Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Schroder, Martin' 'Blake, A.' 'Caltagirone, Claudia' 'Cooke, Paul A.' 'Demartin, Francesco' 'Lippolis, Vito' 'Morale, Francesca' 'Tei, Lorenzo' 'Wilson, Claire' _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'M.Schroder@nottingham.ac.uk' _publ_section_title ; Nitrile functionalised pendant-arm derivatives of aza- and mixed donor macrocyclic ligands as new building blocks for inorganic crystal engineering ; data_da173 _database_code_CSD 173745 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H40 Ag2 B2 F8 N4 O2 S4' _chemical_formula_weight 910.18 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' '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 axis b unique' _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 6.9410(10) _cell_length_b 21.102(2) _cell_length_c 11.5340(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.480(10) _cell_angle_gamma 90.00 _cell_volume 1628.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type 'empirical "SADABS"' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 _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 'SMART CCD' _diffrn_measurement_method omega _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18557 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.7043 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.98 _reflns_number_total 4423 _reflns_number_observed 2245 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0405P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4423 _refine_ls_number_parameters 219 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_obs 0.0482 _refine_ls_wR_factor_all 0.1118 _refine_ls_wR_factor_obs 0.1089 _refine_ls_goodness_of_fit_all 0.828 _refine_ls_goodness_of_fit_obs 1.158 _refine_ls_restrained_S_all 0.852 _refine_ls_restrained_S_obs 1.193 _refine_ls_shift/esd_max 1.040 _refine_ls_shift/esd_mean 0.040 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 1.09186(6) 1.07503(2) -0.27939(4) 0.04478(14) Uani 1 d . . S10 S 1.2063(2) 1.18560(7) -0.18695(14) 0.0545(4) Uani 1 d . . S4 S 0.8152(3) 1.04736(8) -0.46447(14) 0.0617(4) Uani 1 d . . F1 F 0.6725(7) 0.8815(3) -0.1118(4) 0.124(2) Uani 1 d . . F2 F 0.8289(12) 0.9243(3) -0.2307(7) 0.182(3) Uani 1 d . . F3 F 0.6222(8) 0.8514(3) -0.3016(4) 0.136(2) Uani 1 d . . F4 F 0.8982(10) 0.8284(4) -0.1745(4) 0.178(3) Uani 1 d . . O7 O 1.1451(10) 1.1577(3) -0.4568(5) 0.127(2) Uani 1 d D . N1 N 0.7971(6) 1.1036(2) -0.2030(3) 0.0355(9) Uani 1 d . . N4A N 0.7341(6) 1.0015(2) 0.1575(4) 0.0438(11) Uani 1 d . . C9 C 1.1507(12) 1.2412(3) -0.3109(6) 0.070(2) Uani 1 d D . H9A H 1.0074(12) 1.2483(3) -0.3363(6) 0.178(47) Uiso 1 calc R . H9B H 1.2143(12) 1.2814(3) -0.2832(6) 0.087(22) Uiso 1 calc R . C8 C 1.2186(18) 1.2194(3) -0.4164(8) 0.139(4) Uani 1 d D . H8A H 1.1735(18) 1.2494(3) -0.4817(8) 0.233(60) Uiso 1 calc R . H8B H 1.3636(18) 1.2188(3) -0.3947(8) 2.000(954) Uiso 1 calc R . C6 C 0.9498(12) 1.1639(4) -0.5327(10) 0.151(5) Uani 1 d D . H6A H 0.9522(12) 1.1918(4) -0.5990(10) 0.086(22) Uiso 1 calc R . H6B H 0.8648(12) 1.1831(4) -0.4879(10) 0.101(32) Uiso 1 calc R . C5 C 0.8624(12) 1.1005(3) -0.5821(5) 0.078(2) Uani 1 d D . H5A H 0.9538(12) 1.0797(3) -0.6205(5) 0.292(81) Uiso 1 calc R . H5B H 0.7376(12) 1.1076(3) -0.6430(5) 0.137(33) Uiso 1 calc R . C3 C 0.6182(10) 1.0909(4) -0.4230(6) 0.069(2) Uani 1 d . . H3A H 0.6340(10) 1.1357(4) -0.4363(6) 0.187(49) Uiso 1 calc R . H3B H 0.4899(10) 1.0777(4) -0.4745(6) 0.161(41) Uiso 1 calc R . C2 C 0.6193(7) 1.0806(3) -0.2937(4) 0.0514(15) Uani 1 d . . H2A H 0.5025(7) 1.1013(3) -0.2799(4) 0.046(14) Uiso 1 calc R . H2B H 0.6058(7) 1.0355(3) -0.2812(4) 0.084(23) Uiso 1 calc R . C12 C 0.8001(8) 1.1723(2) -0.1918(5) 0.0464(14) Uani 1 d . . H12A H 0.6988(8) 1.1848(2) -0.1524(5) 0.053(15) Uiso 1 calc R . H12B H 0.7639(8) 1.1906(2) -0.2719(5) 0.044(14) Uiso 1 calc R . C11 C 0.9978(9) 1.2000(2) -0.1226(5) 0.0531(15) Uani 1 d . . H11A H 1.0316(9) 1.1827(2) -0.0417(5) 0.066(18) Uiso 1 calc R . H11B H 0.9818(9) 1.2454(2) -0.1161(5) 0.041(14) Uiso 1 calc R . C1A C 0.8314(7) 1.0700(2) -0.0882(4) 0.0365(11) Uani 1 d . . H1AA H 0.9666(7) 1.0789(2) -0.0409(4) 0.026(11) Uiso 1 calc R . H1AB H 0.8231(7) 1.0248(2) -0.1046(4) 0.062(17) Uiso 1 calc R . C2A C 0.6871(8) 1.0860(2) -0.0114(4) 0.0393(12) Uani 1 d . . H2AA H 0.7165(8) 1.1280(2) 0.0231(4) 0.044(14) Uiso 1 calc R . H2AB H 0.5505(8) 1.0859(2) -0.0615(4) 0.032(12) Uiso 1 calc R . C3A C 0.7093(7) 1.0393(2) 0.0847(4) 0.0363(11) Uani 1 d . . B1 B 0.7516(11) 0.8706(4) -0.2049(7) 0.057(2) Uani 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 0.0441(2) 0.0486(2) 0.0461(2) 0.0136(2) 0.0199(2) 0.0132(2) S10 0.0496(9) 0.0504(9) 0.0604(9) 0.0092(7) 0.0093(7) -0.0077(7) S4 0.0652(10) 0.0705(10) 0.0498(9) -0.0115(8) 0.0161(8) 0.0146(8) F1 0.109(4) 0.182(5) 0.098(3) 0.015(4) 0.058(3) 0.044(4) F2 0.246(8) 0.112(4) 0.252(8) -0.074(5) 0.179(7) -0.092(5) F3 0.110(4) 0.169(5) 0.103(4) -0.025(4) -0.019(3) -0.042(4) F4 0.197(6) 0.257(8) 0.073(3) 0.009(4) 0.024(4) 0.156(6) O7 0.162(7) 0.130(6) 0.095(4) 0.024(4) 0.042(4) -0.011(5) N1 0.037(2) 0.036(2) 0.037(2) 0.010(2) 0.017(2) 0.007(2) N4A 0.049(3) 0.043(3) 0.042(2) 0.011(2) 0.017(2) 0.009(2) C9 0.101(6) 0.043(4) 0.070(4) 0.018(3) 0.030(4) -0.012(4) C8 0.293(15) 0.046(5) 0.093(6) 0.009(5) 0.076(8) -0.023(7) C6 0.062(5) 0.102(7) 0.255(13) 0.123(8) -0.016(8) -0.013(6) C5 0.103(6) 0.100(6) 0.037(3) 0.019(3) 0.027(4) 0.035(5) C3 0.048(4) 0.101(6) 0.057(4) 0.001(4) 0.014(3) 0.014(3) C2 0.031(3) 0.080(5) 0.047(3) 0.017(3) 0.016(2) 0.008(3) C12 0.057(4) 0.041(3) 0.051(3) 0.012(3) 0.032(3) 0.013(3) C11 0.081(4) 0.030(3) 0.054(4) 0.003(3) 0.028(3) 0.002(3) C1A 0.041(3) 0.032(3) 0.037(3) 0.002(2) 0.012(2) 0.006(2) C2A 0.046(3) 0.034(3) 0.043(3) 0.012(2) 0.020(2) 0.008(2) C3A 0.032(3) 0.040(3) 0.039(3) -0.001(2) 0.014(2) 0.003(2) B1 0.049(4) 0.063(5) 0.058(4) -0.004(4) 0.012(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4A 2.266(4) 3_775 ? Ag1 N1 2.508(4) . ? Ag1 S4 2.529(2) . ? Ag1 S10 2.600(2) . ? S10 C9 1.809(6) . ? S10 C11 1.819(6) . ? S4 C3 1.814(6) . ? S4 C5 1.855(7) . ? F1 B1 1.351(8) . ? F2 B1 1.321(9) . ? F3 B1 1.296(8) . ? F4 B1 1.327(8) . ? O7 C6 1.410(5) . ? O7 C8 1.430(5) . ? N1 C12 1.455(6) . ? N1 C1A 1.465(6) . ? N1 C2 1.472(6) . ? N4A C3A 1.138(6) . ? N4A Ag1 2.266(4) 3_775 ? C9 C8 1.490(5) . ? C6 C5 1.517(5) . ? C3 C2 1.505(8) . ? C12 C11 1.508(8) . ? C1A C2A 1.542(7) . ? C2A C3A 1.461(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4A Ag1 N1 107.66(13) 3_775 . ? N4A Ag1 S4 121.19(12) 3_775 . ? N1 Ag1 S4 81.11(10) . . ? N4A Ag1 S10 109.34(12) 3_775 . ? N1 Ag1 S10 80.12(10) . . ? S4 Ag1 S10 129.29(5) . . ? C9 S10 C11 100.9(3) . . ? C9 S10 Ag1 106.3(2) . . ? C11 S10 Ag1 97.3(2) . . ? C3 S4 C5 100.4(3) . . ? C3 S4 Ag1 96.7(2) . . ? C5 S4 Ag1 103.6(3) . . ? C6 O7 C8 108.6(8) . . ? C12 N1 C1A 114.1(4) . . ? C12 N1 C2 112.5(4) . . ? C1A N1 C2 112.7(4) . . ? C12 N1 Ag1 106.1(3) . . ? C1A N1 Ag1 104.5(3) . . ? C2 N1 Ag1 106.2(3) . . ? C3A N4A Ag1 155.2(4) . 3_775 ? C8 C9 S10 113.4(5) . . ? O7 C8 C9 112.6(6) . . ? O7 C6 C5 111.9(7) . . ? C6 C5 S4 112.9(5) . . ? C2 C3 S4 112.6(4) . . ? N1 C2 C3 116.0(5) . . ? N1 C12 C11 114.9(4) . . ? C12 C11 S10 115.5(4) . . ? N1 C1A C2A 116.1(4) . . ? C3A C2A C1A 109.5(4) . . ? N4A C3A C2A 176.5(5) . . ? F3 B1 F2 107.7(7) . . ? F3 B1 F4 109.0(7) . . ? F2 B1 F4 107.9(8) . . ? F3 B1 F1 113.7(7) . . ? F2 B1 F1 107.9(7) . . ? F4 B1 F1 110.5(6) . . ? _refine_diff_density_max 1.193 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.110 data_agcn2s _database_code_CSD 173746 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H20 Ag B F4 N4 S' _chemical_formula_weight 447.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6037(11) _cell_length_b 13.542(2) _cell_length_c 15.674(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.598(13) _cell_angle_gamma 90.00 _cell_volume 1613.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 13.2 _cell_measurement_theta_max 27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method ? _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.732 _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 'Stoe Stadi-4' _diffrn_measurement_method omega/theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2877 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2848 _reflns_number_observed 2577 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0147P)^2^+2.5828P] 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 riding/model _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2832 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_obs 0.0238 _refine_ls_wR_factor_all 0.0551 _refine_ls_wR_factor_obs 0.0490 _refine_ls_goodness_of_fit_all 1.154 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.210 _refine_ls_restrained_S_obs 1.137 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.41847(3) 0.14952(2) 0.014230(13) 0.01875(7) Uani 1 d . . S1 S 0.66684(9) 0.14049(5) 0.11808(4) 0.01899(15) Uani 1 d . . N4 N 0.2581(3) 0.0862(2) 0.14451(14) 0.0162(5) Uani 1 d . . N7 N 0.3390(3) 0.2954(2) 0.10014(14) 0.0168(5) Uani 1 d . . C3 C 0.3926(3) 0.0286(2) 0.1902(2) 0.0184(6) Uani 1 d . . H3A H 0.4235(3) -0.0296(2) 0.1552(2) 0.022 Uiso 1 calc R . H3B H 0.3421(3) 0.0041(2) 0.2442(2) 0.022 Uiso 1 calc R . C8 C 0.4800(4) 0.3148(2) 0.1637(2) 0.0203(6) Uani 1 d . . H8A H 0.4443(4) 0.2865(2) 0.2191(2) 0.024 Uiso 1 calc R . H8B H 0.4915(4) 0.3871(2) 0.1713(2) 0.024 Uiso 1 calc R . C6 C 0.1729(4) 0.2651(2) 0.1414(2) 0.0200(6) Uani 1 d . . H6A H 0.0814(4) 0.2561(2) 0.0967(2) 0.024 Uiso 1 calc R . H6B H 0.1338(4) 0.3191(2) 0.1794(2) 0.024 Uiso 1 calc R . C2 C 0.5599(4) 0.0860(2) 0.2108(2) 0.0203(6) Uani 1 d . . H2A H 0.6443(4) 0.0411(2) 0.2397(2) 0.024 Uiso 1 calc R . H2B H 0.5311(4) 0.1395(2) 0.2514(2) 0.024 Uiso 1 calc R . C5 C 0.1869(4) 0.1701(2) 0.1936(2) 0.0182(6) Uani 1 d . . H5A H 0.2638(4) 0.1822(2) 0.2439(2) 0.022 Uiso 1 calc R . H5B H 0.0687(4) 0.1523(2) 0.2146(2) 0.022 Uiso 1 calc R . C9 C 0.6589(4) 0.2729(2) 0.1405(2) 0.0203(6) Uani 1 d . . H9A H 0.7419(4) 0.2870(2) 0.1880(2) 0.024 Uiso 1 calc R . H9B H 0.7017(4) 0.3086(2) 0.0897(2) 0.024 Uiso 1 calc R . C71 C 0.3108(4) 0.3850(2) 0.0473(2) 0.0225(6) Uani 1 d . . H71A H 0.4262(4) 0.4131(2) 0.0317(2) 0.027 Uiso 1 calc R . H71B H 0.2472(4) 0.4350(2) 0.0811(2) 0.027 Uiso 1 calc R . C73 C 0.1659(4) 0.4521(2) -0.0824(2) 0.0260(7) Uani 1 d . . C72 C 0.2058(5) 0.3627(2) -0.0339(2) 0.0379(8) Uani 1 d . . H72A H 0.2739(5) 0.3168(2) -0.0700(2) 0.045 Uiso 1 calc R . H72B H 0.0945(5) 0.3295(2) -0.0186(2) 0.045 Uiso 1 calc R . F1 F 0.8477(2) 0.22139(15) -0.04577(11) 0.0372(5) Uani 1 d . . F2 F 0.8681(3) 0.2996(2) -0.17300(13) 0.0549(6) Uani 1 d . . F3 F 0.6942(4) 0.3607(2) -0.07077(15) 0.0702(8) Uani 1 d . . F4 F 0.6198(3) 0.2215(2) -0.13905(14) 0.0587(7) Uani 1 d . . C41 C 0.1208(3) 0.0236(2) 0.1070(2) 0.0182(6) Uani 1 d . . H41A H 0.1752(3) -0.0207(2) 0.0645(2) 0.022 Uiso 1 calc R . H41B H 0.0352(3) 0.0661(2) 0.0763(2) 0.022 Uiso 1 calc R . N74 N 0.1346(4) 0.5206(2) -0.1209(2) 0.0360(7) Uani 1 d . . B1 B 0.7576(5) 0.2764(3) -0.1073(2) 0.0231(7) Uani 1 d . . C42 C 0.0200(4) -0.0404(2) 0.1728(2) 0.0211(6) Uani 1 d . . H42A H 0.0977(4) -0.0933(2) 0.1951(2) 0.025 Uiso 1 calc R . H42B H -0.0173(4) 0.0011(2) 0.2214(2) 0.025 Uiso 1 calc R . C43 C -0.1339(4) -0.0838(2) 0.1308(2) 0.0187(6) Uani 1 d . . N44 N -0.2539(3) -0.1128(2) 0.0949(2) 0.0217(5) Uani 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 0.01941(11) 0.02059(12) 0.01625(11) -0.00176(9) 0.00018(7) -0.00298(9) S1 0.0147(3) 0.0193(3) 0.0229(3) 0.0021(3) 0.0003(3) -0.0007(3) N4 0.0147(11) 0.0163(12) 0.0177(11) 0.0013(9) -0.0004(9) 0.0005(9) N7 0.0172(12) 0.0147(12) 0.0183(12) 0.0023(9) -0.0006(9) -0.0001(9) C3 0.0163(14) 0.0163(14) 0.0226(14) 0.0042(11) 0.0008(11) 0.0011(11) C8 0.0241(15) 0.0168(14) 0.0199(14) -0.0006(11) -0.0046(11) -0.0006(12) C6 0.0184(14) 0.0188(14) 0.0230(15) 0.0012(12) 0.0018(11) 0.0030(12) C2 0.0163(14) 0.0224(15) 0.0220(14) 0.0032(12) -0.0007(11) -0.0006(11) C5 0.0183(14) 0.0181(14) 0.0185(14) -0.0007(11) 0.0034(11) 0.0013(11) C9 0.0197(14) 0.0188(14) 0.0224(15) -0.0008(12) -0.0039(11) -0.0049(12) C71 0.028(2) 0.0161(14) 0.0239(15) 0.0022(12) -0.0019(12) -0.0018(12) C73 0.030(2) 0.025(2) 0.023(2) 0.0012(13) -0.0048(12) -0.0036(13) C72 0.057(2) 0.021(2) 0.036(2) 0.0105(14) -0.019(2) -0.006(2) F1 0.0352(10) 0.0470(12) 0.0293(10) 0.0095(9) -0.0002(8) 0.0041(9) F2 0.0374(12) 0.093(2) 0.0345(11) 0.0200(12) 0.0089(9) -0.0149(12) F3 0.118(2) 0.0473(14) 0.0456(14) -0.0046(11) 0.0061(14) 0.0326(15) F4 0.0596(15) 0.071(2) 0.0454(13) 0.0160(12) -0.0193(11) -0.0390(13) C41 0.0167(13) 0.0207(15) 0.0172(14) 0.0009(11) -0.0016(11) -0.0016(11) N74 0.050(2) 0.027(2) 0.0304(15) 0.0091(13) -0.0090(13) -0.0044(13) B1 0.026(2) 0.026(2) 0.017(2) -0.0001(14) 0.0018(13) -0.0052(14) C42 0.0167(14) 0.026(2) 0.0205(14) 0.0023(12) -0.0040(11) -0.0065(12) C43 0.0221(15) 0.0180(14) 0.0161(13) 0.0031(11) 0.0059(12) -0.0009(12) N44 0.0209(13) 0.0222(13) 0.0220(12) -0.0016(10) 0.0015(10) -0.0043(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 N44 2.166(2) 3 y Ag1 N7 2.470(2) . y Ag1 S1 2.4834(8) . y Ag1 N4 2.539(2) . y S1 C9 1.828(3) . ? S1 C2 1.828(3) . ? N4 C41 1.463(3) . ? N4 C3 1.467(3) . ? N4 C5 1.478(3) . ? N7 C8 1.479(3) . ? N7 C71 1.483(3) . ? N7 C6 1.483(3) . ? C3 C2 1.523(4) . ? C8 C9 1.522(4) . ? C6 C5 1.527(4) . ? C71 C72 1.524(4) . ? C73 N74 1.132(4) . ? C73 C72 1.460(4) . ? F1 B1 1.393(4) . ? F2 B1 1.373(4) . ? F3 B1 1.366(4) . ? F4 B1 1.374(4) . ? C41 C42 1.555(4) . ? C42 C43 1.460(4) . ? C43 N44 1.137(4) . ? N44 Ag1 2.166(2) 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 N44 Ag1 N7 118.13(8) 3 . y N44 Ag1 S1 159.26(7) 3 . y N7 Ag1 S1 82.57(5) . . y N44 Ag1 N4 106.21(8) 3 . y N7 Ag1 N4 73.09(7) . . y S1 Ag1 N4 79.90(5) . . y C9 S1 C2 103.12(13) . . ? C9 S1 Ag1 92.94(9) . . ? C2 S1 Ag1 101.50(9) . . ? C41 N4 C3 112.2(2) . . ? C41 N4 C5 113.0(2) . . ? C3 N4 C5 114.3(2) . . ? C41 N4 Ag1 102.66(15) . . ? C3 N4 Ag1 103.5(2) . . ? C5 N4 Ag1 109.9(2) . . ? C8 N7 C71 109.3(2) . . ? C8 N7 C6 111.7(2) . . ? C71 N7 C6 110.6(2) . . ? C8 N7 Ag1 109.2(2) . . ? C71 N7 Ag1 112.6(2) . . ? C6 N7 Ag1 103.3(2) . . ? N4 C3 C2 114.1(2) . . ? N7 C8 C9 114.6(2) . . ? N7 C6 C5 114.3(2) . . ? C3 C2 S1 114.5(2) . . ? N4 C5 C6 113.1(2) . . ? C8 C9 S1 116.3(2) . . ? N7 C71 C72 112.1(2) . . ? N74 C73 C72 179.1(3) . . ? C73 C72 C71 112.0(3) . . ? N4 C41 C42 114.3(2) . . ? F3 B1 F2 110.2(3) . . ? F3 B1 F4 109.4(3) . . ? F2 B1 F4 108.8(3) . . ? F3 B1 F1 109.3(3) . . ? F2 B1 F1 109.9(3) . . ? F4 B1 F1 109.2(3) . . ? C43 C42 C41 108.9(2) . . ? N44 C43 C42 175.9(3) . . ? C43 N44 Ag1 157.5(2) . 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 N44 Ag1 S1 C9 150.9(2) 3 . . . ? N7 Ag1 S1 C9 -25.81(11) . . . . ? N4 Ag1 S1 C9 -99.87(11) . . . . ? N44 Ag1 S1 C2 -105.1(2) 3 . . . ? N7 Ag1 S1 C2 78.22(11) . . . . ? N4 Ag1 S1 C2 4.16(11) . . . . ? N44 Ag1 N4 C41 12.4(2) 3 . . . ? N7 Ag1 N4 C41 127.5(2) . . . . ? S1 Ag1 N4 C41 -147.2(2) . . . . ? N44 Ag1 N4 C3 129.4(2) 3 . . . ? N7 Ag1 N4 C3 -115.5(2) . . . . ? S1 Ag1 N4 C3 -30.27(15) . . . . ? N44 Ag1 N4 C5 -108.1(2) 3 . . . ? N7 Ag1 N4 C5 7.0(2) . . . . ? S1 Ag1 N4 C5 92.3(2) . . . . ? N44 Ag1 N7 C8 -172.5(2) 3 . . . ? S1 Ag1 N7 C8 6.1(2) . . . . ? N4 Ag1 N7 C8 87.8(2) . . . . ? N44 Ag1 N7 C71 -50.9(2) 3 . . . ? S1 Ag1 N7 C71 127.8(2) . . . . ? N4 Ag1 N7 C71 -150.6(2) . . . . ? N44 Ag1 N7 C6 68.4(2) 3 . . . ? S1 Ag1 N7 C6 -112.9(2) . . . . ? N4 Ag1 N7 C6 -31.24(15) . . . . ? C41 N4 C3 C2 165.3(2) . . . . ? C5 N4 C3 C2 -64.2(3) . . . . ? Ag1 N4 C3 C2 55.3(2) . . . . ? C71 N7 C8 C9 -100.6(3) . . . . ? C6 N7 C8 C9 136.7(2) . . . . ? Ag1 N7 C8 C9 23.0(3) . . . . ? C8 N7 C6 C5 -61.1(3) . . . . ? C71 N7 C6 C5 176.9(2) . . . . ? Ag1 N7 C6 C5 56.2(2) . . . . ? N4 C3 C2 S1 -56.5(3) . . . . ? C9 S1 C2 C3 118.2(2) . . . . ? Ag1 S1 C2 C3 22.4(2) . . . . ? C41 N4 C5 C6 -95.0(3) . . . . ? C3 N4 C5 C6 134.9(2) . . . . ? Ag1 N4 C5 C6 19.0(3) . . . . ? N7 C6 C5 N4 -53.9(3) . . . . ? N7 C8 C9 S1 -55.4(3) . . . . ? C2 S1 C9 C8 -51.3(2) . . . . ? Ag1 S1 C9 C8 51.3(2) . . . . ? C8 N7 C71 C72 164.3(3) . . . . ? C6 N7 C71 C72 -72.3(3) . . . . ? Ag1 N7 C71 C72 42.7(3) . . . . ? N74 C73 C72 C71 159.1(229) . . . . ? N7 C71 C72 C73 175.4(3) . . . . ? C3 N4 C41 C42 59.4(3) . . . . ? C5 N4 C41 C42 -71.7(3) . . . . ? Ag1 N4 C41 C42 169.9(2) . . . . ? N4 C41 C42 C43 168.9(2) . . . . ? C41 C42 C43 N44 -28.9(41) . . . . ? C42 C43 N44 Ag1 44.9(44) . . . 3 ? _refine_diff_density_max 0.447 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.068 data_AGCNBF _database_code_CSD 173747 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 Ag B F4 N6 O2' _chemical_formula_weight 529.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.876(1) _cell_length_b 15.316(2) _cell_length_c 14.823(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.022(2) _cell_angle_gamma 90.00 _cell_volume 2132.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4803 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.65 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details 'Bruker SADABS' _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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13541 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.93 _reflns_number_total 5006 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0855P)^2^+0.5524P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5006 _refine_ls_number_parameters 263 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 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 Ag Ag 0.39023(4) 0.77740(2) 0.05715(2) 0.03356(14) Uani 1 1 d D . . N1 N 0.2438(4) 0.8013(3) 0.1584(3) 0.0366(9) Uani 1 1 d . A . C2 C 0.3249(6) 0.7783(4) 0.2558(4) 0.0436(12) Uani 1 1 d . . . H2A H 0.3100 0.7156 0.2660 0.052 Uiso 1 1 calc R A . H2B H 0.2877 0.8122 0.2999 0.052 Uiso 1 1 calc R . . C3 C 0.4837(6) 0.7953(3) 0.2797(4) 0.0397(11) Uani 1 1 d . A . H3A H 0.4985 0.8579 0.2687 0.048 Uiso 1 1 calc R . . H3B H 0.5300 0.7833 0.3479 0.048 Uiso 1 1 calc R . . N4 N 0.5534(4) 0.7429(3) 0.2244(3) 0.0403(10) Uani 1 1 d D A . C5 C 0.6817(8) 0.7950(5) 0.2162(5) 0.0349(16) Uiso 0.65 1 d PD A 1 H5A H 0.6564 0.8577 0.2089 0.042 Uiso 0.65 1 calc PR A 1 H5B H 0.7618 0.7880 0.2756 0.042 Uiso 0.65 1 calc PR A 1 C6 C 0.7297(8) 0.7660(5) 0.1330(5) 0.0401(17) Uiso 0.65 1 d PD A 1 H6A H 0.8236 0.7920 0.1380 0.048 Uiso 0.65 1 calc PR A 1 H6B H 0.7393 0.7016 0.1332 0.048 Uiso 0.65 1 calc PR A 1 C8 C 0.6306(11) 0.7383(6) -0.0351(7) 0.059(2) Uiso 0.65 1 d PD A 1 H8A H 0.5763 0.7688 -0.0941 0.071 Uiso 0.65 1 calc PR A 1 H8B H 0.7306 0.7340 -0.0351 0.071 Uiso 0.65 1 calc PR A 1 C5' C 0.7035(10) 0.7523(10) 0.2304(9) 0.036(3) Uiso 0.35 1 d PD A 2 H5'1 H 0.7437 0.6950 0.2211 0.043 Uiso 0.35 1 calc PR A 2 H5'2 H 0.7590 0.7753 0.2934 0.043 Uiso 0.35 1 calc PR A 2 C6' C 0.7094(15) 0.8154(9) 0.1528(7) 0.042(3) Uiso 0.35 1 d PD A 2 H6'1 H 0.8109 0.8231 0.1573 0.051 Uiso 0.35 1 calc PR A 2 H6'2 H 0.6747 0.8726 0.1674 0.051 Uiso 0.35 1 calc PR A 2 C8' C 0.6895(11) 0.7148(6) 0.0247(9) 0.035(3) Uiso 0.35 1 d PD A 2 H8'1 H 0.7425 0.6843 0.0840 0.042 Uiso 0.35 1 calc PR A 2 H8'2 H 0.7582 0.7304 -0.0093 0.042 Uiso 0.35 1 calc PR A 2 N7 N 0.6270(4) 0.7936(3) 0.0479(3) 0.0419(10) Uani 1 1 d D A . C9 C 0.5756(7) 0.6530(5) -0.0378(5) 0.075(2) Uani 0.35 1 d PD A 1 H9A H 0.6021 0.6170 -0.0853 0.090 Uiso 0.35 1 calc PR A 1 H9B H 0.6131 0.6246 0.0250 0.090 Uiso 0.35 1 calc PR A 1 C9' C 0.5756(7) 0.6530(5) -0.0378(5) 0.075(2) Uani 0.65 1 d P A 2 H9'1 H 0.5249 0.6825 -0.0983 0.090 Uiso 0.65 1 calc PR A 2 H9'2 H 0.6222 0.6001 -0.0528 0.090 Uiso 0.65 1 calc PR A 2 O10' O 0.4789(5) 0.6290(3) 0.0081(4) 0.0516(13) Uiso 0.70 1 d PD A 2 O10 O 0.4275(7) 0.6623(5) -0.0630(8) 0.055(3) Uiso 0.30 1 d PD A 1 C11 C 0.3582(7) 0.5859(4) -0.0517(5) 0.0698(19) Uani 1 1 d D . . H11A H 0.3851 0.5288 -0.0724 0.084 Uiso 0.30 1 calc PR A 2 H11B H 0.3119 0.6217 -0.1085 0.084 Uiso 0.30 1 calc PR A 2 H11C H 0.4343 0.5418 -0.0284 0.084 Uiso 0.70 1 calc PR A 1 H11D H 0.3026 0.5675 -0.1166 0.084 Uiso 0.70 1 calc PR A 1 C12 C 0.2637(8) 0.5742(3) 0.0056(5) 0.0635(18) Uani 1 1 d . A . H12A H 0.1843 0.5350 -0.0277 0.076 Uiso 1 1 calc R . . H12B H 0.3165 0.5469 0.0669 0.076 Uiso 1 1 calc R . . O13 O 0.2080(4) 0.6572(2) 0.0222(3) 0.0528(10) Uani 1 1 d . A . C14 C 0.1428(6) 0.6563(4) 0.0960(5) 0.0554(16) Uani 1 1 d . . . H14A H 0.2068 0.6271 0.1529 0.066 Uiso 1 1 calc R A . H14B H 0.0527 0.6229 0.0748 0.066 Uiso 1 1 calc R . . C15 C 0.1131(6) 0.7480(4) 0.1206(5) 0.0494(14) Uani 1 1 d . A . H15A H 0.0500 0.7767 0.0630 0.059 Uiso 1 1 calc R . . H15B H 0.0619 0.7460 0.1683 0.059 Uiso 1 1 calc R . . C1A C 0.2090(6) 0.8950(3) 0.1480(4) 0.0391(11) Uani 1 1 d . . . H1A1 H 0.1617 0.9080 0.0801 0.047 Uiso 1 1 calc R A . H1A2 H 0.2985 0.9291 0.1688 0.047 Uiso 1 1 calc R . . C2A C 0.1152(7) 0.9236(4) 0.2031(4) 0.0548(15) Uani 1 1 d . A . N3A N 0.0423(8) 0.9439(4) 0.2456(5) 0.084(2) Uani 1 1 d . . . C1B C 0.5700(6) 0.6517(4) 0.2553(4) 0.0554(17) Uani 1 1 d . . . H1B3 H 0.6043 0.6171 0.2103 0.066 Uiso 1 1 calc R A . H1B4 H 0.4761 0.6281 0.2542 0.066 Uiso 1 1 calc R . . C2B C 0.6714(6) 0.6419(4) 0.3521(4) 0.0521(15) Uani 1 1 d . A . C1C C 0.6340(6) 0.8785(4) 0.0086(4) 0.0467(13) Uani 1 1 d . . . H1C1 H 0.6235 0.9231 0.0543 0.056 Uiso 1 1 calc R A . H1C2 H 0.5525 0.8850 -0.0500 0.056 Uiso 1 1 calc R . . C2C C 0.7677(6) 0.8962(4) -0.0143(5) 0.0539(15) Uani 1 1 d . A . N3C N 0.8689(6) 0.9048(4) -0.0352(5) 0.0752(18) Uani 1 1 d . . . B B 0.5431(5) 1.0497(3) 0.2494(3) 0.0445(14) Uani 1 1 d D . . F1 F 0.4423(9) 1.0189(7) 0.2887(7) 0.080(4) Uiso 0.50 1 d PD B 1 F2 F 0.5312(8) 1.1387(3) 0.2247(5) 0.0492(18) Uiso 0.50 1 d PD B 1 F3 F 0.5079(7) 0.9995(4) 0.1637(4) 0.0322(16) Uiso 0.50 1 d PD B 1 F4 F 0.6906(6) 1.0385(5) 0.2922(5) 0.0520(18) Uiso 0.50 1 d PD B 1 F1' F 0.4785(8) 1.0049(4) 0.3080(5) 0.0440(18) Uiso 0.50 1 d PD B 2 F2' F 0.4767(7) 1.1303(4) 0.2264(5) 0.0470(17) Uiso 0.50 1 d PD B 2 F3' F 0.5489(9) 1.0027(5) 0.1735(5) 0.057(3) Uiso 0.50 1 d PD B 2 F4' F 0.6703(7) 1.0593(5) 0.3196(5) 0.068(2) Uiso 0.50 1 d PD B 2 N3B N 0.7501(5) 0.6383(4) 0.4271(3) 0.0551(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0301(2) 0.0349(2) 0.0334(2) -0.00363(15) 0.00652(14) -0.00140(15) N1 0.032(2) 0.035(2) 0.044(2) 0.0112(18) 0.0152(18) 0.0039(16) C2 0.044(3) 0.053(3) 0.037(3) 0.013(2) 0.018(2) 0.013(2) C3 0.042(3) 0.042(3) 0.031(2) -0.005(2) 0.005(2) 0.005(2) N4 0.028(2) 0.058(3) 0.032(2) -0.0101(19) 0.0034(17) 0.0008(19) N7 0.034(2) 0.036(2) 0.058(3) 0.009(2) 0.018(2) 0.0070(17) C9 0.070(4) 0.097(6) 0.062(4) -0.036(4) 0.027(4) 0.002(4) C9' 0.070(4) 0.097(6) 0.062(4) -0.036(4) 0.027(4) 0.002(4) C11 0.067(4) 0.049(3) 0.087(5) -0.014(3) 0.015(4) -0.004(3) C12 0.090(5) 0.030(3) 0.063(4) -0.006(3) 0.013(4) -0.013(3) O13 0.064(3) 0.0350(18) 0.057(2) 0.0041(17) 0.015(2) -0.0100(18) C14 0.043(3) 0.050(3) 0.067(4) 0.016(3) 0.007(3) -0.017(3) C15 0.031(3) 0.055(3) 0.063(4) 0.020(3) 0.014(3) -0.002(2) C1A 0.044(3) 0.039(2) 0.037(3) 0.004(2) 0.016(2) 0.009(2) C2A 0.061(4) 0.059(3) 0.050(3) 0.017(3) 0.026(3) 0.025(3) N3A 0.102(5) 0.092(5) 0.075(4) 0.025(4) 0.052(4) 0.049(4) C1B 0.049(3) 0.056(3) 0.042(3) -0.018(3) -0.012(3) 0.021(3) C2B 0.037(3) 0.067(4) 0.045(3) -0.018(3) 0.002(2) 0.013(3) C1C 0.043(3) 0.046(3) 0.056(3) 0.021(3) 0.022(3) 0.013(2) C2C 0.044(3) 0.051(3) 0.066(4) 0.023(3) 0.016(3) 0.008(3) N3C 0.050(3) 0.075(4) 0.106(5) 0.045(4) 0.033(3) 0.009(3) B 0.054(4) 0.034(3) 0.040(3) 0.001(2) 0.005(3) -0.001(3) N3B 0.045(3) 0.069(3) 0.042(3) -0.010(2) 0.002(2) 0.008(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 Ag N1 2.413(4) . Y Ag N4 2.559(4) . Y Ag N7 2.398(4) . Y Ag N3B 2.377(5) 4_575 Y Ag O10' 2.618(5) . Y Ag O13 2.514(4) . Y N1 C2 1.461(7) . ? N1 C1A 1.472(6) . ? N1 C15 1.483(7) . ? C2 C3 1.520(7) . ? C3 N4 1.462(7) . ? N4 C1B 1.464(7) . ? N4 C5' 1.464(9) . ? N4 C5 1.533(7) . ? C5 C6 1.519(8) . ? C6 N7 1.417(7) . ? C8 C9 1.411(8) . ? C8 N7 1.504(8) . ? C5' C6' 1.518(10) . ? C6' N7 1.552(9) . ? C8' N7 1.445(9) . ? N7 C1C 1.435(6) . ? C9 O10 1.401(7) . ? O10' C11 1.410(6) . ? O10 C11 1.391(7) . ? C11 C12 1.454(10) . ? C12 O13 1.436(7) . ? O13 C14 1.432(8) . ? C14 C15 1.503(9) . ? C1A C2A 1.478(8) . ? C2A N3A 1.137(8) . ? C1B C2B 1.481(7) . ? C2B N3B 1.143(7) . ? C1C C2C 1.487(8) . ? C2C N3C 1.141(8) . ? B F3' 1.351(6) . ? B F4' 1.369(6) . ? B F1 1.382(7) . ? B F2' 1.390(6) . ? B F1' 1.405(6) . ? B F2 1.407(6) . ? B F4 1.408(6) . ? B F3 1.433(6) . ? N3B Ag 2.377(5) 4_676 ? 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 Ag N4 75.37(13) . . Y N7 Ag N1 143.40(15) . . Y N3B Ag N1 96.41(17) 4_575 . Y N1 Ag O13 73.20(14) . . Y N1 Ag O10' 128.39(15) . . Y N7 Ag N4 75.17(14) . . Y N3B Ag N4 158.75(17) 4_575 . Y N4 Ag O10' 85.73(15) . . Y O13 Ag N4 104.16(13) . . Y N3B Ag N7 103.34(16) 4_575 . Y N7 Ag O10' 70.00(14) . . Y N7 Ag O13 135.46(14) . . Y N3B Ag O10' 114.02(18) 4_575 . Y N3B Ag O13 91.75(15) 4_575 . Y O13 Ag O10' 65.58(14) . . Y C2 N1 C1A 112.2(4) . . ? C2 N1 C15 112.8(4) . . ? C1A N1 C15 110.4(4) . . ? C2 N1 Ag 109.1(3) . . ? C1A N1 Ag 104.4(3) . . ? C15 N1 Ag 107.4(3) . . ? N1 C2 C3 113.5(4) . . ? N4 C3 C2 113.9(4) . . ? C3 N4 C1B 112.0(5) . . ? C3 N4 C5' 123.7(7) . . ? C1B N4 C5' 93.5(7) . . ? C3 N4 C5 107.6(4) . . ? C1B N4 C5 120.4(5) . . ? C5' N4 C5 26.9(5) . . ? C3 N4 Ag 99.5(3) . . ? C1B N4 Ag 118.4(3) . . ? C5' N4 Ag 111.2(5) . . ? C5 N4 Ag 96.0(4) . . ? C6 C5 N4 112.7(6) . . ? N7 C6 C5 108.5(6) . . ? C9 C8 N7 116.1(7) . . ? N4 C5' C6' 107.0(10) . . ? C5' C6' N7 119.4(10) . . ? C6 N7 C1C 121.4(5) . . ? C6 N7 C8' 73.8(6) . . ? C1C N7 C8' 125.6(7) . . ? C6 N7 C8 111.6(6) . . ? C1C N7 C8 99.4(5) . . ? C8' N7 C8 38.2(6) . . ? C6 N7 C6' 33.2(6) . . ? C1C N7 C6' 97.8(6) . . ? C8' N7 C6' 106.7(8) . . ? C8 N7 C6' 143.4(8) . . ? C6 N7 Ag 111.1(4) . . ? C1C N7 Ag 106.7(3) . . ? C8' N7 Ag 115.0(5) . . ? C8 N7 Ag 105.0(4) . . ? C6' N7 Ag 100.6(6) . . ? O10 C9 C8 105.9(7) . . ? C11 O10' Ag 106.9(4) . . ? C11 O10 C9 113.2(6) . . ? O10 C11 O10' 48.0(5) . . ? O10 C11 C12 127.1(7) . . ? O10' C11 C12 105.2(6) . . ? O13 C12 C11 109.9(5) . . ? C14 O13 C12 114.1(4) . . ? C14 O13 Ag 108.2(3) . . ? C12 O13 Ag 113.3(4) . . ? O13 C14 C15 110.1(4) . . ? N1 C15 C14 113.2(4) . . ? N1 C1A C2A 113.4(4) . . ? N3A C2A C1A 178.6(7) . . ? N4 C1B C2B 112.1(5) . . ? N3B C2B C1B 176.9(7) . . ? N7 C1C C2C 114.6(4) . . ? N3C C2C C1C 175.5(8) . . ? F3' B F4' 115.1(6) . . ? F3' B F1 113.0(6) . . ? F4' B F1 109.1(6) . . ? F3' B F2' 114.1(5) . . ? F4' B F2' 110.1(5) . . ? F1 B F2' 93.4(6) . . ? F3' B F1' 113.5(5) . . ? F4' B F1' 93.9(5) . . ? F1 B F1' 18.1(5) . . ? F2' B F1' 108.4(5) . . ? F3' B F2 108.8(6) . . ? F4' B F2 94.4(5) . . ? F1 B F2 115.3(6) . . ? F2' B F2 23.2(4) . . ? F1' B F2 128.1(6) . . ? F3' B F4 90.3(6) . . ? F4' B F4 24.8(4) . . ? F1 B F4 123.2(6) . . ? F2' B F4 124.2(5) . . ? F1' B F4 105.4(5) . . ? F2 B F4 103.1(5) . . ? F3' B F3 15.7(5) . . ? F4' B F3 130.2(6) . . ? F1 B F3 100.5(5) . . ? F2' B F3 107.0(5) . . ? F1' B F3 104.7(5) . . ? F2 B F3 108.1(5) . . ? F4 B F3 105.5(5) . . ? C2B N3B Ag 144.3(5) . 4_676 ? 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 N3B Ag N1 C2 -163.4(3) 4_575 . . . ? N7 Ag N1 C2 -40.7(4) . . . . ? O13 Ag N1 C2 106.7(3) . . . . ? N4 Ag N1 C2 -3.3(3) . . . . ? O10' Ag N1 C2 68.9(4) . . . . ? N3B Ag N1 C1A -43.3(3) 4_575 . . . ? N7 Ag N1 C1A 79.4(4) . . . . ? O13 Ag N1 C1A -133.2(3) . . . . ? N4 Ag N1 C1A 116.8(3) . . . . ? O10' Ag N1 C1A -171.0(3) . . . . ? N3B Ag N1 C15 74.0(3) 4_575 . . . ? N7 Ag N1 C15 -163.3(3) . . . . ? O13 Ag N1 C15 -15.9(3) . . . . ? N4 Ag N1 C15 -126.0(3) . . . . ? O10' Ag N1 C15 -53.7(4) . . . . ? C1A N1 C2 C3 -83.0(5) . . . . ? C15 N1 C2 C3 151.5(5) . . . . ? Ag N1 C2 C3 32.1(5) . . . . ? N1 C2 C3 N4 -63.5(6) . . . . ? C2 C3 N4 C1B -73.8(5) . . . . ? C2 C3 N4 C5' 175.7(7) . . . . ? C2 C3 N4 C5 151.7(5) . . . . ? C2 C3 N4 Ag 52.3(5) . . . . ? N3B Ag N4 C3 44.6(6) 4_575 . . . ? N7 Ag N4 C3 133.3(3) . . . . ? N1 Ag N4 C3 -24.8(3) . . . . ? O13 Ag N4 C3 -92.8(3) . . . . ? O10' Ag N4 C3 -156.3(3) . . . . ? N3B Ag N4 C1B 166.1(5) 4_575 . . . ? N7 Ag N4 C1B -105.2(4) . . . . ? N1 Ag N4 C1B 96.8(4) . . . . ? O13 Ag N4 C1B 28.8(4) . . . . ? O10' Ag N4 C1B -34.7(4) . . . . ? N3B Ag N4 C5' -87.4(8) 4_575 . . . ? N7 Ag N4 C5' 1.4(7) . . . . ? N1 Ag N4 C5' -156.7(7) . . . . ? O13 Ag N4 C5' 135.3(7) . . . . ? O10' Ag N4 C5' 71.8(7) . . . . ? N3B Ag N4 C5 -64.4(6) 4_575 . . . ? N7 Ag N4 C5 24.3(3) . . . . ? N1 Ag N4 C5 -133.8(4) . . . . ? O13 Ag N4 C5 158.2(3) . . . . ? O10' Ag N4 C5 94.7(3) . . . . ? C3 N4 C5 C6 -158.5(5) . . . . ? C1B N4 C5 C6 71.5(7) . . . . ? C5' N4 C5 C6 70.0(14) . . . . ? Ag N4 C5 C6 -56.6(6) . . . . ? N4 C5 C6 N7 71.4(8) . . . . ? C3 N4 C5' C6' -93.5(11) . . . . ? C1B N4 C5' C6' 147.0(10) . . . . ? C5 N4 C5' C6' -34.3(9) . . . . ? Ag N4 C5' C6' 24.6(12) . . . . ? N4 C5' C6' N7 -58.7(16) . . . . ? C5 C6 N7 C1C 87.5(7) . . . . ? C5 C6 N7 C8' -150.2(8) . . . . ? C5 C6 N7 C8 -155.9(6) . . . . ? C5 C6 N7 C6' 37.5(10) . . . . ? C5 C6 N7 Ag -39.1(6) . . . . ? C9 C8 N7 C6 72.5(9) . . . . ? C9 C8 N7 C1C -158.1(8) . . . . ? C9 C8 N7 C8' 63.7(10) . . . . ? C9 C8 N7 C6' 84.9(13) . . . . ? C9 C8 N7 Ag -47.9(9) . . . . ? C5' C6' N7 C6 -55.7(11) . . . . ? C5' C6' N7 C1C 165.7(12) . . . . ? C5' C6' N7 C8' -63.4(14) . . . . ? C5' C6' N7 C8 -76.9(17) . . . . ? C5' C6' N7 Ag 56.9(13) . . . . ? N3B Ag N7 C6 165.4(4) 4_575 . . . ? N1 Ag N7 C6 44.6(5) . . . . ? O13 Ag N7 C6 -88.0(4) . . . . ? N4 Ag N7 C6 7.2(4) . . . . ? O10' Ag N7 C6 -83.6(4) . . . . ? N3B Ag N7 C1C 31.0(4) 4_575 . . . ? N1 Ag N7 C1C -89.8(4) . . . . ? O13 Ag N7 C1C 137.6(3) . . . . ? N4 Ag N7 C1C -127.1(4) . . . . ? O10' Ag N7 C1C 142.1(4) . . . . ? N3B Ag N7 C8' -113.2(6) 4_575 . . . ? N1 Ag N7 C8' 126.0(6) . . . . ? O13 Ag N7 C8' -6.6(7) . . . . ? N4 Ag N7 C8' 88.7(6) . . . . ? O10' Ag N7 C8' -2.2(6) . . . . ? N3B Ag N7 C8 -73.8(5) 4_575 . . . ? N1 Ag N7 C8 165.4(4) . . . . ? O13 Ag N7 C8 32.8(5) . . . . ? N4 Ag N7 C8 128.0(5) . . . . ? O10' Ag N7 C8 37.2(4) . . . . ? N3B Ag N7 C6' 132.6(6) 4_575 . . . ? N1 Ag N7 C6' 11.8(6) . . . . ? O13 Ag N7 C6' -120.8(6) . . . . ? N4 Ag N7 C6' -25.6(6) . . . . ? O10' Ag N7 C6' -116.4(6) . . . . ? N7 C8 C9 O10 73.4(10) . . . . ? N3B Ag O10' C11 -51.8(5) 4_575 . . . ? N7 Ag O10' C11 -147.9(4) . . . . ? N1 Ag O10' C11 68.8(5) . . . . ? O13 Ag O10' C11 28.7(4) . . . . ? N4 Ag O10' C11 136.3(4) . . . . ? C8 C9 O10 C11 -168.6(8) . . . . ? C9 O10 C11 O10' 46.9(6) . . . . ? C9 O10 C11 C12 123.2(8) . . . . ? Ag O10' C11 O10 66.6(5) . . . . ? Ag O10' C11 C12 -60.0(5) . . . . ? O10 C11 C12 O13 21.1(10) . . . . ? O10' C11 C12 O13 69.5(7) . . . . ? C11 C12 O13 C14 -165.4(5) . . . . ? C11 C12 O13 Ag -40.9(6) . . . . ? N3B Ag O13 C14 -110.3(4) 4_575 . . . ? N7 Ag O13 C14 138.6(3) . . . . ? N1 Ag O13 C14 -14.1(3) . . . . ? N4 Ag O13 C14 55.5(3) . . . . ? O10' Ag O13 C14 134.0(4) . . . . ? N3B Ag O13 C12 122.1(4) 4_575 . . . ? N7 Ag O13 C12 11.0(5) . . . . ? N1 Ag O13 C12 -141.8(4) . . . . ? N4 Ag O13 C12 -72.1(4) . . . . ? O10' Ag O13 C12 6.4(4) . . . . ? C12 O13 C14 C15 169.4(5) . . . . ? Ag O13 C14 C15 42.2(5) . . . . ? C2 N1 C15 C14 -74.4(6) . . . . ? C1A N1 C15 C14 159.2(5) . . . . ? Ag N1 C15 C14 45.9(5) . . . . ? O13 C14 C15 N1 -62.7(6) . . . . ? C2 N1 C1A C2A -63.5(6) . . . . ? C15 N1 C1A C2A 63.3(6) . . . . ? Ag N1 C1A C2A 178.5(4) . . . . ? N1 C1A C2A N3A -18(29) . . . . ? C3 N4 C1B C2B -67.1(6) . . . . ? C5' N4 C1B C2B 61.6(8) . . . . ? C5 N4 C1B C2B 60.9(7) . . . . ? Ag N4 C1B C2B 177.9(4) . . . . ? N4 C1B C2B N3B 4(13) . . . . ? C6 N7 C1C C2C 58.9(8) . . . . ? C8' N7 C1C C2C -33.1(9) . . . . ? C8 N7 C1C C2C -63.6(7) . . . . ? C6' N7 C1C C2C 84.0(8) . . . . ? Ag N7 C1C C2C -172.4(4) . . . . ? N7 C1C C2C N3C 52(8) . . . . ? C1B C2B N3B Ag 0(13) . . . 4_676 ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.022 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.106 data_agcnsf _database_code_CSD 173748 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H16 Ag B F4 N2 S2' _chemical_formula_weight 411.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 31.961(5) _cell_length_b 6.893(4) _cell_length_c 13.144(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.000(10) _cell_angle_gamma 90.00 _cell_volume 2894.0(18) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13 _cell_measurement_theta_max 17 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Stoe Stadi-4' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3165 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2512 _reflns_number_gt 2334 _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^)+(0.0747P)^2^+12.2089P] 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 0.0034(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2512 _refine_ls_number_parameters 212 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.027 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 0.145140(10) 1.06648(5) 0.71758(3) 0.0308(2) Uani 1 1 d . . . N7 N 0.14778(11) 0.7163(6) 0.6828(3) 0.0272(8) Uani 1 1 d . . . C8 C 0.13264(15) 0.6711(7) 0.5779(3) 0.0334(10) Uani 1 1 d . . . H8A H 0.1031 0.6341 0.5795 0.040 Uiso 1 1 calc R . . H8B H 0.1482 0.5590 0.5533 0.040 Uiso 1 1 calc R . . C9 C 0.13704(15) 0.8377(8) 0.5026(3) 0.0370(12) Uani 1 1 d . . . H9A H 0.1244 0.7967 0.4371 0.044 Uiso 1 1 calc R . . H9B H 0.1670 0.8580 0.4924 0.044 Uiso 1 1 calc R . . S1 S 0.11426(4) 1.06945(18) 0.53564(9) 0.0336(3) Uani 1 1 d . . . C2 C 0.06022(15) 1.0026(9) 0.5575(4) 0.0362(11) Uani 1 1 d . . . H2A H 0.0423 1.0642 0.5049 0.043 Uiso 1 1 calc R . . H2B H 0.0575 0.8619 0.5489 0.043 Uiso 1 1 calc R . . C3 C 0.04389(15) 1.0569(8) 0.6610(4) 0.0379(12) Uani 1 1 d . . . H3A H 0.0152 1.0073 0.6642 0.045 Uiso 1 1 calc R . . H3B H 0.0422 1.1987 0.6641 0.045 Uiso 1 1 calc R . . S4 S 0.07253(4) 0.9753(2) 0.77456(9) 0.0339(3) Uani 1 1 d . . . C5 C 0.07554(15) 0.7133(8) 0.7580(4) 0.0388(12) Uani 1 1 d . . . H5A H 0.0601 0.6509 0.8123 0.047 Uiso 1 1 calc R . . H5B H 0.0615 0.6790 0.6930 0.047 Uiso 1 1 calc R . . C6 C 0.11981(16) 0.6319(8) 0.7595(4) 0.0362(11) Uani 1 1 d . . . H6A H 0.1327 0.6529 0.8274 0.043 Uiso 1 1 calc R . . H6B H 0.1181 0.4914 0.7484 0.043 Uiso 1 1 calc R . . C71 C 0.19045(14) 0.6454(7) 0.7050(4) 0.0334(10) Uani 1 1 d . . . H71A H 0.1913 0.5050 0.6933 0.040 Uiso 1 1 calc R . . H71B H 0.1979 0.6688 0.7769 0.040 Uiso 1 1 calc R . . C72 C 0.22251(14) 0.7439(8) 0.6393(4) 0.0351(11) Uani 1 1 d . . . H72A H 0.2187 0.6995 0.5688 0.042 Uiso 1 1 calc R . . H72B H 0.2181 0.8846 0.6404 0.042 Uiso 1 1 calc R . . C73 C 0.26506(15) 0.7000(8) 0.6762(4) 0.0355(11) Uani 1 1 d . . . N74 N 0.29786(12) 0.6653(6) 0.7072(3) 0.0379(9) Uani 1 1 d . . . B1 B 0.0000 0.5000 0.5000 0.080(4) Uani 1 2 d SD . . F1 F -0.0053(3) 0.6684(11) 0.5591(7) 0.072(2) Uani 0.50 1 d PD A -1 F2 F -0.0201(6) 0.492(3) 0.4196(9) 0.157(8) Uani 0.50 1 d PD A -1 F3 F 0.0404(3) 0.4503(15) 0.5165(12) 0.093(3) Uani 0.50 1 d PD A -1 F4 F -0.0232(3) 0.3620(13) 0.5756(8) 0.084(3) Uani 0.50 1 d PD A -1 B2 B 0.2500 0.2500 0.5000 0.050(2) Uani 1 2 d SD . . F5 F 0.2775(5) 0.0854(15) 0.5412(8) 0.111(4) Uani 0.50 1 d PD B -2 F6 F 0.2148(5) 0.195(4) 0.532(2) 0.220(12) Uani 0.50 1 d PD B -2 F7 F 0.2567(6) 0.222(2) 0.4010(6) 0.103(4) Uani 0.50 1 d PD B -2 F8 F 0.2697(7) 0.3949(19) 0.5380(19) 0.164(8) Uani 0.50 1 d PD B -2 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 0.0158(3) 0.0349(3) 0.0412(3) -0.00363(13) -0.00498(16) -0.00106(12) N7 0.0177(18) 0.035(2) 0.0291(18) 0.0050(16) -0.0002(14) 0.0052(15) C8 0.028(2) 0.040(3) 0.032(2) -0.007(2) -0.0031(18) 0.006(2) C9 0.021(2) 0.063(3) 0.027(2) 0.000(2) -0.0002(17) 0.012(2) S1 0.0192(6) 0.0489(8) 0.0325(6) 0.0113(5) -0.0006(5) 0.0027(5) C2 0.020(2) 0.054(3) 0.033(2) 0.006(2) -0.0063(19) 0.004(2) C3 0.013(2) 0.059(3) 0.042(3) 0.003(2) -0.0010(19) 0.007(2) S4 0.0156(6) 0.0563(8) 0.0300(6) -0.0018(5) 0.0028(4) 0.0032(5) C5 0.023(2) 0.049(3) 0.045(3) 0.009(2) 0.005(2) -0.012(2) C6 0.031(3) 0.041(3) 0.037(2) 0.011(2) 0.005(2) -0.001(2) C71 0.023(2) 0.037(3) 0.039(2) 0.006(2) -0.0053(19) 0.009(2) C72 0.017(2) 0.050(3) 0.039(2) 0.005(2) 0.0017(18) 0.011(2) C73 0.026(3) 0.042(3) 0.037(2) -0.003(2) 0.001(2) 0.008(2) N74 0.021(2) 0.048(2) 0.044(2) -0.003(2) -0.0033(17) 0.0090(18) B1 0.060(8) 0.048(6) 0.127(12) -0.018(7) -0.043(8) 0.002(6) F1 0.065(5) 0.054(5) 0.097(6) -0.010(4) 0.017(5) -0.005(4) F2 0.20(2) 0.188(17) 0.080(9) 0.007(10) -0.074(11) -0.098(16) F3 0.072(7) 0.080(7) 0.128(10) 0.005(6) 0.018(7) 0.018(5) F4 0.071(6) 0.057(5) 0.121(8) 0.024(5) -0.013(5) -0.012(4) B2 0.060(6) 0.053(5) 0.037(4) -0.010(4) 0.017(4) -0.015(5) F5 0.163(13) 0.084(7) 0.084(7) 0.006(5) -0.020(8) 0.040(7) F6 0.144(17) 0.27(3) 0.26(3) 0.09(2) 0.105(19) -0.044(19) F7 0.150(12) 0.108(9) 0.052(5) -0.014(5) 0.002(6) 0.049(9) F8 0.191(19) 0.082(9) 0.22(2) -0.071(12) -0.014(16) -0.042(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N74 2.153(4) 4_556 ? Ag1 N7 2.459(4) . ? Ag1 S4 2.5423(13) . ? Ag1 S1 2.5551(13) . ? N7 C71 1.468(5) . ? N7 C8 1.478(6) . ? N7 C6 1.489(6) . ? C8 C9 1.526(7) . ? C9 S1 1.814(5) . ? S1 C2 1.820(5) . ? C2 C3 1.521(7) . ? C3 S4 1.813(5) . ? S4 C5 1.822(6) . ? C5 C6 1.522(7) . ? C71 C72 1.523(7) . ? C72 C73 1.459(6) . ? C73 N74 1.137(6) . ? N74 Ag1 2.153(4) 4_546 ? B1 F2 1.218(9) . ? B1 F2 1.218(9) 5_566 ? B1 F3 1.347(9) 5_566 ? B1 F3 1.347(10) . ? B1 F1 1.410(7) 5_566 ? B1 F1 1.410(7) . ? B1 F4 1.579(8) 5_566 ? B1 F4 1.579(8) . ? B2 F6 1.274(11) 7_556 ? B2 F6 1.274(11) . ? B2 F8 1.274(10) 7_556 ? B2 F8 1.274(10) . ? B2 F7 1.341(8) . ? B2 F7 1.341(8) 7_556 ? B2 F5 1.524(9) 7_556 ? B2 F5 1.524(9) . ? 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 N74 Ag1 N7 111.23(15) 4_556 . ? N74 Ag1 S4 135.18(12) 4_556 . ? N7 Ag1 S4 81.36(9) . . ? N74 Ag1 S1 136.09(12) 4_556 . ? N7 Ag1 S1 81.27(9) . . ? S4 Ag1 S1 87.19(4) . . ? C71 N7 C8 112.8(4) . . ? C71 N7 C6 108.1(4) . . ? C8 N7 C6 111.4(4) . . ? C71 N7 Ag1 109.1(3) . . ? C8 N7 Ag1 111.6(3) . . ? C6 N7 Ag1 103.4(3) . . ? N7 C8 C9 114.3(4) . . ? C8 C9 S1 117.4(3) . . ? C9 S1 C2 101.9(3) . . ? C9 S1 Ag1 94.13(15) . . ? C2 S1 Ag1 100.83(16) . . ? C3 C2 S1 115.9(4) . . ? C2 C3 S4 118.8(3) . . ? C3 S4 C5 103.7(3) . . ? C3 S4 Ag1 96.93(17) . . ? C5 S4 Ag1 99.05(16) . . ? C6 C5 S4 114.7(4) . . ? N7 C6 C5 115.3(4) . . ? N7 C71 C72 112.2(4) . . ? C73 C72 C71 110.9(4) . . ? N74 C73 C72 178.4(5) . . ? C73 N74 Ag1 170.4(4) . 4_546 ? F2 B1 F2 180.0(17) . 5_566 ? F2 B1 F3 53.0(10) . 5_566 ? F2 B1 F3 127.0(10) 5_566 5_566 ? F2 B1 F3 127.0(10) . . ? F2 B1 F3 53.0(10) 5_566 . ? F3 B1 F3 180.0(13) 5_566 . ? F2 B1 F1 63.6(10) . 5_566 ? F2 B1 F1 116.4(10) 5_566 5_566 ? F3 B1 F1 104.6(6) 5_566 5_566 ? F3 B1 F1 75.4(6) . 5_566 ? F2 B1 F1 116.4(10) . . ? F2 B1 F1 63.6(10) 5_566 . ? F3 B1 F1 75.4(6) 5_566 . ? F3 B1 F1 104.6(6) . . ? F1 B1 F1 180.0(7) 5_566 . ? F2 B1 F4 74.1(8) . 5_566 ? F2 B1 F4 105.9(8) 5_566 5_566 ? F3 B1 F4 102.4(6) 5_566 5_566 ? F3 B1 F4 77.6(6) . 5_566 ? F1 B1 F4 94.6(5) 5_566 5_566 ? F1 B1 F4 85.4(5) . 5_566 ? F2 B1 F4 105.9(8) . . ? F2 B1 F4 74.1(8) 5_566 . ? F3 B1 F4 77.6(6) 5_566 . ? F3 B1 F4 102.4(6) . . ? F1 B1 F4 85.4(5) 5_566 . ? F1 B1 F4 94.6(5) . . ? F4 B1 F4 180.0(6) 5_566 . ? F6 B2 F6 180.0(6) 7_556 . ? F6 B2 F8 122.1(13) 7_556 7_556 ? F6 B2 F8 57.9(13) . 7_556 ? F6 B2 F8 57.9(13) 7_556 . ? F6 B2 F8 122.1(13) . . ? F8 B2 F8 180(2) 7_556 . ? F6 B2 F7 62.9(12) 7_556 . ? F6 B2 F7 117.1(12) . . ? F8 B2 F7 66.5(10) 7_556 . ? F8 B2 F7 113.5(10) . . ? F6 B2 F7 117.1(12) 7_556 7_556 ? F6 B2 F7 62.9(12) . 7_556 ? F8 B2 F7 113.5(10) 7_556 7_556 ? F8 B2 F7 66.5(10) . 7_556 ? F7 B2 F7 180.0(15) . 7_556 ? F6 B2 F5 99.6(11) 7_556 7_556 ? F6 B2 F5 80.4(11) . 7_556 ? F8 B2 F5 99.9(9) 7_556 7_556 ? F8 B2 F5 80.1(9) . 7_556 ? F7 B2 F5 82.7(6) . 7_556 ? F7 B2 F5 97.3(6) 7_556 7_556 ? F6 B2 F5 80.4(11) 7_556 . ? F6 B2 F5 99.6(11) . . ? F8 B2 F5 80.1(9) 7_556 . ? F8 B2 F5 99.9(9) . . ? F7 B2 F5 97.3(6) . . ? F7 B2 F5 82.7(6) 7_556 . ? F5 B2 F5 180.0(9) 7_556 . ? 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 N74 Ag1 N7 C71 -9.1(3) 4_556 . . . ? S4 Ag1 N7 C71 -144.4(3) . . . . ? S1 Ag1 N7 C71 127.2(3) . . . . ? N74 Ag1 N7 C8 -134.4(3) 4_556 . . . ? S4 Ag1 N7 C8 90.3(3) . . . . ? S1 Ag1 N7 C8 1.9(3) . . . . ? N74 Ag1 N7 C6 105.8(3) 4_556 . . . ? S4 Ag1 N7 C6 -29.5(3) . . . . ? S1 Ag1 N7 C6 -118.0(3) . . . . ? C71 N7 C8 C9 -97.8(5) . . . . ? C6 N7 C8 C9 140.5(4) . . . . ? Ag1 N7 C8 C9 25.4(4) . . . . ? N7 C8 C9 S1 -53.8(5) . . . . ? C8 C9 S1 C2 -55.1(4) . . . . ? C8 C9 S1 Ag1 46.9(4) . . . . ? N74 Ag1 S1 C9 89.7(3) 4_556 . . . ? N7 Ag1 S1 C9 -21.92(19) . . . . ? S4 Ag1 S1 C9 -103.61(17) . . . . ? N74 Ag1 S1 C2 -167.3(3) 4_556 . . . ? N7 Ag1 S1 C2 81.0(2) . . . . ? S4 Ag1 S1 C2 -0.7(2) . . . . ? C9 S1 C2 C3 124.1(4) . . . . ? Ag1 S1 C2 C3 27.5(4) . . . . ? S1 C2 C3 S4 -54.7(6) . . . . ? C2 C3 S4 C5 -55.3(5) . . . . ? C2 C3 S4 Ag1 45.9(4) . . . . ? N74 Ag1 S4 C3 147.4(2) 4_556 . . . ? N7 Ag1 S4 C3 -101.1(2) . . . . ? S1 Ag1 S4 C3 -19.51(19) . . . . ? N74 Ag1 S4 C5 -107.5(2) 4_556 . . . ? N7 Ag1 S4 C5 4.01(19) . . . . ? S1 Ag1 S4 C5 85.60(18) . . . . ? C3 S4 C5 C6 122.1(4) . . . . ? Ag1 S4 C5 C6 22.6(4) . . . . ? C71 N7 C6 C5 171.2(4) . . . . ? C8 N7 C6 C5 -64.4(6) . . . . ? Ag1 N7 C6 C5 55.6(5) . . . . ? S4 C5 C6 N7 -56.8(6) . . . . ? C8 N7 C71 C72 63.9(5) . . . . ? C6 N7 C71 C72 -172.5(4) . . . . ? Ag1 N7 C71 C72 -60.7(4) . . . . ? N7 C71 C72 C73 168.8(4) . . . . ? C71 C72 C73 N74 -28(21) . . . . ? C72 C73 N74 Ag1 36(23) . . . 4_546 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.803 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.127 data_AGNOCN _database_code_CSD 173749 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H32 Ag F2 N6 O4 P' _chemical_formula_weight 585.35 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8248(4) _cell_length_b 14.6417(7) _cell_length_c 17.5430(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.747(1) _cell_angle_gamma 90.00 _cell_volume 2428.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6833 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.95 _exptl_crystal_description flake _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15628 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.95 _reflns_number_total 5930 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5712 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Ag Ag 0.685016(17) 0.278966(11) 0.096591(9) 0.02042(6) Uani 1 1 d . . . N1 N 0.78585(19) 0.43181(12) 0.12598(10) 0.0201(4) Uani 1 1 d . . . C3 C 0.9922(2) 0.33531(16) 0.19747(13) 0.0241(5) Uani 1 1 d . . . H3A H 1.0159 0.3264 0.1466 0.029 Uiso 1 1 calc R . . H3B H 1.0820 0.3384 0.2400 0.029 Uiso 1 1 calc R . . C2 C 0.9134(2) 0.42485(15) 0.19472(13) 0.0235(5) Uani 1 1 d . . . H2A H 0.8844 0.4316 0.2442 0.028 Uiso 1 1 calc R . . H2B H 0.9783 0.4758 0.1923 0.028 Uiso 1 1 calc R . . N4 N 0.9090(2) 0.25652(12) 0.21188(11) 0.0205(4) Uani 1 1 d . . . C5 C 0.9593(2) 0.16979(15) 0.18726(13) 0.0243(5) Uani 1 1 d . . . H5A H 1.0438 0.1494 0.2287 0.029 Uiso 1 1 calc R . . H5B H 0.9879 0.1798 0.1380 0.029 Uiso 1 1 calc R . . C6 C 0.8474(3) 0.09503(15) 0.17308(13) 0.0253(5) Uani 1 1 d . . . H6A H 0.8915 0.0360 0.1658 0.030 Uiso 1 1 calc R . . H6B H 0.8114 0.0896 0.2204 0.030 Uiso 1 1 calc R . . N7 N 0.7277(2) 0.11297(13) 0.10315(10) 0.0228(4) Uani 1 1 d . . . C8 C 0.5974(3) 0.06572(16) 0.10896(15) 0.0301(5) Uani 1 1 d . . . H8A H 0.6233 0.0055 0.1345 0.036 Uiso 1 1 calc R . . H8B H 0.5356 0.0548 0.0549 0.036 Uiso 1 1 calc R . . C9 C 0.5163(3) 0.11908(16) 0.15551(14) 0.0272(5) Uani 1 1 d . . . H9A H 0.4429 0.0800 0.1680 0.033 Uiso 1 1 calc R . . H9B H 0.5809 0.1407 0.2059 0.033 Uiso 1 1 calc R . . O10 O 0.45197(17) 0.19495(11) 0.10835(9) 0.0275(4) Uani 1 1 d . . . C11 C 0.3638(3) 0.25021(17) 0.14286(15) 0.0302(5) Uani 1 1 d . . . H11A H 0.3163 0.2107 0.1736 0.036 Uiso 1 1 calc R . . H11B H 0.2896 0.2794 0.1001 0.036 Uiso 1 1 calc R . . C12 C 0.4471(3) 0.32346(16) 0.19669(14) 0.0288(5) Uani 1 1 d . . . H12A H 0.3835 0.3603 0.2196 0.035 Uiso 1 1 calc R . . H12B H 0.5203 0.2952 0.2406 0.035 Uiso 1 1 calc R . . O13 O 0.51189(17) 0.38005(10) 0.14988(9) 0.0256(4) Uani 1 1 d . . . C14 C 0.5975(3) 0.44936(16) 0.19582(14) 0.0267(5) Uani 1 1 d . . . H14A H 0.6620 0.4224 0.2440 0.032 Uiso 1 1 calc R . . H14B H 0.5373 0.4953 0.2124 0.032 Uiso 1 1 calc R . . C15 C 0.6821(2) 0.49415(15) 0.14610(14) 0.0246(5) Uani 1 1 d . . . H15A H 0.6164 0.5169 0.0965 0.030 Uiso 1 1 calc R . . H15B H 0.7329 0.5474 0.1752 0.030 Uiso 1 1 calc R . . C1A C 0.8304(2) 0.46701(16) 0.05756(12) 0.0236(5) Uani 1 1 d . . . H1A1 H 0.9091 0.4291 0.0499 0.028 Uiso 1 1 calc R . . H1A2 H 0.8657 0.5303 0.0689 0.028 Uiso 1 1 calc R . . C2A C 0.7090(3) 0.46630(18) -0.01888(13) 0.0289(5) Uani 1 1 d . . . H2A1 H 0.6548 0.4088 -0.0218 0.035 Uiso 1 1 calc R . . H2A2 H 0.6441 0.5177 -0.0178 0.035 Uiso 1 1 calc R . . C3A C 0.7610(3) 0.47423(17) -0.08923(14) 0.0300(5) Uani 1 1 d . . . N4A N 0.8002(3) 0.47931(18) -0.14459(13) 0.0474(6) Uani 1 1 d . . . C1B C 0.8910(3) 0.25412(16) 0.29224(13) 0.0232(5) Uani 1 1 d . . . H1B1 H 0.8245 0.2043 0.2952 0.028 Uiso 1 1 calc R . . H1B2 H 0.8477 0.3123 0.3023 0.028 Uiso 1 1 calc R . . C2B C 1.0295(3) 0.2396(2) 0.35783(14) 0.0357(6) Uani 1 1 d . . . H2B1 H 1.0749 0.1823 0.3473 0.043 Uiso 1 1 calc R . . H2B2 H 1.0950 0.2906 0.3568 0.043 Uiso 1 1 calc R . . C3B C 1.0049(3) 0.23452(17) 0.43610(14) 0.0324(6) Uani 1 1 d . . . N4B N 0.9864(3) 0.23007(16) 0.49690(14) 0.0465(6) Uani 1 1 d . . . C1C C 0.7609(3) 0.09150(15) 0.02834(13) 0.0240(5) Uani 1 1 d . . . H1C1 H 0.8437 0.1285 0.0254 0.029 Uiso 1 1 calc R . . H1C2 H 0.6800 0.1109 -0.0159 0.029 Uiso 1 1 calc R . . C2C C 0.7932(3) -0.01003(15) 0.01562(13) 0.0267(5) Uani 1 1 d . . . H2C1 H 0.8765 -0.0306 0.0579 0.032 Uiso 1 1 calc R . . H2C2 H 0.7114 -0.0487 0.0173 0.032 Uiso 1 1 calc R . . C3C C 0.8217(3) -0.01793(17) -0.06200(15) 0.0289(5) Uani 1 1 d . . . N4C N 0.8441(2) -0.01871(17) -0.12265(14) 0.0416(6) Uani 1 1 d . . . P P 0.42651(7) 0.24885(4) -0.08689(4) 0.02572(14) Uani 1 1 d . . . O1 O 0.5752(2) 0.26487(13) -0.04654(11) 0.0399(5) Uani 1 1 d . . . F2 F 0.33603(16) 0.31151(10) -0.04716(8) 0.0372(4) Uani 1 1 d . . . F3 F 0.3924(2) 0.30060(10) -0.16764(8) 0.0469(4) Uani 1 1 d . . . O4 O 0.3615(2) 0.15937(13) -0.10003(12) 0.0513(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02180(10) 0.01996(9) 0.01917(9) -0.00005(6) 0.00498(7) -0.00034(7) N1 0.0233(10) 0.0217(9) 0.0162(9) -0.0013(7) 0.0068(8) -0.0008(8) C3 0.0221(12) 0.0330(12) 0.0166(11) 0.0007(9) 0.0041(9) -0.0027(10) C2 0.0275(12) 0.0260(12) 0.0163(11) -0.0042(8) 0.0049(9) -0.0062(9) N4 0.0224(10) 0.0246(9) 0.0152(9) -0.0014(7) 0.0065(8) -0.0004(8) C5 0.0248(12) 0.0293(12) 0.0168(11) -0.0013(9) 0.0022(9) 0.0069(10) C6 0.0347(13) 0.0234(11) 0.0169(11) 0.0029(8) 0.0055(10) 0.0043(10) N7 0.0251(10) 0.0238(10) 0.0188(9) -0.0013(7) 0.0046(8) -0.0012(8) C8 0.0359(14) 0.0250(12) 0.0309(13) -0.0023(10) 0.0117(11) -0.0045(11) C9 0.0296(13) 0.0261(12) 0.0279(12) 0.0043(9) 0.0111(11) -0.0038(10) O10 0.0319(9) 0.0310(9) 0.0233(9) 0.0039(7) 0.0137(7) 0.0016(7) C11 0.0272(13) 0.0350(13) 0.0318(14) 0.0060(10) 0.0139(11) 0.0007(10) C12 0.0340(14) 0.0316(13) 0.0262(13) 0.0025(10) 0.0172(11) 0.0011(11) O13 0.0304(9) 0.0263(8) 0.0237(8) 0.0008(6) 0.0135(7) -0.0015(7) C14 0.0318(13) 0.0270(12) 0.0237(12) -0.0020(9) 0.0113(10) 0.0023(10) C15 0.0305(13) 0.0202(11) 0.0243(12) -0.0023(9) 0.0095(10) 0.0013(9) C1A 0.0278(13) 0.0252(11) 0.0178(11) -0.0001(9) 0.0063(10) -0.0037(9) C2A 0.0291(13) 0.0370(13) 0.0207(12) 0.0037(10) 0.0071(10) -0.0037(11) C3A 0.0312(14) 0.0346(14) 0.0232(13) 0.0016(10) 0.0058(11) 0.0004(11) N4A 0.0456(15) 0.0726(18) 0.0267(12) 0.0012(12) 0.0144(11) 0.0009(13) C1B 0.0259(12) 0.0277(11) 0.0166(11) 0.0021(9) 0.0070(9) 0.0034(9) C2B 0.0357(15) 0.0542(17) 0.0170(12) 0.0020(11) 0.0066(11) 0.0055(12) C3B 0.0417(16) 0.0332(14) 0.0201(13) 0.0007(10) 0.0047(11) 0.0061(11) N4B 0.0647(18) 0.0519(15) 0.0238(12) 0.0033(10) 0.0136(12) 0.0077(13) C1C 0.0296(13) 0.0250(12) 0.0166(11) -0.0001(8) 0.0050(10) -0.0009(10) C2C 0.0301(13) 0.0278(12) 0.0222(12) -0.0022(9) 0.0069(10) 0.0009(10) C3C 0.0258(13) 0.0309(13) 0.0292(13) -0.0044(10) 0.0063(11) 0.0011(10) N4C 0.0418(14) 0.0523(15) 0.0323(13) -0.0067(11) 0.0129(11) 0.0058(11) P 0.0313(4) 0.0192(3) 0.0242(3) 0.0000(2) 0.0034(3) 0.0014(2) O1 0.0337(11) 0.0557(12) 0.0272(10) 0.0023(8) 0.0029(8) -0.0031(9) F2 0.0457(9) 0.0363(8) 0.0305(8) -0.0033(6) 0.0117(7) 0.0087(7) F3 0.0775(13) 0.0419(9) 0.0202(7) 0.0062(6) 0.0117(8) 0.0261(8) O4 0.0664(14) 0.0271(10) 0.0646(14) -0.0134(9) 0.0248(12) -0.0143(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 Ag N1 2.4451(18) . y Ag O1 2.4579(18) . y Ag N7 2.4637(19) . y Ag N4 2.5742(19) . y N1 C1A 1.477(3) . ? N1 C15 1.481(3) . ? N1 C2 1.488(3) . ? C3 N4 1.475(3) . ? C3 C2 1.517(3) . ? N4 C1B 1.468(3) . ? N4 C5 1.469(3) . ? C5 C6 1.523(3) . ? C6 N7 1.475(3) . ? N7 C1C 1.470(3) . ? N7 C8 1.483(3) . ? C8 C9 1.505(3) . ? C9 O10 1.426(3) . ? O10 C11 1.434(3) . ? C11 C12 1.514(3) . ? C12 O13 1.432(3) . ? O13 C14 1.421(3) . ? C14 C15 1.508(3) . ? C1A C2A 1.534(3) . ? C2A C3A 1.463(3) . ? C3A N4A 1.141(3) . ? C1B C2B 1.539(3) . ? C2B C3B 1.459(4) . ? C3B N4B 1.132(3) . ? C1C C2C 1.549(3) . ? C2C C3C 1.467(3) . ? C3C N4C 1.144(3) . ? P O4 1.4484(19) . ? P O1 1.4588(19) . ? P F3 1.5606(15) . ? P F2 1.5666(16) . ? 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 Ag O1 109.43(6) . . y N1 Ag N7 147.04(6) . . y O1 Ag N7 89.25(6) . . y N1 Ag N4 74.94(6) . . y O1 Ag N4 146.79(6) . . y N7 Ag N4 74.87(6) . . y C1A N1 C15 110.71(17) . . ? C1A N1 C2 108.19(17) . . ? C15 N1 C2 109.38(17) . . ? C1A N1 Ag 109.90(13) . . ? C15 N1 Ag 110.41(13) . . ? C2 N1 Ag 108.18(13) . . ? N4 C3 C2 112.31(18) . . ? N1 C2 C3 113.29(17) . . ? C1B N4 C5 113.54(18) . . ? C1B N4 C3 113.59(18) . . ? C5 N4 C3 112.30(18) . . ? C1B N4 Ag 117.21(14) . . ? C5 N4 Ag 99.40(12) . . ? C3 N4 Ag 99.26(12) . . ? N4 C5 C6 112.56(19) . . ? N7 C6 C5 112.66(18) . . ? C1C N7 C6 112.60(18) . . ? C1C N7 C8 111.52(18) . . ? C6 N7 C8 111.61(18) . . ? C1C N7 Ag 104.21(13) . . ? C6 N7 Ag 107.56(13) . . ? C8 N7 Ag 108.93(14) . . ? N7 C8 C9 112.90(19) . . ? O10 C9 C8 107.81(19) . . ? C9 O10 C11 114.69(17) . . ? O10 C11 C12 112.1(2) . . ? O13 C12 C11 107.55(19) . . ? C14 O13 C12 112.02(17) . . ? O13 C14 C15 108.47(18) . . ? N1 C15 C14 113.13(18) . . ? N1 C1A C2A 112.11(18) . . ? C3A C2A C1A 111.7(2) . . ? N4A C3A C2A 178.9(3) . . ? N4 C1B C2B 114.1(2) . . ? C3B C2B C1B 111.8(2) . . ? N4B C3B C2B 179.5(3) . . ? N7 C1C C2C 115.96(18) . . ? C3C C2C C1C 107.91(19) . . ? N4C C3C C2C 176.1(3) . . ? O4 P O1 124.27(13) . . ? O4 P F3 108.54(11) . . ? O1 P F3 107.60(11) . . ? O4 P F2 108.75(11) . . ? O1 P F2 107.71(10) . . ? F3 P F2 96.41(8) . . ? P O1 Ag 127.83(11) . . ? 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 O1 Ag N1 C1A -29.84(15) . . . . ? N7 Ag N1 C1A 91.39(17) . . . . ? N4 Ag N1 C1A 115.62(14) . . . . ? O1 Ag N1 C15 92.56(14) . . . . ? N7 Ag N1 C15 -146.21(13) . . . . ? N4 Ag N1 C15 -121.97(14) . . . . ? O1 Ag N1 C2 -147.77(13) . . . . ? N7 Ag N1 C2 -26.5(2) . . . . ? N4 Ag N1 C2 -2.31(13) . . . . ? C1A N1 C2 C3 -86.2(2) . . . . ? C15 N1 C2 C3 153.09(18) . . . . ? Ag N1 C2 C3 32.8(2) . . . . ? N4 C3 C2 N1 -66.3(2) . . . . ? C2 C3 N4 C1B -69.7(2) . . . . ? C2 C3 N4 C5 159.76(18) . . . . ? C2 C3 N4 Ag 55.53(18) . . . . ? N1 Ag N4 C1B 95.73(15) . . . . ? O1 Ag N4 C1B -161.68(14) . . . . ? N7 Ag N4 C1B -97.64(16) . . . . ? N1 Ag N4 C5 -141.56(14) . . . . ? O1 Ag N4 C5 -38.98(19) . . . . ? N7 Ag N4 C5 25.06(13) . . . . ? N1 Ag N4 C3 -26.93(12) . . . . ? O1 Ag N4 C3 75.65(17) . . . . ? N7 Ag N4 C3 139.69(14) . . . . ? C1B N4 C5 C6 70.4(2) . . . . ? C3 N4 C5 C6 -158.98(18) . . . . ? Ag N4 C5 C6 -54.84(18) . . . . ? N4 C5 C6 N7 68.4(2) . . . . ? C5 C6 N7 C1C 78.2(2) . . . . ? C5 C6 N7 C8 -155.48(19) . . . . ? C5 C6 N7 Ag -36.0(2) . . . . ? N1 Ag N7 C1C -90.27(16) . . . . ? O1 Ag N7 C1C 35.97(14) . . . . ? N4 Ag N7 C1C -114.52(14) . . . . ? N1 Ag N7 C6 29.5(2) . . . . ? O1 Ag N7 C6 155.71(14) . . . . ? N4 Ag N7 C6 5.22(14) . . . . ? N1 Ag N7 C8 150.59(14) . . . . ? O1 Ag N7 C8 -83.16(14) . . . . ? N4 Ag N7 C8 126.34(15) . . . . ? C1C N7 C8 C9 -148.59(19) . . . . ? C6 N7 C8 C9 84.5(2) . . . . ? Ag N7 C8 C9 -34.1(2) . . . . ? N7 C8 C9 O10 72.2(2) . . . . ? C8 C9 O10 C11 176.72(19) . . . . ? C9 O10 C11 C12 86.8(2) . . . . ? O10 C11 C12 O13 59.9(3) . . . . ? C11 C12 O13 C14 -177.77(19) . . . . ? C12 O13 C14 C15 169.68(18) . . . . ? C1A N1 C15 C14 161.09(19) . . . . ? C2 N1 C15 C14 -79.8(2) . . . . ? Ag N1 C15 C14 39.2(2) . . . . ? O13 C14 C15 N1 -65.6(2) . . . . ? C15 N1 C1A C2A -66.7(2) . . . . ? C2 N1 C1A C2A 173.45(18) . . . . ? Ag N1 C1A C2A 55.5(2) . . . . ? N1 C1A C2A C3A -162.8(2) . . . . ? C1A C2A C3A N4A 132(17) . . . . ? C5 N4 C1B C2B 64.3(3) . . . . ? C3 N4 C1B C2B -65.6(3) . . . . ? Ag N4 C1B C2B 179.45(16) . . . . ? N4 C1B C2B C3B -178.0(2) . . . . ? C1B C2B C3B N4B 131(52) . . . . ? C6 N7 C1C C2C 63.7(3) . . . . ? C8 N7 C1C C2C -62.7(3) . . . . ? Ag N7 C1C C2C 179.97(16) . . . . ? N7 C1C C2C C3C 179.23(19) . . . . ? C1C C2C C3C N4C 11(4) . . . . ? O4 P O1 Ag -85.22(18) . . . . ? F3 P O1 Ag 146.48(12) . . . . ? F2 P O1 Ag 43.53(16) . . . . ? N1 Ag O1 P -117.20(14) . . . . ? N7 Ag O1 P 90.53(14) . . . . ? N4 Ag O1 P 150.76(11) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.809 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.081 data_CNAGBF _database_code_CSD 173750 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Ag B F4 N6' _chemical_formula_weight 441.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3140(10) _cell_length_b 14.846(2) _cell_length_c 10.6040(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.543(2) _cell_angle_gamma 90.00 _cell_volume 1620.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5089 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.59 _exptl_crystal_description 'block' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details 'SADABS' _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 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14047 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.0114 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.67 _reflns_number_total 3848 _reflns_number_gt 3553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.9725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier map' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3848 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.230510(12) 0.729269(8) 0.231875(12) 0.01970(5) Uani 1 1 d . . . N1 N 0.10963(13) 0.69025(9) 0.42026(13) 0.0182(3) Uani 1 1 d . . . C2 C 0.15168(17) 0.76106(12) 0.51214(17) 0.0209(3) Uani 1 1 d . . . H2A H 0.1086 0.7508 0.5918 0.025 Uiso 1 1 calc R . . H2B H 0.1226 0.8203 0.4783 0.025 Uiso 1 1 calc R . . C3 C 0.29886(17) 0.76393(11) 0.54141(17) 0.0201(3) Uani 1 1 d . . . H3A H 0.3204 0.8163 0.5966 0.024 Uiso 1 1 calc R . . H3B H 0.3260 0.7088 0.5885 0.024 Uiso 1 1 calc R . . N4 N 0.37321(14) 0.77055(9) 0.42645(14) 0.0185(3) Uani 1 1 d . . . C5 C 0.47751(16) 0.70266(12) 0.41957(17) 0.0206(3) Uani 1 1 d . . . H5A H 0.5422 0.7122 0.4912 0.025 Uiso 1 1 calc R . . H5B H 0.5220 0.7121 0.3406 0.025 Uiso 1 1 calc R . . C6 C 0.42945(17) 0.60581(11) 0.42294(16) 0.0202(3) Uani 1 1 d . . . H6A H 0.5035 0.5645 0.4128 0.024 Uiso 1 1 calc R . . H6B H 0.3950 0.5937 0.5064 0.024 Uiso 1 1 calc R . . N7 N 0.32645(13) 0.58691(9) 0.32235(13) 0.0183(3) Uani 1 1 d . . . C8 C 0.21077(17) 0.54166(11) 0.36874(17) 0.0209(3) Uani 1 1 d . . . H8A H 0.2376 0.4835 0.4079 0.025 Uiso 1 1 calc R . . H8B H 0.1488 0.5286 0.2960 0.025 Uiso 1 1 calc R . . C9 C 0.14225(17) 0.59789(11) 0.46508(17) 0.0213(3) Uani 1 1 d . . . H9A H 0.0613 0.5668 0.4856 0.026 Uiso 1 1 calc R . . H9B H 0.1989 0.6020 0.5437 0.026 Uiso 1 1 calc R . . C11 C -0.02791(16) 0.69907(13) 0.37759(16) 0.0217(3) Uani 1 1 d . . . H11A H -0.0527 0.6484 0.3203 0.026 Uiso 1 1 calc R . . H11B H -0.0406 0.7558 0.3293 0.026 Uiso 1 1 calc R . . C12 C -0.11351(17) 0.69925(13) 0.48521(18) 0.0244(4) Uani 1 1 d . . . N13 N -0.17209(18) 0.70307(13) 0.57240(18) 0.0343(4) Uani 1 1 d . . . C41 C 0.42432(17) 0.86166(12) 0.40893(17) 0.0225(3) Uani 1 1 d . . . H41A H 0.3536 0.9062 0.4151 0.027 Uiso 1 1 calc R . . H41B H 0.4581 0.8668 0.3238 0.027 Uiso 1 1 calc R . . C42 C 0.53024(17) 0.88129(12) 0.50662(18) 0.0234(4) Uani 1 1 d . . . N43 N 0.61007(17) 0.88577(12) 0.58517(17) 0.0319(4) Uani 1 1 d . . . C71 C 0.37877(17) 0.53869(12) 0.21587(17) 0.0216(3) Uani 1 1 d . . . H71A H 0.4590 0.5692 0.1918 0.026 Uiso 1 1 calc R . . H71B H 0.3148 0.5412 0.1424 0.026 Uiso 1 1 calc R . . C72 C 0.40868(17) 0.44303(12) 0.24650(17) 0.0230(3) Uani 1 1 d . . . N73 N 0.42445(16) 0.36934(11) 0.27455(16) 0.0289(3) Uani 1 1 d . . . B B 0.2446(2) 0.51277(17) 0.7929(2) 0.0311(5) Uani 1 1 d . . . F1 F 0.25890(17) 0.60539(11) 0.78326(15) 0.0586(4) Uani 1 1 d . . . F2 F 0.11360(13) 0.49299(11) 0.78757(17) 0.0550(4) Uani 1 1 d . . . F3 F 0.30344(18) 0.48236(11) 0.90585(14) 0.0572(4) Uani 1 1 d . . . F4 F 0.29961(16) 0.47145(14) 0.69279(15) 0.0633(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02129(8) 0.02048(8) 0.01738(8) 0.00300(4) 0.00170(5) -0.00022(4) N1 0.0181(6) 0.0176(6) 0.0192(7) -0.0014(5) 0.0021(5) -0.0015(5) C2 0.0225(8) 0.0211(8) 0.0193(8) -0.0031(6) 0.0022(6) -0.0013(6) C3 0.0227(8) 0.0201(8) 0.0173(8) -0.0013(6) -0.0012(6) -0.0017(6) N4 0.0186(7) 0.0160(7) 0.0205(7) 0.0002(5) -0.0016(5) -0.0020(5) C5 0.0181(8) 0.0210(8) 0.0225(8) -0.0001(7) -0.0018(6) 0.0000(6) C6 0.0211(8) 0.0186(8) 0.0204(8) 0.0003(6) -0.0026(6) 0.0021(6) N7 0.0189(7) 0.0173(6) 0.0187(7) -0.0014(5) 0.0001(5) 0.0002(5) C8 0.0234(8) 0.0162(7) 0.0231(8) 0.0007(6) 0.0021(6) -0.0021(6) C9 0.0240(8) 0.0184(8) 0.0218(8) 0.0021(6) 0.0044(6) -0.0031(6) C11 0.0194(8) 0.0253(8) 0.0207(8) -0.0018(7) 0.0039(6) -0.0029(7) C12 0.0200(8) 0.0255(9) 0.0279(9) -0.0041(7) 0.0043(7) -0.0022(7) N13 0.0326(9) 0.0358(9) 0.0358(10) -0.0090(8) 0.0131(7) -0.0049(7) C41 0.0237(8) 0.0188(8) 0.0242(9) 0.0025(6) -0.0052(7) -0.0045(6) C42 0.0233(8) 0.0184(7) 0.0283(9) 0.0009(7) -0.0003(7) -0.0039(6) N43 0.0298(8) 0.0327(9) 0.0321(9) -0.0004(7) -0.0063(7) -0.0055(7) C71 0.0229(8) 0.0203(8) 0.0214(8) -0.0016(6) 0.0011(6) 0.0021(6) C72 0.0207(8) 0.0250(9) 0.0232(9) -0.0063(7) 0.0005(6) 0.0011(7) N73 0.0301(8) 0.0230(8) 0.0339(9) -0.0054(7) 0.0048(7) 0.0020(6) B 0.0287(11) 0.0346(12) 0.0305(11) 0.0041(9) 0.0053(9) 0.0013(9) F1 0.0739(11) 0.0426(8) 0.0583(10) 0.0176(7) -0.0033(8) -0.0171(7) F2 0.0313(7) 0.0552(9) 0.0799(11) -0.0206(8) 0.0153(7) -0.0084(6) F3 0.0797(11) 0.0521(9) 0.0383(8) 0.0093(7) -0.0082(7) 0.0134(8) F4 0.0487(9) 0.0983(14) 0.0442(8) -0.0105(9) 0.0130(7) 0.0245(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.4877(14) . y Ag N4 2.5344(15) . y Ag N7 2.4997(14) . y Ag N13 2.2556(17) 4_675 y Ag N43 2.5771(18) 4_575 y Ag N73 2.6210(17) 2_555 y N1 C11 1.468(2) . ? N1 C2 1.480(2) . ? N1 C9 1.483(2) . ? C2 C3 1.531(2) . ? C3 N4 1.483(2) . ? N4 C41 1.468(2) . ? N4 C5 1.479(2) . ? C5 C6 1.522(2) . ? C6 N7 1.485(2) . ? N7 C71 1.468(2) . ? N7 C8 1.480(2) . ? C8 C9 1.526(2) . ? C11 C12 1.485(2) . ? C12 N13 1.137(2) . ? C41 C42 1.487(2) . ? C42 N43 1.136(2) . ? C71 C72 1.485(2) . ? C72 N73 1.143(2) . ? B F4 1.378(3) . ? B F2 1.380(3) . ? B F3 1.384(3) . ? B F1 1.387(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 Ag N4 72.38(5) . . y N1 Ag N7 72.61(5) . . y N7 Ag N4 72.29(4) . . y N13 Ag N1 166.97(6) 4_675 . y N13 Ag N4 103.86(6) 4_675 . y N13 Ag N7 118.70(6) 4_675 . y N13 Ag N43 93.61(7) 4_675 4_575 y N13 Ag N73 85.77(6) 4_675 2 y N43 Ag N73 103.87(5) 4_575 2 y N1 Ag N43 94.80(5) . 4_575 y N7 Ag N43 80.56(5) . 4_575 y N4 Ag N43 152.34(5) . 4_575 y N1 Ag N73 82.56(5) . 2 y N7 Ag N73 155.10(5) . 2 y N4 Ag N73 98.73(5) . 2 y C11 N1 C2 112.20(13) . . ? C11 N1 C9 112.15(13) . . ? C2 N1 C9 113.22(14) . . ? C11 N1 Ag 104.74(10) . . ? C2 N1 Ag 102.84(10) . . ? C9 N1 Ag 110.95(10) . . ? N1 C2 C3 113.57(14) . . ? N4 C3 C2 113.06(14) . . ? C41 N4 C5 110.71(14) . . ? C41 N4 C3 111.91(13) . . ? C5 N4 C3 114.20(13) . . ? C41 N4 Ag 108.35(10) . . ? C5 N4 Ag 100.53(10) . . ? C3 N4 Ag 110.45(10) . . ? N4 C5 C6 113.80(14) . . ? N7 C6 C5 112.40(14) . . ? C71 N7 C8 112.13(13) . . ? C71 N7 C6 111.35(13) . . ? C8 N7 C6 113.75(13) . . ? C71 N7 Ag 105.83(10) . . ? C8 N7 Ag 101.73(10) . . ? C6 N7 Ag 111.39(10) . . ? N7 C8 C9 112.99(13) . . ? N1 C9 C8 113.36(14) . . ? N1 C11 C12 111.85(15) . . ? N13 C12 C11 174.9(2) . . ? C12 N13 Ag 156.31(17) . 4_576 ? N4 C41 C42 110.28(14) . . ? N43 C42 C41 171.82(19) . . ? C42 N43 Ag 134.75(15) . 4_676 ? N7 C71 C72 112.31(14) . . ? N73 C72 C71 175.43(19) . . ? C72 N73 Ag 132.54(14) . 2_545 ? F4 B F2 108.79(19) . . ? F4 B F3 109.99(19) . . ? F2 B F3 110.0(2) . . ? F4 B F1 109.5(2) . . ? F2 B F1 108.43(19) . . ? F3 B F1 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 N13 Ag N1 C11 76.2(3) 4_675 . . . ? N7 Ag N1 C11 -132.36(11) . . . . ? N4 Ag N1 C11 151.23(11) . . . . ? N43 Ag N1 C11 -53.83(11) 4_575 . . . ? N73 Ag N1 C11 49.57(10) 2 . . . ? N13 Ag N1 C2 -41.2(3) 4_675 . . . ? N7 Ag N1 C2 110.20(11) . . . . ? N4 Ag N1 C2 33.79(10) . . . . ? N43 Ag N1 C2 -171.26(10) 4_575 . . . ? N73 Ag N1 C2 -67.87(10) 2 . . . ? N13 Ag N1 C9 -162.6(2) 4_675 . . . ? N7 Ag N1 C9 -11.15(10) . . . . ? N4 Ag N1 C9 -87.56(11) . . . . ? N43 Ag N1 C9 67.39(11) 4_575 . . . ? N73 Ag N1 C9 170.78(11) 2 . . . ? C11 N1 C2 C3 -170.10(14) . . . . ? C9 N1 C2 C3 61.70(18) . . . . ? Ag N1 C2 C3 -58.09(15) . . . . ? N1 C2 C3 N4 53.18(19) . . . . ? C2 C3 N4 C41 104.47(16) . . . . ? C2 C3 N4 C5 -128.76(15) . . . . ? C2 C3 N4 Ag -16.34(16) . . . . ? N13 Ag N4 C41 34.35(12) 4_675 . . . ? N1 Ag N4 C41 -132.69(12) . . . . ? N7 Ag N4 C41 150.48(12) . . . . ? N43 Ag N4 C41 161.96(12) 4_575 . . . ? N73 Ag N4 C41 -53.42(11) 2 . . . ? N13 Ag N4 C5 -81.79(11) 4_675 . . . ? N1 Ag N4 C5 111.17(10) . . . . ? N7 Ag N4 C5 34.34(9) . . . . ? N43 Ag N4 C5 45.82(16) 4_575 . . . ? N73 Ag N4 C5 -169.56(10) 2 . . . ? N13 Ag N4 C3 157.25(10) 4_675 . . . ? N1 Ag N4 C3 -9.79(10) . . . . ? N7 Ag N4 C3 -86.62(10) . . . . ? N43 Ag N4 C3 -75.14(15) 4_575 . . . ? N73 Ag N4 C3 69.48(10) 2 . . . ? C41 N4 C5 C6 -173.86(15) . . . . ? C3 N4 C5 C6 58.75(19) . . . . ? Ag N4 C5 C6 -59.50(15) . . . . ? N4 C5 C6 N7 55.43(19) . . . . ? C5 C6 N7 C71 101.27(16) . . . . ? C5 C6 N7 C8 -130.86(15) . . . . ? C5 C6 N7 Ag -16.61(16) . . . . ? N13 Ag N7 C71 -34.86(12) 4_675 . . . ? N1 Ag N7 C71 152.20(11) . . . . ? N4 Ag N7 C71 -131.28(11) . . . . ? N43 Ag N7 C71 54.10(10) 4_575 . . . ? N73 Ag N7 C71 156.74(12) 2 . . . ? N13 Ag N7 C8 -152.16(10) 4_675 . . . ? N1 Ag N7 C8 34.89(9) . . . . ? N4 Ag N7 C8 111.42(10) . . . . ? N43 Ag N7 C8 -63.21(10) 4_575 . . . ? N73 Ag N7 C8 39.44(17) 2 . . . ? N13 Ag N7 C6 86.30(12) 4_675 . . . ? N1 Ag N7 C6 -86.64(11) . . . . ? N4 Ag N7 C6 -10.12(10) . . . . ? N43 Ag N7 C6 175.26(11) 4_575 . . . ? N73 Ag N7 C6 -82.10(16) 2 . . . ? C71 N7 C8 C9 -170.96(14) . . . . ? C6 N7 C8 C9 61.58(18) . . . . ? Ag N7 C8 C9 -58.31(14) . . . . ? C11 N1 C9 C8 101.64(16) . . . . ? C2 N1 C9 C8 -130.14(15) . . . . ? Ag N1 C9 C8 -15.10(17) . . . . ? N7 C8 C9 N1 52.93(19) . . . . ? C2 N1 C11 C12 -55.73(19) . . . . ? C9 N1 C11 C12 73.02(18) . . . . ? Ag N1 C11 C12 -166.56(12) . . . . ? N1 C11 C12 N13 38(3) . . . . ? C11 C12 N13 Ag 52(3) . . . 4_576 ? C5 N4 C41 C42 -58.39(19) . . . . ? C3 N4 C41 C42 70.25(19) . . . . ? Ag N4 C41 C42 -167.73(12) . . . . ? N4 C41 C42 N43 7.9(15) . . . . ? C41 C42 N43 Ag 6.9(16) . . . 4_676 ? C8 N7 C71 C72 -55.21(18) . . . . ? C6 N7 C71 C72 73.52(17) . . . . ? Ag N7 C71 C72 -165.29(11) . . . . ? N7 C71 C72 N73 38(2) . . . . ? C71 C72 N73 Ag 48(3) . . . 2_545 ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.708 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.066 data_ag2n3c _database_code_CSD 173751 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 Ag2 F12 N10 P2' _chemical_formula_weight 1002.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.003(4) _cell_length_b 10.756(6) _cell_length_c 11.083(7) _cell_angle_alpha 101.80(5) _cell_angle_beta 101.96(5) _cell_angle_gamma 97.02(5) _cell_volume 900.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 502 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.479 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Stoe stadi-4' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3463 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0125 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3463 _reflns_number_gt 3237 _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^)+(0.0460P)^2^+2.7100P] 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 3463 _refine_ls_number_parameters 235 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.085 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.09134(4) 0.33007(3) 0.40739(3) 0.03299(12) Uani 1 1 d U . . N1 N 0.3548(4) 0.4054(3) 0.3404(3) 0.0315(7) Uani 1 1 d U . . C2 C 0.2754(5) 0.4493(4) 0.2275(4) 0.0380(9) Uani 1 1 d U . . H2A H 0.3674 0.4801 0.1891 0.046 Uiso 1 1 calc R . . H2B H 0.2186 0.5222 0.2545 0.046 Uiso 1 1 calc R . . C3 C 0.1428(5) 0.3451(4) 0.1271(4) 0.0371(9) Uani 1 1 d U . . H3A H 0.0926 0.3831 0.0577 0.045 Uiso 1 1 calc R . . H3B H 0.2030 0.2774 0.0922 0.045 Uiso 1 1 calc R . . N4 N 0.0006(4) 0.2855(3) 0.1742(3) 0.0332(7) Uani 1 1 d U . . C5 C -0.0233(6) 0.1432(4) 0.1443(4) 0.0394(9) Uani 1 1 d U . . H5A H -0.0622 0.1110 0.0519 0.047 Uiso 1 1 calc R . . H5B H -0.1161 0.1112 0.1813 0.047 Uiso 1 1 calc R . . C6 C 0.1356(6) 0.0869(4) 0.1906(4) 0.0365(9) Uani 1 1 d U . . H6A H 0.1040 -0.0072 0.1713 0.044 Uiso 1 1 calc R . . H6B H 0.2233 0.1078 0.1445 0.044 Uiso 1 1 calc R . . N7 N 0.2114(4) 0.1355(3) 0.3283(3) 0.0292(6) Uani 1 1 d U . . C8 C 0.4005(5) 0.1807(4) 0.3607(4) 0.0340(8) Uani 1 1 d U . . H8A H 0.4570 0.1105 0.3258 0.041 Uiso 1 1 calc R . . H8B H 0.4434 0.2029 0.4532 0.041 Uiso 1 1 calc R . . C9 C 0.4505(5) 0.2988(4) 0.3092(4) 0.0353(8) Uani 1 1 d U . . H9A H 0.5749 0.3312 0.3434 0.042 Uiso 1 1 calc R . . H9B H 0.4302 0.2714 0.2167 0.042 Uiso 1 1 calc R . . C11 C 0.4620(5) 0.5173(4) 0.4377(4) 0.0351(8) Uani 1 1 d U . . H11A H 0.3909 0.5840 0.4543 0.042 Uiso 1 1 calc R . . H11B H 0.5569 0.5534 0.4049 0.042 Uiso 1 1 calc R . . C41 C -0.1665(6) 0.3195(5) 0.1179(4) 0.0442(10) Uani 1 1 d U . . H41A H -0.2587 0.2723 0.1453 0.053 Uiso 1 1 calc R . . H41B H -0.1897 0.2907 0.0253 0.053 Uiso 1 1 calc R . . C42 C -0.1748(6) 0.4617(5) 0.1521(4) 0.0444(10) Uani 1 1 d U . . H42A H -0.0868 0.5091 0.1209 0.053 Uiso 1 1 calc R . . H42B H -0.2886 0.4756 0.1092 0.053 Uiso 1 1 calc R . . C43 C -0.1468(6) 0.5131(4) 0.2885(4) 0.0408(9) Uani 1 1 d U . . N44 N -0.1242(5) 0.5481(4) 0.3943(4) 0.0493(9) Uani 1 1 d U . . C71 C 0.1632(5) 0.0439(4) 0.4017(4) 0.0316(8) Uani 1 1 d U . . H71A H 0.0365 0.0207 0.3803 0.038 Uiso 1 1 calc R . . H71B H 0.2001 0.0871 0.4921 0.038 Uiso 1 1 calc R . . C72 C 0.2408(7) -0.0820(4) 0.3806(5) 0.0460(10) Uani 1 1 d U . . H72A H 0.1963 -0.1307 0.2923 0.055 Uiso 1 1 calc R . . H72B H 0.3673 -0.0604 0.3968 0.055 Uiso 1 1 calc R . . C73 C 0.1955(6) -0.1605(4) 0.4650(5) 0.0417(10) Uani 1 1 d U . . N74 N 0.1624(6) -0.2178(4) 0.5345(5) 0.0550(11) Uani 1 1 d U . . P P 0.37721(15) 0.19284(11) 0.82915(11) 0.0417(3) Uani 1 1 d DU . . F1 F 0.1849(4) 0.2199(4) 0.8100(4) 0.1087(15) Uani 1 1 d DU . . F2 F 0.3107(5) 0.0579(3) 0.7300(3) 0.0812(11) Uani 1 1 d DU . . F3 F 0.3478(7) 0.1290(4) 0.9396(4) 0.1133(17) Uani 1 1 d DU . . F4 F 0.3991(7) 0.2567(4) 0.7181(4) 0.1226(18) Uani 1 1 d DU . . F5 F 0.4395(5) 0.3269(3) 0.9277(3) 0.0880(12) Uani 1 1 d DU . . F6 F 0.5657(4) 0.1647(5) 0.8480(4) 0.1138(18) Uani 1 1 d DU . . 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 Ag 0.03642(18) 0.03551(18) 0.02534(17) 0.00263(12) 0.00966(12) 0.00353(12) N1 0.0291(15) 0.0290(15) 0.0354(17) 0.0090(13) 0.0063(13) 0.0007(12) C2 0.039(2) 0.039(2) 0.039(2) 0.0168(17) 0.0126(17) 0.0036(17) C3 0.044(2) 0.045(2) 0.0250(18) 0.0122(16) 0.0111(16) 0.0062(18) N4 0.0337(16) 0.0395(18) 0.0219(15) 0.0029(13) 0.0044(12) 0.0004(13) C5 0.043(2) 0.038(2) 0.0263(19) -0.0046(16) 0.0025(16) -0.0016(17) C6 0.048(2) 0.0303(19) 0.0240(18) -0.0036(15) 0.0075(16) -0.0020(16) N7 0.0321(16) 0.0268(15) 0.0267(15) 0.0031(12) 0.0082(12) 0.0010(12) C8 0.0301(18) 0.035(2) 0.036(2) 0.0087(16) 0.0093(16) 0.0016(15) C9 0.0305(19) 0.035(2) 0.040(2) 0.0074(16) 0.0125(16) 0.0011(15) C11 0.0310(19) 0.0294(19) 0.041(2) 0.0094(16) 0.0035(16) -0.0021(15) C41 0.041(2) 0.053(3) 0.029(2) 0.0008(18) -0.0024(17) 0.0046(19) C42 0.050(3) 0.053(3) 0.029(2) 0.0089(18) 0.0050(18) 0.015(2) C43 0.039(2) 0.044(2) 0.037(2) 0.0054(18) 0.0081(18) 0.0101(18) N44 0.054(2) 0.056(2) 0.035(2) 0.0025(18) 0.0094(17) 0.0169(19) C71 0.036(2) 0.0257(17) 0.0313(18) 0.0025(14) 0.0112(16) 0.0023(14) C72 0.055(3) 0.038(2) 0.054(3) 0.014(2) 0.027(2) 0.014(2) C73 0.039(2) 0.030(2) 0.056(3) 0.0089(19) 0.015(2) 0.0042(17) N74 0.053(2) 0.050(2) 0.073(3) 0.027(2) 0.026(2) 0.0100(19) P 0.0461(6) 0.0413(6) 0.0338(6) 0.0044(5) 0.0072(5) 0.0041(5) F1 0.057(2) 0.120(4) 0.126(4) -0.005(3) -0.001(2) 0.022(2) F2 0.101(3) 0.0552(19) 0.069(2) -0.0097(16) 0.008(2) 0.0054(18) F3 0.201(5) 0.098(3) 0.077(3) 0.044(2) 0.073(3) 0.053(3) F4 0.188(5) 0.106(3) 0.075(3) 0.048(3) 0.030(3) -0.015(3) F5 0.084(2) 0.060(2) 0.089(3) -0.0276(19) 0.005(2) -0.0019(18) F6 0.058(2) 0.169(5) 0.082(3) -0.038(3) -0.0015(19) 0.042(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N44 2.262(4) 2_566 ? Ag N4 2.464(4) . ? Ag N1 2.476(3) . ? Ag N7 2.483(3) . ? Ag N74 2.501(4) 2_556 ? N1 C2 1.475(5) . ? N1 C11 1.477(5) . ? N1 C9 1.478(5) . ? C2 C3 1.526(6) . ? C3 N4 1.477(5) . ? N4 C41 1.476(6) . ? N4 C5 1.477(5) . ? C5 C6 1.515(6) . ? C6 N7 1.477(5) . ? N7 C71 1.465(5) . ? N7 C8 1.476(5) . ? C8 C9 1.539(6) . ? C11 C11 1.527(8) 2_666 ? C41 C42 1.511(7) . ? C42 C43 1.459(6) . ? C43 N44 1.124(6) . ? N44 Ag 2.262(4) 2_566 ? C71 C72 1.552(6) . ? C72 C73 1.452(6) . ? C73 N74 1.132(6) . ? N74 Ag 2.501(4) 2_556 ? P F6 1.555(3) . ? P F4 1.556(3) . ? P F3 1.564(3) . ? P F5 1.573(3) . ? P F1 1.581(4) . ? P F2 1.585(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 N44 Ag N4 153.55(14) 2_566 . ? N44 Ag N1 105.16(15) 2_566 . ? N4 Ag N1 75.10(12) . . ? N44 Ag N7 131.46(13) 2_566 . ? N4 Ag N7 74.52(12) . . ? N1 Ag N7 73.13(11) . . ? N44 Ag N74 80.61(17) 2_566 2_556 ? N4 Ag N74 103.16(15) . 2_556 ? N1 Ag N74 170.56(13) . 2_556 ? N7 Ag N74 97.44(13) . 2_556 ? C2 N1 C11 109.1(3) . . ? C2 N1 C9 112.5(3) . . ? C11 N1 C9 113.2(3) . . ? C2 N1 Ag 100.1(2) . . ? C11 N1 Ag 110.0(2) . . ? C9 N1 Ag 111.1(2) . . ? N1 C2 C3 113.9(3) . . ? N4 C3 C2 114.5(3) . . ? C41 N4 C5 106.7(3) . . ? C41 N4 C3 111.1(3) . . ? C5 N4 C3 113.2(3) . . ? C41 N4 Ag 117.6(3) . . ? C5 N4 Ag 99.3(2) . . ? C3 N4 Ag 108.5(2) . . ? N4 C5 C6 115.5(3) . . ? N7 C6 C5 112.9(3) . . ? C71 N7 C8 111.7(3) . . ? C71 N7 C6 112.6(3) . . ? C8 N7 C6 113.6(3) . . ? C71 N7 Ag 104.9(2) . . ? C8 N7 Ag 104.1(2) . . ? C6 N7 Ag 109.1(2) . . ? N7 C8 C9 112.6(3) . . ? N1 C9 C8 114.4(3) . . ? N1 C11 C11 112.8(4) . 2_666 ? N4 C41 C42 114.6(4) . . ? C43 C42 C41 112.8(4) . . ? N44 C43 C42 177.2(5) . . ? C43 N44 Ag 164.2(4) . 2_566 ? N7 C71 C72 115.2(3) . . ? C73 C72 C71 110.3(4) . . ? N74 C73 C72 177.4(5) . . ? C73 N74 Ag 141.5(4) . 2_556 ? F6 P F4 91.2(3) . . ? F6 P F3 91.0(2) . . ? F4 P F3 177.9(3) . . ? F6 P F5 91.4(2) . . ? F4 P F5 91.0(2) . . ? F3 P F5 89.3(2) . . ? F6 P F1 179.4(3) . . ? F4 P F1 89.2(2) . . ? F3 P F1 88.6(2) . . ? F5 P F1 89.0(2) . . ? F6 P F2 89.7(2) . . ? F4 P F2 89.3(2) . . ? F3 P F2 90.5(2) . . ? F5 P F2 178.9(2) . . ? F1 P F2 89.9(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 N44 Ag N1 C2 -119.8(3) 2_566 . . . ? N4 Ag N1 C2 32.8(2) . . . . ? N7 Ag N1 C2 110.8(3) . . . . ? N74 Ag N1 C2 113.3(8) 2_556 . . . ? N44 Ag N1 C11 -5.0(3) 2_566 . . . ? N4 Ag N1 C11 147.6(3) . . . . ? N7 Ag N1 C11 -134.4(3) . . . . ? N74 Ag N1 C11 -131.9(8) 2_556 . . . ? N44 Ag N1 C9 121.1(3) 2_566 . . . ? N4 Ag N1 C9 -86.3(3) . . . . ? N7 Ag N1 C9 -8.3(2) . . . . ? N74 Ag N1 C9 -5.7(9) 2_556 . . . ? C11 N1 C2 C3 -172.4(3) . . . . ? C9 N1 C2 C3 61.1(4) . . . . ? Ag N1 C2 C3 -56.9(4) . . . . ? N1 C2 C3 N4 55.7(5) . . . . ? C2 C3 N4 C41 112.3(4) . . . . ? C2 C3 N4 C5 -127.6(4) . . . . ? C2 C3 N4 Ag -18.4(4) . . . . ? N44 Ag N4 C41 -41.3(5) 2_566 . . . ? N1 Ag N4 C41 -135.5(3) . . . . ? N7 Ag N4 C41 148.3(3) . . . . ? N74 Ag N4 C41 54.1(3) 2_556 . . . ? N44 Ag N4 C5 -155.7(3) 2_566 . . . ? N1 Ag N4 C5 110.1(3) . . . . ? N7 Ag N4 C5 33.8(2) . . . . ? N74 Ag N4 C5 -60.4(3) 2_556 . . . ? N44 Ag N4 C3 85.8(4) 2_566 . . . ? N1 Ag N4 C3 -8.4(2) . . . . ? N7 Ag N4 C3 -84.6(3) . . . . ? N74 Ag N4 C3 -178.8(3) 2_556 . . . ? C41 N4 C5 C6 178.4(3) . . . . ? C3 N4 C5 C6 55.9(4) . . . . ? Ag N4 C5 C6 -59.0(4) . . . . ? N4 C5 C6 N7 54.8(5) . . . . ? C5 C6 N7 C71 100.6(4) . . . . ? C5 C6 N7 C8 -131.1(4) . . . . ? C5 C6 N7 Ag -15.4(4) . . . . ? N44 Ag N7 C71 54.0(3) 2_566 . . . ? N4 Ag N7 C71 -131.6(2) . . . . ? N1 Ag N7 C71 149.6(2) . . . . ? N74 Ag N7 C71 -30.0(3) 2_556 . . . ? N44 Ag N7 C8 -63.5(3) 2_566 . . . ? N4 Ag N7 C8 110.8(2) . . . . ? N1 Ag N7 C8 32.1(2) . . . . ? N74 Ag N7 C8 -147.5(2) 2_556 . . . ? N44 Ag N7 C6 174.9(2) 2_566 . . . ? N4 Ag N7 C6 -10.8(2) . . . . ? N1 Ag N7 C6 -89.6(3) . . . . ? N74 Ag N7 C6 90.9(3) 2_556 . . . ? C71 N7 C8 C9 -166.7(3) . . . . ? C6 N7 C8 C9 64.6(4) . . . . ? Ag N7 C8 C9 -54.0(3) . . . . ? C2 N1 C9 C8 -128.3(4) . . . . ? C11 N1 C9 C8 107.4(4) . . . . ? Ag N1 C9 C8 -17.0(4) . . . . ? N7 C8 C9 N1 50.7(5) . . . . ? C2 N1 C11 C11 175.5(4) . . . 2_666 ? C9 N1 C11 C11 -58.4(5) . . . 2_666 ? Ag N1 C11 C11 66.5(5) . . . 2_666 ? C5 N4 C41 C42 172.9(4) . . . . ? C3 N4 C41 C42 -63.3(5) . . . . ? Ag N4 C41 C42 62.5(4) . . . . ? N4 C41 C42 C43 -60.0(5) . . . . ? C41 C42 C43 N44 2(11) . . . . ? C42 C43 N44 Ag 180(100) . . . 2_566 ? C8 N7 C71 C72 -61.4(4) . . . . ? C6 N7 C71 C72 67.9(5) . . . . ? Ag N7 C71 C72 -173.6(3) . . . . ? N7 C71 C72 C73 175.6(4) . . . . ? C71 C72 C73 N74 -51(11) . . . . ? C72 C73 N74 Ag 113(11) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.916 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.099