data_[Cu(CM-TTF)](ClO4) #------------------------------------------------------------------------------ _audit_creation_date 'Sat Jul 12 19:38:40 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution MULTAN88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 701.86 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H22 Cl Cu N2 O5 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.979(3) _cell_length_b 25.785(4) _cell_length_c 11.086(4) _cell_angle_alpha 90 _cell_angle_beta 92.51(3) _cell_angle_gamma 90 _cell_volume 2849(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 6.4 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1432.00 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_correction_T_min 0.803 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.61 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 2 1 -5 2 0 0 2 _diffrn_reflns_number 7070 _reflns_number_total 6700 _reflns_number_observed 2963 _reflns_observed_criterion >2.5sigma(I) _diffrn_reflns_av_R_equivalents 4.44 _diffrn_reflns_av_sigmaI/netI 0.159 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.09436 _diffrn_orient_matrix_UB_12 0.00633 _diffrn_orient_matrix_UB_13 0.03055 _diffrn_orient_matrix_UB_21 -0.03078 _diffrn_orient_matrix_UB_22 0.03038 _diffrn_orient_matrix_UB_23 0.04755 _diffrn_orient_matrix_UB_31 -0.01452 _diffrn_orient_matrix_UB_32 -0.02326 _diffrn_orient_matrix_UB_33 0.07042 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 4 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 20 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 72 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 88 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Cu1 1.0032(2) 0.32245(6) 0.5811(1) 0.0625(5) Uani d . 1.00 . Cl1 0.5288(5) 0.2380(2) 0.1735(4) 0.086(2) Uani d . 1.00 . S1 1.0973(4) 0.6170(1) -0.1112(3) 0.061(1) Uani d . 1.00 . S2 1.1387(3) 0.4624(1) 0.3204(3) 0.058(1) Uani d . 1.00 . S3 0.8458(3) 0.3876(1) 0.5411(3) 0.059(1) Uani d . 1.00 . S4 1.1090(3) 0.5451(1) 0.1014(3) 0.059(1) Uani d . 1.00 . S5 0.8555(3) 0.4784(1) 0.3739(3) 0.0533(10) Uani d . 1.00 . S6 0.7711(4) 0.6260(1) -0.0697(3) 0.072(1) Uani d . 1.00 . S7 0.8227(3) 0.5567(1) 0.1467(3) 0.066(1) Uani d . 1.00 . S8 1.1653(5) 0.3694(2) 0.4811(7) 0.175(3) Uani d . 1.00 . O1 0.523(2) 0.1922(5) 0.223(1) 0.183(8) Uani d . 1.00 . O2 0.541(1) 0.2429(5) 0.0488(10) 0.121(5) Uani d . 1.00 . O3 0.432(3) 0.267(1) 0.200(2) 0.37(2) Uani d . 1.00 . O4 0.631(3) 0.2593(9) 0.225(2) 0.33(2) Uani d . 1.00 . O5 0.498(3) 0.022(1) 0.697(3) 0.34(1) Uiso d . 1.00 . N1* 1.075(1) 0.7591(4) -0.010(1) 0.068(4) Uani d . 1.00 . N2* 0.913(1) 0.6910(4) 0.259(1) 0.066(4) Uani d . 1.00 . C1 0.937(1) 0.4247(4) 0.440(1) 0.046(4) Uani d . 1.00 . C2 1.064(1) 0.4175(4) 0.417(1) 0.048(4) Uani d . 1.00 . C3 0.990(1) 0.4945(4) 0.2826(10) 0.042(3) Uani d . 1.00 . C4 0.975(1) 0.5285(4) 0.1913(10) 0.044(3) Uani d . 1.00 . C5 0.885(1) 0.5926(4) 0.027(1) 0.051(4) Uani d . 1.00 . C6 1.016(1) 0.5877(4) 0.005(1) 0.047(4) Uani d . 1.00 . C7* 1.135(2) 0.7255(5) 0.024(1) 0.062(5) Uani d . 1.00 . C8* 0.842(2) 0.7001(5) 0.182(1) 0.068(5) Uani d . 1.00 . C10 0.676(1) 0.6630(5) 0.033(1) 0.070(5) Uani d . 1.00 . C11 1.247(1) 0.6429(5) -0.035(1) 0.064(4) Uani d . 1.00 . C12* 1.218(1) 0.6810(5) 0.065(1) 0.072(5) Uani d . 1.00 . C13* 0.743(1) 0.7113(5) 0.084(1) 0.063(4) Uani d . 1.00 . C14 0.720(1) 0.3599(6) 0.441(2) 0.090(6) Uani d . 1.00 . C15 1.282(2) 0.360(1) 0.432(5) 0.43(3) Uani d . 1.00 . C16 0.494(3) 0.031(1) 0.845(3) 0.22(1) Uiso d . 1.00 . C17 0.486(4) -0.032(2) 0.851(4) 0.26(2) Uiso d . 1.00 . C18 0.468(3) -0.059(1) 0.742(3) 0.22(1) Uiso d . 1.00 . C19 0.464(4) -0.035(2) 0.614(4) 0.33(2) Uiso d . 1.00 . H1 0.6690 0.3858 0.3974 0.1019 Uiso calc . 1.00 . H2 0.7625 0.3388 0.3779 0.1019 Uiso calc . 1.00 . H3 0.6612 0.3375 0.4800 0.1019 Uiso calc . 1.00 . H4 1.3307 0.3318 0.4674 0.4210 Uiso calc . 1.00 . H5 1.2634 0.3476 0.3441 0.4210 Uiso calc . 1.00 . H6 1.3376 0.3889 0.4239 0.4210 Uiso calc . 1.00 . H7 0.5907 0.6722 -0.0065 0.0796 Uiso calc . 1.00 . H8 0.6543 0.6408 0.1007 0.0796 Uiso calc . 1.00 . H9 1.3013 0.6144 -0.0052 0.0754 Uiso calc . 1.00 . H10 1.2990 0.6608 -0.0943 0.0754 Uiso calc . 1.00 . H11 1.3028 0.6925 0.1020 0.0860 Uiso calc . 1.00 . H12 1.1741 0.6614 0.1275 0.0860 Uiso calc . 1.00 . H13 0.6771 0.7349 0.1126 0.0765 Uiso calc . 1.00 . H14 0.7870 0.7284 0.0190 0.0765 Uiso calc . 1.00 . 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) 0.077(1) 0.0512(9) 0.059(1) -0.0021(9) 0.0000(8) 0.0166(8) Cl(1) 0.087(3) 0.099(3) 0.073(3) 0.010(3) 0.007(2) 0.025(3) S(1) 0.089(3) 0.050(2) 0.045(2) -0.016(2) 0.006(2) 0.002(2) S(2) 0.051(2) 0.053(2) 0.070(2) 0.002(2) 0.011(2) 0.025(2) S(3) 0.060(2) 0.049(2) 0.070(2) 0.001(2) 0.022(2) 0.016(2) S(4) 0.047(2) 0.055(2) 0.076(2) 0.001(2) 0.010(2) 0.022(2) S(5) 0.053(2) 0.042(2) 0.067(2) 0.006(1) 0.017(2) 0.009(2) S(6) 0.081(3) 0.075(2) 0.058(2) 0.023(2) -0.014(2) 0.005(2) S(7) 0.051(2) 0.068(2) 0.078(2) 0.007(2) 0.008(2) 0.025(2) S(8) 0.081(3) 0.168(5) 0.282(8) 0.066(3) 0.086(4) 0.180(6) O(1) 0.26(2) 0.11(1) 0.18(2) -0.03(1) -0.04(1) 0.07(1) O(2) 0.16(1) 0.133(10) 0.070(8) 0.059(9) 0.016(8) 0.007(7) O(3) 0.39(3) 0.54(4) 0.20(2) 0.34(4) 0.20(2) 0.22(2) O(4) 0.54(5) 0.25(3) 0.19(2) -0.22(3) -0.15(3) 0.11(2) N(1*) 0.092(10) 0.049(7) 0.063(8) -0.002(7) 0.003(7) 0.006(6) N(2*) 0.075(8) 0.060(7) 0.062(7) 0.000(6) -0.007(7) 0.012(6) C(1) 0.047(7) 0.040(6) 0.049(7) -0.012(6) -0.002(6) -0.001(5) C(2) 0.047(7) 0.034(6) 0.064(8) 0.008(5) 0.004(6) 0.017(6) C(3) 0.043(7) 0.033(6) 0.051(7) -0.002(5) 0.001(6) -0.006(5) C(4) 0.049(7) 0.035(6) 0.048(7) 0.002(5) 0.007(6) 0.012(5) C(5) 0.069(9) 0.034(6) 0.051(8) 0.005(6) -0.002(7) 0.003(5) C(6) 0.066(9) 0.029(6) 0.046(7) 0.002(6) 0.005(6) 0.000(5) C(7*) 0.08(1) 0.061(9) 0.046(8) -0.023(8) 0.008(7) -0.004(7) C(8*) 0.08(1) 0.057(8) 0.07(1) 0.007(8) 0.003(9) 0.016(8) C(10) 0.056(9) 0.074(10) 0.078(10) 0.021(7) -0.009(7) 0.026(8) C(11) 0.051(8) 0.044(7) 0.10(1) 0.006(6) 0.020(8) 0.020(7) C(12*) 0.066(9) 0.061(9) 0.09(1) -0.007(8) -0.010(8) 0.017(8) C(13*) 0.067(9) 0.054(8) 0.069(9) 0.009(7) 0.004(7) 0.003(7) C(14) 0.051(9) 0.08(1) 0.13(1) -0.026(8) -0.019(9) 0.04(1) C(15) 0.08(2) 0.27(3) 0.9(1) 0.09(2) 0.14(4) 0.42(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2963 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0922 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1005 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.540 _refine_ls_shift/esd_max 0.0740 _refine_ls_shift/esd_mean 0.0050 _refine_diff_density_min -1.71 _refine_diff_density_max 1.81 #------------------------------------------------------------------------------ _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) S(5) 2.338(5) 1_555 1_555 yes Cu(1) S(6) 2.328(4) 1_555 1_555 yes Cu(1) N(1) 1.96(1) 1_555 2_745 yes Cu(1) N(2) 1.96(1) 1_555 3_766 yes Cl(1) O(1) 1.27(2) 1_555 1_555 yes Cl(1) O(2) 1.31(1) 1_555 1_555 yes Cl(1) O(3) 1.27(2) 1_555 1_555 yes Cl(1) O(4) 1.40(1) 1_555 1_555 yes S(1) C(1) 1.74(1) 1_555 1_555 yes S(1) C(3) 1.76(1) 1_555 1_555 yes S(2) C(1) 1.76(1) 1_555 1_555 yes S(2) C(4) 1.75(1) 1_555 1_555 yes S(3) C(2) 1.76(1) 1_555 1_555 yes S(3) C(5) 1.76(1) 1_555 1_555 yes S(4) C(2) 1.74(1) 1_555 1_555 yes S(4) C(6) 1.75(1) 1_555 1_555 yes S(5) C(3) 1.73(1) 1_555 1_555 yes S(5) C(7) 1.33(3) 1_555 1_555 yes S(6) C(4) 1.75(1) 1_555 1_555 yes S(6) C(8) 1.79(1) 1_555 1_555 yes S(7) C(5) 1.73(1) 1_555 1_555 yes S(7) C(9) 1.81(1) 1_555 1_555 yes S(8) C(6) 1.76(1) 1_555 1_555 yes S(8) C(12) 1.79(1) 1_555 1_555 yes O(5) C(15) 1.65(4) 1_555 1_555 yes O(5) C(18) 1.75(5) 1_555 1_555 yes N(1) C(11) 1.11(2) 1_555 1_555 yes N(2) C(14) 1.11(2) 1_555 1_555 yes C(1) C(2) 1.34(1) 1_555 1_555 yes C(3) C(4) 1.33(1) 1_555 1_555 yes C(5) C(6) 1.34(2) 1_555 1_555 yes C(7) H(4) 1.031 1_555 1_555 no C(7) H(5) 0.947 1_555 1_555 no C(7) H(6) 0.944 1_555 1_555 no C(8) H(1) 0.956 1_555 1_555 no C(8) H(2) 0.942 1_555 1_555 no C(8) H(3) 0.997 1_555 1_555 no C(9) C(10) 1.52(2) 1_555 1_555 yes C(9) H(7) 0.965 1_555 1_555 no C(9) H(8) 0.971 1_555 1_555 no C(10) C(11) 1.48(2) 1_555 1_555 yes C(10) H(9) 0.981 1_555 1_555 no C(10) H(10) 0.971 1_555 1_555 no C(12) C(13) 1.51(2) 1_555 1_555 yes C(12) H(11) 0.977 1_555 1_555 no C(12) H(12) 0.966 1_555 1_555 no C(13) C(14) 1.46(2) 1_555 1_555 yes C(13) H(13) 0.962 1_555 1_555 no C(13) H(14) 0.964 1_555 1_555 no C(15) C(16) 1.63(4) 1_555 1_555 yes C(16) C(17) 1.40(4) 1_555 1_555 yes C(17) C(18) 1.53(4) 1_555 1_555 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 S(5) Cu(1) S(6) 90.7(1) 1_555 1_555 1_555 yes S(5) Cu(1) N(1) 120.7(4) 1_555 1_555 2_745 yes S(5) Cu(1) N(2) 104.2(4) 1_555 1_555 3_766 yes S(6) Cu(1) N(1) 105.9(4) 1_555 1_555 2_745 yes S(6) Cu(1) N(2) 123.9(4) 1_555 1_555 3_766 yes N(1) Cu(1) N(2) 111.1(5) 2_745 1_555 3_766 yes O(1) Cl(1) O(2) 104(1) 1_555 1_555 1_555 yes O(1) Cl(1) O(3) 103(2) 1_555 1_555 1_555 yes O(1) Cl(1) O(4) 107(1) 1_555 1_555 1_555 yes O(2) Cl(1) O(3) 113(1) 1_555 1_555 1_555 yes O(2) Cl(1) O(4) 120(1) 1_555 1_555 1_555 yes O(3) Cl(1) O(4) 106(1) 1_555 1_555 1_555 yes C(1) S(1) C(3) 94.7(5) 1_555 1_555 1_555 yes C(1) S(2) C(4) 94.5(5) 1_555 1_555 1_555 yes C(2) S(3) C(5) 95.7(5) 1_555 1_555 1_555 yes C(2) S(4) C(6) 95.8(6) 1_555 1_555 1_555 yes Cu(1) S(5) C(3) 99.4(4) 1_555 1_555 1_555 yes Cu(1) S(5) C(7) 137(1) 1_555 1_555 1_555 yes C(3) S(5) C(7) 117(1) 1_555 1_555 1_555 yes Cu(1) S(6) C(4) 98.8(4) 1_555 1_555 1_555 yes Cu(1) S(6) C(8) 106.3(5) 1_555 1_555 1_555 yes C(4) S(6) C(8) 101.0(6) 1_555 1_555 1_555 yes C(5) S(7) C(9) 102.6(6) 1_555 1_555 1_555 yes C(6) S(8) C(12) 102.8(6) 1_555 1_555 1_555 yes C(15) O(5) C(18) 128(3) 1_555 1_555 1_555 yes Cu(1) N(1) C(11) 170(1) 2_755 1_555 1_555 yes Cu(1) N(2) C(14) 164(1) 3_766 1_555 1_555 yes S(1) C(1) S(2) 114.3(6) 1_555 1_555 1_555 yes S(1) C(1) C(2) 124.1(9) 1_555 1_555 1_555 yes S(2) C(1) C(2) 121.6(9) 1_555 1_555 1_555 yes S(3) C(2) S(4) 114.5(6) 1_555 1_555 1_555 yes S(3) C(2) C(1) 121.6(9) 1_555 1_555 1_555 yes S(4) C(2) C(1) 123.8(9) 1_555 1_555 1_555 yes S(1) C(3) S(5) 117.9(7) 1_555 1_555 1_555 yes S(1) C(3) C(4) 117.5(8) 1_555 1_555 1_555 yes S(5) C(3) C(4) 124.6(9) 1_555 1_555 1_555 yes S(2) C(4) S(6) 117.3(7) 1_555 1_555 1_555 yes S(2) C(4) C(3) 117.3(9) 1_555 1_555 1_555 yes S(6) C(4) C(3) 125.2(9) 1_555 1_555 1_555 yes S(3) C(5) S(7) 118.0(7) 1_555 1_555 1_555 yes S(3) C(5) C(6) 116.1(9) 1_555 1_555 1_555 yes S(7) C(5) C(6) 125.8(9) 1_555 1_555 1_555 yes S(4) C(6) S(8) 118.6(8) 1_555 1_555 1_555 yes S(4) C(6) C(5) 117.8(9) 1_555 1_555 1_555 yes S(8) C(6) C(5) 122.9(10) 1_555 1_555 1_555 yes S(5) C(7) H(4) 108(2) 1_555 1_555 1_555 no S(5) C(7) H(5) 114(2) 1_555 1_555 1_555 no S(5) C(7) H(6) 114(3) 1_555 1_555 1_555 no H(4) C(7) H(5) 103(4) 1_555 1_555 1_555 no H(4) C(7) H(6) 103(3) 1_555 1_555 1_555 no H(5) C(7) H(6) 110(2) 1_555 1_555 1_555 no S(6) C(8) H(1) 112(1) 1_555 1_555 1_555 no S(6) C(8) H(2) 113(1) 1_555 1_555 1_555 no S(6) C(8) H(3) 109(1) 1_555 1_555 1_555 no H(1) C(8) H(2) 109(1) 1_555 1_555 1_555 no H(1) C(8) H(3) 105(1) 1_555 1_555 1_555 no H(2) C(8) H(3) 106(1) 1_555 1_555 1_555 no S(7) C(9) C(10) 113.6(9) 1_555 1_555 1_555 yes S(7) C(9) H(7) 108.6(10) 1_555 1_555 1_555 no S(7) C(9) H(8) 108(1) 1_555 1_555 1_555 no C(10) C(9) H(7) 111(1) 1_555 1_555 1_555 no C(10) C(9) H(8) 107(1) 1_555 1_555 1_555 no H(7) C(9) H(8) 106(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 113(1) 1_555 1_555 1_555 yes C(9) C(10) H(9) 106(1) 1_555 1_555 1_555 no C(9) C(10) H(10) 108(1) 1_555 1_555 1_555 no C(11) C(10) H(9) 110(1) 1_555 1_555 1_555 no C(11) C(10) H(10) 111(1) 1_555 1_555 1_555 no H(9) C(10) H(10) 105(1) 1_555 1_555 1_555 no N(1) C(11) C(10) 176(1) 1_555 1_555 1_555 yes S(8) C(12) C(13) 115.9(10) 1_555 1_555 1_555 yes S(8) C(12) H(11) 108.4(10) 1_555 1_555 1_555 no S(8) C(12) H(12) 109(1) 1_555 1_555 1_555 no C(13) C(12) H(11) 107(1) 1_555 1_555 1_555 no C(13) C(12) H(12) 109(1) 1_555 1_555 1_555 no H(11) C(12) H(12) 105(1) 1_555 1_555 1_555 no C(12) C(13) C(14) 112(1) 1_555 1_555 1_555 yes C(12) C(13) H(13) 110(1) 1_555 1_555 1_555 no C(12) C(13) H(14) 108(1) 1_555 1_555 1_555 no C(14) C(13) H(13) 108(1) 1_555 1_555 1_555 no C(14) C(13) H(14) 109(1) 1_555 1_555 1_555 no H(13) C(13) H(14) 107(1) 1_555 1_555 1_555 no N(2) C(14) C(13) 177(1) 1_555 1_555 1_555 yes O(5) C(15) C(16) 85(2) 1_555 1_555 1_555 yes C(15) C(16) C(17) 115(3) 1_555 1_555 1_555 yes C(16) C(17) C(18) 128(3) 1_555 1_555 1_555 yes O(5) C(18) C(17) 81(2) 1_555 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 S(1) C(15) 3.55(3) 1_555 4_654 ? S(3) C(18) 3.55(4) 1_555 4_654 ? S(7) C(1) 3.53(1) 1_555 3_765 ? O(1) C(10) 3.39(3) 1_555 2_745 ? O(1) C(9) 3.53(2) 1_555 3_765 ? O(2) C(10) 3.43(2) 1_555 2_745 ? O(2) C(17) 3.47(3) 1_555 3_656 ? O(2) C(12) 3.50(2) 1_555 2_645 ? O(2) C(13) 3.52(2) 1_555 2_645 ? O(3) C(12) 3.29(2) 1_555 3_665 ? O(3) C(13) 3.36(2) 1_555 2_645 ? O(3) C(14) 3.54(3) 1_555 2_645 ? O(3) C(13) 3.58(3) 1_555 3_665 ? O(4) C(12) 3.35(2) 1_555 3_665 ? O(4) C(13) 3.35(2) 1_555 3_665 ? O(4) C(10) 3.39(2) 1_555 3_765 ? O(4) C(8) 3.44(2) 1_555 4_554 ? O(4) C(11) 3.47(2) 1_555 3_765 ? O(5) C(18) 3.50(5) 1_555 3_656 ? N(1) N(2) 3.23(2) 1_555 4_564 ? N(1) C(8) 3.38(2) 1_555 2_755 ? C(15) C(16) 3.37(4) 1_555 3_657 ? C(18) C(18) 3.24(9) 1_555 3_656 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ data_[Ag(cm-ttf)](CF3SO3) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Aug 7 04:28:13 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution MULTAN88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 723.69 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H14 Ag F3 N2 O3 S9 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.946(3) _cell_length_b 11.202(4) _cell_length_c 7.707(3) _cell_angle_alpha 92.95(3) _cell_angle_beta 109.25(2) _cell_angle_gamma 93.28(3) _cell_volume 644.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 8.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360.00 _exptl_absorpt_coefficient_mu 1.552 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.33 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 1 -2 1 -1 -1 2 0 _diffrn_reflns_number 3181 _reflns_number_total 2968 _reflns_number_gt 2915 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05213 _diffrn_orient_matrix_UB_12 0.07914 _diffrn_orient_matrix_UB_13 0.00035 _diffrn_orient_matrix_UB_21 -0.12293 _diffrn_orient_matrix_UB_22 -0.04058 _diffrn_orient_matrix_UB_23 -0.05725 _diffrn_orient_matrix_UB_31 -0.00697 _diffrn_orient_matrix_UB_32 -0.01140 _diffrn_orient_matrix_UB_33 0.12536 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_group Ag(1) Ag -1.256(2) 0.145(1) -1.660(2) 0.05759(9) Uani 1.00 d . . S(1) S -0.174(2) -0.665(1) -0.808(2) 0.0529(3) Uani 1.00 d . . S(2) S -0.434(2) -0.665(1) -0.548(2) 0.0539(3) Uani 1.00 d . . S(3) S -0.440(2) -0.515(1) -1.058(2) 0.0482(2) Uani 1.00 d . . S(4) S -0.677(2) -0.521(1) -0.833(2) 0.0455(2) Uani 1.00 d . . S(5) S -0.759(2) -0.432(1) -1.403(2) 0.0497(3) Uani 1.00 d . . S(6) S -0.998(2) -0.433(1) -1.181(2) 0.0496(3) Uani 1.00 d . . S(7) S -1.017(2) -0.319(1) -1.718(2) 0.0523(3) Uani 1.00 d . . S(8) S -1.288(2) -0.319(1) -1.466(2) 0.0557(3) Uani 1.00 d . . S(9) S -0.602(2) -1.017(1) -1.028(2) 0.0590(3) Uani 1.00 d . . F(1) F -0.655(2) -0.794(1) -1.079(2) 0.121(1) Uani 1.00 d . . F(2) F -0.830(2) -0.912(1) -1.292(2) 0.099(1) Uani 1.00 d . . F(3) F -0.870(2) -0.895(1) -1.037(2) 0.129(2) Uani 1.00 d . . O(1) O -0.534(2) -0.986(1) -0.837(2) 0.104(1) Uani 1.00 d . . O(2) O -0.476(2) -1.005(1) -1.124(2) 0.135(2) Uani 1.00 d . . O(3) O -0.718(2) -1.124(1) -1.091(2) 0.100(1) Uani 1.00 d . . N(1) N -1.027(2) 0.029(1) -1.716(2) 0.067(1) Uani 1.00 d . . N(2) N -1.256(2) 0.034(1) -1.421(2) 0.067(1) Uani 1.00 d . . C(1) C -0.184(2) -0.732(1) -1.032(2) 0.071(1) Uani 1.00 d . . C(2) C -0.641(2) -0.747(1) -0.566(2) 0.070(1) Uani 1.00 d . . C(3) C -0.376(2) -0.598(1) -0.862(2) 0.0383(7) Uani 1.00 d . . C(4) C -0.483(2) -0.599(1) -0.759(2) 0.0383(7) Uani 1.00 d . . C(5) C -0.653(2) -0.493(1) -1.047(2) 0.0378(7) Uani 1.00 d . . C(6) C -0.784(2) -0.457(1) -1.189(2) 0.0393(7) Uani 1.00 d . . C(7) C -0.962(2) -0.365(1) -1.494(2) 0.0411(7) Uani 1.00 d . . C(8) C -1.071(2) -0.366(1) -1.393(2) 0.0408(7) Uani 1.00 d . . C(9) C -0.818(2) -0.233(1) -1.710(2) 0.0501(9) Uani 1.00 d . . C(10) C -0.779(2) -0.116(1) -1.592(2) 0.0506(10) Uani 1.00 d . . C(11) C -0.919(2) -0.034(1) -1.660(2) 0.0493(10) Uani 1.00 d . . C(12) C -1.298(2) -0.243(1) -1.255(2) 0.0490(9) Uani 1.00 d . . C(13) C -1.173(2) -0.131(1) -1.190(2) 0.0436(9) Uani 1.00 d . . C(14) C -1.220(2) -0.037(1) -1.321(2) 0.0439(9) Uani 1.00 d . . C(15) C -0.740(2) -0.898(1) -1.114(2) 0.070(1) Uani 1.00 d . . H(1) H -0.1959 -0.6713 -1.1186 0.0868 Uiso 1.00 calc . . H(2) H -0.2859 -0.7884 -1.0784 0.0868 Uiso 1.00 calc . . H(3) H -0.0792 -0.7708 -1.0216 0.0868 Uiso 1.00 calc . . H(4) H -0.7341 -0.6917 -0.5833 0.0837 Uiso 1.00 calc . . H(5) H -0.6287 -0.7849 -0.4570 0.0837 Uiso 1.00 calc . . H(6) H -0.6748 -0.8033 -0.6690 0.0837 Uiso 1.00 calc . . H(7) H -0.8286 -0.2122 -1.8322 0.0599 Uiso 1.00 calc . . H(8) H -0.7193 -0.2777 -1.6637 0.0599 Uiso 1.00 calc . . H(9) H -0.6677 -0.0750 -1.5905 0.0622 Uiso 1.00 calc . . H(10) H -0.7689 -0.1291 -1.4681 0.0622 Uiso 1.00 calc . . H(11) H -1.2710 -0.2946 -1.1598 0.0585 Uiso 1.00 calc . . H(12) H -1.4182 -0.2184 -1.2766 0.0585 Uiso 1.00 calc . . H(13) H -1.0548 -0.1482 -1.1728 0.0535 Uiso 1.00 calc . . H(14) H -1.1785 -0.0978 -1.0722 0.0535 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) 0.0618(2) 0.0470(2) 0.0659(2) 0.0182(1) 0.0184(1) 0.0267(1) S(1) 0.0366(4) 0.0450(5) 0.0725(6) 0.0135(4) 0.0084(4) 0.0191(4) S(2) 0.0707(7) 0.0479(5) 0.0374(4) 0.0106(5) 0.0079(4) 0.0161(4) S(3) 0.0422(5) 0.0530(5) 0.0553(5) 0.0176(4) 0.0183(4) 0.0287(4) S(4) 0.0532(5) 0.0498(5) 0.0380(4) 0.0238(4) 0.0170(4) 0.0116(4) S(5) 0.0522(6) 0.0609(6) 0.0407(4) 0.0251(5) 0.0161(4) 0.0195(4) S(6) 0.0440(5) 0.0610(6) 0.0480(5) 0.0208(4) 0.0156(4) 0.0208(4) S(7) 0.0643(6) 0.0452(5) 0.0335(4) 0.0036(4) -0.0031(4) 0.0088(3) S(8) 0.0372(5) 0.0476(5) 0.0640(6) 0.0113(4) -0.0077(4) -0.0019(4) S(9) 0.0444(5) 0.0671(7) 0.0639(6) -0.0010(5) 0.0185(5) -0.0060(5) F(1) 0.122(3) 0.057(2) 0.137(3) -0.009(2) -0.011(3) -0.019(2) F(2) 0.108(3) 0.098(3) 0.065(2) 0.009(2) -0.004(2) -0.003(2) F(3) 0.090(3) 0.188(5) 0.134(3) 0.051(3) 0.067(3) -0.003(3) O(1) 0.097(3) 0.122(4) 0.064(2) 0.003(3) -0.009(2) 0.000(2) O(2) 0.106(4) 0.174(5) 0.181(5) 0.025(4) 0.121(4) 0.015(4) O(3) 0.096(3) 0.067(2) 0.108(3) -0.021(2) 0.002(3) 0.002(2) N(1) 0.075(3) 0.053(2) 0.076(3) 0.028(2) 0.024(2) 0.013(2) N(2) 0.088(3) 0.050(2) 0.063(2) 0.009(2) 0.022(2) 0.022(1) C(1) 0.078(3) 0.074(3) 0.084(2) 0.039(3) 0.051(3) 0.026(2) C(2) 0.083(3) 0.064(3) 0.072(3) 0.002(2) 0.036(3) 0.020(2) C(3) 0.037(1) 0.026(1) 0.046(2) 0.007(1) 0.003(1) 0.008(1) C(4) 0.046(2) 0.027(1) 0.035(1) 0.007(1) 0.002(1) 0.005(1) C(5) 0.040(1) 0.036(2) 0.039(1) 0.012(1) 0.013(1) 0.010(1) C(6) 0.042(1) 0.036(2) 0.039(1) 0.013(1) 0.012(1) 0.011(1) C(7) 0.046(2) 0.033(1) 0.037(1) 0.007(1) 0.002(1) 0.005(1) C(8) 0.039(1) 0.033(1) 0.042(1) 0.009(1) 0.001(1) 0.004(1) C(9) 0.068(2) 0.043(2) 0.045(2) 0.022(1) 0.021(2) 0.012(1) C(10) 0.053(2) 0.044(2) 0.049(2) 0.008(2) 0.009(2) 0.008(1) C(11) 0.058(2) 0.040(2) 0.048(2) 0.005(1) 0.016(2) 0.000(1) C(12) 0.041(2) 0.041(2) 0.071(2) 0.012(1) 0.023(2) 0.020(1) C(13) 0.040(2) 0.045(2) 0.043(2) 0.010(1) 0.009(1) 0.010(1) C(14) 0.043(2) 0.043(2) 0.044(2) 0.001(1) 0.013(2) 0.006(1) C(15) 0.070(3) 0.061(2) 0.063(2) 0.002(2) 0.005(2) -0.015(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2915 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0314 _refine_ls_wR_factor_gt 0.0314 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.416 _refine_ls_shift/su_max 0.0020 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.37 _refine_diff_density_max 0.36 #------------------------------------------------------------------------------ _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 S(1) C(1) 1.815(8) 1_555 1_555 yes S(1) C(3) 1.756(4) 1_555 1_555 yes S(2) C(2) 1.808(7) 1_555 1_555 yes S(2) C(4) 1.749(4) 1_555 1_555 yes S(3) C(3) 1.752(4) 1_555 1_555 yes S(3) C(5) 1.761(5) 1_555 1_555 yes S(4) C(4) 1.754(4) 1_555 1_555 yes S(4) C(5) 1.761(4) 1_555 1_555 yes S(5) C(6) 1.763(5) 1_555 1_555 yes S(5) C(7) 1.771(5) 1_555 1_555 yes S(6) C(6) 1.753(5) 1_555 1_555 yes S(6) C(8) 1.769(5) 1_555 1_555 yes S(7) C(7) 1.748(4) 1_555 1_555 yes S(7) C(9) 1.785(6) 1_555 1_555 yes S(8) C(8) 1.736(4) 1_555 1_555 yes S(8) C(12) 1.821(6) 1_555 1_555 yes S(9) O(1) 1.411(6) 1_555 1_555 yes S(9) O(2) 1.435(5) 1_555 1_555 yes S(9) O(3) 1.432(5) 1_555 1_555 yes S(9) C(15) 1.792(7) 1_555 1_555 yes F(1) F(2) 2.103(6) 1_555 1_555 yes F(1) F(3) 2.112(9) 1_555 1_555 yes F(1) C(15) 1.284(9) 1_555 1_555 yes F(2) F(3) 2.087(8) 1_555 1_555 yes F(2) C(15) 1.310(8) 1_555 1_555 yes F(3) C(15) 1.351(9) 1_555 1_555 yes N(1) C(11) 1.133(7) 1_555 1_555 yes N(2) C(14) 1.123(7) 1_555 1_555 yes C(3) C(4) 1.340(7) 1_555 1_555 yes C(5) C(6) 1.334(6) 1_555 1_555 yes C(7) C(8) 1.339(7) 1_555 1_555 yes C(9) C(10) 1.511(8) 1_555 1_555 yes C(10) C(11) 1.465(7) 1_555 1_555 yes C(12) C(13) 1.503(8) 1_555 1_555 yes C(13) C(14) 1.474(7) 1_555 1_555 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 C(1) S(1) C(3) 102.1(3) 1_555 1_555 1_555 yes C(2) S(2) C(4) 103.3(3) 1_555 1_555 1_555 yes C(3) S(3) C(5) 94.3(2) 1_555 1_555 1_555 yes C(4) S(4) C(5) 94.5(2) 1_555 1_555 1_555 yes C(6) S(5) C(7) 95.2(2) 1_555 1_555 1_555 yes C(6) S(6) C(8) 95.8(2) 1_555 1_555 1_555 yes C(7) S(7) C(9) 102.6(2) 1_555 1_555 1_555 yes C(8) S(8) C(12) 101.9(2) 1_555 1_555 1_555 yes O(1) S(9) O(2) 117.0(5) 1_555 1_555 1_555 yes O(1) S(9) O(3) 117.1(4) 1_555 1_555 1_555 yes O(1) S(9) C(15) 103.3(4) 1_555 1_555 1_555 yes O(2) S(9) O(3) 111.5(5) 1_555 1_555 1_555 yes O(2) S(9) C(15) 100.7(4) 1_555 1_555 1_555 yes O(3) S(9) C(15) 104.5(3) 1_555 1_555 1_555 yes F(2) F(1) F(3) 59.4(3) 1_555 1_555 1_555 yes F(2) F(1) C(15) 36.2(4) 1_555 1_555 1_555 yes F(3) F(1) C(15) 37.9(4) 1_555 1_555 1_555 yes F(1) F(2) F(3) 60.5(3) 1_555 1_555 1_555 yes F(1) F(2) C(15) 35.4(4) 1_555 1_555 1_555 yes F(3) F(2) C(15) 39.0(4) 1_555 1_555 1_555 yes F(1) F(3) F(2) 60.1(3) 1_555 1_555 1_555 yes F(1) F(3) C(15) 35.7(4) 1_555 1_555 1_555 yes F(2) F(3) C(15) 37.6(3) 1_555 1_555 1_555 yes S(1) C(1) H(1) 109(1) 1_555 1_555 1_555 no S(1) C(1) H(2) 108(1) 1_555 1_555 1_555 no S(1) C(1) H(3) 109(1) 1_555 1_555 1_555 no H(1) C(1) H(2) 108(1) 1_555 1_555 1_555 no H(1) C(1) H(3) 111(1) 1_555 1_555 1_555 no H(2) C(1) H(3) 109(2) 1_555 1_555 1_555 no S(2) C(2) H(4) 110(1) 1_555 1_555 1_555 no S(2) C(2) H(5) 110(1) 1_555 1_555 1_555 no S(2) C(2) H(6) 110(1) 1_555 1_555 1_555 no H(4) C(2) H(5) 106(1) 1_555 1_555 1_555 no H(4) C(2) H(6) 109(1) 1_555 1_555 1_555 no H(5) C(2) H(6) 109(1) 1_555 1_555 1_555 no S(1) C(3) S(3) 117.7(3) 1_555 1_555 1_555 yes S(1) C(3) C(4) 124.6(3) 1_555 1_555 1_555 yes S(3) C(3) C(4) 117.6(3) 1_555 1_555 1_555 yes S(2) C(4) S(4) 118.6(3) 1_555 1_555 1_555 yes S(2) C(4) C(3) 124.1(3) 1_555 1_555 1_555 yes S(4) C(4) C(3) 117.1(3) 1_555 1_555 1_555 yes S(3) C(5) S(4) 113.8(2) 1_555 1_555 1_555 yes S(3) C(5) C(6) 122.5(3) 1_555 1_555 1_555 yes S(4) C(5) C(6) 123.6(3) 1_555 1_555 1_555 yes S(5) C(6) S(6) 113.8(2) 1_555 1_555 1_555 yes S(5) C(6) C(5) 122.8(4) 1_555 1_555 1_555 yes S(6) C(6) C(5) 123.4(4) 1_555 1_555 1_555 yes S(5) C(7) S(7) 117.0(3) 1_555 1_555 1_555 yes S(5) C(7) C(8) 117.3(3) 1_555 1_555 1_555 yes S(7) C(7) C(8) 125.3(3) 1_555 1_555 1_555 yes S(6) C(8) S(8) 118.2(3) 1_555 1_555 1_555 yes S(6) C(8) C(7) 116.7(3) 1_555 1_555 1_555 yes S(8) C(8) C(7) 124.9(4) 1_555 1_555 1_555 yes S(7) C(9) C(10) 115.4(4) 1_555 1_555 1_555 yes S(7) C(9) H(7) 108(1) 1_555 1_555 1_555 no S(7) C(9) H(8) 108(1) 1_555 1_555 1_555 no S(7) C(9) H(9) 141.0(6) 1_555 1_555 1_555 no S(7) C(9) H(10) 100.0(6) 1_555 1_555 1_555 no C(10) C(9) H(7) 106(1) 1_555 1_555 1_555 no C(10) C(9) H(8) 107(1) 1_555 1_555 1_555 no C(10) C(9) H(9) 25.7(5) 1_555 1_555 1_555 no C(10) C(9) H(10) 26.3(6) 1_555 1_555 1_555 no H(7) C(9) H(8) 111(1) 1_555 1_555 1_555 no H(7) C(9) H(9) 94(1) 1_555 1_555 1_555 no H(7) C(9) H(10) 132(1) 1_555 1_555 1_555 no H(8) C(9) H(9) 91(1) 1_555 1_555 1_555 no H(8) C(9) H(10) 93(1) 1_555 1_555 1_555 no H(9) C(9) H(10) 44.2(4) 1_555 1_555 1_555 no C(9) C(10) C(11) 111.9(4) 1_555 1_555 1_555 yes C(9) C(10) H(7) 26.7(6) 1_555 1_555 1_555 no C(9) C(10) H(8) 26.7(6) 1_555 1_555 1_555 no C(9) C(10) H(9) 111(1) 1_555 1_555 1_555 no C(9) C(10) H(10) 110(1) 1_555 1_555 1_555 no C(11) C(10) H(7) 96.4(6) 1_555 1_555 1_555 no C(11) C(10) H(8) 138.6(7) 1_555 1_555 1_555 no C(11) C(10) H(9) 108(1) 1_555 1_555 1_555 no C(11) C(10) H(10) 108(1) 1_555 1_555 1_555 no H(7) C(10) H(8) 45.7(4) 1_555 1_555 1_555 no H(7) C(10) H(9) 97(1) 1_555 1_555 1_555 no H(7) C(10) H(10) 137(1) 1_555 1_555 1_555 no H(8) C(10) H(9) 94(1) 1_555 1_555 1_555 no H(8) C(10) H(10) 96(1) 1_555 1_555 1_555 no H(9) C(10) H(10) 107(1) 1_555 1_555 1_555 no N(1) C(11) C(10) 178.7(6) 1_555 1_555 1_555 yes N(1) C(11) H(9) 152.1(8) 1_555 1_555 1_555 no N(1) C(11) H(10) 153.6(7) 1_555 1_555 1_555 no C(10) C(11) H(9) 27.2(6) 1_555 1_555 1_555 no C(10) C(11) H(10) 27.7(6) 1_555 1_555 1_555 no H(9) C(11) H(10) 45.9(5) 1_555 1_555 1_555 no S(8) C(12) C(13) 114.3(4) 1_555 1_555 1_555 yes S(8) C(12) H(11) 110(1) 1_555 1_555 1_555 no S(8) C(12) H(12) 110(1) 1_555 1_555 1_555 no S(8) C(12) H(13) 99.2(6) 1_555 1_555 1_555 no S(8) C(12) H(14) 141.2(6) 1_555 1_555 1_555 no C(13) C(12) H(11) 107(1) 1_555 1_555 1_555 no C(13) C(12) H(12) 107(1) 1_555 1_555 1_555 no C(13) C(12) H(13) 25.8(6) 1_555 1_555 1_555 no C(13) C(12) H(14) 27.1(5) 1_555 1_555 1_555 no H(11) C(12) H(12) 105(1) 1_555 1_555 1_555 no H(11) C(12) H(13) 96(1) 1_555 1_555 1_555 no H(11) C(12) H(14) 90(1) 1_555 1_555 1_555 no H(12) C(12) H(13) 132(1) 1_555 1_555 1_555 no H(12) C(12) H(14) 93(1) 1_555 1_555 1_555 no H(13) C(12) H(14) 44.6(4) 1_555 1_555 1_555 no C(12) C(13) C(14) 111.9(4) 1_555 1_555 1_555 yes C(12) C(13) H(11) 27.1(6) 1_555 1_555 1_555 no C(12) C(13) H(12) 27.5(6) 1_555 1_555 1_555 no C(12) C(13) H(13) 110(1) 1_555 1_555 1_555 no C(12) C(13) H(14) 109(1) 1_555 1_555 1_555 no C(14) C(13) H(11) 138.6(6) 1_555 1_555 1_555 no C(14) C(13) H(12) 96.0(6) 1_555 1_555 1_555 no C(14) C(13) H(13) 109(1) 1_555 1_555 1_555 no C(14) C(13) H(14) 108(1) 1_555 1_555 1_555 no H(11) C(13) H(12) 45.1(4) 1_555 1_555 1_555 no H(11) C(13) H(13) 97(1) 1_555 1_555 1_555 no H(11) C(13) H(14) 91(1) 1_555 1_555 1_555 no H(12) C(13) H(13) 137(1) 1_555 1_555 1_555 no H(12) C(13) H(14) 95(1) 1_555 1_555 1_555 no H(13) C(13) H(14) 106(1) 1_555 1_555 1_555 no N(2) C(14) C(13) 179.9(6) 1_555 1_555 1_555 yes N(2) C(14) H(13) 153.9(7) 1_555 1_555 1_555 no N(2) C(14) H(14) 152.4(7) 1_555 1_555 1_555 no C(13) C(14) H(13) 26.2(5) 1_555 1_555 1_555 no C(13) C(14) H(14) 27.7(6) 1_555 1_555 1_555 no H(13) C(14) H(14) 45.3(5) 1_555 1_555 1_555 no S(9) C(15) F(1) 113.7(5) 1_555 1_555 1_555 yes S(9) C(15) F(2) 114.3(5) 1_555 1_555 1_555 yes S(9) C(15) F(3) 109.9(6) 1_555 1_555 1_555 yes F(1) C(15) F(2) 108.3(7) 1_555 1_555 1_555 yes F(1) C(15) F(3) 106.5(6) 1_555 1_555 1_555 yes F(2) C(15) F(3) 103.3(6) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ? ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_(CM-TTF)(CuCl2) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Aug 7 04:30:42 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution MITHRIL90 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 601.21 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H14 Cl2 Cu N2 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.487(2) _cell_length_b 13.620(6) _cell_length_c 9.908(8) _cell_angle_alpha 107.95(5) _cell_angle_beta 90.54(5) _cell_angle_gamma 74.99(3) _cell_volume 1296(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.2 _cell_measurement_theta_max 13.8 #---------------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606.00 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.994 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 2 0 1 2 2 0 2 _diffrn_reflns_number 6278 _reflns_number_total 5953 _reflns_number_gt 0 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02435 _diffrn_orient_matrix_UB_12 0.06940 _diffrn_orient_matrix_UB_13 0.03492 _diffrn_orient_matrix_UB_21 -0.09596 _diffrn_orient_matrix_UB_22 0.03981 _diffrn_orient_matrix_UB_23 0.01844 _diffrn_orient_matrix_UB_31 0.00114 _diffrn_orient_matrix_UB_32 -0.00464 _diffrn_orient_matrix_UB_33 0.09880 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1') Cl 0.5558(3) -0.1672(2) 0.4250(3) 0.0838(7) Uani 1.00 d ... Cl(2') Cl 1.0952(2) -0.1624(2) -0.0516(3) 0.0855(8) Uani 1.00 d ... Cu(1) Cu 0.5000 0.0000 0.5000 0.0610(4) Uani 1.00 d S.. Cu(2) Cu 1.0000 0.0000 0.0000 0.0670(4) Uani 1.00 d S.. Cl(1) Cl 0.4442(3) 0.1672(2) 0.5750(3) 0.0838(7) Uani 1.00 d ... Cl(2) Cl 0.9048(2) 0.1624(2) 0.0516(3) 0.0855(8) Uani 1.00 d ... S(1) S 0.1009(2) 0.3759(1) 1.0057(2) 0.0585(5) Uani 1.00 d ... S(2) S 0.1006(2) 0.3686(2) 1.3226(2) 0.0610(5) Uani 1.00 d ... S(3) S 0.2544(2) 0.1426(1) 0.9144(2) 0.0399(4) Uani 1.00 d ... S(4) S 0.2520(2) 0.1350(1) 1.2042(2) 0.0408(4) Uani 1.00 d ... S(5) S 0.4099(2) -0.1075(1) 0.7992(2) 0.0398(4) Uani 1.00 d ... S(6) S 0.4103(2) -0.1156(1) 1.0906(2) 0.0400(4) Uani 1.00 d ... S(7) S 0.5348(2) -0.3440(1) 0.6693(2) 0.0506(5) Uani 1.00 d ... S(8) S 0.5381(2) -0.3534(1) 0.9992(2) 0.0527(5) Uani 1.00 d ... N(1) N 0.3077(9) -0.5070(7) 0.712(1) 0.091(3) Uani 1.00 d ... N(2) N 0.1565(9) -0.369(1) 1.3017(10) 0.116(4) Uani 1.00 d ... C(1) C 0.1420(8) 0.3402(6) 0.8185(8) 0.059(2) Uani 1.00 d ... C(2) C 0.1199(9) 0.3219(7) 1.4707(8) 0.072(3) Uani 1.00 d ... C(3) C 0.1783(6) 0.2601(5) 1.0451(6) 0.037(2) Uani 1.00 d ... C(4) C 0.1769(6) 0.2566(5) 1.1824(6) 0.035(2) Uani 1.00 d ... C(5) C 0.2959(6) 0.0667(5) 1.0256(6) 0.033(1) Uani 1.00 d ... C(6) C 0.3639(6) -0.0405(5) 0.9766(6) 0.037(2) Uani 1.00 d ... C(7) C 0.4662(6) -0.2345(4) 0.8199(7) 0.039(2) Uani 1.00 d ... C(8) C 0.4674(6) -0.2379(5) 0.9546(7) 0.039(2) Uani 1.00 d ... C(9) C 0.3987(8) -0.3374(6) 0.5559(7) 0.054(2) Uani 1.00 d ... C(10) C 0.2700(7) -0.3430(6) 0.6199(8) 0.059(2) Uani 1.00 d ... C(11) C 0.2890(7) -0.4359(8) 0.6706(8) 0.063(2) Uani 1.00 d ... C(12) C 0.4260(7) -0.3441(6) 1.1435(7) 0.049(2) Uani 1.00 d ... C(13) C 0.2925(7) -0.3578(6) 1.0945(8) 0.052(2) Uani 1.00 d ... C(14) C 0.2151(8) -0.3644(8) 1.2081(10) 0.071(3) Uani 1.00 d ... loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1') 0.107(2) 0.054(1) 0.083(2) -0.019(1) -0.009(1) 0.014(1) Cl(2') 0.053(1) 0.067(1) 0.129(2) -0.0082(10) -0.007(1) 0.029(1) Cu(1) 0.0775(9) 0.0528(8) 0.0521(8) -0.0192(7) -0.0056(6) 0.0144(6) Cu(2) 0.0437(7) 0.0655(9) 0.089(1) -0.0079(6) -0.0029(7) 0.0261(8) Cl(1) 0.107(2) 0.054(1) 0.083(2) -0.019(1) -0.009(1) 0.014(1) Cl(2) 0.053(1) 0.067(1) 0.129(2) -0.0082(10) -0.007(1) 0.029(1) S(1) 0.069(1) 0.047(1) 0.048(1) 0.0125(9) 0.0054(9) 0.0229(8) S(2) 0.073(1) 0.048(1) 0.0415(10) 0.0116(9) 0.0070(9) 0.0082(8) S(3) 0.0434(9) 0.0380(8) 0.0321(8) -0.0008(7) -0.0015(6) 0.0108(7) S(4) 0.0461(9) 0.0382(8) 0.0359(8) -0.0036(7) 0.0007(7) 0.0151(7) S(5) 0.0463(9) 0.0357(8) 0.0356(8) -0.0093(7) -0.0060(7) 0.0105(6) S(6) 0.0451(9) 0.0364(8) 0.0401(8) -0.0095(7) -0.0012(7) 0.0154(7) S(7) 0.0456(9) 0.0382(9) 0.056(1) -0.0059(7) -0.0011(8) 0.0021(8) S(8) 0.0496(10) 0.0393(9) 0.072(1) -0.0050(7) 0.0001(8) 0.0264(9) N(1) 0.096(6) 0.076(5) 0.121(7) -0.037(5) -0.012(5) 0.046(5) N(2) 0.090(6) 0.21(1) 0.079(6) -0.079(7) -0.009(5) 0.057(6) C(1) 0.060(5) 0.071(5) 0.055(4) -0.011(4) -0.010(3) 0.037(4) C(2) 0.084(6) 0.087(6) 0.034(4) -0.008(5) 0.006(4) 0.017(4) C(3) 0.036(3) 0.033(3) 0.039(3) -0.002(2) -0.002(3) 0.012(3) C(4) 0.036(3) 0.036(3) 0.029(3) -0.004(2) 0.001(2) 0.010(2) C(5) 0.032(3) 0.032(3) 0.037(3) -0.006(2) 0.001(2) 0.013(2) C(6) 0.038(3) 0.038(3) 0.038(3) -0.014(3) -0.007(3) 0.011(3) C(7) 0.041(3) 0.026(3) 0.046(4) -0.008(3) -0.007(3) 0.007(3) C(8) 0.037(3) 0.031(3) 0.048(4) -0.009(3) -0.002(3) 0.012(3) C(9) 0.074(5) 0.052(4) 0.037(4) -0.022(4) -0.010(3) 0.013(3) C(10) 0.059(5) 0.060(5) 0.057(4) -0.017(4) -0.016(4) 0.018(4) C(11) 0.051(4) 0.076(6) 0.057(5) -0.024(4) -0.005(4) 0.009(4) C(12) 0.053(4) 0.050(4) 0.054(4) -0.020(3) -0.012(3) 0.026(3) C(13) 0.055(4) 0.056(4) 0.052(4) -0.012(3) -0.008(3) 0.026(3) C(14) 0.055(5) 0.097(7) 0.065(5) -0.028(5) -0.013(4) 0.026(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2733 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0000 _refine_ls_R_factor_gt 0.0000 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0000 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.393 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.41 _refine_diff_density_max 0.67 #------------------------------------------------------------------------------ _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) Cl(1) 2.087(2) 1_555 1_555 yes Cu(1) Cl(1) 2.087(2) 1_555 2_656 yes Cu(2) Cl(2) 2.078(2) 1_555 1_555 yes Cu(2) Cl(2) 2.078(2) 1_555 2_755 yes S(1) C(1) 1.793(8) 1_555 1_555 yes S(1) C(3) 1.735(6) 1_555 1_555 yes S(2) C(2) 1.762(8) 1_555 1_555 yes S(2) C(4) 1.726(6) 1_555 1_555 yes S(3) C(3) 1.719(6) 1_555 1_555 yes S(3) C(5) 1.712(6) 1_555 1_555 yes S(4) C(4) 1.719(6) 1_555 1_555 yes S(4) C(5) 1.728(6) 1_555 1_555 yes S(5) C(6) 1.719(6) 1_555 1_555 yes S(5) C(7) 1.752(6) 1_555 1_555 yes S(6) C(6) 1.732(6) 1_555 1_555 yes S(6) C(8) 1.751(6) 1_555 1_555 yes S(7) C(7) 1.749(6) 1_555 1_555 yes S(7) C(9) 1.809(7) 1_555 1_555 yes S(8) C(8) 1.742(6) 1_555 1_555 yes S(8) C(12) 1.813(7) 1_555 1_555 yes N(1) C(11) 1.13(1) 1_555 1_555 yes N(2) C(14) 1.15(1) 1_555 1_555 yes C(3) C(4) 1.375(8) 1_555 1_555 yes C(5) C(6) 1.382(8) 1_555 1_555 yes C(7) C(8) 1.349(9) 1_555 1_555 yes C(9) C(10) 1.53(1) 1_555 1_555 yes C(10) C(11) 1.47(1) 1_555 1_555 yes C(12) C(13) 1.516(10) 1_555 1_555 yes C(13) C(14) 1.43(1) 1_555 1_555 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 Cl(1) Cu(1) Cl(1) 180.0 1_555 1_555 2_656 yes Cl(2) Cu(2) Cl(2) 180.0 1_555 1_555 2_755 yes C(1) S(1) C(3) 103.3(3) 1_555 1_555 1_555 yes C(2) S(2) C(4) 103.5(3) 1_555 1_555 1_555 yes C(3) S(3) C(5) 96.0(3) 1_555 1_555 1_555 yes C(4) S(4) C(5) 95.9(3) 1_555 1_555 1_555 yes C(6) S(5) C(7) 95.2(3) 1_555 1_555 1_555 yes C(6) S(6) C(8) 94.9(3) 1_555 1_555 1_555 yes C(7) S(7) C(9) 100.9(3) 1_555 1_555 1_555 yes C(8) S(8) C(12) 103.4(3) 1_555 1_555 1_555 yes S(1) C(1) H(1) 110.3(6) 1_555 1_555 1_555 no S(1) C(1) H(2) 110.0(6) 1_555 1_555 1_555 no S(1) C(1) H(3) 110.4(6) 1_555 1_555 1_555 no H(1) C(1) H(2) 108.5(7) 1_555 1_555 1_555 no H(1) C(1) H(3) 109.0(8) 1_555 1_555 1_555 no H(2) C(1) H(3) 108.6(8) 1_555 1_555 1_555 no S(2) C(2) H(4) 110.1(7) 1_555 1_555 1_555 no S(2) C(2) H(5) 110.5(6) 1_555 1_555 1_555 no S(2) C(2) H(6) 110.2(6) 1_555 1_555 1_555 no H(4) C(2) H(5) 108.8(8) 1_555 1_555 1_555 no H(4) C(2) H(6) 108.3(8) 1_555 1_555 1_555 no H(5) C(2) H(6) 108.8(9) 1_555 1_555 1_555 no S(1) C(3) S(3) 121.9(4) 1_555 1_555 1_555 yes S(1) C(3) C(4) 121.4(4) 1_555 1_555 1_555 yes S(3) C(3) C(4) 116.6(4) 1_555 1_555 1_555 yes S(2) C(4) S(4) 122.7(3) 1_555 1_555 1_555 yes S(2) C(4) C(3) 121.1(4) 1_555 1_555 1_555 yes S(4) C(4) C(3) 116.2(4) 1_555 1_555 1_555 yes S(3) C(5) S(4) 115.3(3) 1_555 1_555 1_555 yes S(3) C(5) C(6) 122.3(4) 1_555 1_555 1_555 yes S(4) C(5) C(6) 122.4(4) 1_555 1_555 1_555 yes S(5) C(6) S(6) 115.8(3) 1_555 1_555 1_555 yes S(5) C(6) C(5) 122.2(4) 1_555 1_555 1_555 yes S(6) C(6) C(5) 122.0(4) 1_555 1_555 1_555 yes S(5) C(7) S(7) 118.3(4) 1_555 1_555 1_555 yes S(5) C(7) C(8) 116.5(4) 1_555 1_555 1_555 yes S(7) C(7) C(8) 124.7(5) 1_555 1_555 1_555 yes S(6) C(8) S(8) 119.2(4) 1_555 1_555 1_555 yes S(6) C(8) C(7) 116.9(4) 1_555 1_555 1_555 yes S(8) C(8) C(7) 123.6(5) 1_555 1_555 1_555 yes S(7) C(9) C(10) 114.7(5) 1_555 1_555 1_555 yes S(7) C(9) H(7) 108.2(5) 1_555 1_555 1_555 no S(7) C(9) H(8) 108.3(6) 1_555 1_555 1_555 no S(7) C(9) H(9) 102.9(3) 1_555 1_555 1_555 no S(7) C(9) H(10) 140.4(4) 1_555 1_555 1_555 no C(10) C(9) H(7) 109.2(7) 1_555 1_555 1_555 no C(10) C(9) H(8) 108.7(6) 1_555 1_555 1_555 no C(10) C(9) H(9) 26.2(3) 1_555 1_555 1_555 no C(10) C(9) H(10) 25.9(3) 1_555 1_555 1_555 no H(7) C(9) H(8) 107.6(6) 1_555 1_555 1_555 no H(7) C(9) H(9) 92.8(5) 1_555 1_555 1_555 no H(7) C(9) H(10) 96.7(5) 1_555 1_555 1_555 no H(8) C(9) H(9) 134.4(6) 1_555 1_555 1_555 no H(8) C(9) H(10) 92.1(5) 1_555 1_555 1_555 no H(9) C(9) H(10) 44.3(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 112.3(6) 1_555 1_555 1_555 yes C(9) C(10) H(7) 26.3(3) 1_555 1_555 1_555 no C(9) C(10) H(8) 26.4(3) 1_555 1_555 1_555 no C(9) C(10) H(9) 109.3(7) 1_555 1_555 1_555 no C(9) C(10) H(10) 110.1(7) 1_555 1_555 1_555 no C(11) C(10) H(7) 138.3(6) 1_555 1_555 1_555 no C(11) C(10) H(8) 100.9(5) 1_555 1_555 1_555 no C(11) C(10) H(9) 108.5(7) 1_555 1_555 1_555 no C(11) C(10) H(10) 108.7(7) 1_555 1_555 1_555 no H(7) C(10) H(8) 44.5(2) 1_555 1_555 1_555 no H(7) C(10) H(9) 92.9(5) 1_555 1_555 1_555 no H(7) C(10) H(10) 97.4(6) 1_555 1_555 1_555 no H(8) C(10) H(9) 135.3(7) 1_555 1_555 1_555 no H(8) C(10) H(10) 93.1(5) 1_555 1_555 1_555 no H(9) C(10) H(10) 107.8(7) 1_555 1_555 1_555 no N(1) C(11) C(10) 177.6(8) 1_555 1_555 1_555 yes N(1) C(11) H(9) 152.3(8) 1_555 1_555 1_555 no N(1) C(11) H(10) 155.2(7) 1_555 1_555 1_555 no C(10) C(11) H(9) 27.2(4) 1_555 1_555 1_555 no C(10) C(11) H(10) 27.1(3) 1_555 1_555 1_555 no H(9) C(11) H(10) 45.8(2) 1_555 1_555 1_555 no S(8) C(12) C(13) 112.6(5) 1_555 1_555 1_555 yes S(8) C(12) H(11) 109.0(5) 1_555 1_555 1_555 no S(8) C(12) H(12) 109.1(5) 1_555 1_555 1_555 no S(8) C(12) H(13) 100.7(3) 1_555 1_555 1_555 no S(8) C(12) H(14) 95.2(3) 1_555 1_555 1_555 no C(13) C(12) H(11) 109.0(6) 1_555 1_555 1_555 no C(13) C(12) H(12) 109.3(6) 1_555 1_555 1_555 no C(13) C(12) H(13) 26.1(3) 1_555 1_555 1_555 no C(13) C(12) H(14) 26.1(3) 1_555 1_555 1_555 no H(11) C(12) H(12) 107.8(6) 1_555 1_555 1_555 no H(11) C(12) H(13) 134.8(5) 1_555 1_555 1_555 no H(11) C(12) H(14) 98.5(5) 1_555 1_555 1_555 no H(12) C(12) H(13) 93.1(5) 1_555 1_555 1_555 no H(12) C(12) H(14) 135.1(6) 1_555 1_555 1_555 no H(13) C(12) H(14) 44.4(1) 1_555 1_555 1_555 no C(12) C(13) C(14) 109.9(6) 1_555 1_555 1_555 yes C(12) C(13) H(11) 26.4(3) 1_555 1_555 1_555 no C(12) C(13) H(12) 26.3(3) 1_555 1_555 1_555 no C(12) C(13) H(13) 109.9(6) 1_555 1_555 1_555 no C(12) C(13) H(14) 109.9(6) 1_555 1_555 1_555 no C(14) C(13) H(11) 92.4(5) 1_555 1_555 1_555 no C(14) C(13) H(12) 98.0(5) 1_555 1_555 1_555 no C(14) C(13) H(13) 109.7(7) 1_555 1_555 1_555 no C(14) C(13) H(14) 109.8(7) 1_555 1_555 1_555 no H(11) C(13) H(12) 44.6(2) 1_555 1_555 1_555 no H(11) C(13) H(13) 136.0(6) 1_555 1_555 1_555 no H(11) C(13) H(14) 99.2(5) 1_555 1_555 1_555 no H(12) C(13) H(13) 93.6(5) 1_555 1_555 1_555 no H(12) C(13) H(14) 135.9(6) 1_555 1_555 1_555 no H(13) C(13) H(14) 107.7(7) 1_555 1_555 1_555 no N(2) C(14) C(13) 177.8(9) 1_555 1_555 1_555 yes N(2) C(14) H(13) 153.8(9) 1_555 1_555 1_555 no N(2) C(14) H(14) 153.8(9) 1_555 1_555 1_555 no C(13) C(14) H(13) 27.3(3) 1_555 1_555 1_555 no C(13) C(14) H(14) 27.2(3) 1_555 1_555 1_555 no H(13) C(14) H(14) 46.2(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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 Cu(2) C(5) 3.439(6) 1_555 1_654 ? Cu(2) C(5) 3.439(6) 1_555 2_656 ? Cl(1) C(12) 3.595(7) 1_555 2_657 ? Cl(2) C(3) 3.469(7) 1_555 1_654 ? Cl(2) C(4) 3.503(6) 1_555 1_654 ? Cl(2) C(10) 3.585(8) 1_555 2_656 ? Cl(2) C(6) 3.591(6) 1_555 2_656 ? Cl(2) C(13) 3.596(7) 1_555 2_656 ? S(1) S(1) 3.526(3) 1_555 2_567 ? S(3) S(6) 3.439(2) 1_555 2_657 ? S(3) C(8) 3.569(6) 1_555 2_657 ? S(4) S(5) 3.467(2) 1_555 2_657 ? S(4) C(7) 3.593(6) 1_555 2_657 ? S(6) C(5) 3.587(6) 1_555 2_657 ? N(1) C(1) 3.43(1) 1_555 1_545 ? N(1) C(12) 3.57(1) 1_555 2_647 ? N(2) C(10) 3.31(1) 1_555 1_556 ? N(2) C(1) 3.31(1) 1_555 2_557 ? N(2) C(2) 3.49(1) 1_555 2_558 ? N(2) C(9) 3.57(1) 1_555 1_556 ? C(1) C(2) 3.388(10) 1_555 1_554 ? C(5) C(6) 3.491(8) 1_555 2_657 ? C(6) C(6) 3.30(1) 1_555 2_657 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ? ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;