Supplementary Material (ESI) for J. Mater. Chem. This journal is (C) The Royal Society of Chemistry data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name _publ_author_address 'Akira Ota' ; Division of Chemistry, Graduate School of Science, Kyoto University ; 'Hideki Yamochi' ; Division of Chemistry, Graduate School of Science, Kyoto University ; 'Gunzi Saito' ; Division of Chemistry, Graduate School of Science, Kyoto University ; _publ_contact_author_name 'Dr Hideki Yamochi' _publ_contact_author_address ; Dr Hideki Yamochi Division of Chemistry, Graduate School of Science Kyoto University Sakyo-ku Kyoto 606-8502 JAPAN ; _publ_contact_author_email 'YAMOCHI@KUCHEM.KYOTO-U.AC.JP' data_edopf6(04rt2) _database_code_CSD 157198 _publ_section_title ; Crystal and molecular structure of EDO-TTF PF6 at room temperature ; _refine_special_details ; Two positions are assigned to each of the ethylene carbon atom in EDO-TTF and fluorine atom in PF6 to express the disorder. ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _chemical_formula_moiety 'S8 O4 C16 P1 F6 H12 ' _chemical_formula_weight 669.76 _cell_length_a 7.1970(9) _cell_length_b 7.3430(6) _cell_length_c 11.948(1) _cell_angle_alpha 93.454(7) _cell_angle_beta 75.158(6) _cell_angle_gamma 97.405(7) _cell_volume 605.0(1) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.838 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.875 _cell_measurement_temperature 'room temperature' _diffrn_measurement_device 'Mac Science DIP-2020K' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 2281 _reflns_number_total 2218 _reflns_number_gt 1986 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_theta_max 25.41 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+0.4592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1986 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_extinction_method 'None' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 -0.12977 _diffrn_orient_matrix_UB_12 -0.02622 _diffrn_orient_matrix_UB_13 -0.00656 _diffrn_orient_matrix_UB_21 0.01700 _diffrn_orient_matrix_UB_22 -0.12125 _diffrn_orient_matrix_UB_23 0.04140 _diffrn_orient_matrix_UB_31 -0.06192 _diffrn_orient_matrix_UB_32 0.05933 _diffrn_orient_matrix_UB_33 0.07598 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL 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 S3 S 0.38869(11) 0.31205(12) 0.67984(7) 0.0441(3) Uani 1 d . . . S4 S 0.21736(12) 0.15751(12) 0.46308(9) 0.0493(3) Uani 1 d . . . S5 S 0.78266(11) 0.34290(12) 0.52330(7) 0.0414(3) Uani 1 d . . . S6 S 0.61043(14) 0.18828(13) 0.31157(8) 0.0511(3) Uani 1 d . . . O11 O 0.5442(4) 0.4084(4) 0.8564(2) 0.0593(7) Uani 1 d . . . O12 O 0.9282(3) 0.4323(4) 0.7036(2) 0.0568(7) Uani 1 d . . . C1 C 0.5348(4) 0.2855(4) 0.5410(3) 0.0358(7) Uani 1 d . . . C2 C 0.4630(4) 0.2191(4) 0.4495(3) 0.0381(7) Uani 1 d . . . C7 C 0.5830(5) 0.3753(5) 0.7403(3) 0.0424(7) Uani 1 d . . . C8 C 0.2425(7) 0.0914(6) 0.3195(4) 0.0630(11) Uani 1 d . . . H8 H 0.1276 0.0445 0.2891 0.076 Uiso 1 calc . . . C9 C 0.7619(5) 0.3859(5) 0.6697(3) 0.0415(7) Uani 1 d . . . C10 C 0.4220(7) 0.1053(6) 0.2504(4) 0.0645(11) Uani 1 d . . . H10 H 0.4463 0.0690 0.1664 0.077 Uiso 1 calc . . . C13A C 0.7274(19) 0.499(2) 0.8899(12) 0.063(5) Uiso 0.340(18) d P . . C13B C 0.7102(9) 0.3911(11) 0.8998(5) 0.058(2) Uiso 0.660(18) d P . . C14A C 0.8996(18) 0.432(2) 0.8245(11) 0.051(3) Uiso 0.340(18) d P . . C14B C 0.8884(10) 0.5036(13) 0.8221(6) 0.056(2) Uiso 0.660(18) d P . . P15 P 0.0000 0.0000 0.0000 0.0498(4) Uani 0.5000 d S . . F16A F 0.011(4) -0.2060(14) -0.0141(19) 0.205(11) Uani 0.570(17) d P . . F17A F -0.033(2) -0.024(3) 0.1296(8) 0.164(7) Uani 0.570(17) d P . . F18A F 0.2161(9) 0.0342(19) -0.0041(11) 0.131(5) Uani 0.570(17) d P . . F16B F 0.070(3) 0.0180(19) 0.1131(14) 0.133(8) Uani 0.430(17) d P . . F17B F -0.119(4) -0.173(3) 0.0469(18) 0.214(14) Uani 0.430(17) d P . . F18B F 0.150(3) -0.124(3) -0.0575(10) 0.169(13) Uani 0.430(17) d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S3 0.0261(4) 0.0532(5) 0.0488(5) 0.0015(4) -0.0004(3) 0.0070(3) S4 0.0345(5) 0.0485(5) 0.0676(6) 0.0018(4) -0.0185(4) 0.0035(3) S5 0.0251(4) 0.0542(5) 0.0421(5) 0.0026(4) -0.0029(3) 0.0054(3) S6 0.0509(6) 0.0512(6) 0.0479(5) -0.0021(4) -0.0053(4) 0.0095(4) O11 0.0497(15) 0.083(2) 0.0412(13) -0.0053(12) -0.0032(11) 0.0122(13) O12 0.0339(13) 0.0858(19) 0.0513(14) -0.0027(13) -0.0141(10) 0.0044(12) C1 0.0250(14) 0.0361(16) 0.0450(16) 0.0056(13) -0.0041(12) 0.0067(11) C2 0.0306(15) 0.0345(16) 0.0499(17) 0.0026(13) -0.0092(13) 0.0073(11) C7 0.0349(17) 0.0487(19) 0.0423(17) 0.0027(14) -0.0050(13) 0.0087(13) C8 0.065(3) 0.055(2) 0.078(3) 0.004(2) -0.038(2) -0.0028(18) C9 0.0333(16) 0.0483(19) 0.0435(17) 0.0027(14) -0.0100(13) 0.0060(13) C10 0.089(3) 0.054(2) 0.056(2) -0.0042(18) -0.032(2) 0.003(2) P15 0.0563(8) 0.0582(9) 0.0389(6) -0.0030(6) -0.0202(6) 0.0070(6) F16A 0.40(3) 0.056(5) 0.262(19) -0.047(8) -0.27(2) 0.061(10) F17A 0.158(11) 0.305(17) 0.036(4) 0.020(6) -0.019(5) 0.060(10) F18A 0.051(4) 0.189(11) 0.161(10) 0.040(9) -0.043(5) -0.006(4) F16B 0.23(2) 0.111(8) 0.119(14) -0.039(8) -0.142(16) 0.049(9) F17B 0.27(3) 0.145(16) 0.177(17) 0.077(13) -0.033(14) -0.125(16) F18B 0.22(2) 0.22(2) 0.080(6) -0.021(9) 0.004(9) 0.17(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S3 C7 1.733(4) . ? S3 C1 1.736(3) . ? S4 C8 1.725(5) . ? S4 C2 1.735(3) . ? S5 C9 1.730(3) . ? S5 C1 1.740(3) . ? S6 C10 1.728(5) . ? S6 C2 1.736(3) . ? O11 C7 1.357(4) . ? O11 C13B 1.441(7) . ? O11 C13A 1.534(14) . ? O12 C9 1.357(4) . ? O12 C14A 1.406(13) . ? O12 C14B 1.450(7) . ? C1 C2 1.365(5) . ? C7 C9 1.342(5) . ? C8 C10 1.338(6) . ? C13A C13B 0.799(14) . ? C13A C14B 1.230(14) . ? C13A C14A 1.41(2) . ? C13B C14A 1.434(13) . ? C13B C14B 1.549(11) . ? C14A C14B 0.543(13) . ? P15 F17B 1.490(11) 2 ? P15 F17B 1.490(11) . ? P15 F18B 1.504(9) 2 ? P15 F18B 1.504(9) . ? P15 F16A 1.522(9) 2 ? P15 F16A 1.522(9) . ? P15 F17A 1.523(9) . ? P15 F17A 1.523(9) 2 ? P15 F18A 1.532(5) . ? P15 F18A 1.532(5) 2 ? P15 F16B 1.551(10) . ? P15 F16B 1.551(10) 2 ? F16A F17B 1.08(3) . ? F16A F18B 1.12(2) . ? F17A F16B 0.75(2) . ? F17A F17B 1.60(2) . ? F18A F18B 1.38(2) . ? F18A F17B 1.49(2) 2 ? F18A F16B 1.522(19) . ? F17B F18A 1.49(2) 2 ? 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_3 _geom_angle_publ_flag C7 S3 C1 93.62(15) . . ? C8 S4 C2 95.04(19) . . ? C9 S5 C1 93.77(15) . . ? C10 S6 C2 94.8(2) . . ? C7 O11 C13B 111.1(3) . . ? C7 O11 C13A 109.9(5) . . ? C13B O11 C13A 31.0(5) . . ? C9 O12 C14A 112.8(5) . . ? C9 O12 C14B 111.0(4) . . ? C14A O12 C14B 21.8(6) . . ? C2 C1 S3 122.7(3) . . ? C2 C1 S5 120.5(3) . . ? S3 C1 S5 116.71(19) . . ? C1 C2 S4 122.3(3) . . ? C1 C2 S6 122.5(3) . . ? S4 C2 S6 115.2(2) . . ? C9 C7 O11 124.3(3) . . ? C9 C7 S3 118.0(3) . . ? O11 C7 S3 117.7(2) . . ? C10 C8 S4 117.3(3) . . ? C7 C9 O12 125.1(3) . . ? C7 C9 S5 117.7(3) . . ? O12 C9 S5 117.2(2) . . ? C8 C10 S6 117.6(3) . . ? C13B C13A C14B 97.3(16) . . ? C13B C13A C14A 75.1(15) . . ? C14B C13A C14A 22.3(6) . . ? C13B C13A O11 68.0(11) . . ? C14B C13A O11 121.9(11) . . ? C14A C13A O11 113.8(12) . . ? C13A C13B C14A 72.3(14) . . ? C13A C13B O11 81.0(11) . . ? C14A C13B O11 118.6(7) . . ? C13A C13B C14B 51.9(11) . . ? C14A C13B C14B 20.5(6) . . ? O11 C13B C14B 108.1(6) . . ? C14B C14A O12 83.6(18) . . ? C14B C14A C13A 59.3(18) . . ? O12 C14A C13A 115.5(12) . . ? C14B C14A C13B 91.8(19) . . ? O12 C14A C13B 121.3(9) . . ? C13A C14A C13B 32.6(6) . . ? C14A C14B C13A 98(2) . . ? C14A C14B O12 74.5(17) . . ? C13A C14B O12 125.5(9) . . ? C14A C14B C13B 67.7(17) . . ? C13A C14B C13B 30.8(8) . . ? O12 C14B C13B 111.2(6) . . ? F17B P15 F17B 180.000(1) 2 . ? F17B P15 F18B 84.8(12) 2 2 ? F17B P15 F18B 95.2(12) . 2 ? F17B P15 F18B 95.2(12) 2 . ? F17B P15 F18B 84.8(12) . . ? F18B P15 F18B 180.000(1) 2 . ? F17B P15 F16A 41.8(10) 2 2 ? F17B P15 F16A 138.2(10) . 2 ? F18B P15 F16A 43.4(8) 2 2 ? F18B P15 F16A 136.6(8) . 2 ? F17B P15 F16A 138.2(10) 2 . ? F17B P15 F16A 41.8(10) . . ? F18B P15 F16A 136.6(8) 2 . ? F18B P15 F16A 43.4(8) . . ? F16A P15 F16A 180.000(1) 2 . ? F17B P15 F17A 115.7(9) 2 . ? F17B P15 F17A 64.3(9) . . ? F18B P15 F17A 74.2(7) 2 . ? F18B P15 F17A 105.8(7) . . ? F16A P15 F17A 92.9(10) 2 . ? F16A P15 F17A 87.1(10) . . ? F17B P15 F17A 64.3(9) 2 2 ? F17B P15 F17A 115.7(9) . 2 ? F18B P15 F17A 105.8(7) 2 2 ? F18B P15 F17A 74.2(7) . 2 ? F16A P15 F17A 87.1(10) 2 2 ? F16A P15 F17A 92.9(10) . 2 ? F17A P15 F17A 180.0 . 2 ? F17B P15 F18A 58.9(10) 2 . ? F17B P15 F18A 121.1(10) . . ? F18B P15 F18A 125.9(9) 2 . ? F18B P15 F18A 54.1(9) . . ? F16A P15 F18A 89.5(7) 2 . ? F16A P15 F18A 90.5(7) . . ? F17A P15 F18A 86.4(5) . . ? F17A P15 F18A 93.6(5) 2 . ? F17B P15 F18A 121.1(10) 2 2 ? F17B P15 F18A 58.9(10) . 2 ? F18B P15 F18A 54.1(9) 2 2 ? F18B P15 F18A 125.9(9) . 2 ? F16A P15 F18A 90.5(7) 2 2 ? F16A P15 F18A 89.5(7) . 2 ? F17A P15 F18A 93.6(5) . 2 ? F17A P15 F18A 86.4(5) 2 2 ? F18A P15 F18A 180.0 . 2 ? F17B P15 F16B 93.2(10) 2 . ? F17B P15 F16B 86.8(10) . . ? F18B P15 F16B 87.5(9) 2 . ? F18B P15 F16B 92.5(9) . . ? F16A P15 F16B 86.0(6) 2 . ? F16A P15 F16B 94.0(6) . . ? F17A P15 F16B 28.1(8) . . ? F17A P15 F16B 151.9(8) 2 . ? F18A P15 F16B 59.2(7) . . ? F18A P15 F16B 120.8(7) 2 . ? F17B P15 F16B 86.8(10) 2 2 ? F17B P15 F16B 93.2(10) . 2 ? F18B P15 F16B 92.5(9) 2 2 ? F18B P15 F16B 87.5(9) . 2 ? F16A P15 F16B 94.0(6) 2 2 ? F16A P15 F16B 86.0(6) . 2 ? F17A P15 F16B 151.9(8) . 2 ? F17A P15 F16B 28.1(8) 2 2 ? F18A P15 F16B 120.8(7) . 2 ? F18A P15 F16B 59.2(7) 2 2 ? F16B P15 F16B 180.0 . 2 ? F17B F16A F18B 134.0(15) . . ? F17B F16A P15 67.5(9) . . ? F18B F16A P15 67.5(7) . . ? F16B F17A P15 78.0(15) . . ? F16B F17A F17B 121(2) . . ? P15 F17A F17B 56.9(6) . . ? F18B F18A F17B 100.8(11) . 2 ? F18B F18A F16B 98.9(8) . . ? F17B F18A F16B 94.5(10) 2 . ? F18B F18A P15 61.9(6) . . ? F17B F18A P15 59.1(6) 2 . ? F16B F18A P15 61.0(5) . . ? F17A F16B F18A 131.3(17) . . ? F17A F16B P15 73.8(13) . . ? F18A F16B P15 59.8(6) . . ? F16A F17B F18A 113.1(16) . 2 ? F16A F17B P15 70.7(9) . . ? F18A F17B P15 62.0(7) 2 . ? F16A F17B F17A 101.3(17) . . ? F18A F17B F17A 92.2(13) 2 . ? P15 F17B F17A 58.9(7) . . ? F16A F18B F18A 120.0(13) . . ? F16A F18B P15 69.1(8) . . ? F18A F18B P15 64.0(6) . . ? _diffrn_measured_fraction_theta_max 0.809 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.551 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.165 #=================================================== #===END data_edopf6(04LT7) _database_code_CSD 157199 _publ_section_title ; Crystal and molecular structure of edopf6 at 260 K ; _refine_special_details ; Two positions are assigned to each of the ethylene carbon atom in EDO-TTF to express the disorder. Four among the crystallographically independent six fluorine atoms are also treated to occupy each two sites. ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _chemical_formula_moiety 'C16 H12 O4 S8 P1 F6 ' _chemical_formula_weight 669.76 _cell_length_a 9.822(1) _cell_length_b 11.000(2) _cell_length_c 11.487(2) _cell_angle_alpha 101.865(8) _cell_angle_beta 99.128(8) _cell_angle_gamma 90.445(8) _cell_volume 1198.1(3) _cell_formula_units_Z 2 _exptl_crystal_density_meas 1.838 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.884 _cell_measurement_temperature '260' _diffrn_measurement_device 'Mac Science DIP-2020K' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 4169 _reflns_number_total 3950 _reflns_number_gt 3283 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_theta_max 25.33 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+1.4790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3283 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_extinction_method 'None' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.07646 _diffrn_orient_matrix_UB_12 0.04373 _diffrn_orient_matrix_UB_13 0.06401 _diffrn_orient_matrix_UB_21 -0.06939 _diffrn_orient_matrix_UB_22 0.05141 _diffrn_orient_matrix_UB_23 0.04149 _diffrn_orient_matrix_UB_31 -0.00976 _diffrn_orient_matrix_UB_32 -0.06460 _diffrn_orient_matrix_UB_33 0.04913 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL 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 C1 C 0.3701(3) 0.1224(3) 0.5250(3) 0.0324(7) Uani 1 d . . . C2 C 0.4442(3) 0.1348(3) 0.4353(3) 0.0318(7) Uani 1 d . . . C7 C 0.1931(4) 0.0581(3) 0.6410(3) 0.0356(8) Uani 1 d . . . C8 C 0.5304(5) 0.1250(4) 0.2372(4) 0.0510(10) Uani 1 d . . . H8 H 0.5401 0.1056 0.1501 0.061 Uiso 1 calc . . . C9 C 0.2844(4) 0.1356(3) 0.7231(3) 0.0366(8) Uani 1 d . . . C10 C 0.6210(4) 0.2015(4) 0.3186(4) 0.0515(10) Uani 1 d . . . H10 H 0.7011 0.2420 0.2952 0.062 Uiso 1 calc . . . C13A C 0.0861(10) 0.0143(11) 0.7969(8) 0.048(3) Uiso 0.503(18) d P . . C13B C 0.0500(11) 0.0605(11) 0.7822(8) 0.048(3) Uiso 0.497(18) d P . . C14A C 0.1392(11) 0.1338(11) 0.8643(8) 0.052(3) Uiso 0.503(18) d P . . C14B C 0.1846(11) 0.0853(10) 0.8785(8) 0.047(3) Uiso 0.497(18) d P . . C21 C 0.1744(3) 0.3674(3) 0.4573(3) 0.0323(7) Uani 1 d . . . C22 C 0.1095(3) 0.3703(3) 0.5526(3) 0.0350(8) Uani 1 d . . . C27 C 0.3286(4) 0.4284(3) 0.3179(3) 0.0373(8) Uani 1 d . . . C28 C 0.0285(5) 0.4339(4) 0.7570(4) 0.0533(10) Uani 1 d . . . H28 H 0.0195 0.4762 0.8410 0.064 Uiso 1 calc . . . C29 C 0.2358(4) 0.3459(3) 0.2469(3) 0.0375(8) Uani 1 d . . . C30 C -0.0678(4) 0.3544(4) 0.6905(4) 0.0520(10) Uani 1 d . . . H30 H -0.1522 0.3344 0.7226 0.062 Uiso 1 calc . . . C33 C 0.4335(5) 0.4414(5) 0.1551(4) 0.0631(12) Uani 1 d . . . H33A H 0.4914 0.3667 0.1493 0.076 Uiso 1 calc . . . H33B H 0.4794 0.5047 0.1213 0.076 Uiso 1 calc . . . C34 C 0.2969(6) 0.4059(5) 0.0822(4) 0.0711(14) Uani 1 d . . . H34A H 0.2404 0.4814 0.0844 0.085 Uiso 1 calc . . . H34B H 0.3078 0.3727 -0.0035 0.085 Uiso 1 calc . . . O11 O 0.0807(3) 0.0032(3) 0.6655(2) 0.0460(6) Uani 1 d . . . O12 O 0.2779(3) 0.1677(3) 0.8423(2) 0.0503(7) Uani 1 d . . . O31 O 0.4272(3) 0.4919(3) 0.2804(2) 0.0520(7) Uani 1 d . . . O32 O 0.2250(3) 0.3136(3) 0.1245(2) 0.0565(8) Uani 1 d . . . S3 S 0.22011(9) 0.03023(8) 0.49309(8) 0.0369(2) Uani 1 d . . . S4 S 0.39555(10) 0.06025(9) 0.28732(8) 0.0431(2) Uani 1 d . . . S5 S 0.42200(9) 0.19655(9) 0.67324(8) 0.0382(2) Uani 1 d . . . S6 S 0.59390(9) 0.22733(9) 0.46528(9) 0.0412(2) Uani 1 d . . . S23 S 0.32746(9) 0.45791(8) 0.47311(8) 0.0374(2) Uani 1 d . . . S24 S 0.17197(11) 0.46325(10) 0.69457(9) 0.0477(3) Uani 1 d . . . S25 S 0.11544(9) 0.27686(9) 0.31320(8) 0.0399(2) Uani 1 d . . . S26 S -0.04447(9) 0.28492(9) 0.54497(9) 0.0438(2) Uani 1 d . . . P40 P 0.76003(11) 0.22885(10) -0.02141(9) 0.0442(3) Uani 1 d . . . F41 F 0.6450(4) 0.1232(4) -0.0342(3) 0.1080(13) Uani 1 d . . . F42 F 0.8754(4) 0.3321(3) -0.0120(3) 0.0950(10) Uani 1 d . . . F43A F 0.7593(13) 0.1935(12) -0.1659(7) 0.087(3) Uani 0.66(2) d P . . F44A F 0.7565(14) 0.2546(14) 0.1140(9) 0.095(4) Uani 0.66(2) d P . . F45A F 0.8854(11) 0.1386(11) -0.0062(12) 0.094(3) Uani 0.66(2) d P . . F46A F 0.6340(8) 0.3123(11) -0.0455(15) 0.104(4) Uani 0.66(2) d P . . F43B F 0.716(2) 0.251(3) -0.1466(16) 0.088(7) Uani 0.34(2) d P . . F44B F 0.807(3) 0.223(3) 0.120(2) 0.097(8) Uani 0.34(2) d P . . F45B F 0.830(3) 0.1143(16) -0.061(2) 0.110(6) Uani 0.34(2) d P . . F46B F 0.691(3) 0.3560(13) 0.033(2) 0.096(7) Uani 0.34(2) d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0276(16) 0.0269(18) 0.0411(18) 0.0072(15) 0.0006(14) -0.0013(14) C2 0.0296(16) 0.0239(18) 0.0420(18) 0.0082(14) 0.0045(14) -0.0011(14) C7 0.0330(17) 0.0332(19) 0.0411(18) 0.0075(15) 0.0079(15) -0.0009(15) C8 0.057(2) 0.054(3) 0.049(2) 0.016(2) 0.020(2) 0.018(2) C9 0.0349(18) 0.033(2) 0.0408(18) 0.0053(15) 0.0055(15) -0.0031(16) C10 0.050(2) 0.053(3) 0.061(3) 0.022(2) 0.024(2) 0.005(2) C21 0.0290(16) 0.0264(18) 0.0412(18) 0.0071(14) 0.0049(14) -0.0017(14) C22 0.0299(16) 0.0288(19) 0.0465(19) 0.0078(15) 0.0071(15) 0.0000(15) C27 0.0392(19) 0.034(2) 0.0403(18) 0.0091(16) 0.0101(16) -0.0027(16) C28 0.059(3) 0.058(3) 0.048(2) 0.011(2) 0.023(2) 0.009(2) C29 0.043(2) 0.0322(19) 0.0368(17) 0.0065(15) 0.0072(16) -0.0016(16) C30 0.047(2) 0.060(3) 0.058(2) 0.022(2) 0.024(2) 0.007(2) C33 0.070(3) 0.072(3) 0.056(3) 0.021(2) 0.025(2) -0.007(3) C34 0.107(4) 0.063(3) 0.047(2) 0.016(2) 0.022(3) -0.012(3) O11 0.0379(13) 0.0468(16) 0.0516(15) 0.0046(12) 0.0106(12) -0.0154(12) O12 0.0495(16) 0.0563(18) 0.0411(14) 0.0003(13) 0.0093(12) -0.0140(14) O31 0.0559(17) 0.0536(18) 0.0490(15) 0.0123(13) 0.0150(13) -0.0169(14) O32 0.079(2) 0.0514(18) 0.0348(13) 0.0022(12) 0.0068(13) -0.0161(16) S3 0.0313(4) 0.0358(5) 0.0397(5) 0.0049(4) -0.0008(4) -0.0091(4) S4 0.0430(5) 0.0419(6) 0.0413(5) 0.0043(4) 0.0033(4) 0.0035(4) S5 0.0339(4) 0.0347(5) 0.0416(5) 0.0019(4) 0.0019(4) -0.0109(4) S6 0.0371(5) 0.0333(5) 0.0541(5) 0.0088(4) 0.0106(4) -0.0064(4) S23 0.0340(4) 0.0352(5) 0.0407(5) 0.0027(4) 0.0064(4) -0.0089(4) S24 0.0491(6) 0.0443(6) 0.0456(5) -0.0021(4) 0.0110(4) -0.0043(5) S25 0.0378(5) 0.0343(5) 0.0432(5) 0.0010(4) 0.0030(4) -0.0078(4) S26 0.0337(5) 0.0425(6) 0.0570(6) 0.0110(5) 0.0120(4) -0.0043(4) P40 0.0487(6) 0.0457(6) 0.0410(5) 0.0116(4) 0.0129(4) -0.0024(5) F41 0.113(3) 0.132(3) 0.084(2) 0.032(2) 0.0197(19) -0.069(2) F42 0.103(2) 0.089(2) 0.086(2) 0.0094(17) 0.0121(18) -0.048(2) F43A 0.112(7) 0.101(7) 0.046(3) 0.004(4) 0.026(3) -0.054(5) F44A 0.114(8) 0.132(8) 0.036(4) -0.001(4) 0.028(5) -0.005(6) F45A 0.069(5) 0.114(6) 0.131(7) 0.072(6) 0.043(5) 0.041(4) F46A 0.078(4) 0.112(6) 0.140(10) 0.062(7) 0.020(5) 0.041(4) F43B 0.105(13) 0.126(16) 0.035(7) 0.038(8) -0.010(7) -0.039(11) F44B 0.124(18) 0.108(14) 0.059(8) 0.044(9) -0.019(10) -0.038(12) F45B 0.090(12) 0.088(8) 0.139(14) -0.009(10) 0.024(11) 0.050(8) F46B 0.127(15) 0.077(8) 0.092(11) 0.017(7) 0.038(11) 0.041(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(5) . ? C1 S5 1.724(3) . ? C1 S3 1.727(3) . ? C2 S4 1.719(3) . ? C2 S6 1.729(3) . ? C7 C9 1.345(5) . ? C7 O11 1.348(4) . ? C7 S3 1.727(4) . ? C8 C10 1.333(6) . ? C8 S4 1.728(4) . ? C9 O12 1.353(4) . ? C9 S5 1.730(4) . ? C10 S6 1.714(4) . ? C13A C13B 0.657(10) . ? C13A C14B 1.351(12) . ? C13A C14A 1.429(15) . ? C13A O11 1.482(9) . ? C13B C14A 1.312(12) . ? C13B O11 1.439(9) . ? C13B C14B 1.566(16) . ? C14A C14B 0.725(10) . ? C14A O12 1.484(9) . ? C14B O12 1.449(9) . ? C21 C22 1.346(5) . ? C21 S25 1.754(3) . ? C21 S23 1.761(3) . ? C22 S24 1.752(4) . ? C22 S26 1.755(3) . ? C27 C29 1.329(5) . ? C27 O31 1.363(4) . ? C27 S23 1.747(4) . ? C28 C30 1.314(6) . ? C28 S24 1.735(4) . ? C29 O32 1.364(4) . ? C29 S25 1.750(4) . ? C30 S26 1.741(4) . ? C33 O31 1.444(5) . ? C33 C34 1.468(7) . ? C34 O32 1.438(5) . ? P40 F45B 1.466(15) . ? P40 F43B 1.503(14) . ? P40 F44A 1.528(10) . ? P40 F46A 1.571(5) . ? P40 F42 1.574(3) . ? P40 F41 1.583(3) . ? P40 F45A 1.599(8) . ? P40 F46B 1.608(11) . ? P40 F43A 1.624(8) . ? P40 F44B 1.63(2) . ? F43A F43B 0.77(2) . ? F43A F45B 1.69(2) . ? F44A F44B 0.61(3) . ? F44A F46B 1.666(18) . ? F45A F45B 0.765(19) . ? F46A F46B 1.006(16) . ? F46A F43B 1.56(2) . ? 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_3 _geom_angle_publ_flag C2 C1 S5 122.1(3) . . ? C2 C1 S3 121.0(3) . . ? S5 C1 S3 116.88(19) . . ? C1 C2 S4 122.9(3) . . ? C1 C2 S6 121.7(3) . . ? S4 C2 S6 115.39(19) . . ? C9 C7 O11 124.8(3) . . ? C9 C7 S3 117.3(3) . . ? O11 C7 S3 117.9(3) . . ? C10 C8 S4 117.8(3) . . ? C7 C9 O12 124.8(3) . . ? C7 C9 S5 117.7(3) . . ? O12 C9 S5 117.5(3) . . ? C8 C10 S6 116.9(3) . . ? C13B C13A C14B 96.3(16) . . ? C13B C13A C14A 66.3(14) . . ? C14B C13A C14A 30.1(5) . . ? C13B C13A O11 73.4(12) . . ? C14B C13A O11 121.8(7) . . ? C14A C13A O11 112.1(8) . . ? C13A C13B C14A 86.3(16) . . ? C13A C13B O11 80.6(13) . . ? C14A C13B O11 122.7(8) . . ? C13A C13B C14B 59.0(13) . . ? C14A C13B C14B 27.4(5) . . ? O11 C13B C14B 110.9(8) . . ? C14B C14A C13B 96.3(15) . . ? C14B C14A C13A 69.0(13) . . ? C13B C14A C13A 27.3(5) . . ? C14B C14A O12 73.0(11) . . ? C13B C14A O12 122.5(8) . . ? C13A C14A O12 113.7(9) . . ? C14A C14B C13A 80.9(14) . . ? C14A C14B O12 78.4(11) . . ? C13A C14B O12 121.1(8) . . ? C14A C14B C13B 56.3(12) . . ? C13A C14B C13B 24.7(5) . . ? O12 C14B C13B 108.8(8) . . ? C22 C21 S25 123.8(3) . . ? C22 C21 S23 120.1(3) . . ? S25 C21 S23 116.11(19) . . ? C21 C22 S24 122.0(3) . . ? C21 C22 S26 123.3(3) . . ? S24 C22 S26 114.62(20) . . ? C29 C27 O31 125.6(3) . . ? C29 C27 S23 118.1(3) . . ? O31 C27 S23 116.3(3) . . ? C30 C28 S24 118.0(3) . . ? C27 C29 O32 124.3(3) . . ? C27 C29 S25 118.3(3) . . ? O32 C29 S25 117.3(3) . . ? C28 C30 S26 118.2(3) . . ? O31 C33 C34 112.9(4) . . ? O32 C34 C33 112.2(4) . . ? C7 O11 C13B 111.5(4) . . ? C7 O11 C13A 111.6(4) . . ? C13B O11 C13A 26.0(4) . . ? C9 O12 C14B 112.1(4) . . ? C9 O12 C14A 110.1(4) . . ? C14B O12 C14A 28.6(4) . . ? C27 O31 C33 110.1(3) . . ? C29 O32 C34 109.6(3) . . ? C7 S3 C1 94.17(16) . . ? C2 S4 C8 94.59(19) . . ? C1 S5 C9 93.97(17) . . ? C10 S6 C2 95.32(19) . . ? C27 S23 C21 93.25(16) . . ? C28 S24 C22 94.5(2) . . ? C29 S25 C21 93.29(16) . . ? C30 S26 C22 94.20(19) . . ? F45B P40 F43B 94.4(10) . . ? F45B P40 F44A 111.9(9) . . ? F43B P40 F44A 153.1(10) . . ? F45B P40 F46A 147.7(8) . . ? F43B P40 F46A 61.1(9) . . ? F44A P40 F46A 92.3(5) . . ? F45B P40 F42 102.3(9) . . ? F43B P40 F42 84.4(8) . . ? F44A P40 F42 94.8(6) . . ? F46A P40 F42 96.3(4) . . ? F45B P40 F41 76.7(9) . . ? F43B P40 F41 94.6(8) . . ? F44A P40 F41 86.7(6) . . ? F46A P40 F41 84.2(4) . . ? F42 P40 F41 178.46(19) . . ? F45B P40 F45A 28.5(8) . . ? F43B P40 F45A 115.5(10) . . ? F44A P40 F45A 91.2(5) . . ? F46A P40 F45A 176.1(4) . . ? F42 P40 F45A 85.1(4) . . ? F41 P40 F45A 94.3(5) . . ? F45B P40 F46B 175.3(8) . . ? F43B P40 F46B 89.8(9) . . ? F44A P40 F46B 64.1(7) . . ? F46A P40 F46B 36.9(6) . . ? F42 P40 F46B 76.1(8) . . ? F41 P40 F46B 105.1(9) . . ? F45A P40 F46B 147.0(8) . . ? F45B P40 F43A 66.2(9) . . ? F43B P40 F43A 28.3(9) . . ? F44A P40 F43A 176.6(6) . . ? F46A P40 F43A 88.4(5) . . ? F42 P40 F43A 88.4(4) . . ? F41 P40 F43A 90.1(4) . . ? F45A P40 F43A 88.0(4) . . ? F46B P40 F43A 117.9(6) . . ? F45B P40 F44B 91.7(11) . . ? F43B P40 F44B 173.0(12) . . ? F44A P40 F44B 22.0(11) . . ? F46A P40 F44B 114.3(9) . . ? F42 P40 F44B 91.1(9) . . ? F41 P40 F44B 90.0(9) . . ? F45A P40 F44B 69.2(10) . . ? F46B P40 F44B 84.0(10) . . ? F43A P40 F44B 157.2(9) . . ? F43B F43A P40 67.1(14) . . ? F43B F43A F45B 119.3(17) . . ? P40 F43A F45B 52.4(6) . . ? F44B F44A P40 89(3) . . ? F44B F44A F46B 140(4) . . ? P40 F44A F46B 60.3(5) . . ? F45B F45A P40 66.1(15) . . ? F46B F46A F43B 115.7(12) . . ? F46B F46A P40 73.6(8) . . ? F43B F46A P40 57.3(6) . . ? F43A F43B P40 84.6(18) . . ? F43A F43B F46A 142(2) . . ? P40 F43B F46A 61.6(7) . . ? F44A F44B P40 69(3) . . ? F45A F45B P40 85.5(18) . . ? F45A F45B F43A 127(2) . . ? P40 F45B F43A 61.4(7) . . ? F46A F46B P40 69.5(8) . . ? F46A F46B F44A 111.2(13) . . ? P40 F46B F44A 55.6(5) . . ? _diffrn_measured_fraction_theta_max 0.680 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.485 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.063 #=================================================== #===END