# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yoshiro Yamashita' _publ_contact_author_email YOSHIRO@ECHEM.TITECH.AC.JP _publ_section_title ; Anthraquinone Derivatives Affording n-Type Organic Thin Film Transistors ; loop_ _publ_author_name 'Yoshiro Yamashita' 'Masashi Mamada' 'Jun-ichi Nishida' 'Shizuo Tokito' # Attachment 'CIF.dat' #=================================================================== data_1_ _database_code_depnum_ccdc_archive 'CCDC 709632' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H14 F6 O2 ' _chemical_formula_moiety 'C28 H14 F6 O2 ' _chemical_formula_weight 496.41 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.149(6) _cell_length_b 8.160(7) _cell_length_c 31.23(2) _cell_angle_alpha 90 _cell_angle_beta 91.70(3) _cell_angle_gamma 90 _cell_volume 2075(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16976 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.993 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 20240 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9979 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4754 _reflns_number_gt 3698 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1098 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4754 _refine_ls_number_parameters 325 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.37 _refine_diff_density_min -0.17 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _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 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) ; 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) ; #------------------------------------------------------------------------------ # 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 F(1) F 0.4036(1) -0.7362(1) -0.24695(3) 0.0358(3) Uani 1.00 d . . . F(2) F 0.1561(1) -0.6659(1) -0.23524(3) 0.0297(3) Uani 1.00 d . . . F(3) F 0.2693(1) -0.8595(1) -0.19808(3) 0.0347(3) Uani 1.00 d . . . F(4) F 1.2324(1) 0.7025(1) 0.23563(3) 0.0307(3) Uani 1.00 d . . . F(5) F 1.3412(1) 0.8150(1) 0.18077(3) 0.0287(3) Uani 1.00 d . . . F(6) F 1.0905(1) 0.8643(1) 0.19489(3) 0.0292(3) Uani 1.00 d . . . O(1) O 0.6941(1) 0.3120(1) -0.02737(3) 0.0244(3) Uani 1.00 d . . . O(2) O 0.7719(1) -0.3165(1) 0.02208(3) 0.0275(3) Uani 1.00 d . . . C(1) C 0.7130(2) 0.1699(2) -0.01619(4) 0.0181(4) Uani 1.00 d . . . C(2) C 0.6437(2) 0.0326(2) -0.04241(4) 0.0179(3) Uani 1.00 d . . . C(3) C 0.5586(2) 0.0693(2) -0.08053(4) 0.0195(4) Uani 1.00 d . . . C(4) C 0.5005(2) -0.0552(2) -0.10683(4) 0.0205(4) Uani 1.00 d . . . C(5) C 0.5228(2) -0.2198(2) -0.09546(4) 0.0189(4) Uani 1.00 d . . . C(6) C 0.6018(2) -0.2571(2) -0.05634(4) 0.0183(4) Uani 1.00 d . . . C(7) C 0.6645(2) -0.1320(2) -0.03014(4) 0.0180(4) Uani 1.00 d . . . C(8) C 0.7561(2) -0.1743(2) 0.01035(4) 0.0196(4) Uani 1.00 d . . . C(9) C 0.8273(2) -0.0370(2) 0.03616(4) 0.0182(4) Uani 1.00 d . . . C(10) C 0.9161(2) -0.0729(2) 0.07389(5) 0.0205(4) Uani 1.00 d . . . C(11) C 0.9816(2) 0.0515(2) 0.09894(4) 0.0210(4) Uani 1.00 d . . . C(12) C 0.9620(2) 0.2165(2) 0.08702(4) 0.0186(4) Uani 1.00 d . . . C(13) C 0.8756(2) 0.2522(2) 0.04886(4) 0.0189(4) Uani 1.00 d . . . C(14) C 0.8078(2) 0.1269(2) 0.02365(4) 0.0178(4) Uani 1.00 d . . . C(15) C 0.4656(2) -0.3505(2) -0.12549(4) 0.0192(4) Uani 1.00 d . . . C(16) C 0.4869(2) -0.3303(2) -0.16942(5) 0.0222(4) Uani 1.00 d . . . C(17) C 0.4351(2) -0.4493(2) -0.19811(4) 0.0232(4) Uani 1.00 d . . . C(18) C 0.3576(2) -0.5890(2) -0.18352(4) 0.0210(4) Uani 1.00 d . . . C(19) C 0.3353(2) -0.6115(2) -0.13988(5) 0.0211(4) Uani 1.00 d . . . C(20) C 0.3903(2) -0.4929(2) -0.11107(4) 0.0205(4) Uani 1.00 d . . . C(21) C 0.2976(2) -0.7125(2) -0.21550(5) 0.0255(4) Uani 1.00 d . . . C(22) C 1.0301(2) 0.3496(2) 0.11475(4) 0.0190(4) Uani 1.00 d . . . C(23) C 1.0304(2) 0.3344(2) 0.15942(5) 0.0216(4) Uani 1.00 d . . . C(24) C 1.0890(2) 0.4600(2) 0.18557(4) 0.0214(4) Uani 1.00 d . . . C(25) C 1.1497(2) 0.6019(2) 0.16733(4) 0.0193(4) Uani 1.00 d . . . C(26) C 1.1537(2) 0.6168(2) 0.12293(4) 0.0203(4) Uani 1.00 d . . . C(27) C 1.0938(2) 0.4920(2) 0.09692(4) 0.0201(4) Uani 1.00 d . . . C(28) C 1.2042(2) 0.7436(2) 0.19467(5) 0.0225(4) Uani 1.00 d . . . H(1) H 0.5454 0.1847 -0.0905 0.0413 Uiso 1.00 calc . . . H(2) H 0.4509 -0.0363 -0.1350 0.0413 Uiso 1.00 calc . . . H(3) H 0.6220 -0.3754 -0.0478 0.0413 Uiso 1.00 calc . . . H(4) H 0.9417 -0.1863 0.0833 0.0413 Uiso 1.00 calc . . . H(5) H 1.0437 0.0302 0.1261 0.0413 Uiso 1.00 calc . . . H(6) H 0.8674 0.3674 0.0402 0.0413 Uiso 1.00 calc . . . H(7) H 0.5448 -0.2277 -0.1793 0.0413 Uiso 1.00 calc . . . H(8) H 0.4509 -0.4300 -0.2289 0.0413 Uiso 1.00 calc . . . H(9) H 0.2819 -0.7086 -0.1268 0.0413 Uiso 1.00 calc . . . H(10) H 0.3747 -0.5198 -0.0811 0.0413 Uiso 1.00 calc . . . H(11) H 0.9835 0.2305 0.1758 0.0413 Uiso 1.00 calc . . . H(12) H 1.0845 0.4503 0.2175 0.0413 Uiso 1.00 calc . . . H(13) H 1.2085 0.7140 0.1125 0.0413 Uiso 1.00 calc . . . H(14) H 1.0914 0.5147 0.0654 0.0413 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 F(1) 0.0309(5) 0.0436(7) 0.0332(5) 0.0018(5) 0.0048(4) -0.0183(5) F(2) 0.0265(5) 0.0303(6) 0.0318(5) 0.0035(4) -0.0069(4) -0.0063(4) F(3) 0.0471(6) 0.0187(5) 0.0379(5) -0.0014(4) -0.0080(4) -0.0037(4) F(4) 0.0423(6) 0.0279(6) 0.0215(4) -0.0053(4) -0.0049(4) 0.0006(4) F(5) 0.0262(5) 0.0269(6) 0.0330(5) -0.0066(4) 0.0024(4) -0.0025(4) F(6) 0.0303(5) 0.0219(5) 0.0355(5) 0.0042(4) 0.0016(4) -0.0050(4) O(1) 0.0357(6) 0.0139(6) 0.0236(5) 0.0005(5) -0.0018(4) 0.0031(4) O(2) 0.0407(7) 0.0133(6) 0.0283(6) 0.0003(5) -0.0049(5) 0.0033(4) C(1) 0.0206(7) 0.0143(8) 0.0196(7) 0.0004(6) 0.0051(6) 0.0010(6) C(2) 0.0196(7) 0.0150(8) 0.0193(6) 0.0003(6) 0.0050(5) 0.0010(6) C(3) 0.0221(7) 0.0152(8) 0.0213(7) 0.0016(6) 0.0027(6) 0.0028(6) C(4) 0.0218(7) 0.0184(8) 0.0213(7) 0.0008(6) 0.0020(6) 0.0021(6) C(5) 0.0193(7) 0.0172(8) 0.0205(7) -0.0001(6) 0.0048(6) -0.0004(6) C(6) 0.0210(7) 0.0138(8) 0.0205(7) 0.0016(6) 0.0044(6) 0.0011(6) C(7) 0.0198(7) 0.0151(8) 0.0192(7) 0.0015(6) 0.0048(6) 0.0007(6) C(8) 0.0227(7) 0.0154(8) 0.0209(7) 0.0003(6) 0.0045(6) 0.0016(6) C(9) 0.0196(7) 0.0154(8) 0.0199(7) 0.0011(6) 0.0044(5) 0.0004(6) C(10) 0.0227(7) 0.0153(8) 0.0236(7) 0.0025(6) 0.0017(6) 0.0029(6) C(11) 0.0231(7) 0.0187(8) 0.0213(7) 0.0012(6) 0.0008(6) 0.0028(6) C(12) 0.0190(7) 0.0174(8) 0.0197(7) 0.0004(6) 0.0041(6) 0.0000(6) C(13) 0.0212(7) 0.0145(8) 0.0211(7) 0.0013(6) 0.0050(6) 0.0026(6) C(14) 0.0185(7) 0.0163(8) 0.0189(7) 0.0012(6) 0.0056(6) 0.0013(6) C(15) 0.0199(7) 0.0158(8) 0.0220(7) 0.0028(6) 0.0007(6) -0.0009(6) C(16) 0.0263(8) 0.0175(8) 0.0231(7) 0.0008(6) 0.0024(6) 0.0017(6) C(17) 0.0281(8) 0.0226(9) 0.0191(7) 0.0038(7) 0.0009(6) 0.0010(6) C(18) 0.0198(7) 0.0191(8) 0.0241(7) 0.0049(6) -0.0003(6) -0.0034(6) C(19) 0.0214(7) 0.0172(8) 0.0248(7) 0.0030(6) 0.0015(6) 0.0011(6) C(20) 0.0220(7) 0.0180(8) 0.0215(7) 0.0026(6) 0.0026(5) 0.0019(6) C(21) 0.0267(8) 0.0226(9) 0.0270(8) 0.0031(7) -0.0009(6) -0.0031(6) C(22) 0.0183(7) 0.0164(8) 0.0224(7) 0.0031(6) 0.0013(6) 0.0009(6) C(23) 0.0249(7) 0.0176(8) 0.0224(7) 0.0012(6) 0.0023(6) 0.0025(6) C(24) 0.0246(7) 0.0195(9) 0.0203(7) 0.0012(6) 0.0001(6) 0.0015(6) C(25) 0.0168(7) 0.0186(8) 0.0226(7) 0.0030(6) -0.0005(5) -0.0002(6) C(26) 0.0190(7) 0.0174(8) 0.0244(7) 0.0004(6) 0.0009(6) 0.0035(6) C(27) 0.0204(7) 0.0199(8) 0.0199(7) 0.0020(6) 0.0008(5) 0.0019(6) C(28) 0.0234(8) 0.0206(9) 0.0234(7) 0.0005(6) -0.0002(6) 0.0018(6) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _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 F(1) C(21) 1.341(2) . . yes F(2) C(21) 1.346(2) . . yes F(3) C(21) 1.340(2) . . yes F(4) C(28) 1.336(2) . . yes F(5) C(28) 1.343(2) . . yes F(6) C(28) 1.352(2) . . yes O(1) C(1) 1.219(2) . . yes O(2) C(8) 1.222(2) . . yes C(1) C(2) 1.489(2) . . yes C(1) C(14) 1.487(2) . . yes C(2) C(3) 1.392(2) . . yes C(2) C(7) 1.405(2) . . yes C(3) C(4) 1.381(2) . . yes C(4) C(5) 1.400(2) . . yes C(5) C(6) 1.397(2) . . yes C(5) C(15) 1.486(2) . . yes C(6) C(7) 1.396(2) . . yes C(7) C(8) 1.490(2) . . yes C(8) C(9) 1.488(2) . . yes C(9) C(10) 1.395(2) . . yes C(9) C(14) 1.401(2) . . yes C(10) C(11) 1.379(2) . . yes C(11) C(12) 1.405(2) . . yes C(12) C(13) 1.397(2) . . yes C(12) C(22) 1.486(2) . . yes C(13) C(14) 1.395(2) . . yes C(15) C(16) 1.398(2) . . yes C(15) C(20) 1.395(2) . . yes C(16) C(17) 1.379(2) . . yes C(17) C(18) 1.387(2) . . yes C(18) C(19) 1.392(2) . . yes C(18) C(21) 1.491(2) . . yes C(19) C(20) 1.387(2) . . yes C(22) C(23) 1.400(2) . . yes C(22) C(27) 1.396(2) . . yes C(23) C(24) 1.386(2) . . yes C(24) C(25) 1.388(2) . . yes C(25) C(26) 1.393(2) . . yes C(25) C(28) 1.497(2) . . yes C(26) C(27) 1.383(2) . . 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 O(1) C(1) C(2) 121.0(1) . . . yes O(1) C(1) C(14) 121.5(1) . . . yes C(2) C(1) C(14) 117.5(1) . . . yes C(1) C(2) C(3) 118.7(1) . . . yes C(1) C(2) C(7) 121.9(1) . . . yes C(3) C(2) C(7) 119.4(1) . . . yes C(2) C(3) C(4) 120.2(1) . . . yes C(3) C(4) C(5) 121.0(1) . . . yes C(4) C(5) C(6) 118.9(1) . . . yes C(4) C(5) C(15) 119.5(1) . . . yes C(6) C(5) C(15) 121.5(1) . . . yes C(5) C(6) C(7) 120.3(1) . . . yes C(2) C(7) C(6) 120.0(1) . . . yes C(2) C(7) C(8) 120.4(1) . . . yes C(6) C(7) C(8) 119.5(1) . . . yes O(2) C(8) C(7) 121.4(1) . . . yes O(2) C(8) C(9) 121.1(1) . . . yes C(7) C(8) C(9) 117.5(1) . . . yes C(8) C(9) C(10) 118.9(1) . . . yes C(8) C(9) C(14) 121.9(1) . . . yes C(10) C(9) C(14) 119.1(1) . . . yes C(9) C(10) C(11) 120.5(1) . . . yes C(10) C(11) C(12) 121.0(1) . . . yes C(11) C(12) C(13) 118.5(1) . . . yes C(11) C(12) C(22) 120.6(1) . . . yes C(13) C(12) C(22) 121.0(1) . . . yes C(12) C(13) C(14) 120.7(1) . . . yes C(1) C(14) C(9) 120.7(1) . . . yes C(1) C(14) C(13) 119.1(1) . . . yes C(9) C(14) C(13) 120.2(1) . . . yes C(5) C(15) C(16) 119.3(1) . . . yes C(5) C(15) C(20) 121.8(1) . . . yes C(16) C(15) C(20) 119.0(1) . . . yes C(15) C(16) C(17) 120.6(1) . . . yes C(16) C(17) C(18) 119.9(1) . . . yes C(17) C(18) C(19) 120.3(1) . . . yes C(17) C(18) C(21) 118.6(1) . . . yes C(19) C(18) C(21) 121.1(1) . . . yes C(18) C(19) C(20) 119.6(1) . . . yes C(15) C(20) C(19) 120.6(1) . . . yes F(1) C(21) F(2) 105.5(1) . . . yes F(1) C(21) F(3) 106.9(1) . . . yes F(1) C(21) C(18) 112.5(1) . . . yes F(2) C(21) F(3) 106.5(1) . . . yes F(2) C(21) C(18) 112.0(1) . . . yes F(3) C(21) C(18) 113.0(1) . . . yes C(12) C(22) C(23) 120.4(1) . . . yes C(12) C(22) C(27) 120.9(1) . . . yes C(23) C(22) C(27) 118.8(1) . . . yes C(22) C(23) C(24) 120.8(1) . . . yes C(23) C(24) C(25) 119.7(1) . . . yes C(24) C(25) C(26) 120.0(1) . . . yes C(24) C(25) C(28) 120.9(1) . . . yes C(26) C(25) C(28) 119.0(1) . . . yes C(25) C(26) C(27) 120.1(1) . . . yes C(22) C(27) C(26) 120.6(1) . . . yes F(4) C(28) F(5) 107.3(1) . . . yes F(4) C(28) F(6) 106.0(1) . . . yes F(4) C(28) C(25) 113.1(1) . . . yes F(5) C(28) F(6) 105.2(1) . . . yes F(5) C(28) C(25) 112.7(1) . . . yes F(6) C(28) C(25) 112.0(1) . . . yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F(1) C(21) C(18) C(17) 40.6(2) . . . . yes F(1) C(21) C(18) C(19) -140.0(1) . . . . yes F(2) C(21) C(18) C(17) -78.0(2) . . . . yes F(2) C(21) C(18) C(19) 101.4(2) . . . . yes F(3) C(21) C(18) C(17) 161.8(1) . . . . yes F(3) C(21) C(18) C(19) -18.8(2) . . . . yes F(4) C(28) C(25) C(24) 18.1(2) . . . . yes F(4) C(28) C(25) C(26) -164.8(1) . . . . yes F(5) C(28) C(25) C(24) 140.0(1) . . . . yes F(5) C(28) C(25) C(26) -42.9(2) . . . . yes F(6) C(28) C(25) C(24) -101.6(2) . . . . yes F(6) C(28) C(25) C(26) 75.4(2) . . . . yes O(1) C(1) C(2) C(3) 1.0(2) . . . . yes O(1) C(1) C(2) C(7) 179.8(1) . . . . yes O(1) C(1) C(14) C(9) 179.5(1) . . . . yes O(1) C(1) C(14) C(13) 0.4(2) . . . . yes O(2) C(8) C(7) C(2) 178.1(1) . . . . yes O(2) C(8) C(7) C(6) -3.0(2) . . . . yes O(2) C(8) C(9) C(10) 1.3(2) . . . . yes O(2) C(8) C(9) C(14) -178.8(1) . . . . yes C(1) C(2) C(3) C(4) 176.4(1) . . . . yes C(1) C(2) C(7) C(6) -178.0(1) . . . . yes C(1) C(2) C(7) C(8) 0.8(2) . . . . yes C(1) C(14) C(9) C(8) 0.5(2) . . . . yes C(1) C(14) C(9) C(10) -179.5(1) . . . . yes C(1) C(14) C(13) C(12) 178.4(1) . . . . yes C(2) C(1) C(14) C(9) -1.4(2) . . . . yes C(2) C(1) C(14) C(13) 179.5(1) . . . . yes C(2) C(3) C(4) C(5) 1.3(2) . . . . yes C(2) C(7) C(6) C(5) 2.1(2) . . . . yes C(2) C(7) C(8) C(9) -1.6(2) . . . . yes C(3) C(2) C(1) C(14) -178.1(1) . . . . yes C(3) C(2) C(7) C(6) 0.7(2) . . . . yes C(3) C(2) C(7) C(8) 179.6(1) . . . . yes C(3) C(4) C(5) C(6) 1.5(2) . . . . yes C(3) C(4) C(5) C(15) -177.1(1) . . . . yes C(4) C(3) C(2) C(7) -2.4(2) . . . . yes C(4) C(5) C(6) C(7) -3.2(2) . . . . yes C(4) C(5) C(15) C(16) 39.7(2) . . . . yes C(4) C(5) C(15) C(20) -140.0(1) . . . . yes C(5) C(6) C(7) C(8) -176.8(1) . . . . yes C(5) C(15) C(16) C(17) -180.0(1) . . . . yes C(5) C(15) C(20) C(19) 178.8(1) . . . . yes C(6) C(5) C(15) C(16) -139.0(1) . . . . yes C(6) C(5) C(15) C(20) 41.4(2) . . . . yes C(6) C(7) C(8) C(9) 177.2(1) . . . . yes C(7) C(2) C(1) C(14) 0.7(2) . . . . yes C(7) C(6) C(5) C(15) 175.4(1) . . . . yes C(7) C(8) C(9) C(10) -179.0(1) . . . . yes C(7) C(8) C(9) C(14) 1.0(2) . . . . yes C(8) C(9) C(10) C(11) -179.0(1) . . . . yes C(8) C(9) C(14) C(13) 179.6(1) . . . . yes C(9) C(10) C(11) C(12) -0.5(2) . . . . yes C(9) C(14) C(13) C(12) -0.7(2) . . . . yes C(10) C(9) C(14) C(13) -0.5(2) . . . . yes C(10) C(11) C(12) C(13) -0.6(2) . . . . yes C(10) C(11) C(12) C(22) 178.6(1) . . . . yes C(11) C(10) C(9) C(14) 1.1(2) . . . . yes C(11) C(12) C(13) C(14) 1.2(2) . . . . yes C(11) C(12) C(22) C(23) -35.8(2) . . . . yes C(11) C(12) C(22) C(27) 144.6(1) . . . . yes C(12) C(22) C(23) C(24) -178.0(1) . . . . yes C(12) C(22) C(27) C(26) 178.6(1) . . . . yes C(13) C(12) C(22) C(23) 143.5(1) . . . . yes C(13) C(12) C(22) C(27) -36.2(2) . . . . yes C(14) C(13) C(12) C(22) -178.0(1) . . . . yes C(15) C(16) C(17) C(18) 1.6(2) . . . . yes C(15) C(20) C(19) C(18) 0.9(2) . . . . yes C(16) C(15) C(20) C(19) -0.9(2) . . . . yes C(16) C(17) C(18) C(19) -1.6(2) . . . . yes C(16) C(17) C(18) C(21) 177.8(1) . . . . yes C(17) C(16) C(15) C(20) -0.3(2) . . . . yes C(17) C(18) C(19) C(20) 0.4(2) . . . . yes C(20) C(19) C(18) C(21) -179.0(1) . . . . yes C(22) C(23) C(24) C(25) -0.7(2) . . . . yes C(22) C(27) C(26) C(25) -0.5(2) . . . . yes C(23) C(22) C(27) C(26) -1.1(2) . . . . yes C(23) C(24) C(25) C(26) -0.8(2) . . . . yes C(23) C(24) C(25) C(28) 176.2(1) . . . . yes C(24) C(23) C(22) C(27) 1.7(2) . . . . yes C(24) C(25) C(26) C(27) 1.4(2) . . . . yes C(27) C(26) C(25) C(28) -175.7(1) . . . . yes C(27) C(26) C(25) C(28) -175.7(1) . . . . 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 F(1) F(5) 2.958(2) . 3_755 ? F(1) F(4) 2.989(2) . 3_755 ? F(1) C(24) 3.201(2) . 4_444 ? F(1) C(23) 3.231(2) . 4_444 ? F(1) C(28) 3.546(3) . 3_755 ? F(1) F(2) 3.581(1) . 2_544 ? F(2) F(6) 2.898(2) . 3_655 ? F(2) C(24) 3.066(2) . 3_655 ? F(2) F(4) 3.180(3) . 3_655 ? F(2) C(17) 3.185(2) . 2_544 ? F(2) C(28) 3.294(3) . 3_655 ? F(2) F(3) 3.322(1) . 2_554 ? F(2) C(25) 3.361(2) . 3_655 ? F(2) C(16) 3.437(2) . 2_544 ? F(3) F(6) 2.937(2) . 3_655 ? F(3) F(5) 3.224(3) . 3_755 ? F(4) C(24) 3.518(2) . 2_755 ? F(5) C(18) 3.070(2) . 3_755 ? F(5) C(21) 3.217(3) . 3_755 ? F(5) C(4) 3.318(2) . 3_765 ? F(5) C(3) 3.392(2) . 3_765 ? F(5) C(19) 3.397(2) . 3_755 ? F(5) C(17) 3.530(2) . 3_755 ? F(6) C(11) 3.455(2) . 1_565 ? F(6) C(21) 3.475(3) . 3_655 ? O(1) C(27) 3.238(2) . 3_765 ? O(1) C(26) 3.317(2) . 3_765 ? O(1) O(2) 3.453(2) . 1_565 ? O(2) C(20) 3.480(2) . 3_645 ? C(1) C(7) 3.452(3) . 3_655 ? C(1) C(6) 3.544(2) . 3_655 ? C(2) C(7) 3.526(2) . 3_655 ? C(3) C(9) 3.484(3) . 3_655 ? C(3) C(8) 3.528(2) . 3_655 ? C(4) C(9) 3.595(2) . 3_655 ? C(6) C(27) 3.409(2) . 3_755 ? C(10) C(26) 3.511(2) . 1_545 ? C(13) C(20) 3.547(2) . 3_655 ? #===END #------------------------------------------------------------------------------ data_2_ _database_code_depnum_ccdc_archive 'CCDC 709633' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C36 H18 F6 O2 S2 ' _chemical_formula_moiety 'C36 H18 F6 O2 S2 ' _chemical_formula_weight 660.65 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.6863(8) _cell_length_b 10.3804(9) _cell_length_c 17.944(2) _cell_angle_alpha 73.353(5) _cell_angle_beta 95.705(7) _cell_angle_gamma 101.578(6) _cell_volume 1342.4(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6985 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.973 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.33 _diffrn_reflns_number 12738 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9762 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9762 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5990 _reflns_number_gt 1518 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.1481 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5990 _refine_ls_number_parameters 415 _refine_ls_goodness_of_fit_ref 0.754 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.00100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0067 _refine_diff_density_max 1.55 _refine_diff_density_min -0.98 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _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 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) ; 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) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # 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 S(1) S 0.9887(2) 0.6579(2) 0.67392(9) 0.0439(5) Uani 1.00 d . . . S(2) S 0.5170(2) -0.2677(2) 0.29686(9) 0.0440(5) Uani 1.00 d . . . F(1) F 1.1735(6) 1.1706(4) 0.8869(2) 0.082(2) Uani 1.00 d . . . F(2) F 1.4207(5) 1.1111(4) 0.9328(2) 0.065(1) Uani 1.00 d . . . F(3) F 1.1881(5) 1.0081(3) 0.9923(2) 0.066(1) Uani 1.00 d . . . F(4) F 0.3670(5) -0.6476(3) 0.0011(2) 0.066(1) Uani 1.00 d . . . F(5) F 0.0904(5) -0.7025(3) 0.0236(2) 0.056(1) Uani 1.00 d . . . F(6) F 0.2777(5) -0.8058(3) 0.1033(2) 0.057(1) Uani 1.00 d . . . O(1) O 0.5323(6) 0.3342(4) 0.3788(2) 0.051(2) Uani 1.00 d . . . O(2) O 0.8970(6) 0.0315(4) 0.6125(2) 0.049(1) Uani 1.00 d . . . C(1) C 1.250(1) 1.0629(7) 0.9203(4) 0.047(2) Uani 1.00 d . . . C(2) C 1.2211(9) 0.9609(5) 0.8740(3) 0.038(2) Uani 1.00 d . . . C(3) C 1.1120(9) 0.9714(6) 0.8078(3) 0.042(2) Uani 1.00 d . . . C(4) C 1.0763(9) 0.8706(6) 0.7687(3) 0.041(2) Uani 1.00 d . . . C(5) C 1.1536(8) 0.7542(6) 0.7981(3) 0.039(2) Uani 1.00 d . . . C(6) C 1.2670(9) 0.7442(6) 0.8631(3) 0.044(2) Uani 1.00 d . . . C(7) C 1.3035(9) 0.8472(6) 0.9015(3) 0.043(2) Uani 1.00 d . . . C(8) C 1.1149(8) 0.6426(6) 0.7607(3) 0.038(2) Uani 1.00 d . . . C(9) C 1.1577(8) 0.5152(6) 0.7854(3) 0.043(2) Uani 1.00 d . . . C(10) C 1.0908(9) 0.4310(6) 0.7364(3) 0.043(2) Uani 1.00 d . . . C(11) C 0.9933(8) 0.4948(5) 0.6714(3) 0.036(2) Uani 1.00 d . . . C(12) C 0.9023(8) 0.4392(5) 0.6099(3) 0.032(2) Uani 1.00 d . . . C(13) C 0.7994(8) 0.5139(5) 0.5502(3) 0.039(2) Uani 1.00 d . . . C(14) C 0.7144(8) 0.4607(6) 0.4921(3) 0.040(2) Uani 1.00 d . . . C(15) C 0.7216(8) 0.3276(6) 0.4911(3) 0.037(2) Uani 1.00 d . . . C(16) C 0.6248(9) 0.2689(6) 0.4294(3) 0.039(2) Uani 1.00 d . . . C(17) C 0.6472(8) 0.1301(5) 0.4290(3) 0.033(2) Uani 1.00 d . . . C(18) C 0.5683(8) 0.0777(6) 0.3687(3) 0.037(2) Uani 1.00 d . . . C(19) C 0.5749(8) -0.0532(5) 0.3651(3) 0.033(2) Uani 1.00 d . . . C(20) C 0.6775(8) -0.1312(5) 0.4275(3) 0.038(2) Uani 1.00 d . . . C(21) C 0.7566(8) -0.0801(5) 0.4882(3) 0.036(2) Uani 1.00 d . . . C(22) C 0.7436(8) 0.0545(6) 0.4892(3) 0.035(2) Uani 1.00 d . . . C(23) C 0.8272(8) 0.1063(6) 0.5545(3) 0.036(2) Uani 1.00 d . . . C(24) C 0.8206(8) 0.2500(6) 0.5516(3) 0.035(2) Uani 1.00 d . . . C(25) C 0.9099(8) 0.3051(5) 0.6096(3) 0.035(2) Uani 1.00 d . . . C(26) C 0.4896(8) -0.1094(5) 0.3050(3) 0.038(2) Uani 1.00 d . . . C(27) C 0.3706(8) -0.0579(6) 0.2483(3) 0.039(2) Uani 1.00 d . . . C(28) C 0.3015(9) -0.1425(6) 0.1991(3) 0.041(2) Uani 1.00 d . . . C(29) C 0.3688(8) -0.2614(6) 0.2172(3) 0.037(2) Uani 1.00 d . . . C(30) C 0.3336(8) -0.3703(6) 0.1787(3) 0.039(2) Uani 1.00 d . . . C(31) C 0.2434(8) -0.3559(6) 0.1069(3) 0.042(2) Uani 1.00 d . . . C(32) C 0.2142(9) -0.4558(6) 0.0686(3) 0.046(2) Uani 1.00 d . . . C(33) C 0.2746(8) -0.5772(6) 0.1030(3) 0.039(2) Uani 1.00 d . . . C(34) C 0.3588(8) -0.5980(6) 0.1749(3) 0.041(2) Uani 1.00 d . . . C(35) C 0.3893(9) -0.4948(6) 0.2133(3) 0.046(2) Uani 1.00 d . . . C(36) C 0.252(1) -0.6804(6) 0.0578(4) 0.044(2) Uani 1.00 d . . . H(1) H 1.0616 1.0536 0.7884 0.0373 Uiso 1.00 calc . . . H(2) H 0.9991 0.8810 0.7229 0.0478 Uiso 1.00 calc . . . H(3) H 1.3271 0.6644 0.8830 0.0450 Uiso 1.00 calc . . . H(4) H 1.3848 0.8350 0.9473 0.0502 Uiso 1.00 calc . . . H(5) H 1.2237 0.4854 0.8317 0.0441 Uiso 1.00 calc . . . H(6) H 1.1084 0.3391 0.7450 0.0600 Uiso 1.00 calc . . . H(7) H 0.7895 0.6042 0.5501 0.0482 Uiso 1.00 calc . . . H(8) H 0.6465 0.5142 0.4506 0.0385 Uiso 1.00 calc . . . H(9) H 0.5011 0.1339 0.3276 0.0419 Uiso 1.00 calc . . . H(10) H 0.6926 -0.2184 0.4257 0.0392 Uiso 1.00 calc . . . H(11) H 0.8264 -0.1324 0.5301 0.0409 Uiso 1.00 calc . . . H(12) H 0.9765 0.2488 0.6504 0.0347 Uiso 1.00 calc . . . H(13) H 0.3376 0.0291 0.2415 0.0545 Uiso 1.00 calc . . . H(14) H 0.2226 -0.1206 0.1553 0.0359 Uiso 1.00 calc . . . H(15) H 0.2100 -0.2646 0.0818 0.0533 Uiso 1.00 calc . . . H(16) H 0.1401 -0.4496 0.0217 0.0523 Uiso 1.00 calc . . . H(17) H 0.3689 -0.6934 0.2024 0.0499 Uiso 1.00 calc . . . H(18) H 0.4559 -0.5069 0.2625 0.0513 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 S(1) 0.060(1) 0.0437(10) 0.0327(9) 0.0083(9) 0.0012(8) -0.0194(8) S(2) 0.061(1) 0.0444(10) 0.0335(9) 0.0107(9) -0.0004(9) -0.0212(8) F(1) 0.135(4) 0.063(3) 0.074(3) 0.059(3) -0.038(3) -0.047(2) F(2) 0.072(3) 0.072(3) 0.060(3) -0.006(2) 0.012(2) -0.046(2) F(3) 0.096(4) 0.065(3) 0.048(2) -0.004(2) 0.020(2) -0.039(2) F(4) 0.088(4) 0.068(3) 0.053(3) -0.005(2) 0.031(2) -0.039(2) F(5) 0.058(3) 0.062(2) 0.064(3) 0.015(2) -0.019(2) -0.044(2) F(6) 0.086(3) 0.049(2) 0.046(2) 0.022(2) -0.009(2) -0.026(2) O(1) 0.074(4) 0.046(3) 0.038(3) 0.011(2) -0.008(2) -0.021(2) O(2) 0.074(4) 0.048(3) 0.034(2) 0.022(2) -0.009(2) -0.021(2) C(1) 0.060(6) 0.053(5) 0.030(4) 0.002(4) 0.003(4) -0.021(3) C(2) 0.056(5) 0.027(3) 0.038(4) 0.003(3) 0.010(3) -0.018(3) C(3) 0.060(5) 0.041(4) 0.028(3) 0.016(3) 0.003(3) -0.013(3) C(4) 0.059(5) 0.033(3) 0.037(4) 0.007(3) 0.009(3) -0.016(3) C(5) 0.048(5) 0.047(4) 0.026(3) 0.003(3) 0.008(3) -0.017(3) C(6) 0.063(5) 0.041(4) 0.036(4) 0.013(3) -0.001(3) -0.021(3) C(7) 0.058(5) 0.046(4) 0.033(4) 0.013(3) -0.001(3) -0.021(3) C(8) 0.055(5) 0.039(4) 0.022(3) 0.008(3) 0.003(3) -0.012(3) C(9) 0.051(5) 0.054(4) 0.029(3) 0.008(3) -0.011(3) -0.026(3) C(10) 0.061(5) 0.044(4) 0.033(4) 0.018(3) -0.002(3) -0.020(3) C(11) 0.044(5) 0.041(4) 0.030(3) 0.005(3) 0.007(3) -0.019(3) C(12) 0.036(4) 0.034(3) 0.030(3) 0.002(3) 0.008(3) -0.015(3) C(13) 0.047(5) 0.044(4) 0.032(3) 0.002(3) 0.007(3) -0.022(3) C(14) 0.051(5) 0.044(4) 0.029(3) 0.007(3) 0.002(3) -0.015(3) C(15) 0.040(5) 0.046(4) 0.032(4) 0.006(3) 0.008(3) -0.018(3) C(16) 0.050(5) 0.045(4) 0.024(3) 0.010(3) 0.010(3) -0.010(3) C(17) 0.041(4) 0.036(3) 0.024(3) -0.001(3) 0.012(3) -0.016(3) C(18) 0.043(4) 0.043(4) 0.030(3) 0.005(3) 0.005(3) -0.017(3) C(19) 0.052(5) 0.025(3) 0.026(3) -0.001(3) 0.014(3) -0.012(3) C(20) 0.049(5) 0.039(4) 0.031(3) 0.009(3) -0.002(3) -0.021(3) C(21) 0.039(4) 0.041(4) 0.033(3) 0.005(3) 0.001(3) -0.020(3) C(22) 0.047(5) 0.039(4) 0.023(3) 0.008(3) 0.007(3) -0.014(3) C(23) 0.042(4) 0.040(4) 0.031(3) 0.002(3) 0.009(3) -0.017(3) C(24) 0.040(4) 0.044(4) 0.027(3) 0.007(3) 0.006(3) -0.019(3) C(25) 0.052(5) 0.031(3) 0.027(3) 0.007(3) 0.008(3) -0.011(3) C(26) 0.061(5) 0.033(3) 0.025(3) 0.007(3) 0.010(3) -0.013(3) C(27) 0.052(5) 0.045(4) 0.024(3) 0.012(3) 0.001(3) -0.014(3) C(28) 0.061(5) 0.035(3) 0.029(3) 0.002(3) 0.008(3) -0.014(3) C(29) 0.055(5) 0.037(3) 0.022(3) 0.003(3) 0.005(3) -0.016(3) C(30) 0.056(5) 0.039(4) 0.027(3) 0.002(3) 0.010(3) -0.017(3) C(31) 0.051(5) 0.045(4) 0.034(4) 0.007(3) 0.002(3) -0.016(3) C(32) 0.075(6) 0.038(4) 0.035(4) 0.019(4) -0.007(4) -0.023(3) C(33) 0.051(5) 0.043(4) 0.030(3) 0.008(3) 0.004(3) -0.020(3) C(34) 0.054(5) 0.039(4) 0.036(4) 0.009(3) 0.004(3) -0.022(3) C(35) 0.063(5) 0.049(4) 0.035(4) 0.016(4) 0.005(3) -0.020(3) C(36) 0.066(6) 0.036(4) 0.038(4) 0.012(4) 0.001(4) -0.020(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _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 S(1) C(8) 1.735(6) . . yes S(1) C(11) 1.714(6) . . yes S(2) C(26) 1.746(6) . . yes S(2) C(29) 1.731(6) . . yes F(1) C(1) 1.329(7) . . yes F(2) C(1) 1.328(7) . . yes F(3) C(1) 1.347(6) . . yes F(4) C(36) 1.339(7) . . yes F(5) C(36) 1.337(7) . . yes F(6) C(36) 1.364(6) . . yes O(1) C(16) 1.226(6) . . yes O(2) C(23) 1.251(6) . . yes C(1) C(2) 1.493(8) . . yes C(2) C(3) 1.374(7) . . yes C(2) C(7) 1.393(7) . . yes C(3) C(4) 1.389(8) . . yes C(4) C(5) 1.397(8) . . yes C(5) C(6) 1.377(7) . . yes C(5) C(8) 1.466(7) . . yes C(6) C(7) 1.400(7) . . yes C(8) C(9) 1.365(7) . . yes C(9) C(10) 1.404(7) . . yes C(10) C(11) 1.394(7) . . yes C(11) C(12) 1.446(7) . . yes C(12) C(13) 1.405(7) . . yes C(12) C(25) 1.407(7) . . yes C(13) C(14) 1.367(7) . . yes C(14) C(15) 1.400(7) . . yes C(15) C(16) 1.480(8) . . yes C(15) C(24) 1.410(7) . . yes C(16) C(17) 1.488(7) . . yes C(17) C(18) 1.381(7) . . yes C(17) C(22) 1.386(7) . . yes C(18) C(19) 1.390(7) . . yes C(19) C(20) 1.446(7) . . yes C(19) C(26) 1.414(7) . . yes C(20) C(21) 1.382(7) . . yes C(21) C(22) 1.426(7) . . yes C(22) C(23) 1.466(7) . . yes C(23) C(24) 1.488(7) . . yes C(24) C(25) 1.386(7) . . yes C(26) C(27) 1.363(7) . . yes C(27) C(28) 1.413(7) . . yes C(28) C(29) 1.375(8) . . yes C(29) C(30) 1.454(7) . . yes C(30) C(31) 1.385(7) . . yes C(30) C(35) 1.395(7) . . yes C(31) C(32) 1.372(7) . . yes C(32) C(33) 1.384(7) . . yes C(33) C(34) 1.363(7) . . yes C(33) C(36) 1.494(8) . . yes C(34) C(35) 1.403(8) . . 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(8) S(1) C(11) 93.7(3) . . . yes C(26) S(2) C(29) 93.2(3) . . . yes F(1) C(1) F(2) 106.6(5) . . . yes F(1) C(1) F(3) 107.3(6) . . . yes F(1) C(1) C(2) 113.0(5) . . . yes F(2) C(1) F(3) 103.9(5) . . . yes F(2) C(1) C(2) 113.2(6) . . . yes F(3) C(1) C(2) 112.1(5) . . . yes C(1) C(2) C(3) 123.1(6) . . . yes C(1) C(2) C(7) 117.9(6) . . . yes C(3) C(2) C(7) 118.9(5) . . . yes C(2) C(3) C(4) 122.4(6) . . . yes C(3) C(4) C(5) 118.6(6) . . . yes C(4) C(5) C(6) 119.5(6) . . . yes C(4) C(5) C(8) 120.8(5) . . . yes C(6) C(5) C(8) 119.6(6) . . . yes C(5) C(6) C(7) 121.2(6) . . . yes C(2) C(7) C(6) 119.3(5) . . . yes S(1) C(8) C(5) 120.9(5) . . . yes S(1) C(8) C(9) 109.3(4) . . . yes C(5) C(8) C(9) 129.7(5) . . . yes C(8) C(9) C(10) 114.4(5) . . . yes C(9) C(10) C(11) 113.1(5) . . . yes S(1) C(11) C(10) 109.5(4) . . . yes S(1) C(11) C(12) 121.9(4) . . . yes C(10) C(11) C(12) 128.6(5) . . . yes C(11) C(12) C(13) 122.0(5) . . . yes C(11) C(12) C(25) 120.3(5) . . . yes C(13) C(12) C(25) 117.7(5) . . . yes C(12) C(13) C(14) 121.6(5) . . . yes C(13) C(14) C(15) 121.2(6) . . . yes C(14) C(15) C(16) 121.0(5) . . . yes C(14) C(15) C(24) 118.0(5) . . . yes C(16) C(15) C(24) 121.0(5) . . . yes O(1) C(16) C(15) 121.1(6) . . . yes O(1) C(16) C(17) 120.7(6) . . . yes C(15) C(16) C(17) 118.2(5) . . . yes C(16) C(17) C(18) 119.1(5) . . . yes C(16) C(17) C(22) 119.9(5) . . . yes C(18) C(17) C(22) 121.0(5) . . . yes C(17) C(18) C(19) 123.2(5) . . . yes C(18) C(19) C(20) 115.6(5) . . . yes C(18) C(19) C(26) 123.6(5) . . . yes C(20) C(19) C(26) 120.8(5) . . . yes C(19) C(20) C(21) 121.7(5) . . . yes C(20) C(21) C(22) 120.1(5) . . . yes C(17) C(22) C(21) 118.3(5) . . . yes C(17) C(22) C(23) 122.5(5) . . . yes C(21) C(22) C(23) 119.2(5) . . . yes O(2) C(23) C(22) 121.5(5) . . . yes O(2) C(23) C(24) 120.4(5) . . . yes C(22) C(23) C(24) 118.0(5) . . . yes C(15) C(24) C(23) 119.9(5) . . . yes C(15) C(24) C(25) 120.8(5) . . . yes C(23) C(24) C(25) 119.3(5) . . . yes C(12) C(25) C(24) 120.8(5) . . . yes S(2) C(26) C(19) 122.7(5) . . . yes S(2) C(26) C(27) 109.2(4) . . . yes C(19) C(26) C(27) 128.1(6) . . . yes C(26) C(27) C(28) 114.5(6) . . . yes C(27) C(28) C(29) 113.5(5) . . . yes S(2) C(29) C(28) 109.7(4) . . . yes S(2) C(29) C(30) 121.1(5) . . . yes C(28) C(29) C(30) 129.2(6) . . . yes C(29) C(30) C(31) 122.0(6) . . . yes C(29) C(30) C(35) 120.9(6) . . . yes C(31) C(30) C(35) 117.1(5) . . . yes C(30) C(31) C(32) 122.7(6) . . . yes C(31) C(32) C(33) 119.3(6) . . . yes C(32) C(33) C(34) 120.2(6) . . . yes C(32) C(33) C(36) 118.2(5) . . . yes C(34) C(33) C(36) 121.6(6) . . . yes C(33) C(34) C(35) 120.1(6) . . . yes C(30) C(35) C(34) 120.6(6) . . . yes F(4) C(36) F(5) 106.0(5) . . . yes F(4) C(36) F(6) 105.0(5) . . . yes F(4) C(36) C(33) 113.4(5) . . . yes F(5) C(36) F(6) 105.1(5) . . . yes F(5) C(36) C(33) 114.1(6) . . . yes F(6) C(36) C(33) 112.4(5) . . . yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S(1) C(8) C(5) C(4) 6.1(9) . . . . yes S(1) C(8) C(5) C(6) -174.2(5) . . . . yes S(1) C(8) C(9) C(10) -0.2(7) . . . . yes S(1) C(11) C(10) C(9) 0.0(7) . . . . yes S(1) C(11) C(12) C(13) -2.4(9) . . . . yes S(1) C(11) C(12) C(25) 179.6(4) . . . . yes S(2) C(26) C(19) C(18) 173.8(5) . . . . yes S(2) C(26) C(19) C(20) -5.7(8) . . . . yes S(2) C(26) C(27) C(28) 0.1(7) . . . . yes S(2) C(29) C(28) C(27) 0.7(7) . . . . yes S(2) C(29) C(30) C(31) -167.4(5) . . . . yes S(2) C(29) C(30) C(35) 12.9(9) . . . . yes F(1) C(1) C(2) C(3) -6.0(10) . . . . yes F(1) C(1) C(2) C(7) 176.6(6) . . . . yes F(2) C(1) C(2) C(3) -127.3(7) . . . . yes F(2) C(1) C(2) C(7) 55.3(8) . . . . yes F(3) C(1) C(2) C(3) 115.4(7) . . . . yes F(3) C(1) C(2) C(7) -62.0(8) . . . . yes F(4) C(36) C(33) C(32) 75.2(8) . . . . yes F(4) C(36) C(33) C(34) -102.1(7) . . . . yes F(5) C(36) C(33) C(32) -46.2(8) . . . . yes F(5) C(36) C(33) C(34) 136.5(6) . . . . yes F(6) C(36) C(33) C(32) -165.7(6) . . . . yes F(6) C(36) C(33) C(34) 16.9(10) . . . . yes O(1) C(16) C(15) C(14) -1.8(10) . . . . yes O(1) C(16) C(15) C(24) 176.7(6) . . . . yes O(1) C(16) C(17) C(18) 2.7(9) . . . . yes O(1) C(16) C(17) C(22) -176.2(6) . . . . yes O(2) C(23) C(22) C(17) 172.1(6) . . . . yes O(2) C(23) C(22) C(21) -5.9(9) . . . . yes O(2) C(23) C(24) C(15) -171.7(6) . . . . yes O(2) C(23) C(24) C(25) 7.2(9) . . . . yes C(1) C(2) C(3) C(4) -175.2(6) . . . . yes C(1) C(2) C(7) C(6) 174.7(6) . . . . yes C(2) C(3) C(4) C(5) 0.3(10) . . . . yes C(2) C(7) C(6) C(5) 1(1) . . . . yes C(3) C(2) C(7) C(6) -2.8(10) . . . . yes C(3) C(4) C(5) C(6) -2.1(10) . . . . yes C(3) C(4) C(5) C(8) 177.6(6) . . . . yes C(4) C(3) C(2) C(7) 2.2(10) . . . . yes C(4) C(5) C(6) C(7) 1(1) . . . . yes C(4) C(5) C(8) C(9) -170.8(6) . . . . yes C(5) C(8) S(1) C(11) -177.2(5) . . . . yes C(5) C(8) C(9) C(10) 176.9(6) . . . . yes C(6) C(5) C(8) C(9) 8(1) . . . . yes C(7) C(6) C(5) C(8) -178.3(6) . . . . yes C(8) S(1) C(11) C(10) -0.1(5) . . . . yes C(8) S(1) C(11) C(12) 178.5(5) . . . . yes C(8) C(9) C(10) C(11) 0.2(9) . . . . yes C(9) C(8) S(1) C(11) 0.2(5) . . . . yes C(9) C(10) C(11) C(12) -178.5(6) . . . . yes C(10) C(11) C(12) C(13) 175.9(6) . . . . yes C(10) C(11) C(12) C(25) -2(1) . . . . yes C(11) C(12) C(13) C(14) 179.7(6) . . . . yes C(11) C(12) C(25) C(24) 178.9(6) . . . . yes C(12) C(13) C(14) C(15) 2.1(10) . . . . yes C(12) C(25) C(24) C(15) 0.7(9) . . . . yes C(12) C(25) C(24) C(23) -178.1(5) . . . . yes C(13) C(12) C(25) C(24) 0.8(9) . . . . yes C(13) C(14) C(15) C(16) 178.1(6) . . . . yes C(13) C(14) C(15) C(24) -0.5(9) . . . . yes C(14) C(13) C(12) C(25) -2.2(9) . . . . yes C(14) C(15) C(16) C(17) 176.3(5) . . . . yes C(14) C(15) C(24) C(23) 177.9(6) . . . . yes C(14) C(15) C(24) C(25) -0.9(9) . . . . yes C(15) C(16) C(17) C(18) -175.4(5) . . . . yes C(15) C(16) C(17) C(22) 5.7(8) . . . . yes C(15) C(24) C(23) C(22) 6.0(8) . . . . yes C(16) C(15) C(24) C(23) -0.7(9) . . . . yes C(16) C(15) C(24) C(25) -179.5(6) . . . . yes C(16) C(17) C(18) C(19) -177.0(5) . . . . yes C(16) C(17) C(22) C(21) 177.7(5) . . . . yes C(16) C(17) C(22) C(23) -0.3(9) . . . . yes C(17) C(16) C(15) C(24) -5.2(9) . . . . yes C(17) C(18) C(19) C(20) -2.6(9) . . . . yes C(17) C(18) C(19) C(26) 177.8(6) . . . . yes C(17) C(22) C(21) C(20) 1.4(9) . . . . yes C(17) C(22) C(23) C(24) -5.6(9) . . . . yes C(18) C(17) C(22) C(21) -1.2(9) . . . . yes C(18) C(17) C(22) C(23) -179.2(6) . . . . yes C(18) C(19) C(20) C(21) 2.7(9) . . . . yes C(18) C(19) C(26) C(27) -9(1) . . . . yes C(19) C(18) C(17) C(22) 2.0(10) . . . . yes C(19) C(20) C(21) C(22) -2.2(9) . . . . yes C(19) C(26) S(2) C(29) 177.2(5) . . . . yes C(19) C(26) C(27) C(28) -176.7(6) . . . . yes C(20) C(19) C(26) C(27) 170.7(6) . . . . yes C(20) C(21) C(22) C(23) 179.4(6) . . . . yes C(21) C(20) C(19) C(26) -177.7(6) . . . . yes C(21) C(22) C(23) C(24) 176.4(5) . . . . yes C(22) C(23) C(24) C(25) -175.1(5) . . . . yes C(26) S(2) C(29) C(28) -0.5(5) . . . . yes C(26) S(2) C(29) C(30) 178.3(5) . . . . yes C(26) C(27) C(28) C(29) -0.6(8) . . . . yes C(27) C(26) S(2) C(29) 0.2(5) . . . . yes C(27) C(28) C(29) C(30) -178.0(6) . . . . yes C(28) C(29) C(30) C(31) 11(1) . . . . yes C(28) C(29) C(30) C(35) -168.5(6) . . . . yes C(29) C(30) C(31) C(32) 177.8(6) . . . . yes C(29) C(30) C(35) C(34) -178.4(6) . . . . yes C(30) C(31) C(32) C(33) 0(1) . . . . yes C(30) C(35) C(34) C(33) 0(1) . . . . yes C(31) C(30) C(35) C(34) 2.0(10) . . . . yes C(31) C(32) C(33) C(34) 1(1) . . . . yes C(31) C(32) C(33) C(36) -175.9(6) . . . . yes C(32) C(31) C(30) C(35) -2(1) . . . . yes C(32) C(33) C(34) C(35) -1(1) . . . . yes C(35) C(34) C(33) C(36) 175.3(6) . . . . yes C(35) C(34) C(33) C(36) 175.3(6) . . . . 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(16) 3.497(6) . 2_766 ? S(1) C(17) 3.509(6) . 2_766 ? S(1) C(35) 3.554(7) . 2_656 ? F(1) F(4) 3.234(5) . 1_676 ? F(1) F(5) 3.266(5) . 1_676 ? F(1) C(10) 3.341(7) . 1_565 ? F(1) C(9) 3.539(7) . 1_565 ? F(1) F(3) 3.563(6) . 2_777 ? F(2) C(29) 3.121(7) . 2_766 ? F(2) F(2) 3.160(8) . 2_877 ? F(2) F(4) 3.197(5) . 1_676 ? F(2) C(31) 3.213(7) . 2_766 ? F(2) C(30) 3.230(6) . 2_766 ? F(2) C(28) 3.248(7) . 2_766 ? F(2) F(3) 3.481(6) . 2_877 ? F(2) C(7) 3.556(7) . 2_877 ? F(3) F(3) 2.899(8) . 2_777 ? F(3) F(6) 3.094(5) . 1_676 ? F(3) F(5) 3.445(5) . 1_676 ? F(3) F(5) 3.521(5) . 2_656 ? F(4) F(4) 3.317(7) . 2_645 ? F(4) C(32) 3.424(8) . 2_645 ? F(4) C(33) 3.531(7) . 2_645 ? F(4) C(7) 3.593(7) . 2_756 ? F(5) C(32) 3.184(7) . 2_545 ? F(5) C(31) 3.324(7) . 2_545 ? F(5) C(7) 3.325(7) . 2_656 ? F(5) C(2) 3.431(6) . 2_656 ? F(5) C(6) 3.463(8) . 2_656 ? F(6) C(27) 3.257(6) . 1_545 ? F(6) C(7) 3.345(8) . 2_756 ? F(6) C(3) 3.433(7) . 2_656 ? F(6) C(6) 3.453(7) . 2_756 ? F(6) C(28) 3.457(7) . 1_545 ? F(6) C(4) 3.571(7) . 2_656 ? O(1) C(35) 3.208(7) . 1_565 ? O(1) C(21) 3.561(7) . 2_656 ? O(2) C(4) 3.166(7) . 1_545 ? O(2) C(21) 3.241(7) . 2_756 ? O(2) C(20) 3.312(7) . 2_756 ? O(2) C(27) 3.491(7) . 2_656 ? O(2) C(18) 3.547(7) . 2_656 ? C(9) C(35) 3.529(9) . 2_756 ? C(12) C(14) 3.445(8) . 2_766 ? C(15) C(20) 3.517(8) . 2_656 ? C(16) C(21) 3.393(9) . 2_656 ? C(16) C(20) 3.432(8) . 2_656 ? C(17) C(22) 3.436(8) . 2_656 ? C(17) C(21) 3.455(8) . 2_656 ? C(18) C(23) 3.432(8) . 2_656 ? C(18) C(22) 3.468(8) . 2_656 ? C(19) C(23) 3.418(8) . 2_656 ? C(19) C(24) 3.508(8) . 2_656 ? C(21) C(23) 3.443(9) . 2_756 ? C(24) C(26) 3.479(8) . 2_656 ? C(25) C(26) 3.543(8) . 2_656 ? C(25) C(27) 3.586(8) . 2_656 ? #===END #------------------------------------------------------------------------------ data_3_ _database_code_depnum_ccdc_archive 'CCDC 709634' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C34 H16 F6 N2 O2 S2 ' _chemical_formula_moiety ? _chemical_formula_weight 662.62 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.23(2) _cell_length_b 13.19(2) _cell_length_c 14.43(3) _cell_angle_alpha 73.14(6) _cell_angle_beta 106.48(6) _cell_angle_gamma 114.82(5) _cell_volume 1986(5) _cell_formula_units_Z 3 _cell_measurement_reflns_used 12135 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.972 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 5.33 _diffrn_reflns_number 18811 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9486 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9486 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8628 _reflns_number_gt 3211 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0970 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8628 _refine_ls_number_parameters 622 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.01000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 0.99 _refine_diff_density_min -0.62 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _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 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) ; 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) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # 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 S(1) S 1.2612(1) -0.1118(1) -0.35234(9) 0.0273(4) Uani 1.00 d . . . S(2) S 0.4405(1) -0.8515(1) 0.16782(9) 0.0260(4) Uani 1.00 d . . . S(3) S 0.4187(1) -0.6369(1) -0.25548(10) 0.0263(4) Uani 1.00 d . . . F(1) F 1.7941(2) 0.3487(2) -0.5579(2) 0.0411(9) Uani 1.00 d . . . F(2) F 1.7187(3) 0.4656(2) -0.5511(2) 0.0453(10) Uani 1.00 d . . . F(3) F 1.6377(2) 0.3670(2) -0.6663(2) 0.0376(9) Uani 1.00 d . . . F(4) F -0.0063(3) -1.2942(2) 0.4561(2) 0.0450(10) Uani 1.00 d . . . F(5) F 0.0103(2) -1.4165(2) 0.3974(2) 0.0375(9) Uani 1.00 d . . . F(6) F -0.1244(3) -1.3466(2) 0.3223(2) 0.060(1) Uani 1.00 d . . . F(7) F 0.9647(2) -0.1546(2) -0.4416(2) 0.0408(9) Uani 1.00 d . . . F(8) F 0.8557(3) -0.0568(2) -0.4647(2) 0.0417(10) Uani 1.00 d . . . F(9) F 0.8142(3) -0.1667(2) -0.5644(2) 0.0433(9) Uani 1.00 d . . . O(1) O 0.7450(3) -0.6291(2) -0.2157(2) 0.0283(10) Uani 1.00 d . . . O(2) O 0.9702(3) -0.3422(2) 0.0383(2) 0.032(1) Uani 1.00 d . . . O(3) O 0.1084(3) -0.8524(3) 0.1241(2) 0.029(1) Uani 1.00 d . . . N(1) N 1.3733(3) 0.0188(3) -0.2271(3) 0.025(1) Uani 1.00 d . . . N(2) N 0.3509(3) -0.9957(3) 0.0551(3) 0.023(1) Uani 1.00 d . . . N(3) N 0.5152(3) -0.4961(3) -0.1389(3) 0.021(1) Uani 1.00 d . . . C(1) C 1.6878(5) 0.3626(4) -0.5686(4) 0.027(2) Uani 1.00 d . . . C(2) C 1.6031(4) 0.2692(4) -0.5049(3) 0.024(1) Uani 1.00 d . . . C(3) C 1.6211(4) 0.2793(4) -0.4077(4) 0.029(2) Uani 1.00 d . . . C(4) C 1.5460(4) 0.1925(4) -0.3456(3) 0.027(2) Uani 1.00 d . . . C(5) C 1.4535(4) 0.0977(4) -0.3815(4) 0.022(1) Uani 1.00 d . . . C(6) C 1.4400(4) 0.0889(4) -0.4774(3) 0.026(1) Uani 1.00 d . . . C(7) C 1.5139(4) 0.1745(4) -0.5397(3) 0.029(1) Uani 1.00 d . . . C(8) C 1.3718(4) 0.0111(3) -0.3159(4) 0.020(1) Uani 1.00 d . . . C(9) C 1.2838(4) -0.0737(4) -0.1866(3) 0.024(1) Uani 1.00 d . . . C(10) C 1.2119(4) -0.1542(4) -0.2417(3) 0.021(1) Uani 1.00 d . . . C(11) C 1.1072(4) -0.2593(4) -0.2202(4) 0.023(1) Uani 1.00 d . . . C(12) C 1.0496(4) -0.3363(4) -0.2842(3) 0.024(1) Uani 1.00 d . . . C(13) C 0.9513(4) -0.4338(4) -0.2627(4) 0.026(1) Uani 1.00 d . . . C(14) C 0.9051(4) -0.4597(4) -0.1783(4) 0.022(1) Uani 1.00 d . . . C(15) C 0.7987(4) -0.5656(4) -0.1550(3) 0.024(1) Uani 1.00 d . . . C(16) C 0.7555(4) -0.5900(4) -0.0623(3) 0.021(1) Uani 1.00 d . . . C(17) C 0.6569(4) -0.6901(4) -0.0410(4) 0.023(1) Uani 1.00 d . . . C(18) C 0.6102(4) -0.7134(4) 0.0432(4) 0.022(1) Uani 1.00 d . . . C(19) C 0.6644(4) -0.6350(4) 0.1059(3) 0.023(1) Uani 1.00 d . . . C(20) C 0.7630(4) -0.5366(4) 0.0837(3) 0.024(1) Uani 1.00 d . . . C(21) C 0.8093(4) -0.5131(4) 0.0004(3) 0.020(1) Uani 1.00 d . . . C(22) C 0.9168(4) -0.4065(4) -0.0214(4) 0.026(1) Uani 1.00 d . . . C(23) C 0.9612(4) -0.3840(4) -0.1139(3) 0.021(1) Uani 1.00 d . . . C(24) C 1.0621(4) -0.2822(4) -0.1350(4) 0.023(1) Uani 1.00 d . . . C(25) C 0.5041(4) -0.8192(4) 0.0651(3) 0.023(1) Uani 1.00 d . . . C(26) C 0.4437(4) -0.9060(4) 0.0142(3) 0.024(1) Uani 1.00 d . . . C(27) C 0.3376(4) -0.9811(4) 0.1363(3) 0.020(1) Uani 1.00 d . . . C(28) C 0.2485(4) -1.0618(4) 0.1977(3) 0.020(1) Uani 1.00 d . . . C(29) C 0.1684(4) -1.1632(4) 0.1671(4) 0.028(2) Uani 1.00 d . . . C(30) C 0.0841(5) -1.2458(4) 0.2240(4) 0.026(2) Uani 1.00 d . . . C(31) C 0.0814(4) -1.2276(4) 0.3128(4) 0.022(1) Uani 1.00 d . . . C(32) C 0.1593(5) -1.1251(4) 0.3435(4) 0.029(2) Uani 1.00 d . . . C(33) C 0.2411(4) -1.0447(4) 0.2854(4) 0.026(1) Uani 1.00 d . . . C(34) C -0.0104(5) -1.3198(4) 0.3715(4) 0.032(2) Uani 1.00 d . . . C(35) C 0.8492(5) -0.1585(4) -0.4696(4) 0.026(2) Uani 1.00 d . . . C(36) C 0.7632(4) -0.2538(4) -0.4066(4) 0.022(1) Uani 1.00 d . . . C(37) C 0.7687(4) -0.2396(4) -0.3145(4) 0.027(2) Uani 1.00 d . . . C(38) C 0.6914(4) -0.3240(4) -0.2539(4) 0.026(2) Uani 1.00 d . . . C(39) C 0.6081(4) -0.4252(4) -0.2858(4) 0.022(1) Uani 1.00 d . . . C(40) C 0.6075(4) -0.4391(4) -0.3775(4) 0.023(1) Uani 1.00 d . . . C(41) C 0.6842(5) -0.3545(4) -0.4385(4) 0.028(2) Uani 1.00 d . . . C(42) C 0.5222(4) -0.5101(4) -0.2226(4) 0.020(1) Uani 1.00 d . . . C(43) C 0.4238(4) -0.5873(4) -0.0985(3) 0.022(1) Uani 1.00 d . . . C(44) C 0.3593(4) -0.6725(4) -0.1503(4) 0.023(1) Uani 1.00 d . . . C(45) C 0.2539(4) -0.7762(4) -0.1288(4) 0.021(1) Uani 1.00 d . . . C(46) C 0.1983(4) -0.8551(4) -0.1917(3) 0.023(1) Uani 1.00 d . . . C(47) C 0.0988(4) -0.9527(4) -0.1711(3) 0.022(1) Uani 1.00 d . . . C(48) C 0.0509(4) -0.9758(4) -0.0876(3) 0.021(1) Uani 1.00 d . . . C(49) C 0.0568(4) -0.9182(4) 0.0664(4) 0.023(1) Uani 1.00 d . . . C(50) C 0.1044(4) -0.8979(4) -0.0237(4) 0.022(1) Uani 1.00 d . . . C(51) C 0.2052(4) -0.7985(4) -0.0458(3) 0.022(1) Uani 1.00 d . . . H(1) H 1.6808 0.3457 -0.3839 0.0319 Uiso 1.00 calc . . . H(2) H 1.5542 0.1984 -0.2793 0.0315 Uiso 1.00 calc . . . H(3) H 1.3768 0.0219 -0.5013 0.0314 Uiso 1.00 calc . . . H(4) H 1.5034 0.1688 -0.6070 0.0316 Uiso 1.00 calc . . . H(5) H 1.2730 -0.0846 -0.1204 0.0290 Uiso 1.00 calc . . . H(6) H 1.0808 -0.3189 -0.3440 0.0288 Uiso 1.00 calc . . . H(7) H 0.9143 -0.4877 -0.3073 0.0308 Uiso 1.00 calc . . . H(8) H 0.6206 -0.7442 -0.0847 0.0239 Uiso 1.00 calc . . . H(9) H 0.6325 -0.6480 0.1647 0.0308 Uiso 1.00 calc . . . H(10) H 0.7994 -0.4823 0.1279 0.0332 Uiso 1.00 calc . . . H(11) H 1.0970 -0.2302 -0.0901 0.0286 Uiso 1.00 calc . . . H(12) H 0.4654 -0.9044 -0.0445 0.0290 Uiso 1.00 calc . . . H(13) H 0.1711 -1.1756 0.1056 0.0315 Uiso 1.00 calc . . . H(14) H 0.0294 -1.3166 0.2026 0.0276 Uiso 1.00 calc . . . H(15) H 0.1541 -1.1120 0.4044 0.0333 Uiso 1.00 calc . . . H(16) H 0.2983 -0.9742 0.3076 0.0301 Uiso 1.00 calc . . . H(17) H 0.8282 -0.1727 -0.2921 0.0313 Uiso 1.00 calc . . . H(18) H 0.6948 -0.3126 -0.1898 0.0324 Uiso 1.00 calc . . . H(19) H 0.5529 -0.5090 -0.3996 0.0290 Uiso 1.00 calc . . . H(20) H 0.6821 -0.3634 -0.5024 0.0330 Uiso 1.00 calc . . . H(21) H 0.4049 -0.5889 -0.0363 0.0292 Uiso 1.00 calc . . . H(22) H 0.2318 -0.8423 -0.2479 0.0277 Uiso 1.00 calc . . . H(23) H 0.0588 -1.0039 -0.2154 0.0295 Uiso 1.00 calc . . . H(24) H 0.2412 -0.7452 -0.0022 0.0317 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 S(1) 0.0241(8) 0.0291(7) 0.0249(8) 0.0015(6) 0.0075(6) -0.0094(6) S(2) 0.0242(8) 0.0270(7) 0.0247(8) 0.0033(6) 0.0074(6) -0.0086(6) S(3) 0.0244(8) 0.0263(7) 0.0251(8) 0.0020(6) 0.0077(6) -0.0086(6) F(1) 0.024(2) 0.051(2) 0.045(2) 0.008(2) 0.013(1) -0.006(1) F(2) 0.062(2) 0.028(2) 0.047(2) 0.006(2) 0.026(2) -0.009(1) F(3) 0.037(2) 0.045(2) 0.026(2) 0.012(1) 0.006(1) -0.004(1) F(4) 0.062(2) 0.040(2) 0.040(2) 0.015(2) 0.031(2) -0.003(1) F(5) 0.049(2) 0.023(1) 0.044(2) 0.013(1) 0.022(2) -0.001(1) F(6) 0.017(2) 0.071(2) 0.048(2) -0.005(2) 0.004(2) 0.017(2) F(7) 0.022(2) 0.041(2) 0.051(2) 0.008(1) 0.015(1) 0.007(1) F(8) 0.051(2) 0.020(2) 0.060(2) 0.012(2) 0.029(2) 0.000(1) F(9) 0.050(2) 0.045(2) 0.021(2) 0.001(2) 0.015(2) -0.004(1) O(1) 0.028(2) 0.027(2) 0.026(2) 0.002(2) 0.010(2) -0.006(1) O(2) 0.034(2) 0.030(2) 0.027(2) 0.000(2) 0.012(2) -0.010(2) O(3) 0.031(2) 0.030(2) 0.023(2) 0.000(2) 0.008(2) -0.014(2) N(1) 0.025(2) 0.028(2) 0.024(2) 0.013(2) 0.005(2) -0.005(2) N(2) 0.020(2) 0.020(2) 0.026(2) 0.004(2) 0.007(2) -0.004(2) N(3) 0.025(3) 0.016(2) 0.022(2) 0.008(2) 0.009(2) 0.003(2) C(1) 0.032(3) 0.026(3) 0.027(3) 0.011(3) 0.008(3) -0.006(2) C(2) 0.023(3) 0.027(3) 0.025(3) 0.008(2) 0.010(2) -0.005(2) C(3) 0.024(3) 0.032(3) 0.028(3) 0.003(3) 0.004(3) -0.014(2) C(4) 0.028(3) 0.031(3) 0.024(3) 0.009(3) 0.009(2) -0.006(2) C(5) 0.016(3) 0.025(3) 0.027(3) 0.007(2) 0.005(2) -0.006(2) C(6) 0.018(3) 0.029(3) 0.025(3) -0.004(2) 0.006(2) -0.014(2) C(7) 0.020(3) 0.039(3) 0.023(3) -0.002(2) 0.007(2) -0.015(2) C(8) 0.014(3) 0.017(2) 0.030(3) 0.004(2) 0.000(2) -0.010(2) C(9) 0.018(3) 0.026(3) 0.025(3) 0.007(2) -0.001(2) -0.008(2) C(10) 0.017(3) 0.025(3) 0.022(3) 0.004(2) 0.009(2) -0.004(2) C(11) 0.017(3) 0.027(3) 0.029(3) 0.010(2) 0.006(2) -0.006(2) C(12) 0.017(3) 0.028(3) 0.021(3) -0.002(2) 0.007(2) -0.009(2) C(13) 0.019(3) 0.035(3) 0.023(3) 0.008(3) -0.001(2) -0.013(2) C(14) 0.014(3) 0.022(3) 0.027(3) 0.002(2) 0.002(2) -0.009(2) C(15) 0.022(3) 0.025(3) 0.024(3) 0.005(2) 0.002(2) -0.012(2) C(16) 0.017(3) 0.029(3) 0.016(3) 0.007(2) 0.001(2) -0.009(2) C(17) 0.027(3) 0.018(3) 0.027(3) 0.012(2) 0.000(2) -0.005(2) C(18) 0.018(3) 0.029(3) 0.021(3) 0.012(2) -0.001(2) -0.008(2) C(19) 0.019(3) 0.027(3) 0.020(3) 0.008(2) 0.003(2) -0.003(2) C(20) 0.022(3) 0.026(3) 0.025(3) 0.009(2) -0.002(2) -0.012(2) C(21) 0.015(3) 0.024(3) 0.021(3) 0.005(2) 0.003(2) -0.007(2) C(22) 0.023(3) 0.032(3) 0.027(3) 0.010(3) -0.001(2) -0.015(2) C(23) 0.018(3) 0.031(3) 0.016(3) 0.007(2) 0.004(2) -0.010(2) C(24) 0.020(3) 0.023(3) 0.026(3) 0.009(2) -0.003(2) -0.011(2) C(25) 0.023(3) 0.025(3) 0.022(3) 0.010(2) 0.005(2) -0.005(2) C(26) 0.022(3) 0.029(3) 0.023(3) 0.008(2) 0.005(2) -0.006(2) C(27) 0.015(3) 0.019(3) 0.021(3) 0.003(2) -0.003(2) -0.008(2) C(28) 0.012(3) 0.021(3) 0.022(3) 0.003(2) 0.000(2) -0.004(2) C(29) 0.026(3) 0.029(3) 0.028(3) 0.004(2) 0.006(2) -0.013(2) C(30) 0.028(3) 0.024(3) 0.024(3) 0.004(3) 0.009(3) -0.006(2) C(31) 0.026(3) 0.018(3) 0.021(3) 0.007(2) 0.010(2) 0.002(2) C(32) 0.030(3) 0.033(3) 0.029(3) 0.010(3) 0.005(3) -0.015(2) C(33) 0.019(3) 0.026(3) 0.028(3) -0.001(2) 0.002(2) -0.013(2) C(34) 0.036(4) 0.029(3) 0.035(3) 0.016(3) 0.005(3) -0.009(3) C(35) 0.023(3) 0.034(3) 0.026(3) 0.010(3) 0.005(2) -0.011(2) C(36) 0.024(3) 0.022(3) 0.025(3) 0.010(2) 0.009(2) -0.003(2) C(37) 0.020(3) 0.031(3) 0.024(3) -0.002(3) 0.002(3) -0.016(2) C(38) 0.022(3) 0.031(3) 0.028(3) 0.007(3) 0.009(3) -0.009(2) C(39) 0.010(3) 0.028(3) 0.027(3) 0.007(2) -0.001(2) -0.011(2) C(40) 0.023(3) 0.014(2) 0.025(3) 0.001(2) 0.007(2) -0.003(2) C(41) 0.028(3) 0.035(3) 0.022(3) 0.004(3) 0.010(2) -0.014(2) C(42) 0.018(3) 0.023(3) 0.020(3) 0.009(2) -0.001(2) -0.006(2) C(43) 0.020(3) 0.023(3) 0.022(3) 0.008(2) 0.006(2) 0.001(2) C(44) 0.023(3) 0.030(3) 0.019(3) 0.012(3) 0.003(2) -0.007(2) C(45) 0.016(3) 0.027(3) 0.020(3) 0.008(2) 0.002(2) -0.007(2) C(46) 0.019(3) 0.032(3) 0.019(3) 0.009(2) 0.003(2) -0.009(2) C(47) 0.022(3) 0.023(3) 0.019(3) 0.005(2) 0.000(2) -0.010(2) C(48) 0.015(3) 0.024(3) 0.020(3) 0.003(2) 0.003(2) -0.004(2) C(49) 0.018(3) 0.027(3) 0.023(3) 0.005(2) 0.001(2) -0.010(2) C(50) 0.013(3) 0.022(3) 0.028(3) 0.005(2) 0.001(2) -0.008(2) C(51) 0.023(3) 0.026(3) 0.018(3) 0.008(2) 0.001(2) -0.008(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _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 S(1) C(8) 1.727(4) . . yes S(1) C(10) 1.724(5) . . yes S(2) C(25) 1.731(5) . . yes S(2) C(27) 1.742(4) . . yes S(3) C(42) 1.723(4) . . yes S(3) C(44) 1.725(5) . . yes F(1) C(1) 1.347(5) . . yes F(2) C(1) 1.330(5) . . yes F(3) C(1) 1.363(5) . . yes F(4) C(34) 1.341(6) . . yes F(5) C(34) 1.332(5) . . yes F(6) C(34) 1.320(6) . . yes F(7) C(35) 1.337(6) . . yes F(8) C(35) 1.332(5) . . yes F(9) C(35) 1.335(5) . . yes O(1) C(15) 1.240(5) . . yes O(2) C(22) 1.237(5) . . yes O(3) C(49) 1.227(5) . . yes N(1) C(8) 1.309(6) . . yes N(1) C(9) 1.363(5) . . yes N(2) C(26) 1.373(6) . . yes N(2) C(27) 1.305(6) . . yes N(3) C(42) 1.305(6) . . yes N(3) C(43) 1.367(6) . . yes C(1) C(2) 1.499(6) . . yes C(2) C(3) 1.394(6) . . yes C(2) C(7) 1.382(6) . . yes C(3) C(4) 1.396(6) . . yes C(4) C(5) 1.403(6) . . yes C(5) C(6) 1.378(6) . . yes C(5) C(8) 1.467(6) . . yes C(6) C(7) 1.384(6) . . yes C(9) C(10) 1.357(6) . . yes C(10) C(11) 1.464(6) . . yes C(11) C(12) 1.398(6) . . yes C(11) C(24) 1.391(7) . . yes C(12) C(13) 1.371(6) . . yes C(13) C(14) 1.380(7) . . yes C(14) C(15) 1.486(6) . . yes C(14) C(23) 1.390(6) . . yes C(15) C(16) 1.477(7) . . yes C(16) C(17) 1.389(6) . . yes C(16) C(21) 1.385(6) . . yes C(17) C(18) 1.388(7) . . yes C(18) C(19) 1.397(6) . . yes C(18) C(25) 1.479(6) . . yes C(19) C(20) 1.380(6) . . yes C(20) C(21) 1.373(6) . . yes C(21) C(22) 1.493(6) . . yes C(22) C(23) 1.487(7) . . yes C(23) C(24) 1.416(6) . . yes C(25) C(26) 1.365(6) . . yes C(27) C(28) 1.461(6) . . yes C(28) C(29) 1.394(6) . . yes C(28) C(33) 1.381(6) . . yes C(29) C(30) 1.394(7) . . yes C(30) C(31) 1.382(7) . . yes C(31) C(32) 1.399(6) . . yes C(31) C(34) 1.501(7) . . yes C(32) C(33) 1.378(7) . . yes C(35) C(36) 1.510(7) . . yes C(36) C(37) 1.374(7) . . yes C(36) C(41) 1.391(6) . . yes C(37) C(38) 1.385(6) . . yes C(38) C(39) 1.408(6) . . yes C(39) C(40) 1.386(6) . . yes C(39) C(42) 1.467(6) . . yes C(40) C(41) 1.386(6) . . yes C(43) C(44) 1.361(6) . . yes C(44) C(45) 1.459(6) . . yes C(45) C(46) 1.405(6) . . yes C(45) C(51) 1.389(7) . . yes C(46) C(47) 1.376(6) . . yes C(47) C(48) 1.387(7) . . yes C(48) C(49) 1.489(6) . 2_535 yes C(48) C(50) 1.407(6) . . yes C(49) C(50) 1.483(7) . . yes C(50) C(51) 1.401(6) . . 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(8) S(1) C(10) 90.2(2) . . . yes C(25) S(2) C(27) 90.0(2) . . . yes C(42) S(3) C(44) 90.0(3) . . . yes C(8) N(1) C(9) 110.3(4) . . . yes C(26) N(2) C(27) 112.7(4) . . . yes C(42) N(3) C(43) 110.6(4) . . . yes F(1) C(1) F(2) 106.0(4) . . . yes F(1) C(1) F(3) 105.1(4) . . . yes F(1) C(1) C(2) 112.9(4) . . . yes F(2) C(1) F(3) 106.8(4) . . . yes F(2) C(1) C(2) 113.7(4) . . . yes F(3) C(1) C(2) 111.8(4) . . . yes C(1) C(2) C(3) 117.3(5) . . . yes C(1) C(2) C(7) 121.5(5) . . . yes C(3) C(2) C(7) 121.1(5) . . . yes C(2) C(3) C(4) 118.8(5) . . . yes C(3) C(4) C(5) 120.0(5) . . . yes C(4) C(5) C(6) 119.7(5) . . . yes C(4) C(5) C(8) 118.6(5) . . . yes C(6) C(5) C(8) 121.7(4) . . . yes C(5) C(6) C(7) 120.8(4) . . . yes C(2) C(7) C(6) 119.5(5) . . . yes S(1) C(8) N(1) 114.0(4) . . . yes S(1) C(8) C(5) 121.4(4) . . . yes N(1) C(8) C(5) 124.7(4) . . . yes N(1) C(9) C(10) 117.6(4) . . . yes S(1) C(10) C(9) 108.0(4) . . . yes S(1) C(10) C(11) 121.8(4) . . . yes C(9) C(10) C(11) 130.2(5) . . . yes C(10) C(11) C(12) 121.7(5) . . . yes C(10) C(11) C(24) 119.2(5) . . . yes C(12) C(11) C(24) 119.1(5) . . . yes C(11) C(12) C(13) 120.5(5) . . . yes C(12) C(13) C(14) 121.9(4) . . . yes C(13) C(14) C(15) 121.7(4) . . . yes C(13) C(14) C(23) 118.4(5) . . . yes C(15) C(14) C(23) 119.9(5) . . . yes O(1) C(15) C(14) 119.3(5) . . . yes O(1) C(15) C(16) 121.4(4) . . . yes C(14) C(15) C(16) 119.2(4) . . . yes C(15) C(16) C(17) 118.5(4) . . . yes C(15) C(16) C(21) 120.8(4) . . . yes C(17) C(16) C(21) 120.6(5) . . . yes C(16) C(17) C(18) 120.2(4) . . . yes C(17) C(18) C(19) 118.9(5) . . . yes C(17) C(18) C(25) 120.1(4) . . . yes C(19) C(18) C(25) 121.0(5) . . . yes C(18) C(19) C(20) 120.0(5) . . . yes C(19) C(20) C(21) 121.3(4) . . . yes C(16) C(21) C(20) 119.0(5) . . . yes C(16) C(21) C(22) 120.7(5) . . . yes C(20) C(21) C(22) 120.3(4) . . . yes O(2) C(22) C(21) 120.5(5) . . . yes O(2) C(22) C(23) 121.4(5) . . . yes C(21) C(22) C(23) 118.0(4) . . . yes C(14) C(23) C(22) 121.3(5) . . . yes C(14) C(23) C(24) 120.8(5) . . . yes C(22) C(23) C(24) 117.8(4) . . . yes C(11) C(24) C(23) 119.3(4) . . . yes S(2) C(25) C(18) 122.1(4) . . . yes S(2) C(25) C(26) 109.4(4) . . . yes C(18) C(25) C(26) 128.5(5) . . . yes N(2) C(26) C(25) 115.0(5) . . . yes S(2) C(27) N(2) 112.9(4) . . . yes S(2) C(27) C(28) 121.2(4) . . . yes N(2) C(27) C(28) 125.9(4) . . . yes C(27) C(28) C(29) 117.9(5) . . . yes C(27) C(28) C(33) 123.9(4) . . . yes C(29) C(28) C(33) 118.2(5) . . . yes C(28) C(29) C(30) 120.9(5) . . . yes C(29) C(30) C(31) 119.5(5) . . . yes C(30) C(31) C(32) 120.3(5) . . . yes C(30) C(31) C(34) 117.2(4) . . . yes C(32) C(31) C(34) 122.4(5) . . . yes C(31) C(32) C(33) 118.9(5) . . . yes C(28) C(33) C(32) 122.2(4) . . . yes F(4) C(34) F(5) 105.6(4) . . . yes F(4) C(34) F(6) 108.2(5) . . . yes F(4) C(34) C(31) 112.9(4) . . . yes F(5) C(34) F(6) 104.9(4) . . . yes F(5) C(34) C(31) 111.4(4) . . . yes F(6) C(34) C(31) 113.4(4) . . . yes F(7) C(35) F(8) 105.2(4) . . . yes F(7) C(35) F(9) 107.1(4) . . . yes F(7) C(35) C(36) 113.0(4) . . . yes F(8) C(35) F(9) 107.2(4) . . . yes F(8) C(35) C(36) 111.8(4) . . . yes F(9) C(35) C(36) 112.1(4) . . . yes C(35) C(36) C(37) 117.6(4) . . . yes C(35) C(36) C(41) 121.6(5) . . . yes C(37) C(36) C(41) 120.7(5) . . . yes C(36) C(37) C(38) 120.1(5) . . . yes C(37) C(38) C(39) 120.2(5) . . . yes C(38) C(39) C(40) 118.5(5) . . . yes C(38) C(39) C(42) 119.0(5) . . . yes C(40) C(39) C(42) 122.4(4) . . . yes C(39) C(40) C(41) 121.3(4) . . . yes C(36) C(41) C(40) 119.1(5) . . . yes S(3) C(42) N(3) 114.3(4) . . . yes S(3) C(42) C(39) 121.9(4) . . . yes N(3) C(42) C(39) 123.8(4) . . . yes N(3) C(43) C(44) 116.7(5) . . . yes S(3) C(44) C(43) 108.4(4) . . . yes S(3) C(44) C(45) 122.5(4) . . . yes C(43) C(44) C(45) 129.1(5) . . . yes C(44) C(45) C(46) 121.1(5) . . . yes C(44) C(45) C(51) 120.5(5) . . . yes C(46) C(45) C(51) 118.4(5) . . . yes C(45) C(46) C(47) 120.9(5) . . . yes C(46) C(47) C(48) 120.9(4) . . . yes C(47) C(48) C(49) 120.2(5) . . 2_535 yes C(47) C(48) C(50) 119.4(5) . . . yes C(49) C(48) C(50) 120.4(4) 2_535 . . yes O(3) C(49) C(48) 121.1(5) . . 2_535 yes O(3) C(49) C(50) 120.9(5) . . . yes C(48) C(49) C(50) 117.9(4) 2_535 . . yes C(48) C(50) C(49) 121.7(4) . . . yes C(48) C(50) C(51) 119.2(5) . . . yes C(49) C(50) C(51) 119.2(4) . . . yes C(45) C(51) C(50) 121.3(5) . . . yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S(1) C(8) N(1) C(9) -0.9(5) . . . . yes S(1) C(8) C(5) C(4) -176.4(3) . . . . yes S(1) C(8) C(5) C(6) 4.8(6) . . . . yes S(1) C(10) C(9) N(1) 0.7(5) . . . . yes S(1) C(10) C(11) C(12) 6.5(6) . . . . yes S(1) C(10) C(11) C(24) -172.1(3) . . . . yes S(2) C(25) C(18) C(17) -178.9(3) . . . . yes S(2) C(25) C(18) C(19) 0.5(6) . . . . yes S(2) C(25) C(26) N(2) -0.6(5) . . . . yes S(2) C(27) N(2) C(26) 0.6(5) . . . . yes S(2) C(27) C(28) C(29) 179.4(3) . . . . yes S(2) C(27) C(28) C(33) -2.4(6) . . . . yes S(3) C(42) N(3) C(43) -1.0(5) . . . . yes S(3) C(42) C(39) C(38) -179.2(3) . . . . yes S(3) C(42) C(39) C(40) 3.2(6) . . . . yes S(3) C(44) C(43) N(3) 0.9(5) . . . . yes S(3) C(44) C(45) C(46) 2.7(6) . . . . yes S(3) C(44) C(45) C(51) -176.6(3) . . . . yes F(1) C(1) C(2) C(3) 84.0(5) . . . . yes F(1) C(1) C(2) C(7) -93.4(5) . . . . yes F(2) C(1) C(2) C(3) -36.8(6) . . . . yes F(2) C(1) C(2) C(7) 145.8(4) . . . . yes F(3) C(1) C(2) C(3) -157.8(4) . . . . yes F(3) C(1) C(2) C(7) 24.8(6) . . . . yes F(4) C(34) C(31) C(30) -179.8(4) . . . . yes F(4) C(34) C(31) C(32) -1.8(6) . . . . yes F(5) C(34) C(31) C(30) 61.7(6) . . . . yes F(5) C(34) C(31) C(32) -120.3(5) . . . . yes F(6) C(34) C(31) C(30) -56.4(6) . . . . yes F(6) C(34) C(31) C(32) 121.6(5) . . . . yes F(7) C(35) C(36) C(37) 75.9(6) . . . . yes F(7) C(35) C(36) C(41) -101.7(5) . . . . yes F(8) C(35) C(36) C(37) -42.6(6) . . . . yes F(8) C(35) C(36) C(41) 139.8(4) . . . . yes F(9) C(35) C(36) C(37) -163.0(4) . . . . yes F(9) C(35) C(36) C(41) 19.4(6) . . . . yes O(1) C(15) C(14) C(13) -4.5(7) . . . . yes O(1) C(15) C(14) C(23) 175.8(4) . . . . yes O(1) C(15) C(16) C(17) 3.9(6) . . . . yes O(1) C(15) C(16) C(21) -174.0(4) . . . . yes O(2) C(22) C(21) C(16) -174.6(4) . . . . yes O(2) C(22) C(21) C(20) 4.9(6) . . . . yes O(2) C(22) C(23) C(14) 176.3(4) . . . . yes O(2) C(22) C(23) C(24) -4.3(7) . . . . yes O(3) C(49) C(48) C(47) 3.4(6) . . 2_535 2_535 yes O(3) C(49) C(48) C(50) -176.1(4) . . 2_535 2_535 yes O(3) C(49) C(50) C(48) 176.1(4) . . . . yes O(3) C(49) C(50) C(51) -4.0(7) . . . . yes N(1) C(8) S(1) C(10) 1.2(4) . . . . yes N(1) C(8) C(5) C(4) 4.6(6) . . . . yes N(1) C(8) C(5) C(6) -174.2(4) . . . . yes N(1) C(9) C(10) C(11) -177.6(4) . . . . yes N(2) C(26) C(25) C(18) 177.5(4) . . . . yes N(2) C(27) S(2) C(25) -0.8(3) . . . . yes N(2) C(27) C(28) C(29) -1.1(7) . . . . yes N(2) C(27) C(28) C(33) 177.1(5) . . . . yes N(3) C(42) S(3) C(44) 1.3(4) . . . . yes N(3) C(42) C(39) C(38) 2.3(7) . . . . yes N(3) C(42) C(39) C(40) -175.3(4) . . . . yes N(3) C(43) C(44) C(45) -176.4(4) . . . . yes C(1) C(2) C(3) C(4) -178.3(4) . . . . yes C(1) C(2) C(7) C(6) 178.2(4) . . . . yes C(2) C(3) C(4) C(5) -0.7(7) . . . . yes C(2) C(7) C(6) C(5) 0.8(7) . . . . yes C(3) C(2) C(7) C(6) 0.9(7) . . . . yes C(3) C(4) C(5) C(6) 2.3(7) . . . . yes C(3) C(4) C(5) C(8) -176.6(4) . . . . yes C(4) C(3) C(2) C(7) -0.9(7) . . . . yes C(4) C(5) C(6) C(7) -2.3(7) . . . . yes C(5) C(8) S(1) C(10) -177.9(4) . . . . yes C(5) C(8) N(1) C(9) 178.1(4) . . . . yes C(7) C(6) C(5) C(8) 176.5(4) . . . . yes C(8) S(1) C(10) C(9) -1.0(3) . . . . yes C(8) S(1) C(10) C(11) 177.5(4) . . . . yes C(8) N(1) C(9) C(10) 0.1(5) . . . . yes C(9) C(10) C(11) C(12) -175.3(5) . . . . yes C(9) C(10) C(11) C(24) 6.1(7) . . . . yes C(10) C(11) C(12) C(13) -179.6(4) . . . . yes C(10) C(11) C(24) C(23) -179.7(4) . . . . yes C(11) C(12) C(13) C(14) 0.3(7) . . . . yes C(11) C(24) C(23) C(14) -1.6(7) . . . . yes C(11) C(24) C(23) C(22) 179.0(4) . . . . yes C(12) C(11) C(24) C(23) 1.7(7) . . . . yes C(12) C(13) C(14) C(15) -179.9(4) . . . . yes C(12) C(13) C(14) C(23) -0.2(7) . . . . yes C(13) C(12) C(11) C(24) -1.0(7) . . . . yes C(13) C(14) C(15) C(16) 178.4(4) . . . . yes C(13) C(14) C(23) C(22) -179.8(4) . . . . yes C(13) C(14) C(23) C(24) 0.8(7) . . . . yes C(14) C(15) C(16) C(17) -179.1(4) . . . . yes C(14) C(15) C(16) C(21) 3.0(6) . . . . yes C(14) C(23) C(22) C(21) -0.2(6) . . . . yes C(15) C(14) C(23) C(22) -0.1(7) . . . . yes C(15) C(14) C(23) C(24) -179.5(4) . . . . yes C(15) C(16) C(17) C(18) -177.1(4) . . . . yes C(15) C(16) C(21) C(20) 177.1(4) . . . . yes C(15) C(16) C(21) C(22) -3.3(6) . . . . yes C(16) C(15) C(14) C(23) -1.2(6) . . . . yes C(16) C(17) C(18) C(19) -0.3(6) . . . . yes C(16) C(17) C(18) C(25) 179.1(4) . . . . yes C(16) C(21) C(20) C(19) 0.1(7) . . . . yes C(16) C(21) C(22) C(23) 1.9(6) . . . . yes C(17) C(16) C(21) C(20) -0.7(7) . . . . yes C(17) C(16) C(21) C(22) 178.8(4) . . . . yes C(17) C(18) C(19) C(20) -0.3(7) . . . . yes C(17) C(18) C(25) C(26) 3.2(7) . . . . yes C(18) C(17) C(16) C(21) 0.8(7) . . . . yes C(18) C(19) C(20) C(21) 0.4(7) . . . . yes C(18) C(25) S(2) C(27) -177.5(4) . . . . yes C(19) C(18) C(25) C(26) -177.4(5) . . . . yes C(19) C(20) C(21) C(22) -179.5(4) . . . . yes C(20) C(19) C(18) C(25) -179.7(4) . . . . yes C(20) C(21) C(22) C(23) -178.5(4) . . . . yes C(21) C(22) C(23) C(24) 179.2(4) . . . . yes C(25) S(2) C(27) C(28) 178.8(4) . . . . yes C(25) C(26) N(2) C(27) 0.0(6) . . . . yes C(26) N(2) C(27) C(28) -179.0(4) . . . . yes C(26) C(25) S(2) C(27) 0.7(3) . . . . yes C(27) C(28) C(29) C(30) 177.6(4) . . . . yes C(27) C(28) C(33) C(32) -177.1(4) . . . . yes C(28) C(29) C(30) C(31) -1.0(7) . . . . yes C(28) C(33) C(32) C(31) 0.3(7) . . . . yes C(29) C(28) C(33) C(32) 1.1(7) . . . . yes C(29) C(30) C(31) C(32) 2.5(7) . . . . yes C(29) C(30) C(31) C(34) -179.5(4) . . . . yes C(30) C(29) C(28) C(33) -0.7(7) . . . . yes C(30) C(31) C(32) C(33) -2.1(7) . . . . yes C(33) C(32) C(31) C(34) 179.9(4) . . . . yes C(35) C(36) C(37) C(38) 179.6(4) . . . . yes C(35) C(36) C(41) C(40) 179.8(4) . . . . yes C(36) C(37) C(38) C(39) 0.9(7) . . . . yes C(36) C(41) C(40) C(39) 0.1(7) . . . . yes C(37) C(36) C(41) C(40) 2.3(7) . . . . yes C(37) C(38) C(39) C(40) 1.4(7) . . . . yes C(37) C(38) C(39) C(42) -176.3(4) . . . . yes C(38) C(37) C(36) C(41) -2.8(7) . . . . yes C(38) C(39) C(40) C(41) -1.9(7) . . . . yes C(39) C(42) S(3) C(44) -177.4(4) . . . . yes C(39) C(42) N(3) C(43) 177.7(4) . . . . yes C(41) C(40) C(39) C(42) 175.7(4) . . . . yes C(42) S(3) C(44) C(43) -1.1(3) . . . . yes C(42) S(3) C(44) C(45) 176.4(4) . . . . yes C(42) N(3) C(43) C(44) 0.0(6) . . . . yes C(43) C(44) C(45) C(46) 179.7(5) . . . . yes C(43) C(44) C(45) C(51) 0.4(7) . . . . yes C(44) C(45) C(46) C(47) -179.9(4) . . . . yes C(44) C(45) C(51) C(50) -179.6(4) . . . . yes C(45) C(46) C(47) C(48) -0.2(7) . . . . yes C(45) C(51) C(50) C(48) -0.8(6) . . . . yes C(45) C(51) C(50) C(49) 179.4(4) . . . . yes C(46) C(45) C(51) C(50) 1.1(6) . . . . yes C(46) C(47) C(48) C(49) -179.9(4) . . . 2_535 yes C(46) C(47) C(48) C(50) 0.5(7) . . . . yes C(47) C(46) C(45) C(51) -0.6(7) . . . . yes C(47) C(48) C(49) C(50) -179.8(4) . . 2_535 2_535 yes C(47) C(48) C(50) C(49) 179.8(4) . . . . yes C(47) C(48) C(50) C(51) 0.0(6) . . . . yes C(48) C(49) C(50) C(51) -179.6(4) . 2_535 2_535 2_535 yes C(49) C(48) C(50) C(51) 179.6(4) . 2_535 2_535 2_535 yes C(49) C(48) C(50) C(51) 179.6(4) . 2_535 2_535 2_535 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) F(8) 3.329(3) . 2_754 ? S(1) F(7) 3.343(6) . . ? S(1) F(1) 3.463(3) . 2_854 ? S(2) N(1) 3.578(5) . 2_745 ? S(2) C(8) 3.596(5) . 2_745 ? S(3) F(6) 3.378(6) . 2_535 ? S(3) F(2) 3.548(3) . 2_754 ? F(1) F(5) 2.854(4) . 2_745 ? F(1) F(4) 2.864(5) . 2_745 ? F(1) F(5) 3.151(4) . 1_774 ? F(1) C(34) 3.255(6) . 2_745 ? F(1) C(12) 3.438(6) . 2_854 ? F(2) F(6) 2.920(4) . 1_774 ? F(2) F(5) 3.443(7) . 1_774 ? F(2) C(41) 3.452(5) . 1_665 ? F(2) F(4) 3.522(5) . 1_774 ? F(2) C(34) 3.553(7) . 1_774 ? F(3) C(42) 3.086(5) . 2_754 ? F(3) C(39) 3.249(7) . 2_754 ? F(3) N(3) 3.349(4) . 2_754 ? F(3) C(19) 3.404(6) . 1_664 ? F(4) F(7) 2.850(4) . 1_446 ? F(4) F(9) 3.189(5) . 1_446 ? F(4) C(35) 3.511(6) . 1_446 ? F(4) C(12) 3.533(5) . 1_446 ? F(5) F(5) 3.139(5) . 2_526 ? F(5) C(13) 3.381(5) . 2_635 ? F(6) C(46) 3.098(5) . 2_535 ? F(6) C(45) 3.154(5) . 2_535 ? F(6) C(44) 3.267(6) . 2_535 ? F(7) F(8) 2.964(4) . 2_754 ? F(7) C(12) 3.095(5) . . ? F(7) C(11) 3.385(5) . . ? F(7) C(10) 3.536(6) . . ? F(8) C(6) 3.339(8) . 2_754 ? F(8) C(32) 3.441(5) . 2_645 ? F(8) F(8) 3.528(8) . 2_754 ? F(9) C(46) 3.412(5) . 2_644 ? F(9) C(8) 3.465(6) . 2_754 ? F(9) C(5) 3.577(7) . 2_754 ? O(1) C(3) 3.075(6) . 1_445 ? O(1) C(29) 3.166(5) . 2_635 ? O(1) C(4) 3.184(6) . 1_445 ? O(1) C(30) 3.202(6) . 2_635 ? O(1) C(39) 3.507(6) . . ? O(1) C(40) 3.533(5) . . ? O(2) C(30) 3.018(6) . 1_665 ? O(2) C(29) 3.175(6) . 1_665 ? O(2) O(3) 3.211(4) . 2_645 ? O(2) C(15) 3.361(7) . 2_745 ? O(2) C(51) 3.412(6) . 2_645 ? O(2) C(14) 3.431(5) . 2_745 ? O(2) C(49) 3.443(5) . 2_645 ? O(2) C(50) 3.583(5) . 2_645 ? O(3) C(37) 3.057(6) . 2_645 ? O(3) C(38) 3.172(6) . 2_645 ? O(3) C(24) 3.314(6) . 2_645 ? O(3) C(22) 3.413(5) . 2_645 ? O(3) C(23) 3.517(5) . 2_645 ? O(3) C(33) 3.519(6) . . ? O(3) C(28) 3.596(6) . . ? N(1) C(46) 3.421(7) . 1_665 ? N(1) C(25) 3.522(6) . 2_745 ? N(1) C(26) 3.592(6) . 2_745 ? N(1) C(27) 3.595(8) . 2_745 ? N(2) C(51) 3.506(6) . . ? N(2) C(50) 3.537(7) . . ? N(3) C(17) 3.434(6) . . ? N(3) C(16) 3.437(7) . . ? N(3) C(19) 3.507(7) . 2_645 ? C(4) C(28) 3.507(7) . 2_745 ? C(6) C(6) 3.523(9) . 2_854 ? C(9) C(25) 3.295(7) . 2_745 ? C(9) C(47) 3.353(7) . 1_665 ? C(9) C(46) 3.432(6) . 1_665 ? C(9) C(18) 3.466(6) . 2_745 ? C(10) C(19) 3.543(6) . 2_745 ? C(10) C(18) 3.569(6) . 2_745 ? C(11) C(19) 3.433(7) . 2_745 ? C(11) C(20) 3.520(6) . 2_745 ? C(14) C(38) 3.521(7) . . ? C(14) C(22) 3.589(6) . 2_745 ? C(15) C(39) 3.394(7) . . ? C(15) C(42) 3.565(8) . . ? C(16) C(42) 3.459(7) . . ? C(16) C(24) 3.564(6) . 2_745 ? C(17) C(43) 3.451(7) . . ? C(17) C(42) 3.529(6) . . ? C(18) C(43) 3.274(6) . . ? C(19) C(43) 3.490(6) . 2_645 ? C(20) C(43) 3.397(7) . 2_645 ? C(21) C(23) 3.421(7) . 2_745 ? C(21) C(24) 3.512(6) . 2_745 ? C(22) C(23) 3.516(6) . 2_745 ? C(25) C(44) 3.579(6) . . ? C(25) C(43) 3.595(6) . . ? C(26) C(45) 3.339(6) . . ? C(26) C(26) 3.464(9) . 2_635 ? C(26) C(51) 3.549(8) . . ? C(27) C(50) 3.477(7) . . ? C(27) C(51) 3.539(6) . . ? C(28) C(49) 3.435(7) . . ? #===END #------------------------------------------------------------------------------ # END of CIF #------------------------------------------------------------------------------