4 C12 H12 118.4 . . ? C8 C12 H12 118.4 . . ? N5 C13 C14 178.8(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 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 N4 Ag1 N1 C1 -158.5(10) 1_545 . . . ? N4 Ag1 N1 C5 22.9(11) 1_545 . . . ? C6 N2 N3 C7 176.9(2) . . . . ? C5 N1 C1 C2 -0.8(4) . . . . ? Ag1 N1 C1 C2 -179.5(2) . . . . ? N1 C1 C2 C3 0.7(4) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C2 C3 C4 C6 178.5(2) . . . . ? C1 N1 C5 C4 -0.1(4) . . . . ? Ag1 N1 C5 C4 178.59(19) . . . . ? C3 C4 C5 N1 1.1(4) . . . . ? C6 C4 C5 N1 -178.6(2) . . . . ? N3 N2 C6 C4 -179.8(2) . . . . ? C5 C4 C6 N2 176.4(2) . . . . ? C3 C4 C6 N2 -3.3(4) . . . . ? N2 N3 C7 C8 178.0(2) . . . . ? N3 C7 C8 C12 -174.6(2) . . . . ? N3 C7 C8 C9 4.8(4) . . . . ? C12 C8 C9 C10 1.2(4) . . . . ? C7 C8 C9 C10 -178.3(2) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C12 N4 C11 C10 0.2(4) . . . . ? Ag1 N4 C11 C10 -179.8(2) 1_565 . . . ? C9 C10 C11 N4 -1.1(4) . . . . ? C11 N4 C12 C8 1.4(4) . . . . ? Ag1 N4 C12 C8 -178.62(19) 1_565 . . . ? C9 C8 C12 N4 -2.1(4) . . . . ? C7 C8 C12 N4 177.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.502 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.079 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 3A - Ag(ligand3) dimer ---------------------------- #------------------------------------------------------------------------- data_jen1 _database_code_depnum_ccdc_archive 'CCDC 266722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 Ag2 N10 O6' _chemical_formula_weight 760.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0933(2) _cell_length_b 8.8628(3) _cell_length_c 9.3988(4) _cell_angle_alpha 89.868(2) _cell_angle_beta 82.849(2) _cell_angle_gamma 72.614(2) _cell_volume 637.93(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 26083 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 1.599 _exptl_absorpt_correction_type multiscan _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi & omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17254 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.43 _reflns_number_total 2893 _reflns_number_gt 2520 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.2033P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2893 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.25574(2) 0.51102(2) 0.33581(2) 0.02411(8) Uani 1 d . . . O1 O 0.0582(3) 0.1186(2) 0.1800(2) 0.0402(5) Uani 1 d . . . O2 O 0.0996(3) 0.2820(2) 0.3301(2) 0.0383(5) Uani 1 d . . . O3 O -0.0674(2) 0.3682(2) 0.1664(2) 0.0378(5) Uani 1 d . . . N1 N 0.4269(2) 0.3323(2) 0.4636(2) 0.0208(4) Uani 1 d . . . N2 N 0.1243(2) 0.2332(2) 0.7265(2) 0.0201(4) Uani 1 d . . . N3 N -0.0587(2) 0.2913(2) 0.7610(2) 0.0186(4) Uani 1 d . . . N4 N -0.4114(2) 0.3721(2) 0.8498(2) 0.0185(4) Uani 1 d . . . N5 N 0.0292(2) 0.2561(2) 0.2255(2) 0.0213(4) Uani 1 d . . . C1 C 0.6001(3) 0.2867(3) 0.4159(3) 0.0256(6) Uani 1 d . . . H1 H 0.638(3) 0.348(3) 0.331(3) 0.018(6) Uiso 1 d . . . C2 C 0.7198(3) 0.1657(3) 0.4751(3) 0.0255(6) Uani 1 d . . . H2 H 0.829(4) 0.147(3) 0.435(3) 0.026(7) Uiso 1 d . . . C3 C 0.6632(3) 0.0863(3) 0.5881(3) 0.0234(5) Uani 1 d . . . H3 H 0.744(3) -0.006(3) 0.627(3) 0.027(7) Uiso 1 d . . . C4 C 0.4866(3) 0.1313(3) 0.6381(3) 0.0214(5) Uani 1 d . . . H4 H 0.438(3) 0.078(3) 0.718(3) 0.019(6) Uiso 1 d . . . C5 C 0.3723(3) 0.2539(3) 0.5741(3) 0.0183(5) Uani 1 d . . . C6 C 0.1836(3) 0.3058(3) 0.6248(3) 0.0188(5) Uani 1 d . . . H6 H 0.113(3) 0.387(3) 0.584(3) 0.017(6) Uiso 1 d . . . C7 C -0.1135(3) 0.2234(3) 0.8692(3) 0.0186(5) Uani 1 d . . . H7 H -0.039(3) 0.146(3) 0.918(3) 0.015(6) Uiso 1 d . . . C8 C -0.3018(3) 0.2588(3) 0.9181(3) 0.0187(5) Uani 1 d . . . C9 C -0.3591(3) 0.1734(3) 1.0264(3) 0.0237(5) Uani 1 d . . . H9 H -0.277(3) 0.092(3) 1.071(3) 0.023(7) Uiso 1 d . . . C10 C -0.5377(3) 0.2043(3) 1.0655(3) 0.0261(6) Uani 1 d . . . H10 H -0.579(4) 0.148(4) 1.135(3) 0.037(8) Uiso 1 d . . . C11 C -0.6511(3) 0.3183(3) 0.9951(3) 0.0234(5) Uani 1 d . . . H11 H -0.775(4) 0.347(3) 1.024(3) 0.026(7) Uiso 1 d . . . C12 C -0.5829(3) 0.3998(3) 0.8893(3) 0.0210(5) Uani 1 d . . . H12 H -0.657(4) 0.485(3) 0.841(3) 0.025 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01927(10) 0.02412(12) 0.02660(12) 0.00882(8) -0.00503(8) -0.00225(8) O1 0.0594(13) 0.0220(10) 0.0398(12) 0.0006(9) -0.0203(10) -0.0076(9) O2 0.0564(13) 0.0336(11) 0.0328(11) 0.0062(9) -0.0233(10) -0.0185(10) O3 0.0278(10) 0.0298(11) 0.0490(13) 0.0067(9) -0.0141(9) 0.0051(8) N1 0.0182(9) 0.0221(11) 0.0210(11) 0.0041(9) -0.0042(8) -0.0038(8) N2 0.0139(9) 0.0209(11) 0.0241(11) 0.0010(9) -0.0023(8) -0.0030(8) N3 0.0141(9) 0.0177(10) 0.0218(11) 0.0012(8) -0.0037(8) -0.0012(8) N4 0.0170(9) 0.0174(10) 0.0200(10) 0.0007(8) -0.0022(8) -0.0038(8) N5 0.0146(9) 0.0232(11) 0.0243(11) 0.0026(9) 0.0002(8) -0.0043(8) C1 0.0184(12) 0.0303(15) 0.0262(14) 0.0072(12) -0.0009(10) -0.0052(11) C2 0.0138(12) 0.0296(14) 0.0307(15) 0.0009(11) -0.0004(11) -0.0037(10) C3 0.0193(12) 0.0208(13) 0.0274(14) -0.0012(11) -0.0070(11) -0.0001(10) C4 0.0203(12) 0.0194(13) 0.0240(13) 0.0015(10) -0.0045(10) -0.0044(10) C5 0.0186(11) 0.0165(12) 0.0198(12) 0.0002(10) -0.0062(9) -0.0039(9) C6 0.0161(11) 0.0190(12) 0.0203(13) 0.0020(10) -0.0049(10) -0.0025(10) C7 0.0169(11) 0.0165(12) 0.0203(13) 0.0014(10) -0.0040(10) -0.0010(9) C8 0.0179(11) 0.0174(12) 0.0209(13) 0.0002(10) -0.0033(10) -0.0050(9) C9 0.0234(12) 0.0212(13) 0.0244(13) 0.0047(11) -0.0036(11) -0.0033(10) C10 0.0243(13) 0.0268(14) 0.0264(14) 0.0063(12) 0.0008(11) -0.0080(11) C11 0.0171(12) 0.0252(14) 0.0260(14) -0.0032(11) -0.0009(10) -0.0043(10) C12 0.0176(11) 0.0208(13) 0.0236(13) -0.0007(10) -0.0047(10) -0.0035(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 2.228(2) . ? Ag1 N3 2.2638(19) 2_566 ? Ag1 N4 2.4350(19) 2_566 ? O1 N5 1.237(3) . ? O2 N5 1.250(3) . ? O3 N5 1.245(3) . ? N1 C5 1.350(3) . ? N1 C1 1.354(3) . ? N2 C6 1.275(3) . ? N2 N3 1.411(3) . ? N3 C7 1.279(3) . ? N3 Ag1 2.2637(19) 2_566 ? N4 C12 1.339(3) . ? N4 C8 1.346(3) . ? N4 Ag1 2.4351(19) 2_566 ? C1 C2 1.382(4) . ? C1 H1 1.03(3) . ? C2 C3 1.379(4) . ? C2 H2 0.88(3) . ? C3 C4 1.384(3) . ? C3 H3 0.98(3) . ? C4 C5 1.390(3) . ? C4 H4 0.99(3) . ? C5 C6 1.474(3) . ? C6 H6 0.89(3) . ? C7 C8 1.474(3) . ? C7 H7 0.93(3) . ? C8 C9 1.383(3) . ? C9 C10 1.390(3) . ? C9 H9 0.96(3) . ? C10 C11 1.377(4) . ? C10 H10 0.91(3) . ? C11 C12 1.383(4) . ? C11 H11 0.96(3) . ? C12 H12 0.97(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 171.17(7) . 2_566 ? N1 Ag1 N4 114.63(7) . 2_566 ? N3 Ag1 N4 71.45(7) 2_566 2_566 ? C5 N1 C1 117.2(2) . . ? C5 N1 Ag1 125.91(15) . . ? C1 N1 Ag1 116.50(16) . . ? C6 N2 N3 113.09(19) . . ? C7 N3 N2 111.79(19) . . ? C7 N3 Ag1 118.10(15) . 2_566 ? N2 N3 Ag1 129.99(14) . 2_566 ? C12 N4 C8 117.4(2) . . ? C12 N4 Ag1 130.53(16) . 2_566 ? C8 N4 Ag1 112.06(14) . 2_566 ? O1 N5 O3 120.3(2) . . ? O1 N5 O2 119.6(2) . . ? O3 N5 O2 120.1(2) . . ? N1 C1 C2 123.0(2) . . ? N1 C1 H1 115.5(14) . . ? C2 C1 H1 121.4(14) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 126.0(18) . . ? C1 C2 H2 114.5(18) . . ? C2 C3 C4 118.2(2) . . ? C2 C3 H3 120.8(15) . . ? C4 C3 H3 120.8(15) . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 121.8(14) . . ? C5 C4 H4 118.5(14) . . ? N1 C5 C4 122.4(2) . . ? N1 C5 C6 116.4(2) . . ? C4 C5 C6 121.2(2) . . ? N2 C6 C5 119.0(2) . . ? N2 C6 H6 121.4(16) . . ? C5 C6 H6 119.7(16) . . ? N3 C7 C8 120.9(2) . . ? N3 C7 H7 123.0(15) . . ? C8 C7 H7 116.0(15) . . ? N4 C8 C9 122.9(2) . . ? N4 C8 C7 117.1(2) . . ? C9 C8 C7 120.0(2) . . ? C8 C9 C10 118.7(2) . . ? C8 C9 H9 120.4(16) . . ? C10 C9 H9 120.9(16) . . ? C11 C10 C9 119.0(2) . . ? C11 C10 H10 120.7(19) . . ? C9 C10 H10 120.3(19) . . ? C10 C11 C12 118.7(2) . . ? C10 C11 H11 120.5(16) . . ? C12 C11 H11 120.6(16) . . ? N4 C12 C11 123.4(2) . . ? N4 C12 H12 114.7(16) . . ? C11 C12 H12 121.8(16) . . ? 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 N3 Ag1 N1 C5 46.2(5) 2_566 . . . ? N4 Ag1 N1 C5 178.41(18) 2_566 . . . ? N3 Ag1 N1 C1 -141.3(4) 2_566 . . . ? N4 Ag1 N1 C1 -9.1(2) 2_566 . . . ? C6 N2 N3 C7 -175.9(2) . . . . ? C6 N2 N3 Ag1 0.0(3) . . . 2_566 ? C5 N1 C1 C2 -0.1(4) . . . . ? Ag1 N1 C1 C2 -173.2(2) . . . . ? N1 C1 C2 C3 -0.1(4) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C1 N1 C5 C4 0.1(3) . . . . ? Ag1 N1 C5 C4 172.58(17) . . . . ? C1 N1 C5 C6 179.7(2) . . . . ? Ag1 N1 C5 C6 -7.8(3) . . . . ? C3 C4 C5 N1 -0.1(4) . . . . ? C3 C4 C5 C6 -179.6(2) . . . . ? N3 N2 C6 C5 -177.93(19) . . . . ? N1 C5 C6 N2 178.3(2) . . . . ? C4 C5 C6 N2 -2.1(4) . . . . ? N2 N3 C7 C8 -176.1(2) . . . . ? Ag1 N3 C7 C8 7.5(3) 2_566 . . . ? C12 N4 C8 C9 -0.8(3) . . . . ? Ag1 N4 C8 C9 -179.02(19) 2_566 . . . ? C12 N4 C8 C7 177.0(2) . . . . ? Ag1 N4 C8 C7 -1.2(3) 2_566 . . . ? N3 C7 C8 N4 -4.1(3) . . . . ? N3 C7 C8 C9 173.9(2) . . . . ? N4 C8 C9 C10 0.8(4) . . . . ? C7 C8 C9 C10 -177.0(2) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C8 N4 C12 C11 -0.1(4) . . . . ? Ag1 N4 C12 C11 177.69(17) 2_566 . . . ? C10 C11 C12 N4 1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.410 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.086 #===END #----------------------------------------------------------------------- #--------------DATA FOR 4A - Ag(ligand4).0.25ligand4------------------ #--------------------------------------------------------------------- data_p4ab _database_code_depnum_ccdc_archive 'CCDC 266723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17.5 H17.5 Ag1 Cl1 N5 O4' _chemical_formula_weight 505.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4948(3) _cell_length_b 13.9768(4) _cell_length_c 14.3519(4) _cell_angle_alpha 64.474(2) _cell_angle_beta 88.167(2) _cell_angle_gamma 77.080(1) _cell_volume 1846.64(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7542 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 1.026 _exptl_absorpt_process_details 'denzox and scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15793 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.60 _reflns_number_total 8459 _reflns_number_gt 5505 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzox and Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0329P)^2^+4.8113P] 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 8459 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.005 _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 1.02583(4) -1.09500(3) 0.37106(3) 0.03060(12) Uani 1 1 d . . . Ag2 Ag -0.04546(3) 0.09327(3) 0.13280(3) 0.02762(11) Uani 1 1 d . . . Cl1 Cl 0.25630(13) 0.13622(11) -0.22610(10) 0.0357(3) Uani 1 1 d . . . Cl2 Cl 0.27087(13) -0.88809(10) 0.27809(10) 0.0349(3) Uani 1 1 d . . . N1 N 0.8729(4) -0.9798(3) 0.3944(3) 0.0240(9) Uani 1 1 d . . . N2 N 0.5811(3) -0.6445(3) 0.3880(3) 0.0214(8) Uani 1 1 d . . . N3 N 0.4749(3) -0.5653(3) 0.3921(3) 0.0218(8) Uani 1 1 d . . . N4 N 0.1817(4) -0.2186(3) 0.3636(3) 0.0222(8) Uani 1 1 d . . . N5 N 0.1095(4) -0.0190(3) 0.1060(3) 0.0231(9) Uani 1 1 d . . . N6 N 0.4017(3) -0.3535(3) 0.1115(3) 0.0228(9) Uani 1 1 d . . . N7 N 0.5073(3) -0.4338(3) 0.1095(3) 0.0192(8) Uani 1 1 d . . . N8 N 0.7968(4) -0.7840(3) 0.1433(3) 0.0211(8) Uani 1 1 d . . . N9 N 0.0315(5) -0.5931(6) 0.4272(4) 0.0557(15) Uani 1 1 d . . . N10 N 0.0125(4) -0.5238(3) 0.0547(3) 0.0310(9) Uani 1 1 d . . . C1 C 0.8931(4) -0.8865(4) 0.3908(3) 0.0218(10) Uani 1 1 d . . . H1 H 0.9788 -0.8739 0.3797 0.026 Uiso 1 1 calc R . . C2 C 0.7965(4) -0.8084(4) 0.4022(3) 0.0204(10) Uani 1 1 d . . . H2 H 0.8158 -0.7438 0.3989 0.025 Uiso 1 1 calc R . . C3 C 0.6698(4) -0.8250(4) 0.4189(3) 0.0208(10) Uani 1 1 d . . . C4 C 0.6482(5) -0.9220(4) 0.4237(3) 0.0237(10) Uani 1 1 d . . . H4 H 0.5638 -0.9372 0.4360 0.028 Uiso 1 1 calc R . . C5 C 0.7512(5) -0.9959(4) 0.4106(3) 0.0272(11) Uani 1 1 d . . . H5 H 0.7346 -1.0611 0.4131 0.033 Uiso 1 1 calc R . . C6 C 0.5604(4) -0.7417(4) 0.4283(3) 0.0199(9) Uani 1 1 d . . . C7 C 0.4431(4) -0.7767(4) 0.4812(4) 0.0283(11) Uani 1 1 d . . . H7A H 0.3879 -0.7171 0.4933 0.042 Uiso 1 1 calc R . . H7B H 0.4712 -0.8406 0.5476 0.042 Uiso 1 1 calc R . . H7C H 0.3929 -0.7952 0.4375 0.042 Uiso 1 1 calc R . . C8 C 0.5011(4) -0.4712(4) 0.3647(3) 0.0194(9) Uani 1 1 d . . . C9 C 0.6319(4) -0.4457(4) 0.3355(4) 0.0278(11) Uani 1 1 d . . . H9A H 0.6924 -0.5095 0.3340 0.042 Uiso 1 1 calc R . . H9B H 0.6667 -0.4271 0.3865 0.042 Uiso 1 1 calc R . . H9C H 0.6223 -0.3839 0.2669 0.042 Uiso 1 1 calc R . . C10 C 0.3900(4) -0.3838(3) 0.3637(3) 0.0184(9) Uani 1 1 d . . . C11 C 0.4066(5) -0.2802(4) 0.3405(3) 0.0230(10) Uani 1 1 d . . . H11 H 0.4898 -0.2637 0.3236 0.028 Uiso 1 1 calc R . . C12 C 0.3016(5) -0.2012(4) 0.3420(3) 0.0234(10) Uani 1 1 d . . . H12 H 0.3153 -0.1312 0.3270 0.028 Uiso 1 1 calc R . . C13 C 0.1648(4) -0.3185(3) 0.3841(4) 0.0248(10) Uani 1 1 d . . . H13 H 0.0801 -0.3324 0.3994 0.030 Uiso 1 1 calc R . . C14 C 0.2644(4) -0.4010(4) 0.3840(3) 0.0246(10) Uani 1 1 d . . . H14 H 0.2477 -0.4697 0.3977 0.030 Uiso 1 1 calc R . . C15 C 0.2286(5) 0.0006(4) 0.0835(4) 0.0283(11) Uani 1 1 d . . . H15 H 0.2429 0.0682 0.0761 0.034 Uiso 1 1 calc R . . C16 C 0.3312(5) -0.0719(4) 0.0704(4) 0.0281(11) Uani 1 1 d . . . H16 H 0.4135 -0.0536 0.0533 0.034 Uiso 1 1 calc R . . C17 C 0.3140(4) -0.1726(4) 0.0823(3) 0.0203(10) Uani 1 1 d . . . C18 C 0.1892(4) -0.1922(4) 0.1040(3) 0.0227(10) Uani 1 1 d . . . H18 H 0.1722 -0.2590 0.1114 0.027 Uiso 1 1 calc R . . C19 C 0.0914(4) -0.1152(4) 0.1146(3) 0.0242(10) Uani 1 1 d . . . H19 H 0.0071 -0.1300 0.1287 0.029 Uiso 1 1 calc R . . C20 C 0.4236(4) -0.2572(4) 0.0752(3) 0.0217(10) Uani 1 1 d . . . C21 C 0.5461(4) -0.2238(4) 0.0299(4) 0.0272(11) Uani 1 1 d . . . H21A H 0.5924 -0.2081 0.0780 0.041 Uiso 1 1 calc R . . H21B H 0.5231 -0.1584 -0.0361 0.041 Uiso 1 1 calc R . . H21C H 0.6027 -0.2831 0.0183 0.041 Uiso 1 1 calc R . . C22 C 0.4790(4) -0.5277(4) 0.1378(3) 0.0208(10) Uani 1 1 d . . . C23 C 0.3474(4) -0.5516(4) 0.1669(4) 0.0315(12) Uani 1 1 d . . . H23A H 0.2897 -0.4890 0.1727 0.047 Uiso 1 1 calc R . . H23B H 0.3572 -0.6161 0.2335 0.047 Uiso 1 1 calc R . . H23C H 0.3092 -0.5651 0.1136 0.047 Uiso 1 1 calc R . . C24 C 0.5887(4) -0.6167(4) 0.1410(3) 0.0196(9) Uani 1 1 d . . . C25 C 0.5708(4) -0.7197(4) 0.1595(3) 0.0203(9) Uani 1 1 d . . . H25 H 0.4863 -0.7346 0.1721 0.024 Uiso 1 1 calc R . . C26 C 0.6748(4) -0.7989(4) 0.1594(3) 0.0220(10) Uani 1 1 d . . . H26 H 0.6596 -0.8677 0.1714 0.026 Uiso 1 1 calc R . . C27 C 0.8164(4) -0.6860(4) 0.1269(4) 0.0258(11) Uani 1 1 d . . . H27 H 0.9024 -0.6743 0.1161 0.031 Uiso 1 1 calc R . . C28 C 0.7164(4) -0.6023(4) 0.1253(4) 0.0237(10) Uani 1 1 d . . . H28 H 0.7345 -0.5345 0.1135 0.028 Uiso 1 1 calc R . . C29 C -0.0285(6) -0.4906(6) 0.3710(5) 0.0496(16) Uani 1 1 d . . . H29 H -0.0609 -0.4472 0.4063 0.060 Uiso 1 1 calc R . . C30 C -0.0479(5) -0.4410(5) 0.2630(4) 0.0395(14) Uani 1 1 d . . . H30 H -0.0893 -0.3659 0.2265 0.047 Uiso 1 1 calc R . . C31 C -0.0045(5) -0.5050(5) 0.2101(4) 0.0338(12) Uani 1 1 d . . . C32 C 0.0583(5) -0.6119(5) 0.2674(4) 0.0360(13) Uani 1 1 d . . . H32 H 0.0906 -0.6579 0.2345 0.043 Uiso 1 1 calc R . . C33 C 0.0741(6) -0.6524(6) 0.3753(4) 0.0495(16) Uani 1 1 d . . . H33 H 0.1179 -0.7266 0.4139 0.059 Uiso 1 1 calc R . . C34 C -0.0257(4) -0.4555(4) 0.0942(4) 0.0271(11) Uani 1 1 d . . . C35 C -0.0897(5) -0.3386(4) 0.0382(4) 0.0432(14) Uani 1 1 d . . . H35A H -0.0285 -0.2949 0.0382 0.065 Uiso 1 1 calc R . . H35B H -0.1678 -0.3216 0.0726 0.065 Uiso 1 1 calc R . . H35C H -0.1151 -0.3216 -0.0333 0.065 Uiso 1 1 calc R . . O1 O 0.2093(4) 0.1816(4) -0.1550(3) 0.0542(11) Uani 1 1 d . . . O2 O 0.3865(8) 0.1190(9) -0.2267(7) 0.058(3) Uiso 0.579(15) 1 d P . . O3 O 0.1945(10) 0.2166(6) -0.3342(6) 0.056(3) Uiso 0.579(15) 1 d P . . O4 O 0.2047(8) 0.0423(7) -0.1965(7) 0.040(2) Uiso 0.579(15) 1 d P . . O9 O 0.2699(14) 0.2153(9) -0.3188(8) 0.056(4) Uiso 0.421(15) 1 d P . . O10 O 0.3942(11) 0.0610(13) -0.1812(11) 0.064(4) Uiso 0.421(15) 1 d P . . O11 O 0.1788(10) 0.0669(8) -0.2313(9) 0.029(3) Uiso 0.421(15) 1 d P . . O5 O 0.2981(11) -0.8337(8) 0.3287(8) 0.070(3) Uiso 0.50 1 d P . . O6 O 0.2759(11) -0.7950(9) 0.1868(8) 0.051(3) Uiso 0.50 1 d P . . O7 O 0.1649(6) -0.9323(5) 0.2701(5) 0.0210(14) Uiso 0.50 1 d P . . O8 O 0.3879(11) -0.9586(9) 0.2606(9) 0.084(3) Uiso 0.50 1 d P . . O12 O 0.1858(12) -0.9554(10) 0.3248(10) 0.088(4) Uiso 0.50 1 d P . . O13 O 0.2292(9) -0.8459(7) 0.3587(6) 0.050(2) Uiso 0.50 1 d P . . O14 O 0.3926(7) -0.9709(6) 0.3189(6) 0.0407(19) Uiso 0.50 1 d P . . O15 O 0.269(2) -0.8135(17) 0.1689(16) 0.045(6) Uiso 0.25 1 d P . . O16 O 0.1655(19) -0.8248(15) 0.1886(14) 0.066(5) Uiso 0.25 1 d P . . 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 0.0357(2) 0.0220(2) 0.0288(2) -0.01324(17) 0.00306(16) 0.00792(16) Ag2 0.0279(2) 0.0214(2) 0.0305(2) -0.01331(16) 0.00282(15) 0.00400(15) Cl1 0.0376(7) 0.0421(8) 0.0412(8) -0.0259(6) 0.0149(6) -0.0213(6) Cl2 0.0405(7) 0.0296(7) 0.0351(7) -0.0130(6) -0.0004(5) -0.0112(6) N1 0.030(2) 0.0158(19) 0.023(2) -0.0102(16) 0.0043(16) 0.0035(16) N2 0.0224(19) 0.018(2) 0.022(2) -0.0106(16) 0.0046(15) 0.0012(15) N3 0.0196(19) 0.018(2) 0.025(2) -0.0107(17) 0.0047(15) 0.0019(15) N4 0.030(2) 0.017(2) 0.017(2) -0.0080(16) 0.0019(15) 0.0001(16) N5 0.026(2) 0.020(2) 0.020(2) -0.0081(16) -0.0008(15) 0.0004(16) N6 0.023(2) 0.020(2) 0.023(2) -0.0125(17) 0.0029(15) 0.0047(16) N7 0.0151(18) 0.019(2) 0.022(2) -0.0101(16) 0.0000(14) 0.0024(14) N8 0.026(2) 0.0151(19) 0.022(2) -0.0115(16) -0.0015(15) 0.0045(15) N9 0.043(3) 0.104(5) 0.032(3) -0.036(3) 0.014(2) -0.029(3) N10 0.035(2) 0.037(2) 0.028(2) -0.0173(19) 0.0067(18) -0.0150(19) C1 0.022(2) 0.023(2) 0.019(2) -0.011(2) -0.0002(17) 0.0015(18) C2 0.021(2) 0.019(2) 0.023(2) -0.0127(19) -0.0028(17) 0.0007(18) C3 0.027(2) 0.019(2) 0.014(2) -0.0076(19) -0.0032(17) 0.0016(18) C4 0.029(2) 0.018(2) 0.022(2) -0.0079(19) 0.0083(19) -0.0051(19) C5 0.038(3) 0.016(2) 0.024(3) -0.009(2) 0.006(2) -0.001(2) C6 0.020(2) 0.025(2) 0.016(2) -0.011(2) -0.0031(17) -0.0023(18) C7 0.024(2) 0.023(3) 0.036(3) -0.014(2) 0.004(2) -0.0011(19) C8 0.023(2) 0.019(2) 0.016(2) -0.0087(19) 0.0009(17) -0.0020(18) C9 0.021(2) 0.023(3) 0.044(3) -0.018(2) 0.002(2) -0.0040(19) C10 0.025(2) 0.014(2) 0.014(2) -0.0059(18) -0.0010(17) 0.0000(17) C11 0.027(2) 0.022(2) 0.021(2) -0.011(2) 0.0000(18) -0.0031(19) C12 0.034(3) 0.017(2) 0.021(2) -0.012(2) -0.0001(19) -0.0029(19) C13 0.022(2) 0.016(2) 0.033(3) -0.010(2) 0.0067(19) 0.0008(18) C14 0.029(3) 0.013(2) 0.028(3) -0.0066(19) 0.006(2) -0.0017(18) C15 0.033(3) 0.015(2) 0.031(3) -0.006(2) 0.007(2) -0.002(2) C16 0.029(3) 0.020(2) 0.034(3) -0.011(2) 0.006(2) -0.003(2) C17 0.023(2) 0.021(2) 0.016(2) -0.0111(19) 0.0000(17) 0.0021(18) C18 0.022(2) 0.023(2) 0.025(3) -0.014(2) 0.0011(18) -0.0032(19) C19 0.018(2) 0.026(3) 0.031(3) -0.016(2) -0.0011(18) -0.0010(19) C20 0.018(2) 0.022(2) 0.022(2) -0.009(2) -0.0015(17) -0.0001(18) C21 0.024(2) 0.027(3) 0.036(3) -0.019(2) 0.004(2) -0.005(2) C22 0.019(2) 0.023(2) 0.016(2) -0.0074(19) -0.0019(17) 0.0015(18) C23 0.021(2) 0.029(3) 0.042(3) -0.015(2) 0.002(2) -0.002(2) C24 0.017(2) 0.023(2) 0.017(2) -0.0088(19) 0.0009(16) -0.0001(17) C25 0.023(2) 0.021(2) 0.018(2) -0.0088(19) 0.0006(17) -0.0051(18) C26 0.027(2) 0.020(2) 0.021(2) -0.011(2) 0.0020(18) -0.0041(19) C27 0.018(2) 0.023(3) 0.038(3) -0.016(2) 0.0039(19) -0.0014(19) C28 0.022(2) 0.019(2) 0.035(3) -0.017(2) 0.0024(19) -0.0025(18) C29 0.043(3) 0.085(5) 0.046(4) -0.044(4) 0.017(3) -0.035(4) C30 0.037(3) 0.071(4) 0.039(3) -0.043(3) 0.018(2) -0.029(3) C31 0.023(3) 0.054(4) 0.034(3) -0.024(3) 0.009(2) -0.019(2) C32 0.028(3) 0.058(4) 0.025(3) -0.019(3) 0.007(2) -0.014(3) C33 0.040(3) 0.065(4) 0.038(3) -0.016(3) 0.003(3) -0.014(3) C34 0.019(2) 0.046(3) 0.031(3) -0.027(2) 0.0078(19) -0.014(2) C35 0.041(3) 0.043(3) 0.045(3) -0.027(3) 0.006(3) 0.005(3) O1 0.067(3) 0.065(3) 0.061(3) -0.052(2) 0.015(2) -0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.134(4) . ? Ag1 N4 2.134(4) 1_645 ? Ag1 Ag2 3.2719(5) 1_645 ? Ag2 N5 2.143(4) . ? Ag2 N8 2.154(3) 1_465 ? Ag2 Ag1 3.2719(5) 1_465 ? Cl1 O2 1.333(8) . ? Cl1 O9 1.343(10) . ? Cl1 O4 1.422(8) . ? Cl1 O11 1.423(9) . ? Cl1 O1 1.441(4) . ? Cl1 O3 1.525(8) . ? Cl1 O10 1.553(13) . ? Cl2 O5 1.332(11) . ? Cl2 O12 1.387(12) . ? Cl2 O6 1.403(11) . ? Cl2 O7 1.417(6) . ? Cl2 O14 1.455(8) . ? Cl2 O15 1.46(2) . ? Cl2 O8 1.482(12) . ? Cl2 O13 1.521(9) . ? Cl2 O16 1.526(19) . ? N1 C5 1.342(6) . ? N1 C1 1.346(6) . ? N2 C6 1.294(5) . ? N2 N3 1.405(5) . ? N3 C8 1.293(5) . ? N4 C12 1.337(6) . ? N4 C13 1.350(6) . ? N4 Ag1 2.134(4) 1_465 ? N5 C15 1.339(6) . ? N5 C19 1.353(6) . ? N6 C20 1.290(6) . ? N6 N7 1.400(5) . ? N7 C22 1.298(6) . ? N8 C26 1.340(6) . ? N8 C27 1.349(6) . ? N8 Ag2 2.154(3) 1_645 ? N9 C29 1.316(8) . ? N9 C33 1.337(8) . ? N10 C34 1.294(6) . ? N10 N10 1.423(8) 2_545 ? C1 C2 1.378(6) . ? C1 H1 0.9500 . ? C2 C3 1.395(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C3 C6 1.490(6) . ? C4 C5 1.388(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.491(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.484(6) . ? C8 C9 1.496(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.390(6) . ? C10 C14 1.391(6) . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.395(6) . ? C16 H16 0.9500 . ? C17 C18 1.395(6) . ? C17 C20 1.491(6) . ? C18 C19 1.369(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.498(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.478(6) . ? C22 C23 1.497(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C28 1.397(6) . ? C24 C25 1.403(6) . ? C25 C26 1.370(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.378(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.398(8) . ? C29 H29 0.9500 . ? C30 C31 1.402(7) . ? C30 H30 0.9500 . ? C31 C32 1.371(7) . ? C31 C34 1.502(7) . ? C32 C33 1.402(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.476(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O2 O10 0.780(12) . ? O2 O9 1.699(13) . ? O3 O9 0.823(11) . ? O4 O11 0.510(11) . ? O5 O13 0.842(11) . ? O6 O16 1.31(2) . ? O7 O12 0.727(12) . ? O7 O16 1.454(19) . ? O8 O14 0.779(12) . ? O15 O16 1.14(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N4 174.47(13) . 1_645 ? N1 Ag1 Ag2 79.66(10) . 1_645 ? N4 Ag1 Ag2 105.82(9) 1_645 1_645 ? N5 Ag2 N8 174.28(13) . 1_465 ? N5 Ag2 Ag1 80.94(9) . 1_465 ? N8 Ag2 Ag1 104.78(9) 1_465 1_465 ? O2 Cl1 O9 78.8(6) . . ? O2 Cl1 O4 115.6(5) . . ? O9 Cl1 O4 132.5(6) . . ? O2 Cl1 O11 126.2(5) . . ? O9 Cl1 O11 113.6(6) . . ? O4 Cl1 O11 20.7(4) . . ? O2 Cl1 O1 110.7(4) . . ? O9 Cl1 O1 110.6(5) . . ? O4 Cl1 O1 105.6(4) . . ? O11 Cl1 O1 112.1(4) . . ? O2 Cl1 O3 109.4(5) . . ? O9 Cl1 O3 32.6(5) . . ? O4 Cl1 O3 106.8(5) . . ? O11 Cl1 O3 86.2(5) . . ? O1 Cl1 O3 108.4(4) . . ? O2 Cl1 O10 30.2(5) . . ? O9 Cl1 O10 107.8(7) . . ? O4 Cl1 O10 89.4(6) . . ? O11 Cl1 O10 105.3(6) . . ? O1 Cl1 O10 107.0(5) . . ? O3 Cl1 O10 135.0(5) . . ? O5 Cl2 O12 115.1(7) . . ? O5 Cl2 O6 86.6(6) . . ? O12 Cl2 O6 139.2(7) . . ? O5 Cl2 O7 136.0(5) . . ? O12 Cl2 O7 30.0(5) . . ? O6 Cl2 O7 111.0(5) . . ? O5 Cl2 O14 92.4(6) . . ? O12 Cl2 O14 97.3(6) . . ? O6 Cl2 O14 116.7(6) . . ? O7 Cl2 O14 112.4(4) . . ? O5 Cl2 O15 104.6(10) . . ? O12 Cl2 O15 127.7(10) . . ? O6 Cl2 O15 18.0(9) . . ? O7 Cl2 O15 97.7(9) . . ? O14 Cl2 O15 114.1(9) . . ? O5 Cl2 O8 113.9(7) . . ? O12 Cl2 O8 105.5(7) . . ? O6 Cl2 O8 94.9(6) . . ? O7 Cl2 O8 104.7(5) . . ? O14 Cl2 O8 30.7(5) . . ? O15 Cl2 O8 86.8(10) . . ? O5 Cl2 O13 33.5(5) . . ? O12 Cl2 O13 83.4(6) . . ? O6 Cl2 O13 105.1(6) . . ? O7 Cl2 O13 102.7(4) . . ? O14 Cl2 O13 107.6(5) . . ? O15 Cl2 O13 121.2(9) . . ? O8 Cl2 O13 137.3(6) . . ? O5 Cl2 O16 116.0(9) . . ? O12 Cl2 O16 86.2(9) . . ? O6 Cl2 O16 53.0(8) . . ? O7 Cl2 O16 59.1(7) . . ? O14 Cl2 O16 146.8(8) . . ? O15 Cl2 O16 44.9(9) . . ? O8 Cl2 O16 116.6(9) . . ? O13 Cl2 O16 105.5(8) . . ? C5 N1 C1 117.0(4) . . ? C5 N1 Ag1 121.4(3) . . ? C1 N1 Ag1 121.6(3) . . ? C6 N2 N3 113.4(3) . . ? C8 N3 N2 113.6(3) . . ? C12 N4 C13 117.3(4) . . ? C12 N4 Ag1 121.1(3) . 1_465 ? C13 N4 Ag1 121.6(3) . 1_465 ? C15 N5 C19 117.0(4) . . ? C15 N5 Ag2 122.2(3) . . ? C19 N5 Ag2 120.7(3) . . ? C20 N6 N7 114.5(4) . . ? C22 N7 N6 113.2(4) . . ? C26 N8 C27 117.5(4) . . ? C26 N8 Ag2 121.8(3) . 1_645 ? C27 N8 Ag2 120.5(3) . 1_645 ? C29 N9 C33 116.2(5) . . ? C34 N10 N10 113.5(5) . 2_545 ? N1 C1 C2 123.7(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 119.3(4) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 117.4(4) . . ? C4 C3 C6 120.8(4) . . ? C2 C3 C6 121.7(4) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 123.2(4) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C3 113.6(4) . . ? N2 C6 C7 127.5(4) . . ? C3 C6 C7 118.9(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C10 115.4(4) . . ? N3 C8 C9 125.3(4) . . ? C10 C8 C9 119.3(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 . . ? C11 C10 C14 117.1(4) . . ? C11 C10 C8 121.2(4) . . ? C14 C10 C8 121.7(4) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? N4 C12 C11 123.1(4) . . ? N4 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N4 C13 C14 122.9(4) . . ? N4 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C10 119.9(4) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? N5 C15 C16 123.4(4) . . ? N5 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 119.6(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 117.0(4) . . ? C16 C17 C20 122.1(4) . . ? C18 C17 C20 120.9(4) . . ? C19 C18 C17 119.9(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N5 C19 C18 123.0(4) . . ? N5 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? N6 C20 C17 114.6(4) . . ? N6 C20 C21 127.1(4) . . ? C17 C20 C21 118.2(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C24 115.4(4) . . ? N7 C22 C23 125.5(4) . . ? C24 C22 C23 119.1(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C24 C25 116.2(4) . . ? C28 C24 C22 121.6(4) . . ? C25 C24 C22 122.3(4) . . ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? N8 C26 C25 123.1(4) . . ? N8 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N8 C27 C28 122.6(4) . . ? N8 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C24 120.3(4) . . ? C27 C28 H28 119.8 . . ? C24 C28 H28 119.8 . . ? N9 C29 C30 124.7(6) . . ? N9 C29 H29 117.6 . . ? C30 C29 H29 117.6 . . ? C29 C30 C31 118.3(6) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 117.8(5) . . ? C32 C31 C34 122.2(5) . . ? C30 C31 C34 120.0(5) . . ? C31 C32 C33 118.9(6) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? N9 C33 C32 124.1(6) . . ? N9 C33 H33 117.9 . . ? C32 C33 H33 117.9 . . ? N10 C34 C35 127.0(5) . . ? N10 C34 C31 114.3(5) . . ? C35 C34 C31 118.6(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O10 O2 Cl1 90.7(12) . . ? O10 O2 O9 138.7(14) . . ? Cl1 O2 O9 50.8(5) . . ? O9 O3 Cl1 61.4(10) . . ? O11 O4 Cl1 79.8(16) . . ? O3 O9 Cl1 86.0(12) . . ? O3 O9 O2 132.5(13) . . ? Cl1 O9 O2 50.3(5) . . ? O2 O10 Cl1 59.2(11) . . ? O4 O11 Cl1 79.6(17) . . ? O13 O5 Cl2 85.7(11) . . ? O16 O6 Cl2 68.3(10) . . ? O12 O7 Cl2 72.8(12) . . ? O12 O7 O16 129.1(15) . . ? Cl2 O7 O16 64.2(8) . . ? O14 O8 Cl2 72.7(11) . . ? O7 O12 Cl2 77.2(12) . . ? O5 O13 Cl2 60.8(10) . . ? O8 O14 Cl2 76.5(11) . . ? O16 O15 Cl2 70.7(14) . . ? O15 O16 O6 19.7(13) . . ? O15 O16 O7 112.6(18) . . ? O6 O16 O7 114.2(14) . . ? O15 O16 Cl2 64.4(14) . . ? O6 O16 Cl2 58.7(9) . . ? O7 O16 Cl2 56.7(7) . . ? 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 N4 Ag1 N1 C5 -84.6(16) 1_645 . . . ? Ag2 Ag1 N1 C5 102.9(3) 1_645 . . . ? N4 Ag1 N1 C1 97.3(15) 1_645 . . . ? Ag2 Ag1 N1 C1 -75.2(3) 1_645 . . . ? C6 N2 N3 C8 171.4(4) . . . . ? N8 Ag2 N5 C15 75.2(15) 1_465 . . . ? Ag1 Ag2 N5 C15 -106.7(3) 1_465 . . . ? N8 Ag2 N5 C19 -106.9(14) 1_465 . . . ? Ag1 Ag2 N5 C19 71.2(3) 1_465 . . . ? C20 N6 N7 C22 -174.2(4) . . . . ? C5 N1 C1 C2 -0.3(6) . . . . ? Ag1 N1 C1 C2 178.0(3) . . . . ? N1 C1 C2 C3 0.2(6) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C1 C2 C3 C6 -177.9(4) . . . . ? C2 C3 C4 C5 -0.9(6) . . . . ? C6 C3 C4 C5 177.4(4) . . . . ? C1 N1 C5 C4 -0.3(6) . . . . ? Ag1 N1 C5 C4 -178.5(3) . . . . ? C3 C4 C5 N1 0.9(7) . . . . ? N3 N2 C6 C3 176.8(3) . . . . ? N3 N2 C6 C7 -3.6(6) . . . . ? C4 C3 C6 N2 -157.4(4) . . . . ? C2 C3 C6 N2 20.9(6) . . . . ? C4 C3 C6 C7 22.9(6) . . . . ? C2 C3 C6 C7 -158.8(4) . . . . ? N2 N3 C8 C10 177.6(3) . . . . ? N2 N3 C8 C9 -2.8(6) . . . . ? N3 C8 C10 C11 176.9(4) . . . . ? C9 C8 C10 C11 -2.8(6) . . . . ? N3 C8 C10 C14 -4.4(6) . . . . ? C9 C8 C10 C14 176.0(4) . . . . ? C14 C10 C11 C12 2.3(6) . . . . ? C8 C10 C11 C12 -178.9(4) . . . . ? C13 N4 C12 C11 -0.3(6) . . . . ? Ag1 N4 C12 C11 177.3(3) 1_465 . . . ? C10 C11 C12 N4 -1.0(7) . . . . ? C12 N4 C13 C14 0.2(7) . . . . ? Ag1 N4 C13 C14 -177.4(3) 1_465 . . . ? N4 C13 C14 C10 1.1(7) . . . . ? C11 C10 C14 C13 -2.4(6) . . . . ? C8 C10 C14 C13 178.8(4) . . . . ? C19 N5 C15 C16 -0.9(7) . . . . ? Ag2 N5 C15 C16 177.1(4) . . . . ? N5 C15 C16 C17 -1.0(7) . . . . ? C15 C16 C17 C18 2.1(7) . . . . ? C15 C16 C17 C20 -176.4(4) . . . . ? C16 C17 C18 C19 -1.3(6) . . . . ? C20 C17 C18 C19 177.2(4) . . . . ? C15 N5 C19 C18 1.7(6) . . . . ? Ag2 N5 C19 C18 -176.3(3) . . . . ? C17 C18 C19 N5 -0.6(7) . . . . ? N7 N6 C20 C17 -176.9(3) . . . . ? N7 N6 C20 C21 1.7(6) . . . . ? C16 C17 C20 N6 164.3(4) . . . . ? C18 C17 C20 N6 -14.1(6) . . . . ? C16 C17 C20 C21 -14.5(6) . . . . ? C18 C17 C20 C21 167.1(4) . . . . ? N6 N7 C22 C24 -177.6(3) . . . . ? N6 N7 C22 C23 2.1(6) . . . . ? N7 C22 C24 C28 6.6(6) . . . . ? C23 C22 C24 C28 -173.2(4) . . . . ? N7 C22 C24 C25 -173.2(4) . . . . ? C23 C22 C24 C25 7.1(6) . . . . ? C28 C24 C25 C26 -1.3(6) . . . . ? C22 C24 C25 C26 178.5(4) . . . . ? C27 N8 C26 C25 0.3(6) . . . . ? Ag2 N8 C26 C25 -175.5(3) 1_645 . . . ? C24 C25 C26 N8 0.7(7) . . . . ? C26 N8 C27 C28 -0.7(7) . . . . ? Ag2 N8 C27 C28 175.2(4) 1_645 . . . ? N8 C27 C28 C24 0.1(7) . . . . ? C25 C24 C28 C27 0.9(6) . . . . ? C22 C24 C28 C27 -178.8(4) . . . . ? C33 N9 C29 C30 -1.0(8) . . . . ? N9 C29 C30 C31 2.1(8) . . . . ? C29 C30 C31 C32 -2.1(7) . . . . ? C29 C30 C31 C34 178.8(4) . . . . ? C30 C31 C32 C33 1.1(7) . . . . ? C34 C31 C32 C33 -179.8(4) . . . . ? C29 N9 C33 C32 -0.1(8) . . . . ? C31 C32 C33 N9 0.0(8) . . . . ? N10 N10 C34 C35 -0.1(8) 2_545 . . . ? N10 N10 C34 C31 177.9(4) 2_545 . . . ? C32 C31 C34 N10 4.2(7) . . . . ? C30 C31 C34 N10 -176.7(4) . . . . ? C32 C31 C34 C35 -177.6(5) . . . . ? C30 C31 C34 C35 1.5(7) . . . . ? O9 Cl1 O2 O10 -163.7(14) . . . . ? O4 Cl1 O2 O10 -31.7(14) . . . . ? O11 Cl1 O2 O10 -52.5(14) . . . . ? O1 Cl1 O2 O10 88.3(12) . . . . ? O3 Cl1 O2 O10 -152.3(12) . . . . ? O4 Cl1 O2 O9 132.0(6) . . . . ? O11 Cl1 O2 O9 111.2(7) . . . . ? O1 Cl1 O2 O9 -108.0(5) . . . . ? O3 Cl1 O2 O9 11.4(7) . . . . ? O10 Cl1 O2 O9 163.7(14) . . . . ? O2 Cl1 O3 O9 -21.1(12) . . . . ? O4 Cl1 O3 O9 -147.0(11) . . . . ? O11 Cl1 O3 O9 -148.3(11) . . . . ? O1 Cl1 O3 O9 99.7(11) . . . . ? O10 Cl1 O3 O9 -40.4(14) . . . . ? O2 Cl1 O4 O11 -125.8(16) . . . . ? O9 Cl1 O4 O11 -27.2(19) . . . . ? O1 Cl1 O4 O11 111.5(16) . . . . ? O3 Cl1 O4 O11 -3.8(17) . . . . ? O10 Cl1 O4 O11 -141.0(17) . . . . ? Cl1 O3 O9 O2 21.2(11) . . . . ? O2 Cl1 O9 O3 159.7(12) . . . . ? O4 Cl1 O9 O3 45.0(14) . . . . ? O11 Cl1 O9 O3 34.9(12) . . . . ? O1 Cl1 O9 O3 -92.2(11) . . . . ? O10 Cl1 O9 O3 151.2(10) . . . . ? O4 Cl1 O9 O2 -114.7(7) . . . . ? O11 Cl1 O9 O2 -124.8(6) . . . . ? O1 Cl1 O9 O2 108.1(5) . . . . ? O3 Cl1 O9 O2 -159.7(12) . . . . ? O10 Cl1 O9 O2 -8.5(7) . . . . ? O10 O2 O9 O3 -3(3) . . . . ? Cl1 O2 O9 O3 -28.0(15) . . . . ? O10 O2 O9 Cl1 25(2) . . . . ? O9 O2 O10 Cl1 -19.3(15) . . . . ? O9 Cl1 O10 O2 16.8(14) . . . . ? O4 Cl1 O10 O2 151.7(12) . . . . ? O11 Cl1 O10 O2 138.4(12) . . . . ? O1 Cl1 O10 O2 -102.1(12) . . . . ? O3 Cl1 O10 O2 38.3(16) . . . . ? O2 Cl1 O11 O4 65.1(18) . . . . ? O9 Cl1 O11 O4 158.4(16) . . . . ? O1 Cl1 O11 O4 -75.3(17) . . . . ? O3 Cl1 O11 O4 176.4(17) . . . . ? O10 Cl1 O11 O4 40.7(17) . . . . ? O12 Cl2 O5 O13 -19.8(13) . . . . ? O6 Cl2 O5 O13 124.3(11) . . . . ? O7 Cl2 O5 O13 7.2(14) . . . . ? O14 Cl2 O5 O13 -119.1(10) . . . . ? O15 Cl2 O5 O13 125.2(13) . . . . ? O8 Cl2 O5 O13 -141.8(10) . . . . ? O16 Cl2 O5 O13 78.7(13) . . . . ? O5 Cl2 O6 O16 -126.4(11) . . . . ? O12 Cl2 O6 O16 -0.8(16) . . . . ? O7 Cl2 O6 O16 12.1(11) . . . . ? O14 Cl2 O6 O16 142.6(10) . . . . ? O15 Cl2 O6 O16 57(4) . . . . ? O8 Cl2 O6 O16 119.9(11) . . . . ? O13 Cl2 O6 O16 -98.2(11) . . . . ? O5 Cl2 O7 O12 -55.4(14) . . . . ? O6 Cl2 O7 O12 -163.2(12) . . . . ? O14 Cl2 O7 O12 64.1(13) . . . . ? O15 Cl2 O7 O12 -175.8(15) . . . . ? O8 Cl2 O7 O12 95.5(13) . . . . ? O13 Cl2 O7 O12 -51.3(13) . . . . ? O16 Cl2 O7 O12 -152.0(15) . . . . ? O5 Cl2 O7 O16 96.6(11) . . . . ? O12 Cl2 O7 O16 152.0(15) . . . . ? O6 Cl2 O7 O16 -11.2(11) . . . . ? O14 Cl2 O7 O16 -144.0(9) . . . . ? O15 Cl2 O7 O16 -23.8(12) . . . . ? O8 Cl2 O7 O16 -112.5(10) . . . . ? O13 Cl2 O7 O16 100.7(9) . . . . ? O5 Cl2 O8 O14 49.1(13) . . . . ? O12 Cl2 O8 O14 -78.1(12) . . . . ? O6 Cl2 O8 O14 137.5(11) . . . . ? O7 Cl2 O8 O14 -109.2(11) . . . . ? O15 Cl2 O8 O14 153.6(14) . . . . ? O13 Cl2 O8 O14 18.9(16) . . . . ? O16 Cl2 O8 O14 -171.7(12) . . . . ? O16 O7 O12 Cl2 -33.0(17) . . . . ? O5 Cl2 O12 O7 140.8(11) . . . . ? O6 Cl2 O12 O7 24.5(18) . . . . ? O14 Cl2 O12 O7 -123.0(11) . . . . ? O15 Cl2 O12 O7 5.3(18) . . . . ? O8 Cl2 O12 O7 -92.7(12) . . . . ? O13 Cl2 O12 O7 130.0(12) . . . . ? O16 Cl2 O12 O7 23.8(13) . . . . ? O12 Cl2 O13 O5 162.0(12) . . . . ? O6 Cl2 O13 O5 -58.7(11) . . . . ? O7 Cl2 O13 O5 -174.8(10) . . . . ? O14 Cl2 O13 O5 66.4(11) . . . . ? O15 Cl2 O13 O5 -67.6(15) . . . . ? O8 Cl2 O13 O5 56.4(13) . . . . ? O16 Cl2 O13 O5 -113.8(12) . . . . ? O5 Cl2 O14 O8 -136.3(12) . . . . ? O12 Cl2 O14 O8 108.0(12) . . . . ? O6 Cl2 O14 O8 -48.8(13) . . . . ? O7 Cl2 O14 O8 81.0(12) . . . . ? O15 Cl2 O14 O8 -29.1(15) . . . . ? O13 Cl2 O14 O8 -166.7(11) . . . . ? O16 Cl2 O14 O8 14(2) . . . . ? O5 Cl2 O15 O16 -112.3(15) . . . . ? O12 Cl2 O15 O16 27(2) . . . . ? O6 Cl2 O15 O16 -109(4) . . . . ? O7 Cl2 O15 O16 29.4(15) . . . . ? O14 Cl2 O15 O16 148.3(13) . . . . ? O8 Cl2 O15 O16 133.9(15) . . . . ? O13 Cl2 O15 O16 -80.5(16) . . . . ? Cl2 O15 O16 O6 68(4) . . . . ? Cl2 O15 O16 O7 -30.9(14) . . . . ? Cl2 O6 O16 O15 -102(4) . . . . ? Cl2 O6 O16 O7 -12.0(11) . . . . ? O12 O7 O16 O15 69(3) . . . . ? Cl2 O7 O16 O15 33.7(17) . . . . ? O12 O7 O16 O6 48(3) . . . . ? Cl2 O7 O16 O6 12.3(11) . . . . ? O12 O7 O16 Cl2 35.3(18) . . . . ? O5 Cl2 O16 O15 84.8(16) . . . . ? O12 Cl2 O16 O15 -159.0(16) . . . . ? O6 Cl2 O16 O15 21.5(14) . . . . ? O7 Cl2 O16 O15 -145.4(18) . . . . ? O14 Cl2 O16 O15 -61(2) . . . . ? O8 Cl2 O16 O15 -53.6(17) . . . . ? O13 Cl2 O16 O15 118.9(15) . . . . ? O5 Cl2 O16 O6 63.3(12) . . . . ? O12 Cl2 O16 O6 179.5(10) . . . . ? O7 Cl2 O16 O6 -166.9(12) . . . . ? O14 Cl2 O16 O6 -82.9(15) . . . . ? O15 Cl2 O16 O6 -21.5(14) . . . . ? O8 Cl2 O16 O6 -75.1(11) . . . . ? O13 Cl2 O16 O6 97.5(9) . . . . ? O5 Cl2 O16 O7 -129.8(7) . . . . ? O12 Cl2 O16 O7 -13.6(7) . . . . ? O6 Cl2 O16 O7 166.9(12) . . . . ? O14 Cl2 O16 O7 84.0(14) . . . . ? O15 Cl2 O16 O7 145.4(18) . . . . ? O8 Cl2 O16 O7 91.8(8) . . . . ? O13 Cl2 O16 O7 -95.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.934 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.113 #===END #-------------------------------------------------------------------------- #--------------DATA FOR 5A - Ag(ligand5) NO3------------------------------ #------------------------------------------------------------------------- data_sortav _database_code_depnum_ccdc_archive 'CCDC 266724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Ag1 N5 O3' _chemical_formula_weight 354.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 25.0213(5) _cell_length_b 9.3011(2) _cell_length_c 15.9564(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.683(1) _cell_angle_gamma 90.00 _cell_volume 3496.49(13) _cell_formula_units_Z 12 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4372 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.90 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.920 _exptl_special_details ; To sortav via denzox. ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13990 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4183 _reflns_number_gt 3473 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Denzo and Collect' _computing_cell_refinement 'Denzo and Collect' _computing_data_reduction 'above + Denzox & Sortav' _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL-77 _refine_special_details ; The nitrate ion on the symmetry special position is disoredered. This is spacially close to a site modeled as a partial chloro position. The presence of this chloro substituent/contaminent is experimentally reasonable as the ligand was synthesised by a hypochlorite reduction of the amine 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^)+(0.0148P)^2^+11.4772P] 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 4183 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.213282(9) 0.71552(2) 0.144788(16) 0.02209(7) Uani 1 1 d . . . Ag2 Ag 0.2500 0.2500 1.0000 0.02673(9) Uani 1 2 d S . . N1 N 0.44569(10) 0.5013(3) 0.10618(17) 0.0236(5) Uani 1 1 d . . . N2 N -0.03284(10) 0.8904(3) 0.14751(17) 0.0234(5) Uani 1 1 d . . . N3 N 0.28890(10) 0.6303(3) 0.12509(16) 0.0193(5) Uani 1 1 d . . . N4 N 0.12834(10) 0.7783(3) 0.13923(16) 0.0213(5) Uani 1 1 d . . . N5 N 0.01104(11) 0.4469(3) 1.02302(18) 0.0252(6) Uani 1 1 d . . . N6 N 0.17100(10) 0.3307(3) 1.01268(17) 0.0229(5) Uani 1 1 d . B . N7 N 0.26395(10) 0.0332(3) 0.16845(17) 0.0204(5) Uani 1 1 d . . . N8 N 0.0135(3) 0.3365(7) 1.2463(6) 0.0403(18) Uiso 0.50 1 d P . . O1 O 0.23534(9) -0.0091(2) 0.09171(14) 0.0265(5) Uani 1 1 d . . . O2 O 0.27619(10) -0.0517(2) 0.23256(15) 0.0319(5) Uani 1 1 d . . . O3 O 0.28089(9) 0.1614(2) 0.18029(14) 0.0265(5) Uani 1 1 d . . . O4 O 0.0608(4) 0.4043(10) 1.2584(6) 0.071(3) Uani 0.50 1 d P . . O5 O 0.0277(4) 0.4018(12) 1.2457(6) 0.081(3) Uani 0.50 1 d P . . O6 O 0.0132(3) 0.2119(6) 1.2242(4) 0.067(2) Uani 0.50 1 d P . . C1 C 0.30880(12) 0.4975(3) 0.1520(2) 0.0206(6) Uani 1 1 d . . . H1 H 0.2868 0.4356 0.1748 0.025 Uiso 1 1 calc R . . C2 C 0.35985(12) 0.4472(3) 0.14775(19) 0.0204(6) Uani 1 1 d . . . H2 H 0.3726 0.3526 0.1670 0.024 Uiso 1 1 calc R . . C3 C 0.39214(12) 0.5381(3) 0.11472(19) 0.0201(6) Uani 1 1 d . . . C4 C 0.37171(12) 0.6741(3) 0.0858(2) 0.0217(6) Uani 1 1 d . . . H4 H 0.3927 0.7374 0.0618 0.026 Uiso 1 1 calc R . . C5 C 0.32036(12) 0.7163(3) 0.0925(2) 0.0216(6) Uani 1 1 d . . . H5 H 0.3067 0.8102 0.0733 0.026 Uiso 1 1 calc R . . C6 C 0.09734(12) 0.6882(3) 0.1706(2) 0.0211(6) Uani 1 1 d . . . H6 H 0.1126 0.5965 0.1920 0.025 Uiso 1 1 calc R . . C7 C 0.10681(12) 0.9089(3) 0.1106(2) 0.0220(6) Uani 1 1 d . . . H7 H 0.1287 0.9735 0.0893 0.026 Uiso 1 1 calc R . . C8 C 0.05385(12) 0.9535(3) 0.1109(2) 0.0230(6) Uani 1 1 d . . . H8 H 0.0397 1.0465 0.0904 0.028 Uiso 1 1 calc R . . C9 C 0.02213(12) 0.8576(3) 0.1420(2) 0.0209(6) Uani 1 1 d . . . C10 C 0.04423(12) 0.7237(3) 0.1727(2) 0.0220(6) Uani 1 1 d . . . H10 H 0.0233 0.6575 0.1948 0.026 Uiso 1 1 calc R . . C11 C 0.15506(12) 0.2990(3) 1.0826(2) 0.0239(6) Uani 1 1 d . . . H11 H 0.1810 0.2489 1.1312 0.029 Uiso 1 1 calc R A 2 C12 C 0.10266(13) 0.3355(3) 1.0876(2) 0.0246(6) Uani 1 1 d . B 2 H12 H 0.0923 0.3088 1.1375 0.030 Uiso 0.955(3) 1 calc PR C 2 C13 C 0.06574(12) 0.4124(3) 1.0173(2) 0.0217(6) Uani 1 1 d . . . C14 C 0.08162(12) 0.4489(3) 0.9446(2) 0.0229(6) Uani 1 1 d . B . H14 H 0.0571 0.5026 0.8963 0.027 Uiso 1 1 calc R . . C15 C 0.13396(12) 0.4046(3) 0.9450(2) 0.0237(6) Uani 1 1 d . . . H15 H 0.1448 0.4272 0.8949 0.028 Uiso 1 1 calc R B . Cl1 Cl 0.0905(7) 0.2968(18) 1.1796(11) 0.027(6) Uiso 0.045(3) 1 d P C 1 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 0.01306(11) 0.02457(12) 0.03122(13) 0.00060(9) 0.01084(9) 0.00559(9) Ag2 0.01714(17) 0.0337(2) 0.03079(19) 0.00210(14) 0.01001(14) 0.00883(13) N1 0.0167(12) 0.0287(14) 0.0275(14) 0.0031(11) 0.0103(11) 0.0076(10) N2 0.0160(12) 0.0237(13) 0.0316(15) -0.0009(11) 0.0096(11) 0.0035(10) N3 0.0130(11) 0.0214(13) 0.0244(13) -0.0014(10) 0.0077(10) 0.0028(9) N4 0.0126(12) 0.0259(13) 0.0261(13) -0.0030(10) 0.0075(10) 0.0058(10) N5 0.0186(13) 0.0284(14) 0.0286(15) -0.0001(11) 0.0079(11) 0.0078(10) N6 0.0151(12) 0.0255(13) 0.0283(14) -0.0008(11) 0.0075(10) 0.0049(10) N7 0.0153(12) 0.0221(13) 0.0265(14) 0.0014(10) 0.0107(10) 0.0033(10) O1 0.0262(12) 0.0244(12) 0.0253(12) -0.0037(9) 0.0040(10) 0.0007(9) O2 0.0399(14) 0.0294(13) 0.0277(13) 0.0076(10) 0.0133(11) 0.0017(10) O3 0.0260(12) 0.0194(11) 0.0318(12) -0.0023(9) 0.0068(10) -0.0032(9) O4 0.117(8) 0.058(5) 0.045(5) -0.014(3) 0.037(6) -0.029(6) O5 0.091(7) 0.109(7) 0.030(4) 0.011(4) 0.004(5) -0.079(6) O6 0.074(5) 0.032(3) 0.072(6) -0.025(3) -0.005(3) 0.010(3) C1 0.0177(14) 0.0206(14) 0.0258(16) 0.0000(12) 0.0102(12) 0.0003(11) C2 0.0177(14) 0.0203(15) 0.0235(16) 0.0019(11) 0.0073(12) 0.0061(11) C3 0.0154(14) 0.0256(15) 0.0198(15) -0.0002(12) 0.0065(11) 0.0063(11) C4 0.0169(14) 0.0242(15) 0.0277(16) 0.0024(12) 0.0123(12) 0.0019(12) C5 0.0205(15) 0.0202(14) 0.0265(16) 0.0010(12) 0.0110(12) 0.0052(12) C6 0.0142(14) 0.0217(15) 0.0262(16) -0.0039(12) 0.0053(12) 0.0039(11) C7 0.0154(14) 0.0277(16) 0.0253(16) 0.0027(12) 0.0099(12) 0.0040(12) C8 0.0177(15) 0.0247(16) 0.0275(17) 0.0036(12) 0.0088(12) 0.0065(12) C9 0.0135(14) 0.0246(16) 0.0243(16) -0.0047(12) 0.0060(12) 0.0035(11) C10 0.0167(14) 0.0222(15) 0.0284(16) -0.0035(12) 0.0093(12) -0.0009(11) C11 0.0183(15) 0.0256(16) 0.0253(16) -0.0005(12) 0.0041(12) 0.0069(12) C12 0.0242(16) 0.0265(16) 0.0238(16) -0.0009(13) 0.0090(13) 0.0069(13) C13 0.0155(14) 0.0230(15) 0.0269(17) -0.0025(12) 0.0074(12) 0.0048(11) C14 0.0172(15) 0.0237(15) 0.0266(17) 0.0011(12) 0.0059(12) 0.0039(12) C15 0.0197(15) 0.0265(16) 0.0262(17) -0.0008(12) 0.0093(13) 0.0002(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.170(2) . ? Ag1 N4 2.177(2) . ? Ag2 N6 2.187(2) . ? Ag2 N6 2.187(2) 7_557 ? N1 N2 1.244(4) 3_545 ? N1 C3 1.433(4) . ? N2 N1 1.244(4) 3_455 ? N2 C9 1.440(4) . ? N3 C5 1.344(4) . ? N3 C1 1.346(4) . ? N4 C7 1.345(4) . ? N4 C6 1.347(4) . ? N5 N5 1.244(5) 5_567 ? N5 C13 1.438(4) . ? N6 C11 1.338(4) . ? N6 C15 1.350(4) . ? N7 O2 1.246(3) . ? N7 O1 1.255(3) . ? N7 O3 1.258(3) . ? N8 O5 0.705(9) . ? N8 N8 0.723(12) 2_557 ? N8 O6 1.211(8) . ? N8 O5 1.239(9) 2_557 ? N8 O4 1.297(10) . ? N8 O6 1.491(8) 2_557 ? O4 O5 0.783(11) . ? O4 Cl1 1.940(19) . ? O5 N8 1.239(9) 2_557 ? O5 O5 1.439(19) 2_557 ? O5 O6 1.813(12) . ? O6 O6 1.216(13) 2_557 ? O6 N8 1.491(8) 2_557 ? C1 C2 1.383(4) . ? C1 H1 0.9500 . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.381(4) . ? C6 H6 0.9500 . ? C7 C8 1.390(4) . ? C7 H7 0.9500 . ? C8 C9 1.392(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.388(4) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C14 C15 1.371(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? 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 N3 Ag1 N4 168.27(9) . . ? N6 Ag2 N6 180.000(1) . 7_557 ? N2 N1 C3 113.4(2) 3_545 . ? N1 N2 C9 113.2(2) 3_455 . ? C5 N3 C1 117.9(2) . . ? C5 N3 Ag1 119.41(19) . . ? C1 N3 Ag1 122.42(19) . . ? C7 N4 C6 118.2(2) . . ? C7 N4 Ag1 122.0(2) . . ? C6 N4 Ag1 119.63(19) . . ? N5 N5 C13 112.5(3) 5_567 . ? C11 N6 C15 117.5(3) . . ? C11 N6 Ag2 122.3(2) . . ? C15 N6 Ag2 119.9(2) . . ? O2 N7 O1 120.3(3) . . ? O2 N7 O3 120.0(3) . . ? O1 N7 O3 119.7(2) . . ? O5 N8 O6 140.7(13) . . ? O5 N8 O5 91.2(18) . 2_557 ? O6 N8 O5 125.1(9) . 2_557 ? O5 N8 O4 31.1(13) . . ? O6 N8 O4 115.2(7) . . ? O5 N8 O4 119.7(8) 2_557 . ? O5 N8 O6 162.6(13) . 2_557 ? O6 N8 O6 52.3(6) . 2_557 ? O5 N8 O6 82.7(7) 2_557 2_557 ? O4 N8 O6 144.4(8) . 2_557 ? O5 O4 N8 27.8(11) . . ? O5 O4 Cl1 114.8(14) . . ? N8 O4 Cl1 100.5(8) . . ? N8 O5 O4 121(2) . . ? N8 O5 N8 30.3(7) . 2_557 ? O4 O5 N8 146.2(17) . 2_557 ? O4 O5 O6 101.9(16) . . ? N3 C1 C2 122.9(3) . . ? N3 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.5(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.1(3) . . ? C4 C3 N1 116.0(3) . . ? C2 C3 N1 124.9(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N3 C5 C4 122.8(3) . . ? N3 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N4 C6 C10 122.6(3) . . ? N4 C6 H6 118.7 . . ? C10 C6 H6 118.7 . . ? N4 C7 C8 122.8(3) . . ? N4 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C9 118.0(3) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 N2 116.4(3) . . ? C8 C9 N2 123.9(3) . . ? C6 C10 C9 118.7(3) . . ? C6 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? N6 C11 C12 123.3(3) . . ? N6 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 117.7(3) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 N5 116.9(3) . . ? C14 C13 N5 123.0(3) . . ? C15 C14 C13 117.7(3) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? N6 C15 C14 123.6(3) . . ? N6 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? 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 N4 Ag1 N3 C5 101.3(5) . . . . ? N4 Ag1 N3 C1 -85.1(5) . . . . ? N3 Ag1 N4 C7 -100.4(5) . . . . ? N3 Ag1 N4 C6 84.0(5) . . . . ? N8 N8 O4 O5 -44(3) 2_557 . . . ? O6 N8 O4 O5 151(2) . . . . ? O5 N8 O4 O5 -26(2) 2_557 . . . ? O6 N8 O4 O5 -149(2) 2_557 . . . ? O5 N8 O4 Cl1 -124(2) . . . . ? N8 N8 O4 Cl1 -169(3) 2_557 . . . ? O6 N8 O4 Cl1 27.0(11) . . . . ? O5 N8 O4 Cl1 -150.4(9) 2_557 . . . ? O6 N8 O4 Cl1 86.6(14) 2_557 . . . ? N8 N8 O5 O4 153(2) 2_557 . . . ? O6 N8 O5 O4 -43(3) . . . . ? O5 N8 O5 O4 158(2) 2_557 . . . ? O6 N8 O5 O4 89(5) 2_557 . . . ? O6 N8 O5 N8 163(4) . . . 2_557 ? O5 N8 O5 N8 4.5(18) 2_557 . . 2_557 ? O4 N8 O5 N8 -153(2) . . . 2_557 ? O6 N8 O5 N8 -64(4) 2_557 . . 2_557 ? N8 N8 O5 O5 -4.5(18) 2_557 . . 2_557 ? O6 N8 O5 O5 159(2) . . . 2_557 ? O4 N8 O5 O5 -158(2) . . . 2_557 ? O6 N8 O5 O5 -69(4) 2_557 . . 2_557 ? N8 N8 O5 O6 -163(4) 2_557 . . . ? O5 N8 O5 O6 -159(2) 2_557 . . . ? O4 N8 O5 O6 43(3) . . . . ? O6 N8 O5 O6 132(6) 2_557 . . . ? Cl1 O4 O5 N8 63(2) . . . . ? N8 O4 O5 N8 24(2) . . . 2_557 ? Cl1 O4 O5 N8 88(3) . . . 2_557 ? N8 O4 O5 O5 86(4) . . . 2_557 ? Cl1 O4 O5 O5 149(3) . . . 2_557 ? N8 O4 O5 O6 -17.3(14) . . . . ? Cl1 O4 O5 O6 46.2(13) . . . . ? O5 N8 O6 O6 164(2) . . . 2_557 ? N8 N8 O6 O6 -30.6(14) 2_557 . . 2_557 ? O5 N8 O6 O6 -42.2(11) 2_557 . . 2_557 ? O4 N8 O6 O6 140.6(10) . . . 2_557 ? O5 N8 O6 N8 -166(3) . . . 2_557 ? O5 N8 O6 N8 -11.6(9) 2_557 . . 2_557 ? O4 N8 O6 N8 171(2) . . . 2_557 ? O6 N8 O6 N8 30.6(14) 2_557 . . 2_557 ? N8 N8 O6 O5 166(3) 2_557 . . . ? O5 N8 O6 O5 154(3) 2_557 . . . ? O4 N8 O6 O5 -23.1(18) . . . . ? O6 N8 O6 O5 -164(2) 2_557 . . . ? O4 O5 O6 N8 143(3) . . . . ? N8 O5 O6 N8 -10(2) 2_557 . . . ? O5 O5 O6 N8 -18.1(19) 2_557 . . . ? N8 O5 O6 O6 -16(2) . . . 2_557 ? O4 O5 O6 O6 127.3(13) . . . 2_557 ? N8 O5 O6 O6 -25.9(7) 2_557 . . 2_557 ? O5 O5 O6 O6 -33.8(9) 2_557 . . 2_557 ? N8 O5 O6 N8 10(2) . . . 2_557 ? O4 O5 O6 N8 153.1(15) . . . 2_557 ? O5 O5 O6 N8 -8.0(6) 2_557 . . 2_557 ? C5 N3 C1 C2 0.3(4) . . . . ? Ag1 N3 C1 C2 -173.5(2) . . . . ? N3 C1 C2 C3 0.4(5) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? C1 C2 C3 N1 -179.9(3) . . . . ? N2 N1 C3 C4 167.4(3) 3_545 . . . ? N2 N1 C3 C2 -13.8(4) 3_545 . . . ? C2 C3 C4 C5 1.3(4) . . . . ? N1 C3 C4 C5 -179.8(3) . . . . ? C1 N3 C5 C4 -0.1(4) . . . . ? Ag1 N3 C5 C4 173.8(2) . . . . ? C3 C4 C5 N3 -0.7(5) . . . . ? C7 N4 C6 C10 1.3(4) . . . . ? Ag1 N4 C6 C10 177.1(2) . . . . ? C6 N4 C7 C8 -1.0(4) . . . . ? Ag1 N4 C7 C8 -176.6(2) . . . . ? N4 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 1.1(4) . . . . ? C7 C8 C9 N2 178.8(3) . . . . ? N1 N2 C9 C10 -169.0(3) 3_455 . . . ? N1 N2 C9 C8 13.2(4) 3_455 . . . ? N4 C6 C10 C9 -0.4(5) . . . . ? C8 C9 C10 C6 -0.8(4) . . . . ? N2 C9 C10 C6 -178.7(3) . . . . ? C15 N6 C11 C12 1.3(5) . . . . ? Ag2 N6 C11 C12 -172.7(2) . . . . ? N6 C11 C12 C13 -1.8(5) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C11 C12 C13 N5 178.9(3) . . . . ? N5 N5 C13 C12 156.6(3) 5_567 . . . ? N5 N5 C13 C14 -25.3(5) 5_567 . . . ? C12 C13 C14 C15 0.9(5) . . . . ? N5 C13 C14 C15 -177.2(3) . . . . ? C11 N6 C15 C14 0.4(5) . . . . ? Ag2 N6 C15 C14 174.6(2) . . . . ? C13 C14 C15 N6 -1.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.582 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.099 #===END