# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2192 #------------------------------------------------------------------------------ data_1 #{[Cu2(4-bpbd)3(CH3CN)2](PF6)2.2H2O)}n 1a.2H2O #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H34 Cu2 F12 N8 O2 P2 ' _chemical_formula_moiety 'C46 H34 Cu2 F12 N8 O2 P2 ' _chemical_formula_weight 1147.85 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.639(2) _cell_length_b 15.558(2) _cell_length_c 16.5787(5) _cell_angle_alpha 113.349(1) _cell_angle_beta 91.187(2) _cell_angle_gamma 106.020(1) _cell_volume 2845.3(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12379 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'capillary' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.439 _exptl_absorpt_correction_T_max 0.915 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method w _diffrn_reflns_number 12379 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.54 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12379 _reflns_number_gt 6748 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1110 _refine_ls_wR_factor_ref 0.3583 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6748 _refine_ls_number_parameters 650 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0338 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_diff_density_max 1.13 _refine_diff_density_min -0.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cu(1) Cu 0.26858(6) 0.27291(7) 0.27037(5) 0.0692(3) Uani 1.00 d . . . Cu(2) Cu -0.55621(6) 0.71118(6) -0.08855(5) 0.0673(3) Uani 1.00 d . . . P(1) P 0.4570(3) 0.3082(2) 0.6601(3) 0.138(1) Uani 1.00 d . . . P(2) P 0.2077(3) -0.0395(2) -0.1407(3) 0.155(2) Uani 1.00 d . . . F(1) F 0.371(1) 0.232(1) 0.589(1) 0.38(1) Uani 1.00 d . . . F(2) F 0.552(1) 0.375(1) 0.719(1) 0.311(9) Uani 1.00 d . . . F(3) F 0.516(2) 0.231(1) 0.6341(8) 0.34(1) Uani 1.00 d . . . F(4) F 0.382(2) 0.372(1) 0.6918(9) 0.34(1) Uani 1.00 d . . . F(5) F 0.480(2) 0.348(1) 0.5932(9) 0.308(8) Uani 1.00 d . . . F(6) F 0.432(1) 0.276(2) 0.733(2) 0.35(1) Uani 1.00 d . . . F(7) F 0.226(1) -0.1121(7) -0.2306(6) 0.266(7) Uani 1.00 d . . . F(8) F 0.189(1) 0.0377(6) -0.0553(10) 0.247(6) Uani 1.00 d . . . F(9) F 0.141(1) -0.1277(8) -0.132(1) 0.38(1) Uani 1.00 d . . . F(10) F 0.270(2) 0.0483(7) -0.1594(9) 0.39(1) Uani 1.00 d . . . F(11) F 0.110(2) -0.040(2) -0.185(2) 0.62(3) Uani 1.00 d . . . F(12) F 0.3006(9) -0.037(1) -0.0948(8) 0.285(8) Uani 1.00 d . . . O(1) O 0.367(3) 0.009(1) 0.356(3) 0.65(3) Uani 1.00 d . . . O(2) O 0.062(2) 0.151(1) 0.760(2) 0.59(3) Uani 1.00 d . . . N(1) N 0.2014(4) 0.3444(4) 0.2134(3) 0.065(1) Uani 1.00 d . . . N(2) N -0.4316(4) 0.6626(4) -0.0633(4) 0.065(1) Uani 1.00 d . . . N(3) N 0.1716(5) 0.2692(4) 0.3721(3) 0.069(1) Uani 1.00 d . . . N(4) N -0.3614(4) 0.2706(4) 0.9765(3) 0.064(1) Uani 1.00 d . . . N(5) N 0.4287(4) 0.3185(4) 0.3283(4) 0.065(1) Uani 1.00 d . . . N(6) N 1.3164(4) 0.6385(4) 0.8088(3) 0.064(1) Uani 1.00 d . . . N(7) N 0.2107(6) 0.1295(6) 0.1846(5) 0.092(2) Uani 1.00 d . . . N(8) N -0.4883(5) 0.8429(5) -0.0928(4) 0.076(2) Uani 1.00 d . . . C(1) C 0.2327(6) 0.4410(6) 0.2412(5) 0.074(2) Uani 1.00 d . . . C(2) C 0.1759(6) 0.4904(6) 0.2118(5) 0.079(2) Uani 1.00 d . . . C(3) C 0.0780(5) 0.4373(6) 0.1541(4) 0.066(2) Uani 1.00 d . . . C(4) C 0.0457(6) 0.3371(6) 0.1241(5) 0.079(2) Uani 1.00 d . . . C(5) C 0.1072(6) 0.2935(5) 0.1560(5) 0.075(2) Uani 1.00 d . . . C(6) C -0.4447(6) 0.5694(6) -0.0805(6) 0.083(2) Uani 1.00 d . . . C(7) C -0.3676(7) 0.5387(6) -0.0485(6) 0.091(2) Uani 1.00 d . . . C(8) C -0.2724(6) 0.6075(6) 0.0061(5) 0.070(2) Uani 1.00 d . . . C(9) C -0.2584(6) 0.7031(6) 0.0235(6) 0.082(2) Uani 1.00 d . . . C(10) C -0.3391(6) 0.7268(5) -0.0132(5) 0.077(2) Uani 1.00 d . . . C(11) C 0.0106(6) 0.4819(6) 0.1239(5) 0.074(2) Uani 1.00 d . . . C(12) C -0.0509(6) 0.5167(6) 0.0985(5) 0.081(2) Uani 1.00 d . . . C(13) C -0.1251(6) 0.5500(6) 0.0689(6) 0.083(2) Uani 1.00 d . . . C(14) C -0.1916(7) 0.5762(7) 0.0406(5) 0.084(2) Uani 1.00 d . . . C(15) C 0.0622(6) 0.2544(8) 0.3592(5) 0.091(3) Uani 1.00 d . . . C(16) C -0.0077(6) 0.2465(7) 0.4204(6) 0.088(2) Uani 1.00 d . . . C(17) C 0.0375(6) 0.2529(6) 0.4998(4) 0.074(2) Uani 1.00 d . . . C(18) C 0.1501(7) 0.2705(7) 0.5132(5) 0.090(2) Uani 1.00 d . . . C(19) C 0.2127(6) 0.2763(7) 0.4485(5) 0.087(2) Uani 1.00 d . . . C(20) C -0.2523(5) 0.2824(6) 0.9814(4) 0.077(2) Uani 1.00 d . . . C(21) C -0.1910(6) 0.2776(7) 0.9126(5) 0.081(2) Uani 1.00 d . . . C(22) C -0.2464(6) 0.2575(5) 0.8316(4) 0.070(2) Uani 1.00 d . . . C(23) C -0.3602(7) 0.2421(7) 0.8246(4) 0.084(2) Uani 1.00 d . . . C(24) C -0.4139(6) 0.2502(7) 0.8974(5) 0.083(2) Uani 1.00 d . . . C(25) C -0.0281(7) 0.2483(6) 0.5691(5) 0.079(2) Uani 1.00 d . . . C(26) C -0.0804(7) 0.2504(6) 0.6284(5) 0.080(2) Uani 1.00 d . . . C(27) C -0.1392(7) 0.2504(6) 0.6970(5) 0.081(2) Uani 1.00 d . . . C(28) C -0.1884(7) 0.2518(6) 0.7577(5) 0.077(2) Uani 1.00 d . . . C(29) C 0.4918(7) 0.4117(6) 0.3598(6) 0.092(2) Uani 1.00 d . . . C(30) C 0.5928(6) 0.4481(7) 0.4113(7) 0.095(3) Uani 1.00 d . . . C(31) C 0.6339(5) 0.3845(6) 0.4307(4) 0.076(2) Uani 1.00 d . . . C(32) C 0.5707(7) 0.2872(7) 0.3957(7) 0.098(3) Uani 1.00 d . . . C(33) C 0.4708(6) 0.2571(6) 0.3434(6) 0.088(2) Uani 1.00 d . . . C(34) C 1.2644(6) 0.5433(5) 0.7742(5) 0.074(2) Uani 1.00 d . . . C(35) C 1.1669(7) 0.4983(6) 0.7140(5) 0.082(2) Uani 1.00 d . . . C(36) C 1.1194(5) 0.5536(6) 0.6902(4) 0.069(2) Uani 1.00 d . . . C(37) C 1.1730(6) 0.6540(6) 0.7251(5) 0.073(2) Uani 1.00 d . . . C(38) C 1.2700(6) 0.6932(5) 0.7843(5) 0.073(2) Uani 1.00 d . . . C(39) C 0.7415(6) 0.4191(7) 0.4857(5) 0.084(2) Uani 1.00 d . . . C(40) C 0.8298(6) 0.4479(7) 0.5309(5) 0.084(2) Uani 1.00 d . . . C(41) C 0.9277(6) 0.4827(6) 0.5838(5) 0.083(2) Uani 1.00 d . . . C(42) C 1.0164(6) 0.5113(6) 0.6307(4) 0.080(2) Uani 1.00 d . . . C(43) C 0.1606(9) 0.0512(8) 0.1440(9) 0.116(3) Uani 1.00 d . . . C(44) C 0.099(1) -0.0495(10) 0.086(2) 0.213(9) Uani 1.00 d . . . C(45) C -0.4581(6) 0.9147(6) -0.1010(5) 0.077(2) Uani 1.00 d . . . C(46) C -0.4194(9) 1.0073(7) -0.1061(7) 0.108(3) Uani 1.00 d . . . H(1) H 0.2978 0.4789 0.2839 0.0888 Uiso 1.00 calc . . . H(2) H 0.2044 0.5597 0.2313 0.0954 Uiso 1.00 calc . . . H(3) H -0.0190 0.2976 0.0813 0.0943 Uiso 1.00 calc . . . H(4) H 0.0814 0.2240 0.1363 0.0904 Uiso 1.00 calc . . . H(5) H -0.5109 0.5210 -0.1168 0.0995 Uiso 1.00 calc . . . H(6) H -0.3801 0.4707 -0.0641 0.1091 Uiso 1.00 calc . . . H(7) H -0.1937 0.7533 0.0606 0.0979 Uiso 1.00 calc . . . H(8) H -0.3266 0.7941 -0.0014 0.0922 Uiso 1.00 calc . . . H(9) H 0.0305 0.2491 0.3043 0.1091 Uiso 1.00 calc . . . H(10) H -0.0849 0.2368 0.4082 0.1058 Uiso 1.00 calc . . . H(11) H 0.1850 0.2788 0.5682 0.1085 Uiso 1.00 calc . . . H(12) H 0.2901 0.2861 0.4594 0.1046 Uiso 1.00 calc . . . H(13) H -0.2137 0.2950 1.0367 0.0919 Uiso 1.00 calc . . . H(14) H -0.1131 0.2879 0.9209 0.0973 Uiso 1.00 calc . . . H(15) H -0.4014 0.2258 0.7692 0.1009 Uiso 1.00 calc . . . H(16) H -0.4916 0.2408 0.8910 0.1002 Uiso 1.00 calc . . . H(17) H 0.4648 0.4560 0.3456 0.1103 Uiso 1.00 calc . . . H(18) H 0.6339 0.5160 0.4334 0.1144 Uiso 1.00 calc . . . H(19) H 0.5963 0.2409 0.4077 0.1171 Uiso 1.00 calc . . . H(20) H 0.4301 0.1890 0.3170 0.1062 Uiso 1.00 calc . . . H(21) H 1.2954 0.5030 0.7915 0.0893 Uiso 1.00 calc . . . H(22) H 1.1340 0.4289 0.6898 0.0986 Uiso 1.00 calc . . . H(23) H 1.1433 0.6954 0.7084 0.0877 Uiso 1.00 calc . . . H(24) H 1.3053 0.7623 0.8087 0.0870 Uiso 1.00 calc . . . H(25) H 0.0522 -0.0782 0.1190 0.2553 Uiso 1.00 calc . . . H(26) H 0.0554 -0.0512 0.0383 0.2553 Uiso 1.00 calc . . . H(27) H 0.1499 -0.0855 0.0642 0.2553 Uiso 1.00 calc . . . H(28) H -0.3448 1.0401 -0.0770 0.1300 Uiso 1.00 calc . . . H(29) H -0.4225 0.9970 -0.1666 0.1300 Uiso 1.00 calc . . . H(30) H -0.4652 1.0464 -0.0780 0.1300 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0482(5) 0.0918(7) 0.0710(5) 0.0204(4) -0.0036(3) 0.0391(4) Cu(2) 0.0480(5) 0.0855(6) 0.0679(5) 0.0201(4) -0.0054(3) 0.0324(4) P(1) 0.140(3) 0.096(2) 0.157(3) 0.005(2) -0.067(2) 0.057(2) P(2) 0.116(2) 0.092(2) 0.198(4) 0.025(2) -0.072(2) 0.009(2) F(1) 0.31(2) 0.22(1) 0.48(3) 0.02(1) -0.26(2) 0.08(2) F(2) 0.20(1) 0.29(2) 0.33(2) -0.09(1) -0.11(1) 0.14(1) F(3) 0.49(3) 0.31(2) 0.19(1) 0.28(2) -0.11(1) -0.02(1) F(4) 0.53(3) 0.39(2) 0.23(1) 0.37(2) 0.05(1) 0.11(1) F(5) 0.50(3) 0.33(2) 0.21(1) 0.20(2) 0.08(1) 0.17(1) F(6) 0.18(1) 0.63(3) 0.56(3) 0.18(2) 0.14(1) 0.52(3) F(7) 0.50(2) 0.135(7) 0.143(7) 0.10(1) 0.001(10) 0.034(6) F(8) 0.22(1) 0.104(5) 0.32(1) 0.027(6) 0.082(10) 0.002(7) F(9) 0.32(2) 0.106(7) 0.57(3) 0.006(9) 0.27(2) 0.05(1) F(10) 0.82(4) 0.105(7) 0.20(1) 0.09(1) 0.05(2) 0.062(7) F(11) 0.37(3) 0.35(2) 0.80(5) 0.22(2) -0.39(3) -0.15(3) F(12) 0.145(8) 0.41(2) 0.204(9) 0.11(1) -0.065(7) 0.02(1) O(1) 0.64(5) 0.069(8) 0.95(8) 0.02(2) 0.08(5) -0.03(2) O(2) 0.60(4) 0.25(2) 0.83(5) 0.00(2) -0.53(4) 0.25(3) N(1) 0.054(3) 0.081(4) 0.069(3) 0.022(3) 0.002(2) 0.039(3) N(2) 0.050(3) 0.076(4) 0.070(3) 0.022(3) 0.000(2) 0.030(3) N(3) 0.058(3) 0.088(4) 0.059(3) 0.014(3) 0.004(2) 0.035(3) N(4) 0.053(3) 0.075(3) 0.065(3) 0.019(2) 0.003(2) 0.033(3) N(5) 0.040(3) 0.078(4) 0.077(3) 0.015(2) -0.003(2) 0.036(3) N(6) 0.050(3) 0.079(4) 0.053(3) 0.019(3) -0.006(2) 0.018(2) N(7) 0.084(5) 0.080(5) 0.107(5) 0.031(4) 0.010(4) 0.030(4) N(8) 0.061(3) 0.084(4) 0.076(4) 0.015(3) 0.000(3) 0.031(3) C(1) 0.055(4) 0.078(5) 0.084(4) 0.014(3) -0.011(3) 0.035(4) C(2) 0.068(4) 0.079(5) 0.092(5) 0.020(4) -0.009(4) 0.039(4) C(3) 0.045(3) 0.088(5) 0.074(4) 0.020(3) 0.007(3) 0.044(3) C(4) 0.061(4) 0.090(5) 0.080(4) 0.017(4) -0.016(3) 0.037(4) C(5) 0.057(4) 0.079(4) 0.087(4) 0.014(3) -0.017(3) 0.039(4) C(6) 0.061(4) 0.075(5) 0.100(5) 0.017(3) -0.014(4) 0.028(4) C(7) 0.075(5) 0.079(5) 0.117(6) 0.025(4) -0.009(4) 0.040(5) C(8) 0.064(4) 0.086(5) 0.076(4) 0.040(4) 0.011(3) 0.039(4) C(9) 0.051(4) 0.088(5) 0.102(5) 0.024(3) -0.013(3) 0.037(4) C(10) 0.053(4) 0.070(4) 0.103(5) 0.017(3) -0.014(3) 0.035(4) C(11) 0.070(4) 0.091(5) 0.080(4) 0.031(4) 0.010(3) 0.050(4) C(12) 0.068(4) 0.100(5) 0.087(5) 0.036(4) 0.003(3) 0.047(4) C(13) 0.068(4) 0.104(6) 0.100(5) 0.045(4) 0.012(4) 0.054(5) C(14) 0.075(5) 0.113(6) 0.087(5) 0.048(4) 0.014(4) 0.052(4) C(15) 0.059(4) 0.160(8) 0.075(4) 0.043(5) 0.009(3) 0.064(5) C(16) 0.056(4) 0.130(7) 0.090(5) 0.035(4) 0.009(3) 0.054(5) C(17) 0.072(4) 0.087(5) 0.059(4) 0.020(4) 0.007(3) 0.028(3) C(18) 0.069(5) 0.133(7) 0.067(4) 0.024(5) 0.005(3) 0.044(4) C(19) 0.053(4) 0.131(7) 0.079(5) 0.014(4) -0.007(3) 0.055(5) C(20) 0.048(3) 0.119(6) 0.062(4) 0.021(4) 0.005(3) 0.040(4) C(21) 0.062(4) 0.108(6) 0.074(4) 0.029(4) 0.013(3) 0.037(4) C(22) 0.074(4) 0.077(4) 0.067(4) 0.027(3) 0.016(3) 0.034(3) C(23) 0.092(5) 0.127(7) 0.051(3) 0.051(5) 0.015(3) 0.043(4) C(24) 0.061(4) 0.122(6) 0.077(4) 0.037(4) -0.002(3) 0.046(4) C(25) 0.075(5) 0.089(5) 0.068(4) 0.013(4) 0.009(3) 0.035(4) C(26) 0.079(5) 0.090(5) 0.072(4) 0.018(4) 0.014(4) 0.039(4) C(27) 0.091(5) 0.077(5) 0.066(4) 0.018(4) 0.011(4) 0.028(3) C(28) 0.085(5) 0.078(5) 0.063(4) 0.020(4) 0.015(3) 0.027(3) C(29) 0.065(5) 0.079(5) 0.126(7) 0.016(4) -0.019(4) 0.042(5) C(30) 0.053(4) 0.088(5) 0.135(7) 0.013(4) -0.015(4) 0.044(5) C(31) 0.044(3) 0.105(6) 0.065(4) 0.013(3) -0.004(3) 0.026(4) C(32) 0.069(5) 0.092(6) 0.127(7) 0.020(4) -0.027(5) 0.046(5) C(33) 0.057(4) 0.085(5) 0.110(6) 0.019(4) -0.026(4) 0.031(4) C(34) 0.066(4) 0.064(4) 0.083(4) 0.013(3) -0.016(3) 0.025(3) C(35) 0.072(5) 0.074(5) 0.080(4) 0.009(4) -0.018(3) 0.022(4) C(36) 0.050(3) 0.091(5) 0.058(3) 0.020(3) 0.001(3) 0.025(3) C(37) 0.060(4) 0.081(5) 0.072(4) 0.021(3) -0.009(3) 0.027(3) C(38) 0.057(4) 0.072(4) 0.081(4) 0.021(3) -0.010(3) 0.024(3) C(39) 0.053(4) 0.111(6) 0.071(4) 0.015(4) -0.011(3) 0.028(4) C(40) 0.050(4) 0.107(6) 0.083(4) 0.015(4) -0.005(3) 0.035(4) C(41) 0.059(4) 0.105(6) 0.063(4) 0.017(4) -0.006(3) 0.022(4) C(42) 0.050(4) 0.105(6) 0.061(4) 0.006(3) -0.008(3) 0.025(4) C(43) 0.087(6) 0.087(7) 0.166(10) 0.029(5) 0.004(6) 0.043(7) C(44) 0.13(1) 0.083(8) 0.35(3) 0.028(8) -0.03(1) 0.03(1) C(45) 0.068(4) 0.081(5) 0.072(4) 0.012(4) 0.001(3) 0.032(4) C(46) 0.108(7) 0.101(7) 0.144(8) 0.040(6) 0.044(6) 0.074(6) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.043(8) . . yes Cu(1) N(3) 2.115(6) . . yes Cu(1) N(5) 2.027(5) . . yes Cu(1) N(7) 2.019(7) . . yes Cu(2) N(2) 2.027(7) . . yes Cu(2) N(4) 2.107(6) . 2_466 yes Cu(2) N(6) 2.030(5) . 1_354 yes Cu(2) N(8) 2.022(8) . . yes P(1) F(1) 1.45(2) . . yes P(1) F(2) 1.39(1) . . yes P(1) F(3) 1.51(2) . . yes P(1) F(4) 1.51(2) . . yes P(1) F(5) 1.47(2) . . yes P(1) F(6) 1.48(3) . . yes P(2) F(7) 1.54(1) . . yes P(2) F(8) 1.53(1) . . yes P(2) F(9) 1.46(2) . . yes P(2) F(10) 1.53(2) . . yes P(2) F(11) 1.41(3) . . yes P(2) F(12) 1.37(1) . . yes N(1) C(1) 1.32(1) . . yes N(1) C(5) 1.336(8) . . yes N(2) C(6) 1.32(1) . . yes N(2) C(10) 1.309(7) . . yes N(3) C(15) 1.336(10) . . yes N(3) C(19) 1.31(1) . . yes N(4) C(20) 1.336(9) . . yes N(4) C(24) 1.33(1) . . yes N(5) C(29) 1.325(10) . . yes N(5) C(33) 1.31(1) . . yes N(6) C(34) 1.315(9) . . yes N(6) C(38) 1.33(1) . . yes N(7) C(43) 1.12(1) . . yes N(8) C(45) 1.14(1) . . yes C(1) C(2) 1.39(1) . . yes C(2) C(3) 1.375(9) . . yes C(3) C(4) 1.37(1) . . yes C(3) C(11) 1.43(1) . . yes C(4) C(5) 1.38(1) . . yes C(6) C(7) 1.37(1) . . yes C(7) C(8) 1.375(9) . . yes C(8) C(9) 1.36(1) . . yes C(8) C(14) 1.44(1) . . yes C(9) C(10) 1.38(1) . . yes C(11) C(12) 1.21(1) . . yes C(12) C(13) 1.36(1) . . yes C(13) C(14) 1.19(2) . . yes C(15) C(16) 1.38(1) . . yes C(16) C(17) 1.38(1) . . yes C(17) C(18) 1.37(1) . . yes C(17) C(25) 1.44(1) . . yes C(18) C(19) 1.36(1) . . yes C(20) C(21) 1.38(1) . . yes C(21) C(22) 1.38(1) . . yes C(22) C(23) 1.39(1) . . yes C(22) C(28) 1.43(1) . . yes C(23) C(24) 1.38(1) . . yes C(25) C(26) 1.19(1) . . yes C(26) C(27) 1.37(1) . . yes C(27) C(28) 1.19(1) . . yes C(29) C(30) 1.36(1) . . yes C(30) C(31) 1.37(2) . . yes C(31) C(32) 1.37(1) . . yes C(31) C(39) 1.458(10) . . yes C(32) C(33) 1.37(1) . . yes C(34) C(35) 1.39(1) . . yes C(35) C(36) 1.34(1) . . yes C(36) C(37) 1.38(1) . . yes C(36) C(42) 1.435(9) . . yes C(37) C(38) 1.378(10) . . yes C(39) C(40) 1.20(1) . . yes C(40) C(41) 1.34(1) . . yes C(41) C(42) 1.215(10) . . yes C(43) C(44) 1.44(2) . . yes C(45) C(46) 1.42(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(3) 103.6(3) . 1_555 1_555 yes N(1) Cu(1) N(5) 125.3(2) . 1_555 1_555 yes N(1) Cu(1) N(7) 105.0(3) . 1_555 1_555 yes N(3) Cu(1) N(5) 105.3(2) . 1_555 1_555 yes N(3) Cu(1) N(7) 99.3(3) . 1_555 1_555 yes N(5) Cu(1) N(7) 114.8(3) . 1_555 1_555 yes N(2) Cu(2) N(4) 103.0(3) . 1_555 2_466 yes N(2) Cu(2) N(6) 127.2(2) . 1_555 1_354 yes N(2) Cu(2) N(8) 108.6(3) . 1_555 1_555 yes N(4) Cu(2) N(6) 102.9(2) . 2_466 1_354 yes N(4) Cu(2) N(8) 110.0(2) . 2_466 1_555 yes N(6) Cu(2) N(8) 104.4(3) . 1_354 1_555 yes F(1) P(1) F(2) 169(1) . 1_555 1_555 yes F(1) P(1) F(3) 83.2(10) . 1_555 1_555 yes F(1) P(1) F(4) 92.4(10) . 1_555 1_555 yes F(1) P(1) F(5) 82(1) . 1_555 1_555 yes F(1) P(1) F(6) 100(1) . 1_555 1_555 yes F(2) P(1) F(3) 88.4(10) . 1_555 1_555 yes F(2) P(1) F(4) 96.9(9) . 1_555 1_555 yes F(2) P(1) F(5) 93(1) . 1_555 1_555 yes F(2) P(1) F(6) 84.3(10) . 1_555 1_555 yes F(3) P(1) F(4) 168(1) . 1_555 1_555 yes F(3) P(1) F(5) 102(1) . 1_555 1_555 yes F(3) P(1) F(6) 82(1) . 1_555 1_555 yes F(4) P(1) F(5) 86(1) . 1_555 1_555 yes F(4) P(1) F(6) 88(1) . 1_555 1_555 yes F(5) P(1) F(6) 174(1) . 1_555 1_555 yes F(7) P(2) F(8) 175.4(9) . 1_555 1_555 yes F(7) P(2) F(9) 84.9(9) . 1_555 1_555 yes F(7) P(2) F(10) 91.2(8) . 1_555 1_555 yes F(7) P(2) F(11) 88(1) . 1_555 1_555 yes F(7) P(2) F(12) 93.9(9) . 1_555 1_555 yes F(8) P(2) F(9) 98.6(9) . 1_555 1_555 yes F(8) P(2) F(10) 85.1(8) . 1_555 1_555 yes F(8) P(2) F(11) 88(1) . 1_555 1_555 yes F(8) P(2) F(12) 89.0(8) . 1_555 1_555 yes F(9) P(2) F(10) 173(1) . 1_555 1_555 yes F(9) P(2) F(11) 87(1) . 1_555 1_555 yes F(9) P(2) F(12) 91(1) . 1_555 1_555 yes F(10) P(2) F(11) 87(1) . 1_555 1_555 yes F(10) P(2) F(12) 93(1) . 1_555 1_555 yes F(11) P(2) F(12) 177(1) . 1_555 1_555 yes Cu(1) N(1) C(1) 123.9(5) . 1_555 1_555 yes Cu(1) N(1) C(5) 118.2(6) . 1_555 1_555 yes C(1) N(1) C(5) 116.6(8) . 1_555 1_555 yes Cu(2) N(2) C(6) 123.5(4) . 1_555 1_555 yes Cu(2) N(2) C(10) 119.1(6) . 1_555 1_555 yes C(6) N(2) C(10) 116.3(7) . 1_555 1_555 yes Cu(1) N(3) C(15) 120.6(5) . 1_555 1_555 yes Cu(1) N(3) C(19) 123.0(5) . 1_555 1_555 yes C(15) N(3) C(19) 116.3(7) . 1_555 1_555 yes Cu(2) N(4) C(20) 121.8(5) . 2_466 1_555 yes Cu(2) N(4) C(24) 122.1(5) . 2_466 1_555 yes C(20) N(4) C(24) 116.0(6) . 1_555 1_555 yes Cu(1) N(5) C(29) 122.5(6) . 1_555 1_555 yes Cu(1) N(5) C(33) 120.2(4) . 1_555 1_555 yes C(29) N(5) C(33) 117.0(7) . 1_555 1_555 yes Cu(2) N(6) C(34) 125.5(6) . 1_756 1_555 yes Cu(2) N(6) C(38) 117.0(4) . 1_756 1_555 yes C(34) N(6) C(38) 116.6(6) . 1_555 1_555 yes Cu(1) N(7) C(43) 166.7(9) . 1_555 1_555 yes Cu(2) N(8) C(45) 173.7(6) . 1_555 1_555 yes N(1) C(1) C(2) 123.8(6) . 1_555 1_555 yes C(1) C(2) C(3) 118.9(7) . 1_555 1_555 yes C(2) C(3) C(4) 117.6(8) . 1_555 1_555 yes C(2) C(3) C(11) 123.0(7) . 1_555 1_555 yes C(4) C(3) C(11) 119.4(6) . 1_555 1_555 yes C(3) C(4) C(5) 119.9(6) . 1_555 1_555 yes N(1) C(5) C(4) 123.0(7) . 1_555 1_555 yes N(2) C(6) C(7) 123.6(6) . 1_555 1_555 yes C(6) C(7) C(8) 119.4(8) . 1_555 1_555 yes C(7) C(8) C(9) 117.2(9) . 1_555 1_555 yes C(7) C(8) C(14) 119.8(8) . 1_555 1_555 yes C(9) C(8) C(14) 123.0(6) . 1_555 1_555 yes C(8) C(9) C(10) 119.4(6) . 1_555 1_555 yes N(2) C(10) C(9) 124.1(8) . 1_555 1_555 yes C(3) C(11) C(12) 177.0(8) . 1_555 1_555 yes C(11) C(12) C(13) 176.2(8) . 1_555 1_555 yes C(12) C(13) C(14) 177.8(8) . 1_555 1_555 yes C(8) C(14) C(13) 179.8(8) . 1_555 1_555 yes N(3) C(15) C(16) 124.3(8) . 1_555 1_555 yes C(15) C(16) C(17) 118.2(8) . 1_555 1_555 yes C(16) C(17) C(18) 116.9(7) . 1_555 1_555 yes C(16) C(17) C(25) 122.4(7) . 1_555 1_555 yes C(18) C(17) C(25) 120.5(7) . 1_555 1_555 yes C(17) C(18) C(19) 120.8(8) . 1_555 1_555 yes N(3) C(19) C(18) 123.4(7) . 1_555 1_555 yes N(4) C(20) C(21) 125.4(7) . 1_555 1_555 yes C(20) C(21) C(22) 117.8(7) . 1_555 1_555 yes C(21) C(22) C(23) 117.6(7) . 1_555 1_555 yes C(21) C(22) C(28) 121.0(7) . 1_555 1_555 yes C(23) C(22) C(28) 121.5(7) . 1_555 1_555 yes C(22) C(23) C(24) 120.4(7) . 1_555 1_555 yes N(4) C(24) C(23) 122.8(7) . 1_555 1_555 yes C(17) C(25) C(26) 176.2(9) . 1_555 1_555 yes C(25) C(26) C(27) 178(1) . 1_555 1_555 yes C(26) C(27) C(28) 178.7(7) . 1_555 1_555 yes C(22) C(28) C(27) 177.8(9) . 1_555 1_555 yes N(5) C(29) C(30) 124(1) . 1_555 1_555 yes C(29) C(30) C(31) 118.5(8) . 1_555 1_555 yes C(30) C(31) C(32) 117.6(7) . 1_555 1_555 yes C(30) C(31) C(39) 121.1(7) . 1_555 1_555 yes C(32) C(31) C(39) 121.3(10) . 1_555 1_555 yes C(31) C(32) C(33) 119(1) . 1_555 1_555 yes N(5) C(33) C(32) 122.8(7) . 1_555 1_555 yes N(6) C(34) C(35) 123.8(9) . 1_555 1_555 yes C(34) C(35) C(36) 119.5(7) . 1_555 1_555 yes C(35) C(36) C(37) 117.8(6) . 1_555 1_555 yes C(35) C(36) C(42) 121.8(7) . 1_555 1_555 yes C(37) C(36) C(42) 120.3(9) . 1_555 1_555 yes C(36) C(37) C(38) 119.2(9) . 1_555 1_555 yes N(6) C(38) C(37) 123.0(7) . 1_555 1_555 yes C(31) C(39) C(40) 179(1) . 1_555 1_555 yes C(39) C(40) C(41) 177.9(9) . 1_555 1_555 yes C(40) C(41) C(42) 177(1) . 1_555 1_555 yes C(36) C(42) C(41) 174.8(9) . 1_555 1_555 yes N(7) C(43) C(44) 176(1) . 1_555 1_555 yes N(8) C(45) C(46) 176.9(8) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(2) C(1) 3.19(2) . 2_666 ? F(2) C(2) 3.39(1) . 2_666 ? F(2) C(6) 3.49(2) . 1_656 ? F(2) C(23) 3.55(2) . 1_655 ? F(3) C(23) 3.42(2) . 1_655 ? F(4) C(34) 3.25(2) . 1_455 ? F(5) C(29) 3.41(2) . 2_666 ? F(5) C(30) 3.56(3) . 2_666 ? F(6) C(23) 3.28(3) . 1_655 ? F(6) C(24) 3.54(3) . 1_655 ? F(7) C(37) 3.28(1) . 1_444 ? F(7) C(38) 3.33(2) . 1_444 ? F(8) C(10) 3.33(1) . 2_565 ? F(9) C(5) 3.37(2) . 2_555 ? F(9) C(37) 3.42(2) . 1_444 ? F(9) C(38) 3.45(2) . 1_444 ? F(9) C(4) 3.51(2) . 2_555 ? F(10) C(10) 3.39(1) . 2_565 ? F(11) C(44) 3.47(3) . 2_555 ? F(11) C(43) 3.48(3) . 2_555 ? F(11) C(15) 3.51(2) . 2_555 ? F(12) C(45) 3.30(1) . 2_565 ? F(12) C(45) 3.33(2) . 1_645 ? F(12) C(46) 3.43(2) . 2_565 ? F(12) C(46) 3.44(2) . 1_645 ? F(12) N(8) 3.57(1) . 2_565 ? N(4) N(6) 3.235(7) . 2_667 ? N(6) N(8) 3.202(7) . 1_756 ? N(6) C(20) 3.397(9) . 2_667 ? N(7) C(45) 3.58(1) . 2_565 ? C(1) C(41) 3.57(1) . 2_666 ? C(2) C(41) 3.57(1) . 2_666 ? C(3) C(14) 3.51(1) . 2_565 ? C(5) C(9) 3.58(1) . 2_565 ? C(11) C(13) 3.45(1) . 2_565 ? C(11) C(35) 3.51(1) . 2_666 ? C(11) C(14) 3.60(1) . 2_565 ? C(12) C(12) 3.43(2) . 2_565 ? C(12) C(35) 3.53(1) . 2_666 ? C(12) C(20) 3.550(10) . 1_554 ? C(31) C(37) 3.58(1) . 2_766 ? C(36) C(39) 3.54(1) . 2_766 ? C(37) C(39) 3.52(1) . 2_766 ? C(40) C(42) 3.50(1) . 2_766 ? C(41) C(41) 3.49(2) . 2_766 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_2 #{[Ag(4-bpbd)]NO3.CH3CN}n 2a.CH3CN #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H11 Ag N4 O3 ' _chemical_formula_moiety 'C16 H11 Ag N4 O3 ' _chemical_formula_weight 415.16 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.739(6) _cell_length_b 7.644(4) _cell_length_c 7.582(5) _cell_angle_alpha 75.66(5) _cell_angle_beta 89.36(5) _cell_angle_gamma 80.00(4) _cell_volume 814.7(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.2 _cell_measurement_theta_max 19.1 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.778 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method w-2q _diffrn_reflns_number 4004 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.05 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3723 _reflns_number_gt 2644 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1233 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2644 _refine_ls_number_parameters 218 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.0661P)^2^+0.4519P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_diff_density_max 0.85 _refine_diff_density_min -0.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag(1) Ag 0.05580(2) 0.60769(6) -0.36039(4) 0.0700(2) Uani 1.00 d . . . O(1) O 0.0632(3) 0.2357(5) -0.3522(6) 0.093(1) Uani 1.00 d . . . O(2) O 0.0403(6) -0.017(1) -0.250(3) 0.41(1) Uani 1.00 d . . . O(3) O 0.1694(3) 0.0069(7) -0.2605(8) 0.128(2) Uani 1.00 d . . . N(1) N 0.1896(2) 0.5896(5) -0.4847(4) 0.0511(7) Uani 1.00 d . . . N(2) N 0.9354(2) 0.5899(5) -1.1933(4) 0.0499(7) Uani 1.00 d . . . N(3) N 0.5530(4) 0.9424(8) -0.255(1) 0.136(3) Uani 1.00 d . . . N(4) N 0.0874(3) 0.0736(6) -0.2926(8) 0.086(1) Uani 1.00 d . . . C(1) C 0.2386(2) 0.4307(6) -0.5019(5) 0.0493(8) Uani 1.00 d . . . C(2) C 0.3238(2) 0.4171(6) -0.5795(5) 0.0500(9) Uani 1.00 d . . . C(3) C 0.3611(2) 0.5745(6) -0.6421(5) 0.0479(8) Uani 1.00 d . . . C(4) C 0.3108(3) 0.7389(6) -0.6238(7) 0.061(1) Uani 1.00 d . . . C(5) C 0.2262(3) 0.7395(6) -0.5457(7) 0.063(1) Uani 1.00 d . . . C(6) C 0.8835(3) 0.7420(6) -1.1699(7) 0.061(1) Uani 1.00 d . . . C(7) C 0.8020(3) 0.7404(6) -1.0760(7) 0.062(1) Uani 1.00 d . . . C(8) C 0.7713(2) 0.5763(6) -1.0079(5) 0.0451(8) Uani 1.00 d . . . C(9) C 0.8268(2) 0.4182(6) -1.0278(5) 0.0497(8) Uani 1.00 d . . . C(10) C 0.9075(2) 0.4299(6) -1.1215(5) 0.0503(9) Uani 1.00 d . . . C(11) C 0.4503(2) 0.5681(6) -0.7204(5) 0.0527(9) Uani 1.00 d . . . C(12) C 0.5247(2) 0.5679(6) -0.7854(5) 0.0514(9) Uani 1.00 d . . . C(13) C 0.6100(2) 0.5683(6) -0.8595(5) 0.0490(8) Uani 1.00 d . . . C(14) C 0.6841(2) 0.5718(6) -0.9246(5) 0.0516(9) Uani 1.00 d . . . C(15) C 0.4780(4) 0.9397(7) -0.2307(9) 0.079(1) Uani 1.00 d . . . C(16) C 0.3846(5) 0.9336(9) -0.195(1) 0.103(2) Uani 1.00 d . . . H(1) H 0.2136 0.3220 -0.4586 0.0591 Uiso 1.00 calc . . . H(2) H 0.3563 0.3016 -0.5899 0.0600 Uiso 1.00 calc . . . H(3) H 0.3343 0.8497 -0.6647 0.0737 Uiso 1.00 calc . . . H(4) H 0.1921 0.8535 -0.5346 0.0756 Uiso 1.00 calc . . . H(5) H 0.9027 0.8562 -1.2190 0.0735 Uiso 1.00 calc . . . H(6) H 0.7675 0.8515 -1.0586 0.0747 Uiso 1.00 calc . . . H(7) H 0.8099 0.3021 -0.9776 0.0596 Uiso 1.00 calc . . . H(8) H 0.9448 0.3199 -1.1357 0.0604 Uiso 1.00 calc . . . H(9) H 0.3660 0.9961 -0.1031 0.1236 Uiso 1.00 calc . . . H(10) H 0.3481 0.9912 -0.3029 0.1236 Uiso 1.00 calc . . . H(11) H 0.3766 0.8095 -0.1543 0.1236 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0303(2) 0.1143(4) 0.0641(2) -0.0152(2) 0.0235(1) -0.0191(2) O(1) 0.081(3) 0.069(2) 0.120(3) -0.010(2) 0.009(2) -0.007(2) O(2) 0.135(7) 0.131(6) 0.92(4) -0.078(6) 0.06(1) 0.00(1) O(3) 0.086(3) 0.111(3) 0.167(5) 0.028(3) 0.007(3) -0.028(3) N(1) 0.029(1) 0.074(2) 0.050(2) -0.012(1) 0.017(1) -0.014(2) N(2) 0.028(1) 0.073(2) 0.048(2) -0.011(1) 0.012(1) -0.013(1) N(3) 0.091(4) 0.091(4) 0.232(8) -0.029(3) 0.053(5) -0.043(4) N(4) 0.064(3) 0.052(2) 0.138(4) -0.011(2) 0.043(3) -0.014(2) C(1) 0.034(2) 0.067(2) 0.047(2) -0.014(2) 0.011(1) -0.010(2) C(2) 0.032(2) 0.065(2) 0.051(2) -0.007(2) 0.013(1) -0.014(2) C(3) 0.028(1) 0.074(2) 0.043(2) -0.013(2) 0.012(1) -0.015(2) C(4) 0.046(2) 0.065(3) 0.079(3) -0.019(2) 0.025(2) -0.022(2) C(5) 0.045(2) 0.065(3) 0.081(3) -0.010(2) 0.029(2) -0.023(2) C(6) 0.042(2) 0.065(3) 0.078(3) -0.018(2) 0.023(2) -0.014(2) C(7) 0.045(2) 0.067(3) 0.081(3) -0.015(2) 0.029(2) -0.029(2) C(8) 0.029(1) 0.067(2) 0.043(2) -0.014(1) 0.012(1) -0.018(2) C(9) 0.034(2) 0.059(2) 0.052(2) -0.011(2) 0.010(1) -0.005(2) C(10) 0.033(2) 0.065(2) 0.051(2) -0.003(2) 0.008(1) -0.013(2) C(11) 0.034(2) 0.077(3) 0.049(2) -0.014(2) 0.013(1) -0.017(2) C(12) 0.032(2) 0.073(3) 0.051(2) -0.014(2) 0.015(1) -0.017(2) C(13) 0.033(2) 0.068(2) 0.048(2) -0.014(2) 0.015(1) -0.015(2) C(14) 0.033(2) 0.077(3) 0.049(2) -0.015(2) 0.014(1) -0.021(2) C(15) 0.078(3) 0.055(3) 0.106(4) -0.014(2) 0.020(3) -0.022(3) C(16) 0.074(4) 0.094(4) 0.141(6) -0.013(3) 0.008(4) -0.032(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.174(3) . . yes Ag(1) N(2) 2.172(3) . 1_456 yes O(1) N(4) 1.200(6) . . yes O(2) N(4) 1.06(1) . . yes O(3) N(4) 1.229(7) . . yes N(1) C(1) 1.337(5) . . yes N(1) C(5) 1.328(6) . . yes N(2) C(6) 1.327(6) . . yes N(2) C(10) 1.343(5) . . yes N(3) C(15) 1.121(9) . . yes C(1) C(2) 1.379(5) . . yes C(2) C(3) 1.385(6) . . yes C(3) C(4) 1.381(6) . . yes C(3) C(11) 1.435(5) . . yes C(4) C(5) 1.374(6) . . yes C(6) C(7) 1.390(6) . . yes C(7) C(8) 1.384(6) . . yes C(8) C(9) 1.378(6) . . yes C(8) C(14) 1.428(5) . . yes C(9) C(10) 1.384(5) . . yes C(11) C(12) 1.198(5) . . yes C(12) C(13) 1.371(5) . . yes C(13) C(14) 1.195(5) . . yes C(15) C(16) 1.408(9) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(2) 169.5(1) . 1_555 1_456 yes Ag(1) N(1) C(1) 122.5(3) . 1_555 1_555 yes Ag(1) N(1) C(5) 120.2(3) . 1_555 1_555 yes C(1) N(1) C(5) 117.3(3) . 1_555 1_555 yes Ag(1) N(2) C(6) 119.8(3) . 1_654 1_555 yes Ag(1) N(2) C(10) 122.2(3) . 1_654 1_555 yes C(6) N(2) C(10) 117.9(3) . 1_555 1_555 yes O(1) N(4) O(2) 122.7(6) . 1_555 1_555 yes O(1) N(4) O(3) 120.9(5) . 1_555 1_555 yes O(2) N(4) O(3) 116.0(6) . 1_555 1_555 yes N(1) C(1) C(2) 123.1(4) . 1_555 1_555 yes C(1) C(2) C(3) 118.9(4) . 1_555 1_555 yes C(2) C(3) C(4) 118.2(3) . 1_555 1_555 yes C(2) C(3) C(11) 121.4(4) . 1_555 1_555 yes C(4) C(3) C(11) 120.5(4) . 1_555 1_555 yes C(3) C(4) C(5) 118.9(4) . 1_555 1_555 yes N(1) C(5) C(4) 123.7(4) . 1_555 1_555 yes N(2) C(6) C(7) 122.4(4) . 1_555 1_555 yes C(6) C(7) C(8) 119.8(4) . 1_555 1_555 yes C(7) C(8) C(9) 117.5(3) . 1_555 1_555 yes C(7) C(8) C(14) 121.2(4) . 1_555 1_555 yes C(9) C(8) C(14) 121.3(4) . 1_555 1_555 yes C(8) C(9) C(10) 119.5(4) . 1_555 1_555 yes N(2) C(10) C(9) 122.8(4) . 1_555 1_555 yes C(3) C(11) C(12) 178.1(5) . 1_555 1_555 yes C(11) C(12) C(13) 179.8(5) . 1_555 1_555 yes C(12) C(13) C(14) 178.9(5) . 1_555 1_555 yes C(8) C(14) C(13) 178.1(4) . 1_555 1_555 yes N(3) C(15) C(16) 178.4(7) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(1) 2.706(4) . 2_564 ? Ag(1) O(2) 3.15(1) . 1_565 ? Ag(1) C(9) 3.376(4) . 2_664 ? Ag(1) N(4) 3.532(4) . 2_564 ? Ag(1) Ag(1) 3.5558(9) . 2_564 ? O(1) N(2) 3.374(5) . 2_663 ? O(2) C(6) 3.16(1) . 1_446 ? O(2) C(9) 3.53(1) . 2_654 ? O(2) N(2) 3.54(1) . 1_446 ? O(3) C(16) 3.147(8) . 1_545 ? O(3) C(5) 3.333(8) . 1_545 ? O(3) C(9) 3.429(6) . 2_654 ? N(1) C(10) 3.373(5) . 2_663 ? N(1) C(14) 3.472(5) . 2_664 ? N(2) C(10) 3.302(5) . 2_763 ? N(2) N(2) 3.366(6) . 2_763 ? N(2) C(1) 3.521(5) . 2_663 ? N(3) C(4) 3.370(8) . 2_674 ? N(3) C(2) 3.514(8) . 2_664 ? N(3) C(14) 3.568(7) . 1_556 ? N(3) C(13) 3.586(8) . 1_556 ? C(1) C(10) 3.430(5) . 2_663 ? C(1) C(14) 3.435(6) . 2_664 ? C(1) C(9) 3.554(5) . 2_663 ? C(1) C(13) 3.555(6) . 2_664 ? C(2) C(8) 3.427(6) . 2_663 ? C(2) C(13) 3.513(6) . 2_664 ? C(2) C(9) 3.563(5) . 2_663 ? C(3) C(12) 3.501(5) . 2_664 ? C(11) C(11) 3.501(7) . 2_664 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_3 #{[Ag(4-bpbd)]ClO4.(CH3)2CO}n 2b.(CH3)2CO #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H14 Ag Cl N2 O5 ' _chemical_formula_moiety 'C17 H14 Ag Cl N2 O5 ' _chemical_formula_weight 469.63 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z -x,-y,-z x,1/2-y,z _cell_length_a 5.296(2) _cell_length_b 15.876(6) _cell_length_c 10.889(3) _cell_angle_alpha 90 _cell_angle_beta 100.47(4) _cell_angle_gamma 90 _cell_volume 900.3(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.4 _cell_measurement_theta_max 24.9 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.678 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method w-2q _diffrn_reflns_number 1829 _diffrn_reflns_av_R_equivalents 0.007 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.98 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.69 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1646 _reflns_number_gt 1424 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0708 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1424 _refine_ls_number_parameters 131 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.0394P)^2^+0.4167P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0061 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_diff_density_max 0.44 _refine_diff_density_min -0.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag(1) Ag 0.5000 0.0000 0.5000 0.04381(6) Uani 1.00 d S . . Cl(1) Cl 0.5617(1) 0.2500 0.52267(6) 0.0492(2) Uani 1.00 d S . . O(1) O 0.8244(4) 0.2500 0.5091(3) 0.0857(8) Uani 1.00 d S . . O(2) O 0.4376(3) 0.17655(9) 0.4649(2) 0.0707(4) Uani 1.00 d . . . O(3) O 0.5375(6) 0.2500 0.6512(2) 0.0896(8) Uani 1.00 d S . . O(4) O 0.0981(8) 0.2500 0.0270(5) 0.185(2) Uani 1.00 d S . . N(1) N 0.7743(3) -0.00234(8) 0.3752(1) 0.0368(4) Uani 1.00 d . . . C(1) C 0.8548(4) 0.0693(1) 0.3315(2) 0.0477(4) Uani 1.00 d . . . C(2) C 1.0213(4) 0.0721(1) 0.2483(2) 0.0493(5) Uani 1.00 d . . . C(3) C 1.1125(3) -0.0025(1) 0.2071(2) 0.0376(4) Uani 1.00 d . . . C(4) C 1.0358(4) -0.0770(1) 0.2556(2) 0.0494(5) Uani 1.00 d . . . C(5) C 0.8680(4) -0.0743(1) 0.3383(2) 0.0473(5) Uani 1.00 d . . . C(6) C 1.2809(4) -0.0020(1) 0.1186(2) 0.0435(5) Uani 1.00 d . . . C(7) C 1.4194(4) -0.0008(1) 0.0431(2) 0.0437(5) Uani 1.00 d . . . C(8) C 0.5091(9) 0.2500 0.1494(4) 0.098(1) Uani 1.00 d S . . C(9) C 0.3227(8) 0.2500 0.0310(4) 0.088(1) Uani 1.00 d S . . C(10) C 0.418(1) 0.2500 -0.0854(5) 0.147(2) Uani 1.00 d S . . H(1) H 0.7939 0.1210 0.3591 0.0573 Uiso 1.00 calc . . . H(2) H 1.0733 0.1247 0.2194 0.0591 Uiso 1.00 calc . . . H(3) H 1.0985 -0.1295 0.2319 0.0593 Uiso 1.00 calc . . . H(4) H 0.8165 -0.1258 0.3706 0.0568 Uiso 1.00 calc . . . H(5) H 0.4862 0.2011 0.1914 0.1197 Uiso 1.00 calc . . . H(6) H 0.6745 0.2500 0.1236 0.1197 Uiso 1.00 calc S . . H(8) H 0.5979 0.2500 -0.0677 0.1871 Uiso 1.00 calc S . . H(9) H 0.3532 0.2016 -0.1321 0.1871 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.03645(9) 0.0651(1) 0.0373(1) 0.00133(7) 0.02666(7) 0.00141(8) Cl(1) 0.0573(3) 0.0342(3) 0.0649(4) 0.0000 0.0345(3) 0.0000 O(1) 0.056(1) 0.069(1) 0.141(2) 0.0000 0.042(1) 0.0000 O(2) 0.0859(9) 0.0437(8) 0.0932(10) -0.0138(7) 0.0444(8) -0.0134(7) O(3) 0.135(2) 0.082(2) 0.059(1) 0.0000 0.038(1) 0.0000 O(4) 0.087(2) 0.251(6) 0.224(5) 0.0000 0.042(2) 0.0000 N(1) 0.0331(7) 0.0497(8) 0.0328(7) 0.0007(5) 0.0199(6) -0.0004(5) C(1) 0.0561(9) 0.0444(10) 0.0527(9) -0.0004(8) 0.0365(8) -0.0027(8) C(2) 0.0556(9) 0.048(1) 0.0540(9) -0.0057(8) 0.0365(8) 0.0028(8) C(3) 0.0301(8) 0.057(1) 0.0302(8) -0.0005(7) 0.0171(7) -0.0004(7) C(4) 0.0560(9) 0.046(1) 0.0552(10) 0.0066(8) 0.0355(8) -0.0001(8) C(5) 0.0530(9) 0.044(1) 0.0538(9) -0.0006(8) 0.0338(8) 0.0032(8) C(6) 0.0356(9) 0.063(1) 0.0363(9) -0.0004(7) 0.0188(7) 0.0006(7) C(7) 0.0351(8) 0.064(1) 0.0367(9) 0.0008(7) 0.0194(8) -0.0002(7) C(8) 0.106(3) 0.108(3) 0.077(2) 0.0000 0.005(2) 0.0000 C(9) 0.101(3) 0.070(2) 0.103(3) 0.0000 0.045(2) 0.0000 C(10) 0.238(6) 0.125(4) 0.094(3) 0.0000 0.072(4) 0.0000 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.162(2) . . yes Ag(1) N(1) 2.162(2) . 3_656 yes Cl(1) O(1) 1.426(3) . . yes Cl(1) O(2) 1.427(2) . . yes Cl(1) O(2) 1.427(2) . 4_555 yes Cl(1) O(3) 1.428(3) . . yes O(4) C(9) 1.182(6) . . yes N(1) C(1) 1.333(2) . . yes N(1) C(5) 1.336(2) . . yes C(1) C(2) 1.375(3) . . yes C(2) C(3) 1.385(3) . . yes C(3) C(4) 1.386(3) . . yes C(3) C(6) 1.427(3) . . yes C(4) C(5) 1.376(3) . . yes C(6) C(7) 1.198(3) . . yes C(7) C(7) 1.378(4) . 3_855 yes C(8) C(9) 1.475(6) . . yes C(9) C(10) 1.447(8) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(1) 180.0 . 1_555 3_656 yes O(1) Cl(1) O(2) 109.52(9) . 1_555 1_555 yes O(1) Cl(1) O(2) 109.52(9) . 1_555 4_555 yes O(1) Cl(1) O(3) 111.4(2) . 1_555 1_555 yes O(2) Cl(1) O(2) 109.6(1) . 1_555 4_555 yes O(2) Cl(1) O(3) 108.40(10) . 1_555 1_555 yes O(2) Cl(1) O(3) 108.40(10) . 4_555 1_555 yes Ag(1) N(1) C(1) 120.3(1) . 1_555 1_555 yes Ag(1) N(1) C(5) 122.2(1) . 1_555 1_555 yes C(1) N(1) C(5) 117.5(2) . 1_555 1_555 yes N(1) C(1) C(2) 123.2(2) . 1_555 1_555 yes C(1) C(2) C(3) 119.3(2) . 1_555 1_555 yes C(2) C(3) C(4) 117.6(2) . 1_555 1_555 yes C(2) C(3) C(6) 120.8(2) . 1_555 1_555 yes C(4) C(3) C(6) 121.6(2) . 1_555 1_555 yes C(3) C(4) C(5) 119.4(2) . 1_555 1_555 yes N(1) C(5) C(4) 122.9(2) . 1_555 1_555 yes C(3) C(6) C(7) 178.9(2) . 1_555 1_555 yes C(6) C(7) C(7) 179.5(3) . 1_555 3_855 yes O(4) C(9) C(8) 122.7(5) . 1_555 1_555 yes O(4) C(9) C(10) 118.5(5) . 1_555 1_555 yes C(8) C(9) C(10) 118.8(4) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(2) 2.840(1) . . ? Ag(1) O(2) 2.840(1) . 3_656 ? Ag(1) C(3) 3.465(2) . 1_455 ? Ag(1) C(3) 3.465(2) . 3_756 ? Ag(1) C(4) 3.499(2) . 1_455 ? Ag(1) C(4) 3.499(2) . 3_756 ? Ag(1) C(2) 3.567(2) . 1_455 ? Ag(1) C(2) 3.567(2) . 3_756 ? O(1) C(1) 3.479(3) . . ? O(1) C(1) 3.479(3) . 4_555 ? O(1) C(5) 3.495(2) . 2_756 ? O(1) C(5) 3.495(2) . 3_756 ? O(1) O(2) 3.565(3) . 1_655 ? O(1) O(2) 3.565(3) . 4_655 ? O(2) C(1) 3.325(3) . . ? O(2) C(5) 3.332(3) . 3_656 ? O(2) C(2) 3.359(2) . 1_455 ? O(2) N(1) 3.557(2) . 3_656 ? O(2) N(1) 3.582(2) . . ? O(2) C(1) 3.593(3) . 1_455 ? O(3) C(10) 3.047(7) . 1_556 ? O(3) C(5) 3.535(3) . 2_656 ? O(3) C(5) 3.535(3) . 3_656 ? O(3) C(4) 3.584(3) . 2_756 ? O(3) C(4) 3.584(3) . 3_756 ? O(4) C(10) 3.588(8) . 1_455 ? N(1) N(1) 3.278(3) . 3_756 ? N(1) C(6) 3.461(2) . 1_455 ? N(1) C(5) 3.557(2) . 3_756 ? N(1) C(1) 3.593(2) . 3_756 ? C(3) C(7) 3.546(3) . 3_755 ? C(6) C(6) 3.569(4) . 3_755 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_4 #{[Ag(4-bpbd)]CF3SO3.(CH3)2CO}n 2c.(CH3)2CO #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H14 Ag F3 N2 O4 S ' _chemical_formula_moiety 'C18 H14 Ag F3 N2 O4 S ' _chemical_formula_weight 519.24 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 10.157(3) _cell_length_b 17.818(7) _cell_length_c 11.399(3) _cell_angle_alpha 90 _cell_angle_beta 104.98(2) _cell_angle_gamma 90 _cell_volume 1992.8(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.6 _cell_measurement_theta_max 22.8 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.792 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method w-2q _diffrn_reflns_number 4824 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.53 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.10 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4570 _reflns_number_gt 2583 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1788 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2583 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.0808P)^2^+3.4783P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_diff_density_max 0.78 _refine_diff_density_min -0.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag(1) Ag 0.33218(4) 0.24295(3) 0.24348(4) 0.0617(2) Uani 1.00 d . . . S(1) S 0.2912(2) 0.0168(1) 0.2454(3) 0.0891(7) Uani 1.00 d . . . F(1) F 0.481(2) -0.0168(9) 0.157(1) 0.32(1) Uani 1.00 d . . . F(2) F 0.450(1) -0.0959(4) 0.253(1) 0.282(7) Uani 1.00 d . . . F(3) F 0.541(1) -0.0084(9) 0.324(1) 0.33(1) Uani 1.00 d . . . O(1) O 0.196(1) -0.0187(8) 0.172(2) 0.33(1) Uani 1.00 d . . . O(2) O 0.3159(7) 0.0901(4) 0.2335(8) 0.148(4) Uani 1.00 d . . . O(3) O 0.277(2) 0.0059(10) 0.356(2) 0.36(1) Uani 1.00 d . . . O(4) O 0.8479(7) 0.0963(5) 0.2556(8) 0.147(4) Uani 1.00 d . . . N(1) N 0.5297(4) 0.2394(3) 0.3724(4) 0.046(1) Uani 1.00 d . . . N(2) N 1.6342(4) 0.2513(3) 1.1135(4) 0.047(1) Uani 1.00 d . . . C(1) C 0.5794(6) 0.1748(4) 0.4265(6) 0.054(2) Uani 1.00 d . . . C(2) C 0.7047(6) 0.1690(3) 0.5110(5) 0.051(1) Uani 1.00 d . . . C(3) C 0.7839(5) 0.2325(3) 0.5400(5) 0.041(1) Uani 1.00 d . . . C(4) C 0.7342(5) 0.2992(4) 0.4829(5) 0.048(1) Uani 1.00 d . . . C(5) C 0.6078(6) 0.3010(4) 0.4010(5) 0.050(1) Uani 1.00 d . . . C(6) C 0.9140(5) 0.2299(3) 0.6269(5) 0.045(1) Uani 1.00 d . . . C(7) C 1.0220(5) 0.2310(3) 0.6995(5) 0.045(1) Uani 1.00 d . . . C(8) C 1.1461(5) 0.2326(3) 0.7830(5) 0.046(1) Uani 1.00 d . . . C(9) C 1.2538(5) 0.2361(3) 0.8569(5) 0.046(1) Uani 1.00 d . . . C(10) C 1.5673(6) 0.3130(4) 1.0623(6) 0.052(1) Uani 1.00 d . . . C(11) C 1.4437(5) 0.3102(3) 0.9780(5) 0.050(1) Uani 1.00 d . . . C(12) C 1.3824(5) 0.2414(3) 0.9450(4) 0.043(1) Uani 1.00 d . . . C(13) C 1.4489(6) 0.1785(3) 1.0007(6) 0.056(2) Uani 1.00 d . . . C(14) C 1.5734(6) 0.1860(4) 1.0831(6) 0.056(2) Uani 1.00 d . . . C(15) C 0.438(1) -0.0297(6) 0.246(1) 0.112(4) Uani 1.00 d . . . C(16) C 0.865(2) -0.021(1) 0.169(2) 0.206(9) Uani 1.00 d . . . C(17) C 0.861(1) 0.0324(6) 0.249(1) 0.121(4) Uani 1.00 d . . . C(18) C 0.900(4) -0.014(2) 0.355(4) 0.40(2) Uani 1.00 d . . . H(1) H 0.5260 0.1307 0.4058 0.0652 Uiso 1.00 calc . . . H(2) H 0.7352 0.1222 0.5481 0.0607 Uiso 1.00 calc . . . H(3) H 0.7873 0.3437 0.5002 0.0575 Uiso 1.00 calc . . . H(4) H 0.5748 0.3474 0.3634 0.0606 Uiso 1.00 calc . . . H(5) H 1.6075 0.3606 1.0855 0.0625 Uiso 1.00 calc . . . H(6) H 1.4005 0.3551 0.9427 0.0606 Uiso 1.00 calc . . . H(7) H 1.4089 0.1303 0.9823 0.0675 Uiso 1.00 calc . . . H(8) H 1.6182 0.1420 1.1201 0.0670 Uiso 1.00 calc . . . H(9) H 0.8029 -0.0600 0.1744 0.2469 Uiso 1.00 calc . . . H(10) H 0.8415 -0.0007 0.0892 0.2469 Uiso 1.00 calc . . . H(11) H 0.9549 -0.0413 0.1857 0.2469 Uiso 1.00 calc . . . H(12) H 0.8361 -0.0536 0.3495 0.4756 Uiso 1.00 calc . . . H(13) H 0.9880 -0.0349 0.3605 0.4756 Uiso 1.00 calc . . . H(14) H 0.9033 0.0150 0.4254 0.4756 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0274(2) 0.1065(5) 0.0408(3) 0.0038(2) -0.0098(2) 0.0011(3) S(1) 0.079(1) 0.058(1) 0.121(2) -0.0045(10) 0.010(1) 0.009(1) F(1) 0.37(2) 0.33(2) 0.35(2) 0.16(2) 0.29(2) 0.13(2) F(2) 0.31(1) 0.058(5) 0.51(2) 0.056(6) 0.16(1) 0.008(8) F(3) 0.156(8) 0.35(2) 0.40(2) 0.160(10) -0.10(1) -0.21(2) O(1) 0.115(7) 0.28(1) 0.54(3) -0.054(8) -0.01(1) -0.30(2) O(2) 0.095(5) 0.067(4) 0.24(1) 0.011(3) -0.025(5) 0.011(5) O(3) 0.49(3) 0.33(2) 0.37(2) 0.24(2) 0.33(2) 0.23(2) O(4) 0.094(5) 0.086(5) 0.22(1) 0.005(4) -0.030(5) -0.006(5) N(1) 0.025(2) 0.068(3) 0.036(2) 0.002(2) -0.005(2) -0.005(2) N(2) 0.028(2) 0.069(3) 0.035(2) -0.003(2) -0.005(2) -0.004(2) C(1) 0.035(3) 0.062(4) 0.057(4) -0.007(3) -0.003(3) -0.009(3) C(2) 0.038(3) 0.057(4) 0.048(3) 0.003(2) -0.004(2) 0.002(3) C(3) 0.024(2) 0.060(4) 0.033(2) -0.004(2) -0.002(2) -0.001(2) C(4) 0.031(3) 0.058(4) 0.049(3) -0.008(2) -0.002(2) -0.002(3) C(5) 0.037(3) 0.067(4) 0.043(3) 0.005(3) 0.002(2) 0.011(3) C(6) 0.030(3) 0.061(4) 0.038(3) 0.000(2) -0.001(2) -0.001(2) C(7) 0.027(2) 0.059(4) 0.043(3) -0.003(2) 0.000(2) 0.001(2) C(8) 0.031(3) 0.063(4) 0.038(3) -0.004(2) -0.004(2) 0.004(2) C(9) 0.027(2) 0.069(4) 0.036(3) -0.005(2) -0.001(2) 0.000(2) C(10) 0.037(3) 0.056(4) 0.052(3) -0.006(3) -0.008(2) -0.010(3) C(11) 0.035(3) 0.055(4) 0.050(3) 0.003(2) -0.009(2) -0.001(3) C(12) 0.024(2) 0.068(4) 0.032(2) -0.006(2) -0.004(2) -0.004(2) C(13) 0.041(3) 0.054(4) 0.062(4) -0.006(3) -0.009(3) -0.002(3) C(14) 0.041(3) 0.058(4) 0.056(4) -0.002(3) -0.010(3) 0.007(3) C(15) 0.115(9) 0.065(7) 0.16(1) 0.005(6) 0.044(9) -0.013(6) C(16) 0.19(2) 0.16(2) 0.24(2) -0.02(1) 0.01(2) -0.06(2) C(17) 0.085(7) 0.062(6) 0.20(1) -0.016(5) 0.001(7) -0.014(8) C(18) 0.41(5) 0.21(2) 0.57(6) 0.17(3) 0.13(4) 0.14(3) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.160(4) . . yes Ag(1) N(2) 2.170(4) . 4_354 yes S(1) O(1) 1.27(1) . . yes S(1) O(2) 1.343(7) . . yes S(1) O(3) 1.32(2) . . yes S(1) C(15) 1.70(1) . . yes F(1) C(15) 1.23(3) . . yes F(2) C(15) 1.19(1) . . yes F(3) C(15) 1.24(2) . . yes O(4) C(17) 1.15(1) . . yes N(1) C(1) 1.342(8) . . yes N(1) C(5) 1.344(8) . . yes N(2) C(10) 1.343(8) . . yes N(2) C(14) 1.320(8) . . yes C(1) C(2) 1.387(7) . . yes C(2) C(3) 1.378(8) . . yes C(3) C(4) 1.386(8) . . yes C(3) C(6) 1.432(6) . . yes C(4) C(5) 1.380(7) . . yes C(6) C(7) 1.192(7) . . yes C(7) C(8) 1.369(7) . . yes C(8) C(9) 1.197(7) . . yes C(9) C(12) 1.430(6) . . yes C(10) C(11) 1.370(7) . . yes C(11) C(12) 1.382(8) . . yes C(12) C(13) 1.376(8) . . yes C(13) C(14) 1.373(8) . . yes C(16) C(17) 1.33(3) . . yes C(17) C(18) 1.44(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(2) 178.9(2) . 1_555 4_354 yes O(1) S(1) O(2) 123.1(8) . 1_555 1_555 yes O(1) S(1) O(3) 107(1) . 1_555 1_555 yes O(1) S(1) C(15) 106.0(8) . 1_555 1_555 yes O(2) S(1) O(3) 108.0(9) . 1_555 1_555 yes O(2) S(1) C(15) 106.8(5) . 1_555 1_555 yes O(3) S(1) C(15) 103(1) . 1_555 1_555 yes Ag(1) N(1) C(1) 120.7(4) . 1_555 1_555 yes Ag(1) N(1) C(5) 121.8(4) . 1_555 1_555 yes C(1) N(1) C(5) 117.5(4) . 1_555 1_555 yes Ag(1) N(2) C(10) 122.2(4) . 4_656 1_555 yes Ag(1) N(2) C(14) 120.6(4) . 4_656 1_555 yes C(10) N(2) C(14) 117.2(4) . 1_555 1_555 yes N(1) C(1) C(2) 123.5(5) . 1_555 1_555 yes C(1) C(2) C(3) 118.6(5) . 1_555 1_555 yes C(2) C(3) C(4) 118.2(4) . 1_555 1_555 yes C(2) C(3) C(6) 121.1(5) . 1_555 1_555 yes C(4) C(3) C(6) 120.7(5) . 1_555 1_555 yes C(3) C(4) C(5) 120.0(5) . 1_555 1_555 yes N(1) C(5) C(4) 122.2(6) . 1_555 1_555 yes C(3) C(6) C(7) 177.2(6) . 1_555 1_555 yes C(6) C(7) C(8) 179.7(6) . 1_555 1_555 yes C(7) C(8) C(9) 178.1(7) . 1_555 1_555 yes C(8) C(9) C(12) 179.2(6) . 1_555 1_555 yes N(2) C(10) C(11) 123.0(5) . 1_555 1_555 yes C(10) C(11) C(12) 119.3(5) . 1_555 1_555 yes C(9) C(12) C(11) 121.0(5) . 1_555 1_555 yes C(9) C(12) C(13) 121.3(5) . 1_555 1_555 yes C(11) C(12) C(13) 117.6(4) . 1_555 1_555 yes C(12) C(13) C(14) 119.4(5) . 1_555 1_555 yes N(2) C(14) C(13) 123.4(6) . 1_555 1_555 yes S(1) C(15) F(1) 113(1) . 1_555 1_555 yes S(1) C(15) F(2) 124(1) . 1_555 1_555 yes S(1) C(15) F(3) 115(1) . 1_555 1_555 yes F(1) C(15) F(2) 100(1) . 1_555 1_555 yes F(1) C(15) F(3) 96(1) . 1_555 1_555 yes F(2) C(15) F(3) 101(1) . 1_555 1_555 yes O(4) C(17) C(16) 141(1) . 1_555 1_555 yes O(4) C(17) C(18) 121(1) . 1_555 1_555 yes C(16) C(17) C(18) 96(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(4) 2.869(8) . 4_455 ? Ag(1) C(4) 3.226(6) . 4_455 ? Ag(1) C(5) 3.339(7) . 4_455 ? Ag(1) C(13) 3.475(7) . 1_454 ? Ag(1) C(14) 3.563(7) . 1_454 ? Ag(1) C(3) 3.566(5) . 4_455 ? Ag(1) C(12) 3.568(5) . 1_454 ? F(1) C(13) 3.57(2) . 3_756 ? F(2) C(7) 3.131(10) . 2_646 ? F(2) C(8) 3.20(1) . 2_646 ? F(2) C(6) 3.52(1) . 2_646 ? O(1) C(16) 3.35(2) . 1_455 ? O(3) C(2) 3.45(2) . 3_656 ? O(4) C(5) 3.285(9) . 4_555 ? O(4) C(14) 3.371(9) . 1_454 ? O(4) N(1) 3.532(9) . 4_555 ? N(1) N(2) 3.392(7) . 1_454 ? N(1) C(6) 3.443(8) . 4_455 ? N(1) C(3) 3.549(7) . 4_455 ? N(1) C(14) 3.570(8) . 1_454 ? N(2) C(9) 3.452(8) . 4_555 ? N(2) C(5) 3.471(8) . 1_656 ? N(2) C(12) 3.544(7) . 4_555 ? C(1) C(6) 3.592(9) . 4_455 ? C(3) C(8) 3.467(8) . 4_455 ? C(6) C(9) 3.478(9) . 4_455 ? C(7) C(12) 3.484(8) . 4_455 ? C(7) C(11) 3.544(9) . 4_455 ? C(8) C(11) 3.481(9) . 4_455 ? C(8) C(10) 3.572(9) . 4_455 ? C(9) C(10) 3.482(9) . 4_455 ? C(18) C(18) 3.43(8) . 3_756 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_5 #{[Cu(2-bpbd)2]BF4}n 3b #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H16 B Cu F4 N4 ' _chemical_formula_moiety 'C28 H16 B Cu F4 N4 ' _chemical_formula_weight 558.81 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a (origin at -1)' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2-y,z 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z -x,-y,-z x,1/2+y,-z 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z 1/2-x,-y,1/2+z 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z 1/2+x,y,1/2-z 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z _cell_length_a 10.626(3) _cell_length_b 10.626(3) _cell_length_c 25.718(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2903.8(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 7.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.923 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method w-2q _diffrn_reflns_number 1853 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.52 _diffrn_reflns_limit_h_min 0 _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 33 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.96 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1677 _reflns_number_gt 701 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0930 _refine_ls_wR_factor_ref 0.2968 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 701 _refine_ls_number_parameters 86 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[s^2^(Fo^2^) + (0.1488P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_diff_density_max 0.70 _refine_diff_density_min -0.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cu(1) Cu 1.0000 0.2500 0.1250 0.0530(7) Uani 1.00 d S . . F(1) F 1.041(1) 0.156(1) 0.6006(5) 0.278(8) Uani 1.00 d . . . N(1) N 1.0395(6) 0.0883(6) 0.1668(2) 0.059(2) Uani 1.00 d . . . C(1) C 1.1330(8) 0.0113(8) 0.1541(3) 0.074(2) Uani 1.00 d . . . C(2) C 1.1737(9) -0.0883(9) 0.1811(4) 0.088(3) Uani 1.00 d . . . C(3) C 1.118(1) -0.1129(10) 0.2280(5) 0.108(4) Uani 1.00 d . . . C(4) C 1.0220(10) -0.0338(9) 0.2454(4) 0.091(3) Uani 1.00 d . . . C(5) C 0.9828(7) 0.0618(7) 0.2135(3) 0.066(2) Uani 1.00 d . . . C(6) C 0.8822(8) 0.1437(8) 0.2290(3) 0.068(2) Uani 1.00 d . . . C(7) C 0.7976(8) 0.2104(8) 0.2424(3) 0.068(2) Uani 1.00 d . . . B(1) B 1.0000 0.2500 0.6250 0.075(6) Uani 1.00 d S . . H(1) H 1.1755 0.0287 0.1225 0.0887 Uiso 1.00 calc . . . H(2) H 1.2392 -0.1404 0.1681 0.1059 Uiso 1.00 calc . . . H(3) H 1.1446 -0.1825 0.2484 0.1299 Uiso 1.00 calc . . . H(4) H 0.9846 -0.0459 0.2786 0.1094 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.053(2) 0.0522 0.053(1) 0.0000 0.0000 0.0000 F(1) 0.22(1) 0.32(1) 0.29(1) -0.15(1) 0.143(10) -0.24(1) N(1) 0.055(4) 0.063(4) 0.058(4) 0.017(3) 0.009(3) 0.013(3) C(1) 0.068(5) 0.076(6) 0.077(6) 0.021(5) 0.023(4) 0.007(5) C(2) 0.075(6) 0.074(6) 0.115(8) 0.029(5) 0.031(6) 0.014(6) C(3) 0.101(8) 0.087(7) 0.137(10) 0.049(6) 0.009(7) 0.041(7) C(4) 0.098(7) 0.082(6) 0.094(6) 0.028(6) 0.032(6) 0.034(5) C(5) 0.056(5) 0.062(5) 0.078(5) 0.019(4) 0.011(4) 0.015(4) C(6) 0.063(5) 0.079(6) 0.063(5) 0.018(4) 0.021(4) 0.016(4) C(7) 0.065(5) 0.083(6) 0.055(4) 0.012(4) 0.015(4) 0.022(4) B(1) 0.11(2) 0.0800 0.031(8) 0.0000 0.0000 0.0000 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.070(6) . . yes Cu(1) N(1) 2.070(6) . 7_565 yes Cu(1) N(1) 2.070(6) . 8_645 yes Cu(1) N(1) 2.070(6) . 2_755 yes F(1) B(1) 1.25(1) . . yes N(1) C(1) 1.33(1) . . yes N(1) C(5) 1.373(10) . . yes C(1) C(2) 1.34(1) . . yes C(2) C(3) 1.37(2) . . yes C(3) C(4) 1.40(2) . . yes C(4) C(5) 1.37(1) . . yes C(5) C(6) 1.43(1) . . yes C(6) C(7) 1.20(1) . . yes C(7) C(7) 1.37(2) . 13_655 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(1) 105.7(1) . 1_555 7_565 yes N(1) Cu(1) N(1) 105.7(1) . 1_555 8_645 yes N(1) Cu(1) N(1) 117.4(3) . 1_555 2_755 yes N(1) Cu(1) N(1) 117.4(3) . 7_565 8_645 yes N(1) Cu(1) N(1) 105.7(1) . 7_565 2_755 yes N(1) Cu(1) N(1) 105.7(1) . 8_645 2_755 yes Cu(1) N(1) C(1) 122.4(5) . 1_555 1_555 yes Cu(1) N(1) C(5) 122.4(5) . 1_555 1_555 yes C(1) N(1) C(5) 114.6(6) . 1_555 1_555 yes N(1) C(1) C(2) 127.0(8) . 1_555 1_555 yes C(1) C(2) C(3) 118.0(9) . 1_555 1_555 yes C(2) C(3) C(4) 118.9(10) . 1_555 1_555 yes C(3) C(4) C(5) 118.4(10) . 1_555 1_555 yes N(1) C(5) C(4) 122.9(8) . 1_555 1_555 yes N(1) C(5) C(6) 116.5(7) . 1_555 1_555 yes C(4) C(5) C(6) 120.6(8) . 1_555 1_555 yes C(5) C(6) C(7) 178.9(9) . 1_555 1_555 yes C(6) C(7) C(7) 178(1) . 1_555 13_655 yes F(1) B(1) F(1) 104.5(5) . 1_555 7_566 yes F(1) B(1) F(1) 104.5(5) . 1_555 8_646 yes F(1) B(1) F(1) 119(1) . 1_555 2_755 yes F(1) B(1) F(1) 119(1) . 7_566 8_646 yes F(1) B(1) F(1) 104.5(5) . 7_566 2_755 yes F(1) B(1) F(1) 104.5(5) . 8_646 2_755 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(3) 3.32(2) . 4_665 ? F(1) C(4) 3.37(2) . 4_665 ? F(1) C(2) 3.38(1) . 16_535 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_6 #{[Ag(2-bpbd)(NO3)]}n 4a #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C14 H8 Ag N3 O3 ' _chemical_formula_moiety 'C14 H8 Ag N3 O3 ' _chemical_formula_weight 374.10 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.918(3) _cell_length_b 10.625(2) _cell_length_c 7.398(3) _cell_angle_alpha 95.33(2) _cell_angle_beta 102.96(3) _cell_angle_gamma 113.84(2) _cell_volume 680.0(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.2 _cell_measurement_theta_max 20.8 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.742 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method w-2q _diffrn_reflns_number 3308 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.60 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3126 _reflns_number_gt 2529 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0734 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2529 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[¥s^2^(Fo^2^) + (0.0282P)^2^+0.5390P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^¥l^3^/sin(2¥q)]^-1/4^' _refine_diff_density_max 0.60 _refine_diff_density_min -0.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag(1) Ag 0.42306(2) 0.31864(2) 0.81676(3) 0.05548(5) Uani 1.00 d . . . O(1) O 0.6580(2) 0.5543(2) 0.9258(3) 0.0680(5) Uani 1.00 d . . . O(2) O 0.7253(3) 0.4001(2) 1.0074(4) 0.1180(7) Uani 1.00 d . . . O(3) O 0.8872(2) 0.6186(3) 1.0895(3) 0.1044(9) Uani 1.00 d . . . N(1) N 0.3216(2) 0.1149(2) 0.9110(2) 0.0438(4) Uani 1.00 d . . . N(2) N 0.3144(2) 0.4124(2) 0.5974(2) 0.0449(4) Uani 1.00 d . . . N(3) N 0.7605(2) 0.5242(2) 1.0103(3) 0.0501(4) Uani 1.00 d . . . C(1) C 0.2458(3) 0.1034(2) 1.0412(3) 0.0565(6) Uani 1.00 d . . . C(2) C 0.1828(3) -0.0178(3) 1.1062(3) 0.0615(6) Uani 1.00 d . . . C(3) C 0.1994(3) -0.1333(2) 1.0391(3) 0.0558(6) Uani 1.00 d . . . C(4) C 0.2778(2) -0.1244(2) 0.9064(3) 0.0458(5) Uani 1.00 d . . . C(5) C 0.3344(2) 0.0000(2) 0.8414(3) 0.0378(4) Uani 1.00 d . . . C(6) C 0.4087(2) 0.0080(2) 0.6952(3) 0.0439(5) Uani 1.00 d . . . C(7) C 0.4659(2) 0.0029(2) 0.5704(3) 0.0462(5) Uani 1.00 d . . . C(8) C 0.0335(2) 0.0701(2) 0.4971(3) 0.0505(6) Uani 1.00 d . . . C(9) C 0.0943(2) 0.1925(2) 0.4944(3) 0.0520(6) Uani 1.00 d . . . C(10) C 0.1672(2) 0.3396(2) 0.4889(3) 0.0460(5) Uani 1.00 d . . . C(11) C 0.0894(3) 0.4015(3) 0.3796(3) 0.0591(7) Uani 1.00 d . . . C(12) C 0.1637(3) 0.5426(3) 0.3795(4) 0.0639(6) Uani 1.00 d . . . C(13) C 0.3130(3) 0.6165(2) 0.4879(4) 0.0601(6) Uani 1.00 d . . . C(14) C 0.3834(3) 0.5487(2) 0.5948(3) 0.0525(6) Uani 1.00 d . . . H(1) H 0.236(3) 0.180(3) 1.082(4) 0.06853(10) Uiso 1.00 calc . . . H(2) H 0.130(3) -0.024(3) 1.186(4) 0.06764(10) Uiso 1.00 calc . . . H(3) H 0.162(3) -0.216(3) 1.084(4) 0.07063(10) Uiso 1.00 calc . . . H(4) H 0.293(2) -0.197(2) 0.855(3) 0.04947(8) Uiso 1.00 calc . . . H(5) H -0.018(3) 0.349(3) 0.298(4) 0.0839(1) Uiso 1.00 calc . . . H(6) H 0.113(3) 0.584(3) 0.300(4) 0.0757(1) Uiso 1.00 calc . . . H(7) H 0.364(3) 0.706(3) 0.494(4) 0.0871(1) Uiso 1.00 calc . . . H(8) H 0.481(2) 0.594(2) 0.664(3) 0.04674(8) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.06588(8) 0.03619(6) 0.0718(1) 0.02468(6) 0.02682(7) 0.01693(6) O(1) 0.0742(8) 0.0713(8) 0.070(1) 0.0479(7) 0.0138(8) 0.0093(8) O(2) 0.207(2) 0.0768(8) 0.150(2) 0.0980(9) 0.112(1) 0.0690(9) O(3) 0.0482(9) 0.149(2) 0.082(1) 0.017(1) 0.0116(9) 0.010(1) N(1) 0.0481(7) 0.0339(7) 0.0544(9) 0.0194(6) 0.0200(7) 0.0117(6) N(2) 0.0448(7) 0.0341(7) 0.0519(9) 0.0128(6) 0.0151(7) 0.0097(6) N(3) 0.0554(7) 0.0539(8) 0.0583(9) 0.0319(6) 0.0299(7) 0.0208(7) C(1) 0.065(1) 0.0498(10) 0.068(1) 0.0310(8) 0.0330(10) 0.0131(9) C(2) 0.067(1) 0.067(1) 0.064(1) 0.0294(10) 0.0393(9) 0.0241(10) C(3) 0.063(1) 0.0478(10) 0.062(1) 0.0210(9) 0.0271(9) 0.0252(9) C(4) 0.0500(9) 0.0349(8) 0.056(1) 0.0193(7) 0.0180(8) 0.0133(8) C(5) 0.0376(8) 0.0326(7) 0.0414(9) 0.0139(6) 0.0100(7) 0.0087(7) C(6) 0.0488(9) 0.0340(8) 0.050(1) 0.0172(7) 0.0172(8) 0.0098(7) C(7) 0.0531(9) 0.0338(8) 0.053(1) 0.0166(7) 0.0223(8) 0.0103(7) C(8) 0.0463(10) 0.0409(10) 0.050(1) 0.0071(8) 0.0149(9) 0.0003(9) C(9) 0.0460(10) 0.046(1) 0.051(1) 0.0086(8) 0.0149(9) -0.0003(9) C(10) 0.0474(9) 0.0408(9) 0.046(1) 0.0141(7) 0.0191(8) 0.0035(8) C(11) 0.053(1) 0.067(1) 0.054(1) 0.0260(10) 0.0108(10) 0.012(1) C(12) 0.081(1) 0.073(1) 0.059(1) 0.0487(10) 0.026(1) 0.0260(10) C(13) 0.084(1) 0.0413(9) 0.066(1) 0.0302(9) 0.032(1) 0.0211(9) C(14) 0.055(1) 0.0365(9) 0.060(1) 0.0136(8) 0.0172(9) 0.0110(8) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) O(1) 2.532(1) . . yes Ag(1) N(1) 2.240(2) . . yes Ag(1) N(2) 2.274(2) . . yes O(1) N(3) 1.241(3) . . yes O(2) N(3) 1.217(3) . . yes O(3) N(3) 1.212(2) . . yes N(1) C(1) 1.335(3) . . yes N(1) C(5) 1.345(3) . . yes N(2) C(10) 1.349(2) . . yes N(2) C(14) 1.333(3) . . yes C(1) C(2) 1.371(4) . . yes C(2) C(3) 1.366(4) . . yes C(3) C(4) 1.370(4) . . yes C(4) C(5) 1.390(3) . . yes C(5) C(6) 1.430(3) . . yes C(6) C(7) 1.196(3) . . yes C(7) C(7) 1.372(5) . 2_656 yes C(8) C(8) 1.373(4) . 2_556 yes C(8) C(9) 1.197(3) . . yes C(9) C(10) 1.442(3) . . yes C(10) C(11) 1.382(4) . . yes C(11) C(12) 1.378(4) . . yes C(12) C(13) 1.365(3) . . yes C(13) C(14) 1.377(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ag(1) N(1) 139.69(6) . 1_555 1_555 yes O(1) Ag(1) N(2) 88.30(6) . 1_555 1_555 yes N(1) Ag(1) N(2) 130.81(5) . 1_555 1_555 yes Ag(1) O(1) N(3) 103.1(1) . 1_555 1_555 yes Ag(1) N(1) C(1) 120.6(2) . 1_555 1_555 yes Ag(1) N(1) C(5) 122.3(1) . 1_555 1_555 yes C(1) N(1) C(5) 117.1(2) . 1_555 1_555 yes Ag(1) N(2) C(10) 121.2(1) . 1_555 1_555 yes Ag(1) N(2) C(14) 120.9(1) . 1_555 1_555 yes C(10) N(2) C(14) 116.8(2) . 1_555 1_555 yes O(1) N(3) O(2) 116.7(2) . 1_555 1_555 yes O(1) N(3) O(3) 118.7(2) . 1_555 1_555 yes O(2) N(3) O(3) 124.6(3) . 1_555 1_555 yes N(1) C(1) C(2) 123.3(3) . 1_555 1_555 yes C(1) C(2) C(3) 119.5(3) . 1_555 1_555 yes C(2) C(3) C(4) 118.6(2) . 1_555 1_555 yes C(3) C(4) C(5) 119.2(2) . 1_555 1_555 yes N(1) C(5) C(4) 122.3(2) . 1_555 1_555 yes N(1) C(5) C(6) 118.0(2) . 1_555 1_555 yes C(4) C(5) C(6) 119.7(2) . 1_555 1_555 yes C(5) C(6) C(7) 174.6(2) . 1_555 1_555 yes C(6) C(7) C(7) 178.9(3) . 1_555 2_656 yes C(8) C(8) C(9) 178.8(3) . 2_556 1_555 yes C(8) C(9) C(10) 179.3(2) . 1_555 1_555 yes N(2) C(10) C(9) 116.0(2) . 1_555 1_555 yes N(2) C(10) C(11) 122.5(2) . 1_555 1_555 yes C(9) C(10) C(11) 121.5(2) . 1_555 1_555 yes C(10) C(11) C(12) 119.4(2) . 1_555 1_555 yes C(11) C(12) C(13) 118.3(3) . 1_555 1_555 yes C(12) C(13) C(14) 119.3(2) . 1_555 1_555 yes N(2) C(14) C(13) 123.6(2) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(1) 2.532(1) . . ? Ag(1) O(1) 2.680(2) . 2_667 ? Ag(1) N(3) 3.293(2) . 2_667 ? Ag(1) O(3) 3.595(3) . 2_667 ? O(1) C(1) 3.335(3) . 2_667 ? O(1) O(1) 3.348(4) . 2_667 ? O(1) N(2) 3.449(3) . 2_667 ? O(1) C(12) 3.482(4) . 2_666 ? O(1) N(1) 3.519(3) . 2_667 ? O(1) C(13) 3.540(3) . 2_666 ? O(2) C(4) 3.045(3) . 2_657 ? O(2) C(3) 3.218(4) . 2_657 ? O(2) C(12) 3.312(4) . 2_666 ? O(2) C(14) 3.424(4) . 2_667 ? O(2) N(2) 3.570(3) . 2_667 ? O(2) C(13) 3.578(4) . 2_666 ? O(3) C(3) 3.283(3) . 1_665 ? O(3) C(10) 3.303(3) . 2_667 ? O(3) N(2) 3.340(3) . 2_667 ? O(3) C(9) 3.441(4) . 2_667 ? O(3) C(12) 3.500(4) . 1_656 ? O(3) C(11) 3.523(4) . 2_666 ? O(3) C(12) 3.555(4) . 2_666 ? N(2) N(3) 3.231(3) . 2_667 ? N(2) C(14) 3.492(3) . 2_666 ? N(3) C(12) 3.226(4) . 2_666 ? N(3) C(11) 3.543(3) . 2_666 ? N(3) C(14) 3.546(3) . 2_667 ? C(3) C(7) 3.538(3) . 2_657 ? C(3) C(6) 3.556(3) . 2_657 ? C(4) C(6) 3.463(3) . 2_657 ? C(4) C(5) 3.498(3) . 2_657 ? C(5) C(5) 3.583(4) . 2_657 ? C(11) C(12) 3.584(4) . 2_566 ? C(14) C(14) 3.392(6) . 2_666 ? #------------------------------------------------------------------------------ ###END #------------------------------------------------------------------------------ data_7 #{[Ag(2-bpbd)(CF3SO3)]}n 4c #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C15 H8 Ag F3 N2 O3 S ' _chemical_formula_moiety 'C15 H8 Ag F3 N2 O3 S ' _chemical_formula_weight 461.16 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 9.457(5) _cell_length_b 10.912(4) _cell_length_c 15.870(4) _cell_angle_alpha 90 _cell_angle_beta 99.32(3) _cell_angle_gamma 90 _cell_volume 1616(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 14.2 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K¥a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method ¥w-2¥q _diffrn_reflns_number 3943 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.63 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3714 _reflns_number_gt 2578 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1028 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2578 _refine_ls_number_parameters 227 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[¥s^2^(Fo^2^) + (0.0365P)^2^+1.3110P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^¥l^3^/sin(2¥q)]^-1/4^' _refine_diff_density_max 0.57 _refine_diff_density_min -0.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag(1) Ag 0.44172(4) 0.03818(3) 0.74995(2) 0.0480(1) Uani 1.00 d . . . S(1) S 0.0726(1) 0.1757(1) 0.75644(7) 0.0413(2) Uani 1.00 d . . . F(1) F -0.0325(5) -0.0398(3) 0.7211(3) 0.109(1) Uani 1.00 d . . . F(2) F -0.0078(5) 0.0066(4) 0.8524(3) 0.132(2) Uani 1.00 d . . . F(3) F -0.1773(4) 0.0791(4) 0.7656(3) 0.096(1) Uani 1.00 d . . . O(1) O 0.0527(5) 0.2634(4) 0.8188(3) 0.078(1) Uani 1.00 d . . . O(2) O 0.2099(4) 0.1229(4) 0.7696(4) 0.105(2) Uani 1.00 d . . . O(3) O 0.0178(6) 0.2102(5) 0.6724(3) 0.114(2) Uani 1.00 d . . . N(1) N 0.5300(4) -0.0601(3) 0.8724(2) 0.0395(8) Uani 1.00 d . . . N(2) N 0.3792(4) -0.0334(3) 0.6169(2) 0.0427(8) Uani 1.00 d . . . C(1) C 0.6372(5) -0.0167(4) 0.9305(3) 0.047(1) Uani 1.00 d . . . C(2) C 0.6888(5) -0.0777(5) 1.0043(3) 0.052(1) Uani 1.00 d . . . C(3) C 0.6287(6) -0.1887(5) 1.0207(3) 0.057(1) Uani 1.00 d . . . C(4) C 0.5193(5) -0.2351(4) 0.9620(3) 0.050(1) Uani 1.00 d . . . C(5) C 0.4732(4) -0.1687(4) 0.8883(3) 0.0397(9) Uani 1.00 d . . . C(6) C 0.3585(5) -0.2122(4) 0.8241(3) 0.044(1) Uani 1.00 d . . . C(7) C 0.2661(5) -0.2468(4) 0.7686(3) 0.0441(10) Uani 1.00 d . . . C(8) C 0.1627(5) -0.2893(4) 0.7046(3) 0.044(1) Uani 1.00 d . . . C(9) C 0.0703(5) -0.3283(4) 0.6503(3) 0.045(1) Uani 1.00 d . . . C(10) C 0.4541(5) -0.1258(4) 0.5897(3) 0.0417(10) Uani 1.00 d . . . C(11) C 0.4205(5) -0.1748(5) 0.5085(3) 0.056(1) Uani 1.00 d . . . C(12) C 0.3044(6) -0.1288(6) 0.4547(3) 0.067(2) Uani 1.00 d . . . C(13) C 0.2259(6) -0.0364(6) 0.4822(3) 0.070(2) Uani 1.00 d . . . C(14) C 0.2673(6) 0.0103(5) 0.5636(3) 0.059(1) Uani 1.00 d . . . C(15) C -0.0422(5) 0.0490(5) 0.7758(3) 0.053(1) Uani 1.00 d . . . H(1) H 0.6790 0.0597 0.9199 0.0565 Uiso 1.00 calc . . . H(2) H 0.7651 -0.0441 1.0439 0.0622 Uiso 1.00 calc . . . H(3) H 0.6626 -0.2322 1.0719 0.0684 Uiso 1.00 calc . . . H(4) H 0.4761 -0.3113 0.9718 0.0603 Uiso 1.00 calc . . . H(5) H 0.4765 -0.2389 0.4904 0.0674 Uiso 1.00 calc . . . H(6) H 0.2789 -0.1610 0.3987 0.0808 Uiso 1.00 calc . . . H(7) H 0.1442 -0.0046 0.4461 0.0839 Uiso 1.00 calc . . . H(8) H 0.2138 0.0759 0.5821 0.0703 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0554(2) 0.0459(2) 0.0397(2) 0.0038(2) -0.0012(1) -0.0037(2) S(1) 0.0395(6) 0.0421(6) 0.0423(5) -0.0002(5) 0.0064(4) 0.0014(5) F(1) 0.125(3) 0.058(2) 0.145(4) -0.024(2) 0.024(3) -0.037(2) F(2) 0.153(4) 0.132(3) 0.092(3) -0.065(3) -0.037(3) 0.074(3) F(3) 0.052(2) 0.105(3) 0.131(3) -0.021(2) 0.021(2) 0.009(3) O(1) 0.097(3) 0.058(2) 0.085(3) -0.012(2) 0.033(2) -0.031(2) O(2) 0.040(2) 0.087(3) 0.193(5) 0.005(2) 0.029(3) -0.031(3) O(3) 0.126(4) 0.140(4) 0.062(2) -0.062(3) -0.021(3) 0.053(3) N(1) 0.041(2) 0.039(2) 0.036(2) -0.001(2) 0.002(1) -0.003(1) N(2) 0.045(2) 0.045(2) 0.036(2) 0.009(2) 0.001(1) 0.002(2) C(1) 0.044(2) 0.052(3) 0.043(2) -0.008(2) 0.001(2) -0.007(2) C(2) 0.044(2) 0.068(3) 0.040(2) 0.000(2) -0.004(2) -0.008(2) C(3) 0.061(3) 0.069(3) 0.038(2) 0.012(3) 0.000(2) 0.009(2) C(4) 0.063(3) 0.045(3) 0.041(2) 0.000(2) 0.006(2) 0.005(2) C(5) 0.039(2) 0.040(2) 0.039(2) 0.001(2) 0.006(2) -0.008(2) C(6) 0.046(2) 0.040(2) 0.045(2) -0.003(2) 0.004(2) -0.004(2) C(7) 0.041(2) 0.040(2) 0.050(2) -0.002(2) 0.003(2) 0.001(2) C(8) 0.043(2) 0.042(2) 0.049(2) -0.002(2) 0.006(2) 0.001(2) C(9) 0.047(3) 0.041(2) 0.044(2) -0.006(2) 0.002(2) 0.002(2) C(10) 0.043(2) 0.041(2) 0.040(2) 0.000(2) 0.002(2) -0.001(2) C(11) 0.060(3) 0.059(3) 0.046(3) 0.011(3) 0.001(2) -0.012(2) C(12) 0.073(4) 0.087(4) 0.036(2) 0.006(3) -0.008(2) -0.012(3) C(13) 0.061(3) 0.098(5) 0.044(3) 0.026(3) -0.011(2) -0.001(3) C(14) 0.056(3) 0.070(3) 0.047(3) 0.024(3) 0.000(2) 0.003(2) C(15) 0.057(3) 0.044(3) 0.055(3) -0.007(2) -0.004(2) 0.008(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) O(1) 2.572(4) . 4_555 yes Ag(1) O(2) 2.445(4) . . yes Ag(1) N(1) 2.258(3) . . yes Ag(1) N(2) 2.239(3) . . yes S(1) O(1) 1.410(4) . . yes S(1) O(2) 1.405(4) . . yes S(1) O(3) 1.402(4) . . yes S(1) C(15) 1.814(5) . . yes F(1) C(15) 1.314(7) . . yes F(2) C(15) 1.293(6) . . yes F(3) C(15) 1.304(6) . . yes N(1) C(1) 1.342(5) . . yes N(1) C(5) 1.341(6) . . yes N(2) C(10) 1.344(6) . . yes N(2) C(14) 1.332(6) . . yes C(1) C(2) 1.367(6) . . yes C(2) C(3) 1.381(8) . . yes C(3) C(4) 1.372(7) . . yes C(4) C(5) 1.385(6) . . yes C(5) C(6) 1.444(6) . . yes C(6) C(7) 1.197(6) . . yes C(7) C(8) 1.372(6) . . yes C(8) C(9) 1.201(6) . . yes C(9) C(10) 1.429(6) . 4_445 yes C(10) C(11) 1.383(6) . . yes C(11) C(12) 1.372(7) . . yes C(12) C(13) 1.365(9) . . yes C(13) C(14) 1.384(7) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ag(1) O(2) 86.6(1) . 4_555 1_555 yes O(1) Ag(1) N(1) 88.1(1) . 4_555 1_555 yes O(1) Ag(1) N(2) 136.2(1) . 4_555 1_555 yes O(2) Ag(1) N(1) 106.5(2) . 1_555 1_555 yes O(2) Ag(1) N(2) 98.4(2) . 1_555 1_555 yes N(1) Ag(1) N(2) 130.6(1) . 1_555 1_555 yes O(1) S(1) O(2) 113.5(3) . 1_555 1_555 yes O(1) S(1) O(3) 114.5(3) . 1_555 1_555 yes O(1) S(1) C(15) 104.3(3) . 1_555 1_555 yes O(2) S(1) O(3) 116.2(3) . 1_555 1_555 yes O(2) S(1) C(15) 103.1(3) . 1_555 1_555 yes O(3) S(1) C(15) 103.1(3) . 1_555 1_555 yes Ag(1) O(1) S(1) 111.4(2) . 4_455 1_555 yes Ag(1) O(2) S(1) 164.2(4) . 1_555 1_555 yes Ag(1) N(1) C(1) 123.8(3) . 1_555 1_555 yes Ag(1) N(1) C(5) 118.6(2) . 1_555 1_555 yes C(1) N(1) C(5) 117.6(4) . 1_555 1_555 yes Ag(1) N(2) C(10) 119.5(3) . 1_555 1_555 yes Ag(1) N(2) C(14) 122.4(3) . 1_555 1_555 yes C(10) N(2) C(14) 118.0(4) . 1_555 1_555 yes N(1) C(1) C(2) 122.9(4) . 1_555 1_555 yes C(1) C(2) C(3) 119.2(4) . 1_555 1_555 yes C(2) C(3) C(4) 119.0(4) . 1_555 1_555 yes C(3) C(4) C(5) 118.7(4) . 1_555 1_555 yes N(1) C(5) C(4) 122.7(4) . 1_555 1_555 yes N(1) C(5) C(6) 115.8(4) . 1_555 1_555 yes C(4) C(5) C(6) 121.4(4) . 1_555 1_555 yes C(5) C(6) C(7) 177.6(5) . 1_555 1_555 yes C(6) C(7) C(8) 178.3(5) . 1_555 1_555 yes C(7) C(8) C(9) 178.1(5) . 1_555 1_555 yes C(8) C(9) C(10) 176.3(5) . 1_555 4_445 yes N(2) C(10) C(9) 115.7(4) . 1_555 4_545 yes N(2) C(10) C(11) 122.4(4) . 1_555 1_555 yes C(9) C(10) C(11) 121.9(4) . 4_545 1_555 yes C(10) C(11) C(12) 118.6(5) . 1_555 1_555 yes C(11) C(12) C(13) 119.5(5) . 1_555 1_555 yes C(12) C(13) C(14) 119.0(5) . 1_555 1_555 yes N(2) C(14) C(13) 122.5(5) . 1_555 1_555 yes S(1) C(15) F(1) 110.1(4) . 1_555 1_555 yes S(1) C(15) F(2) 111.5(4) . 1_555 1_555 yes S(1) C(15) F(3) 112.9(4) . 1_555 1_555 yes F(1) C(15) F(2) 108.8(4) . 1_555 1_555 yes F(1) C(15) F(3) 106.0(4) . 1_555 1_555 yes F(2) C(15) F(3) 107.4(5) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(1) 2.572(4) . 4_555 ? Ag(1) C(9) 3.138(5) . 4_545 ? Ag(1) C(8) 3.570(5) . 4_545 ? Ag(1) F(3) 3.599(4) . 1_655 ? F(1) C(13) 3.541(7) . 3_556 ? F(2) C(2) 3.556(6) . 3_657 ? F(3) O(1) 3.299(6) . 4_455 ? F(3) O(2) 3.426(6) . 4_455 ? F(3) C(1) 3.537(7) . 1_455 ? F(3) C(12) 3.550(6) . 3_556 ? O(1) C(1) 3.312(6) . 4_455 ? O(1) C(3) 3.335(7) . 2_557 ? O(1) N(1) 3.364(5) . 4_455 ? O(1) O(2) 3.441(6) . 4_455 ? O(2) C(3) 3.504(7) . 3_657 ? O(2) C(2) 3.595(7) . 3_657 ? O(3) C(11) 3.271(7) . 2_556 ? O(3) C(12) 3.329(8) . 2_556 ? O(3) C(12) 3.486(7) . 3_556 ? N(1) C(2) 3.417(6) . 3_657 ? N(1) C(8) 3.529(6) . 4_545 ? N(2) C(8) 3.414(6) . 4_545 ? C(1) C(3) 3.546(7) . 3_657 ? C(1) C(2) 3.559(7) . 3_657 ? #------------------------------------------------------------------------------ ###END