Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_MIZUNO7#1_971020_50-26-0.8 _database_code_CSD 162981 _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Honda, Kazumasa' 'Kokubo, Hisashi' 'Mizuno, Masagi' _publ_contact_author_name 'Masagi Mizuno' _publ_contact_author_address ; National Institute of Advanced Industrial Science and Technology Tsukuba Central 5, 1-1 Higashi, Tsukuba, Ibaraki 305-8565, Japan ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email 'mizuno-msg@aist.go.jp' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Preparation, Structure and Conduction Properties of SeCN-containing Mixed Anion TTF Conductors ; _publ_section_references ; Enraf-Nonius Delft, Scientific Instruments Division. (1989). Enraf-Nonius CAD4 diffractometer hardware, its controlling software and the operating system. Version 5.0. Enraf-Nonius Delft, Scientific Instruments Division, PO Box 483, 2600 AL Delft, The Netherlands. Johnson, C. K. (1976). ORTEP II. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation (1994) TEXSAN version 1.6f. Single Crystal Structure Analysis Software. MSC, 3200 research forest Drive, The Woodlands, TX77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G. M. (1985). SHELXS86. Program for the Solution of Crystal Structure. University of Gottingen, Germany. ; #------------------------------------------------------------------------------ _audit_creation_date 'Thu Feb 9 19:09:32 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record '20-Apr-2001 Updated by K. Honda' #------------------------------------------------------------------------------ _computing_data_collection 'CAD4 diffractometer control (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 diffractometer control (Enraf-Nonius, 1989)' _computing_data_reduction 'TEXSAN PROCESS' _computing_structure_solution 'SHELXS86(Sheldrick,1985)' _computing_structure_refinement 'TEXSAN LS' _computing_publication_material 'TEXSAN FINISH' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' #------------------------------------------------------------------------------ _chemical_formula_weight 246.88 _chemical_formula_sum 'C6.26 H4 Cl0.43 N0.26 S4 Se0.26' _chemical_formula_moiety '(C6 H4 S4)1 0.69+, (C N Se)0.26 -, Cl0.43 -' #------------------------------------------------------------------------------ _cell_length_a 11.2031(6) _cell_length_b 11.2031(6) _cell_length_c 3.6001(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 451.85(4) _cell_formula_units_Z 2.00 _cell_measurement_temperature 300 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 17.48 _cell_measurement_theta_max 19.59 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/m n m ' _symmetry_Int_Tables_number 136 _symmetry_space_group_name_Hall ' -P 4n 2n' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' '1/2+x,1/2-y,1/2+z' '1/2-x,1/2+y,1/2+z' ' +y, +x, +z' ' -y, -x, +z' '1/2+y,1/2-x,1/2+z' '1/2-y,1/2+x,1/2+z' ' -x, -y, -z' ' +x, +y, -z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2-z' ' -y, -x, -z' ' +y, +x, -z' '1/2-y,1/2+x,1/2-z' '1/2+y,1/2-x,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_meas 1.800 _exptl_crystal_density_method 'flotation in ZnCl~2~ aqueous solution' _exptl_crystal_F_000 247.06 _exptl_absorpt_coefficient_mu 2.1542 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.868 #------------------------------------------------------------------------------ _diffrn_special_details ? _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Nonius CAD4' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.06 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 0 1 3 0 0 0 -2 _diffrn_reflns_number 857 _reflns_number_total 400 _reflns_number_gt 258 _reflns_threshold_expression >1.0sigma(I) _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.082 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _diffrn_reflns_theta_full 78.5 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01135 _diffrn_orient_matrix_UB_12 -0.05690 _diffrn_orient_matrix_UB_13 -0.21136 _diffrn_orient_matrix_UB_21 0.00915 _diffrn_orient_matrix_UB_22 0.06888 _diffrn_orient_matrix_UB_23 -0.17473 _diffrn_orient_matrix_UB_31 0.08814 _diffrn_orient_matrix_UB_32 0.00016 _diffrn_orient_matrix_UB_33 0.04542 #------------------------------------------------------------------------------ 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 Cl 0 0.86 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 12 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 8 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 Cl1 0.0000 0.5000 0.0000 0.045(3) Uiso d . 0.114 P Cl2 0.0000 0.5000 0.2500 0.045(3) Uiso d . 0.101 P S1 0.0100(3) 0.8061(3) 0.0000 0.0584(9) Uani d . 1.0 S C1 0.0412(9) 0.9588 0.0000 0.042(2) Uani d . 1.0 S C2 0.158(1) 0.760(1) 0.0000 0.069(5) Uani d . 1.0 S C11 0.0000 0.5000 0.0000 0.0451 Uiso d . 0.069 P C12 0.0000 0.5000 0.2500 0.0446 Uiso d . 0.061 P H1 0.16(1) 0.665(10) 0.0000 0.07(3) Uiso d . 1.0 S 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 S1 0.066(2) 0.049(2) 0.061(2) -0.002(2) 0.0000 0.0000 C1 0.045(5) 0.0447 0.038(9) -0.010(6) 0.0000 0.0000 C2 0.076(9) 0.061(8) 0.07(1) 0.018(7) 0.0000 0.0000 #------------------------------------------------------------------------------ _refine_special_details ? _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) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 258 _refine_ls_number_parameters 22 _refine_ls_number_restraints 0 _refine_ls_number_constraints 30 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_all 0.1086 _refine_ls_wR_factor_ref 0.1063 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 4.043 _refine_ls_shift/su_max 0.00009 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.77310 _refine_diff_density_min -0.26300 #------------------------------------------------------------------------------ _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 S1 C1 1.746(4) 1_555 1_555 yes S1 C2 1.73(1) 1_555 1_555 yes C1 C1 1.31(1) 1_555 2_575 yes C2 C2 1.31(3) 1_555 6_665 yes C2 H1 1.1(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 C1 S1 C2 95.9(6) 1_555 1_555 1_555 yes S1 C1 S1 113.0(8) 1_555 1_555 6_665 yes S1 C1 C1 123.5(4) 1_555 1_555 2_575 yes S1 C2 C2 117.5(5) 1_555 1_555 6_665 yes S1 C2 H1 108(6) 1_555 1_555 1_555 no C2 C2 H1 134(6) 6_665 1_555 1_555 no #------------------------------------------------------------------------------