Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_GLOBAL _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Gleiter, Rolf' _publ_contact_author_address ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email 'rolf.gleiter@urz.uni-heidelberg.de' _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; paper to be submitted for publication in Dalton Trans. ; #========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reactions and Complexation Properties of 1,6-Diaminohex-3-yne and 1,4-Bis(2-aminoethyl)benzene ; loop_ _publ_author_name _publ_author_address 'Kunze, Andreas' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Gleiter, Rolf' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Oeser, Thomas' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #=== data_ak28_[4.AgCF3SO3]n _database_code_CSD 169018 _audit_creation_method SHELXL-97 _chemical_name_systematic; ?; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H16 Ag F3 N2 O3 S' _chemical_formula_weight 421.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.2075(8) _cell_length_b 10.3223(4) _cell_length_c 18.2280(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3049.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max .28 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details; ?; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15125 _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1816 _reflns_number_gt 1035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+0.4255P] 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 1816 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.019 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 0.87697(3) 0.0000 0.5000 0.03549(14) Uani 1 2 d S . . S1 S 1.0000 -0.33177(13) 0.71261(7) 0.0301(3) Uani 1 2 d S . . N1 N 0.88010(19) 0.0193(3) 0.38304(16) 0.0365(8) Uani 1 1 d . . . H1A H 0.8912 0.1045 0.3720 0.044 Uiso 1 1 calc R . . H1B H 0.9234 -0.0295 0.3656 0.044 Uiso 1 1 calc R . . F1 F 1.0000 -0.4716(3) 0.59225(18) 0.0556(11) Uani 1 2 d S . . C10 C 1.0000 -0.4870(6) 0.6650(3) 0.0401(14) Uani 1 2 d S . . O1 O 1.0000 -0.3686(3) 0.78904(19) 0.0342(9) Uani 1 2 d S . . C2 C 0.8042(2) -0.0196(4) 0.34263(19) 0.0362(10) Uani 1 1 d . . . H2A H 0.8108 0.0018 0.2900 0.043 Uiso 1 1 calc R . . H2B H 0.7566 0.0302 0.3617 0.043 Uiso 1 1 calc R . . F2 F 1.06626(17) -0.5562(2) 0.68221(15) 0.0645(8) Uani 1 1 d . . . O2 O 0.92497(19) -0.2727(3) 0.68789(15) 0.0531(9) Uani 1 1 d . . . C6 C 0.8224(2) -0.2869(4) 0.4663(2) 0.0296(10) Uani 1 1 d . . . H6 H 0.8728 -0.3124 0.4440 0.036 Uiso 1 1 calc R . . C3 C 0.7867(2) -0.1635(4) 0.35043(18) 0.0350(10) Uani 1 1 d . . . H3A H 0.7390 -0.1857 0.3190 0.042 Uiso 1 1 calc R . . H3B H 0.8350 -0.2123 0.3318 0.042 Uiso 1 1 calc R . . C4 C 0.7686(2) -0.2079(4) 0.42773(19) 0.0266(9) Uani 1 1 d . . . C5 C 0.6955(2) -0.1702(4) 0.4632(2) 0.0314(10) Uani 1 1 d . . . H5 H 0.6578 -0.1146 0.4387 0.038 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 0.0446(3) 0.0336(2) 0.0283(2) -0.0029(3) 0.000 0.000 S1 0.0385(9) 0.0235(7) 0.0281(8) 0.0036(6) 0.000 0.000 N1 0.0452(19) 0.030(2) 0.0343(16) 0.0003(15) 0.0107(16) -0.0022(17) F1 0.069(2) 0.065(3) 0.0332(19) -0.0092(18) 0.000 0.000 C10 0.041(4) 0.036(4) 0.043(3) 0.004(3) 0.000 0.000 O1 0.043(2) 0.033(2) 0.026(2) 0.0061(17) 0.000 0.000 C2 0.047(3) 0.041(3) 0.0213(19) 0.0057(19) 0.0006(17) 0.000(2) F2 0.0695(19) 0.0481(16) 0.0760(19) -0.0128(14) -0.0121(16) 0.0290(15) O2 0.067(2) 0.0462(19) 0.046(2) -0.0017(15) -0.0188(17) 0.0272(17) C6 0.024(2) 0.034(2) 0.031(2) -0.003(2) 0.0066(19) 0.0031(19) C3 0.045(3) 0.038(2) 0.022(2) -0.0011(19) 0.0042(19) -0.004(2) C4 0.038(3) 0.023(2) 0.019(2) -0.0029(16) -0.0010(18) -0.0044(17) C5 0.038(3) 0.028(2) 0.029(2) 0.002(2) -0.0058(19) 0.002(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 2.142(3) 4_556 ? Ag1 N1 2.142(3) . ? S1 O2 1.433(3) . ? S1 O2 1.433(3) 12_755 ? S1 O1 1.444(4) . ? S1 C10 1.822(6) . ? N1 C2 1.489(4) . ? F1 C10 1.335(6) . ? C10 F2 1.327(4) . ? C10 F2 1.327(4) 12_755 ? C2 C3 1.518(5) . ? C6 C4 1.385(5) . ? C6 C5 1.389(5) 13_646 ? C3 C4 1.511(4) . ? C4 C5 1.405(5) . ? C5 C6 1.389(5) 13_646 ? 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 177.28(16) 4_556 . ? O2 S1 O2 116.1(3) . 12_755 ? O2 S1 O1 114.54(14) . . ? O2 S1 O1 114.54(14) 12_755 . ? O2 S1 C10 102.98(16) . . ? O2 S1 C10 102.98(16) 12_755 . ? O1 S1 C10 103.2(2) . . ? C2 N1 Ag1 116.6(2) . . ? F2 C10 F2 108.0(5) . 12_755 ? F2 C10 F1 107.4(3) . . ? F2 C10 F1 107.4(3) 12_755 . ? F2 C10 S1 111.1(3) . . ? F2 C10 S1 111.1(3) 12_755 . ? F1 C10 S1 111.6(4) . . ? N1 C2 C3 111.8(3) . . ? C4 C6 C5 121.8(4) . 13_646 ? C4 C3 C2 114.9(3) . . ? C6 C4 C5 117.4(3) . . ? C6 C4 C3 122.1(4) . . ? C5 C4 C3 120.6(4) . . ? C6 C5 C4 120.8(4) 13_646 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.571 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.095 #===END data_772a12_[6.AgCF3SO3]2 _database_code_CSD 169019 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(2-(2'-aminoethyl)-1-pyrroline)-disilver complex (6) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Ag2 F6 N4 O6 S2' _chemical_formula_weight 738.24 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.901(3) _cell_length_b 11.362(3) _cell_length_c 10.975(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.98(3) _cell_angle_gamma 90.00 _cell_volume 1212.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 19.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _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 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.872 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method \w2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 3067 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.026 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.96 _reflns_number_total 2906 _reflns_number_gt 2285 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.4372P] 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 2906 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.076 _refine_ls_wR_factor_gt 0.069 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.09481(3) 0.41687(2) 0.10085(2) 0.04919(10) Uani 1 1 d . . . S1 S -0.28025(8) 0.25569(7) -0.07349(7) 0.04146(18) Uani 1 1 d . A . O1 O -0.2045(3) 0.3330(3) 0.0168(3) 0.0695(8) Uani 1 1 d . . . O2 O -0.3130(3) 0.1433(2) -0.0287(2) 0.0625(7) Uani 1 1 d . . . O3 O -0.2329(3) 0.2501(2) -0.1892(2) 0.0588(6) Uani 1 1 d . . . N1 N 0.1142(3) 0.2891(2) -0.0339(2) 0.0417(6) Uani 1 1 d . B . N8 N 0.0976(3) 0.5300(3) 0.2563(3) 0.0430(6) Uani 1 1 d . . . F1 F -0.526(3) 0.282(3) -0.217(2) 0.083(6) Uani 0.50 1 d P A 1 F2 F -0.436(3) 0.4368(18) -0.164(3) 0.109(6) Uani 0.50 1 d P A 1 F3 F -0.522(3) 0.317(2) -0.024(3) 0.086(5) Uani 0.50 1 d P A 1 F1A F -0.527(3) 0.259(3) -0.195(2) 0.095(6) Uani 0.50 1 d P A 2 F2A F -0.427(4) 0.430(2) -0.147(3) 0.136(10) Uani 0.50 1 d P A 2 F3A F -0.499(3) 0.353(2) -0.024(3) 0.095(6) Uani 0.50 1 d P A 2 C2 C 0.1282(3) 0.2991(3) -0.1454(3) 0.0411(7) Uani 1 1 d . B . C3 C 0.1206(5) 0.1836(3) -0.2125(3) 0.0588(10) Uani 1 1 d . . . C4 C 0.0804(15) 0.0999(14) -0.1210(16) 0.067(4) Uani 0.50 1 d P B 3 H4A H -0.0143 0.0750 -0.1476 0.080 Uiso 0.50 1 calc PR B 3 H4B H 0.1390 0.0308 -0.1124 0.080 Uiso 0.50 1 calc PR B 3 C4A C 0.1398(15) 0.0910(13) -0.1081(12) 0.059(3) Uani 0.50 1 d P B 4 H4C H 0.2345 0.0646 -0.0864 0.071 Uiso 0.50 1 calc PR B 4 H4D H 0.0800 0.0236 -0.1302 0.071 Uiso 0.50 1 calc PR B 4 C5 C 0.0971(5) 0.1640(3) -0.0021(3) 0.0546(9) Uani 1 1 d . . . C6 C 0.1482(4) 0.4131(3) -0.2050(4) 0.0499(8) Uani 1 1 d . . . C7 C -0.0295(4) 0.5516(3) 0.3053(3) 0.0498(8) Uani 1 1 d . . . C9 C -0.4455(4) 0.3264(4) -0.1162(4) 0.0626(10) Uani 1 1 d . . . H3A H 0.039(5) 0.178(4) -0.278(4) 0.089(15) Uiso 1 1 d . . . H3B H 0.194(4) 0.170(4) -0.253(4) 0.070(12) Uiso 1 1 d . . . H5A H 0.010(5) 0.147(4) 0.027(4) 0.070(12) Uiso 1 1 d . . . H5B H 0.156(5) 0.147(4) 0.075(4) 0.080(13) Uiso 1 1 d . . . H6A H 0.167(3) 0.470(3) -0.145(3) 0.049(10) Uiso 1 1 d . . . H6B H 0.233(4) 0.408(3) -0.238(4) 0.066(12) Uiso 1 1 d . . . H7A H -0.053(4) 0.487(3) 0.342(3) 0.050(10) Uiso 1 1 d . . . H7B H -0.015(4) 0.612(3) 0.372(4) 0.058(11) Uiso 1 1 d . . . H8A H 0.131(4) 0.594(3) 0.237(3) 0.048(10) Uiso 1 1 d . . . H8B H 0.159(4) 0.489(4) 0.313(4) 0.067(12) 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 0.06123(18) 0.04713(15) 0.04054(14) -0.00832(11) 0.01310(11) 0.00718(12) S1 0.0444(4) 0.0400(4) 0.0401(4) -0.0018(3) 0.0083(3) -0.0068(3) O1 0.0626(17) 0.0757(19) 0.0663(16) -0.0271(14) 0.0022(13) -0.0146(14) O2 0.0757(18) 0.0488(15) 0.0632(15) 0.0163(12) 0.0133(13) -0.0069(13) O3 0.0684(16) 0.0588(15) 0.0555(14) -0.0053(12) 0.0277(12) -0.0101(13) N1 0.0474(15) 0.0407(14) 0.0363(13) -0.0020(11) 0.0062(11) 0.0057(12) N8 0.0553(17) 0.0336(14) 0.0412(14) 0.0004(11) 0.0121(13) 0.0008(13) F1 0.061(5) 0.133(17) 0.047(4) -0.004(6) -0.010(3) 0.022(7) F2 0.159(15) 0.050(6) 0.102(8) 0.027(5) -0.012(8) 0.031(7) F3 0.062(6) 0.132(14) 0.069(5) 0.012(8) 0.026(4) 0.017(7) F1A 0.065(6) 0.104(9) 0.096(14) -0.015(11) -0.035(8) 0.012(5) F2A 0.144(14) 0.098(12) 0.17(2) 0.049(10) 0.033(14) 0.058(9) F3A 0.078(10) 0.130(14) 0.086(6) -0.011(9) 0.037(6) 0.034(9) C2 0.0406(16) 0.0417(16) 0.0410(15) -0.0024(13) 0.0083(13) 0.0064(13) C3 0.091(3) 0.044(2) 0.0441(19) -0.0040(15) 0.022(2) 0.008(2) C4 0.085(9) 0.034(5) 0.078(7) -0.005(4) 0.008(7) 0.030(6) C4A 0.099(10) 0.035(4) 0.047(5) 0.010(4) 0.025(7) 0.033(7) C5 0.072(3) 0.0454(19) 0.0465(19) 0.0098(15) 0.0118(18) 0.0118(18) C6 0.052(2) 0.0430(18) 0.060(2) 0.0000(17) 0.0245(17) 0.0006(16) C7 0.072(2) 0.0405(18) 0.0434(18) 0.0081(14) 0.0284(17) 0.0070(16) C9 0.068(3) 0.064(3) 0.054(2) 0.003(2) 0.0083(19) 0.014(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 2.107(3) . ? Ag1 N8 2.132(3) . ? Ag1 Ag1 3.2264(10) 3_565 ? S1 O1 1.426(3) . ? S1 O2 1.428(3) . ? S1 O3 1.436(2) . ? S1 C9 1.802(4) . ? N1 C2 1.263(4) . ? N1 C5 1.481(4) . ? N8 C7 1.480(4) . ? N8 H8A 0.84(4) . ? N8 H8B 0.92(4) . ? F1 C9 1.34(3) . ? F2 C9 1.37(2) . ? F3 C9 1.38(2) . ? F1A C9 1.31(3) . ? F2A C9 1.25(3) . ? F3A C9 1.26(3) . ? C2 C6 1.481(5) . ? C2 C3 1.499(5) . ? C3 C4 1.492(18) . ? C3 C4A 1.541(13) . ? C3 H3A 0.98(5) . ? C3 H3B 0.94(4) . ? C4 C5 1.476(17) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4A C5 1.551(14) . ? C4A H4C 0.9700 . ? C4A H4D 0.9700 . ? C5 H5A 0.99(5) . ? C5 H5B 0.95(4) . ? C6 C7 1.504(5) 3_565 ? C6 H6A 0.92(4) . ? C6 H6B 0.98(4) . ? C7 C6 1.504(5) 3_565 ? C7 H7A 0.89(4) . ? C7 H7B 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 N8 171.10(11) . . ? N1 Ag1 Ag1 92.34(7) . 3_565 ? N8 Ag1 Ag1 96.51(9) . 3_565 ? O1 S1 O2 115.81(17) . . ? O1 S1 O3 115.13(17) . . ? O2 S1 O3 113.49(16) . . ? O1 S1 C9 103.8(2) . . ? O2 S1 C9 103.5(2) . . ? O3 S1 C9 102.88(18) . . ? C2 N1 C5 110.6(3) . . ? C2 N1 Ag1 131.3(2) . . ? C5 N1 Ag1 117.8(2) . . ? C7 N8 Ag1 120.6(2) . . ? C7 N8 H8A 111(2) . . ? Ag1 N8 H8A 105(2) . . ? C7 N8 H8B 110(2) . . ? Ag1 N8 H8B 98(3) . . ? H8A N8 H8B 112(4) . . ? N1 C2 C6 123.7(3) . . ? N1 C2 C3 113.2(3) . . ? C6 C2 C3 123.1(3) . . ? C4 C3 C2 102.8(7) . . ? C4 C3 C4A 22.2(7) . . ? C2 C3 C4A 104.2(6) . . ? C4 C3 H3A 99(3) . . ? C2 C3 H3A 112(3) . . ? C4A C3 H3A 118(3) . . ? C4 C3 H3B 123(3) . . ? C2 C3 H3B 114(3) . . ? C4A C3 H3B 104(3) . . ? H3A C3 H3B 105(4) . . ? C5 C4 C3 106.3(11) . . ? C5 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? C5 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C3 C4A C5 100.3(8) . . ? C3 C4A H4C 111.7 . . ? C5 C4A H4C 111.7 . . ? C3 C4A H4D 111.7 . . ? C5 C4A H4D 111.7 . . ? H4C C4A H4D 109.5 . . ? C4 C5 N1 105.3(7) . . ? C4 C5 C4A 22.2(7) . . ? N1 C5 C4A 106.1(6) . . ? C4 C5 H5A 103(3) . . ? N1 C5 H5A 114(3) . . ? C4A C5 H5A 121(3) . . ? C4 C5 H5B 130(3) . . ? N1 C5 H5B 109(3) . . ? C4A C5 H5B 111(3) . . ? H5A C5 H5B 95(4) . . ? C2 C6 C7 113.9(3) . 3_565 ? C2 C6 H6A 109(2) . . ? C7 C6 H6A 111(2) 3_565 . ? C2 C6 H6B 108(2) . . ? C7 C6 H6B 111(2) 3_565 . ? H6A C6 H6B 103(3) . . ? N8 C7 C6 112.2(3) . 3_565 ? N8 C7 H7A 110(2) . . ? C6 C7 H7A 108(2) 3_565 . ? N8 C7 H7B 112(2) . . ? C6 C7 H7B 110(2) 3_565 . ? H7A C7 H7B 105(3) . . ? F2A C9 F3A 95(2) . . ? F2A C9 F1A 118(2) . . ? F3A C9 F1A 111.9(17) . . ? F2A C9 F1 103(2) . . ? F3A C9 F1 118.8(17) . . ? F1A C9 F1 15(3) . . ? F2A C9 F2 7(3) . . ? F3A C9 F2 98.6(18) . . ? F1A C9 F2 111.2(19) . . ? F1 C9 F2 96.1(18) . . ? F2A C9 F3 113.8(19) . . ? F3A C9 F3 20(2) . . ? F1A C9 F3 94.7(16) . . ? F1 C9 F3 104.6(16) . . ? F2 C9 F3 116.1(18) . . ? F2A C9 S1 108.7(16) . . ? F3A C9 S1 113.3(14) . . ? F1A C9 S1 109.0(14) . . ? F1 C9 S1 114.6(13) . . ? F2 C9 S1 112.6(15) . . ? F3 C9 S1 111.8(12) . . ? 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 N8 Ag1 N1 C2 -135.3(6) . . . . ? Ag1 Ag1 N1 C2 38.5(3) 3_565 . . . ? N8 Ag1 N1 C5 50.9(8) . . . . ? Ag1 Ag1 N1 C5 -135.2(2) 3_565 . . . ? N1 Ag1 N8 C7 -118.8(7) . . . . ? Ag1 Ag1 N8 C7 67.4(2) 3_565 . . . ? C5 N1 C2 C6 -179.6(3) . . . . ? Ag1 N1 C2 C6 6.3(5) . . . . ? C5 N1 C2 C3 1.2(4) . . . . ? Ag1 N1 C2 C3 -172.8(3) . . . . ? N1 C2 C3 C4 6.9(7) . . . . ? C6 C2 C3 C4 -172.2(6) . . . . ? N1 C2 C3 C4A -15.9(7) . . . . ? C6 C2 C3 C4A 164.9(6) . . . . ? C2 C3 C4 C5 -12.0(8) . . . . ? C4A C3 C4 C5 84(3) . . . . ? C4 C3 C4A C5 -67(3) . . . . ? C2 C3 C4A C5 21.9(9) . . . . ? C3 C4 C5 N1 12.9(8) . . . . ? C3 C4 C5 C4A -82(3) . . . . ? C2 N1 C5 C4 -9.1(7) . . . . ? Ag1 N1 C5 C4 165.9(6) . . . . ? C2 N1 C5 C4A 14.0(7) . . . . ? Ag1 N1 C5 C4A -171.1(6) . . . . ? C3 C4A C5 C4 69(3) . . . . ? C3 C4A C5 N1 -21.9(9) . . . . ? N1 C2 C6 C7 -112.7(4) . . . 3_565 ? C3 C2 C6 C7 66.4(4) . . . 3_565 ? Ag1 N8 C7 C6 -50.6(4) . . . 3_565 ? O1 S1 C9 F2A 53.1(17) . . . . ? O2 S1 C9 F2A 174.4(16) . . . . ? O3 S1 C9 F2A -67.2(17) . . . . ? O1 S1 C9 F3A -51.4(12) . . . . ? O2 S1 C9 F3A 69.9(12) . . . . ? O3 S1 C9 F3A -171.7(12) . . . . ? O1 S1 C9 F1A -176.7(13) . . . . ? O2 S1 C9 F1A -55.4(13) . . . . ? O3 S1 C9 F1A 63.0(13) . . . . ? O1 S1 C9 F1 167.9(15) . . . . ? O2 S1 C9 F1 -70.8(15) . . . . ? O3 S1 C9 F1 47.6(15) . . . . ? O1 S1 C9 F2 59.4(13) . . . . ? O2 S1 C9 F2 -179.3(13) . . . . ? O3 S1 C9 F2 -60.9(13) . . . . ? O1 S1 C9 F3 -73.3(12) . . . . ? O2 S1 C9 F3 48.0(12) . . . . ? O3 S1 C9 F3 166.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.386 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.074 #===END _eof # End of Crystallographic Information File