# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Lyall Hanton' _publ_contact_author_address ; Department of Chemistry University of Otago PO Box 56 Dunedin 9054 NEW ZEALAND ; _publ_contact_author_email LHANTON@ALKALI.OTAGO.AC.NZ _publ_section_title ; A coordination-polymer strategy for anion encapsulation: anion-? interactions in (4,4) nets formed from Ag(I) salts and a flexible pyrimidine ligand ; loop_ _publ_author_name 'Lyall Hanton' 'Cory A. Black' 'Mark Spicer' # Attachment 'B703522e_hanton_pym_anion_pi.cif' data_cbaf _database_code_depnum_ccdc_archive 'CCDC 639720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 1 cbaf' _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Ag N4 S, B F4' _chemical_formula_sum 'C10 H10 Ag B F4 N4 S' _chemical_formula_weight 412.97 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 7.608(5) _cell_length_b 8.883(5) _cell_length_c 9.914(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 670.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 7742 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 32.43 _exptl_crystal_description irregular _exptl_crystal_colour 'pale bronze' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7150 _exptl_absorpt_correction_T_max 0.9000 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10674 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 32.64 _reflns_number_total 2133 _reflns_number_gt 2007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0221P)^2^+0.3243P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 2133 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1821(3) 0.3036(3) 0.4307(2) 0.0257(4) Uani 1 1 d . . . H1 H 0.2027 0.2919 0.5226 0.031 Uiso 1 1 calc R . . C2 C 0.0451(2) 0.2239(2) 0.2410(2) 0.0184(3) Uani 1 1 d . . . H2 H -0.0307 0.1581 0.1968 0.022 Uiso 1 1 calc R . . C3 C 0.1260(2) 0.3361(2) 0.16808(18) 0.0177(3) Uani 1 1 d . . . H3 H 0.1065 0.3464 0.0759 0.021 Uiso 1 1 calc R . . C4 C 0.2379(2) 0.4337(2) 0.23636(19) 0.0158(3) Uani 1 1 d . . . C5 C 0.3288(2) 0.5617(2) 0.16748(19) 0.0178(3) Uani 1 1 d . . . H5A H 0.3800 0.6273 0.2352 0.021 Uiso 1 1 calc R . . H5B H 0.2427 0.6198 0.1174 0.021 Uiso 1 1 calc R . . Ag1 Ag 0.0000 0.0000 0.502131(16) 0.01940(6) Uani 1 2 d S . . N1 N 0.0723(2) 0.2066(2) 0.37392(17) 0.0201(3) Uani 1 1 d . . . N2 N 0.2660(2) 0.4164(2) 0.36940(17) 0.0218(3) Uani 1 1 d . . . S1 S 0.5000 0.5000 0.05305(5) 0.01885(11) Uani 1 2 d S . . F12 F 0.5179(3) 0.87366(15) 0.29857(15) 0.0439(4) Uani 1 1 d . . . B1 B 0.5000 1.0000 0.2189(3) 0.0243(5) Uani 1 2 d S . . F11 F 0.6472(2) 1.0119(3) 0.13852(19) 0.0726(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0280(9) 0.0356(11) 0.0135(9) 0.0024(8) -0.0020(7) -0.0109(8) C2 0.0204(8) 0.0197(8) 0.0151(8) -0.0011(7) -0.0016(6) 0.0019(6) C3 0.0195(8) 0.0212(8) 0.0123(8) 0.0006(7) -0.0030(6) 0.0018(7) C4 0.0139(7) 0.0201(8) 0.0135(8) -0.0020(7) 0.0002(6) 0.0036(6) C5 0.0160(7) 0.0202(8) 0.0172(9) 0.0013(7) 0.0010(6) 0.0022(6) Ag1 0.02203(8) 0.02156(9) 0.01461(9) 0.000 0.000 0.00366(9) N1 0.0212(7) 0.0246(8) 0.0144(7) 0.0022(6) -0.0016(6) -0.0037(6) N2 0.0225(7) 0.0288(9) 0.0140(8) 0.0006(6) -0.0006(6) -0.0059(7) S1 0.0166(2) 0.0287(3) 0.0112(2) 0.000 0.000 0.0014(3) F12 0.0523(10) 0.0311(6) 0.0483(8) 0.0128(6) 0.0096(9) 0.0018(8) B1 0.0260(12) 0.0266(13) 0.0202(13) 0.000 0.000 0.0018(18) F11 0.0594(9) 0.0959(15) 0.0624(11) 0.0417(14) 0.0385(8) 0.0285(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(3) . ? C1 N2 1.335(3) . ? C1 H1 0.9300 . ? C2 N1 1.343(3) . ? C2 C3 1.377(3) . ? C2 H2 0.9300 . ? C3 C4 1.391(3) . ? C3 H3 0.9300 . ? C4 N2 1.345(2) . ? C4 C5 1.496(3) . ? C5 S1 1.8125(19) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? Ag1 N1 2.2988(19) 2 ? Ag1 N1 2.2988(19) . ? Ag1 N2 2.3112(19) 4_546 ? Ag1 N2 2.3112(19) 3_456 ? N2 Ag1 2.3112(19) 3_556 ? S1 C5 1.8125(19) 2_665 ? F12 B1 1.379(2) . ? B1 F11 1.379(2) 2_675 ? B1 F11 1.379(2) . ? B1 F12 1.379(2) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 126.59(19) . . ? N1 C1 H1 116.7 . . ? N2 C1 H1 116.7 . . ? N1 C2 C3 121.94(17) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C2 C3 C4 118.02(17) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? N2 C4 C3 120.22(17) . . ? N2 C4 C5 117.46(17) . . ? C3 C4 C5 122.31(17) . . ? C4 C5 S1 112.81(13) . . ? C4 C5 H5A 109.0 . . ? S1 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? S1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 Ag1 N1 112.87(9) 2 . ? N1 Ag1 N2 103.45(7) 2 4_546 ? N1 Ag1 N2 112.14(7) . 4_546 ? N1 Ag1 N2 112.14(7) 2 3_456 ? N1 Ag1 N2 103.45(7) . 3_456 ? N2 Ag1 N2 113.12(9) 4_546 3_456 ? C1 N1 C2 116.06(17) . . ? C1 N1 Ag1 115.77(13) . . ? C2 N1 Ag1 126.67(13) . . ? C1 N2 C4 117.15(18) . . ? C1 N2 Ag1 111.01(13) . 3_556 ? C4 N2 Ag1 128.77(13) . 3_556 ? C5 S1 C5 102.50(12) 2_665 . ? F11 B1 F11 109.3(3) 2_675 . ? F11 B1 F12 108.27(13) 2_675 2_675 ? F11 B1 F12 110.41(15) . 2_675 ? F11 B1 F12 110.41(15) 2_675 . ? F11 B1 F12 108.27(13) . . ? F12 B1 F12 110.1(2) 2_675 . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.720 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.080 #===END data_cbf _database_code_depnum_ccdc_archive 'CCDC 639721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2 cbf' _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Ag1 Cl1 N4 O4 S1' _chemical_formula_sum 'C10 H10 Ag Cl N4 O4 S' _chemical_formula_weight 425.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 7.7198(3) _cell_length_b 9.1284(3) _cell_length_c 9.7867(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 689.66(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2970 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 1.827 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6415 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.03 _reflns_number_total 2018 _reflns_number_gt 1837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.9438P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(7) _refine_ls_number_reflns 2018 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8001(6) 0.7085(5) 0.5722(4) 0.0394(9) Uani 1 1 d . . . H1 H 0.7699 0.7275 0.4797 0.047 Uiso 1 1 calc R . . C2 C 0.9528(5) 0.7721(4) 0.7604(3) 0.0286(7) Uani 1 1 d . . . H2 H 1.0338 0.8333 0.8060 0.034 Uiso 1 1 calc R . . C3 C 0.8752(5) 0.6597(4) 0.8311(4) 0.0308(7) Uani 1 1 d . . . H3 H 0.9008 0.6438 0.9249 0.037 Uiso 1 1 calc R . . C4 C 0.7586(5) 0.5699(4) 0.7629(4) 0.0259(7) Uani 1 1 d . . . C5 C 0.6703(5) 0.4430(4) 0.8304(4) 0.0284(7) Uani 1 1 d . . . H5A H 0.7572 0.3852 0.8816 0.034 Uiso 1 1 calc R . . H5B H 0.6200 0.3787 0.7592 0.034 Uiso 1 1 calc R . . Ag1 Ag 1.0000 1.0000 0.50432(3) 0.03059(11) Uani 1 2 d S . . Cl1 Cl 1.0000 0.5000 0.22287(11) 0.0357(2) Uani 1 2 d S . . N1 N 0.9163(4) 0.7974(4) 0.6270(3) 0.0311(6) Uani 1 1 d . . . N2 N 0.7213(4) 0.5966(4) 0.6307(3) 0.0342(7) Uani 1 1 d . . . O1 O 1.1380(10) 0.5263(15) 0.1438(5) 0.221(6) Uani 1 1 d . . . O2 O 0.9963(16) 0.6159(9) 0.3110(9) 0.196(4) Uani 1 1 d . . . S1 S 0.5000 0.5000 0.94658(10) 0.0312(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(2) 0.050(2) 0.0243(17) 0.0039(17) -0.0049(16) -0.0173(19) C2 0.0281(17) 0.0326(17) 0.0252(14) -0.0030(13) -0.0031(11) -0.0012(12) C3 0.0279(17) 0.0357(18) 0.0289(16) 0.0016(14) -0.0043(14) 0.0020(14) C4 0.0223(15) 0.0281(16) 0.0271(16) -0.0007(13) 0.0014(12) 0.0039(13) C5 0.0242(16) 0.0295(15) 0.0314(16) 0.0019(14) 0.0010(14) 0.0015(13) Ag1 0.03322(17) 0.02741(16) 0.03114(17) 0.000 0.000 0.0030(2) Cl1 0.0390(5) 0.0337(5) 0.0342(5) 0.000 0.000 -0.0057(8) N1 0.0313(16) 0.0334(15) 0.0287(14) 0.0022(12) -0.0022(12) -0.0057(13) N2 0.0334(16) 0.0388(17) 0.0303(15) 0.0030(13) -0.0035(13) -0.0092(14) O1 0.141(6) 0.442(15) 0.081(4) -0.053(7) 0.050(4) -0.202(9) O2 0.222(10) 0.149(7) 0.218(8) -0.088(6) 0.063(11) 0.076(7) S1 0.0264(5) 0.0442(6) 0.0231(4) 0.000 0.000 -0.0021(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 C1 N2 1.320(5) . ? C1 N1 1.323(5) . ? C1 H1 0.9500 . ? C2 N1 1.356(5) . ? C2 C3 1.375(5) . ? C2 H2 0.9500 . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 N2 1.347(5) . ? C4 C5 1.498(5) . ? C5 S1 1.814(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? Ag1 N1 2.297(3) 2_775 ? Ag1 N1 2.297(3) . ? Ag1 N2 2.333(3) 4_656 ? Ag1 N2 2.333(3) 3_566 ? Cl1 O1 1.339(5) 2_765 ? Cl1 O1 1.339(5) . ? Cl1 O2 1.365(7) . ? Cl1 O2 1.365(7) 2_765 ? N2 Ag1 2.333(3) 3_466 ? S1 C5 1.814(4) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 127.7(4) . . ? N2 C1 H1 116.2 . . ? N1 C1 H1 116.2 . . ? N1 C2 C3 121.5(3) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 118.7(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? N2 C4 C3 119.6(3) . . ? N2 C4 C5 117.7(3) . . ? C3 C4 C5 122.6(3) . . ? C4 C5 S1 112.6(3) . . ? C4 C5 H5A 109.1 . . ? S1 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? S1 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N1 Ag1 N1 117.01(16) 2_775 . ? N1 Ag1 N2 101.41(12) 2_775 4_656 ? N1 Ag1 N2 113.22(12) . 4_656 ? N1 Ag1 N2 113.22(12) 2_775 3_566 ? N1 Ag1 N2 101.41(12) . 3_566 ? N2 Ag1 N2 110.98(16) 4_656 3_566 ? O1 Cl1 O1 109.3(5) 2_765 . ? O1 Cl1 O2 119.2(7) 2_765 . ? O1 Cl1 O2 104.1(7) . . ? O1 Cl1 O2 104.1(7) 2_765 2_765 ? O1 Cl1 O2 119.2(7) . 2_765 ? O2 Cl1 O2 101.7(8) . 2_765 ? C1 N1 C2 115.3(3) . . ? C1 N1 Ag1 118.2(3) . . ? C2 N1 Ag1 125.6(3) . . ? C1 N2 C4 117.2(3) . . ? C1 N2 Ag1 112.6(3) . 3_466 ? C4 N2 Ag1 129.2(3) . 3_466 ? C5 S1 C5 102.4(2) 2_665 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.987 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.100 #===END data_cbm _database_code_depnum_ccdc_archive 'CCDC 639722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 3 cbm' _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Ag1 N4 S1, F6 P1' _chemical_formula_sum 'C10 H10 Ag F6 N4 P S' _chemical_formula_weight 471.12 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 7.8018(16) _cell_length_b 9.0824(17) _cell_length_c 9.9020(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 701.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2325 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.41 _exptl_crystal_description truncated_re _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6735 _exptl_absorpt_correction_T_max 0.7900 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2953 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.41 _reflns_number_total 1291 _reflns_number_gt 1234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0217P)^2^+2.5618P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(6) _refine_ls_number_reflns 1291 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8133(7) 0.6980(5) 0.5653(5) 0.0220(11) Uani 1 1 d . . . H1 H 0.7939 0.7128 0.4736 0.026 Uiso 1 1 calc R . . C2 C 0.9457(6) 0.7686(5) 0.7562(5) 0.0173(11) Uani 1 1 d . . . H2 H 1.0192 0.8315 0.8025 0.021 Uiso 1 1 calc R . . C3 C 0.8666(7) 0.6575(5) 0.8258(5) 0.0195(10) Uani 1 1 d . . . H3 H 0.8860 0.6441 0.9176 0.023 Uiso 1 1 calc R . . C4 C 0.7563(7) 0.5651(5) 0.7547(5) 0.0157(10) Uani 1 1 d . . . C5 C 0.6655(7) 0.4403(5) 0.8215(5) 0.0190(10) Uani 1 1 d . . . H5A H 0.7485 0.3812 0.8703 0.023 Uiso 1 1 calc R . . H5B H 0.6142 0.3785 0.7527 0.023 Uiso 1 1 calc R . . Ag1 Ag 1.0000 1.0000 0.50806(4) 0.01773(14) Uani 1 2 d S . . N1 N 0.9210(5) 0.7899(4) 0.6238(4) 0.0174(8) Uani 1 1 d . . . N2 N 0.7290(5) 0.5867(4) 0.6219(4) 0.0191(9) Uani 1 1 d . . . S1 S 0.5000 0.5000 0.93769(13) 0.0201(3) Uani 1 2 d S . . P1 P 0.5000 1.0000 0.77758(14) 0.0222(3) Uani 1 2 d S . . F11 F 0.5562(5) 0.8853(7) 0.6678(5) 0.0893(19) Uani 1 1 d . . . F12 F 0.3123(5) 0.9356(4) 0.7734(6) 0.0779(18) Uani 1 1 d . . . F13 F 0.4425(6) 1.1118(5) 0.8877(5) 0.091(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(3) 0.026(2) 0.020(2) 0.0015(19) -0.002(2) -0.002(2) C2 0.016(3) 0.016(2) 0.020(2) -0.0004(16) -0.0023(17) 0.0018(17) C3 0.018(3) 0.022(2) 0.019(2) 0.0031(18) -0.002(2) 0.003(2) C4 0.012(3) 0.0161(19) 0.019(2) 0.0030(17) 0.003(2) 0.0058(19) C5 0.017(3) 0.0158(18) 0.024(2) 0.0015(18) 0.000(2) -0.0003(19) Ag1 0.0184(3) 0.01515(19) 0.0196(2) 0.000 0.000 0.0012(3) N1 0.016(2) 0.0141(17) 0.0220(18) -0.0012(15) 0.0000(16) -0.0008(16) N2 0.013(2) 0.021(2) 0.024(2) -0.0009(16) -0.0006(17) -0.0042(16) S1 0.0204(8) 0.0215(6) 0.0184(6) 0.000 0.000 0.0013(12) P1 0.0215(9) 0.0173(6) 0.0278(7) 0.000 0.000 -0.0018(12) F11 0.026(3) 0.142(5) 0.100(4) -0.086(3) -0.009(2) 0.023(3) F12 0.021(2) 0.0289(17) 0.183(6) -0.017(3) 0.027(3) -0.0087(17) F13 0.090(4) 0.099(3) 0.084(3) -0.068(3) -0.060(3) 0.072(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 C1 N1 1.319(6) . ? C1 N2 1.330(6) . ? C1 H1 0.9300 . ? C2 N1 1.340(6) . ? C2 C3 1.368(7) . ? C2 H2 0.9300 . ? C3 C4 1.393(7) . ? C3 H3 0.9300 . ? C4 N2 1.347(6) . ? C4 C5 1.491(7) . ? C5 S1 1.813(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? Ag1 N1 2.309(4) 2_775 ? Ag1 N1 2.309(4) . ? Ag1 N2 2.338(4) 4_566 ? Ag1 N2 2.338(4) 3_656 ? N2 Ag1 2.338(4) 3_646 ? S1 C5 1.813(5) 2_665 ? P1 F13 1.556(4) . ? P1 F13 1.556(4) 2_675 ? P1 F11 1.568(4) . ? P1 F11 1.568(4) 2_675 ? P1 F12 1.578(4) 2_675 ? P1 F12 1.578(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 127.7(4) . . ? N1 C1 H1 116.1 . . ? N2 C1 H1 116.1 . . ? N1 C2 C3 122.3(4) . . ? N1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? N2 C4 C3 120.2(4) . . ? N2 C4 C5 118.0(4) . . ? C3 C4 C5 121.8(4) . . ? C4 C5 S1 113.1(3) . . ? C4 C5 H5A 109.0 . . ? S1 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? S1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 Ag1 N1 120.51(19) 2_775 . ? N1 Ag1 N2 110.32(15) 2_775 4_566 ? N1 Ag1 N2 101.46(14) . 4_566 ? N1 Ag1 N2 101.46(14) 2_775 3_656 ? N1 Ag1 N2 110.32(15) . 3_656 ? N2 Ag1 N2 113.23(19) 4_566 3_656 ? C1 N1 C2 115.4(4) . . ? C1 N1 Ag1 118.4(3) . . ? C2 N1 Ag1 124.5(3) . . ? C1 N2 C4 116.4(4) . . ? C1 N2 Ag1 113.7(3) . 3_646 ? C4 N2 Ag1 127.5(3) . 3_646 ? C5 S1 C5 101.2(3) . 2_665 ? F13 P1 F13 91.1(4) . 2_675 ? F13 P1 F11 179.1(3) . . ? F13 P1 F11 88.3(3) 2_675 . ? F13 P1 F11 88.3(3) . 2_675 ? F13 P1 F11 179.1(3) 2_675 2_675 ? F11 P1 F11 92.3(5) . 2_675 ? F13 P1 F12 92.5(3) . 2_675 ? F13 P1 F12 89.6(3) 2_675 2_675 ? F11 P1 F12 88.2(3) . 2_675 ? F11 P1 F12 89.7(2) 2_675 2_675 ? F13 P1 F12 89.6(3) . . ? F13 P1 F12 92.5(3) 2_675 . ? F11 P1 F12 89.7(2) . . ? F11 P1 F12 88.2(3) 2_675 . ? F12 P1 F12 177.0(5) 2_675 . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.973 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.100 #===END