Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_theta_(DIETS)2Au(CN)4 _audit_creation_date 'Fri Jul 13 13:31:20 2001' _audit_creation_method 'by teXsan' _audit_update_record ? _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Tatsuro Imakubo' 'Naoya Tajima' 'Masafumi Tamura' 'Reizo Kato' 'Yutaka Nishio' 'Koji Kajita' # SUBMISSION DETAILS _publ_contact_author_name ' Dr. Tatsuro Imakubo' _publ_contact_author_address ; RIKEN, 2-1 Hiorosawa, Wako, Saitama 351-0198, Japan ; _publ_contact_author_email ' imakubo@postman.riken.go.jp ' _publ_contact_author_fax ' +81-48-462-4661 ' _publ_contact_author_phone ' +81-48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; A Supramolecular Organic Superconductor theta-(DIETS)2[Au(CN)4] ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. 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. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _database_code_CSD 167386 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H8 Au I4 N4 S8 Se4 ' _chemical_formula_moiety 'theta (DIETS)2Au(CN)4' _chemical_formula_weight 1581.21 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pnnm' _symmetry_Int_Tables_number 58 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 -x,-y,-z x,y,-z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,1/2+z _cell_length_a 4.274(4) _cell_length_b 11.114(3) _cell_length_c 37.426(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1777(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 11.6 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'rod' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.954 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 12.216 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.191 _exptl_absorpt_correction_T_max 0.295 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3091 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max ? _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.80 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 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 0 _reflns_number_gt 0 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0000 _refine_ls_wR_factor_ref 0.0415 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1905 _refine_ls_number_parameters 0 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.29 _refine_diff_density_min -1.09 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Au' 'Au' -2.013 8.802 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;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) ; #------------------------------------------------------------------------------ # 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 Au(1) Au 1.0000 0.5000 0.0000 0.0264(1) Uani 1.00 d S . . I(1) I 0.2237(1) 0.15117(4) 0.06050(1) 0.0373(1) Uani 1.00 d . . . Se(1) Se 0.1685(2) 0.12747(7) 0.23413(2) 0.0369(2) Uani 1.00 d . . . S(1) S 0.1722(5) 0.1431(2) 0.31475(4) 0.0418(5) Uani 1.00 d . . . S(2) S 0.1619(5) 0.1152(2) 0.14549(4) 0.0396(5) Uani 1.00 d . . . N(1) N 0.506(2) 0.2942(9) 0.0000 0.046(3) Uani 1.00 d S . . N(2) N 1.0000 0.5000 0.0839(2) 0.065(4) Uani 1.00 d S . . C(1) C 0.0000 0.0000 0.2071(2) 0.033(2) Uani 1.00 d S . . C(2) C 0.0000 0.0000 0.1709(2) 0.035(2) Uani 1.00 d S . . C(3) C 0.065(2) 0.0533(6) 0.2785(1) 0.030(2) Uani 1.00 d . . . C(4) C 0.076(2) 0.0527(6) 0.1041(1) 0.027(2) Uani 1.00 d . . . C(5) C -0.026(2) 0.0668(7) 0.3513(2) 0.040(2) Uani 1.00 d . . . C(6) C 0.694(2) 0.3653(9) 0.0000 0.031(2) Uani 1.00 d S . . C(7) C 1.0000 0.5000 0.0534(2) 0.035(2) Uani 1.00 d S . . H(1) H 0.0377 0.1011 0.3735 0.0474 Uiso 1.00 calc . . . H(2) H -0.2505 0.0812 0.3490 0.0474 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 Au(1) 0.0304(3) 0.0265(2) 0.0222(2) -0.0011(2) 0.0000 0.0000 I(1) 0.0478(3) 0.0354(3) 0.0288(2) -0.0018(2) 0.0048(2) 0.0085(2) Se(1) 0.0543(5) 0.0341(4) 0.0222(3) -0.0063(4) 0.0003(3) 0.0004(3) S(1) 0.056(1) 0.045(1) 0.0237(7) -0.006(1) -0.0021(8) -0.0054(7) S(2) 0.062(1) 0.0331(9) 0.0242(7) -0.0129(9) 0.0015(8) -0.0030(6) N(1) 0.041(5) 0.049(6) 0.048(5) -0.007(5) 0.0000 0.0000 N(2) 0.089(9) 0.084(8) 0.023(4) 0.026(7) 0.0000 0.0000 C(1) 0.043(5) 0.033(5) 0.024(4) -0.007(5) 0.0000 0.0000 C(2) 0.052(6) 0.027(4) 0.025(4) -0.005(5) 0.0000 0.0000 C(3) 0.035(4) 0.038(4) 0.018(2) 0.004(3) -0.001(2) -0.002(2) C(4) 0.037(4) 0.025(3) 0.019(2) -0.002(3) 0.000(2) -0.001(2) C(5) 0.047(5) 0.051(4) 0.023(3) 0.009(4) -0.002(3) -0.001(3) C(6) 0.038(5) 0.029(5) 0.025(4) 0.000(5) 0.0000 0.0000 C(7) 0.049(6) 0.030(5) 0.027(4) -0.011(5) 0.0000 0.0000 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SAPI91' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 Au(1) C(6) 1.99(1) . . yes Au(1) C(6) 1.99(1) . 2_765 yes Au(1) C(7) 1.999(9) . . yes Au(1) C(7) 1.999(9) . 5_765 yes I(1) C(4) 2.063(6) . . yes Se(1) C(1) 1.883(5) . . yes Se(1) C(3) 1.906(6) . . yes S(1) C(3) 1.744(6) . . yes S(1) C(5) 1.821(8) . . yes S(2) C(2) 1.738(5) . . yes S(2) C(4) 1.737(6) . . yes N(1) C(6) 1.13(1) . . yes N(2) C(7) 1.14(1) . . yes C(1) C(2) 1.36(1) . . yes C(3) C(3) 1.31(1) . 2_555 yes C(4) C(4) 1.34(1) . 2_555 yes C(5) C(5) 1.50(2) . 2_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(6) Au(1) C(6) 180.0 0_555 0_555 0_555 yes C(6) Au(1) C(7) 90.0 0_555 0_555 0_555 yes C(6) Au(1) C(7) 90.0 0_555 0_555 0_555 yes C(6) Au(1) C(7) 90.0 0_555 0_555 0_555 yes C(6) Au(1) C(7) 90.0 0_555 0_555 0_555 yes C(7) Au(1) C(7) 180.0 0_555 0_555 0_555 yes C(1) Se(1) C(3) 93.1(3) 0_555 0_555 0_555 yes C(3) S(1) C(5) 101.3(3) 0_555 0_555 0_555 yes C(2) S(2) C(4) 96.2(3) 0_555 0_555 0_555 yes Se(1) C(1) Se(1) 115.1(4) 0_555 0_555 0_555 yes Se(1) C(1) C(2) 122.4(2) 0_555 0_555 0_555 yes Se(1) C(1) C(2) 122.4(2) 0_555 0_555 0_555 yes S(2) C(2) S(2) 113.8(5) 0_555 0_555 0_555 yes S(2) C(2) C(1) 123.1(2) 0_555 0_555 0_555 yes S(2) C(2) C(1) 123.1(2) 0_555 0_555 0_555 yes Se(1) C(3) S(1) 111.7(4) 0_555 0_555 0_555 yes Se(1) C(3) C(3) 119.3(2) 0_555 0_555 0_555 yes S(1) C(3) C(3) 129.0(2) 0_555 0_555 0_555 yes I(1) C(4) S(2) 115.4(3) 0_555 0_555 0_555 yes I(1) C(4) C(4) 127.7(2) 0_555 0_555 0_555 yes S(2) C(4) C(4) 116.9(2) 0_555 0_555 0_555 yes S(1) C(5) C(5) 113.0(5) 0_555 0_555 0_555 yes Au(1) C(6) N(1) 175.7(10) 0_555 0_555 0_555 yes Au(1) C(7) N(2) 180.0 0_555 0_555 0_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 Au(1) N(1) 3.15(1) . 1_655 ? Au(1) N(1) 3.15(1) . 2_665 ? Au(1) C(6) 3.32(1) . 1_655 ? Au(1) C(6) 3.32(1) . 2_665 ? I(1) N(1) 3.018(7) . . ? N(1) C(6) 3.56(1) . 1_455 ? N(2) C(5) 3.243(10) . 3_655 ? N(2) C(5) 3.243(10) . 4_555 ? N(2) C(5) 3.388(9) . 3_555 ? N(2) C(5) 3.388(9) . 4_655 ? C(6) C(6) 3.42(2) . 2_665 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------