# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jun-ichi Yamada' _publ_contact_author_address ; Department of Material Science University of Hyogo Graduate School of Material Science 3-2-1 Kouto Kamigori-cho Ako-gun Hyogo 678-1297 JAPAN ; _publ_contact_author_email YAMADA@SCI.U-HYOGO.AC.JP _publ_section_title ; Pressure effect on the electrical conductivity and superconductivity of beta-(BDA-TTP)2I3 ; _audit_creation_date 2004-05-27 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. 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. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; loop_ _publ_author_name 'Jun-ichi Yamada' 'Masashi Aimatsu' 'Hiroki Akutsu' 'Toshiaki Enoki' 'Kazuya Fujimoto' 'Koichi Kikuchi' ; S.Kudo ; 'Akira Miyazaki' 'Shinichi Nakatsuji' #============================================================================== data__BDATTP/I3________________ _database_code_depnum_ccdc_archive 'CCDC 289991' #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows v1.06 (MSC, 1997-99)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v1.06 (MSC, 1997-99)' _computing_publication_material 'teXsan for Windows v1.06 (MSC, 1997-99)' #------------------------------------------------------------------------------ _cell_length_a 9.2460(9) _cell_length_b 16.792(2) _cell_length_c 6.4950(7) _cell_angle_alpha 95.263(9) _cell_angle_beta 106.576(8) _cell_angle_gamma 95.766(9) _cell_volume 953.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1206.13 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 I3 S16 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 583.00 _exptl_absorpt_coefficient_mu 3.354 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North,Phillips & Matthews, 1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.562 _exptl_special_details ; The scan width was (1.57+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _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 AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.78 _diffrn_reflns_number 4780 _reflns_number_total 4393 _reflns_number_gt 3231 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01160 _diffrn_reflns_av_sigmaI/netI 0.042 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.54 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.543 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00924 _diffrn_orient_matrix_UB_12 0.04897 _diffrn_orient_matrix_UB_13 -0.07715 _diffrn_orient_matrix_UB_21 0.09832 _diffrn_orient_matrix_UB_22 0.02696 _diffrn_orient_matrix_UB_23 0.10432 _diffrn_orient_matrix_UB_31 0.05665 _diffrn_orient_matrix_UB_32 -0.02270 _diffrn_orient_matrix_UB_33 -0.09689 #------------------------------------------------------------------------------ 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 C 0 24 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 24 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 16 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; I 0 3 -0.726 1.812 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom I(1) 0.0000 0.0000 0.0000 0.0482(1) 1.000 2 S Uani d ? I(2) -0.25668(3) -0.00507(2) 0.17728(5) 0.06120(9) 1.000 1 . Uani d ? S(1) 0.6431(1) 0.27904(5) 0.8163(1) 0.0404(2) 1.000 1 . Uani d ? S(2) 0.5157(1) 0.22617(6) 0.3294(1) 0.0478(3) 1.000 1 . Uani d ? S(3) 0.45151(9) 0.42340(5) 0.7685(1) 0.0318(2) 1.000 1 . Uani d ? S(4) 0.34288(9) 0.37929(5) 0.2878(1) 0.0330(2) 1.000 1 . Uani d ? S(5) 0.25149(9) 0.55892(5) 0.7263(1) 0.0333(2) 1.000 1 . Uani d ? S(6) 0.14280(9) 0.51446(5) 0.2481(1) 0.0345(2) 1.000 1 . Uani d ? S(7) 0.0447(1) 0.69485(6) 0.6923(1) 0.0457(3) 1.000 1 . Uani d ? S(8) -0.0655(1) 0.65054(5) 0.1988(1) 0.0436(2) 1.000 1 . Uani d ? C(1) 0.5891(4) 0.1729(2) 0.8263(5) 0.046(1) 1.000 1 . Uani d ? C(2) 0.5947(4) 0.1178(2) 0.6313(6) 0.049(1) 1.000 1 . Uani d ? C(3) 0.4795(4) 0.1296(2) 0.4226(6) 0.050(1) 1.000 1 . Uani d ? C(4) 0.5234(3) 0.2909(2) 0.5615(4) 0.0324(8) 1.000 1 . Uani d ? C(5) 0.4494(3) 0.3557(2) 0.5427(4) 0.0275(7) 1.000 1 . Uani d ? C(6) 0.3213(3) 0.4792(2) 0.6164(4) 0.0273(7) 1.000 1 . Uani d ? C(7) 0.2715(3) 0.4587(2) 0.3989(4) 0.0278(7) 1.000 1 . Uani d ? C(8) 0.1402(3) 0.5796(2) 0.4736(4) 0.0281(7) 1.000 1 . Uani d ? C(9) 0.0531(3) 0.6409(2) 0.4542(4) 0.0305(8) 1.000 1 . Uani d ? C(10) 0.0172(7) 0.7915(3) 0.6126(7) 0.084(2) 1.000 1 . Uani d ? C(11) -0.0865(6) 0.7993(3) 0.4046(8) 0.088(2) 1.000 1 . Uani d ? C(12) -0.0672(5) 0.7574(3) 0.2071(7) 0.068(1) 1.000 1 . Uani d ? H(1) 0.6676 0.1608 0.9750 0.051 1.000 1 . Uiso c ? H(2) 0.4878 0.1642 0.8582 0.051 1.000 1 . Uiso c ? H(3) 0.5789 0.0634 0.6579 0.051 1.000 1 . Uiso c ? H(4) 0.6938 0.1286 0.6137 0.051 1.000 1 . Uiso c ? H(5) 0.4775 0.0871 0.3131 0.051 1.000 1 . Uiso c ? H(6) 0.3804 0.1252 0.4454 0.051 1.000 1 . Uiso c ? H(7) -0.0093 0.8222 0.7219 0.051 1.000 1 . Uiso c ? H(8) 0.1172 0.8166 0.6096 0.051 1.000 1 . Uiso c ? H(9) -0.1874 0.7776 0.4096 0.051 1.000 1 . Uiso c ? H(10) -0.0883 0.8547 0.3880 0.051 1.000 1 . Uiso c ? H(11) 0.0286 0.7808 0.1957 0.051 1.000 1 . Uiso c ? H(12) -0.1460 0.7672 0.0856 0.051 1.000 1 . Uiso c ? 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 I(1) 0.0542(2) 0.0365(2) 0.0562(2) 0.0096(2) 0.0197(2) 0.0030(2) I(2) 0.0629(2) 0.0514(2) 0.0823(2) 0.0139(1) 0.0379(2) 0.0151(1) S(1) 0.0518(5) 0.0312(5) 0.0319(4) 0.0109(4) 0.0008(4) 0.0032(3) S(2) 0.0718(6) 0.0432(5) 0.0301(4) 0.0212(5) 0.0145(4) 0.0009(4) S(3) 0.0385(4) 0.0318(4) 0.0218(3) 0.0105(3) 0.0021(3) 0.0024(3) S(4) 0.0404(4) 0.0347(4) 0.0217(3) 0.0108(3) 0.0047(3) 0.0005(3) S(5) 0.0405(4) 0.0356(4) 0.0213(3) 0.0138(3) 0.0029(3) 0.0012(3) S(6) 0.0403(4) 0.0396(5) 0.0206(3) 0.0138(3) 0.0017(3) 0.0029(3) S(7) 0.0534(5) 0.0465(6) 0.0369(4) 0.0164(4) 0.0113(4) 0.0003(4) S(8) 0.0480(5) 0.0411(5) 0.0344(4) 0.0139(4) -0.0031(4) 0.0082(4) C(1) 0.075(3) 0.029(2) 0.040(2) 0.009(2) 0.024(2) 0.008(1) C(2) 0.073(3) 0.026(2) 0.051(2) 0.011(2) 0.022(2) 0.004(2) C(3) 0.065(2) 0.032(2) 0.051(2) 0.007(2) 0.018(2) -0.011(2) C(4) 0.042(2) 0.027(2) 0.026(1) 0.006(1) 0.007(1) 0.001(1) C(5) 0.031(2) 0.028(2) 0.022(1) 0.002(1) 0.007(1) 0.001(1) C(6) 0.030(1) 0.025(2) 0.025(1) 0.005(1) 0.006(1) 0.005(1) C(7) 0.031(2) 0.026(2) 0.025(1) 0.005(1) 0.005(1) 0.003(1) C(8) 0.031(2) 0.029(2) 0.021(1) 0.005(1) 0.004(1) 0.003(1) C(9) 0.032(2) 0.030(2) 0.027(1) 0.006(1) 0.005(1) 0.004(1) C(10) 0.157(5) 0.037(2) 0.065(3) 0.028(3) 0.039(3) 0.006(2) C(11) 0.126(4) 0.053(3) 0.091(4) 0.050(3) 0.025(3) 0.017(3) C(12) 0.091(3) 0.044(2) 0.058(2) 0.019(2) 0.000(2) 0.017(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000136(6) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3231 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_all 0.0670 _refine_ls_wR_factor_ref 0.034 _refine_ls_goodness_of_fit_all 1.913 _refine_ls_goodness_of_fit_ref 1.910 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.26 _refine_diff_density_max 1.59 #============================================================================== # MOLECULAR GEOMETRY _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 I1 I2 2.9160(4) . . ? I1 I2 2.9160(4) . . ? S1 C1 1.816(5) . . ? S1 C4 1.748(4) . . ? S2 C3 1.820(5) . . ? S2 C4 1.757(4) . . ? S3 C5 1.767(4) . . ? S3 C6 1.737(4) . . ? S4 C5 1.771(4) . . ? S4 C7 1.735(4) . . ? S5 C6 1.727(4) . . ? S5 C8 1.756(4) . . ? S6 C7 1.726(4) . . ? S6 C8 1.753(4) . . ? S7 C9 1.744(4) . . ? S7 C10 1.769(6) . . ? S8 C9 1.741(4) . . ? S8 C12 1.794(6) . . ? C1 C2 1.524(6) . . ? C1 H1 1.08 . . no C1 H2 1.01 . . no C2 C3 1.518(7) . . ? C2 H3 0.94 . . no C2 H4 0.95 . . no C3 H5 0.95 . . no C3 H6 0.96 . . no C4 C5 1.339(6) . . ? C6 C7 1.353(5) . . ? C8 C9 1.363(5) . . ? C10 C11 1.450(9) . . ? C10 H7 0.94 . . no C10 H8 0.97 . . no C11 C12 1.477(9) . . ? C11 H9 0.97 . . no C11 H10 0.95 . . no C12 H11 0.96 . . no C12 H12 0.94 . . no #------------------------------------------------------------------------------ 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 I2 I1 I2 180.00 . . . ? C1 S1 C4 100.8(2) . . . ? C3 S2 C4 99.7(2) . . . ? C5 S3 C6 94.0(2) . . . ? C5 S4 C7 93.9(2) . . . ? C6 S5 C8 93.9(2) . . . ? C7 S6 C8 94.0(2) . . . ? C9 S7 C10 102.0(3) . . . ? C9 S8 C12 103.1(2) . . . ? S1 C1 C2 113.9(3) . . . ? S1 C1 H1 103.9 . . . no S1 C1 H2 110.6 . . . no C2 C1 H1 112.0 . . . no C2 C1 H2 113.0 . . . no H1 C1 H2 102.4 . . . no C1 C2 C3 113.4(4) . . . ? C1 C2 H3 108.7 . . . no C1 C2 H4 108.1 . . . no C3 C2 H3 109.1 . . . no C3 C2 H4 107.7 . . . no H3 C2 H4 109.7 . . . no S2 C3 C2 113.7(4) . . . ? S2 C3 H5 109.1 . . . no S2 C3 H6 108.7 . . . no C2 C3 H5 108.6 . . . no C2 C3 H6 108.1 . . . no H5 C3 H6 108.5 . . . no S1 C4 S2 121.2(2) . . . ? S1 C4 C5 118.5(3) . . . ? S2 C4 C5 119.9(3) . . . ? S3 C5 S4 115.5(2) . . . ? S3 C5 C4 122.5(3) . . . ? S4 C5 C4 122.0(3) . . . ? S3 C6 S5 123.9(2) . . . ? S3 C6 C7 118.1(3) . . . ? S5 C6 C7 118.0(3) . . . ? S4 C7 S6 123.8(2) . . . ? S4 C7 C6 118.2(3) . . . ? S6 C7 C6 118.0(3) . . . ? S5 C8 S6 116.0(2) . . . ? S5 C8 C9 122.1(3) . . . ? S6 C8 C9 121.9(3) . . . ? S7 C9 S8 123.4(2) . . . ? S7 C9 C8 117.6(3) . . . ? S8 C9 C8 118.2(3) . . . ? S7 C10 C11 119.8(5) . . . ? S7 C10 H7 108.0 . . . no S7 C10 H8 106.3 . . . no C11 C10 H7 108.6 . . . no C11 C10 H8 105.6 . . . no H7 C10 H8 107.9 . . . no C10 C11 C12 119.1(6) . . . ? C10 C11 H9 106.3 . . . no C10 C11 H10 109.1 . . . no C12 C11 H9 106.1 . . . no C12 C11 H10 107.8 . . . no H9 C11 H10 107.9 . . . no S8 C12 C11 115.8(5) . . . ? S8 C12 H11 107.8 . . . no S8 C12 H12 108.4 . . . no C11 C12 H11 106.6 . . . no C11 C12 H12 108.8 . . . no H11 C12 H12 109.3 . . . 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 S1 S7 3.598(2) . 2_667 no S1 S5 3.676(2) . 2_667 no S2 C1 3.570(5) . 1_554 no S3 C7 3.552(4) . 2_666 no S3 S5 3.593(1) . 2_667 no S3 S3 3.611(2) . 2_667 no S4 S8 3.411(2) . 2_565 no S4 C6 3.579(4) . 2_666 no S6 S6 3.492(2) . 2_565 no S6 S8 3.682(2) . 2_565 no S7 C7 3.573(4) . 2_566 no S8 C6 3.584(4) . 2_566 no C4 C8 3.685(6) . 2_666 no C7 C9 3.691(6) . 2_566 no C8 C8 3.642(8) . 2_566 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================