# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1235 data_xa # number 9 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(\m-5,5'-dicyano-2,2'-bipyridine)nitratosilver(I)] ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H6 Ag N5 O3' _chemical_formula_weight 376.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2230(2) _cell_length_b 7.5328(2) _cell_length_c 20.3896(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.3080(10) _cell_angle_gamma 90.00 _cell_volume 1260.87(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column-prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.775920 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9319 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 31.06 _reflns_number_total 3703 _reflns_number_gt 3269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART CCD' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON _computing_publication_material CIFTAB _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 ; w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+2.0207P] where P=(Fo^2^+2Fc^2^)/3' ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3703 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.015 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 0.31451(2) 0.41993(3) 0.071486(10) 0.03073(7) Uani 1 d . . . O1 O 0.5462(3) 0.6028(3) 0.06108(11) 0.0386(5) Uani 1 d . . . O2 O 0.4349(3) 0.6849(4) 0.14994(13) 0.0524(6) Uani 1 d . . . O3 O 0.6479(3) 0.8220(4) 0.12031(17) 0.0618(8) Uani 1 d . . . N1 N 0.0657(3) 0.3128(3) 0.02620(11) 0.0251(4) Uani 1 d . . . N2 N 0.0997(3) 0.4404(3) 0.14975(11) 0.0269(4) Uani 1 d . . . N3 N -0.0631(4) 0.0294(4) -0.17882(14) 0.0433(6) Uani 1 d . . . N4 N 0.0601(3) 0.6771(4) 0.36597(13) 0.0367(5) Uani 1 d . . . N5 N 0.5434(3) 0.7045(3) 0.11110(13) 0.0341(5) Uani 1 d . . . C1 C 0.0581(3) 0.2424(4) -0.03425(12) 0.0259(5) Uani 1 d . . . H1 H 0.151(5) 0.252(5) -0.0581(18) 0.040(10) Uiso 1 d . . . C2 C -0.0816(3) 0.1573(4) -0.06109(12) 0.0262(5) Uani 1 d . . . C3 C -0.2175(3) 0.1450(4) -0.02392(13) 0.0294(5) Uani 1 d . . . H3 H -0.317(5) 0.085(5) -0.042(2) 0.042(10) Uiso 1 d . . . C4 C -0.2102(3) 0.2195(4) 0.03864(13) 0.0282(5) Uani 1 d . . . H4 H -0.294(5) 0.209(5) 0.0666(19) 0.042(10) Uiso 1 d . . . C5 C -0.0664(3) 0.3037(3) 0.06232(12) 0.0227(4) Uani 1 d . . . C6 C -0.0503(3) 0.3856(3) 0.12962(12) 0.0231(4) Uani 1 d . . . C7 C -0.1833(3) 0.4065(4) 0.16850(14) 0.0304(5) Uani 1 d . . . H7 H -0.297(5) 0.366(5) 0.155(2) 0.049(11) Uiso 1 d . . . C8 C -0.1601(3) 0.4804(4) 0.23090(14) 0.0308(5) Uani 1 d . . . H8 H -0.244(5) 0.481(5) 0.258(2) 0.041(10) Uiso 1 d . . . C9 C -0.0033(3) 0.5320(4) 0.25205(13) 0.0265(5) Uani 1 d . . . C10 C 0.1233(3) 0.5123(4) 0.20978(13) 0.0287(5) Uani 1 d . . . H10 H 0.224(4) 0.546(5) 0.2212(17) 0.031(9) Uiso 1 d . . . C11 C -0.0757(4) 0.0848(4) -0.12717(14) 0.0313(5) Uani 1 d . . . C12 C 0.0318(3) 0.6113(4) 0.31580(14) 0.0295(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 0.02084(10) 0.03741(12) 0.03392(11) -0.00057(9) 0.00133(7) - 0.00248(8) O1 0.0349(11) 0.0423(12) 0.0390(11) -0.0099(9) 0.0058(9) -0.0057(9) O2 0.0452(13) 0.0621(16) 0.0519(14) -0.0132(13) 0.0210(11) -0.0179(12) O3 0.0422(14) 0.0541(15) 0.092(2) -0.0376(15) 0.0295(14) -0.0204(12) N1 0.0243(10) 0.0264(10) 0.0247(9) 0.0016(8) 0.0023(8) 0.0007(8) N2 0.0206(9) 0.0349(12) 0.0252(10) -0.0023(9) 0.0018(8) -0.0028(8) N3 0.0458(16) 0.0505(16) 0.0332(13) -0.0054(12) -0.0004(11) 0.0007(13) N4 0.0299(12) 0.0434(14) 0.0371(12) -0.0100(11) 0.0047(10) -0.0035(10) N5 0.0247(10) 0.0347(12) 0.0436(13) -0.0063(11) 0.0076(9) -0.0014(9) C1 0.0257(11) 0.0265(11) 0.0258(11) 0.0024(9) 0.0036(9) 0.0015(10) C2 0.0298(12) 0.0259(11) 0.0227(10) 0.0020(10) 0.0000(9) 0.0037(10) C3 0.0249(11) 0.0335(13) 0.0293(12) -0.0002(11) -0.0018(9) -0.0008(10) C4 0.0215(11) 0.0338(13) 0.0293(12) -0.0014(10) 0.0027(9) -0.0023(10) C5 0.0212(10) 0.0223(10) 0.0243(10) 0.0030(9) 0.0000(8) 0.0012(8) C6 0.0216(10) 0.0236(11) 0.0242(11) 0.0020(9) 0.0013(8) -0.0004(8) C7 0.0215(11) 0.0375(14) 0.0323(13) -0.0038(11) 0.0036(10) -0.0036(10) C8 0.0264(12) 0.0378(14) 0.0289(12) -0.0037(11) 0.0071(10) -0.0008(11) C9 0.0276(12) 0.0258(11) 0.0260(11) 0.0026(9) 0.0013(9) -0.0011(9) C10 0.0235(11) 0.0353(13) 0.0271(12) -0.0016(11) 0.0000(9) -0.0012(10) C11 0.0330(13) 0.0333(13) 0.0274(12) 0.0007(11) -0.0005(10) -0.0001(11) C12 0.0257(12) 0.0305(13) 0.0324(13) -0.0025(10) 0.0034(10) -0.0015(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 N1 2.339(2) . ? Ag1 O1 2.371(2) . ? Ag1 N4 2.425(3) 2_545 ? Ag1 N2 2.453(2) . ? O1 N5 1.277(3) . ? O2 N5 1.236(3) . ? O3 N5 1.240(3) . ? N1 C1 1.340(3) . ? N1 C5 1.349(3) . ? N2 C6 1.342(3) . ? N2 C10 1.342(3) . ? N3 C11 1.143(4) . ? N4 C12 1.148(4) . ? N4 Ag1 2.426(3) 2 ? C1 C2 1.399(4) . ? C1 H1 0.93(4) . ? C2 C3 1.389(4) . ? C2 C11 1.457(4) . ? C3 C4 1.391(4) . ? C3 H3 0.99(4) . ? C4 C5 1.403(3) . ? C4 H4 0.92(4) . ? C5 C6 1.503(3) . ? C6 C7 1.397(4) . ? C7 C8 1.392(4) . ? C7 H7 1.01(4) . ? C8 C9 1.391(4) . ? C8 H8 0.91(4) . ? C9 C10 1.397(4) . ? C9 C12 1.445(4) . ? C10 H10 0.89(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O1 148.69(8) . . ? N1 Ag1 N4 106.44(8) . 2_545 ? O1 Ag1 N4 99.54(9) . 2_545 ? N1 Ag1 N2 68.42(7) . . ? O1 Ag1 N2 129.38(8) . . ? N4 Ag1 N2 90.32(8) 2_545 . ? N5 O1 Ag1 103.04(17) . . ? C1 N1 C5 119.1(2) . . ? C1 N1 Ag1 119.55(17) . . ? C5 N1 Ag1 121.04(16) . . ? C6 N2 C10 119.0(2) . . ? C6 N2 Ag1 117.72(17) . . ? C10 N2 Ag1 123.16(17) . . ? C12 N4 Ag1 148.4(2) . 2 ? O2 N5 O3 120.5(3) . . ? O2 N5 O1 119.1(3) . . ? O3 N5 O1 120.3(3) . . ? N1 C1 C2 122.3(2) . . ? N1 C1 H1 117(2) . . ? C2 C1 H1 121(2) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C11 123.4(3) . . ? C1 C2 C11 117.6(2) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 120(3) . . ? C4 C3 H3 121(3) . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4 123(2) . . ? C5 C4 H4 118(2) . . ? N1 C5 C4 121.6(2) . . ? N1 C5 C6 116.5(2) . . ? C4 C5 C6 121.9(2) . . ? N2 C6 C7 121.9(2) . . ? N2 C6 C5 115.9(2) . . ? C7 C6 C5 122.2(2) . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 117(2) . . ? C6 C7 H7 123(2) . . ? C9 C8 C7 118.1(3) . . ? C9 C8 H8 122(2) . . ? C7 C8 H8 119(3) . . ? C8 C9 C10 119.3(2) . . ? C8 C9 C12 121.9(3) . . ? C10 C9 C12 118.8(2) . . ? N2 C10 C9 122.1(2) . . ? N2 C10 H10 116(2) . . ? C9 C10 H10 122(2) . . ? N3 C11 C2 176.7(3) . . ? N4 C12 C9 178.8(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 N1 Ag1 O1 N5 122.77(19) . . . . ? N4 Ag1 O1 N5 -91.30(19) 2_545 . . . ? N2 Ag1 O1 N5 7.1(2) . . . . ? O1 Ag1 N1 C1 52.0(3) . . . . ? N4 Ag1 N1 C1 -92.9(2) 2_545 . . . ? N2 Ag1 N1 C1 -176.5(2) . . . . ? O1 Ag1 N1 C5 -134.96(19) . . . . ? N4 Ag1 N1 C5 80.2(2) 2_545 . . . ? N2 Ag1 N1 C5 -3.45(18) . . . . ? N1 Ag1 N2 C6 -0.96(18) . . . . ? O1 Ag1 N2 C6 148.81(18) . . . . ? N4 Ag1 N2 C6 -108.5(2) 2_545 . . . ? N1 Ag1 N2 C10 -177.1(2) . . . . ? O1 Ag1 N2 C10 -27.4(3) . . . . ? N4 Ag1 N2 C10 75.3(2) 2_545 . . . ? Ag1 O1 N5 O2 1.2(3) . . . . ? Ag1 O1 N5 O3 -178.4(3) . . . . ? C5 N1 C1 C2 -1.0(4) . . . . ? Ag1 N1 C1 C2 172.28(19) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? N1 C1 C2 C11 -179.6(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C11 C2 C3 C4 -179.8(3) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C1 N1 C5 C4 1.3(4) . . . . ? Ag1 N1 C5 C4 -171.85(19) . . . . ? C1 N1 C5 C6 -179.8(2) . . . . ? Ag1 N1 C5 C6 7.1(3) . . . . ? C3 C4 C5 N1 -0.7(4) . . . . ? C3 C4 C5 C6 -179.5(2) . . . . ? C10 N2 C6 C7 2.1(4) . . . . ? Ag1 N2 C6 C7 -174.2(2) . . . . ? C10 N2 C6 C5 -179.0(2) . . . . ? Ag1 N2 C6 C5 4.7(3) . . . . ? N1 C5 C6 N2 -7.6(3) . . . . ? C4 C5 C6 N2 171.3(2) . . . . ? N1 C5 C6 C7 171.3(2) . . . . ? C4 C5 C6 C7 -9.8(4) . . . . ? N2 C6 C7 C8 -2.3(4) . . . . ? C5 C6 C7 C8 178.9(3) . . . . ? C6 C7 C8 C9 0.3(4) . . . . ? C7 C8 C9 C10 1.7(4) . . . . ? C7 C8 C9 C12 179.4(3) . . . . ? C6 N2 C10 C9 0.0(4) . . . . ? Ag1 N2 C10 C9 176.2(2) . . . . ? C8 C9 C10 N2 -1.9(4) . . . . ? C12 C9 C10 N2 -179.8(3) . . . . ? C3 C2 C11 N3 -169(6) . . . . ? C1 C2 C11 N3 10(6) . . . . ? Ag1 N4 C12 C9 -24(15) 2 . . . ? C8 C9 C12 N4 -105(15) . . . . ? C10 C9 C12 N4 72(15) . . . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.537 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.097 #=END data_xb number 11 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; [bis(5,5'-dicyano-2,2'bipyridine)silver(I)]-tetrafluoroborate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H12 Ag B F4 N8' _chemical_formula_weight 607.10 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' '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 21.9430(3) _cell_length_b 7.52980(10) _cell_length_c 15.7431(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.6760(10) _cell_angle_gamma 90.00 _cell_volume 2400.10(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description half-prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.576779 _exptl_absorpt_correction_T_max 0.884642 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7335 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 31.16 _reflns_number_total 3420 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON _computing_publication_material CIFTAB _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 ; w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.5906P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3420 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.87773(4) 0.2500 0.03599(12) Uani 1 d S . . N1 N 0.05687(11) 0.7618(3) 0.39876(15) 0.0292(5) Uani 1 d . . . N2 N -0.06433(12) 0.9159(3) 0.33535(15) 0.0273(5) Uani 1 d . . . N3 N 0.26381(15) 0.4800(5) 0.5648(2) 0.0559(8) Uani 1 d . . . N4 N -0.28381(15) 1.1198(4) 0.2743(2) 0.0546(8) Uani 1 d . . . C1 C 0.11684(15) 0.6900(4) 0.4271(2) 0.0343(6) Uani 1 d . . . H1 H 0.1397(16) 0.693(4) 0.389(2) 0.037(9) Uiso 1 d . . . C2 C 0.14623(14) 0.6102(4) 0.5131(2) 0.0312(6) Uani 1 d . . . C3 C 0.11204(14) 0.6049(4) 0.57100(19) 0.0296(6) Uani 1 d . . . H3 H 0.1295(15) 0.552(4) 0.630(2) 0.030(8) Uiso 1 d . . . C4 C 0.04979(14) 0.6791(4) 0.54089(18) 0.0270(6) Uani 1 d . . . H4 H 0.0277(16) 0.680(4) 0.576(2) 0.033(9) Uiso 1 d . . . C5 C 0.02364(13) 0.7574(3) 0.45396(17) 0.0240(5) Uani 1 d . . . C6 C -0.04366(13) 0.8385(3) 0.41870(17) 0.0235(5) Uani 1 d . . . C7 C -0.08347(14) 0.8334(4) 0.4691(2) 0.0291(6) Uani 1 d . . . H7 H -0.0678(17) 0.788(5) 0.527(3) 0.049(10) Uiso 1 d . . . C8 C -0.14621(15) 0.9064(4) 0.4330(2) 0.0312(6) Uani 1 d . . . H8 H -0.1727(17) 0.902(4) 0.463(2) 0.036(9) Uiso 1 d . . . C9 C -0.16697(13) 0.9833(4) 0.3461(2) 0.0303(6) Uani 1 d . . . C10 C -0.12439(15) 0.9881(4) 0.30042(19) 0.0323(6) Uani 1 d . . . H10 H -0.1375(16) 1.041(4) 0.239(2) 0.040(9) Uiso 1 d . . . C11 C 0.21187(16) 0.5375(4) 0.5408(2) 0.0396(7) Uani 1 d . . . C12 C -0.23226(16) 1.0603(4) 0.3051(2) 0.0390(7) Uani 1 d . . . B1 B 0.0000 0.3733(7) 0.2500 0.0422(12) Uani 1 d S . . F1 F 0.03928(12) 0.4783(3) 0.21908(15) 0.0622(6) Uani 1 d . . . F2 F 0.03890(13) 0.2653(3) 0.32037(15) 0.0730(7) 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 0.0493(2) 0.04454(19) 0.02319(15) 0.000 0.02394(14) 0.000 N1 0.0303(12) 0.0384(12) 0.0245(11) -0.0020(9) 0.0169(9) 0.0007(9) N2 0.0323(12) 0.0325(12) 0.0200(10) -0.0022(8) 0.0132(9) -0.0015(8) N3 0.0388(16) 0.086(2) 0.0474(17) -0.0012(16) 0.0211(14) 0.0153(15) N4 0.0409(16) 0.0610(18) 0.0586(19) 0.0031(15) 0.0154(15) 0.0113(14) C1 0.0315(15) 0.0457(16) 0.0312(14) -0.0039(12) 0.0184(13) 0.0001(12) C2 0.0294(14) 0.0337(14) 0.0319(13) -0.0062(11) 0.0133(11) 0.0004(11) C3 0.0326(14) 0.0327(14) 0.0248(12) 0.0001(11) 0.0127(11) -0.0014(11) C4 0.0308(14) 0.0336(13) 0.0208(12) -0.0021(10) 0.0146(11) -0.0032(10) C5 0.0286(13) 0.0271(12) 0.0209(11) -0.0051(9) 0.0146(10) -0.0051(9) C6 0.0284(13) 0.0250(12) 0.0211(11) -0.0064(9) 0.0139(10) -0.0049(9) C7 0.0316(15) 0.0341(14) 0.0257(13) 0.0011(11) 0.0155(11) 0.0000(10) C8 0.0287(14) 0.0358(15) 0.0363(15) -0.0040(11) 0.0203(12) -0.0024(10) C9 0.0271(13) 0.0317(14) 0.0318(13) -0.0061(11) 0.0109(11) -0.0013(10) C10 0.0350(15) 0.0382(15) 0.0232(12) -0.0006(11) 0.0105(11) 0.0019(11) C11 0.0364(17) 0.0508(18) 0.0357(15) -0.0032(14) 0.0183(13) 0.0046(14) C12 0.0346(17) 0.0399(15) 0.0409(16) -0.0040(13) 0.0129(14) 0.0015(12) B1 0.070(4) 0.039(2) 0.029(2) 0.000 0.032(2) 0.000 F1 0.0964(17) 0.0536(13) 0.0619(13) 0.0036(10) 0.0585(13) 0.0000(11) F2 0.099(2) 0.0813(17) 0.0406(12) 0.0222(11) 0.0287(13) 0.0118(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 Ag1 0.0000(7) 2 ? Ag1 N2 2.312(2) 2 ? Ag1 N2 2.312(2) . ? Ag1 N1 2.356(2) 2 ? Ag1 N1 2.356(2) . ? N1 C1 1.331(4) . ? N1 C5 1.333(3) . ? N1 Ag1 2.356(2) 2 ? N2 C10 1.333(4) . ? N2 C6 1.345(3) . ? N2 Ag1 2.312(2) 2 ? N3 C11 1.139(4) . ? N4 C12 1.137(4) . ? C1 C2 1.391(4) . ? C1 H1 0.91(4) . ? C2 C3 1.387(4) . ? C2 C11 1.442(4) . ? C3 C4 1.380(4) . ? C3 H3 0.94(3) . ? C4 C5 1.395(4) . ? C4 H4 0.86(4) . ? C5 C6 1.493(4) . ? C6 C7 1.388(4) . ? C7 C8 1.385(4) . ? C7 H7 0.91(4) . ? C8 C9 1.390(4) . ? C8 H8 0.88(4) . ? C9 C10 1.382(4) . ? C9 C12 1.446(4) . ? C10 H10 0.98(3) . ? B1 F2 1.374(4) . ? B1 F2 1.374(4) 2 ? B1 F1 1.388(4) 2 ? B1 F1 1.389(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 Ag1 Ag1 N2 0(10) 2 2 ? Ag1 Ag1 N2 0(10) 2 . ? N2 Ag1 N2 165.70(11) 2 . ? Ag1 Ag1 N1 0(10) 2 2 ? N2 Ag1 N1 71.12(8) 2 2 ? N2 Ag1 N1 114.57(8) . 2 ? Ag1 Ag1 N1 0(10) 2 . ? N2 Ag1 N1 114.57(8) 2 . ? N2 Ag1 N1 71.12(8) . . ? N1 Ag1 N1 136.50(11) 2 . ? C1 N1 C5 119.3(2) . . ? C1 N1 Ag1 124.1(2) . 2 ? C5 N1 Ag1 116.36(17) . 2 ? C1 N1 Ag1 124.1(2) . . ? C5 N1 Ag1 116.36(17) . . ? Ag1 N1 Ag1 0.000(15) 2 . ? C10 N2 C6 119.2(2) . . ? C10 N2 Ag1 122.64(18) . 2 ? C6 N2 Ag1 117.47(18) . 2 ? C10 N2 Ag1 122.64(18) . . ? C6 N2 Ag1 117.47(18) . . ? Ag1 N2 Ag1 0.000(16) 2 . ? N1 C1 C2 122.0(3) . . ? N1 C1 H1 120(2) . . ? C2 C1 H1 118(2) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 C11 121.3(3) . . ? C1 C2 C11 119.5(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 119(2) . . ? C2 C3 H3 123(2) . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 121(2) . . ? C5 C4 H4 120(2) . . ? N1 C5 C4 121.9(3) . . ? N1 C5 C6 117.3(2) . . ? C4 C5 C6 120.8(2) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 116.9(2) . . ? C7 C6 C5 121.8(2) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 119(2) . . ? C6 C7 H7 121(2) . . ? C7 C8 C9 117.8(3) . . ? C7 C8 H8 122(2) . . ? C9 C8 H8 121(2) . . ? C10 C9 C8 119.5(3) . . ? C10 C9 C12 120.6(3) . . ? C8 C9 C12 119.9(3) . . ? N2 C10 C9 122.3(3) . . ? N2 C10 H10 116(2) . . ? C9 C10 H10 122(2) . . ? N3 C11 C2 178.4(4) . . ? N4 C12 C9 178.8(4) . . ? F2 B1 F2 107.4(4) . 2 ? F2 B1 F1 109.31(15) . 2 ? F2 B1 F1 110.05(16) 2 2 ? F2 B1 F1 110.05(16) . . ? F2 B1 F1 109.31(15) 2 . ? F1 B1 F1 110.6(4) 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 Ag1 N1 C1 0(5) 2 . . . ? N2 Ag1 N1 C1 -13.0(3) 2 . . . ? N2 Ag1 N1 C1 -178.8(2) . . . . ? N1 Ag1 N1 C1 75.0(2) 2 . . . ? Ag1 Ag1 N1 C5 0(3) 2 . . . ? N2 Ag1 N1 C5 172.34(17) 2 . . . ? N2 Ag1 N1 C5 6.48(17) . . . . ? N1 Ag1 N1 C5 -99.67(18) 2 . . . ? N2 Ag1 N1 Ag1 0(49) 2 . . 2 ? N2 Ag1 N1 Ag1 0(100) . . . 2 ? N1 Ag1 N1 Ag1 0(100) 2 . . 2 ? Ag1 Ag1 N2 C10 0(9) 2 . . . ? N2 Ag1 N2 C10 65.9(2) 2 . . . ? N1 Ag1 N2 C10 -44.7(2) 2 . . . ? N1 Ag1 N2 C10 -178.1(2) . . . . ? Ag1 Ag1 N2 C6 0(12) 2 . . . ? N2 Ag1 N2 C6 -123.91(17) 2 . . . ? N1 Ag1 N2 C6 125.40(17) 2 . . . ? N1 Ag1 N2 C6 -7.96(17) . . . . ? N2 Ag1 N2 Ag1 0(79) 2 . . 2 ? N1 Ag1 N2 Ag1 0(100) 2 . . 2 ? N1 Ag1 N2 Ag1 0(95) . . . 2 ? C5 N1 C1 C2 -0.1(4) . . . . ? Ag1 N1 C1 C2 -174.7(2) 2 . . . ? Ag1 N1 C1 C2 -174.7(2) . . . . ? N1 C1 C2 C3 0.2(4) . . . . ? N1 C1 C2 C11 -178.8(3) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C11 C2 C3 C4 179.1(3) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C1 N1 C5 C4 -0.2(4) . . . . ? Ag1 N1 C5 C4 174.78(19) 2 . . . ? Ag1 N1 C5 C4 174.78(19) . . . . ? C1 N1 C5 C6 -179.5(2) . . . . ? Ag1 N1 C5 C6 -4.6(3) 2 . . . ? Ag1 N1 C5 C6 -4.6(3) . . . . ? C3 C4 C5 N1 0.4(4) . . . . ? C3 C4 C5 C6 179.7(2) . . . . ? C10 N2 C6 C7 -0.4(4) . . . . ? Ag1 N2 C6 C7 -170.92(19) 2 . . . ? Ag1 N2 C6 C7 -170.92(19) . . . . ? C10 N2 C6 C5 179.1(2) . . . . ? Ag1 N2 C6 C5 8.6(3) 2 . . . ? Ag1 N2 C6 C5 8.6(3) . . . . ? N1 C5 C6 N2 -2.6(3) . . . . ? C4 C5 C6 N2 178.0(2) . . . . ? N1 C5 C6 C7 176.9(2) . . . . ? C4 C5 C6 C7 -2.4(4) . . . . ? N2 C6 C7 C8 1.1(4) . . . . ? C5 C6 C7 C8 -178.4(2) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 -1.6(4) . . . . ? C7 C8 C9 C12 179.6(3) . . . . ? C6 N2 C10 C9 -1.3(4) . . . . ? Ag1 N2 C10 C9 168.7(2) 2 . . . ? Ag1 N2 C10 C9 168.7(2) . . . . ? C8 C9 C10 N2 2.3(4) . . . . ? C12 C9 C10 N2 -178.9(3) . . . . ? C3 C2 C11 N3 -16(14) . . . . ? C1 C2 C11 N3 163(14) . . . . ? C10 C9 C12 N4 177(100) . . . . ? C8 C9 C12 N4 -4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 31.16 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.562 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.098 #=END data_xd # number 10 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(\m-5,5'-dicyano-2,2'- bipyridine)(trifluoromethanesulfonato)silver(I)] ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H6 Ag F3 N4 O3 S' _chemical_formula_weight 463.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4946(5) _cell_length_b 15.8010(8) _cell_length_c 10.3381(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.242(2) _cell_angle_gamma 90.00 _cell_volume 1549.78(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.750361 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5664 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.1461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.92 _reflns_number_total 2813 _reflns_number_gt 1634 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Zortep/PLATON _computing_publication_material CIFTAB _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 ; w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2813 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.45679(6) 0.23539(3) 0.60789(6) 0.0369(2) Uani 1 d . . . S1 S 0.67914(19) 0.34259(9) 0.4056(2) 0.0327(5) Uani 1 d . . . N1 N 0.2796(5) 0.2381(3) 0.4428(6) 0.0263(14) Uani 1 d . . . C1 C 0.2299(6) 0.3083(3) 0.3845(7) 0.0290(17) Uani 1 d . . . H1 H 0.2763 0.3603 0.4036 0.035 Uiso 1 calc R . . O1 O 0.6978(6) 0.2714(2) 0.4912(5) 0.0470(15) Uani 1 d . . . F1 F 0.9171(5) 0.4021(3) 0.5036(6) 0.0743(17) Uani 1 d . . . N2 N 0.3618(5) 0.1007(3) 0.5816(6) 0.0243(13) Uani 1 d . . . O2 O 0.5385(5) 0.3765(3) 0.4035(6) 0.0568(16) Uani 1 d . . . C2 C 0.1171(6) 0.3093(3) 0.2998(7) 0.0266(17) Uani 1 d . . . F2 F 0.7339(6) 0.4461(3) 0.5994(5) 0.0708(18) Uani 1 d . . . O3 O 0.7400(6) 0.3361(3) 0.2817(6) 0.0549(17) Uani 1 d . . . N3 N 0.0508(6) 0.4543(3) 0.2016(7) 0.0422(18) Uani 1 d . . . F3 F 0.7828(6) 0.4958(2) 0.4142(6) 0.0739(19) Uani 1 d . . . C3 C 0.0463(7) 0.2339(4) 0.2683(8) 0.0358(19) Uani 1 d . . . H3 H -0.0333 0.2327 0.2096 0.043 Uiso 1 calc R . . C4 C 0.0992(7) 0.1600(3) 0.3281(8) 0.0353(19) Uani 1 d . . . H4 H 0.0553 0.1070 0.3105 0.042 Uiso 1 calc R . . N4 N 0.4853(6) -0.1684(3) 0.7521(6) 0.0321(15) Uani 1 d . . . C5 C 0.2138(6) 0.1645(3) 0.4115(7) 0.0252(16) Uani 1 d . . . C6 C 0.2753(7) 0.0873(3) 0.4792(7) 0.0241(16) Uani 1 d . . . C7 C 0.2390(6) 0.0063(3) 0.4317(7) 0.0282(17) Uani 1 d . . . H7 H 0.1817 -0.0010 0.3551 0.034 Uiso 1 calc R . . C8 C 0.2916(7) -0.0632(3) 0.5032(7) 0.0288(17) Uani 1 d . . . H8 H 0.2692 -0.1194 0.4770 0.035 Uiso 1 calc R . . C9 C 0.3756(6) -0.0485(3) 0.6111(7) 0.0277(17) Uani 1 d . . . C10 C 0.4098(7) 0.0340(3) 0.6490(7) 0.0275(17) Uani 1 d . . . H10 H 0.4684 0.0428 0.7244 0.033 Uiso 1 calc R . . C11 C 0.0746(7) 0.3891(3) 0.2442(8) 0.0305(18) Uani 1 d . . . C12 C 0.4363(7) -0.1167(3) 0.6920(7) 0.0264(17) Uani 1 d . . . C13 C 0.7818(9) 0.4255(4) 0.4852(9) 0.044(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0482(3) 0.0263(2) 0.0354(4) -0.0075(2) -0.0090(3) -0.0079(2) S1 0.0422(11) 0.0268(8) 0.0285(15) 0.0034(7) -0.0055(10) -0.0056(7) N1 0.031(3) 0.021(2) 0.028(4) 0.004(2) -0.002(3) 0.000(2) C1 0.028(4) 0.021(3) 0.038(6) 0.004(3) -0.003(4) -0.001(2) O1 0.078(4) 0.027(2) 0.035(4) 0.005(2) -0.005(3) 0.002(2) F1 0.040(3) 0.102(4) 0.080(5) -0.011(3) -0.007(3) -0.019(3) N2 0.027(3) 0.022(2) 0.023(4) 0.002(2) -0.003(3) 0.002(2) O2 0.037(3) 0.061(3) 0.071(5) 0.016(3) -0.014(3) -0.003(2) C2 0.026(4) 0.022(3) 0.033(5) 0.006(3) 0.004(3) 0.004(2) F2 0.093(4) 0.077(3) 0.044(4) -0.031(3) 0.025(3) -0.040(3) O3 0.094(5) 0.050(3) 0.022(4) -0.006(2) 0.016(4) -0.026(3) N3 0.033(3) 0.033(3) 0.060(6) 0.010(3) -0.001(3) 0.004(2) F3 0.111(4) 0.034(2) 0.078(5) -0.002(2) 0.021(4) -0.026(2) C3 0.036(4) 0.032(3) 0.039(6) 0.005(3) -0.009(4) 0.003(3) C4 0.034(4) 0.024(3) 0.047(6) 0.005(3) -0.011(4) 0.001(3) N4 0.043(3) 0.025(3) 0.028(5) 0.001(2) -0.005(3) 0.005(2) C5 0.028(4) 0.020(3) 0.028(5) 0.004(2) 0.001(3) -0.001(2) C6 0.028(4) 0.020(3) 0.025(5) 0.002(2) 0.008(3) 0.000(2) C7 0.031(4) 0.020(3) 0.033(6) 0.000(3) -0.005(3) -0.002(2) C8 0.034(4) 0.019(3) 0.033(5) 0.002(3) -0.001(4) -0.002(2) C9 0.026(4) 0.019(3) 0.038(6) 0.002(3) 0.003(3) 0.003(2) C10 0.028(4) 0.026(3) 0.028(6) -0.004(3) -0.004(3) 0.001(2) C11 0.023(3) 0.030(3) 0.038(6) 0.007(3) 0.003(3) 0.001(3) C12 0.034(4) 0.024(3) 0.022(5) 0.000(3) 0.006(3) 0.004(2) C13 0.055(6) 0.045(4) 0.032(7) -0.005(3) 0.010(5) -0.007(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 N4 2.156(5) 2_656 ? Ag1 N2 2.322(4) . ? Ag1 N1 2.349(6) . ? Ag1 O1 2.689(5) . ? S1 O3 1.430(5) . ? S1 O1 1.438(5) . ? S1 O2 1.438(5) . ? S1 C13 1.811(8) . ? N1 C1 1.339(7) . ? N1 C5 1.354(7) . ? C1 C2 1.357(10) . ? F1 C13 1.343(9) . ? N2 C6 1.331(9) . ? N2 C10 1.334(8) . ? C2 C3 1.401(8) . ? C2 C11 1.438(8) . ? F2 C13 1.323(9) . ? N3 C11 1.139(7) . ? F3 C13 1.331(9) . ? C3 C4 1.405(9) . ? C4 C5 1.363(10) . ? N4 C12 1.116(8) . ? N4 Ag1 2.156(5) 2_646 ? C5 C6 1.512(8) . ? C6 C7 1.409(8) . ? C7 C8 1.404(9) . ? C8 C9 1.365(10) . ? C9 C10 1.396(8) . ? C9 C12 1.468(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N2 144.3(2) 2_656 . ? N4 Ag1 N1 129.18(19) 2_656 . ? N2 Ag1 N1 70.61(17) . . ? N4 Ag1 O1 87.30(18) 2_656 . ? N2 Ag1 O1 118.33(15) . . ? N1 Ag1 O1 105.53(17) . . ? O3 S1 O1 116.8(3) . . ? O3 S1 O2 114.9(4) . . ? O1 S1 O2 113.1(3) . . ? O3 S1 C13 103.3(3) . . ? O1 S1 C13 103.6(4) . . ? O2 S1 C13 102.7(3) . . ? C1 N1 C5 116.9(6) . . ? C1 N1 Ag1 124.9(4) . . ? C5 N1 Ag1 118.0(4) . . ? N1 C1 C2 123.8(5) . . ? S1 O1 Ag1 110.8(3) . . ? C6 N2 C10 118.4(5) . . ? C6 N2 Ag1 117.6(4) . . ? C10 N2 Ag1 122.7(5) . . ? C1 C2 C3 120.0(5) . . ? C1 C2 C11 118.1(5) . . ? C3 C2 C11 121.9(7) . . ? C2 C3 C4 116.3(7) . . ? C5 C4 C3 119.9(6) . . ? C12 N4 Ag1 168.3(6) . 2_646 ? N1 C5 C4 123.0(5) . . ? N1 C5 C6 114.6(6) . . ? C4 C5 C6 122.4(5) . . ? N2 C6 C7 123.9(6) . . ? N2 C6 C5 117.0(5) . . ? C7 C6 C5 119.1(7) . . ? C8 C7 C6 116.7(7) . . ? C9 C8 C7 118.8(5) . . ? C8 C9 C10 120.7(6) . . ? C8 C9 C12 123.0(5) . . ? C10 C9 C12 116.3(7) . . ? N2 C10 C9 121.4(7) . . ? N3 C11 C2 175.0(7) . . ? N4 C12 C9 178.4(7) . . ? F2 C13 F3 107.3(6) . . ? F2 C13 F1 107.6(8) . . ? F3 C13 F1 106.3(6) . . ? F2 C13 S1 112.7(5) . . ? F3 C13 S1 111.6(7) . . ? F1 C13 S1 111.1(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 N4 Ag1 N1 C1 27.0(6) 2_656 . . . ? N2 Ag1 N1 C1 172.5(5) . . . . ? O1 Ag1 N1 C1 -72.4(5) . . . . ? N4 Ag1 N1 C5 -146.9(4) 2_656 . . . ? N2 Ag1 N1 C5 -1.4(4) . . . . ? O1 Ag1 N1 C5 113.7(4) . . . . ? C5 N1 C1 C2 1.6(10) . . . . ? Ag1 N1 C1 C2 -172.4(5) . . . . ? O3 S1 O1 Ag1 -136.8(3) . . . . ? O2 S1 O1 Ag1 0.0(4) . . . . ? C13 S1 O1 Ag1 110.5(3) . . . . ? N4 Ag1 O1 S1 -83.9(3) 2_656 . . . ? N2 Ag1 O1 S1 122.2(3) . . . . ? N1 Ag1 O1 S1 46.2(3) . . . . ? N4 Ag1 N2 C6 141.3(5) 2_656 . . . ? N1 Ag1 N2 C6 10.1(4) . . . . ? O1 Ag1 N2 C6 -87.5(5) . . . . ? N4 Ag1 N2 C10 -51.6(6) 2_656 . . . ? N1 Ag1 N2 C10 177.2(5) . . . . ? O1 Ag1 N2 C10 79.6(5) . . . . ? N1 C1 C2 C3 -0.4(11) . . . . ? N1 C1 C2 C11 179.9(6) . . . . ? C1 C2 C3 C4 -0.3(10) . . . . ? C11 C2 C3 C4 179.3(7) . . . . ? C2 C3 C4 C5 -0.1(10) . . . . ? C1 N1 C5 C4 -2.0(10) . . . . ? Ag1 N1 C5 C4 172.4(5) . . . . ? C1 N1 C5 C6 179.4(5) . . . . ? Ag1 N1 C5 C6 -6.2(7) . . . . ? C3 C4 C5 N1 1.3(11) . . . . ? C3 C4 C5 C6 179.8(6) . . . . ? C10 N2 C6 C7 -4.8(9) . . . . ? Ag1 N2 C6 C7 162.9(5) . . . . ? C10 N2 C6 C5 175.2(5) . . . . ? Ag1 N2 C6 C5 -17.1(7) . . . . ? N1 C5 C6 N2 15.4(8) . . . . ? C4 C5 C6 N2 -163.2(7) . . . . ? N1 C5 C6 C7 -164.6(6) . . . . ? C4 C5 C6 C7 16.8(9) . . . . ? N2 C6 C7 C8 4.1(10) . . . . ? C5 C6 C7 C8 -175.9(5) . . . . ? C6 C7 C8 C9 -1.2(9) . . . . ? C7 C8 C9 C10 -0.7(10) . . . . ? C7 C8 C9 C12 -179.7(6) . . . . ? C6 N2 C10 C9 2.6(9) . . . . ? Ag1 N2 C10 C9 -164.4(4) . . . . ? C8 C9 C10 N2 0.0(10) . . . . ? C12 C9 C10 N2 179.2(6) . . . . ? C1 C2 C11 N3 26(10) . . . . ? C3 C2 C11 N3 -154(9) . . . . ? Ag1 N4 C12 C9 168(26) 2_646 . . . ? C8 C9 C12 N4 97(29) . . . . ? C10 C9 C12 N4 -82(29) . . . . ? O3 S1 C13 F2 174.9(6) . . . . ? O1 S1 C13 F2 -62.8(7) . . . . ? O2 S1 C13 F2 55.1(7) . . . . ? O3 S1 C13 F3 54.1(6) . . . . ? O1 S1 C13 F3 176.3(5) . . . . ? O2 S1 C13 F3 -65.7(6) . . . . ? O3 S1 C13 F1 -64.3(7) . . . . ? O1 S1 C13 F1 57.9(7) . . . . ? O2 S1 C13 F1 175.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.690 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.690 _refine_diff_density_max 0.616 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.138 #=END data_xe # number 13 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(\m3-5,5'-dicyano-2,2'bipyridine)silver(I)]-hexafluorophosphate- hemitoluene-solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H10 Ag F6 N4 P' _chemical_formula_weight 505.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 17.8017(3) _cell_length_b 17.80170(10) _cell_length_c 19.61420(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5383.00(10) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.515140 _exptl_absorpt_correction_T_max 0.730196 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22491 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.21 _reflns_number_total 5094 _reflns_number_gt 3491 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON _computing_publication_material SHELX-97 _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 ; w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+72.8003P] 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 5094 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2037 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.217 _refine_ls_shift/su_mean 0.013 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 0.86443(3) 0.19968(3) 0.61047(4) 0.03584(19) Uani 1 d . . . N1 N 1.0155(4) 0.2601(4) 0.5904(3) 0.0256(12) Uani 1 d . . . N2 N 0.9321(4) 0.3514(4) 0.5751(4) 0.0291(13) Uani 1 d . . . N3 N 1.2156(5) 0.1542(5) 0.5833(5) 0.0480(19) Uani 1 d . . . N4 N 0.8442(6) 0.5640(5) 0.6011(5) 0.053(2) Uani 1 d . . . C1 C 1.0533(5) 0.2118(5) 0.5932(4) 0.0329(17) Uani 1 d . . . H1 H 1.0192 0.1517 0.6032 0.039 Uiso 1 calc R . . C2 C 1.1422(5) 0.2477(5) 0.5818(4) 0.0289(15) Uani 1 d . . . C3 C 1.1922(5) 0.3347(5) 0.5671(5) 0.0358(17) Uani 1 d . . . H3 H 1.2524 0.3595 0.5577 0.043 Uiso 1 calc R . . C4 C 1.1531(4) 0.3852(4) 0.5662(4) 0.0307(16) Uani 1 d . . . H4 H 1.1861 0.4456 0.5573 0.037 Uiso 1 calc R . . C5 C 1.0646(4) 0.3454(4) 0.5788(4) 0.0244(14) Uani 1 d . . . C6 C 1.0191(4) 0.3967(4) 0.5822(4) 0.0246(14) Uani 1 d . . . C7 C 1.0652(5) 0.4851(4) 0.5924(4) 0.0345(17) Uani 1 d . . . H7 H 1.1268 0.5152 0.5950 0.041 Uiso 1 calc R . . C8 C 1.0180(5) 0.5305(5) 0.5991(4) 0.0352(18) Uani 1 d . . . H8 H 1.0470 0.5908 0.6092 0.042 Uiso 1 calc R . . C9 C 0.9301(6) 0.4845(5) 0.5905(4) 0.0348(17) Uani 1 d . . . C10 C 0.8889(5) 0.3947(5) 0.5798(5) 0.0348(17) Uani 1 d . . . H10 H 0.8275 0.3632 0.5756 0.042 Uiso 1 calc R . . C11 C 1.1815(5) 0.1936(5) 0.5841(5) 0.0363(18) Uani 1 d . . . C12 C 0.8810(6) 0.5266(5) 0.5970(5) 0.041(2) Uani 1 d . . . C13 C 0.8620(14) 0.3055(15) 0.7500 0.074(5) Uani 1 d S . . C14 C 0.9519(14) 0.3677(11) 0.7500 0.075(6) Uani 1 d S . . H14 H 0.9699 0.4278 0.7500 0.090 Uiso 1 calc SR . . C15 C 1.0129(14) 0.3425(15) 0.7500 0.076(5) Uani 1 d S . . H15 H 1.0724 0.3860 0.7500 0.092 Uiso 1 calc SR . . C16 C 0.9932(16) 0.2619(16) 0.7500 0.082(6) Uani 1 d S . . H16 H 1.0367 0.2459 0.7500 0.098 Uiso 1 calc SR . . C17 C 0.9047(15) 0.1993(14) 0.7500 0.075(5) Uani 1 d S . . H17 H 0.8887 0.1397 0.7500 0.090 Uiso 1 calc SR . . C18 C 0.8418(11) 0.2197(12) 0.7500 0.065(5) Uani 1 d S . . H18 H 0.7828 0.1749 0.7500 0.078 Uiso 1 calc SR . . C19 C 0.793(2) 0.335(2) 0.7500 0.135(11) Uani 1 d S . . H19A H 0.8226 0.3987 0.7502 0.203 Uiso 1 calc SR . . H19B H 0.7566 0.3125 0.7907 0.203 Uiso 0.50 calc PR . . H19C H 0.7570 0.3130 0.7091 0.203 Uiso 0.50 calc PR . . P1 P 0.6667 0.3333 0.4674(3) 0.0429(10) Uani 1 d S . . F1 F 0.7371(5) 0.4107(5) 0.5079(5) 0.103(3) Uani 1 d . . . F2 F 0.6590(7) 0.4013(7) 0.4214(7) 0.153(5) Uani 1 d . . . P2 P 1.3050(3) 0.3720(3) 0.7500 0.0639(12) Uani 1 d S . . F3 F 1.2028(6) 0.3206(9) 0.7500 0.099(4) Uani 1 d S . . F4 F 1.3019(6) 0.4350(6) 0.6935(4) 0.096(3) Uani 1 d . . . F5 F 1.4088(6) 0.4268(10) 0.7500 0.107(5) Uani 1 d S . . F6 F 1.3088(6) 0.3147(7) 0.6912(5) 0.112(3) Uani 1 d . . . P3 P 1.0000 0.0000 0.7500 0.0566(17) Uani 1 d S . . F7 F 1.0000 0.0000 0.6785(14) 0.33(2) Uani 1 d S . . F8 F 0.928(6) -0.096(4) 0.7500 0.22(4) Uani 0.44 d SP . . F9 F 1.052(6) -0.044(10) 0.7500 0.27(5) Uani 0.44 d SP . . F10 F 0.995(6) -0.081(4) 0.7500 0.35(7) Uani 0.44 d SP . . 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 0.0178(2) 0.0215(3) 0.0659(4) -0.0029(3) 0.0013(3) 0.0080(2) N1 0.020(3) 0.017(2) 0.040(3) 0.001(2) 0.002(2) 0.009(2) N2 0.024(3) 0.024(3) 0.044(4) -0.006(3) -0.006(3) 0.016(2) N3 0.043(4) 0.049(4) 0.068(5) 0.003(4) -0.001(4) 0.035(4) N4 0.061(5) 0.054(5) 0.067(6) -0.012(4) -0.013(4) 0.045(4) C1 0.031(4) 0.022(3) 0.046(5) -0.001(3) 0.000(3) 0.014(3) C2 0.024(3) 0.035(4) 0.031(4) -0.002(3) -0.002(3) 0.017(3) C3 0.019(3) 0.036(4) 0.054(5) 0.005(4) 0.003(3) 0.014(3) C4 0.019(3) 0.022(3) 0.049(5) 0.006(3) 0.004(3) 0.008(3) C5 0.025(3) 0.020(3) 0.028(4) 0.000(3) 0.000(3) 0.011(3) C6 0.022(3) 0.017(3) 0.034(4) 0.002(3) -0.004(3) 0.009(2) C7 0.029(3) 0.018(3) 0.051(5) -0.002(3) 0.000(3) 0.007(3) C8 0.042(4) 0.020(3) 0.046(5) 0.005(3) -0.009(4) 0.017(3) C9 0.052(5) 0.029(4) 0.037(4) 0.002(3) -0.006(4) 0.030(4) C10 0.027(3) 0.034(4) 0.051(5) -0.006(4) -0.007(3) 0.022(3) C11 0.030(4) 0.036(4) 0.050(5) -0.001(4) 0.000(4) 0.022(3) C12 0.053(5) 0.038(4) 0.046(5) -0.006(4) -0.006(4) 0.035(4) C13 0.094(14) 0.112(16) 0.026(7) 0.000 0.000 0.060(13) C14 0.106(15) 0.045(9) 0.043(9) 0.000 0.000 0.015(10) C15 0.078(12) 0.101(16) 0.031(8) 0.000 0.000 0.031(12) C16 0.113(18) 0.103(16) 0.035(8) 0.000 0.000 0.057(15) C17 0.108(16) 0.084(13) 0.029(7) 0.000 0.000 0.045(13) C18 0.055(9) 0.069(11) 0.041(8) 0.000 0.000 0.008(8) C19 0.15(3) 0.20(3) 0.095(19) 0.000 0.000 0.12(3) P1 0.0279(10) 0.0279(10) 0.073(3) 0.000 0.000 0.0140(5) F1 0.070(5) 0.070(5) 0.154(8) -0.029(5) -0.061(5) 0.024(4) F2 0.119(8) 0.116(8) 0.224(13) 0.069(8) -0.042(8) 0.059(7) P2 0.0396(19) 0.101(4) 0.038(2) 0.000 0.000 0.025(2) F3 0.042(5) 0.135(11) 0.100(9) 0.000 0.000 0.028(6) F4 0.100(6) 0.138(8) 0.062(4) 0.017(5) 0.003(4) 0.068(6) F5 0.046(5) 0.173(13) 0.060(6) 0.000 0.000 0.023(7) F6 0.096(6) 0.157(9) 0.101(6) -0.055(6) -0.022(5) 0.078(6) P3 0.049(2) 0.049(2) 0.072(5) 0.000 0.000 0.0244(11) F7 0.45(4) 0.45(4) 0.090(19) 0.000 0.000 0.223(19) F8 0.15(7) 0.04(2) 0.33(8) 0.000 0.000 -0.05(3) F9 0.07(3) 0.31(11) 0.46(12) 0.000 0.000 0.13(5) F10 0.09(3) 0.06(3) 0.9(2) 0.000 0.000 0.03(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 N4 2.294(7) 3_665 ? Ag1 N3 2.375(7) 2_645 ? Ag1 N1 2.377(6) . ? Ag1 N2 2.444(6) . ? N1 C1 1.333(9) . ? N1 C5 1.340(8) . ? N2 C10 1.338(9) . ? N2 C6 1.348(8) . ? N3 C11 1.134(10) . ? N3 Ag1 2.375(7) 3_765 ? N4 C12 1.146(10) . ? N4 Ag1 2.294(7) 2_655 ? C1 C2 1.396(10) . ? C1 H1 0.9500 . ? C2 C3 1.376(11) . ? C2 C11 1.448(10) . ? C3 C4 1.385(10) . ? C3 H3 0.9500 . ? C4 C5 1.390(9) . ? C4 H4 0.9500 . ? C5 C6 1.494(9) . ? C6 C7 1.378(9) . ? C7 C8 1.433(10) . ? C7 H7 0.9500 . ? C8 C9 1.366(12) . ? C8 H8 0.9500 . ? C9 C10 1.402(11) . ? C9 C12 1.414(10) . ? C10 H10 0.9500 . ? C13 C18 1.38(3) . ? C13 C14 1.42(3) . ? C13 C19 1.56(3) . ? C14 C15 1.37(3) . ? C14 H14 0.9500 . ? C15 C16 1.29(3) . ? C15 H15 0.9500 . ? C16 C17 1.40(3) . ? C16 H16 0.9500 . ? C17 C18 1.34(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9802 . ? C19 H19B 0.9802 . ? C19 H19C 0.9802 . ? P1 F1 1.539(7) 3_665 ? P1 F1 1.539(7) . ? P1 F1 1.539(7) 2_655 ? P1 F2 1.569(9) 3_665 ? P1 F2 1.569(9) 2_655 ? P1 F2 1.569(9) . ? P2 F6 1.564(9) . ? P2 F6 1.564(9) 10_557 ? P2 F3 1.576(10) . ? P2 F4 1.596(9) . ? P2 F4 1.596(9) 10_557 ? P2 F5 1.601(11) . ? P3 F10 1.40(4) . ? P3 F10 1.40(4) 2_645 ? P3 F10 1.40(4) 3_765 ? P3 F7 1.40(3) . ? P3 F7 1.40(3) 10_557 ? P3 F9 1.49(8) 2_645 ? P3 F9 1.49(7) 3_765 ? P3 F9 1.49(7) . ? P3 F8 1.54(4) 3_765 ? P3 F8 1.54(4) . ? P3 F8 1.54(4) 2_645 ? F8 F9 1.08(11) 3_765 ? F8 F10 1.07(9) . ? F9 F10 0.90(6) . ? F9 F8 1.08(11) 2_645 ? 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 N3 94.5(3) 3_665 2_645 ? N4 Ag1 N1 164.6(3) 3_665 . ? N3 Ag1 N1 88.4(2) 2_645 . ? N4 Ag1 N2 101.7(3) 3_665 . ? N3 Ag1 N2 144.9(3) 2_645 . ? N1 Ag1 N2 68.38(19) . . ? C1 N1 C5 119.1(6) . . ? C1 N1 Ag1 121.6(5) . . ? C5 N1 Ag1 119.3(4) . . ? C10 N2 C6 117.8(6) . . ? C10 N2 Ag1 120.6(5) . . ? C6 N2 Ag1 114.6(4) . . ? C11 N3 Ag1 151.4(8) . 3_765 ? C12 N4 Ag1 167.5(8) . 2_655 ? N1 C1 C2 121.3(7) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.9(7) . . ? C3 C2 C11 119.9(7) . . ? C1 C2 C11 120.3(7) . . ? C2 C3 C4 118.6(7) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 118.6(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.5(6) . . ? N1 C5 C6 116.1(6) . . ? C4 C5 C6 121.4(6) . . ? N2 C6 C7 123.3(6) . . ? N2 C6 C5 116.1(6) . . ? C7 C6 C5 120.6(6) . . ? C6 C7 C8 118.3(7) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 118.0(7) . . ? C9 C8 H8 121.0 . . ? C7 C8 H8 121.0 . . ? C8 C9 C10 119.5(7) . . ? C8 C9 C12 119.9(7) . . ? C10 C9 C12 120.5(8) . . ? N2 C10 C9 122.9(7) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N3 C11 C2 176.1(10) . . ? N4 C12 C9 176.9(11) . . ? C18 C13 C14 115.5(18) . . ? C18 C13 C19 124(2) . . ? C14 C13 C19 120(2) . . ? C15 C14 C13 121.0(18) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 123(2) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 C16 C17 117(2) . . ? C15 C16 H16 121.5 . . ? C17 C16 H16 121.5 . . ? C18 C17 C16 123(2) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C13 120.6(18) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F1 P1 F1 95.9(6) 3_665 . ? F1 P1 F1 95.9(6) 3_665 2_655 ? F1 P1 F1 95.9(6) . 2_655 ? F1 P1 F2 87.3(5) 3_665 3_665 ? F1 P1 F2 86.5(6) . 3_665 ? F1 P1 F2 175.8(7) 2_655 3_665 ? F1 P1 F2 86.5(6) 3_665 2_655 ? F1 P1 F2 175.8(7) . 2_655 ? F1 P1 F2 87.3(5) 2_655 2_655 ? F2 P1 F2 90.2(8) 3_665 2_655 ? F1 P1 F2 175.8(7) 3_665 . ? F1 P1 F2 87.3(5) . . ? F1 P1 F2 86.5(6) 2_655 . ? F2 P1 F2 90.2(8) 3_665 . ? F2 P1 F2 90.2(8) 2_655 . ? F6 P2 F6 95.0(9) . 10_557 ? F6 P2 F3 92.0(5) . . ? F6 P2 F3 92.0(5) 10_557 . ? F6 P2 F4 88.5(5) . . ? F6 P2 F4 176.4(6) 10_557 . ? F3 P2 F4 88.4(5) . . ? F6 P2 F4 176.4(6) . 10_557 ? F6 P2 F4 88.5(5) 10_557 10_557 ? F3 P2 F4 88.4(5) . 10_557 ? F4 P2 F4 87.9(7) . 10_557 ? F6 P2 F5 89.1(5) . . ? F6 P2 F5 89.1(5) 10_557 . ? F3 P2 F5 178.4(9) . . ? F4 P2 F5 90.4(6) . . ? F4 P2 F5 90.4(6) 10_557 . ? F10 P3 F10 120.00(3) . 2_645 ? F10 P3 F10 120.00(4) . 3_765 ? F10 P3 F10 120.00(3) 2_645 3_765 ? F10 P3 F7 90.000(3) . . ? F10 P3 F7 90.002(7) 2_645 . ? F10 P3 F7 90.001(5) 3_765 . ? F10 P3 F7 90.000(3) . 10_557 ? F10 P3 F7 89.998(6) 2_645 10_557 ? F10 P3 F7 89.999(4) 3_765 10_557 ? F7 P3 F7 180.000(6) . 10_557 ? F10 P3 F9 156(3) . 2_645 ? F10 P3 F9 36(3) 2_645 2_645 ? F10 P3 F9 84(3) 3_765 2_645 ? F7 P3 F9 90.00(5) . 2_645 ? F7 P3 F9 90.00(5) 10_557 2_645 ? F10 P3 F9 84(3) . 3_765 ? F10 P3 F9 156(3) 2_645 3_765 ? F10 P3 F9 36(3) 3_765 3_765 ? F7 P3 F9 90.00(2) . 3_765 ? F7 P3 F9 90.00(2) 10_557 3_765 ? F9 P3 F9 120.01(3) 2_645 3_765 ? F10 P3 F9 36(3) . . ? F10 P3 F9 84(3) 2_645 . ? F10 P3 F9 156(3) 3_765 . ? F7 P3 F9 90.000(7) . . ? F7 P3 F9 90.000(4) 10_557 . ? F9 P3 F9 120.00(6) 2_645 . ? F9 P3 F9 120.00(8) 3_765 . ? F10 P3 F8 162(3) . 3_765 ? F10 P3 F8 78(3) 2_645 3_765 ? F10 P3 F8 42(3) 3_765 3_765 ? F7 P3 F8 90.001(13) . 3_765 ? F7 P3 F8 89.999(12) 10_557 3_765 ? F9 P3 F8 42(4) 2_645 3_765 ? F9 P3 F8 78(4) 3_765 3_765 ? F9 P3 F8 162(4) . 3_765 ? F10 P3 F8 42(3) . . ? F10 P3 F8 162(3) 2_645 . ? F10 P3 F8 78(3) 3_765 . ? F7 P3 F8 90.00(2) . . ? F7 P3 F8 90.00(2) 10_557 . ? F9 P3 F8 162(4) 2_645 . ? F9 P3 F8 42(4) 3_765 . ? F9 P3 F8 78(4) . . ? F8 P3 F8 120.00(4) 3_765 . ? F10 P3 F8 78(3) . 2_645 ? F10 P3 F8 42(3) 2_645 2_645 ? F10 P3 F8 162(3) 3_765 2_645 ? F7 P3 F8 90.00(4) . 2_645 ? F7 P3 F8 90.00(3) 10_557 2_645 ? F9 P3 F8 78(4) 2_645 2_645 ? F9 P3 F8 162(4) 3_765 2_645 ? F9 P3 F8 42(4) . 2_645 ? F8 P3 F8 120.00(3) 3_765 2_645 ? F8 P3 F8 120.000(15) . 2_645 ? F9 F8 F10 128(7) 3_765 . ? F9 F8 P3 66(4) 3_765 . ? F10 F8 P3 62(4) . . ? F10 F9 F8 138(10) . 2_645 ? F10 F9 P3 67(4) . . ? F8 F9 P3 72(7) 2_645 . ? F9 F10 F8 153(8) . . ? F9 F10 P3 78(6) . . ? F8 F10 P3 76(4) . . ? 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 C1 -122.6(11) 3_665 . . . ? N3 Ag1 N1 C1 -21.6(6) 2_645 . . . ? N2 Ag1 N1 C1 -174.6(7) . . . . ? N4 Ag1 N1 C5 60.1(12) 3_665 . . . ? N3 Ag1 N1 C5 161.1(6) 2_645 . . . ? N2 Ag1 N1 C5 8.1(5) . . . . ? N4 Ag1 N2 C10 23.5(7) 3_665 . . . ? N3 Ag1 N2 C10 139.1(6) 2_645 . . . ? N1 Ag1 N2 C10 -168.9(7) . . . . ? N4 Ag1 N2 C6 173.7(6) 3_665 . . . ? N3 Ag1 N2 C6 -70.7(7) 2_645 . . . ? N1 Ag1 N2 C6 -18.7(5) . . . . ? C5 N1 C1 C2 -2.3(12) . . . . ? Ag1 N1 C1 C2 -179.6(6) . . . . ? N1 C1 C2 C3 -0.3(13) . . . . ? N1 C1 C2 C11 -179.1(8) . . . . ? C1 C2 C3 C4 2.1(13) . . . . ? C11 C2 C3 C4 -179.1(8) . . . . ? C2 C3 C4 C5 -1.4(13) . . . . ? C1 N1 C5 C4 3.1(12) . . . . ? Ag1 N1 C5 C4 -179.6(6) . . . . ? C1 N1 C5 C6 -175.0(7) . . . . ? Ag1 N1 C5 C6 2.3(9) . . . . ? C3 C4 C5 N1 -1.2(12) . . . . ? C3 C4 C5 C6 176.8(7) . . . . ? C10 N2 C6 C7 -1.5(12) . . . . ? Ag1 N2 C6 C7 -152.6(6) . . . . ? C10 N2 C6 C5 178.1(7) . . . . ? Ag1 N2 C6 C5 27.0(8) . . . . ? N1 C5 C6 N2 -20.2(10) . . . . ? C4 C5 C6 N2 161.7(7) . . . . ? N1 C5 C6 C7 159.5(7) . . . . ? C4 C5 C6 C7 -18.6(12) . . . . ? N2 C6 C7 C8 3.1(13) . . . . ? C5 C6 C7 C8 -176.6(7) . . . . ? C6 C7 C8 C9 -4.2(12) . . . . ? C7 C8 C9 C10 3.9(13) . . . . ? C7 C8 C9 C12 179.7(8) . . . . ? C6 N2 C10 C9 1.1(13) . . . . ? Ag1 N2 C10 C9 150.4(7) . . . . ? C8 C9 C10 N2 -2.4(14) . . . . ? C12 C9 C10 N2 -178.2(8) . . . . ? Ag1 N3 C11 C2 72(15) 3_765 . . . ? C3 C2 C11 N3 -29(15) . . . . ? C1 C2 C11 N3 150(14) . . . . ? Ag1 N4 C12 C9 -25(22) 2_655 . . . ? C8 C9 C12 N4 33(19) . . . . ? C10 C9 C12 N4 -151(18) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C19 C13 C14 C15 180.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C19 C13 C18 C17 180.0 . . . . ? F10 P3 F8 F9 179.998(2) . . . 3_765 ? F10 P3 F8 F9 179.993(4) 2_645 . . 3_765 ? F10 P3 F8 F9 -0.001(1) 3_765 . . 3_765 ? F7 P3 F8 F9 -90.002(2) . . . 3_765 ? F7 P3 F8 F9 89.998(1) 10_557 . . 3_765 ? F9 P3 F8 F9 0.002(2) 2_645 . . 3_765 ? F9 P3 F8 F9 179.998(1) . . . 3_765 ? F8 P3 F8 F9 -0.001(1) 3_765 . . 3_765 ? F8 P3 F8 F9 179.996(1) 2_645 . . 3_765 ? F10 P3 F8 F10 -0.005(4) 2_645 . . . ? F10 P3 F8 F10 180.002(2) 3_765 . . . ? F7 P3 F8 F10 90.000(7) . . . . ? F7 P3 F8 F10 -90.000(2) 10_557 . . . ? F9 P3 F8 F10 180.005(4) 2_645 . . . ? F9 P3 F8 F10 180.002(3) 3_765 . . . ? F9 P3 F8 F10 0.000(2) . . . . ? F8 P3 F8 F10 180.002(2) 3_765 . . . ? F8 P3 F8 F10 -0.002(2) 2_645 . . . ? F10 P3 F9 F10 179.998(2) 2_645 . . . ? F10 P3 F9 F10 0.004(2) 3_765 . . . ? F7 P3 F9 F10 -90.000(10) . . . . ? F7 P3 F9 F10 90.000(4) 10_557 . . . ? F9 P3 F9 F10 179.998(6) 2_645 . . . ? F9 P3 F9 F10 0.002(2) 3_765 . . . ? F8 P3 F9 F10 179.996(9) 3_765 . . . ? F8 P3 F9 F10 0.000(2) . . . . ? F8 P3 F9 F10 179.998(2) 2_645 . . . ? F10 P3 F9 F8 180.002(2) . . . 2_645 ? F10 P3 F9 F8 0.001(3) 2_645 . . 2_645 ? F10 P3 F9 F8 -179.994(6) 3_765 . . 2_645 ? F7 P3 F9 F8 90.002(18) . . . 2_645 ? F7 P3 F9 F8 -89.998(10) 10_557 . . 2_645 ? F9 P3 F9 F8 0.000(3) 2_645 . . 2_645 ? F9 P3 F9 F8 180.004(4) 3_765 . . 2_645 ? F8 P3 F9 F8 -0.002(6) 3_765 . . 2_645 ? F8 P3 F9 F8 180.002(3) . . . 2_645 ? F8 F9 F10 F8 0.003(7) 2_645 . . . ? P3 F9 F10 F8 0.000(3) . . . . ? F8 F9 F10 P3 0.003(3) 2_645 . . . ? F9 F8 F10 F9 -0.003(5) 3_765 . . . ? P3 F8 F10 F9 0.000(6) . . . . ? F9 F8 F10 P3 -0.003(2) 3_765 . . . ? F10 P3 F10 F9 -0.002(4) 2_645 . . . ? F10 P3 F10 F9 180.002(6) 3_765 . . . ? F7 P3 F10 F9 90.00(2) . . . . ? F7 P3 F10 F9 -90.000(6) 10_557 . . . ? F9 P3 F10 F9 -0.003(2) 2_645 . . . ? F9 P3 F10 F9 180.001(4) 3_765 . . . ? F8 P3 F10 F9 180.005(8) 3_765 . . . ? F8 P3 F10 F9 180.000(3) . . . . ? F8 P3 F10 F9 -0.001(4) 2_645 . . . ? F10 P3 F10 F8 179.998(2) 2_645 . . . ? F10 P3 F10 F8 0.002(1) 3_765 . . . ? F7 P3 F10 F8 -90.000(6) . . . . ? F7 P3 F10 F8 90.000(2) 10_557 . . . ? F9 P3 F10 F8 179.997(3) 2_645 . . . ? F9 P3 F10 F8 0.0 3_765 . . . ? F9 P3 F10 F8 180.000(1) . . . . ? F8 P3 F10 F8 0.005(4) 3_765 . . . ? F8 P3 F10 F8 179.999(1) 2_645 . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 30.21 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.694 _refine_diff_density_min -2.171 _refine_diff_density_rms 0.174 #=END data_xf # number 12 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; [bis(5,5'-dicyano-2,2'-bipyridine)silver(I)]-hexafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H12 Ag F6 N8 P' _chemical_formula_weight 665.26 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' 'P' 'P' 0.1023 0.0942 '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 21.87600(10) _cell_length_b 8.2210(2) _cell_length_c 15.8848(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.2770(10) _cell_angle_gamma 90.00 _cell_volume 2583.24(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.685226 _exptl_absorpt_correction_T_max 0.882130 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.70930 _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4895 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.77 _reflns_number_total 2649 _reflns_number_gt 2286 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON _computing_publication_material CIFTAB _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^)+(0.0260P)^2^+3.2979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2649 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.60977(4) 0.7500 0.03414(13) Uani 1 d S . . N1 N 0.56498(14) 0.5864(3) 0.66687(18) 0.0265(6) Uani 1 d . . . N2 N 0.43907(14) 0.7198(3) 0.59834(18) 0.0285(6) Uani 1 d . . . N3 N 0.7820(2) 0.3655(4) 0.7257(3) 0.0574(10) Uani 1 d . . . N4 N 0.23215(19) 1.0107(4) 0.4378(3) 0.0556(9) Uani 1 d . . . C1 C 0.62481(18) 0.5137(3) 0.7009(2) 0.0297(7) Uani 1 d . . . H1 H 0.640(2) 0.460(4) 0.761(3) 0.038(10) Uiso 1 d . . . C2 C 0.66621(17) 0.5120(3) 0.6540(2) 0.0302(7) Uani 1 d . . . C3 C 0.64343(18) 0.5865(4) 0.5679(3) 0.0336(7) Uani 1 d . . . H3 H 0.674(2) 0.586(4) 0.540(3) 0.041(10) Uiso 1 d . . . C4 C 0.5807(2) 0.6606(4) 0.5323(3) 0.0331(8) Uani 1 d . . . H4 H 0.5655(19) 0.709(4) 0.475(2) 0.031(9) Uiso 1 d . . . C5 C 0.54224(16) 0.6597(3) 0.5831(2) 0.0235(6) Uani 1 d . . . C6 C 0.47463(16) 0.7385(3) 0.5472(2) 0.0240(6) Uani 1 d . . . C7 C 0.44908(18) 0.8287(4) 0.4650(2) 0.0305(7) Uani 1 d . . . H7 H 0.475(2) 0.838(4) 0.430(3) 0.037(9) Uiso 1 d . . . C8 C 0.38614(19) 0.8994(4) 0.4342(2) 0.0337(7) Uani 1 d . . . H8 H 0.368(2) 0.957(4) 0.382(3) 0.036(10) Uiso 1 d . . . C9 C 0.34985(18) 0.8800(4) 0.4873(2) 0.0314(7) Uani 1 d . . . C10 C 0.37884(17) 0.7893(4) 0.5690(2) 0.0314(7) Uani 1 d . . . H10 H 0.3585(19) 0.772(4) 0.610(2) 0.034(9) Uiso 1 d . . . C11 C 0.7312(2) 0.4309(4) 0.6947(3) 0.0388(8) Uani 1 d . . . C12 C 0.2843(2) 0.9529(4) 0.4598(3) 0.0406(8) Uani 1 d . . . P1 P 0.5000 0.11168(14) 0.7500 0.0392(3) Uani 1 d S . . F4 F 0.45834(13) -0.0246(2) 0.77474(16) 0.0503(6) Uani 1 d . . . F7 F 0.44494(15) 0.1115(2) 0.64393(16) 0.0569(7) Uani 1 d . . . F8 F 0.54111(17) 0.2500(3) 0.72567(17) 0.0719(9) 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 0.0509(3) 0.03479(18) 0.0267(2) 0.000 0.0261(2) 0.000 N1 0.0318(16) 0.0266(11) 0.0235(14) -0.0003(9) 0.0143(13) -0.0021(9) N2 0.0304(16) 0.0332(12) 0.0273(15) -0.0029(10) 0.0176(14) -0.0012(10) N3 0.041(2) 0.058(2) 0.071(3) 0.0072(16) 0.021(2) 0.0131(15) N4 0.040(2) 0.077(2) 0.052(2) 0.0026(17) 0.022(2) 0.0174(17) C1 0.033(2) 0.0306(14) 0.0250(18) -0.0012(12) 0.0118(16) -0.0026(12) C2 0.0286(18) 0.0259(13) 0.0356(19) -0.0046(12) 0.0133(16) -0.0004(11) C3 0.034(2) 0.0378(16) 0.038(2) 0.0013(13) 0.0237(18) 0.0050(13) C4 0.038(2) 0.0387(15) 0.031(2) 0.0070(13) 0.0222(19) 0.0068(13) C5 0.0274(18) 0.0231(12) 0.0227(16) -0.0041(10) 0.0132(15) -0.0034(10) C6 0.0292(18) 0.0231(12) 0.0237(16) -0.0040(10) 0.0151(15) -0.0035(10) C7 0.032(2) 0.0369(14) 0.0272(18) 0.0019(13) 0.0172(17) 0.0019(12) C8 0.036(2) 0.0380(16) 0.0262(19) 0.0015(14) 0.0122(17) 0.0013(14) C9 0.0264(19) 0.0357(15) 0.0333(19) -0.0074(13) 0.0138(17) -0.0012(12) C10 0.029(2) 0.0390(16) 0.0313(19) -0.0032(13) 0.0181(17) -0.0022(12) C11 0.038(2) 0.0378(17) 0.041(2) -0.0014(14) 0.017(2) 0.0015(14) C12 0.038(2) 0.0518(19) 0.034(2) -0.0019(15) 0.017(2) 0.0029(15) P1 0.0714(10) 0.0252(5) 0.0313(7) 0.000 0.0317(7) 0.000 F4 0.0690(17) 0.0437(11) 0.0541(14) 0.0156(9) 0.0414(14) 0.0054(10) F7 0.087(2) 0.0480(11) 0.0351(13) 0.0063(9) 0.0254(14) -0.0022(11) F8 0.128(3) 0.0448(12) 0.0568(16) -0.0103(11) 0.0531(18) -0.0366(14) _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 Ag1 0.0000(7) 2_656 ? Ag1 N1 2.325(2) 2_656 ? Ag1 N1 2.325(2) . ? Ag1 N2 2.378(3) 2_656 ? Ag1 N2 2.378(3) . ? N1 C1 1.326(4) . ? N1 C5 1.348(4) . ? N1 Ag1 2.325(2) 2_656 ? N2 C10 1.325(4) . ? N2 C6 1.352(3) . ? N2 Ag1 2.378(3) 2_656 ? N3 C11 1.140(5) . ? N4 C12 1.144(5) . ? C1 C2 1.397(4) . ? C1 H1 0.96(4) . ? C2 C3 1.382(5) . ? C2 C11 1.448(5) . ? C3 C4 1.383(5) . ? C3 H3 0.94(4) . ? C4 C5 1.392(4) . ? C4 H4 0.91(3) . ? C5 C6 1.487(4) . ? C6 C7 1.394(4) . ? C7 C8 1.377(5) . ? C7 H7 0.96(4) . ? C8 C9 1.393(5) . ? C8 H8 0.88(4) . ? C9 C10 1.393(5) . ? C9 C12 1.439(5) . ? C10 H10 0.94(3) . ? P1 F4 1.596(2) 2_656 ? P1 F4 1.596(2) . ? P1 F8 1.596(2) 2_656 ? P1 F8 1.596(2) . ? P1 F7 1.599(3) . ? P1 F7 1.599(3) 2_656 ? 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 Ag1 Ag1 N1 0(10) 2_656 2_656 ? Ag1 Ag1 N1 0(10) 2_656 . ? N1 Ag1 N1 170.51(11) 2_656 . ? Ag1 Ag1 N2 0(10) 2_656 2_656 ? N1 Ag1 N2 70.75(9) 2_656 2_656 ? N1 Ag1 N2 113.12(9) . 2_656 ? Ag1 Ag1 N2 0(10) 2_656 . ? N1 Ag1 N2 113.12(9) 2_656 . ? N1 Ag1 N2 70.75(9) . . ? N2 Ag1 N2 135.27(12) 2_656 . ? C1 N1 C5 119.2(3) . . ? C1 N1 Ag1 122.8(2) . 2_656 ? C5 N1 Ag1 117.8(2) . 2_656 ? C1 N1 Ag1 122.8(2) . . ? C5 N1 Ag1 117.8(2) . . ? Ag1 N1 Ag1 0.000(16) 2_656 . ? C10 N2 C6 118.8(3) . . ? C10 N2 Ag1 124.3(2) . 2_656 ? C6 N2 Ag1 115.7(2) . 2_656 ? C10 N2 Ag1 124.3(2) . . ? C6 N2 Ag1 115.7(2) . . ? Ag1 N2 Ag1 0.000(15) 2_656 . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1 119(2) . . ? C2 C1 H1 119(2) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C11 121.1(3) . . ? C1 C2 C11 120.2(3) . . ? C2 C3 C4 118.4(3) . . ? C2 C3 H3 115(2) . . ? C4 C3 H3 126(2) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 118(2) . . ? C5 C4 H4 122(2) . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 117.4(2) . . ? C4 C5 C6 121.6(3) . . ? N2 C6 C7 121.3(3) . . ? N2 C6 C5 117.0(3) . . ? C7 C6 C5 121.7(3) . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7 121(2) . . ? C6 C7 H7 119(2) . . ? C7 C8 C9 118.5(3) . . ? C7 C8 H8 122(2) . . ? C9 C8 H8 119(2) . . ? C8 C9 C10 118.4(3) . . ? C8 C9 C12 121.3(3) . . ? C10 C9 C12 120.3(3) . . ? N2 C10 C9 123.1(3) . . ? N2 C10 H10 113(2) . . ? C9 C10 H10 124(2) . . ? N3 C11 C2 179.0(4) . . ? N4 C12 C9 179.9(5) . . ? F4 P1 F4 90.80(16) 2_656 . ? F4 P1 F8 179.16(13) 2_656 2_656 ? F4 P1 F8 90.03(13) . 2_656 ? F4 P1 F8 90.03(13) 2_656 . ? F4 P1 F8 179.16(13) . . ? F8 P1 F8 89.1(2) 2_656 . ? F4 P1 F7 89.56(13) 2_656 . ? F4 P1 F7 90.37(12) . . ? F8 P1 F7 90.40(14) 2_656 . ? F8 P1 F7 89.67(13) . . ? F4 P1 F7 90.37(12) 2_656 2_656 ? F4 P1 F7 89.56(13) . 2_656 ? F8 P1 F7 89.67(13) 2_656 2_656 ? F8 P1 F7 90.39(14) . 2_656 ? F7 P1 F7 179.91(17) . 2_656 ? 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 Ag1 Ag1 N1 C1 0(9) 2_656 . . . ? N1 Ag1 N1 C1 -61.0(2) 2_656 . . . ? N2 Ag1 N1 C1 51.3(2) 2_656 . . . ? N2 Ag1 N1 C1 -176.7(2) . . . . ? Ag1 Ag1 N1 C5 0(11) 2_656 . . . ? N1 Ag1 N1 C5 123.4(2) 2_656 . . . ? N2 Ag1 N1 C5 -124.2(2) 2_656 . . . ? N2 Ag1 N1 C5 7.76(19) . . . . ? N1 Ag1 N1 Ag1 0(100) 2_656 . . 2_656 ? N2 Ag1 N1 Ag1 0(42) 2_656 . . 2_656 ? N2 Ag1 N1 Ag1 0(100) . . . 2_656 ? Ag1 Ag1 N2 C10 0(5) 2_656 . . . ? N1 Ag1 N2 C10 12.0(3) 2_656 . . . ? N1 Ag1 N2 C10 -177.3(3) . . . . ? N2 Ag1 N2 C10 -73.5(2) 2_656 . . . ? Ag1 Ag1 N2 C6 0.0(11) 2_656 . . . ? N1 Ag1 N2 C6 179.06(18) 2_656 . . . ? N1 Ag1 N2 C6 -10.24(18) . . . . ? N2 Ag1 N2 C6 93.55(19) 2_656 . . . ? N1 Ag1 N2 Ag1 0(100) 2_656 . . 2_656 ? N1 Ag1 N2 Ag1 0(99) . . . 2_656 ? N2 Ag1 N2 Ag1 0(77) 2_656 . . 2_656 ? C5 N1 C1 C2 1.1(4) . . . . ? Ag1 N1 C1 C2 -174.4(2) 2_656 . . . ? Ag1 N1 C1 C2 -174.4(2) . . . . ? N1 C1 C2 C3 -1.2(5) . . . . ? N1 C1 C2 C11 179.9(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C11 C2 C3 C4 179.4(3) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C1 N1 C5 C4 -0.2(4) . . . . ? Ag1 N1 C5 C4 175.5(2) 2_656 . . . ? Ag1 N1 C5 C4 175.5(2) . . . . ? C1 N1 C5 C6 179.5(2) . . . . ? Ag1 N1 C5 C6 -4.8(3) 2_656 . . . ? Ag1 N1 C5 C6 -4.8(3) . . . . ? C3 C4 C5 N1 -0.5(5) . . . . ? C3 C4 C5 C6 179.8(3) . . . . ? C10 N2 C6 C7 0.0(4) . . . . ? Ag1 N2 C6 C7 -167.9(2) 2_656 . . . ? Ag1 N2 C6 C7 -167.9(2) . . . . ? C10 N2 C6 C5 179.5(3) . . . . ? Ag1 N2 C6 C5 11.7(3) 2_656 . . . ? Ag1 N2 C6 C5 11.7(3) . . . . ? N1 C5 C6 N2 -4.8(4) . . . . ? C4 C5 C6 N2 174.9(3) . . . . ? N1 C5 C6 C7 174.7(3) . . . . ? C4 C5 C6 C7 -5.6(4) . . . . ? N2 C6 C7 C8 -0.6(5) . . . . ? C5 C6 C7 C8 179.9(3) . . . . ? C6 C7 C8 C9 0.7(5) . . . . ? C7 C8 C9 C10 -0.2(5) . . . . ? C7 C8 C9 C12 179.0(3) . . . . ? C6 N2 C10 C9 0.6(5) . . . . ? Ag1 N2 C10 C9 167.3(2) 2_656 . . . ? Ag1 N2 C10 C9 167.3(2) . . . . ? C8 C9 C10 N2 -0.4(5) . . . . ? C12 C9 C10 N2 -179.7(3) . . . . ? C3 C2 C11 N3 -67(22) . . . . ? C1 C2 C11 N3 112(22) . . . . ? C8 C9 C12 N4 93(100) . . . . ? C10 C9 C12 N4 -88(100) . . . . ? _diffrn_measured_fraction_theta_max 0.783 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.783 _refine_diff_density_max 0.369 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.085 --Message-Boundary-2260 Content-type: text/plain; charset=US-ASCII Content-transfer-encoding: 7BIT Content-description: Text from file 'xg.cif' data_xg _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Cl2 N4 Ni O2 S2' _chemical_formula_weight 492.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2485(3) _cell_length_b 10.3776(3) _cell_length_c 11.2003(3) _cell_angle_alpha 75.7300(10) _cell_angle_beta 85.8830(10) _cell_angle_gamma 72.9420(10) _cell_volume 995.97(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour gelb _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.743084 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SMART-CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7782 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 31.19 _reflns_number_total 5638 _reflns_number_gt 4129 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ZORTEP/PLATON _computing_publication_material CIFTAB _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 ; w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.8293P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5638 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.37848(4) 0.83841(4) 0.46084(3) 0.01881(10) Uani 1 d . . . Cl1 Cl 0.41631(9) 0.89721(10) 0.62895(8) 0.0369(2) Uani 1 d . . . Cl2 Cl 0.56479(10) 0.72370(10) 0.36145(10) 0.0435(2) Uani 1 d . . . S1 S 0.04230(10) 0.23514(9) 0.84465(8) 0.0343(2) Uani 1 d . . . S2 S 0.23848(10) 1.48803(9) -0.06027(8) 0.03234(19) Uani 1 d . . . O1 O -0.1490(3) 0.4598(2) 0.7140(2) 0.0341(5) Uani 1 d . . . O2 O 0.3765(2) 1.2314(2) 0.0602(2) 0.0318(5) Uani 1 d . . . N1 N 0.2014(3) 0.7467(3) 0.4984(2) 0.0236(5) Uani 1 d . . . N2 N 0.2175(3) 0.9830(3) 0.3434(2) 0.0236(5) Uani 1 d . . . N3 N 0.0918(3) 0.4523(3) 0.6879(2) 0.0270(5) Uani 1 d . . . H3N H 0.204(5) 0.395(5) 0.706(4) 0.067(15) Uiso 1 d . . . N4 N 0.1337(3) 1.3102(3) 0.1053(3) 0.0269(6) Uani 1 d . . . H4N H 0.043(4) 1.374(4) 0.079(3) 0.027(9) Uiso 1 d . . . C1 C 0.2009(3) 0.6273(3) 0.5782(3) 0.0243(6) Uani 1 d . . . H1 H 0.297(4) 0.572(4) 0.615(3) 0.030(9) Uiso 1 d . . . C2 C 0.0722(3) 0.5827(3) 0.6056(3) 0.0237(6) Uani 1 d . . . C3 C -0.0629(3) 0.6695(3) 0.5495(3) 0.0257(6) Uani 1 d . . . H3 H -0.159(4) 0.646(4) 0.563(3) 0.029(9) Uiso 1 d . . . C4 C -0.0617(3) 0.7926(3) 0.4674(3) 0.0252(6) Uani 1 d . . . H4 H -0.156(4) 0.857(4) 0.428(3) 0.026(9) Uiso 1 d . . . C5 C 0.0721(3) 0.8294(3) 0.4423(3) 0.0221(6) Uani 1 d . . . C6 C 0.0830(3) 0.9563(3) 0.3520(3) 0.0220(6) Uani 1 d . . . C7 C -0.0367(3) 1.0439(3) 0.2787(3) 0.0281(6) Uani 1 d . . . H7 H -0.138(4) 1.029(4) 0.292(3) 0.030(9) Uiso 1 d . . . C8 C -0.0168(3) 1.1591(3) 0.1954(3) 0.0282(7) Uani 1 d . . . H8 H -0.095(4) 1.224(3) 0.145(3) 0.020(8) Uiso 1 d . . . C9 C 0.1219(3) 1.1867(3) 0.1865(3) 0.0243(6) Uani 1 d . . . C10 C 0.2379(3) 1.0949(3) 0.2629(3) 0.0248(6) Uani 1 d . . . H10 H 0.342(4) 1.108(4) 0.260(3) 0.032(9) Uiso 1 d . . . C11 C -0.0093(4) 0.3874(3) 0.7462(3) 0.0272(6) Uani 1 d . . . C12 C 0.2532(3) 1.3363(3) 0.0383(3) 0.0266(6) Uani 1 d . . . C13 C -0.2738(4) 0.4094(4) 0.7707(3) 0.0319(7) Uani 1 d . . . H12A H -0.254(4) 0.378(4) 0.860(4) 0.034(10) Uiso 1 d . . . H12B H -0.265(4) 0.323(4) 0.744(3) 0.022(8) Uiso 1 d . . . C14 C -0.4128(4) 0.5257(4) 0.7305(4) 0.0409(9) Uani 1 d . . . H14A H -0.408(5) 0.614(5) 0.752(4) 0.061(14) Uiso 1 d . . . H14B H -0.430(5) 0.549(4) 0.638(4) 0.048(12) Uiso 1 d . . . H14C H -0.506(5) 0.498(5) 0.780(4) 0.063(14) Uiso 1 d . . . C15 C 0.5142(4) 1.2464(4) -0.0075(4) 0.0401(9) Uani 1 d . . . H14A H 0.535(5) 1.331(5) 0.008(4) 0.052(13) Uiso 1 d . . . H14B H 0.487(5) 1.274(5) -0.098(5) 0.066(15) Uiso 1 d . . . C16 C 0.6334(5) 1.1128(5) 0.0307(4) 0.0476(10) Uani 1 d . . . H16A H 0.623(7) 1.032(7) 0.014(6) 0.10(2) Uiso 1 d . . . H16B H 0.740(6) 1.115(5) -0.009(5) 0.073(15) Uiso 1 d . . . H16C H 0.644(7) 1.095(7) 0.130(6) 0.11(2) Uiso 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 Ni1 0.01147(16) 0.02024(18) 0.02119(18) -0.00148(13) -0.00094(12) - 0.00179(12) Cl1 0.0266(4) 0.0490(5) 0.0371(4) -0.0134(4) -0.0039(3) -0.0099(3) Cl2 0.0292(4) 0.0398(5) 0.0588(6) -0.0191(4) 0.0121(4) -0.0023(3) S1 0.0363(4) 0.0294(4) 0.0328(4) 0.0008(3) -0.0012(3) -0.0091(3) S2 0.0309(4) 0.0266(4) 0.0351(4) 0.0004(3) 0.0016(3) -0.0085(3) O1 0.0258(11) 0.0350(13) 0.0344(13) 0.0038(10) 0.0018(10) -0.0081(10) O2 0.0237(11) 0.0291(12) 0.0352(13) 0.0006(10) 0.0031(9) -0.0040(9) N1 0.0184(11) 0.0248(12) 0.0254(13) -0.0042(10) 0.0002(10) -0.0045(9) N2 0.0178(11) 0.0236(12) 0.0267(13) -0.0040(10) 0.0002(10) -0.0035(9) N3 0.0228(13) 0.0263(13) 0.0276(13) 0.0001(10) -0.0001(10) -0.0058(10) N4 0.0207(12) 0.0252(13) 0.0299(14) 0.0012(11) -0.0007(10) -0.0053(10) C1 0.0198(14) 0.0245(15) 0.0268(15) -0.0042(12) -0.0010(11) -0.0050(11) C2 0.0230(14) 0.0226(14) 0.0243(14) -0.0047(11) 0.0004(11) -0.0054(11) C3 0.0199(14) 0.0272(15) 0.0279(15) -0.0033(12) 0.0013(12) -0.0065(12) C4 0.0196(14) 0.0245(14) 0.0268(15) -0.0020(12) -0.0009(11) -0.0023(11) C5 0.0190(13) 0.0235(14) 0.0224(14) -0.0054(11) 0.0007(11) -0.0040(11) C6 0.0190(13) 0.0223(14) 0.0228(14) -0.0048(11) 0.0028(11) -0.0040(10) C7 0.0200(14) 0.0256(15) 0.0353(17) -0.0018(13) -0.0027(12) -0.0051(12) C8 0.0210(14) 0.0276(16) 0.0318(16) -0.0009(13) -0.0035(12) -0.0047(12) C9 0.0236(14) 0.0225(14) 0.0245(14) -0.0032(11) 0.0002(11) -0.0049(11) C10 0.0206(14) 0.0255(15) 0.0263(15) -0.0031(12) -0.0001(11) -0.0061(11) C11 0.0275(15) 0.0277(15) 0.0255(15) -0.0056(12) -0.0004(12) -0.0072(12) C12 0.0253(15) 0.0265(15) 0.0271(15) -0.0053(12) -0.0008(12) -0.0067(12) C13 0.0272(16) 0.0347(18) 0.0328(18) -0.0035(14) 0.0055(13) -0.0124(14) C14 0.0252(17) 0.044(2) 0.046(2) 0.0014(17) 0.0013(15) -0.0092(15) C15 0.0277(17) 0.040(2) 0.042(2) 0.0017(17) 0.0106(15) -0.0064(15) C16 0.0287(19) 0.050(2) 0.052(3) -0.005(2) 0.0051(17) -0.0006(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 Ni1 N2 2.049(2) . ? Ni1 N1 2.094(2) . ? Ni1 Cl2 2.1909(10) . ? Ni1 Cl1 2.1969(9) . ? S1 C11 1.647(3) . ? S2 C12 1.660(3) . ? O1 C11 1.315(4) . ? O1 C13 1.447(4) . ? O2 C12 1.314(4) . ? O2 C15 1.463(4) . ? N1 C1 1.339(4) . ? N1 C5 1.342(4) . ? N2 C10 1.336(4) . ? N2 C6 1.343(4) . ? N3 C11 1.349(4) . ? N3 C2 1.406(4) . ? N3 H3N 1.04(5) . ? N4 C12 1.347(4) . ? N4 C9 1.406(4) . ? N4 H4N 0.92(4) . ? C1 C2 1.388(4) . ? C1 H1 0.96(4) . ? C2 C3 1.393(4) . ? C3 C4 1.380(4) . ? C3 H3 0.99(4) . ? C4 C5 1.390(4) . ? C4 H4 0.99(3) . ? C5 C6 1.475(4) . ? C6 C7 1.378(4) . ? C7 C8 1.374(4) . ? C7 H7 0.99(4) . ? C8 C9 1.386(4) . ? C8 H8 0.94(3) . ? C9 C10 1.386(4) . ? C10 H10 1.01(4) . ? C13 C14 1.489(5) . ? C13 H12A 0.98(4) . ? C13 H12B 0.99(3) . ? C14 H14A 1.02(5) . ? C14 H14B 1.02(4) . ? C14 H14C 1.07(5) . ? C15 C16 1.482(5) . ? C15 H14A 1.01(5) . ? C15 H14B 1.02(5) . ? C16 H16A 0.93(6) . ? C16 H16B 1.06(5) . ? C16 H16C 1.08(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 80.26(10) . . ? N2 Ni1 Cl2 111.95(8) . . ? N1 Ni1 Cl2 112.38(8) . . ? N2 Ni1 Cl1 115.41(8) . . ? N1 Ni1 Cl1 106.97(8) . . ? Cl2 Ni1 Cl1 121.97(4) . . ? C11 O1 C13 119.9(3) . . ? C12 O2 C15 118.4(3) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Ni1 127.75(19) . . ? C5 N1 Ni1 112.48(19) . . ? C10 N2 C6 120.5(3) . . ? C10 N2 Ni1 125.6(2) . . ? C6 N2 Ni1 113.90(19) . . ? C11 N3 C2 131.4(3) . . ? C11 N3 H3N 114(3) . . ? C2 N3 H3N 114(3) . . ? C12 N4 C9 129.3(3) . . ? C12 N4 H4N 114(2) . . ? C9 N4 H4N 115(2) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 116(2) . . ? C2 C1 H1 121(2) . . ? C1 C2 C3 117.7(3) . . ? C1 C2 N3 116.1(3) . . ? C3 C2 N3 126.2(3) . . ? C4 C3 C2 118.9(3) . . ? C4 C3 H3 118(2) . . ? C2 C3 H3 123(2) . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H4 120(2) . . ? C5 C4 H4 119(2) . . ? N1 C5 C4 120.6(3) . . ? N1 C5 C6 116.2(2) . . ? C4 C5 C6 123.3(3) . . ? N2 C6 C7 120.8(3) . . ? N2 C6 C5 116.6(2) . . ? C7 C6 C5 122.6(3) . . ? C8 C7 C6 119.1(3) . . ? C8 C7 H7 120(2) . . ? C6 C7 H7 120(2) . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 123(2) . . ? C9 C8 H8 117(2) . . ? C8 C9 C10 118.2(3) . . ? C8 C9 N4 117.8(3) . . ? C10 C9 N4 124.0(3) . . ? N2 C10 C9 121.3(3) . . ? N2 C10 H10 116(2) . . ? C9 C10 H10 122(2) . . ? O1 C11 N3 111.9(3) . . ? O1 C11 S1 125.8(2) . . ? N3 C11 S1 122.3(2) . . ? O2 C12 N4 113.1(3) . . ? O2 C12 S2 125.7(2) . . ? N4 C12 S2 121.2(2) . . ? O1 C13 C14 105.6(3) . . ? O1 C13 H12A 107(2) . . ? C14 C13 H12A 116(2) . . ? O1 C13 H12B 106(2) . . ? C14 C13 H12B 116.1(19) . . ? H12A C13 H12B 104(3) . . ? C13 C14 H14A 112(3) . . ? C13 C14 H14B 112(3) . . ? H14A C14 H14B 107(4) . . ? C13 C14 H14C 108(2) . . ? H14A C14 H14C 106(4) . . ? H14B C14 H14C 111(3) . . ? O2 C15 C16 107.4(3) . . ? O2 C15 H14A 107(3) . . ? C16 C15 H14A 116(2) . . ? O2 C15 H14B 106(3) . . ? C16 C15 H14B 115(3) . . ? H14A C15 H14B 104(4) . . ? C15 C16 H16A 121(4) . . ? C15 C16 H16B 113(3) . . ? H16A C16 H16B 101(5) . . ? C15 C16 H16C 106(4) . . ? H16A C16 H16C 108(5) . . ? H16B C16 H16C 108(4) . . ? 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 N2 Ni1 N1 C1 -179.8(3) . . . . ? Cl2 Ni1 N1 C1 70.4(3) . . . . ? Cl1 Ni1 N1 C1 -66.0(3) . . . . ? N2 Ni1 N1 C5 -7.0(2) . . . . ? Cl2 Ni1 N1 C5 -116.9(2) . . . . ? Cl1 Ni1 N1 C5 106.7(2) . . . . ? N1 Ni1 N2 C10 -175.6(3) . . . . ? Cl2 Ni1 N2 C10 -65.3(3) . . . . ? Cl1 Ni1 N2 C10 80.1(3) . . . . ? N1 Ni1 N2 C6 3.8(2) . . . . ? Cl2 Ni1 N2 C6 114.2(2) . . . . ? Cl1 Ni1 N2 C6 -100.4(2) . . . . ? C5 N1 C1 C2 0.8(5) . . . . ? Ni1 N1 C1 C2 173.0(2) . . . . ? N1 C1 C2 C3 -2.1(5) . . . . ? N1 C1 C2 N3 177.7(3) . . . . ? C11 N3 C2 C1 169.7(3) . . . . ? C11 N3 C2 C3 -10.5(6) . . . . ? C1 C2 C3 C4 1.9(5) . . . . ? N3 C2 C3 C4 -177.8(3) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C1 N1 C5 C4 0.7(4) . . . . ? Ni1 N1 C5 C4 -172.7(2) . . . . ? C1 N1 C5 C6 -177.7(3) . . . . ? Ni1 N1 C5 C6 9.0(3) . . . . ? C3 C4 C5 N1 -0.8(5) . . . . ? C3 C4 C5 C6 177.4(3) . . . . ? C10 N2 C6 C7 -0.4(5) . . . . ? Ni1 N2 C6 C7 -179.8(2) . . . . ? C10 N2 C6 C5 179.2(3) . . . . ? Ni1 N2 C6 C5 -0.3(3) . . . . ? N1 C5 C6 N2 -6.0(4) . . . . ? C4 C5 C6 N2 175.7(3) . . . . ? N1 C5 C6 C7 173.5(3) . . . . ? C4 C5 C6 C7 -4.8(5) . . . . ? N2 C6 C7 C8 0.5(5) . . . . ? C5 C6 C7 C8 -179.0(3) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C7 C8 C9 N4 -176.2(3) . . . . ? C12 N4 C9 C8 -147.4(3) . . . . ? C12 N4 C9 C10 36.2(5) . . . . ? C6 N2 C10 C9 0.2(5) . . . . ? Ni1 N2 C10 C9 179.6(2) . . . . ? C8 C9 C10 N2 -0.2(5) . . . . ? N4 C9 C10 N2 176.1(3) . . . . ? C13 O1 C11 N3 -177.6(3) . . . . ? C13 O1 C11 S1 2.8(5) . . . . ? C2 N3 C11 O1 3.2(5) . . . . ? C2 N3 C11 S1 -177.2(3) . . . . ? C15 O2 C12 N4 179.6(3) . . . . ? C15 O2 C12 S2 -0.4(5) . . . . ? C9 N4 C12 O2 -4.5(5) . . . . ? C9 N4 C12 S2 175.5(3) . . . . ? C11 O1 C13 C14 170.3(3) . . . . ? C12 O2 C15 C16 -177.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 31.19 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 0.699 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.102 --Message-Boundary-2260--