# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2024 data_Compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{Silver(I)(2,2'-bipyrazine)](tetrafluoroborate)}n.MeNO2 solvate' ; _chemical_name_common '{[Ag(2,2'-bpyz)]BF4.2MeNO2}' _chemical_formula_moiety '{[Ag(2,2'-bpyz)]BF4.2MeNO2}' _chemical_formula_sum 'C10 H12 Ag B F4 N6 O4' _chemical_formula_weight 474.94 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 11.396(7) _cell_length_b 11.396(7) _cell_length_c 13.913(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1807(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.782 _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 'Stoe Stadi-4 Four-Circle Diffractometer' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% '4% decay corrected during processing' _diffrn_reflns_number 2365 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1595 _reflns_number_gt 1391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+7.9908P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.12(12) _refine_ls_number_reflns 1595 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.60919(5) 0.39081(5) 0.2500 0.0268(3) Uani 1 d S . . N1 N 0.6951(6) 0.2291(7) 0.3387(5) 0.0289(17) Uani 1 d . . . C2 C 0.7879(7) 0.1772(8) 0.2997(6) 0.027(2) Uani 1 d . . . C3 C 0.8468(7) 0.0896(8) 0.3486(6) 0.027(2) Uani 1 d . . . H3A H 0.9126 0.0537 0.3188 0.032 Uiso 1 calc R . . N4 N 0.8148(7) 0.0530(7) 0.4367(5) 0.0274(16) Uani 1 d . . . C5 C 0.7205(7) 0.1077(10) 0.4742(5) 0.032(2) Uani 1 d . . . H5A H 0.6925 0.0840 0.5355 0.038 Uiso 1 calc R . . C6 C 0.6636(9) 0.1966(9) 0.4265(6) 0.036(2) Uani 1 d . . . H6A H 0.6001 0.2357 0.4571 0.043 Uiso 1 calc R . . B1 B 0.1258(8) -0.1258(8) 0.2500 0.036(3) Uani 1 d S . . F1 F 0.0577(7) -0.0986(9) 0.3263(5) 0.088(3) Uani 1 d . . . F2 F 0.2414(6) -0.1075(9) 0.2696(8) 0.103(3) Uani 1 d . . . C1S C 0.0088(14) -0.4667(12) 0.1059(9) 0.064(4) Uani 1 d . . . H1S1 H 0.0140 -0.5476 0.0824 0.096 Uiso 1 calc R . . H1S2 H -0.0736 -0.4418 0.1066 0.096 Uiso 1 calc R . . H1S3 H 0.0409 -0.4623 0.1711 0.096 Uiso 1 calc R . . N1S N 0.0641(12) -0.4030(14) 0.0535(9) 0.082(4) Uani 1 d . . . O2S O 0.1681(13) -0.4132(15) 0.0292(9) 0.130(5) Uani 1 d . . . O1S O -0.0002(14) -0.2958(12) 0.0216(10) 0.136(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 0.0284(3) 0.0284(3) 0.0235(4) -0.0051(3) -0.0051(3) 0.0036(5) N1 0.025(4) 0.039(4) 0.023(4) 0.004(3) 0.005(3) 0.007(3) C2 0.028(5) 0.030(5) 0.022(4) -0.001(4) 0.001(3) 0.003(4) C3 0.024(4) 0.033(5) 0.024(4) 0.000(4) 0.002(3) 0.005(4) N4 0.028(4) 0.032(4) 0.022(3) 0.003(3) 0.001(3) 0.002(3) C5 0.034(5) 0.042(5) 0.020(4) 0.004(4) 0.006(3) 0.000(5) C6 0.035(5) 0.045(6) 0.029(5) 0.004(4) 0.013(4) 0.012(5) B1 0.032(5) 0.032(5) 0.043(7) 0.004(5) 0.004(5) 0.008(6) F1 0.075(5) 0.127(8) 0.061(4) 0.005(5) 0.026(4) 0.038(6) F2 0.040(4) 0.110(6) 0.159(9) 0.013(8) 0.001(5) -0.006(5) C1S 0.068(9) 0.064(8) 0.060(8) 0.029(7) -0.014(7) -0.032(7) N1S 0.086(9) 0.098(11) 0.062(7) -0.018(8) -0.028(7) 0.015(9) O2S 0.111(10) 0.173(14) 0.105(9) -0.020(9) 0.023(8) 0.022(10) O1S 0.168(14) 0.116(11) 0.123(12) 0.006(10) -0.019(10) -0.029(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 N4 2.223(8) 5_655 y Ag1 N4 2.223(8) 3_544 ? Ag1 N1 2.425(7) 8_665 y Ag1 N1 2.425(7) . ? N1 C6 1.326(11) . ? N1 C2 1.327(11) . ? C2 C3 1.382(12) . ? C2 C2 1.494(16) 8_665 ? C3 N4 1.345(10) . ? N4 C5 1.348(12) . ? N4 Ag1 2.223(8) 4 ? C5 C6 1.374(13) . ? B1 F1 1.352(10) 8 ? B1 F1 1.352(10) . ? B1 F2 1.362(11) . ? B1 F2 1.362(11) 8 ? C1S N1S 1.206(18) . ? N1S O2S 1.239(16) . ? N1S O1S 1.492(19) . ? 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 N4 Ag1 N4 143.6(4) 5_655 3_544 y N4 Ag1 N1 104.0(3) 5_655 8_665 y N4 Ag1 N1 105.9(3) 3_544 8_665 y N4 Ag1 N1 105.9(3) 5_655 . y N4 Ag1 N1 104.0(3) 3_544 . ? N1 Ag1 N1 69.2(3) 8_665 . y C6 N1 C2 117.9(8) . . ? C6 N1 Ag1 124.8(6) . . ? C2 N1 Ag1 116.9(5) . . ? N1 C2 C3 120.5(7) . . ? N1 C2 C2 118.2(5) . 8_665 ? C3 C2 C2 121.3(5) . 8_665 ? N4 C3 C2 122.8(8) . . ? C3 N4 C5 115.2(8) . . ? C3 N4 Ag1 120.9(6) . 4 ? C5 N4 Ag1 122.8(6) . 4 ? N4 C5 C6 122.1(7) . . ? N1 C6 C5 121.5(9) . . ? F1 B1 F1 110.7(12) 8 . ? F1 B1 F2 106.9(6) 8 . ? F1 B1 F2 111.3(6) . . ? F1 B1 F2 111.3(6) 8 8 ? F1 B1 F2 106.9(6) . 8 ? F2 B1 F2 109.7(13) . 8 ? C1S N1S O2S 127.5(18) . . ? C1S N1S O1S 114.5(15) . . ? O2S N1S O1S 117.7(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ag1 N1 C6 76.6(8) 5_655 . . . ? N4 Ag1 N1 C6 -82.2(8) 3_544 . . . ? N1 Ag1 N1 C6 175.8(10) 8_665 . . . ? N4 Ag1 N1 C2 -96.6(7) 5_655 . . . ? N4 Ag1 N1 C2 104.6(7) 3_544 . . . ? N1 Ag1 N1 C2 2.7(5) 8_665 . . . ? C6 N1 C2 C3 2.0(13) . . . . ? Ag1 N1 C2 C3 175.6(7) . . . . ? C6 N1 C2 C2 179.1(10) . . . 8_665 ? Ag1 N1 C2 C2 -7.2(13) . . . 8_665 ? N1 C2 C3 N4 -0.4(14) . . . . ? C2 C2 C3 N4 -177.4(10) 8_665 . . . ? C2 C3 N4 C5 0.2(12) . . . . ? C2 C3 N4 Ag1 168.4(7) . . . 4 ? C3 N4 C5 C6 -1.8(13) . . . . ? Ag1 N4 C5 C6 -169.7(8) 4 . . . ? C2 N1 C6 C5 -3.5(15) . . . . ? Ag1 N1 C6 C5 -176.6(7) . . . . ? N4 C5 C6 N1 3.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.742 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.122 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Silver(I)(2,2'-bipyrazine) hexafluorophosphate' ; _chemical_name_common Ag(bpyz)PF6 _chemical_melting_point unknown _chemical_formula_moiety [Ag(C8H6N4)]PF6 _chemical_formula_sum 'C10 H12 Ag F6 N6 O4 P' _chemical_formula_weight 533.10 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.828(2) _cell_length_b 12.828(2) _cell_length_c 11.0200(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1813.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6322 _cell_measurement_theta_min 2.245 _cell_measurement_theta_max 28.22 _exptl_crystal_description 'Irregular plate' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details ? _exptl_special_details ; 'Silver(I)(2,2'-bipyrazine) hexafluorophosphate' ; _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 10 _diffrn_standards_decay_% none _diffrn_reflns_number 2228 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.89 _reflns_number_total 2228 _reflns_number_gt 2054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.08(3) _refine_ls_number_reflns 2228 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.843203(12) 0.843203(12) 0.0000 0.02356(8) Uani 1 2 d S . . N1 N 0.68877(16) 0.78360(16) 0.09686(19) 0.0233(4) Uani 1 1 d . . . C2 C 0.64283(19) 0.69916(18) 0.0498(2) 0.0210(5) Uani 1 1 d . . . C3 C 0.54677(19) 0.6653(2) 0.0907(2) 0.0250(5) Uani 1 1 d . . . H3A H 0.5164 0.6048 0.0558 0.030 Uiso 1 1 calc R . . N4 N 0.49553(17) 0.71631(16) 0.1787(2) 0.0241(4) Uani 1 1 d . . . C5 C 0.5402(2) 0.80068(19) 0.2234(2) 0.0253(6) Uani 1 1 d . . . H5A H 0.5051 0.8396 0.2843 0.030 Uiso 1 1 calc R . . C6 C 0.63691(18) 0.8337(2) 0.1835(2) 0.0236(5) Uani 1 1 d . . . H6A H 0.6672 0.8939 0.2191 0.028 Uiso 1 1 calc R . . N1S N 0.48000(19) 0.1482(2) 0.2500(2) 0.0440(6) Uani 1 1 d . . . O1S O 0.4004(2) 0.1484(3) 0.3068(3) 0.0630(7) Uani 1 1 d . . . O2S O 0.4995(2) 0.0871(2) 0.1672(2) 0.0569(7) Uani 1 1 d . . . C2S C 0.5601(3) 0.2270(3) 0.2786(4) 0.0547(9) Uani 1 1 d . . . H2SA H 0.5357 0.2711 0.3454 0.082 Uiso 1 1 calc R . . H2SB H 0.5730 0.2702 0.2068 0.082 Uiso 1 1 calc R . . H2SC H 0.6248 0.1919 0.3024 0.082 Uiso 1 1 calc R . . P1 P 0.38434(5) 0.38434(5) 0.0000 0.0333(2) Uani 1 2 d S . . F1 F 0.33349(19) 0.31348(18) 0.1017(2) 0.0700(7) Uani 1 1 d . . . F2 F 0.2985(2) 0.4697(2) 0.0218(2) 0.0871(9) Uani 1 1 d . . . F3 F 0.4548(2) 0.43567(18) 0.10123(19) 0.0709(7) 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 Ag1 0.01760(8) 0.01760(8) 0.03547(13) 0.00159(8) -0.00159(8) -0.00078(10) N1 0.0224(10) 0.0210(10) 0.0264(11) 0.0005(9) 0.0029(8) -0.0027(8) C2 0.0200(12) 0.0182(10) 0.0248(11) 0.0006(9) -0.0005(9) -0.0015(9) C3 0.0220(11) 0.0224(12) 0.0308(13) -0.0021(11) 0.0019(10) -0.0022(11) N4 0.0214(11) 0.0206(10) 0.0304(11) -0.0012(9) 0.0024(9) -0.0009(8) C5 0.0279(13) 0.0200(11) 0.0280(14) -0.0026(9) 0.0052(9) 0.0021(10) C6 0.0256(12) 0.0203(12) 0.0249(12) -0.0027(10) 0.0025(9) -0.0041(11) N1S 0.0356(12) 0.0536(15) 0.0427(13) 0.0043(17) 0.0042(13) 0.0049(11) O1S 0.0413(13) 0.0791(19) 0.0687(16) 0.0089(15) 0.0186(12) 0.0050(15) O2S 0.0549(15) 0.0648(17) 0.0509(14) -0.0128(13) 0.0030(12) 0.0058(13) C2S 0.049(2) 0.049(2) 0.066(2) -0.0044(16) 0.0002(17) -0.0022(16) P1 0.0282(3) 0.0282(3) 0.0434(6) -0.0053(3) 0.0053(3) 0.0014(4) F1 0.0721(16) 0.0571(13) 0.0809(15) 0.0199(11) 0.0159(13) -0.0124(11) F2 0.110(2) 0.0784(16) 0.0724(17) 0.0012(13) 0.0172(15) 0.0652(15) F3 0.0941(19) 0.0555(14) 0.0631(12) 0.0019(11) -0.0232(12) -0.0283(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.240(2) 6_565 ? Ag1 N4 2.240(2) 3_654 ? Ag1 N1 2.377(2) 7 ? Ag1 N1 2.377(2) . ? N1 C6 1.329(3) . ? N1 C2 1.338(3) . ? C2 C3 1.382(3) . ? C2 C2 1.500(5) 7 ? C3 N4 1.342(3) . ? N4 C5 1.320(3) . ? N4 Ag1 2.240(2) 4_465 ? C5 C6 1.383(3) . ? N1S O1S 1.198(3) . ? N1S O2S 1.229(3) . ? N1S C2S 1.475(4) . ? P1 F2 1.572(2) 7 ? P1 F2 1.572(2) . ? P1 F3 1.579(2) . ? P1 F3 1.579(2) 7 ? P1 F1 1.583(2) 7 ? P1 F1 1.583(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N4 135.85(11) 6_565 3_654 ? N4 Ag1 N1 98.87(8) 6_565 7 ? N4 Ag1 N1 117.38(7) 3_654 7 ? N4 Ag1 N1 117.38(7) 6_565 . ? N4 Ag1 N1 98.87(8) 3_654 . ? N1 Ag1 N1 70.45(10) 7 . ? C6 N1 C2 116.7(2) . . ? C6 N1 Ag1 125.75(17) . . ? C2 N1 Ag1 116.99(16) . . ? N1 C2 C3 121.4(2) . . ? N1 C2 C2 117.48(14) . 7 ? C3 C2 C2 121.11(15) . 7 ? N4 C3 C2 121.3(2) . . ? C5 N4 C3 117.2(2) . . ? C5 N4 Ag1 121.81(17) . 4_465 ? C3 N4 Ag1 120.98(17) . 4_465 ? N4 C5 C6 121.5(2) . . ? N1 C6 C5 122.0(2) . . ? O1S N1S O2S 124.2(3) . . ? O1S N1S C2S 118.8(3) . . ? O2S N1S C2S 117.0(3) . . ? F2 P1 F2 179.7(3) 7 . ? F2 P1 F3 90.08(15) 7 . ? F2 P1 F3 90.12(15) . . ? F2 P1 F3 90.12(15) 7 7 ? F2 P1 F3 90.08(15) . 7 ? F3 P1 F3 91.26(16) . 7 ? F2 P1 F1 90.19(14) 7 7 ? F2 P1 F1 89.61(15) . 7 ? F3 P1 F1 179.69(15) . 7 ? F3 P1 F1 88.58(12) 7 7 ? F2 P1 F1 89.61(15) 7 . ? F2 P1 F1 90.19(14) . . ? F3 P1 F1 88.58(12) . . ? F3 P1 F1 179.69(15) 7 . ? F1 P1 F1 91.59(18) 7 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ag1 N1 C6 96.4(2) 6_565 . . . ? N4 Ag1 N1 C6 -57.6(2) 3_654 . . . ? N1 Ag1 N1 C6 -173.6(3) 7 . . . ? N4 Ag1 N1 C2 -92.58(19) 6_565 . . . ? N4 Ag1 N1 C2 113.45(18) 3_654 . . . ? N1 Ag1 N1 C2 -2.56(13) 7 . . . ? C6 N1 C2 C3 -0.7(4) . . . . ? Ag1 N1 C2 C3 -172.6(2) . . . . ? C6 N1 C2 C2 178.8(3) . . . 7 ? Ag1 N1 C2 C2 6.9(4) . . . 7 ? N1 C2 C3 N4 0.4(4) . . . . ? C2 C2 C3 N4 -179.1(3) 7 . . . ? C2 C3 N4 C5 0.8(4) . . . . ? C2 C3 N4 Ag1 -177.2(2) . . . 4_465 ? C3 N4 C5 C6 -1.6(4) . . . . ? Ag1 N4 C5 C6 176.39(19) 4_465 . . . ? C2 N1 C6 C5 -0.1(4) . . . . ? Ag1 N1 C6 C5 170.94(18) . . . . ? N4 C5 C6 N1 1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.745 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.074 #===END data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(pyrazino(2,3-f)quinoxaline)Silver(I)tetrafluoroborate.MeNO2 solvate' ; _chemical_name_common '[Ag(pyq)]BF4.1.5MeNO2' _chemical_melting_point ? _chemical_formula_moiety '[Ag(C6H6N4)]BF4.1.5MeNO2' _chemical_formula_sum 'C11.50 H10.50 Ag B F4 N5.50 O3' _chemical_formula_weight 468.43 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 16.981(2) _cell_length_b 15.1658(17) _cell_length_c 19.436(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.8250(10) _cell_angle_gamma 90.00 _cell_volume 4979.5(10) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6076 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 24.90 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details ? _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 'SMART CCD' _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 12036 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.93 _reflns_number_total 12036 _reflns_number_gt 7692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1169P)^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 12036 _refine_ls_number_parameters 692 _refine_ls_number_restraints 239 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.984 _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 Ag1 Ag 1.03364(3) 0.07026(3) 0.17958(2) 0.03923(14) Uani 1 1 d . . . Ag2 Ag 0.73580(3) 0.38877(3) 0.03149(2) 0.03799(14) Uani 1 1 d . . . Ag3 Ag 0.46745(3) 0.09043(3) 0.21097(3) 0.03980(14) Uani 1 1 d . . . N1 N 1.1735(3) 0.0623(3) 0.1810(3) 0.0344(11) Uani 1 1 d . . . C2 C 1.2144(3) 0.0633(3) 0.2448(3) 0.0291(12) Uani 1 1 d . . . C3 C 1.2969(3) 0.0572(3) 0.2543(3) 0.0292(12) Uani 1 1 d . . . N4 N 1.3395(3) 0.0538(3) 0.1975(3) 0.0367(11) Uani 1 1 d . . . C5 C 1.2983(4) 0.0510(4) 0.1363(3) 0.0402(14) Uani 1 1 d . . . H5A H 1.3260 0.0464 0.0964 0.048 Uiso 1 1 calc R . . C6 C 1.2149(4) 0.0546(4) 0.1275(3) 0.0384(14) Uani 1 1 d . . . H6A H 1.1881 0.0515 0.0822 0.046 Uiso 1 1 calc R . . C7 C 1.1711(3) 0.0708(3) 0.3055(3) 0.0269(11) Uani 1 1 d . . . N8 N 1.0921(3) 0.0804(3) 0.2974(2) 0.0307(10) Uani 1 1 d . . . C9 C 1.0557(3) 0.0876(4) 0.3534(3) 0.0330(12) Uani 1 1 d . . . H9A H 0.9998 0.0952 0.3491 0.040 Uiso 1 1 calc R . . C10 C 1.0978(4) 0.0845(4) 0.4202(3) 0.0367(13) Uani 1 1 d . . . H10A H 1.0693 0.0883 0.4598 0.044 Uiso 1 1 calc R . . N11 N 1.1755(3) 0.0764(3) 0.4288(2) 0.0327(11) Uani 1 1 d . . . C12 C 1.2143(3) 0.0698(3) 0.3709(3) 0.0277(11) Uani 1 1 d . . . C13 C 1.2983(3) 0.0614(4) 0.3775(3) 0.0309(12) Uani 1 1 d . . . H13A H 1.3264 0.0600 0.4223 0.037 Uiso 1 1 calc R . . C14 C 1.3379(3) 0.0553(4) 0.3223(3) 0.0314(12) Uani 1 1 d . . . H14A H 1.3939 0.0497 0.3280 0.038 Uiso 1 1 calc R . . N21 N 0.8336(3) 0.2814(3) 0.0666(2) 0.0300(10) Uani 1 1 d . . . C22 C 0.8870(3) 0.3100(3) 0.1185(3) 0.0249(11) Uani 1 1 d . . . C23 C 0.9457(3) 0.2546(3) 0.1504(3) 0.0273(11) Uani 1 1 d . . . N24 N 0.9486(3) 0.1676(3) 0.1319(2) 0.0316(10) Uani 1 1 d . . . C25 C 0.8937(4) 0.1413(4) 0.0823(3) 0.0369(13) Uani 1 1 d . . . H25A H 0.8928 0.0810 0.0689 0.044 Uiso 1 1 calc R . . C26 C 0.8377(4) 0.1977(4) 0.0492(3) 0.0379(14) Uani 1 1 d . . . H26A H 0.8014 0.1755 0.0129 0.045 Uiso 1 1 calc R . . C27 C 0.8838(3) 0.3996(4) 0.1414(3) 0.0271(11) Uani 1 1 d . . . N28 N 0.8227(3) 0.4515(3) 0.1148(3) 0.0343(11) Uani 1 1 d . . . C29 C 0.8222(4) 0.5335(4) 0.1382(4) 0.0443(15) Uani 1 1 d . . . H29A H 0.7797 0.5713 0.1220 0.053 Uiso 1 1 calc R . . C30 C 0.8812(4) 0.5659(4) 0.1853(4) 0.0494(17) Uani 1 1 d . . . H30A H 0.8782 0.6258 0.1992 0.059 Uiso 1 1 calc R . . N31 N 0.9408(3) 0.5189(3) 0.2118(3) 0.0373(11) Uani 1 1 d . . . C32 C 0.9418(3) 0.4322(4) 0.1907(3) 0.0300(12) Uani 1 1 d . . . C33 C 1.0026(3) 0.3750(4) 0.2200(3) 0.0309(12) Uani 1 1 d . . . H33A H 1.0426 0.3973 0.2532 0.037 Uiso 1 1 calc R . . C34 C 1.0044(3) 0.2892(4) 0.2013(3) 0.0299(12) Uani 1 1 d . . . H34A H 1.0448 0.2516 0.2220 0.036 Uiso 1 1 calc R . . N41 N 0.5471(3) 0.1842(3) 0.1519(3) 0.0365(11) Uani 1 1 d . . . C42 C 0.5585(3) 0.2674(4) 0.1755(3) 0.0353(13) Uani 1 1 d . . . C43 C 0.6065(3) 0.3275(4) 0.1427(3) 0.0346(13) Uani 1 1 d . . . N44 N 0.6411(3) 0.3021(4) 0.0861(3) 0.0414(12) Uani 1 1 d . . . C45 C 0.6294(4) 0.2209(5) 0.0644(3) 0.0452(16) Uani 1 1 d . . . H45A H 0.6533 0.2016 0.0249 0.054 Uiso 1 1 calc R . . C46 C 0.5824(4) 0.1614(5) 0.0982(3) 0.0426(15) Uani 1 1 d . . . H46A H 0.5762 0.1028 0.0812 0.051 Uiso 1 1 calc R . . C47 C 0.5193(3) 0.2970(4) 0.2339(3) 0.0338(13) Uani 1 1 d . . . N48 N 0.4731(3) 0.2394(3) 0.2655(3) 0.0381(12) Uani 1 1 d . . . C49 C 0.4354(4) 0.2728(4) 0.3161(4) 0.0447(16) Uani 1 1 d . . . H49A H 0.4036 0.2346 0.3404 0.054 Uiso 1 1 calc R . . C50 C 0.4401(4) 0.3620(4) 0.3355(4) 0.0420(15) Uani 1 1 d . . . H50A H 0.4096 0.3827 0.3706 0.050 Uiso 1 1 calc R . . N51 N 0.4864(3) 0.4176(3) 0.3058(3) 0.0377(12) Uani 1 1 d . . . C52 C 0.5275(3) 0.3853(4) 0.2549(3) 0.0343(13) Uani 1 1 d . . . C53 C 0.5799(3) 0.4423(4) 0.2218(4) 0.0389(14) Uani 1 1 d . . . H53A H 0.5884 0.5009 0.2382 0.047 Uiso 1 1 calc R . . C54 C 0.6164(4) 0.4144(4) 0.1688(3) 0.0395(14) Uani 1 1 d . . . H54A H 0.6502 0.4538 0.1477 0.047 Uiso 1 1 calc R . . O1S O 0.7270(7) 1.0263(6) 0.0462(5) 0.082(3) Uiso 0.65 1 d PD A 1 O1S' O 0.7749(10) 0.9865(14) 0.0461(10) 0.089(6) Uiso 0.35 1 d PD A 2 O2S O 0.6780(6) 0.9025(6) 0.0406(4) 0.130(4) Uani 1 1 d D A . N3S N 0.7214(5) 0.9541(5) 0.0735(3) 0.071(2) Uani 1 1 d D . . C4S C 0.7405(7) 0.9451(9) 0.1471(4) 0.101(4) Uani 1 1 d D A . H4SA H 0.6944 0.9224 0.1679 0.151 Uiso 1 1 calc R . . H4SB H 0.7553 1.0028 0.1672 0.151 Uiso 1 1 calc R . . H4SC H 0.7849 0.9041 0.1564 0.151 Uiso 1 1 calc R . . O5S O 0.4498(5) 0.9484(6) 0.0502(4) 0.112(3) Uani 1 1 d D . . O6S O 0.5390(4) 0.9612(4) 0.1353(3) 0.0840(19) Uani 1 1 d D . . N7S N 0.4990(4) 0.9173(4) 0.0935(3) 0.0657(19) Uani 1 1 d D . . C8S C 0.5104(5) 0.8217(5) 0.0938(5) 0.070(2) Uani 1 1 d D . . H8SA H 0.5513 0.8056 0.1310 0.105 Uiso 1 1 calc R . . H8SB H 0.5270 0.8030 0.0492 0.105 Uiso 1 1 calc R . . H8SC H 0.4606 0.7924 0.1015 0.105 Uiso 1 1 calc R . . O9S O 1.0455(4) -0.1556(5) 0.4831(4) 0.095(2) Uani 1 1 d D . . O10S O 1.1145(5) -0.0600(4) 0.5432(4) 0.094(2) Uani 1 1 d D . . N11S N 1.1086(4) -0.1303(4) 0.5123(3) 0.0611(17) Uani 1 1 d D . . C12S C 1.1792(5) -0.1850(7) 0.5137(5) 0.089(3) Uani 1 1 d D . . H12A H 1.1666 -0.2394 0.4878 0.134 Uiso 1 1 calc R . . H12B H 1.1979 -0.1995 0.5618 0.134 Uiso 1 1 calc R . . H12C H 1.2206 -0.1528 0.4926 0.134 Uiso 1 1 calc R . . O13S O 1.3226(6) 0.2424(4) 0.1543(5) 0.138(4) Uani 1 1 d D . . O14S O 1.3293(6) 0.3787(5) 0.1701(7) 0.145(4) Uani 1 1 d D . . N15S N 1.2910(5) 0.3123(4) 0.1637(4) 0.081(2) Uani 1 1 d D . . C16S C 1.2049(6) 0.3163(7) 0.1594(5) 0.086(3) Uani 1 1 d D . . H16A H 1.1824 0.2656 0.1330 0.129 Uiso 1 1 calc R . . H16B H 1.1865 0.3710 0.1361 0.129 Uiso 1 1 calc R . . H16C H 1.1880 0.3151 0.2061 0.129 Uiso 1 1 calc R . . B1 B 0.6982(4) 0.7029(4) 0.2274(3) 0.066(3) Uani 1 1 d D . . F1 F 0.6484(8) 0.6417(9) 0.1967(8) 0.190(8) Uiso 0.60 1 d PD B 1 F2 F 0.6632(5) 0.7846(5) 0.2334(4) 0.069(2) Uiso 0.60 1 d PD B 1 F3 F 0.7631(5) 0.7162(6) 0.1902(5) 0.080(3) Uiso 0.60 1 d PD B 1 F4 F 0.7300(7) 0.6799(9) 0.2927(5) 0.119(4) Uiso 0.60 1 d PD B 1 F1' F 0.7344(7) 0.7066(8) 0.1679(5) 0.063(3) Uiso 0.40 1 d PD B 2 F2' F 0.6206(6) 0.6744(10) 0.2088(7) 0.099(5) Uiso 0.40 1 d PD B 2 F3' F 0.6983(9) 0.7789(7) 0.2634(7) 0.099(5) Uiso 0.40 1 d PD B 2 F4' F 0.7334(11) 0.6359(11) 0.2679(9) 0.164(9) Uiso 0.40 1 d PD B 2 B2 B 1.2154(3) 0.3103(3) 0.3602(3) 0.0374(15) Uani 1 1 d D . . F5 F 1.2724(4) 0.3676(5) 0.3885(4) 0.067(2) Uiso 0.60 1 d PD C 1 F6 F 1.1529(4) 0.3543(5) 0.3244(4) 0.071(2) Uiso 0.60 1 d PD C 1 F7 F 1.2476(4) 0.2513(4) 0.3150(3) 0.0597(18) Uiso 0.60 1 d PD C 1 F8 F 1.1877(4) 0.2618(4) 0.4135(3) 0.0584(18) Uiso 0.60 1 d PD C 1 F5' F 1.2495(5) 0.3667(6) 0.3151(4) 0.051(2) Uiso 0.40 1 d PD C 2 F6' F 1.1535(5) 0.2651(7) 0.3261(5) 0.066(3) Uiso 0.40 1 d PD C 2 F7' F 1.2746(5) 0.2563(6) 0.3916(5) 0.063(3) Uiso 0.40 1 d PD C 2 F8' F 1.1898(6) 0.3634(7) 0.4123(5) 0.072(3) Uiso 0.40 1 d PD C 2 B3 B 0.9547(8) 0.5827(10) -0.0015(8) 0.122(11) Uiso 0.50 1 d PD . . F9 F 0.9707(12) 0.5105(12) 0.0396(10) 0.214(10) Uiso 0.50 1 d PD . . F10 F 0.9649(11) 0.5611(14) -0.0677(8) 0.195(9) Uiso 0.50 1 d PD . . F11 F 0.8798(7) 0.6119(8) 0.0015(6) 0.097(4) Uiso 0.50 1 d PD . . F12 F 1.0060(11) 0.6477(13) 0.0214(12) 0.253(12) Uiso 0.50 1 d PD . . O17S O 1.1191(10) 0.2167(11) -0.1016(8) 0.108(5) Uiso 0.50 1 d PD D 1 O18S O 1.1811(12) 0.2004(15) 0.0030(10) 0.147(7) Uiso 0.50 1 d PD D 1 N19S N 1.1240(11) 0.2019(14) -0.0399(8) 0.104(6) Uiso 0.50 1 d PD D 1 C20S C 1.0630(15) 0.1791(19) 0.0036(14) 0.122(9) Uiso 0.50 1 d PD D 1 H20A H 1.0864 0.1728 0.0516 0.184 Uiso 0.50 1 calc PR D 1 H20B H 1.0383 0.1232 -0.0121 0.184 Uiso 0.50 1 calc PR D 1 H20C H 1.0228 0.2257 0.0010 0.184 Uiso 0.50 1 calc PR D 1 B4 B 1.0359(6) 0.0627(7) -0.0183(5) 0.069(6) Uani 0.50 1 d PD . 2 F13 F 1.0585(6) 0.0242(7) 0.0440(5) 0.077(3) Uiso 0.50 1 d PD . 2 F14 F 1.0987(6) 0.0629(6) -0.0574(5) 0.076(3) Uiso 0.50 1 d PD E 2 F15 F 1.0117(8) 0.1482(8) -0.0125(7) 0.118(5) Uiso 0.50 1 d PD F 2 F16 F 0.9726(6) 0.0148(8) -0.0495(6) 0.088(3) Uiso 0.50 1 d PD . 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 0.0441(3) 0.0333(3) 0.0388(3) 0.00513(19) -0.0031(2) 0.0131(2) Ag2 0.0240(2) 0.0507(3) 0.0377(2) 0.0164(2) -0.00423(18) 0.00092(19) Ag3 0.0342(3) 0.0318(2) 0.0558(3) 0.0099(2) 0.0165(2) 0.00414(19) N1 0.037(3) 0.028(2) 0.039(3) 0.005(2) 0.007(2) 0.004(2) C2 0.035(3) 0.021(3) 0.032(3) 0.002(2) 0.006(2) 0.000(2) C3 0.030(3) 0.020(3) 0.039(3) 0.006(2) 0.010(2) 0.000(2) N4 0.038(3) 0.029(3) 0.045(3) 0.004(2) 0.015(2) 0.006(2) C5 0.043(4) 0.039(3) 0.041(3) 0.005(3) 0.015(3) 0.004(3) C6 0.047(4) 0.032(3) 0.037(3) 0.006(3) 0.007(3) 0.002(3) C7 0.027(3) 0.018(2) 0.036(3) 0.000(2) 0.003(2) 0.001(2) N8 0.029(2) 0.027(2) 0.035(2) -0.0016(19) -0.001(2) -0.0008(19) C9 0.022(3) 0.041(3) 0.035(3) -0.005(2) 0.002(2) -0.005(2) C10 0.027(3) 0.044(4) 0.039(3) -0.009(3) 0.005(2) -0.003(3) N11 0.030(2) 0.034(3) 0.034(2) -0.008(2) 0.002(2) -0.005(2) C12 0.027(3) 0.023(3) 0.033(3) -0.002(2) 0.005(2) -0.001(2) C13 0.028(3) 0.028(3) 0.037(3) -0.001(2) 0.002(2) -0.001(2) C14 0.024(3) 0.028(3) 0.042(3) 0.006(2) 0.003(2) 0.002(2) N21 0.025(2) 0.032(3) 0.031(2) 0.0012(19) -0.0058(19) 0.0005(19) C22 0.021(2) 0.025(3) 0.027(3) 0.002(2) -0.002(2) -0.001(2) C23 0.026(3) 0.024(3) 0.031(3) 0.002(2) 0.000(2) 0.003(2) N24 0.030(2) 0.026(2) 0.037(3) -0.001(2) -0.005(2) 0.0006(19) C25 0.035(3) 0.028(3) 0.047(3) -0.008(3) -0.001(3) 0.000(2) C26 0.036(3) 0.042(4) 0.033(3) -0.007(3) -0.008(3) -0.002(3) C27 0.020(2) 0.030(3) 0.031(3) 0.005(2) 0.001(2) 0.001(2) N28 0.025(2) 0.030(3) 0.047(3) 0.004(2) 0.001(2) 0.003(2) C29 0.037(3) 0.024(3) 0.070(4) 0.005(3) 0.001(3) 0.009(3) C30 0.046(4) 0.028(3) 0.075(5) -0.015(3) 0.004(4) 0.003(3) N31 0.035(3) 0.028(3) 0.049(3) -0.006(2) 0.002(2) -0.003(2) C32 0.029(3) 0.028(3) 0.033(3) 0.000(2) 0.002(2) -0.002(2) C33 0.026(3) 0.029(3) 0.036(3) -0.003(2) -0.004(2) -0.002(2) C34 0.023(3) 0.034(3) 0.031(3) 0.003(2) -0.006(2) 0.004(2) N41 0.031(3) 0.036(3) 0.043(3) 0.008(2) 0.007(2) 0.001(2) C42 0.024(3) 0.037(3) 0.045(3) 0.013(3) 0.002(2) 0.002(2) C43 0.021(3) 0.039(3) 0.043(3) 0.014(3) 0.001(2) 0.002(2) N44 0.032(3) 0.049(3) 0.043(3) 0.011(2) 0.004(2) -0.003(2) C45 0.036(3) 0.056(4) 0.045(4) 0.012(3) 0.014(3) -0.001(3) C46 0.038(3) 0.044(4) 0.048(4) 0.001(3) 0.010(3) -0.001(3) C47 0.025(3) 0.033(3) 0.044(3) 0.011(2) 0.004(2) 0.003(2) N48 0.035(3) 0.029(3) 0.054(3) 0.009(2) 0.018(2) 0.005(2) C49 0.040(3) 0.032(3) 0.065(4) 0.009(3) 0.018(3) -0.002(3) C50 0.039(3) 0.034(3) 0.056(4) 0.005(3) 0.020(3) 0.004(3) N51 0.030(3) 0.029(3) 0.054(3) 0.007(2) 0.005(2) 0.001(2) C52 0.023(3) 0.030(3) 0.049(3) 0.012(3) -0.001(2) 0.000(2) C53 0.024(3) 0.029(3) 0.061(4) 0.014(3) -0.003(3) -0.004(2) C54 0.028(3) 0.040(3) 0.050(4) 0.016(3) 0.003(3) -0.005(3) O2S 0.173(10) 0.125(7) 0.086(5) -0.004(5) -0.013(6) -0.060(7) N3S 0.077(5) 0.074(5) 0.064(4) -0.002(4) 0.017(4) -0.018(4) C4S 0.094(8) 0.129(10) 0.073(6) 0.006(6) -0.027(6) -0.007(7) O5S 0.124(7) 0.116(7) 0.091(5) 0.011(5) -0.012(5) 0.037(6) O6S 0.117(6) 0.063(4) 0.075(4) -0.020(3) 0.023(4) -0.008(4) N7S 0.073(5) 0.064(5) 0.063(4) -0.012(4) 0.018(4) -0.005(4) C8S 0.065(5) 0.053(5) 0.094(6) -0.023(5) 0.023(5) -0.003(4) O9S 0.052(4) 0.121(6) 0.110(6) -0.022(5) 0.000(4) -0.005(4) O10S 0.142(7) 0.050(4) 0.091(5) -0.021(3) 0.011(4) -0.010(4) N11S 0.072(5) 0.053(4) 0.062(4) -0.001(3) 0.027(4) -0.001(4) C12S 0.063(6) 0.110(9) 0.093(7) -0.029(6) -0.003(5) 0.005(6) O13S 0.165(9) 0.054(4) 0.172(8) -0.016(5) -0.088(7) 0.039(5) O14S 0.143(8) 0.039(4) 0.250(12) -0.005(6) 0.011(8) -0.007(5) N15S 0.128(8) 0.035(4) 0.074(5) 0.003(3) -0.013(5) 0.011(4) C16S 0.110(9) 0.064(6) 0.080(6) 0.005(5) -0.006(6) 0.006(6) B1 0.091(8) 0.055(6) 0.054(5) 0.010(4) 0.022(5) 0.019(5) B2 0.037(4) 0.031(3) 0.043(4) 0.002(3) -0.004(3) 0.002(3) B4 0.114(18) 0.061(12) 0.036(9) -0.002(8) 0.027(10) 0.014(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N24 2.202(5) . y Ag1 N51 2.362(5) 2_645 y Ag1 N1 2.376(5) . y Ag1 N8 2.406(5) . y Ag2 N11 2.213(5) 4_565 y Ag2 N28 2.284(5) . y Ag2 N21 2.377(5) . y Ag2 N44 2.406(5) . y Ag3 N4 2.232(5) 1_455 y Ag3 N31 2.320(5) 2_645 y Ag3 N41 2.341(5) . y Ag3 N48 2.493(5) . y N1 C6 1.318(8) . ? N1 C2 1.358(7) . ? C2 C3 1.399(8) . ? C2 C7 1.456(7) . ? C3 N4 1.379(7) . ? C3 C14 1.431(8) . ? N4 C5 1.318(8) . ? N4 Ag3 2.232(5) 1_655 ? C5 C6 1.410(9) . ? C7 N8 1.342(7) . ? C7 C12 1.403(8) . ? N8 C9 1.310(7) . ? C9 C10 1.419(8) . ? C10 N11 1.319(8) . ? N11 C12 1.365(7) . ? N11 Ag2 2.213(5) 4_666 ? C12 C13 1.424(8) . ? C13 C14 1.326(8) . ? N21 C26 1.317(8) . ? N21 C22 1.357(7) . ? C22 C23 1.400(7) . ? C22 C27 1.432(7) . ? C23 N24 1.371(7) . ? C23 C34 1.429(8) . ? N24 C25 1.334(7) . ? C25 C26 1.388(8) . ? C27 N28 1.363(7) . ? C27 C32 1.394(8) . ? N28 C29 1.325(8) . ? C29 C30 1.377(10) . ? C30 N31 1.302(9) . ? N31 C32 1.378(7) . ? N31 Ag3 2.320(5) 2_655 ? C32 C33 1.422(8) . ? C33 C34 1.352(8) . ? N41 C46 1.302(8) . ? N41 C42 1.350(8) . ? C42 C43 1.416(8) . ? C42 C47 1.444(8) . ? C43 N44 1.354(8) . ? C43 C54 1.416(9) . ? N44 C45 1.310(9) . ? C45 C46 1.411(9) . ? C47 N48 1.361(7) . ? C47 C52 1.402(8) . ? N48 C49 1.329(8) . ? C49 C50 1.403(9) . ? C50 N51 1.325(8) . ? N51 C52 1.359(8) . ? N51 Ag1 2.362(5) 2_655 ? C52 C53 1.438(8) . ? C53 C54 1.324(9) . ? O1S N3S 1.225(7) . ? O1S' N3S 1.205(8) . ? O2S N3S 1.211(6) . ? N3S C4S 1.442(8) . ? O5S N7S 1.219(6) . ? O6S N7S 1.205(6) . ? N7S C8S 1.463(8) . ? O9S N11S 1.222(6) . ? O10S N11S 1.223(6) . ? N11S C12S 1.455(8) . ? O13S N15S 1.212(6) . ? O14S N15S 1.198(7) . ? N15S C16S 1.456(8) . ? B1 F3' 1.348(8) . ? B1 F1 1.352(8) . ? B1 F1' 1.364(7) . ? B1 F4 1.373(7) . ? B1 F4' 1.384(8) . ? B1 F2 1.385(7) . ? B1 F3 1.392(7) . ? B1 F2' 1.399(8) . ? B2 F6' 1.368(7) . ? B2 F5 1.373(6) . ? B2 F6 1.379(6) . ? B2 F7' 1.389(7) . ? B2 F8 1.391(6) . ? B2 F5' 1.393(7) . ? B2 F8' 1.396(7) . ? B2 F7 1.404(6) . ? B3 F11 1.354(9) . ? B3 F10 1.355(9) . ? B3 F12 1.360(9) . ? B3 F9 1.367(9) . ? F9 F10 1.60(3) 3_765 ? F10 F9 1.60(3) 3_765 ? O17S N19S 1.214(8) . ? O18S N19S 1.213(8) . ? N19S C20S 1.445(10) . ? B4 F13 1.363(8) . ? B4 F15 1.368(8) . ? B4 F14 1.373(8) . ? B4 F16 1.384(8) . ? B4 F16 1.782(16) 3_755 ? F13 F16 0.808(13) 3_755 ? F16 F13 0.808(13) 3_755 ? F16 B4 1.782(16) 3_755 ? 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 N24 Ag1 N51 127.70(18) . 2_645 y N24 Ag1 N1 130.61(17) . . y N51 Ag1 N1 96.02(17) 2_645 . y N24 Ag1 N8 123.17(17) . . y N51 Ag1 N8 89.91(17) 2_645 . y N1 Ag1 N8 71.13(16) . . y N11 Ag2 N28 138.25(18) 4_565 . y N11 Ag2 N21 131.98(17) 4_565 . y N28 Ag2 N21 72.51(16) . . y N11 Ag2 N44 105.05(18) 4_565 . y N28 Ag2 N44 109.12(18) . . y N21 Ag2 N44 88.75(17) . . y N4 Ag3 N31 122.74(18) 1_455 2_645 y N4 Ag3 N41 134.24(18) 1_455 . y N31 Ag3 N41 102.58(17) 2_645 . y N4 Ag3 N48 105.69(17) 1_455 . y N31 Ag3 N48 98.90(18) 2_645 . y N41 Ag3 N48 70.03(17) . . y C6 N1 C2 117.2(5) . . ? C6 N1 Ag1 127.4(4) . . ? C2 N1 Ag1 115.3(4) . . ? N1 C2 C3 122.1(5) . . ? N1 C2 C7 119.2(5) . . ? C3 C2 C7 118.7(5) . . ? N4 C3 C2 119.8(5) . . ? N4 C3 C14 119.5(5) . . ? C2 C3 C14 120.7(5) . . ? C5 N4 C3 116.7(5) . . ? C5 N4 Ag3 122.3(4) . 1_655 ? C3 N4 Ag3 118.7(4) . 1_655 ? N4 C5 C6 122.9(6) . . ? N1 C6 C5 121.1(6) . . ? N8 C7 C12 122.2(5) . . ? N8 C7 C2 119.6(5) . . ? C12 C7 C2 118.2(5) . . ? C9 N8 C7 117.6(5) . . ? C9 N8 Ag1 127.7(4) . . ? C7 N8 Ag1 114.5(4) . . ? N8 C9 C10 121.4(5) . . ? N11 C10 C9 121.5(5) . . ? C10 N11 C12 117.7(5) . . ? C10 N11 Ag2 117.2(4) . 4_666 ? C12 N11 Ag2 122.9(4) . 4_666 ? N11 C12 C7 119.6(5) . . ? N11 C12 C13 119.7(5) . . ? C7 C12 C13 120.7(5) . . ? C14 C13 C12 121.3(5) . . ? C13 C14 C3 120.5(5) . . ? C26 N21 C22 116.8(5) . . ? C26 N21 Ag2 129.8(4) . . ? C22 N21 Ag2 112.9(3) . . ? N21 C22 C23 121.9(5) . . ? N21 C22 C27 119.4(5) . . ? C23 C22 C27 118.7(5) . . ? N24 C23 C22 120.3(5) . . ? N24 C23 C34 119.5(5) . . ? C22 C23 C34 120.1(5) . . ? C25 N24 C23 115.9(5) . . ? C25 N24 Ag1 119.0(4) . . ? C23 N24 Ag1 125.1(4) . . ? N24 C25 C26 123.1(5) . . ? N21 C26 C25 121.8(5) . . ? N28 C27 C32 121.0(5) . . ? N28 C27 C22 118.8(5) . . ? C32 C27 C22 120.2(5) . . ? C29 N28 C27 116.3(5) . . ? C29 N28 Ag2 127.5(4) . . ? C27 N28 Ag2 116.1(4) . . ? N28 C29 C30 122.3(6) . . ? N31 C30 C29 123.5(6) . . ? C30 N31 C32 116.0(5) . . ? C30 N31 Ag3 116.4(4) . 2_655 ? C32 N31 Ag3 127.7(4) . 2_655 ? N31 C32 C27 120.9(5) . . ? N31 C32 C33 119.6(5) . . ? C27 C32 C33 119.5(5) . . ? C34 C33 C32 121.0(5) . . ? C33 C34 C23 120.4(5) . . ? C46 N41 C42 117.3(5) . . ? C46 N41 Ag3 124.6(4) . . ? C42 N41 Ag3 118.2(4) . . ? N41 C42 C43 121.2(6) . . ? N41 C42 C47 119.7(5) . . ? C43 C42 C47 119.0(6) . . ? N44 C43 C54 120.7(5) . . ? N44 C43 C42 119.9(6) . . ? C54 C43 C42 119.4(6) . . ? C45 N44 C43 117.7(5) . . ? C45 N44 Ag2 117.2(4) . . ? C43 N44 Ag2 124.6(4) . . ? N44 C45 C46 121.7(6) . . ? N41 C46 C45 122.1(6) . . ? N48 C47 C52 121.8(5) . . ? N48 C47 C42 119.2(5) . . ? C52 C47 C42 119.0(5) . . ? C49 N48 C47 115.6(5) . . ? C49 N48 Ag3 131.3(4) . . ? C47 N48 Ag3 112.9(4) . . ? N48 C49 C50 123.3(6) . . ? N51 C50 C49 121.1(6) . . ? C50 N51 C52 117.4(5) . . ? C50 N51 Ag1 118.2(4) . 2_655 ? C52 N51 Ag1 122.1(4) . 2_655 ? N51 C52 C47 120.8(5) . . ? N51 C52 C53 119.7(6) . . ? C47 C52 C53 119.5(6) . . ? C54 C53 C52 121.0(6) . . ? C53 C54 C43 121.9(5) . . ? O1S' N3S O2S 118.5(12) . . ? O1S' N3S O1S 49.3(11) . . ? O2S N3S O1S 114.8(9) . . ? O1S' N3S C4S 111.9(12) . . ? O2S N3S C4S 121.8(8) . . ? O1S N3S C4S 119.6(9) . . ? O6S N7S O5S 123.4(8) . . ? O6S N7S C8S 118.6(7) . . ? O5S N7S C8S 117.9(8) . . ? O9S N11S O10S 121.7(8) . . ? O9S N11S C12S 120.8(7) . . ? O10S N11S C12S 117.4(8) . . ? O14S N15S O13S 120.5(9) . . ? O14S N15S C16S 120.1(8) . . ? O13S N15S C16S 119.0(8) . . ? F3' B1 F1 141.5(10) . . ? F3' B1 F1' 115.4(8) . . ? F1 B1 F1' 88.3(9) . . ? F3' B1 F4 75.9(8) . . ? F1 B1 F4 113.8(8) . . ? F1' B1 F4 128.7(8) . . ? F3' B1 F4' 110.7(9) . . ? F1 B1 F4' 87.8(11) . . ? F1' B1 F4' 107.9(8) . . ? F4 B1 F4' 35.0(9) . . ? F3' B1 F2 33.8(6) . . ? F1 B1 F2 113.4(8) . . ? F1' B1 F2 105.7(7) . . ? F4 B1 F2 106.3(7) . . ? F4' B1 F2 140.6(9) . . ? F3' B1 F3 100.8(8) . . ? F1 B1 F3 111.3(8) . . ? F1' B1 F3 26.6(6) . . ? F4 B1 F3 105.0(7) . . ? F4' B1 F3 94.8(9) . . ? F2 B1 F3 106.5(6) . . ? F3' B1 F2' 110.4(8) . . ? F1 B1 F2' 31.1(9) . . ? F1' B1 F2' 106.8(8) . . ? F4 B1 F2' 115.6(9) . . ? F4' B1 F2' 105.1(9) . . ? F2 B1 F2' 84.1(8) . . ? F3 B1 F2' 133.3(8) . . ? F6' B2 F5 170.5(7) . . ? F6' B2 F6 59.0(6) . . ? F5 B2 F6 111.7(5) . . ? F6' B2 F7' 113.8(6) . . ? F5 B2 F7' 75.4(6) . . ? F6 B2 F7' 172.5(6) . . ? F6' B2 F8 78.2(6) . . ? F5 B2 F8 108.3(5) . . ? F6 B2 F8 109.4(5) . . ? F7' B2 F8 69.2(5) . . ? F6' B2 F5' 110.5(6) . . ? F5 B2 F5' 62.8(5) . . ? F6 B2 F5' 74.5(5) . . ? F7' B2 F5' 108.1(6) . . ? F8 B2 F5' 171.0(6) . . ? F6' B2 F8' 111.1(6) . . ? F5 B2 F8' 66.6(6) . . ? F6 B2 F8' 78.9(6) . . ? F7' B2 F8' 106.6(6) . . ? F8 B2 F8' 67.2(6) . . ? F5' B2 F8' 106.4(6) . . ? F6' B2 F7 72.9(6) . . ? F5 B2 F7 110.5(5) . . ? F6 B2 F7 108.7(5) . . ? F7' B2 F7 65.7(5) . . ? F8 B2 F7 108.2(5) . . ? F5' B2 F7 77.5(5) . . ? F8' B2 F7 172.3(6) . . ? F11 B3 F10 109.3(10) . . ? F11 B3 F12 108.7(10) . . ? F10 B3 F12 110.3(10) . . ? F11 B3 F9 111.6(10) . . ? F10 B3 F9 109.0(10) . . ? F12 B3 F9 107.9(10) . . ? B3 F9 F10 146.4(17) . 3_765 ? B3 F10 F9 89.3(15) . 3_765 ? O18S N19S O17S 131(2) . . ? O18S N19S C20S 99.4(19) . . ? O17S N19S C20S 130(2) . . ? F13 B4 F15 113.0(8) . . ? F13 B4 F14 109.2(8) . . ? F15 B4 F14 107.4(8) . . ? F13 B4 F16 107.5(8) . . ? F15 B4 F16 108.0(8) . . ? F14 B4 F16 111.8(8) . . ? F13 B4 F16 25.6(6) . 3_755 ? F15 B4 F16 121.1(9) . 3_755 ? F14 B4 F16 122.5(9) . 3_755 ? F16 B4 F16 82.0(8) . 3_755 ? F16 F13 B4 107.5(14) 3_755 . ? F13 F16 B4 144.6(15) 3_755 . ? F13 F16 B4 46.9(10) 3_755 3_755 ? B4 F16 B4 98.0(8) . 3_755 ? 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 N24 Ag1 N1 C6 -61.4(6) . . . . ? N51 Ag1 N1 C6 92.9(5) 2_645 . . . ? N8 Ag1 N1 C6 -179.3(5) . . . . ? N24 Ag1 N1 C2 120.7(4) . . . . ? N51 Ag1 N1 C2 -85.1(4) 2_645 . . . ? N8 Ag1 N1 C2 2.7(4) . . . . ? C6 N1 C2 C3 0.4(8) . . . . ? Ag1 N1 C2 C3 178.6(4) . . . . ? C6 N1 C2 C7 -179.4(5) . . . . ? Ag1 N1 C2 C7 -1.2(6) . . . . ? N1 C2 C3 N4 2.8(8) . . . . ? C7 C2 C3 N4 -177.3(5) . . . . ? N1 C2 C3 C14 -177.7(5) . . . . ? C7 C2 C3 C14 2.1(8) . . . . ? C2 C3 N4 C5 -4.1(8) . . . . ? C14 C3 N4 C5 176.5(5) . . . . ? C2 C3 N4 Ag3 159.1(4) . . . 1_655 ? C14 C3 N4 Ag3 -20.3(7) . . . 1_655 ? C3 N4 C5 C6 2.3(9) . . . . ? Ag3 N4 C5 C6 -160.2(5) 1_655 . . . ? C2 N1 C6 C5 -2.3(8) . . . . ? Ag1 N1 C6 C5 179.8(4) . . . . ? N4 C5 C6 N1 0.9(10) . . . . ? N1 C2 C7 N8 -2.8(8) . . . . ? C3 C2 C7 N8 177.3(5) . . . . ? N1 C2 C7 C12 178.6(5) . . . . ? C3 C2 C7 C12 -1.3(7) . . . . ? C12 C7 N8 C9 -0.9(8) . . . . ? C2 C7 N8 C9 -179.4(5) . . . . ? C12 C7 N8 Ag1 -176.2(4) . . . . ? C2 C7 N8 Ag1 5.2(6) . . . . ? N24 Ag1 N8 C9 54.3(5) . . . . ? N51 Ag1 N8 C9 -82.6(5) 2_645 . . . ? N1 Ag1 N8 C9 -179.0(5) . . . . ? N24 Ag1 N8 C7 -130.9(4) . . . . ? N51 Ag1 N8 C7 92.2(4) 2_645 . . . ? N1 Ag1 N8 C7 -4.2(3) . . . . ? C7 N8 C9 C10 -0.8(8) . . . . ? Ag1 N8 C9 C10 173.9(4) . . . . ? N8 C9 C10 N11 1.7(9) . . . . ? C9 C10 N11 C12 -0.9(9) . . . . ? C9 C10 N11 Ag2 162.5(5) . . . 4_666 ? C10 N11 C12 C7 -0.7(8) . . . . ? Ag2 N11 C12 C7 -163.1(4) 4_666 . . . ? C10 N11 C12 C13 179.7(5) . . . . ? Ag2 N11 C12 C13 17.3(7) 4_666 . . . ? N8 C7 C12 N11 1.7(8) . . . . ? C2 C7 C12 N11 -179.8(5) . . . . ? N8 C7 C12 C13 -178.7(5) . . . . ? C2 C7 C12 C13 -0.2(8) . . . . ? N11 C12 C13 C14 -179.6(5) . . . . ? C7 C12 C13 C14 0.8(8) . . . . ? C12 C13 C14 C3 0.0(9) . . . . ? N4 C3 C14 C13 177.9(5) . . . . ? C2 C3 C14 C13 -1.5(8) . . . . ? N11 Ag2 N21 C26 -45.8(6) 4_565 . . . ? N28 Ag2 N21 C26 174.0(5) . . . . ? N44 Ag2 N21 C26 63.5(5) . . . . ? N11 Ag2 N21 C22 142.9(3) 4_565 . . . ? N28 Ag2 N21 C22 2.7(4) . . . . ? N44 Ag2 N21 C22 -107.8(4) . . . . ? C26 N21 C22 C23 2.3(8) . . . . ? Ag2 N21 C22 C23 174.9(4) . . . . ? C26 N21 C22 C27 -177.9(5) . . . . ? Ag2 N21 C22 C27 -5.4(6) . . . . ? N21 C22 C23 N24 -3.0(8) . . . . ? C27 C22 C23 N24 177.2(5) . . . . ? N21 C22 C23 C34 175.4(5) . . . . ? C27 C22 C23 C34 -4.4(8) . . . . ? C22 C23 N24 C25 0.9(8) . . . . ? C34 C23 N24 C25 -177.5(5) . . . . ? C22 C23 N24 Ag1 -177.4(4) . . . . ? C34 C23 N24 Ag1 4.2(7) . . . . ? N51 Ag1 N24 C25 -29.7(5) 2_645 . . . ? N1 Ag1 N24 C25 117.2(4) . . . . ? N8 Ag1 N24 C25 -149.9(4) . . . . ? N51 Ag1 N24 C23 148.5(4) 2_645 . . . ? N1 Ag1 N24 C23 -64.6(5) . . . . ? N8 Ag1 N24 C23 28.3(5) . . . . ? C23 N24 C25 C26 1.8(9) . . . . ? Ag1 N24 C25 C26 -179.9(5) . . . . ? C22 N21 C26 C25 0.3(9) . . . . ? Ag2 N21 C26 C25 -170.7(4) . . . . ? N24 C25 C26 N21 -2.4(10) . . . . ? N21 C22 C27 N28 6.0(8) . . . . ? C23 C22 C27 N28 -174.3(5) . . . . ? N21 C22 C27 C32 -175.0(5) . . . . ? C23 C22 C27 C32 4.8(8) . . . . ? C32 C27 N28 C29 0.3(8) . . . . ? C22 C27 N28 C29 179.3(5) . . . . ? C32 C27 N28 Ag2 177.8(4) . . . . ? C22 C27 N28 Ag2 -3.2(6) . . . . ? N11 Ag2 N28 C29 43.0(6) 4_565 . . . ? N21 Ag2 N28 C29 177.4(6) . . . . ? N44 Ag2 N28 C29 -100.3(5) . . . . ? N11 Ag2 N28 C27 -134.2(4) 4_565 . . . ? N21 Ag2 N28 C27 0.3(4) . . . . ? N44 Ag2 N28 C27 82.6(4) . . . . ? C27 N28 C29 C30 1.9(10) . . . . ? Ag2 N28 C29 C30 -175.3(5) . . . . ? N28 C29 C30 N31 -1.7(12) . . . . ? C29 C30 N31 C32 -0.8(10) . . . . ? C29 C30 N31 Ag3 179.3(6) . . . 2_655 ? C30 N31 C32 C27 2.9(9) . . . . ? Ag3 N31 C32 C27 -177.2(4) 2_655 . . . ? C30 N31 C32 C33 -176.7(6) . . . . ? Ag3 N31 C32 C33 3.2(8) 2_655 . . . ? N28 C27 C32 N31 -2.8(8) . . . . ? C22 C27 C32 N31 178.2(5) . . . . ? N28 C27 C32 C33 176.8(5) . . . . ? C22 C27 C32 C33 -2.2(8) . . . . ? N31 C32 C33 C34 178.8(5) . . . . ? C27 C32 C33 C34 -0.9(8) . . . . ? C32 C33 C34 C23 1.3(9) . . . . ? N24 C23 C34 C33 179.8(5) . . . . ? C22 C23 C34 C33 1.4(8) . . . . ? N4 Ag3 N41 C46 -86.7(5) 1_455 . . . ? N31 Ag3 N41 C46 85.5(5) 2_645 . . . ? N48 Ag3 N41 C46 -179.4(5) . . . . ? N4 Ag3 N41 C42 94.3(5) 1_455 . . . ? N31 Ag3 N41 C42 -93.4(4) 2_645 . . . ? N48 Ag3 N41 C42 1.6(4) . . . . ? C46 N41 C42 C43 0.4(9) . . . . ? Ag3 N41 C42 C43 179.5(4) . . . . ? C46 N41 C42 C47 178.5(6) . . . . ? Ag3 N41 C42 C47 -2.5(7) . . . . ? N41 C42 C43 N44 0.8(9) . . . . ? C47 C42 C43 N44 -177.2(5) . . . . ? N41 C42 C43 C54 179.5(5) . . . . ? C47 C42 C43 C54 1.5(8) . . . . ? C54 C43 N44 C45 -179.8(6) . . . . ? C42 C43 N44 C45 -1.1(8) . . . . ? C54 C43 N44 Ag2 8.6(8) . . . . ? C42 C43 N44 Ag2 -172.7(4) . . . . ? N11 Ag2 N44 C45 74.8(5) 4_565 . . . ? N28 Ag2 N44 C45 -129.6(5) . . . . ? N21 Ag2 N44 C45 -58.6(5) . . . . ? N11 Ag2 N44 C43 -113.6(5) 4_565 . . . ? N28 Ag2 N44 C43 42.1(5) . . . . ? N21 Ag2 N44 C43 113.0(5) . . . . ? C43 N44 C45 C46 0.2(9) . . . . ? Ag2 N44 C45 C46 172.4(5) . . . . ? C42 N41 C46 C45 -1.4(9) . . . . ? Ag3 N41 C46 C45 179.7(5) . . . . ? N44 C45 C46 N41 1.1(10) . . . . ? N41 C42 C47 N48 1.9(8) . . . . ? C43 C42 C47 N48 180.0(5) . . . . ? N41 C42 C47 C52 -175.8(5) . . . . ? C43 C42 C47 C52 2.2(8) . . . . ? C52 C47 N48 C49 1.5(9) . . . . ? C42 C47 N48 C49 -176.2(6) . . . . ? C52 C47 N48 Ag3 177.3(4) . . . . ? C42 C47 N48 Ag3 -0.4(7) . . . . ? N4 Ag3 N48 C49 42.4(6) 1_455 . . . ? N31 Ag3 N48 C49 -85.4(6) 2_645 . . . ? N41 Ag3 N48 C49 174.4(6) . . . . ? N4 Ag3 N48 C47 -132.6(4) 1_455 . . . ? N31 Ag3 N48 C47 99.7(4) 2_645 . . . ? N41 Ag3 N48 C47 -0.6(4) . . . . ? C47 N48 C49 C50 1.6(10) . . . . ? Ag3 N48 C49 C50 -173.3(5) . . . . ? N48 C49 C50 N51 -3.2(11) . . . . ? C49 C50 N51 C52 1.4(10) . . . . ? C49 C50 N51 Ag1 164.6(5) . . . 2_655 ? C50 N51 C52 C47 1.6(9) . . . . ? Ag1 N51 C52 C47 -160.8(4) 2_655 . . . ? C50 N51 C52 C53 -178.8(6) . . . . ? Ag1 N51 C52 C53 18.8(7) 2_655 . . . ? N48 C47 C52 N51 -3.2(9) . . . . ? C42 C47 C52 N51 174.5(5) . . . . ? N48 C47 C52 C53 177.2(5) . . . . ? C42 C47 C52 C53 -5.1(8) . . . . ? N51 C52 C53 C54 -175.2(6) . . . . ? C47 C52 C53 C54 4.5(9) . . . . ? C52 C53 C54 C43 -0.6(9) . . . . ? N44 C43 C54 C53 176.4(6) . . . . ? C42 C43 C54 C53 -2.3(9) . . . . ? F11 B3 F9 F10 -179(3) . . . 3_765 ? F10 B3 F9 F10 60(3) . . . 3_765 ? F12 B3 F9 F10 -59(3) . . . 3_765 ? F11 B3 F10 F9 -151.0(17) . . . 3_765 ? F12 B3 F10 F9 89.5(17) . . . 3_765 ? F9 B3 F10 F9 -28.7(19) . . . 3_765 ? F15 B4 F13 F16 114.3(16) . . . 3_755 ? F14 B4 F13 F16 -126.2(16) . . . 3_755 ? F16 B4 F13 F16 -4.8(18) . . . 3_755 ? F13 B4 F16 F13 8(3) . . . 3_755 ? F15 B4 F16 F13 -114(3) . . . 3_755 ? F14 B4 F16 F13 128(3) . . . 3_755 ? F16 B4 F16 F13 6(2) 3_755 . . 3_755 ? F13 B4 F16 B4 2.1(8) . . . 3_755 ? F15 B4 F16 B4 -120.2(9) . . . 3_755 ? F14 B4 F16 B4 121.9(10) . . . 3_755 ? F16 B4 F16 B4 0.0 3_755 . . 3_755 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.819 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.152 #===END data_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Ag(2,2'-bipyrazine)(acetonitrile)]tetrafluoroborate' ; _chemical_name_common AgbpzBF4 _chemical_melting_point ? _chemical_formula_moiety [Ag(C8H6N4)(CH3CN)]BF4 _chemical_formula_sum 'C10 H9 Ag B F4 N5' _chemical_formula_weight 393.90 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 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 7.326(3) _cell_length_b 18.423(6) _cell_length_c 10.218(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.35(4) _cell_angle_gamma 90.00 _cell_volume 1356.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description trapezoid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_T_max 0.8873 _exptl_absorpt_process_details ? _exptl_special_details ; '[Ag(2,2'-bipyrazine)(acetonitrile)]tetrafluoroborate' ; _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 'Stoe Stadi-4' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/- 4.3%' _diffrn_reflns_number 2384 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2384 _reflns_number_gt 1794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0155P)^2^+7.6397P] 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 2384 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.23180(7) 0.88430(3) 0.90371(6) 0.02231(17) Uani 1 1 d . . . N1 N 0.3941(8) 0.7881(3) 1.0329(6) 0.0210(14) Uani 1 1 d . . . C2 C 0.5755(9) 0.7985(4) 1.0821(7) 0.0187(16) Uani 1 1 d . . . C3 C 0.6675(10) 0.7552(4) 1.1844(7) 0.0213(17) Uani 1 1 d . . . H3A H 0.7948 0.7643 1.2186 0.026 Uiso 1 1 calc R . . N4 N 0.5807(8) 0.7008(3) 1.2363(6) 0.0240(15) Uani 1 1 d . . . C5 C 0.3998(10) 0.6910(4) 1.1841(7) 0.0239(17) Uani 1 1 d . . . H5A H 0.3339 0.6528 1.2173 0.029 Uiso 1 1 calc R . . C6 C 0.3082(10) 0.7344(4) 1.0850(7) 0.0226(17) Uani 1 1 d . . . H6A H 0.1801 0.7261 1.0524 0.027 Uiso 1 1 calc R . . C7 C 0.6694(9) 0.8573(4) 1.0199(7) 0.0191(16) Uani 1 1 d . . . N8 N 0.5598(8) 0.9078(3) 0.9521(6) 0.0204(14) Uani 1 1 d . . . C9 C 0.6414(10) 0.9594(4) 0.8909(8) 0.0241(18) Uani 1 1 d . . . H9A H 0.5683 0.9970 0.8442 0.029 Uiso 1 1 calc R . . C10 C 0.8321(9) 0.9587(4) 0.8948(7) 0.0193(16) Uani 1 1 d . . . H10A H 0.8857 0.9953 0.8483 0.023 Uiso 1 1 calc R . . N11 N 0.9423(8) 0.9085(3) 0.9615(6) 0.0200(14) Uani 1 1 d . . . C12 C 0.8601(9) 0.8587(4) 1.0255(7) 0.0202(16) Uani 1 1 d . . . H12A H 0.9345 0.8230 1.0767 0.024 Uiso 1 1 calc R . . N1S N 0.2003(9) 0.9936(4) 0.7618(8) 0.0376(18) Uani 1 1 d . . . C1S C 0.2197(11) 1.0196(5) 0.6660(9) 0.035(2) Uani 1 1 d . . . C2S C 0.2511(14) 1.0523(6) 0.5428(10) 0.065(3) Uani 1 1 d . . . H2S1 H 0.3705 1.0778 0.5584 0.098 Uiso 1 1 calc R . . H2S2 H 0.1514 1.0869 0.5110 0.098 Uiso 1 1 calc R . . H2SS H 0.2525 1.0144 0.4758 0.098 Uiso 1 1 calc R . . B1 B 0.2378(13) 0.8494(6) 0.3711(9) 0.036(2) Uani 1 1 d . . . F1 F 0.3876(8) 0.8121(3) 0.4368(7) 0.073(2) Uani 1 1 d . . . F2 F 0.1121(8) 0.8003(4) 0.3075(6) 0.077(2) Uani 1 1 d . . . F3 F 0.2892(10) 0.8950(4) 0.2821(7) 0.086(2) Uani 1 1 d . . . F4 F 0.1581(12) 0.8846(5) 0.4624(8) 0.113(3) 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 Ag1 0.0107(2) 0.0225(3) 0.0322(3) 0.0021(3) -0.00018(19) 0.0012(3) N1 0.014(3) 0.019(3) 0.029(4) 0.000(3) 0.001(3) 0.001(3) C2 0.016(3) 0.019(4) 0.021(4) -0.006(3) 0.001(3) 0.000(3) C3 0.019(4) 0.024(4) 0.021(4) 0.005(3) 0.002(3) -0.001(3) N4 0.018(3) 0.026(4) 0.025(4) 0.004(3) -0.004(3) -0.001(3) C5 0.022(4) 0.023(4) 0.025(4) 0.001(3) 0.001(3) -0.006(3) C6 0.024(4) 0.021(4) 0.023(4) -0.001(3) 0.003(3) -0.003(3) C7 0.016(3) 0.017(4) 0.024(4) -0.006(3) 0.006(3) 0.005(3) N8 0.018(3) 0.017(3) 0.026(3) 0.001(3) 0.005(3) 0.000(2) C9 0.026(4) 0.019(4) 0.029(4) 0.000(3) 0.007(3) 0.007(3) C10 0.015(4) 0.020(4) 0.024(4) -0.006(3) 0.004(3) -0.004(3) N11 0.016(3) 0.020(3) 0.023(3) -0.005(3) 0.000(2) 0.002(2) C12 0.016(3) 0.017(4) 0.026(4) 0.004(3) 0.000(3) 0.009(3) N1S 0.023(4) 0.044(5) 0.044(5) 0.017(4) 0.003(3) 0.003(3) C1S 0.021(4) 0.034(5) 0.046(6) 0.009(4) 0.000(4) -0.004(4) C2S 0.049(6) 0.076(8) 0.067(7) 0.035(6) -0.001(6) -0.015(6) B1 0.030(5) 0.049(6) 0.030(6) 0.005(5) 0.003(5) 0.006(5) F1 0.036(3) 0.068(4) 0.104(5) 0.020(4) -0.017(3) 0.006(3) F2 0.045(3) 0.112(6) 0.067(4) 0.005(4) -0.011(3) -0.030(4) F3 0.099(5) 0.070(5) 0.091(5) 0.044(4) 0.026(4) -0.002(4) F4 0.147(7) 0.106(6) 0.098(6) -0.022(5) 0.053(5) 0.047(6) _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 N11 2.345(6) 1_455 y Ag1 N1 2.394(6) . y Ag1 N8 2.404(6) . y Ag1 N4 2.435(6) 4_575 y Ag1 N1S 2.467(7) . y N1 C6 1.334(9) . ? N1 C2 1.347(9) . ? C2 C3 1.388(10) . ? C2 C7 1.487(10) . ? C3 N4 1.346(9) . ? N4 C5 1.349(9) . ? N4 Ag1 2.435(6) 4_676 ? C5 C6 1.368(10) . ? C7 N8 1.338(9) . ? C7 C12 1.388(9) . ? N8 C9 1.336(9) . ? C9 C10 1.390(9) . ? C10 N11 1.331(9) . ? N11 C12 1.331(9) . ? N11 Ag1 2.345(6) 1_655 ? N1S C1S 1.122(10) . ? C1S C2S 1.451(13) . ? B1 F3 1.340(11) . ? B1 F4 1.352(11) . ? B1 F1 1.366(11) . ? B1 F2 1.369(12) . ? 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 N11 Ag1 N1 112.6(2) 1_455 . y N11 Ag1 N8 146.1(2) 1_455 . y N1 Ag1 N8 69.0(2) . . y N11 Ag1 N4 89.0(2) 1_455 4_575 y N1 Ag1 N4 91.6(2) . 4_575 y N8 Ag1 N4 124.9(2) . 4_575 y N11 Ag1 N1S 90.0(2) 1_455 . y N1 Ag1 N1S 155.9(2) . . y N8 Ag1 N1S 87.6(2) . . y N4 Ag1 N1S 97.5(2) 4_575 . y C6 N1 C2 117.4(6) . . ? C6 N1 Ag1 123.1(5) . . ? C2 N1 Ag1 117.4(5) . . ? N1 C2 C3 120.9(7) . . ? N1 C2 C7 116.4(6) . . ? C3 C2 C7 122.7(6) . . ? N4 C3 C2 121.6(7) . . ? C3 N4 C5 116.4(6) . . ? C3 N4 Ag1 124.7(5) . 4_676 ? C5 N4 Ag1 118.8(5) . 4_676 ? N4 C5 C6 122.1(7) . . ? N1 C6 C5 121.7(7) . . ? N8 C7 C12 120.9(7) . . ? N8 C7 C2 116.6(6) . . ? C12 C7 C2 122.4(6) . . ? C9 N8 C7 117.4(6) . . ? C9 N8 Ag1 123.1(5) . . ? C7 N8 Ag1 117.8(5) . . ? N8 C9 C10 120.7(7) . . ? N11 C10 C9 122.3(7) . . ? C10 N11 C12 116.3(6) . . ? C10 N11 Ag1 119.7(5) . 1_655 ? C12 N11 Ag1 120.1(4) . 1_655 ? N11 C12 C7 122.2(6) . . ? C1S N1S Ag1 148.1(7) . . ? N1S C1S C2S 178.1(10) . . ? F3 B1 F4 112.2(9) . . ? F3 B1 F1 110.5(8) . . ? F4 B1 F1 108.1(8) . . ? F3 B1 F2 109.8(8) . . ? F4 B1 F2 107.9(9) . . ? F1 B1 F2 108.2(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.739 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.144 #===END data_compund6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Bis(2,2'-bipyrazine)Bis Silver(I)benzonitrile tetrafluoroborate' ; _chemical_name_common '[Ag(bpyz)2Ag(PhCN)](BF4)2' _chemical_melting_point ? _chemical_formula_moiety '[Ag(C8H6N4)2Ag(C6H5CN)](BF4)2' _chemical_formula_sum 'C46 H34 Ag4 B4 F16 N18' _chemical_formula_weight 1617.63 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)/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 11.410(3) _cell_length_b 14.379(3) _cell_length_c 16.153(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.497(4) _cell_angle_gamma 90.00 _cell_volume 2649.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6783 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.6 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 0.684 _exptl_absorpt_process_details ? _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 'SMART CCD' _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 6338 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.82 _reflns_number_total 6338 _reflns_number_gt 5219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0466P)^2^+1.9029P] 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 6338 _refine_ls_number_parameters 436 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.266 _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 Ag1 Ag 0.74608(2) 0.862148(18) 0.229848(17) 0.03268(9) Uani 1 1 d U . . Ag2 Ag 0.26391(2) 0.768738(18) 0.503192(17) 0.03324(9) Uani 1 1 d U . . N1 N 0.3667(2) 0.62858(18) 0.46643(17) 0.0245(5) Uani 1 1 d U . . C2 C 0.4404(3) 0.6401(2) 0.40380(19) 0.0222(6) Uani 1 1 d U . . C3 C 0.4801(3) 0.5638(2) 0.3591(2) 0.0279(7) Uani 1 1 d U . . H3A H 0.5318 0.5741 0.3149 0.033 Uiso 1 1 calc R . . N4 N 0.4480(3) 0.47693(19) 0.37616(19) 0.0314(6) Uani 1 1 d U . . C5 C 0.3764(3) 0.4661(2) 0.4394(2) 0.0289(7) Uani 1 1 d U . . H5A H 0.3524 0.4051 0.4541 0.035 Uiso 1 1 calc R . . C6 C 0.3359(3) 0.5409(2) 0.4843(2) 0.0287(7) Uani 1 1 d U . . H6A H 0.2851 0.5300 0.5290 0.034 Uiso 1 1 calc R . . C7 C 0.4747(3) 0.7366(2) 0.38286(18) 0.0210(6) Uani 1 1 d U . . N8 N 0.4038(2) 0.80564(18) 0.40705(16) 0.0235(5) Uani 1 1 d U . . C9 C 0.4337(3) 0.8920(2) 0.3863(2) 0.0270(7) Uani 1 1 d U . . H9A H 0.3865 0.9424 0.4036 0.032 Uiso 1 1 calc R . . C10 C 0.5317(3) 0.9102(2) 0.3402(2) 0.0262(6) Uani 1 1 d U . . H10A H 0.5488 0.9726 0.3253 0.031 Uiso 1 1 calc R . . N11 N 0.6026(2) 0.84192(18) 0.31606(17) 0.0250(5) Uani 1 1 d U . . C12 C 0.5754(3) 0.7549(2) 0.3385(2) 0.0243(6) Uani 1 1 d U . . H12A H 0.6254 0.7050 0.3241 0.029 Uiso 1 1 calc R . . N21 N 0.1714(2) 0.89889(19) 0.56193(17) 0.0257(5) Uani 1 1 d U . . C22 C 0.0607(3) 0.8862(2) 0.5859(2) 0.0250(6) Uani 1 1 d U . . C23 C -0.0090(3) 0.9617(2) 0.6063(2) 0.0296(7) Uani 1 1 d U . . H23A H -0.0868 0.9504 0.6232 0.036 Uiso 1 1 calc R . . N24 N 0.0291(3) 1.0494(2) 0.60308(19) 0.0329(6) Uani 1 1 d U . . C25 C 0.1398(3) 1.0610(2) 0.5798(2) 0.0311(7) Uani 1 1 d U . . H25A H 0.1709 1.1222 0.5773 0.037 Uiso 1 1 calc R . . C26 C 0.2109(3) 0.9864(2) 0.5591(2) 0.0290(7) Uani 1 1 d U . . H26A H 0.2889 0.9977 0.5427 0.035 Uiso 1 1 calc R . . C27 C 0.0181(3) 0.7886(2) 0.5904(2) 0.0250(6) Uani 1 1 d U . . N28 N 0.0799(2) 0.72307(19) 0.55133(18) 0.0288(6) Uani 1 1 d U . . C29 C 0.0444(3) 0.6355(2) 0.5590(2) 0.0325(8) Uani 1 1 d U . . H29A H 0.0860 0.5879 0.5316 0.039 Uiso 1 1 calc R . . C30 C -0.0511(3) 0.6114(2) 0.6056(2) 0.0316(7) Uani 1 1 d U . . H30A H -0.0728 0.5478 0.6101 0.038 Uiso 1 1 calc R . . N31 N -0.1132(2) 0.67627(19) 0.64442(18) 0.0276(6) Uani 1 1 d U . . C32 C -0.0797(3) 0.7652(2) 0.6364(2) 0.0272(7) Uani 1 1 d U . . H32A H -0.1231 0.8130 0.6623 0.033 Uiso 1 1 calc R . . N1S N 0.7960(3) 1.0273(2) 0.2240(2) 0.0370(7) Uani 1 1 d U . . C1S C 0.7726(3) 1.2036(2) 0.2501(2) 0.0256(6) Uani 1 1 d U . . C2S C 0.6760(3) 1.2299(2) 0.2962(2) 0.0280(7) Uani 1 1 d U . . H2SA H 0.6229 1.1845 0.3157 0.034 Uiso 1 1 calc R . . C3S C 0.6591(3) 1.3233(3) 0.3131(2) 0.0326(7) Uani 1 1 d U . . H3SA H 0.5937 1.3425 0.3441 0.039 Uiso 1 1 calc R . . C4S C 0.7374(3) 1.3888(3) 0.2848(2) 0.0365(8) Uani 1 1 d U . . H4SA H 0.7254 1.4528 0.2966 0.044 Uiso 1 1 calc R . . C5S C 0.8335(3) 1.3620(2) 0.2393(2) 0.0361(8) Uani 1 1 d U . . H5SA H 0.8870 1.4077 0.2208 0.043 Uiso 1 1 calc R . . C6S C 0.8520(3) 1.2689(2) 0.2208(2) 0.0304(7) Uani 1 1 d U . . H6SA H 0.9168 1.2501 0.1890 0.037 Uiso 1 1 calc R . . C7S C 0.7883(3) 1.1057(2) 0.2341(2) 0.0283(7) Uani 1 1 d U . . B B 0.6023(3) 0.8474(2) 0.5989(2) 0.0380(9) Uani 1 1 d DU . . F1 F 0.6095(6) 0.8767(4) 0.6824(3) 0.099(2) Uani 0.65 1 d PDU A 1 F2 F 0.5936(5) 0.7557(3) 0.6007(5) 0.088(2) Uani 0.65 1 d PDU A 1 F3 F 0.6915(5) 0.8810(4) 0.5612(5) 0.109(3) Uani 0.65 1 d PDU A 1 F1A F 0.6941(6) 0.9087(6) 0.6057(9) 0.092(5) Uani 0.35 1 d PDU A 2 F2A F 0.6043(8) 0.7878(9) 0.6608(7) 0.120(6) Uani 0.35 1 d PDU A 2 F3A F 0.6321(9) 0.7945(10) 0.5264(6) 0.145(6) Uani 0.35 1 d PDU A 2 F4 F 0.4986(2) 0.88835(18) 0.57712(18) 0.0593(7) Uani 1 1 d DU A . B' B 0.8680(4) 0.6305(3) 0.3564(3) 0.0403(10) Uani 1 1 d DU . . F1' F 0.8556(5) 0.7216(4) 0.3294(4) 0.0354(19) Uiso 0.40 1 d PDU B 1 F2' F 0.7774(7) 0.5978(5) 0.3982(5) 0.0472(19) Uiso 0.40 1 d PDU B 1 F3' F 0.8725(6) 0.5814(4) 0.2742(4) 0.0401(16) Uiso 0.40 1 d PDU B 1 F4' F 0.9785(6) 0.6145(5) 0.3927(5) 0.0463(17) Uiso 0.40 1 d PDU B 1 F1A' F 0.8077(8) 0.6137(7) 0.2847(5) 0.071(2) Uiso 0.35 1 d PDU B 2 F3A' F 0.8103(9) 0.5950(7) 0.4230(6) 0.072(3) Uiso 0.35 1 d PDU B 2 F2A' F 0.8699(7) 0.7266(4) 0.3542(7) 0.0291(16) Uiso 0.35 1 d PDU B 2 F4A' F 0.9807(7) 0.6003(8) 0.3637(7) 0.073(3) Uiso 0.35 1 d PDU B 2 F1B' F 0.7539(7) 0.5940(6) 0.3693(6) 0.036(2) Uiso 0.25 1 d PDU B 3 F2B' F 0.9109(13) 0.5861(9) 0.2856(7) 0.065(4) Uiso 0.25 1 d PDU B 3 F3B' F 0.8833(14) 0.7210(7) 0.3866(10) 0.077(5) Uiso 0.25 1 d PDU B 3 F4B' F 0.9381(11) 0.5801(9) 0.4102(7) 0.068(3) Uiso 0.25 1 d PDU B 3 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 0.02905(15) 0.03039(14) 0.03948(16) 0.00258(11) 0.01773(11) 0.00010(10) Ag2 0.02931(15) 0.03047(14) 0.04094(16) -0.00490(11) 0.01988(11) - 0.00119(10) N1 0.0231(13) 0.0234(12) 0.0274(13) 0.0018(10) 0.0061(10) -0.0032(10) C2 0.0204(15) 0.0219(14) 0.0244(15) 0.0007(12) 0.0029(12) -0.0004(11) C3 0.0280(17) 0.0242(15) 0.0319(17) -0.0017(13) 0.0065(13) 0.0028(12) N4 0.0352(16) 0.0217(13) 0.0373(16) -0.0029(12) 0.0019(12) 0.0013(11) C5 0.0284(17) 0.0233(15) 0.0349(18) 0.0039(13) -0.0026(13) -0.0028(12) C6 0.0266(16) 0.0273(15) 0.0322(17) 0.0052(13) 0.0035(13) -0.0029(13) C7 0.0216(15) 0.0206(13) 0.0209(14) -0.0010(11) 0.0040(11) -0.0006(11) N8 0.0223(13) 0.0218(12) 0.0267(13) -0.0023(10) 0.0065(10) -0.0004(10) C9 0.0289(17) 0.0216(14) 0.0310(17) -0.0039(13) 0.0084(13) 0.0011(12) C10 0.0276(16) 0.0206(14) 0.0307(16) 0.0002(13) 0.0074(13) -0.0026(12) N11 0.0223(13) 0.0248(13) 0.0281(14) 0.0004(11) 0.0075(11) -0.0006(10) C12 0.0217(15) 0.0234(14) 0.0281(16) 0.0000(12) 0.0072(12) 0.0019(12) N21 0.0231(13) 0.0280(13) 0.0260(13) 0.0007(11) 0.0050(10) -0.0016(10) C22 0.0244(15) 0.0260(15) 0.0248(15) -0.0002(12) 0.0057(12) -0.0005(12) C23 0.0279(17) 0.0285(16) 0.0328(17) -0.0002(14) 0.0084(13) 0.0007(13) N24 0.0354(16) 0.0267(14) 0.0369(16) -0.0009(12) 0.0074(13) 0.0002(12) C25 0.0353(18) 0.0268(16) 0.0312(17) 0.0002(14) 0.0016(14) -0.0053(13) C26 0.0261(16) 0.0326(17) 0.0287(16) 0.0014(14) 0.0049(13) -0.0056(13) C27 0.0224(15) 0.0274(15) 0.0255(15) -0.0019(12) 0.0047(12) 0.0003(12) N28 0.0254(14) 0.0291(14) 0.0323(15) -0.0058(11) 0.0100(11) -0.0019(11) C29 0.0292(18) 0.0291(16) 0.0398(19) -0.0099(14) 0.0130(15) -0.0003(13) C30 0.0298(17) 0.0246(15) 0.0411(19) -0.0057(14) 0.0123(14) -0.0032(13) N31 0.0226(13) 0.0256(13) 0.0353(15) -0.0029(11) 0.0111(11) -0.0019(10) C32 0.0240(16) 0.0249(15) 0.0331(17) -0.0019(13) 0.0091(13) 0.0018(12) N1S 0.0379(17) 0.0291(15) 0.0443(18) -0.0027(13) 0.0057(14) -0.0017(13) C1S 0.0256(16) 0.0246(14) 0.0267(16) -0.0011(13) 0.0013(12) 0.0009(12) C2S 0.0241(16) 0.0308(16) 0.0290(16) 0.0017(13) 0.0005(13) -0.0023(13) C3S 0.0302(18) 0.0361(18) 0.0316(18) -0.0052(15) 0.0037(14) 0.0084(14) C4S 0.039(2) 0.0268(16) 0.044(2) -0.0045(15) -0.0014(16) 0.0064(14) C5S 0.0339(19) 0.0284(17) 0.046(2) 0.0059(15) 0.0029(16) -0.0051(14) C6S 0.0253(17) 0.0314(17) 0.0349(18) 0.0034(14) 0.0059(14) 0.0021(13) C7S 0.0257(16) 0.0293(16) 0.0299(17) 0.0002(14) 0.0027(13) 0.0004(13) B 0.043(2) 0.0294(19) 0.042(2) 0.0101(17) 0.0043(18) 0.0000(17) F1 0.148(6) 0.106(4) 0.041(3) 0.009(3) -0.023(3) -0.020(4) F2 0.097(4) 0.0207(18) 0.150(6) 0.012(3) 0.058(5) 0.013(2) F3 0.090(4) 0.075(4) 0.168(7) 0.076(5) 0.103(5) 0.036(3) F1A 0.032(4) 0.036(5) 0.209(16) 0.009(6) -0.002(7) 0.003(3) F2A 0.059(6) 0.162(14) 0.142(10) 0.134(11) 0.027(8) 0.024(8) F3A 0.113(10) 0.225(16) 0.094(7) -0.103(9) -0.049(7) 0.094(10) F4 0.0527(16) 0.0475(14) 0.0775(19) 0.0062(13) -0.0039(13) 0.0062(12) B' 0.037(2) 0.034(2) 0.050(3) 0.0121(19) -0.0023(19) -0.0034(17) _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 N11 2.196(3) . y Ag1 N31 2.214(3) 4_675 y Ag1 N1S 2.444(3) . y Ag2 N8 2.318(3) . y Ag2 N28 2.351(3) . y Ag2 N21 2.360(3) . y Ag2 N1 2.414(3) . y N1 C6 1.342(4) . ? N1 C2 1.343(4) . ? C2 C3 1.395(4) . ? C2 C7 1.484(4) . ? C3 N4 1.332(4) . ? N4 C5 1.334(5) . ? C5 C6 1.384(5) . ? C7 N8 1.345(4) . ? C7 C12 1.394(4) . ? N8 C9 1.333(4) . ? C9 C10 1.384(4) . ? C10 N11 1.337(4) . ? N11 C12 1.342(4) . ? N21 C26 1.337(4) . ? N21 C22 1.343(4) . ? C22 C23 1.390(5) . ? C22 C27 1.487(4) . ? C23 N24 1.336(4) . ? N24 C25 1.337(5) . ? C25 C26 1.392(5) . ? C27 N28 1.345(4) . ? C27 C32 1.397(4) . ? N28 C29 1.329(4) . ? C29 C30 1.385(5) . ? C30 N31 1.337(4) . ? N31 C32 1.343(4) . ? N31 Ag1 2.214(3) 4_476 ? N1S C7S 1.143(4) . ? C1S C6S 1.395(5) . ? C1S C2S 1.399(5) . ? C1S C7S 1.444(4) . ? C2S C3S 1.386(5) . ? C3S C4S 1.384(5) . ? C4S C5S 1.391(5) . ? C5S C6S 1.390(5) . ? B F3 1.294(5) . ? B F2A 1.316(6) . ? B F2 1.323(5) . ? B F4 1.360(4) . ? B F1A 1.370(7) . ? B F1 1.413(5) . ? B F3A 1.445(7) . ? B' F2' 1.336(8) . ? B' F1A' 1.353(7) . ? B' F4A' 1.359(8) . ? B' F4B' 1.373(8) . ? B' F3A' 1.375(8) . ? B' F2A' 1.382(6) . ? B' F1' 1.387(7) . ? B' F4' 1.395(8) . ? B' F3B' 1.398(8) . ? B' F2B' 1.408(8) . ? B' F1B' 1.424(7) . ? B' F3' 1.506(8) . ? 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 N11 Ag1 N31 157.94(10) . 4_675 y N11 Ag1 N1S 109.35(10) . . y N31 Ag1 N1S 92.58(10) 4_675 . y N8 Ag2 N28 157.24(10) . . y N8 Ag2 N21 114.27(9) . . y N28 Ag2 N21 71.08(9) . . y N8 Ag2 N1 71.26(9) . . y N28 Ag2 N1 106.96(9) . . y N21 Ag2 N1 170.53(9) . . y C6 N1 C2 116.8(3) . . ? C6 N1 Ag2 126.9(2) . . ? C2 N1 Ag2 113.63(19) . . ? N1 C2 C3 120.7(3) . . ? N1 C2 C7 117.4(3) . . ? C3 C2 C7 121.8(3) . . ? N4 C3 C2 122.4(3) . . ? C3 N4 C5 116.4(3) . . ? N4 C5 C6 122.0(3) . . ? N1 C6 C5 121.7(3) . . ? N8 C7 C12 121.3(3) . . ? N8 C7 C2 117.4(3) . . ? C12 C7 C2 121.3(3) . . ? C9 N8 C7 117.0(3) . . ? C9 N8 Ag2 124.5(2) . . ? C7 N8 Ag2 117.1(2) . . ? N8 C9 C10 121.8(3) . . ? N11 C10 C9 121.4(3) . . ? C10 N11 C12 117.4(3) . . ? C10 N11 Ag1 123.7(2) . . ? C12 N11 Ag1 118.5(2) . . ? N11 C12 C7 120.9(3) . . ? C26 N21 C22 117.3(3) . . ? C26 N21 Ag2 125.3(2) . . ? C22 N21 Ag2 116.2(2) . . ? N21 C22 C23 120.7(3) . . ? N21 C22 C27 117.0(3) . . ? C23 C22 C27 122.4(3) . . ? N24 C23 C22 122.7(3) . . ? C23 N24 C25 116.1(3) . . ? N24 C25 C26 122.1(3) . . ? N21 C26 C25 121.2(3) . . ? N28 C27 C32 121.1(3) . . ? N28 C27 C22 117.5(3) . . ? C32 C27 C22 121.3(3) . . ? C29 N28 C27 117.1(3) . . ? C29 N28 Ag2 124.9(2) . . ? C27 N28 Ag2 116.3(2) . . ? N28 C29 C30 122.3(3) . . ? N31 C30 C29 120.9(3) . . ? C30 N31 C32 117.6(3) . . ? C30 N31 Ag1 121.3(2) . 4_476 ? C32 N31 Ag1 120.8(2) . 4_476 ? N31 C32 C27 121.0(3) . . ? C7S N1S Ag1 159.1(3) . . ? C6S C1S C2S 121.8(3) . . ? C6S C1S C7S 120.7(3) . . ? C2S C1S C7S 117.5(3) . . ? C3S C2S C1S 118.9(3) . . ? C4S C3S C2S 120.0(3) . . ? C3S C4S C5S 120.7(3) . . ? C6S C5S C4S 120.5(3) . . ? C5S C6S C1S 118.1(3) . . ? N1S C7S C1S 176.5(4) . . ? F3 B F2A 127.1(6) . . ? F3 B F2 116.3(4) . . ? F2A B F2 48.3(6) . . ? F3 B F4 114.0(4) . . ? F2A B F4 118.5(5) . . ? F2 B F4 111.8(4) . . ? F3 B F1A 35.8(6) . . ? F2A B F1A 111.1(6) . . ? F2 B F1A 134.2(6) . . ? F4 B F1A 113.6(4) . . ? F3 B F1 108.2(5) . . ? F2A B F1 58.0(7) . . ? F2 B F1 106.2(4) . . ? F4 B F1 98.5(4) . . ? F1A B F1 73.0(6) . . ? F3 B F3A 67.0(6) . . ? F2A B F3A 105.9(6) . . ? F2 B F3A 60.8(6) . . ? F4 B F3A 103.8(4) . . ? F1A B F3A 102.0(6) . . ? F1 B F3A 157.2(5) . . ? F2' B' F1A' 89.2(6) . . ? F2' B' F4A' 125.9(7) . . ? F1A' B' F4A' 118.4(8) . . ? F2' B' F4B' 86.5(7) . . ? F1A' B' F4B' 136.2(8) . . ? F4A' B' F4B' 40.8(7) . . ? F2' B' F3A' 23.0(5) . . ? F1A' B' F3A' 111.0(7) . . ? F4A' B' F3A' 106.5(7) . . ? F4B' B' F3A' 65.8(7) . . ? F2' B' F2A' 112.2(6) . . ? F1A' B' F2A' 99.5(7) . . ? F4A' B' F2A' 107.8(6) . . ? F4B' B' F2A' 122.3(8) . . ? F3A' B' F2A' 113.6(7) . . ? F2' B' F1' 114.7(5) . . ? F1A' B' F1' 81.6(5) . . ? F4A' B' F1' 114.7(6) . . ? F4B' B' F1' 138.7(7) . . ? F3A' B' F1' 123.4(6) . . ? F2A' B' F1' 18.1(4) . . ? F2' B' F4' 115.5(5) . . ? F1A' B' F4' 139.9(7) . . ? F4A' B' F4' 21.4(5) . . ? F4B' B' F4' 30.9(6) . . ? F3A' B' F4' 93.2(6) . . ? F2A' B' F4' 99.3(6) . . ? F1' B' F4' 111.8(5) . . ? F2' B' F3B' 104.0(8) . . ? F1A' B' F3B' 121.4(8) . . ? F4A' B' F3B' 99.1(9) . . ? F4B' B' F3B' 101.8(9) . . ? F3A' B' F3B' 97.5(9) . . ? F2A' B' F3B' 22.7(7) . . ? F1' B' F3B' 40.7(7) . . ? F4' B' F3B' 84.4(8) . . ? F2' B' F2B' 122.8(8) . . ? F1A' B' F2B' 53.4(7) . . ? F4A' B' F2B' 65.0(8) . . ? F4B' B' F2B' 93.8(9) . . ? F3A' B' F2B' 130.5(8) . . ? F2A' B' F2B' 115.3(8) . . ? F1' B' F2B' 102.0(7) . . ? F4' B' F2B' 86.5(7) . . ? F3B' B' F2B' 131.5(10) . . ? F2' B' F1B' 22.1(5) . . ? F1A' B' F1B' 67.2(6) . . ? F4A' B' F1B' 137.4(7) . . ? F4B' B' F1B' 103.4(8) . . ? F3A' B' F1B' 44.7(6) . . ? F2A' B' F1B' 112.8(6) . . ? F1' B' F1B' 107.9(6) . . ? F4' B' F1B' 134.1(6) . . ? F3B' B' F1B' 113.4(8) . . ? F2B' B' F1B' 106.9(8) . . ? F2' B' F3' 109.0(5) . . ? F1A' B' F3' 35.9(4) . . ? F4A' B' F3' 82.7(6) . . ? F4B' B' F3' 106.1(7) . . ? F3A' B' F3' 122.9(6) . . ? F2A' B' F3' 116.4(6) . . ? F1' B' F3' 99.9(4) . . ? F4' B' F3' 104.0(5) . . ? F3B' B' F3' 137.5(8) . . ? F2B' B' F3' 18.4(6) . . ? F1B' B' F3' 90.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Ag2 N1 C6 -167.9(3) . . . . ? N28 Ag2 N1 C6 -11.7(3) . . . . ? N21 Ag2 N1 C6 64.9(7) . . . . ? N8 Ag2 N1 C2 -7.4(2) . . . . ? N28 Ag2 N1 C2 148.7(2) . . . . ? N21 Ag2 N1 C2 -134.6(5) . . . . ? C6 N1 C2 C3 1.4(5) . . . . ? Ag2 N1 C2 C3 -161.1(2) . . . . ? C6 N1 C2 C7 179.6(3) . . . . ? Ag2 N1 C2 C7 17.1(4) . . . . ? N1 C2 C3 N4 -0.4(5) . . . . ? C7 C2 C3 N4 -178.6(3) . . . . ? C2 C3 N4 C5 -0.8(5) . . . . ? C3 N4 C5 C6 0.9(5) . . . . ? C2 N1 C6 C5 -1.3(5) . . . . ? Ag2 N1 C6 C5 158.6(2) . . . . ? N4 C5 C6 N1 0.1(5) . . . . ? N1 C2 C7 N8 -21.4(4) . . . . ? C3 C2 C7 N8 156.8(3) . . . . ? N1 C2 C7 C12 159.8(3) . . . . ? C3 C2 C7 C12 -22.0(5) . . . . ? C12 C7 N8 C9 0.5(5) . . . . ? C2 C7 N8 C9 -178.4(3) . . . . ? C12 C7 N8 Ag2 -167.2(2) . . . . ? C2 C7 N8 Ag2 13.9(4) . . . . ? N28 Ag2 N8 C9 100.3(3) . . . . ? N21 Ag2 N8 C9 1.3(3) . . . . ? N1 Ag2 N8 C9 -170.4(3) . . . . ? N28 Ag2 N8 C7 -93.1(3) . . . . ? N21 Ag2 N8 C7 167.9(2) . . . . ? N1 Ag2 N8 C7 -3.8(2) . . . . ? C7 N8 C9 C10 1.5(5) . . . . ? Ag2 N8 C9 C10 168.1(2) . . . . ? N8 C9 C10 N11 -1.7(5) . . . . ? C9 C10 N11 C12 -0.2(5) . . . . ? C9 C10 N11 Ag1 171.8(2) . . . . ? N31 Ag1 N11 C10 -167.6(3) 4_675 . . . ? N1S Ag1 N11 C10 19.0(3) . . . . ? N31 Ag1 N11 C12 4.4(4) 4_675 . . . ? N1S Ag1 N11 C12 -169.1(2) . . . . ? C10 N11 C12 C7 2.1(5) . . . . ? Ag1 N11 C12 C7 -170.3(2) . . . . ? N8 C7 C12 N11 -2.4(5) . . . . ? C2 C7 C12 N11 176.5(3) . . . . ? N8 Ag2 N21 C26 -16.4(3) . . . . ? N28 Ag2 N21 C26 -172.5(3) . . . . ? N1 Ag2 N21 C26 107.8(6) . . . . ? N8 Ag2 N21 C22 150.5(2) . . . . ? N28 Ag2 N21 C22 -5.7(2) . . . . ? N1 Ag2 N21 C22 -85.3(6) . . . . ? C26 N21 C22 C23 0.3(5) . . . . ? Ag2 N21 C22 C23 -167.7(2) . . . . ? C26 N21 C22 C27 -178.8(3) . . . . ? Ag2 N21 C22 C27 13.2(4) . . . . ? N21 C22 C23 N24 0.2(5) . . . . ? C27 C22 C23 N24 179.3(3) . . . . ? C22 C23 N24 C25 -0.7(5) . . . . ? C23 N24 C25 C26 0.7(5) . . . . ? C22 N21 C26 C25 -0.3(5) . . . . ? Ag2 N21 C26 C25 166.4(2) . . . . ? N24 C25 C26 N21 -0.2(5) . . . . ? N21 C22 C27 N28 -16.4(4) . . . . ? C23 C22 C27 N28 164.4(3) . . . . ? N21 C22 C27 C32 161.0(3) . . . . ? C23 C22 C27 C32 -18.1(5) . . . . ? C32 C27 N28 C29 -0.6(5) . . . . ? C22 C27 N28 C29 176.9(3) . . . . ? C32 C27 N28 Ag2 -166.5(3) . . . . ? C22 C27 N28 Ag2 11.0(4) . . . . ? N8 Ag2 N28 C29 84.3(4) . . . . ? N21 Ag2 N28 C29 -167.9(3) . . . . ? N1 Ag2 N28 C29 2.4(3) . . . . ? N8 Ag2 N28 C27 -111.0(3) . . . . ? N21 Ag2 N28 C27 -3.2(2) . . . . ? N1 Ag2 N28 C27 167.1(2) . . . . ? C27 N28 C29 C30 -0.7(5) . . . . ? Ag2 N28 C29 C30 163.9(3) . . . . ? N28 C29 C30 N31 0.9(6) . . . . ? C29 C30 N31 C32 0.1(5) . . . . ? C29 C30 N31 Ag1 -173.4(3) . . . 4_476 ? C30 N31 C32 C27 -1.3(5) . . . . ? Ag1 N31 C32 C27 172.2(2) 4_476 . . . ? N28 C27 C32 N31 1.6(5) . . . . ? C22 C27 C32 N31 -175.8(3) . . . . ? N11 Ag1 N1S C7S -11.1(9) . . . . ? N31 Ag1 N1S C7S 171.3(8) 4_675 . . . ? C6S C1S C2S C3S 0.0(5) . . . . ? C7S C1S C2S C3S 179.5(3) . . . . ? C1S C2S C3S C4S -0.4(5) . . . . ? C2S C3S C4S C5S 0.1(6) . . . . ? C3S C4S C5S C6S 0.6(6) . . . . ? C4S C5S C6S C1S -1.0(6) . . . . ? C2S C1S C6S C5S 0.7(5) . . . . ? C7S C1S C6S C5S -178.9(3) . . . . ? Ag1 N1S C7S C1S 7(7) . . . . ? C6S C1S C7S N1S 174(6) . . . . ? C2S C1S C7S N1S -5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.82 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.893 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.092 #===END data_compound7a _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Bis(pyrazino-2,3(f)-quinoxaline)Silver(I) Tetrafluoroborate' ; _chemical_name_common '[Ag(pyq)2]BF4' _chemical_melting_point ? _chemical_formula_moiety '[Ag(C10H6N4)2]BF4' _chemical_formula_sum 'C20 H12 Ag B F4 N8' _chemical_formula_weight 559.06 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 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 16.898(2) _cell_length_b 7.2786(6) _cell_length_c 17.146(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.751(2) _cell_angle_gamma 90.00 _cell_volume 1958.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7783 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.64 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4430 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 28.67 _reflns_number_total 2332 _reflns_number_gt 2229 _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^)+(0.0341P)^2^+0.8919P] 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 2332 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 -0.52282(2) 0.2500 0.03050(7) Uani 1 2 d S . . N1 N -0.35494(8) -0.43340(18) 0.31139(7) 0.0227(2) Uani 1 1 d . . . C2 C -0.31622(9) -0.47128(17) 0.39407(9) 0.0184(3) Uani 1 1 d . . . C3 C -0.22980(8) -0.42865(19) 0.43860(9) 0.0209(3) Uani 1 1 d . . . N4 N -0.18145(8) -0.35273(18) 0.39913(8) 0.0280(3) Uani 1 1 d . . . C5 C -0.22044(10) -0.3181(2) 0.31848(10) 0.0319(3) Uani 1 1 d . . . H5A H -0.1884 -0.2662 0.2886 0.038 Uiso 1 1 calc R . . C6 C -0.30736(10) -0.3547(2) 0.27463(10) 0.0296(3) Uani 1 1 d . . . H6A H -0.3326 -0.3219 0.2170 0.035 Uiso 1 1 calc R . . C7 C -0.36453(8) -0.55889(18) 0.43796(8) 0.0184(2) Uani 1 1 d . . . N8 N -0.44596(7) -0.60982(17) 0.39452(7) 0.0226(2) Uani 1 1 d . . . C9 C -0.48545(9) -0.6970(2) 0.43743(10) 0.0292(3) Uani 1 1 d . . . H9A H -0.5422 -0.7384 0.4088 0.035 Uiso 1 1 calc R . . C10 C -0.44599(11) -0.7301(2) 0.52394(10) 0.0311(3) Uani 1 1 d . . . H10A H -0.4773 -0.7918 0.5520 0.037 Uiso 1 1 calc R . . N11 N -0.36725(9) -0.67888(18) 0.56770(8) 0.0277(3) Uani 1 1 d . . . C12 C -0.32463(9) -0.59368(19) 0.52442(8) 0.0210(3) Uani 1 1 d . . . C13 C -0.23720(10) -0.5445(2) 0.56808(9) 0.0242(3) Uani 1 1 d . . . H13A H -0.2110 -0.5673 0.6266 0.029 Uiso 1 1 calc R . . C14 C -0.19138(9) -0.46568(19) 0.52666(10) 0.0241(3) Uani 1 1 d . . . H14A H -0.1333 -0.4348 0.5564 0.029 Uiso 1 1 calc R . . B1 B -0.5000 -0.0197(3) 0.2500 0.0246(4) Uani 1 2 d S . . F1 F -0.48775(6) -0.12994(15) 0.31992(6) 0.0373(2) Uani 1 1 d . . . F2 F -0.42865(6) 0.09165(15) 0.26427(7) 0.0379(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 Ag1 0.02318(10) 0.03046(11) 0.02361(10) 0.000 -0.00791(7) 0.000 N1 0.0223(6) 0.0260(6) 0.0170(5) 0.0003(4) 0.0039(4) 0.0000(5) C2 0.0163(6) 0.0186(6) 0.0183(6) -0.0022(4) 0.0040(5) 0.0007(4) C3 0.0162(6) 0.0205(6) 0.0236(7) -0.0022(5) 0.0046(5) 0.0006(5) N4 0.0212(6) 0.0289(6) 0.0349(7) -0.0015(5) 0.0118(5) -0.0022(5) C5 0.0326(8) 0.0347(8) 0.0339(8) 0.0012(6) 0.0188(7) -0.0047(6) C6 0.0334(8) 0.0337(8) 0.0219(7) 0.0019(6) 0.0107(6) -0.0015(6) C7 0.0166(6) 0.0190(6) 0.0176(6) -0.0024(5) 0.0042(5) 0.0008(5) N8 0.0167(5) 0.0250(6) 0.0236(6) -0.0013(4) 0.0046(4) -0.0012(4) C9 0.0214(6) 0.0331(8) 0.0336(8) -0.0015(6) 0.0106(6) -0.0047(6) C10 0.0338(8) 0.0313(8) 0.0347(8) 0.0008(6) 0.0204(7) -0.0039(6) N11 0.0348(7) 0.0286(6) 0.0220(6) 0.0000(5) 0.0132(5) 0.0004(5) C12 0.0229(6) 0.0205(6) 0.0182(6) -0.0018(5) 0.0060(5) 0.0015(5) C13 0.0245(7) 0.0249(7) 0.0167(6) -0.0028(5) 0.0002(5) 0.0034(5) C14 0.0160(6) 0.0252(7) 0.0236(7) -0.0043(5) -0.0013(5) 0.0002(5) B1 0.0187(11) 0.0310(11) 0.0194(11) 0.000 0.0015(9) 0.000 F1 0.0406(5) 0.0431(5) 0.0231(5) 0.0066(4) 0.0060(4) -0.0004(4) F2 0.0228(5) 0.0435(6) 0.0426(6) -0.0005(5) 0.0065(4) -0.0066(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 N1 2.3723(12) . ? Ag1 N1 2.3723(12) 2_455 ? Ag1 N8 2.3870(12) 2_455 ? Ag1 N8 2.3870(12) . ? N1 C6 1.3219(19) . ? N1 C2 1.3515(18) . ? C2 C3 1.4089(19) . ? C2 C7 1.4473(18) . ? C3 N4 1.3567(18) . ? C3 C14 1.431(2) . ? N4 C5 1.317(2) . ? C5 C6 1.405(2) . ? C7 N8 1.3513(17) . ? C7 C12 1.4055(19) . ? N8 C9 1.3242(19) . ? C9 C10 1.403(2) . ? C10 N11 1.316(2) . ? N11 C12 1.3601(18) . ? C12 C13 1.432(2) . ? C13 C14 1.356(2) . ? B1 F1 1.3930(16) 2_455 ? B1 F1 1.3930(16) . ? B1 F2 1.3968(16) 2_455 ? B1 F2 1.3968(17) . ? 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 148.15(6) . 2_455 ? N1 Ag1 N8 117.93(4) . 2_455 ? N1 Ag1 N8 71.17(4) 2_455 2_455 ? N1 Ag1 N8 71.17(4) . . ? N1 Ag1 N8 117.92(4) 2_455 . ? N8 Ag1 N8 149.23(6) 2_455 . ? C6 N1 C2 116.42(13) . . ? C6 N1 Ag1 128.20(10) . . ? C2 N1 Ag1 115.37(9) . . ? N1 C2 C3 121.68(12) . . ? N1 C2 C7 119.22(12) . . ? C3 C2 C7 119.10(13) . . ? N4 C3 C2 120.95(13) . . ? N4 C3 C14 118.77(13) . . ? C2 C3 C14 120.27(13) . . ? C5 N4 C3 116.23(12) . . ? N4 C5 C6 122.86(13) . . ? N1 C6 C5 121.79(14) . . ? N8 C7 C12 121.63(12) . . ? N8 C7 C2 119.31(12) . . ? C12 C7 C2 119.03(12) . . ? C9 N8 C7 116.43(13) . . ? C9 N8 Ag1 128.77(10) . . ? C7 N8 Ag1 114.78(9) . . ? N8 C9 C10 121.98(14) . . ? N11 C10 C9 122.54(13) . . ? C10 N11 C12 116.49(13) . . ? N11 C12 C7 120.90(13) . . ? N11 C12 C13 118.76(13) . . ? C7 C12 C13 120.32(12) . . ? C14 C13 C12 120.69(13) . . ? C13 C14 C3 120.55(13) . . ? F1 B1 F1 109.62(18) 2_455 . ? F1 B1 F2 109.88(6) 2_455 2_455 ? F1 B1 F2 109.17(6) . 2_455 ? F1 B1 F2 109.17(6) 2_455 . ? F1 B1 F2 109.88(6) . . ? F2 B1 F2 109.10(18) 2_455 . ? 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 N1 Ag1 N1 C6 -69.57(13) 2_455 . . . ? N8 Ag1 N1 C6 29.70(14) 2_455 . . . ? N8 Ag1 N1 C6 177.55(14) . . . . ? N1 Ag1 N1 C2 111.72(10) 2_455 . . . ? N8 Ag1 N1 C2 -149.01(9) 2_455 . . . ? N8 Ag1 N1 C2 -1.16(9) . . . . ? C6 N1 C2 C3 0.1(2) . . . . ? Ag1 N1 C2 C3 179.00(10) . . . . ? C6 N1 C2 C7 -179.49(13) . . . . ? Ag1 N1 C2 C7 -0.62(15) . . . . ? N1 C2 C3 N4 -2.1(2) . . . . ? C7 C2 C3 N4 177.55(12) . . . . ? N1 C2 C3 C14 178.17(13) . . . . ? C7 C2 C3 C14 -2.2(2) . . . . ? C2 C3 N4 C5 1.6(2) . . . . ? C14 C3 N4 C5 -178.67(14) . . . . ? C3 N4 C5 C6 0.7(2) . . . . ? C2 N1 C6 C5 2.1(2) . . . . ? Ag1 N1 C6 C5 -176.56(11) . . . . ? N4 C5 C6 N1 -2.7(3) . . . . ? N1 C2 C7 N8 3.48(19) . . . . ? C3 C2 C7 N8 -176.14(12) . . . . ? N1 C2 C7 C12 -178.35(12) . . . . ? C3 C2 C7 C12 2.02(19) . . . . ? C12 C7 N8 C9 -1.2(2) . . . . ? C2 C7 N8 C9 176.92(12) . . . . ? C12 C7 N8 Ag1 177.49(10) . . . . ? C2 C7 N8 Ag1 -4.40(15) . . . . ? N1 Ag1 N8 C9 -178.61(14) . . . . ? N1 Ag1 N8 C9 34.77(14) 2_455 . . . ? N8 Ag1 N8 C9 -65.38(12) 2_455 . . . ? N1 Ag1 N8 C7 2.90(9) . . . . ? N1 Ag1 N8 C7 -143.72(9) 2_455 . . . ? N8 Ag1 N8 C7 116.13(10) 2_455 . . . ? C7 N8 C9 C10 1.9(2) . . . . ? Ag1 N8 C9 C10 -176.57(11) . . . . ? N8 C9 C10 N11 -0.8(3) . . . . ? C9 C10 N11 C12 -1.0(2) . . . . ? C10 N11 C12 C7 1.7(2) . . . . ? C10 N11 C12 C13 -176.49(13) . . . . ? N8 C7 C12 N11 -0.6(2) . . . . ? C2 C7 C12 N11 -178.74(12) . . . . ? N8 C7 C12 C13 177.55(13) . . . . ? C2 C7 C12 C13 -0.57(19) . . . . ? N11 C12 C13 C14 177.48(13) . . . . ? C7 C12 C13 C14 -0.7(2) . . . . ? C12 C13 C14 C3 0.6(2) . . . . ? N4 C3 C14 C13 -178.83(13) . . . . ? C2 C3 C14 C13 0.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.67 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.339 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.078 #===END data_compound7b _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Bis(pyrazino(2,3-f)quinoxaline) silver(I) tetrafluoroborate' ; _chemical_name_common [Ag(pyq)2]BF4 _chemical_melting_point ? _chemical_formula_moiety [Ag(C6H6N4)2]BF4 _chemical_formula_sum 'C20 H12 Ag B F4 N8' _chemical_formula_weight 559.06 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 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 9.3750(19) _cell_length_b 15.608(3) _cell_length_c 13.999(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.37(3) _cell_angle_gamma 90.00 _cell_volume 1955.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5462 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.8 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _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 'SMART CCD' _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 2292 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 28.80 _reflns_number_total 2292 _reflns_number_gt 2116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0388P)^2^+3.8449P] 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 2292 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.018457(16) 0.2500 0.02719(10) Uani 1 2 d S . . N1 N 0.57784(19) 0.07552(11) 0.12257(13) 0.0195(3) Uani 1 1 d . . . C2 C 0.6652(2) 0.02483(12) 0.08478(15) 0.0177(4) Uani 1 1 d . . . C3 C 0.7156(2) 0.05195(14) 0.00466(15) 0.0198(4) Uani 1 1 d . . . N4 N 0.6830(2) 0.13165(12) -0.03528(14) 0.0238(4) Uani 1 1 d . . . C5 C 0.6018(2) 0.18061(14) 0.00455(17) 0.0245(4) Uani 1 1 d . . . H5A H 0.5794 0.2373 -0.0202 0.029 Uiso 1 1 calc R . . C6 C 0.5468(2) 0.15277(14) 0.08214(16) 0.0227(4) Uani 1 1 d . . . H6A H 0.4856 0.1903 0.1064 0.027 Uiso 1 1 calc R . . C7 C 0.7042(2) -0.06009(13) 0.12562(15) 0.0191(4) Uani 1 1 d . . . N8 N 0.6582(2) -0.08572(11) 0.20373(13) 0.0226(4) Uani 1 1 d . . . C9 C 0.6909(3) -0.16502(15) 0.23559(17) 0.0284(5) Uani 1 1 d . . . H9A H 0.6595 -0.1856 0.2899 0.034 Uiso 1 1 calc R . . C10 C 0.7716(3) -0.21965(15) 0.19062(18) 0.0317(5) Uani 1 1 d . . . H10A H 0.7908 -0.2766 0.2149 0.038 Uiso 1 1 calc R . . N11 N 0.8218(2) -0.19549(13) 0.11653(15) 0.0297(4) Uani 1 1 d . . . C12 C 0.7879(2) -0.11410(14) 0.08203(16) 0.0229(4) Uani 1 1 d . . . C13 C 0.8359(2) -0.08464(15) -0.00001(17) 0.0255(4) Uani 1 1 d . . . H13A H 0.8927 -0.1214 -0.0287 0.031 Uiso 1 1 calc R . . C14 C 0.8009(3) -0.00448(15) -0.03730(17) 0.0244(4) Uani 1 1 d . . . H14A H 0.8334 0.0143 -0.0919 0.029 Uiso 1 1 calc R . . B1 B 1.0000 0.1198(2) 0.2500 0.0247(7) Uani 1 2 d S . . F1 F 0.9205(2) 0.16982(11) 0.17059(13) 0.0568(5) Uani 1 1 d . . . F2 F 1.0942(4) 0.0712(2) 0.21941(17) 0.1256(15) 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 Ag1 0.03250(15) 0.03112(15) 0.02509(14) 0.000 0.01949(10) 0.000 N1 0.0198(8) 0.0216(8) 0.0189(8) -0.0018(6) 0.0084(7) -0.0002(7) C2 0.0165(9) 0.0202(9) 0.0170(9) -0.0027(7) 0.0061(7) -0.0018(7) C3 0.0177(9) 0.0236(9) 0.0188(9) -0.0011(8) 0.0064(7) -0.0026(8) N4 0.0250(9) 0.0260(9) 0.0217(9) 0.0023(7) 0.0089(7) -0.0022(7) C5 0.0257(11) 0.0220(10) 0.0248(11) 0.0030(8) 0.0062(8) 0.0004(8) C6 0.0224(10) 0.0230(10) 0.0237(10) -0.0022(8) 0.0084(8) 0.0025(8) C7 0.0192(9) 0.0209(9) 0.0182(9) -0.0019(8) 0.0071(7) -0.0012(8) N8 0.0281(9) 0.0222(8) 0.0201(9) -0.0010(7) 0.0110(7) -0.0019(7) C9 0.0401(13) 0.0246(10) 0.0223(11) 0.0022(8) 0.0122(9) 0.0016(9) C10 0.0433(14) 0.0234(10) 0.0283(12) 0.0032(9) 0.0105(10) 0.0067(10) N11 0.0352(11) 0.0260(9) 0.0288(10) 0.0001(8) 0.0112(8) 0.0090(8) C12 0.0225(10) 0.0247(10) 0.0221(10) -0.0027(8) 0.0074(8) 0.0021(8) C13 0.0235(10) 0.0311(11) 0.0256(11) -0.0044(9) 0.0131(9) 0.0034(9) C14 0.0226(11) 0.0330(11) 0.0212(10) -0.0019(8) 0.0120(8) -0.0019(8) B1 0.0291(18) 0.0250(16) 0.0205(16) 0.000 0.0082(13) 0.000 F1 0.0735(13) 0.0381(9) 0.0364(9) 0.0011(7) -0.0177(9) 0.0087(9) F2 0.130(2) 0.194(3) 0.0431(12) -0.0153(16) 0.0106(14) 0.123(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 2.2989(18) 2_655 y Ag1 N1 2.2990(18) . y Ag1 N8 2.4157(19) . y Ag1 N8 2.4157(19) 2_655 y N1 C6 1.327(3) . ? N1 C2 1.355(3) . ? C2 C3 1.406(3) . ? C2 C7 1.446(3) . ? C3 N4 1.361(3) . ? C3 C14 1.428(3) . ? N4 C5 1.315(3) . ? C5 C6 1.403(3) . ? C7 N8 1.350(3) . ? C7 C12 1.409(3) . ? N8 C9 1.321(3) . ? C9 C10 1.407(3) . ? C10 N11 1.315(3) . ? N11 C12 1.363(3) . ? C12 C13 1.429(3) . ? C13 C14 1.358(3) . ? B1 F2 1.328(3) . ? B1 F2 1.328(3) 2_755 ? B1 F1 1.381(3) 2_755 ? B1 F1 1.381(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 134.42(9) 2_655 . y N1 Ag1 N8 146.23(6) 2_655 . y N1 Ag1 N8 71.95(6) . . y N1 Ag1 N8 71.95(6) 2_655 2_655 y N1 Ag1 N8 146.23(6) . 2_655 y N8 Ag1 N8 95.39(9) . 2_655 y C6 N1 C2 116.44(18) . . ? C6 N1 Ag1 127.08(14) . . ? C2 N1 Ag1 116.48(13) . . ? N1 C2 C3 121.47(18) . . ? N1 C2 C7 119.43(18) . . ? C3 C2 C7 119.08(18) . . ? N4 C3 C2 121.03(19) . . ? N4 C3 C14 118.64(19) . . ? C2 C3 C14 120.3(2) . . ? C5 N4 C3 116.39(19) . . ? N4 C5 C6 122.8(2) . . ? N1 C6 C5 121.8(2) . . ? N8 C7 C12 121.82(19) . . ? N8 C7 C2 119.18(18) . . ? C12 C7 C2 118.99(18) . . ? C9 N8 C7 116.93(19) . . ? C9 N8 Ag1 129.78(16) . . ? C7 N8 Ag1 112.81(13) . . ? N8 C9 C10 121.3(2) . . ? N11 C10 C9 123.1(2) . . ? C10 N11 C12 116.5(2) . . ? N11 C12 C7 120.4(2) . . ? N11 C12 C13 119.3(2) . . ? C7 C12 C13 120.4(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C3 120.7(2) . . ? F2 B1 F2 110.3(5) . 2_755 ? F2 B1 F1 109.36(17) . 2_755 ? F2 B1 F1 108.34(15) 2_755 2_755 ? F2 B1 F1 108.34(15) . . ? F2 B1 F1 109.36(17) 2_755 . ? F1 B1 F1 111.1(3) 2_755 . ? 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 N1 Ag1 N1 C6 -23.37(16) 2_655 . . . ? N8 Ag1 N1 C6 -178.16(19) . . . . ? N8 Ag1 N1 C6 109.87(18) 2_655 . . . ? N1 Ag1 N1 C2 156.46(15) 2_655 . . . ? N8 Ag1 N1 C2 1.67(14) . . . . ? N8 Ag1 N1 C2 -70.30(19) 2_655 . . . ? C6 N1 C2 C3 -2.1(3) . . . . ? Ag1 N1 C2 C3 178.01(15) . . . . ? C6 N1 C2 C7 179.71(18) . . . . ? Ag1 N1 C2 C7 -0.1(2) . . . . ? N1 C2 C3 N4 2.6(3) . . . . ? C7 C2 C3 N4 -179.24(18) . . . . ? N1 C2 C3 C14 -176.60(19) . . . . ? C7 C2 C3 C14 1.5(3) . . . . ? C2 C3 N4 C5 -0.5(3) . . . . ? C14 C3 N4 C5 178.7(2) . . . . ? C3 N4 C5 C6 -1.8(3) . . . . ? C2 N1 C6 C5 -0.2(3) . . . . ? Ag1 N1 C6 C5 179.67(15) . . . . ? N4 C5 C6 N1 2.3(3) . . . . ? N1 C2 C7 N8 -3.0(3) . . . . ? C3 C2 C7 N8 178.83(19) . . . . ? N1 C2 C7 C12 176.38(19) . . . . ? C3 C2 C7 C12 -1.8(3) . . . . ? C12 C7 N8 C9 -2.2(3) . . . . ? C2 C7 N8 C9 177.2(2) . . . . ? C12 C7 N8 Ag1 -175.09(16) . . . . ? C2 C7 N8 Ag1 4.3(2) . . . . ? N1 Ag1 N8 C9 38.3(3) 2_655 . . . ? N1 Ag1 N8 C9 -174.9(2) . . . . ? N8 Ag1 N8 C9 -26.94(17) 2_655 . . . ? N1 Ag1 N8 C7 -149.92(13) 2_655 . . . ? N1 Ag1 N8 C7 -3.10(13) . . . . ? N8 Ag1 N8 C7 144.83(17) 2_655 . . . ? C7 N8 C9 C10 0.7(3) . . . . ? Ag1 N8 C9 C10 172.19(17) . . . . ? N8 C9 C10 N11 1.4(4) . . . . ? C9 C10 N11 C12 -2.0(4) . . . . ? C10 N11 C12 C7 0.5(3) . . . . ? C10 N11 C12 C13 -178.4(2) . . . . ? N8 C7 C12 N11 1.7(3) . . . . ? C2 C7 C12 N11 -177.69(19) . . . . ? N8 C7 C12 C13 -179.4(2) . . . . ? C2 C7 C12 C13 1.2(3) . . . . ? N11 C12 C13 C14 178.6(2) . . . . ? C7 C12 C13 C14 -0.3(3) . . . . ? C12 C13 C14 C3 0.1(3) . . . . ? N4 C3 C14 C13 -179.9(2) . . . . ? C2 C3 C14 C13 -0.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 0.956 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.078 #===END data_bpzhcl _audit_creation_method SHELXL-97 _chemical_name_systematic ; '2,2'-bipyrazine' ; _chemical_name_common 'bipyrazine' _chemical_melting_point ? _chemical_formula_moiety '(C4H3N2)2' _chemical_formula_sum 'C8 H6 N4' _chemical_formula_weight 158.17 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' _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 3.686(5) _cell_length_b 5.290(6) _cell_length_c 9.470(14) _cell_angle_alpha 102.43(11) _cell_angle_beta 92.78(11) _cell_angle_gamma 100.93(9) _cell_volume 176.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 12 _cell_measurement_theta_max 14 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.78 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 82 _exptl_absorpt_coefficient_mu 0.099 _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 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 'Stoe Stadi-4' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/-1.3' _diffrn_reflns_number 688 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0078 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 25.97 _reflns_number_total 688 _reflns_number_gt 618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0794P)^2^+0.0286P] 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 688 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 N1 N 0.7172(3) 0.63945(19) 0.35924(11) 0.0222(3) Uani 1 1 d . . . C2 C 0.5257(3) 0.4583(2) 0.42180(12) 0.0189(4) Uani 1 1 d . . . C3 C 0.3785(3) 0.1989(2) 0.34166(14) 0.0221(4) Uani 1 1 d . . . H3A H 0.2457 0.0749 0.3895 0.027 Uiso 1 1 calc R . . N4 N 0.4198(3) 0.12145(19) 0.20037(11) 0.0247(4) Uani 1 1 d . . . C5 C 0.6089(4) 0.3044(3) 0.13883(14) 0.0237(4) Uani 1 1 d . . . H5A H 0.6433 0.2583 0.0385 0.028 Uiso 1 1 calc R . . C6 C 0.7572(3) 0.5614(2) 0.21808(13) 0.0235(4) Uani 1 1 d . . . H6A H 0.8908 0.6847 0.1701 0.028 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 N1 0.0236(6) 0.0174(6) 0.0249(6) 0.0047(4) 0.0024(4) 0.0026(4) C2 0.0178(6) 0.0158(6) 0.0231(7) 0.0044(5) 0.0005(5) 0.0041(5) C3 0.0241(7) 0.0170(6) 0.0239(7) 0.0037(5) 0.0028(5) 0.0019(5) N4 0.0283(6) 0.0198(6) 0.0237(6) 0.0013(4) 0.0019(4) 0.0035(5) C5 0.0262(7) 0.0226(7) 0.0217(6) 0.0032(5) 0.0028(5) 0.0056(5) C6 0.0255(7) 0.0203(7) 0.0244(7) 0.0061(5) 0.0040(5) 0.0028(5) _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 N1 C6 1.336(3) . y N1 C2 1.340(2) . y C2 C3 1.408(3) . y C2 C2 1.484(3) 2_666 y C3 N4 1.337(3) . y N4 C5 1.337(2) . y C5 C6 1.396(3) . y 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 C6 N1 C2 116.61(15) . . y N1 C2 C3 121.08(15) . . ? N1 C2 C2 117.49(17) . 2_666 ? C3 C2 C2 121.43(17) . 2_666 ? N4 C3 C2 122.10(15) . . ? C3 N4 C5 116.30(15) . . y N4 C5 C6 121.79(15) . . ? N1 C6 C5 122.11(15) . . ? 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 C6 N1 C2 C3 0.56(18) . . . . ? C6 N1 C2 C2 -179.33(11) . . . 2_666 y N1 C2 C3 N4 -0.5(2) . . . . ? C2 C2 C3 N4 179.41(11) 2_666 . . . y C2 C3 N4 C5 -0.05(18) . . . . ? C3 N4 C5 C6 0.45(18) . . . . ? C2 N1 C6 C5 -0.17(19) . . . . ? N4 C5 C6 N1 -0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.289 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.053 #===END data_tcbipz _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Pyrazino(2,3-f)quinoxaline' ; _chemical_name_common Pyrazino(2,3-f)quinoxaline _chemical_melting_point 250-252 _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 N4' _chemical_formula_weight 182.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 3.7611(8) _cell_length_b 8.271(2) _cell_length_c 26.110(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 812.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1196 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 25.91 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'Pyrazino(2,3-f)quinoxaline' ; _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' _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 1197 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.85 _reflns_number_total 1197 _reflns_number_gt 823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT version 6.01 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0774P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 7(5) _refine_ls_number_reflns 1197 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -1.3687(7) -0.3128(3) 0.79527(8) 0.0251(6) Uani 1 1 d . . . C2 C -1.2529(9) -0.3162(4) 0.84502(10) 0.0203(7) Uani 1 1 d . . . C3 C -1.0928(9) -0.1802(3) 0.86766(10) 0.0211(7) Uani 1 1 d . . . N4 N -1.0418(8) -0.0396(3) 0.84113(9) 0.0278(7) Uani 1 1 d . . . C5 C -1.1596(10) -0.0402(4) 0.79349(12) 0.0299(8) Uani 1 1 d . . . H5 H -1.124(9) 0.060(4) 0.7753(11) 0.020(8) Uiso 1 1 d . . . C6 C -1.3197(10) -0.1748(4) 0.77068(12) 0.0283(8) Uani 1 1 d . . . H6 H -1.398(10) -0.167(4) 0.7363(13) 0.036(10) Uiso 1 1 d . . . C7 C -1.3024(8) -0.4608(4) 0.87507(10) 0.0192(7) Uani 1 1 d . . . N8 N -1.4623(8) -0.5924(3) 0.85399(8) 0.0236(6) Uani 1 1 d . . . C9 C -1.5052(10) -0.7186(4) 0.88439(12) 0.0265(8) Uani 1 1 d . . . H9 H -1.631(9) -0.812(3) 0.8739(10) 0.015(8) Uiso 1 1 d . . . C10 C -1.3945(10) -0.7169(4) 0.93595(12) 0.0292(8) Uani 1 1 d . . . H10 H -1.419(9) -0.812(4) 0.9592(11) 0.019(8) Uiso 1 1 d . . . N11 N -1.2385(8) -0.5924(3) 0.95713(9) 0.0260(7) Uani 1 1 d . . . C12 C -1.1862(9) -0.4615(4) 0.92660(10) 0.0200(7) Uani 1 1 d . . . C13 C -1.0188(9) -0.3230(4) 0.94773(11) 0.0240(7) Uani 1 1 d . . . H13 H -0.948(10) -0.326(3) 0.9839(12) 0.028(8) Uiso 1 1 d . . . C14 C -0.9743(9) -0.1863(4) 0.91969(10) 0.0242(7) Uani 1 1 d . . . H14 H -0.865(11) -0.088(4) 0.9354(13) 0.040(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0303(15) 0.0309(15) 0.0140(12) 0.0004(11) -0.0034(12) 0.0052(13) C2 0.0189(15) 0.0259(17) 0.0160(14) 0.0002(12) 0.0002(13) 0.0026(14) C3 0.0215(17) 0.0231(16) 0.0186(14) -0.0011(12) 0.0016(13) 0.0009(14) N4 0.0298(15) 0.0249(14) 0.0288(14) 0.0039(11) 0.0022(13) -0.0017(14) C5 0.0329(19) 0.0303(18) 0.0266(16) 0.0109(15) 0.0012(15) -0.0007(16) C6 0.034(2) 0.0355(19) 0.0159(14) 0.0052(14) 0.0021(15) 0.0061(17) C7 0.0220(16) 0.0211(15) 0.0146(13) -0.0029(12) 0.0014(12) 0.0026(13) N8 0.0291(16) 0.0211(12) 0.0207(12) -0.0016(11) 0.0020(12) 0.0011(14) C9 0.0292(19) 0.0228(16) 0.0275(17) -0.0017(13) 0.0033(15) -0.0025(15) C10 0.034(2) 0.0257(17) 0.0280(17) 0.0083(15) 0.0030(16) -0.0020(15) N11 0.0311(16) 0.0282(15) 0.0188(12) 0.0060(11) 0.0030(12) 0.0028(14) C12 0.0240(16) 0.0221(16) 0.0138(13) 0.0015(12) 0.0015(13) 0.0040(14) C13 0.0262(18) 0.0322(17) 0.0136(13) -0.0035(13) -0.0012(13) 0.0041(16) C14 0.0248(18) 0.0272(17) 0.0206(15) -0.0090(13) -0.0007(14) -0.0022(16) _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 N1 C6 1.322(4) . ? N1 C2 1.370(3) . ? C2 C3 1.406(4) . ? C2 C7 1.442(4) . ? C3 N4 1.368(4) . ? C3 C14 1.430(4) . ? N4 C5 1.320(4) . ? C5 C6 1.399(5) . ? C7 N8 1.359(4) . ? C7 C12 1.415(4) . ? N8 C9 1.322(4) . ? C9 C10 1.409(4) . ? C10 N11 1.308(4) . ? N11 C12 1.359(4) . ? C12 C13 1.419(4) . ? C13 C14 1.358(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 C6 N1 C2 115.7(3) . . ? N1 C2 C3 121.2(3) . . ? N1 C2 C7 119.5(3) . . ? C3 C2 C7 119.3(2) . . ? N4 C3 C2 121.8(3) . . ? N4 C3 C14 117.9(3) . . ? C2 C3 C14 120.3(3) . . ? C5 N4 C3 115.3(3) . . ? N4 C5 C6 123.3(3) . . ? N1 C6 C5 122.7(3) . . ? N8 C7 C12 121.3(3) . . ? N8 C7 C2 120.0(2) . . ? C12 C7 C2 118.7(3) . . ? C9 N8 C7 116.3(3) . . ? N8 C9 C10 122.0(3) . . ? N11 C10 C9 123.0(3) . . ? C10 N11 C12 116.4(2) . . ? N11 C12 C7 121.1(3) . . ? N11 C12 C13 118.6(2) . . ? C7 C12 C13 120.3(3) . . ? C14 C13 C12 121.2(3) . . ? C13 C14 C3 120.2(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 C6 N1 C2 C3 0.0(4) . . . . ? C6 N1 C2 C7 178.7(3) . . . . ? N1 C2 C3 N4 -0.7(5) . . . . ? C7 C2 C3 N4 -179.5(3) . . . . ? N1 C2 C3 C14 179.9(3) . . . . ? C7 C2 C3 C14 1.2(4) . . . . ? C2 C3 N4 C5 1.3(5) . . . . ? C14 C3 N4 C5 -179.3(3) . . . . ? C3 N4 C5 C6 -1.2(5) . . . . ? C2 N1 C6 C5 0.1(5) . . . . ? N4 C5 C6 N1 0.5(6) . . . . ? N1 C2 C7 N8 0.1(4) . . . . ? C3 C2 C7 N8 178.9(3) . . . . ? N1 C2 C7 C12 -179.0(3) . . . . ? C3 C2 C7 C12 -0.3(4) . . . . ? C12 C7 N8 C9 0.7(4) . . . . ? C2 C7 N8 C9 -178.4(3) . . . . ? C7 N8 C9 C10 0.5(5) . . . . ? N8 C9 C10 N11 -0.9(6) . . . . ? C9 C10 N11 C12 0.0(5) . . . . ? C10 N11 C12 C7 1.2(5) . . . . ? C10 N11 C12 C13 179.8(3) . . . . ? N8 C7 C12 N11 -1.6(5) . . . . ? C2 C7 C12 N11 177.5(3) . . . . ? N8 C7 C12 C13 179.8(3) . . . . ? C2 C7 C12 C13 -1.1(4) . . . . ? N11 C12 C13 C14 -177.0(3) . . . . ? C7 C12 C13 C14 1.6(5) . . . . ? C12 C13 C14 C3 -0.8(5) . . . . ? N4 C3 C14 C13 179.9(3) . . . . ? C2 C3 C14 C13 -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.233 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.066 #===END