Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Brammer, L.' 'Burgard, Michael D.' 'Rath, Nigam P.' 'Rodger, Colin S.' 'Swearingen, John K.' _publ_contact_author_name 'Prof L Brammer' _publ_contact_author_address ; Department of Chemistry University of Missouri-St. Louis 8001 Natural Bridge Road St Louis MO 63121 USA ; _publ_section_title ; Silver (I) carboxylates: versatile inorganic analogs of carboxylic acids for supramolecular network formation ; data_l3601 _database_code_CSD 171148 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Ag F3 N2 O2' _chemical_formula_weight 333.07 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 12.5745(2) _cell_length_b 12.3972(2) _cell_length_c 14.2861(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2227.04(6) _cell_formula_units_Z 8 _cell_measurement_temperature 223(5) _cell_measurement_reflns_used 17088 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.4 _exptl_crystal_description 'rectangular rod' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6270 _exptl_absorpt_correction_T_max 0.8095 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-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 29715 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.0081 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1688 _reflns_number_gt 1591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0379P)^2^+8.8058P] 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 1688 _refine_ls_number_parameters 82 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.02812(3) 0.62883(2) 0.03831(12) Uani 1 2 d S . . F1 F 0.5000 0.2796(3) 0.5990(2) 0.0796(13) Uani 1 2 d SD . . F2 F 0.4238(6) 0.3664(4) 0.4976(3) 0.208(4) Uani 1 1 d D . . O1 O 0.5000 0.1178(3) 0.4799(3) 0.096(2) Uani 1 2 d S . . O2 O 0.5000 0.2269(4) 0.3606(3) 0.095(2) Uani 1 2 d S . . N1 N 0.33873(19) 0.03552(19) 0.70463(16) 0.0322(5) Uani 1 1 d . . . C1 C 0.5000 0.3015(4) 0.5107(4) 0.0652(18) Uani 1 2 d SD . . C2 C 0.5000 0.2062(4) 0.4436(3) 0.0440(10) Uani 1 2 d S . . C3 C 0.3510(3) -0.0178(4) 0.7964(3) 0.0570(10) Uani 1 1 d . . . H3A H 0.4024 0.0223 0.8344 0.068 Uiso 1 1 calc R . . H3B H 0.3786 -0.0910 0.7873 0.068 Uiso 1 1 calc R . . C4 C 0.2564(3) -0.0232(4) 0.6521(3) 0.0571(10) Uani 1 1 d . . . H4A H 0.2778 -0.0987 0.6446 0.068 Uiso 1 1 calc R . . H4B H 0.2489 0.0085 0.5896 0.068 Uiso 1 1 calc R . . C5 C 0.3014(3) 0.1464(3) 0.7205(3) 0.0592(11) Uani 1 1 d . . . H5A H 0.2878 0.1814 0.6602 0.071 Uiso 1 1 calc R . . H5B H 0.3566 0.1876 0.7532 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03581(18) 0.0439(2) 0.03524(18) -0.00254(13) 0.000 0.000 F1 0.143(4) 0.0544(19) 0.0414(16) -0.0108(15) 0.000 0.000 F2 0.342(9) 0.154(4) 0.128(3) -0.063(3) -0.094(4) 0.176(5) O1 0.221(7) 0.0267(16) 0.0402(19) 0.0002(15) 0.000 0.000 O2 0.179(7) 0.066(3) 0.040(2) 0.004(2) 0.000 0.000 N1 0.0301(11) 0.0355(11) 0.0309(11) -0.0007(9) -0.0009(9) 0.0000(9) C1 0.120(6) 0.031(2) 0.045(3) 0.002(2) 0.000 0.000 C2 0.059(3) 0.036(2) 0.036(2) -0.0011(17) 0.000 0.000 C3 0.0366(16) 0.089(3) 0.0450(18) 0.0217(18) 0.0011(14) 0.0133(18) C4 0.0408(17) 0.083(3) 0.0475(17) -0.0254(18) 0.0031(15) -0.0115(18) C5 0.054(2) 0.0352(15) 0.088(3) 0.0032(16) 0.028(2) -0.0008(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.301(2) 12_655 ? Ag1 N1 2.301(2) . ? Ag1 O1 2.384(4) 9_656 ? Ag1 O1 2.400(4) . ? F1 C1 1.291(5) . ? F2 C1 1.266(5) . ? O1 C2 1.213(6) . ? O1 Ag1 2.384(4) 9_656 ? O2 C2 1.213(6) . ? N1 C5 1.470(4) . ? N1 C4 1.471(4) . ? N1 C3 1.476(4) . ? C1 F2 1.266(5) 12_655 ? C1 C2 1.521(7) . ? C3 C4 1.540(5) 7_546 ? C4 C3 1.540(5) 7_546 ? C5 C5 1.543(7) 7_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 123.62(12) 12_655 . ? N1 Ag1 O1 109.69(7) 12_655 9_656 ? N1 Ag1 O1 109.69(7) . 9_656 ? N1 Ag1 O1 113.50(6) 12_655 . ? N1 Ag1 O1 113.50(6) . . ? O1 Ag1 O1 76.92(13) 9_656 . ? C2 O1 Ag1 114.0(3) . 9_656 ? C2 O1 Ag1 142.9(3) . . ? Ag1 O1 Ag1 103.08(13) 9_656 . ? C5 N1 C4 108.5(3) . . ? C5 N1 C3 108.4(3) . . ? C4 N1 C3 107.8(3) . . ? C5 N1 Ag1 113.05(19) . . ? C4 N1 Ag1 111.12(19) . . ? C3 N1 Ag1 107.9(2) . . ? F2 C1 F2 98.5(8) 12_655 . ? F2 C1 F1 106.1(4) 12_655 . ? F2 C1 F1 106.1(4) . . ? F2 C1 C2 113.6(4) 12_655 . ? F2 C1 C2 113.6(4) . . ? F1 C1 C2 116.9(4) . . ? O1 C2 O2 127.5(5) . . ? O1 C2 C1 115.6(4) . . ? O2 C2 C1 116.8(5) . . ? N1 C3 C4 110.6(3) . 7_546 ? N1 C4 C3 110.6(3) . 7_546 ? N1 C5 C5 110.60(17) . 7_546 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.975 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.098 #==END #=============================================================================# # Crystallographic data for [Ag(tetramethylpyrazine)]CF3CO2, compound 2 data_l8101 _database_code_CSD 171149 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H12 Ag F3 N2 O2' _chemical_formula_weight 357.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0587(2) _cell_length_b 9.1231(2) _cell_length_c 9.6097(2) _cell_angle_alpha 117.553(1) _cell_angle_beta 116.433(1) _cell_angle_gamma 91.471(1) _cell_volume 603.07(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9815 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 28.0 _exptl_crystal_description hexagon _exptl_crystal_colour colorle _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5868 _exptl_absorpt_correction_T_max 0.8480 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-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 12608 _diffrn_reflns_av_R_equivalents 0.02 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.05 _reflns_number_total 2874 _reflns_number_gt 2717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0249P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2874 _refine_ls_number_parameters 211 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.392119(19) -0.109663(19) 0.740580(19) 0.03972(6) Uani 1 1 d . . . F1 F 0.5867(2) 0.4995(2) 1.1749(3) 0.0737(5) Uani 1 1 d . . . F2 F 0.8339(3) 0.4783(2) 1.3247(2) 0.0785(5) Uani 1 1 d . . . F3 F 0.7924(2) 0.5640(2) 1.1417(3) 0.0685(4) Uani 1 1 d . . . O1 O 0.5724(2) 0.16023(19) 1.0079(2) 0.0452(3) Uani 1 1 d . . . O2 O 0.7324(3) 0.2299(3) 0.9143(3) 0.0794(7) Uani 1 1 d . . . N1 N 0.46502(19) -0.34711(19) 0.5839(2) 0.0305(3) Uani 1 1 d . . . N2 N 0.14594(19) -0.0333(2) 0.5994(2) 0.0309(3) Uani 1 1 d . . . C1 C 0.6701(3) 0.2614(3) 1.0094(3) 0.0401(4) Uani 1 1 d . . . C2 C 0.7199(3) 0.4522(3) 1.1613(3) 0.0453(5) Uani 1 1 d . . . C3 C 0.3559(2) -0.4669(2) 0.4056(2) 0.0300(3) Uani 1 1 d . . . C4 C 0.6089(2) -0.3778(2) 0.6791(2) 0.0296(3) Uani 1 1 d . . . C5 C 0.1996(3) -0.4271(3) 0.3017(3) 0.0466(5) Uani 1 1 d D . . C6 C 0.7270(3) -0.2404(3) 0.8764(3) 0.0410(4) Uani 1 1 d D . . C7 C 0.1469(2) 0.0334(2) 0.5007(2) 0.0308(3) Uani 1 1 d . . . C8 C 0.0009(2) -0.0669(2) 0.5997(2) 0.0304(3) Uani 1 1 d . . . C9 C 0.3098(3) 0.0703(3) 0.5018(3) 0.0437(5) Uani 1 1 d D . . C10 C 0.0023(3) -0.1404(3) 0.7105(3) 0.0430(5) Uani 1 1 d D . . H5A H 0.105(3) -0.520(4) 0.222(4) 0.081(10) Uiso 1 1 d DU . . H5B H 0.172(4) -0.342(4) 0.372(4) 0.079(9) Uiso 1 1 d DU . . H5C H 0.213(5) -0.405(5) 0.225(5) 0.103(12) Uiso 1 1 d DU . . H6A H 0.840(3) -0.237(4) 0.919(4) 0.075(9) Uiso 1 1 d DU . . H6B H 0.726(5) -0.131(3) 0.900(5) 0.093(11) Uiso 1 1 d DU . . H6C H 0.718(5) -0.256(5) 0.959(4) 0.083(10) Uiso 1 1 d DU . . H9A H 0.292(4) 0.002(4) 0.387(3) 0.073(9) Uiso 1 1 d DU . . H9B H 0.401(3) 0.073(4) 0.597(3) 0.063(8) Uiso 1 1 d DU . . H9C H 0.340(4) 0.177(3) 0.521(5) 0.077(9) Uiso 1 1 d DU . . H10A H -0.077(3) -0.249(3) 0.640(4) 0.063(8) Uiso 1 1 d DU . . H10B H 0.114(3) -0.135(4) 0.784(4) 0.068(8) Uiso 1 1 d DU . . H10C H -0.034(5) -0.074(4) 0.790(4) 0.083(10) Uiso 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 Ag1 0.04114(9) 0.03611(9) 0.03316(9) 0.01528(7) 0.01558(7) 0.01903(6) F1 0.0738(11) 0.0502(8) 0.1009(13) 0.0293(9) 0.0587(10) 0.0247(8) F2 0.0949(13) 0.0528(9) 0.0359(7) 0.0109(7) 0.0097(8) 0.0084(9) F3 0.0675(10) 0.0467(8) 0.0938(12) 0.0403(9) 0.0406(9) 0.0087(7) O1 0.0518(9) 0.0364(7) 0.0345(7) 0.0157(6) 0.0167(7) 0.0019(6) O2 0.1079(18) 0.0627(12) 0.0698(13) 0.0179(10) 0.0663(14) 0.0078(12) N1 0.0307(7) 0.0290(7) 0.0294(7) 0.0135(6) 0.0157(6) 0.0113(6) N2 0.0293(7) 0.0299(7) 0.0283(7) 0.0135(6) 0.0129(6) 0.0127(6) C1 0.0436(11) 0.0376(10) 0.0320(9) 0.0175(8) 0.0155(8) 0.0092(8) C2 0.0462(11) 0.0360(10) 0.0463(11) 0.0196(9) 0.0209(10) 0.0090(9) C3 0.0282(8) 0.0315(8) 0.0292(8) 0.0153(7) 0.0147(7) 0.0104(7) C4 0.0282(8) 0.0301(8) 0.0283(8) 0.0139(7) 0.0146(7) 0.0087(7) C5 0.0416(11) 0.0444(12) 0.0378(11) 0.0173(10) 0.0129(9) 0.0231(10) C6 0.0350(10) 0.0384(10) 0.0308(9) 0.0103(8) 0.0115(8) 0.0116(8) C7 0.0285(8) 0.0299(8) 0.0285(8) 0.0119(7) 0.0144(7) 0.0105(7) C8 0.0316(8) 0.0280(8) 0.0263(8) 0.0119(7) 0.0136(7) 0.0103(7) C9 0.0333(10) 0.0557(13) 0.0474(12) 0.0285(11) 0.0233(9) 0.0165(9) C10 0.0428(11) 0.0455(12) 0.0380(11) 0.0254(10) 0.0156(9) 0.0090(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 Ag1 N1 2.3102(15) . ? Ag1 O1 2.3528(15) . ? Ag1 N2 2.3579(15) . ? Ag1 O1 2.5506(15) 2_657 ? F1 C2 1.332(3) . ? F2 C2 1.336(3) . ? F3 C2 1.327(3) . ? O1 C1 1.253(3) . ? O1 Ag1 2.5506(15) 2_657 ? O2 C1 1.208(3) . ? N1 C4 1.345(2) . ? N1 C3 1.346(2) . ? N2 C8 1.343(2) . ? N2 C7 1.346(2) . ? C1 C2 1.545(3) . ? C3 C4 1.400(2) 2_646 ? C3 C5 1.495(3) . ? C4 C3 1.400(2) 2_646 ? C4 C6 1.496(3) . ? C7 C8 1.400(2) 2_556 ? C7 C9 1.499(3) . ? C8 C7 1.400(2) 2_556 ? C8 C10 1.493(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O1 129.34(6) . . ? N1 Ag1 N2 123.99(5) . . ? O1 Ag1 N2 100.87(6) . . ? N1 Ag1 O1 97.77(5) . 2_657 ? O1 Ag1 O1 77.80(5) . 2_657 ? N2 Ag1 O1 118.01(5) . 2_657 ? C1 O1 Ag1 121.14(13) . . ? C1 O1 Ag1 130.78(13) . 2_657 ? Ag1 O1 Ag1 102.20(5) . 2_657 ? C4 N1 C3 119.22(15) . . ? C4 N1 Ag1 118.73(12) . . ? C3 N1 Ag1 121.42(12) . . ? C8 N2 C7 118.80(15) . . ? C8 N2 Ag1 123.18(12) . . ? C7 N2 Ag1 117.76(12) . . ? O2 C1 O1 129.5(2) . . ? O2 C1 C2 117.3(2) . . ? O1 C1 C2 113.21(19) . . ? F3 C2 F1 106.94(19) . . ? F3 C2 F2 106.3(2) . . ? F1 C2 F2 105.9(2) . . ? F3 C2 C1 113.8(2) . . ? F1 C2 C1 113.12(19) . . ? F2 C2 C1 110.23(18) . . ? N1 C3 C4 120.32(16) . 2_646 ? N1 C3 C5 118.05(16) . . ? C4 C3 C5 121.61(17) 2_646 . ? N1 C4 C3 120.46(16) . 2_646 ? N1 C4 C6 117.34(16) . . ? C3 C4 C6 122.20(17) 2_646 . ? N2 C7 C8 120.46(16) . 2_556 ? N2 C7 C9 118.14(17) . . ? C8 C7 C9 121.40(18) 2_556 . ? N2 C8 C7 120.75(16) . 2_556 ? N2 C8 C10 118.11(17) . . ? C7 C8 C10 121.15(18) 2_556 . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.531 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.061 #==END #=============================================================================# # Crystallographic data for [Ag(pyrazine)]CF3CO2, compound 3 data_l14600sd _database_code_CSD 171150 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 Ag F3 N2 O2' _chemical_formula_weight 300.98 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' '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 12.766(2) _cell_length_b 10.1410(16) _cell_length_c 7.0078(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.030(3) _cell_angle_gamma 90.00 _cell_volume 887.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5159 _cell_measurement_theta_min 5.174 _cell_measurement_theta_max 61.118 _exptl_crystal_description 'multifacetted block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 2.295 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 0.8150 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _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 6208 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 30.56 _reflns_number_total 1285 _reflns_number_gt 1215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0400P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0107(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1285 _refine_ls_number_parameters 80 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.413 _refine_ls_restrained_S_all 1.430 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.40599(2) 0.2500 0.05324(13) Uani 1 2 d S . . N1 N 0.33692(14) 0.31771(19) 0.1098(2) 0.0521(4) Uani 1 1 d . . . C2 C 0.30342(19) 0.2032(2) 0.1690(3) 0.0598(5) Uani 1 1 d . . . H2 H 0.3389 0.1681 0.2875 0.072 Uiso 1 1 calc R . . C3 C 0.28225(18) 0.3652(2) -0.0603(3) 0.0549(4) Uani 1 1 d . . . H3 H 0.3022 0.4455 -0.1060 0.066 Uiso 1 1 calc R . . O1 O 0.5554(2) 0.6379(2) 0.3944(3) 0.0800(6) Uani 1 1 d . . . C11 C 0.5000 0.6910(3) 0.2500 0.0526(6) Uani 1 2 d S . . C12 C 0.5000 0.8409(3) 0.2500 0.0700(9) Uani 1 2 d SD . . F1 F 0.5355(12) 0.8943(8) 0.4155(12) 0.229(9) Uani 0.50 1 d PD . . F2 F 0.5543(11) 0.8888(6) 0.133(2) 0.201(8) Uani 0.50 1 d PD . . F3 F 0.4051(5) 0.8897(5) 0.1932(17) 0.117(2) Uani 0.50 1 d PD . . 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 0.04305(16) 0.04788(17) 0.06124(18) 0.000 -0.00647(10) 0.000 N1 0.0445(8) 0.0574(9) 0.0494(7) 0.0037(7) -0.0018(6) -0.0080(7) C2 0.0537(10) 0.0681(13) 0.0499(9) 0.0168(8) -0.0072(7) -0.0088(9) C3 0.0470(9) 0.0551(10) 0.0578(10) 0.0135(9) 0.0000(8) -0.0077(8) O1 0.0951(15) 0.0698(12) 0.0788(12) 0.0266(10) 0.0267(11) 0.0231(12) C11 0.0697(17) 0.0391(13) 0.0528(13) 0.000 0.0215(12) 0.000 C12 0.097(3) 0.0407(15) 0.0680(18) 0.000 0.0064(17) 0.000 F1 0.40(2) 0.092(4) 0.120(6) -0.064(5) -0.118(10) 0.080(8) F2 0.281(14) 0.059(3) 0.340(18) 0.066(7) 0.238(15) 0.031(5) F3 0.130(5) 0.072(3) 0.150(6) 0.013(4) 0.029(4) 0.056(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.2909(17) . ? Ag1 N1 2.2909(17) 2_655 ? Ag1 O1 2.599(3) . ? Ag1 O1 2.599(3) 2_655 ? N1 C2 1.333(3) . ? N1 C3 1.339(3) . ? C2 C3 1.382(3) 7 ? C2 H2 0.9300 . ? C3 C2 1.382(3) 7 ? C3 H3 0.9300 . ? O1 C11 1.231(2) . ? C11 O1 1.231(2) 2_655 ? C11 C12 1.520(4) . ? C12 F2 1.272(5) 2_655 ? C12 F2 1.272(5) . ? C12 F1 1.274(4) . ? C12 F1 1.274(4) 2_655 ? C12 F3 1.293(5) 2_655 ? C12 F3 1.293(5) . ? F1 F2 1.127(9) 2_655 ? F1 F3 1.183(11) 2_655 ? F2 F1 1.127(9) 2_655 ? F2 F3 1.217(11) 2_655 ? F3 F1 1.183(11) 2_655 ? F3 F2 1.217(11) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 134.00(10) . 2_655 ? N1 Ag1 O1 132.04(7) . . ? N1 Ag1 O1 92.15(7) 2_655 . ? N1 Ag1 O1 92.15(7) . 2_655 ? N1 Ag1 O1 132.04(7) 2_655 2_655 ? O1 Ag1 O1 50.40(9) . 2_655 ? C2 N1 C3 116.66(17) . . ? C2 N1 Ag1 121.92(13) . . ? C3 N1 Ag1 119.98(14) . . ? N1 C2 C3 122.28(18) . 7 ? N1 C2 H2 118.9 . . ? C3 C2 H2 118.9 7 . ? N1 C3 C2 121.0(2) . 7 ? N1 C3 H3 119.5 . . ? C2 C3 H3 119.5 7 . ? C11 O1 Ag1 90.75(19) . . ? O1 C11 O1 128.1(4) 2_655 . ? O1 C11 C12 115.95(18) 2_655 . ? O1 C11 C12 115.95(18) . . ? F2 C12 F2 135.1(7) 2_655 . ? F2 C12 F1 52.5(4) 2_655 . ? F2 C12 F1 106.5(4) . . ? F2 C12 F1 106.5(4) 2_655 2_655 ? F2 C12 F1 52.5(4) . 2_655 ? F1 C12 F1 129.8(9) . 2_655 ? F2 C12 F3 104.9(3) 2_655 2_655 ? F2 C12 F3 56.7(5) . 2_655 ? F1 C12 F3 54.9(5) . 2_655 ? F1 C12 F3 104.5(3) 2_655 2_655 ? F2 C12 F3 56.7(5) 2_655 . ? F2 C12 F3 104.9(3) . . ? F1 C12 F3 104.5(3) . . ? F1 C12 F3 54.9(5) 2_655 . ? F3 C12 F3 135.0(6) 2_655 . ? F2 C12 C11 112.5(4) 2_655 . ? F2 C12 C11 112.5(4) . . ? F1 C12 C11 115.1(4) . . ? F1 C12 C11 115.1(4) 2_655 . ? F3 C12 C11 112.5(3) 2_655 . ? F3 C12 C11 112.5(3) . . ? F2 F1 F3 123.4(7) 2_655 2_655 ? F2 F1 C12 63.6(3) 2_655 . ? F3 F1 C12 63.3(3) 2_655 . ? F1 F2 F3 119.9(8) 2_655 2_655 ? F1 F2 C12 63.8(3) 2_655 . ? F3 F2 C12 62.5(3) 2_655 . ? F1 F3 F2 116.5(6) 2_655 2_655 ? F1 F3 C12 61.8(3) 2_655 . ? F2 F3 C12 60.8(3) 2_655 . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.077