Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistr' loop_ _publ_author_name 'Geiser, Urs' 'Kini, Aravinda M.' 'Morales, Emilio' 'Parakka, James' 'Schlueter, John A.' 'Wang, Hau H.' 'Ward, Brian H.' _publ_contact_author_name 'Dr John A Schlueter' _publ_contact_author_address ; Dr John A Schlueter Chemistry and Materials Science Divisions Argonne National Laboratory Argonne IL 60439 UNITED STATES OF AMERICA ; data_chfsf5RT _database_code_CSD 158389 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethylenedithio)tetrathiafulvalenium 1-pentafluorothio-1,2,2-trifluoro-ethylsulfonate (2:1) ; _chemical_formula_moiety '2(C10 H8 S8)0.5+ (SF5CHFCF2SO3)-' _chemical_formula_sum 'C22 H17 F8 O3 S18' _chemical_formula_weight 1058.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'O' 'O' 0.0106 0.0060 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2233(5) _cell_length_b 11.5932(6) _cell_length_c 17.8088(9) _cell_angle_alpha 93.863(1) _cell_angle_beta 94.543(1) _cell_angle_gamma 103.071(1) _cell_volume 1841.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7010 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 28.28 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1066 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.905 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.013 cm. Coverage of the unique set is over 98% complete to at least 28.28\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART with CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_reflns_number 15961 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8088 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL 5.10 (Sheldrick, 1997)' _computing_molecular_graphics ; SHELXTL 5.10 (Sheldrick, 1997) and ORTEP-II ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered ethylene groups were refined with isotropic atomic displacement parameters that were constrained to be equal within each group. An analogous procedure was used with the disordered anion. All other non-hydrogen atoms were refined independently with anisotropic displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+7.4546P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8088 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1922 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.150 _refine_ls_shift/su_mean 0.008 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.82362(17) 0.12448(12) 0.46119(7) 0.0504(4) Uani 1 1 d . . . S2 S 0.61804(17) -0.10938(13) 0.45932(8) 0.0538(4) Uani 1 1 d . . . S3 S 0.97221(18) 0.08697(13) 0.62789(8) 0.0530(4) Uani 1 1 d . . . S4 S 0.77379(16) -0.15073(12) 0.61877(7) 0.0482(4) Uani 1 1 d . . . S5 S 0.7083(2) 0.17823(15) 0.31281(9) 0.0689(5) Uani 1 1 d . . . S6 S 0.4548(2) -0.09508(16) 0.31309(11) 0.0816(6) Uani 1 1 d . . . S7 S 1.0926(2) 0.08483(13) 0.78670(8) 0.0608(5) Uani 1 1 d . . . S8 S 0.84893(18) -0.19823(13) 0.77481(8) 0.0563(4) Uani 1 1 d . . . C1 C 0.7664(6) -0.0027(5) 0.5075(3) 0.0407(11) Uani 1 1 d . . . C2 C 0.8305(6) -0.0202(5) 0.5763(3) 0.0408(11) Uani 1 1 d . . . C3 C 0.6944(6) 0.0792(5) 0.3818(3) 0.0434(12) Uani 1 1 d . A . C4 C 0.5989(6) -0.0281(5) 0.3822(3) 0.0474(13) Uani 1 1 d . A . C5 C 0.9731(6) 0.0104(5) 0.7091(3) 0.0427(12) Uani 1 1 d . B . C6 C 0.8809(6) -0.0994(5) 0.7054(3) 0.0421(12) Uani 1 1 d . B . C7A C 0.5426(15) 0.1196(11) 0.2515(7) 0.0588(16) Uiso 0.568(12) 1 d P A 1 H7A H 0.4594 0.1419 0.2740 0.071 Uiso 0.568(12) 1 calc PR A 1 H7B H 0.5527 0.1557 0.2041 0.071 Uiso 0.568(12) 1 calc PR A 1 C8A C 0.5066(16) -0.0129(11) 0.2353(7) 0.0588(16) Uiso 0.568(12) 1 d P A 1 H8A H 0.5933 -0.0355 0.2168 0.071 Uiso 0.568(12) 1 calc PR A 1 H8B H 0.4256 -0.0353 0.1951 0.071 Uiso 0.568(12) 1 calc PR A 1 C7B C 0.5916(19) 0.0894(15) 0.2331(9) 0.0588(16) Uiso 0.432(12) 1 d P A 2 H7C H 0.5690 0.1422 0.1961 0.071 Uiso 0.432(12) 1 calc PR A 2 H7D H 0.6478 0.0380 0.2095 0.071 Uiso 0.432(12) 1 calc PR A 2 C8B C 0.4464(19) 0.0136(14) 0.2532(9) 0.0588(16) Uiso 0.432(12) 1 d P A 2 H8C H 0.3890 -0.0242 0.2065 0.071 Uiso 0.432(12) 1 calc PR A 2 H8D H 0.3904 0.0662 0.2757 0.071 Uiso 0.432(12) 1 calc PR A 2 C9A C 1.0181(10) -0.0017(7) 0.8628(4) 0.0490(13) Uiso 0.770(11) 1 d P B 1 H9A1 H 1.0838 0.0247 0.9090 0.059 Uiso 0.770(11) 1 calc PR B 1 H9A2 H 0.9207 0.0123 0.8714 0.059 Uiso 0.770(11) 1 calc PR B 1 C10A C 1.0032(10) -0.1364(7) 0.8441(5) 0.0490(13) Uiso 0.770(11) 1 d P B 1 H10A H 0.9890 -0.1768 0.8898 0.059 Uiso 0.770(11) 1 calc PR B 1 H10B H 1.0947 -0.1490 0.8252 0.059 Uiso 0.770(11) 1 calc PR B 1 C9B C 1.092(3) -0.029(2) 0.8488(14) 0.0490(13) Uiso 0.230(11) 1 d P B 2 H9B1 H 1.1610 -0.0750 0.8322 0.059 Uiso 0.230(11) 1 calc PR B 2 H9B2 H 1.1322 0.0091 0.8986 0.059 Uiso 0.230(11) 1 calc PR B 2 C10B C 0.959(3) -0.108(2) 0.8571(15) 0.0490(13) Uiso 0.230(11) 1 d P B 2 H10C H 0.8952 -0.0636 0.8805 0.059 Uiso 0.230(11) 1 calc PR B 2 H10D H 0.9815 -0.1628 0.8930 0.059 Uiso 0.230(11) 1 calc PR B 2 S11 S 0.96772(17) 0.59352(12) 0.62313(8) 0.0516(4) Uani 1 1 d . . . S12 S 0.77241(17) 0.35516(12) 0.61321(7) 0.0495(4) Uani 1 1 d . . . S13 S 0.81999(17) 0.63000(12) 0.45605(7) 0.0505(4) Uani 1 1 d . . . S14 S 0.61661(18) 0.39570(13) 0.45418(8) 0.0559(4) Uani 1 1 d . . . S15 S 1.10164(18) 0.58555(13) 0.77866(8) 0.0555(4) Uani 1 1 d . . . S16 S 0.86305(18) 0.30093(14) 0.76510(8) 0.0573(4) Uani 1 1 d . . . S17 S 0.7027(2) 0.68520(14) 0.30877(8) 0.0636(5) Uani 1 1 d . . . S18 S 0.4544(2) 0.40862(17) 0.30688(11) 0.0835(7) Uani 1 1 d . . . C11 C 0.8274(6) 0.4865(4) 0.5711(3) 0.0409(11) Uani 1 1 d . . . C12 C 0.7627(6) 0.5025(5) 0.5016(3) 0.0429(12) Uani 1 1 d . . . C13 C 0.9781(6) 0.5135(4) 0.7021(3) 0.0401(11) Uani 1 1 d . C . C14 C 0.8848(6) 0.4031(4) 0.6979(3) 0.0396(11) Uani 1 1 d . C . C15 C 0.6905(6) 0.5843(5) 0.3769(3) 0.0430(12) Uani 1 1 d . D . C16 C 0.5958(6) 0.4769(5) 0.3768(3) 0.0496(14) Uani 1 1 d . D . C17A C 1.0278(9) 0.4972(6) 0.8542(4) 0.0474(13) Uiso 0.770(9) 1 d P C 1 H17A H 1.0934 0.5235 0.9005 0.057 Uiso 0.770(9) 1 calc PR C 1 H17B H 0.9302 0.5107 0.8630 0.057 Uiso 0.770(9) 1 calc PR C 1 C18A C 1.0136(9) 0.3659(7) 0.8360(4) 0.0474(13) Uiso 0.770(9) 1 d P C 1 H18A H 0.9976 0.3257 0.8817 0.057 Uiso 0.770(9) 1 calc PR C 1 H18B H 1.1065 0.3538 0.8186 0.057 Uiso 0.770(9) 1 calc PR C 1 C17B C 1.109(3) 0.471(2) 0.8377(14) 0.0474(13) Uiso 0.230(9) 1 d P C 2 H17C H 1.1660 0.4187 0.8151 0.057 Uiso 0.230(9) 1 calc PR C 2 H17D H 1.1629 0.5055 0.8860 0.057 Uiso 0.230(9) 1 calc PR C 2 C18B C 0.961(3) 0.399(2) 0.8510(14) 0.0474(13) Uiso 0.230(9) 1 d P C 2 H18C H 0.8994 0.4520 0.8667 0.057 Uiso 0.230(9) 1 calc PR C 2 H18D H 0.9735 0.3500 0.8920 0.057 Uiso 0.230(9) 1 calc PR C 2 C19A C 0.5848(16) 0.5932(13) 0.2269(8) 0.0560(16) Uiso 0.497(10) 1 d P D 1 H19A H 0.5618 0.6449 0.1893 0.067 Uiso 0.497(10) 1 calc PR D 1 H19B H 0.6407 0.5409 0.2040 0.067 Uiso 0.497(10) 1 calc PR D 1 C20A C 0.4425(15) 0.5203(12) 0.2492(7) 0.0560(16) Uiso 0.497(10) 1 d P D 1 H20A H 0.3802 0.4846 0.2033 0.067 Uiso 0.497(10) 1 calc PR D 1 H20B H 0.3909 0.5736 0.2745 0.067 Uiso 0.497(10) 1 calc PR D 1 C19B C 0.5437(16) 0.6234(12) 0.2434(8) 0.0560(16) Uiso 0.503(10) 1 d P D 2 H19C H 0.4562 0.6438 0.2624 0.067 Uiso 0.503(10) 1 calc PR D 2 H19D H 0.5581 0.6580 0.1956 0.067 Uiso 0.503(10) 1 calc PR D 2 C20B C 0.5162(15) 0.4884(11) 0.2301(7) 0.0560(16) Uiso 0.503(10) 1 d P D 2 H20C H 0.6084 0.4688 0.2171 0.067 Uiso 0.503(10) 1 calc PR D 2 H20D H 0.4424 0.4617 0.1869 0.067 Uiso 0.503(10) 1 calc PR D 2 S21 S 0.66142(18) 0.20364(15) -0.01944(10) 0.0607(4) Uani 1 1 d . . . F1 F 0.5421(5) 0.0897(3) -0.0518(2) 0.0817(12) Uani 1 1 d . E . F2 F 0.7896(4) 0.3115(4) 0.0109(3) 0.115(2) Uani 1 1 d . E . F3A F 0.6398(8) 0.2618(7) -0.1014(4) 0.0805(18) Uiso 0.628(5) 1 d P E 1 F4A F 0.6824(8) 0.1554(7) 0.0558(5) 0.0817(18) Uiso 0.628(5) 1 d P E 1 F5A F 0.7780(8) 0.1460(6) -0.0546(4) 0.0727(16) Uiso 0.628(5) 1 d P E 1 C21A C 0.5338(10) 0.2963(8) 0.0184(5) 0.0418(17) Uiso 0.628(5) 1 d P E 1 H21A H 0.5595 0.3740 -0.0020 0.050 Uiso 0.628(5) 1 calc PR E 1 F6A F 0.5661(7) 0.3131(6) 0.0908(4) 0.0646(17) Uiso 0.628(5) 1 d P E 1 C22A C 0.3646(9) 0.2421(7) -0.0047(5) 0.0391(16) Uiso 0.628(5) 1 d P E 1 F7A F 0.3176(6) 0.1378(5) 0.0266(3) 0.0542(13) Uiso 0.628(5) 1 d P E 1 F8A F 0.3342(7) 0.2116(5) -0.0782(3) 0.0581(15) Uiso 0.628(5) 1 d P E 1 O1A O 0.1001(9) 0.2821(7) -0.0045(4) 0.0604(17) Uiso 0.628(5) 1 d P E 1 O3A O 0.2701(11) 0.3816(9) 0.0942(6) 0.081(2) Uiso 0.628(5) 1 d P E 1 F3B F 0.6931(14) 0.2330(11) -0.0936(7) 0.0805(18) Uiso 0.37 1 d P E 2 F4B F 0.6303(15) 0.1307(13) 0.0616(8) 0.0817(18) Uiso 0.37 1 d P E 2 F5B F 0.7924(13) 0.1239(10) -0.0186(7) 0.0727(16) Uiso 0.37 1 d P E 2 C21B C 0.5088(16) 0.2766(13) -0.0180(8) 0.0418(17) Uiso 0.37 1 d P E 2 H21B H 0.5456 0.3613 -0.0242 0.050 Uiso 0.372(5) 1 calc PR E 2 F6B F 0.3991(13) 0.2159(10) -0.0886(6) 0.0646(17) Uiso 0.37 1 d P E 2 C22B C 0.4064(15) 0.2632(12) 0.0374(8) 0.0391(16) Uiso 0.37 1 d P E 2 F7B F 0.3467(11) 0.1565(9) 0.0556(6) 0.0542(13) Uiso 0.37 1 d P E 2 F8B F 0.5136(12) 0.3087(10) 0.1013(6) 0.0581(15) Uiso 0.37 1 d P E 2 O1B O 0.1220(15) 0.2458(12) -0.0196(7) 0.0604(17) Uiso 0.37 1 d P E 2 O3B O 0.239(2) 0.3468(15) 0.1042(10) 0.081(2) Uiso 0.37 1 d P E 2 S22 S 0.24819(16) 0.34299(15) 0.01945(9) 0.0543(4) Uani 1 1 d . . . O2 O 0.3051(5) 0.4385(4) -0.0247(4) 0.0877(17) Uani 1 1 d . E . 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 S1 0.0598(9) 0.0433(8) 0.0370(7) 0.0071(6) -0.0108(6) -0.0067(6) S2 0.0610(9) 0.0468(8) 0.0412(7) 0.0118(6) -0.0144(6) -0.0093(7) S3 0.0630(9) 0.0479(8) 0.0363(7) 0.0078(6) -0.0117(6) -0.0071(7) S4 0.0569(8) 0.0452(8) 0.0329(6) 0.0058(5) -0.0104(6) -0.0038(6) S5 0.0937(13) 0.0505(9) 0.0498(8) 0.0191(7) -0.0202(8) -0.0044(9) S6 0.0816(12) 0.0654(11) 0.0728(11) 0.0211(9) -0.0462(10) -0.0210(9) S7 0.0802(11) 0.0436(8) 0.0458(8) 0.0072(6) -0.0286(7) -0.0016(7) S8 0.0650(9) 0.0501(8) 0.0431(7) 0.0144(6) -0.0200(7) -0.0028(7) C1 0.042(3) 0.043(3) 0.031(2) 0.004(2) -0.001(2) 0.000(2) C2 0.046(3) 0.045(3) 0.030(2) 0.004(2) -0.003(2) 0.008(2) C3 0.052(3) 0.040(3) 0.035(2) 0.006(2) -0.009(2) 0.006(2) C4 0.052(3) 0.042(3) 0.041(3) 0.010(2) -0.013(2) -0.002(2) C5 0.049(3) 0.039(3) 0.036(3) 0.002(2) -0.012(2) 0.008(2) C6 0.050(3) 0.044(3) 0.032(2) 0.005(2) -0.007(2) 0.015(2) S11 0.0636(9) 0.0428(8) 0.0382(7) 0.0099(6) -0.0150(6) -0.0043(7) S12 0.0625(9) 0.0432(7) 0.0331(6) 0.0076(5) -0.0114(6) -0.0037(6) S13 0.0592(9) 0.0450(8) 0.0362(7) 0.0095(6) -0.0148(6) -0.0060(6) S14 0.0663(9) 0.0463(8) 0.0415(7) 0.0118(6) -0.0154(7) -0.0105(7) S15 0.0694(10) 0.0424(8) 0.0442(7) 0.0051(6) -0.0232(7) 0.0008(7) S16 0.0668(10) 0.0524(9) 0.0418(7) 0.0168(6) -0.0156(7) -0.0054(7) S17 0.0847(12) 0.0503(9) 0.0448(8) 0.0173(7) -0.0207(8) -0.0015(8) S18 0.0875(13) 0.0670(11) 0.0682(11) 0.0170(9) -0.0463(10) -0.0246(10) C11 0.047(3) 0.038(3) 0.032(2) 0.006(2) -0.005(2) 0.003(2) C12 0.049(3) 0.045(3) 0.030(2) 0.006(2) -0.006(2) 0.003(2) C13 0.048(3) 0.037(3) 0.032(2) 0.004(2) -0.005(2) 0.007(2) C14 0.046(3) 0.041(3) 0.029(2) 0.003(2) -0.005(2) 0.007(2) C15 0.050(3) 0.040(3) 0.033(2) 0.005(2) -0.010(2) 0.003(2) C16 0.054(3) 0.044(3) 0.041(3) 0.007(2) -0.017(2) -0.002(3) S21 0.0494(9) 0.0591(10) 0.0700(10) -0.0106(8) 0.0115(7) 0.0080(7) F1 0.080(3) 0.060(2) 0.094(3) -0.008(2) 0.009(2) -0.004(2) F2 0.050(2) 0.083(3) 0.194(5) -0.061(3) 0.001(3) 0.006(2) S22 0.0418(8) 0.0619(9) 0.0570(9) 0.0067(7) -0.0071(6) 0.0114(7) O2 0.056(3) 0.057(3) 0.151(5) 0.034(3) 0.002(3) 0.012(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 S1 C1 1.736(5) . ? S1 C3 1.745(5) . ? S2 C4 1.737(5) . ? S2 C1 1.745(5) . ? S3 C2 1.737(5) . ? S3 C5 1.748(5) . ? S4 C2 1.730(5) . ? S4 C6 1.755(5) . ? S5 C3 1.730(5) . ? S5 C7A 1.776(12) . ? S5 C7B 1.815(15) . ? S6 C8B 1.716(15) . ? S6 C4 1.740(5) . ? S6 C8A 1.770(12) . ? S7 C5 1.743(5) . ? S7 C9B 1.78(2) . ? S7 C9A 1.826(8) . ? S8 C6 1.739(5) . ? S8 C10A 1.789(8) . ? S8 C10B 1.83(3) . ? C1 C2 1.366(7) . ? C3 C4 1.353(7) . ? C5 C6 1.355(7) . ? C7A C8A 1.499(18) . ? C7B C8B 1.51(2) . ? C9A C10A 1.547(12) . ? C9B C10B 1.38(4) . ? S11 C11 1.732(5) . ? S11 C13 1.745(5) . ? S12 C11 1.733(5) . ? S12 C14 1.743(5) . ? S13 C12 1.732(5) . ? S13 C15 1.743(5) . ? S14 C12 1.728(5) . ? S14 C16 1.742(5) . ? S15 C13 1.739(5) . ? S15 C17B 1.76(2) . ? S15 C17A 1.827(7) . ? S16 C14 1.731(5) . ? S16 C18A 1.792(7) . ? S16 C18B 1.88(2) . ? S17 C15 1.734(5) . ? S17 C19B 1.778(13) . ? S17 C19A 1.860(13) . ? S18 C20A 1.723(12) . ? S18 C16 1.738(5) . ? S18 C20B 1.762(12) . ? C11 C12 1.374(7) . ? C13 C14 1.364(7) . ? C15 C16 1.350(7) . ? C17A C18A 1.508(11) . ? C17B C18B 1.48(4) . ? C19A C20A 1.490(19) . ? C19B C20B 1.527(19) . ? S21 F3B 1.423(13) . ? S21 F4A 1.501(9) . ? S21 F5A 1.540(7) . ? S21 F2 1.547(4) . ? S21 F1 1.558(4) . ? S21 F3A 1.665(8) . ? S21 F5B 1.678(12) . ? S21 F4B 1.732(14) . ? S21 C21B 1.800(15) . ? S21 C21A 1.896(9) . ? C21A F6A 1.291(11) . ? C21A C22A 1.556(12) . ? C22A F8A 1.324(10) . ? C22A F7A 1.361(10) . ? C22A S22 1.811(8) . ? C21B C22B 1.412(19) . ? C21B F6B 1.568(18) . ? C22B F7B 1.309(16) . ? C22B F8B 1.433(17) . ? C22B S22 1.914(14) . ? S22 O1A 1.406(8) . ? S22 O3A 1.360(11) . ? S22 O1B 1.510(13) . ? S22 O3B 1.517(18) . ? S22 O2 1.428(5) . ? 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 C1 S1 C3 96.0(2) . . ? C4 S2 C1 95.2(2) . . ? C2 S3 C5 95.3(2) . . ? C2 S4 C6 95.5(2) . . ? C3 S5 C7A 102.6(4) . . ? C3 S5 C7B 102.3(5) . . ? C8B S6 C4 104.2(5) . . ? C4 S6 C8A 101.4(4) . . ? C5 S7 C9B 102.5(8) . . ? C5 S7 C9A 101.0(3) . . ? C6 S8 C10A 101.6(3) . . ? C6 S8 C10B 101.1(9) . . ? C2 C1 S1 123.7(4) . . ? C2 C1 S2 121.5(4) . . ? S1 C1 S2 114.8(3) . . ? C1 C2 S4 122.0(4) . . ? C1 C2 S3 122.7(4) . . ? S4 C2 S3 115.3(3) . . ? C4 C3 S5 129.0(4) . . ? C4 C3 S1 116.1(4) . . ? S5 C3 S1 114.9(3) . . ? C3 C4 S2 117.9(4) . . ? C3 C4 S6 126.9(4) . . ? S2 C4 S6 115.3(3) . . ? C6 C5 S7 127.0(4) . . ? C6 C5 S3 117.0(4) . . ? S7 C5 S3 115.9(3) . . ? C5 C6 S8 129.7(4) . . ? C5 C6 S4 116.4(4) . . ? S8 C6 S4 113.9(3) . . ? C8A C7A S5 114.3(10) . . ? C7A C8A S6 115.3(10) . . ? C8B C7B S5 114.5(13) . . ? C7B C8B S6 118.2(13) . . ? C10A C9A S7 111.8(6) . . ? C9A C10A S8 111.3(6) . . ? C10B C9B S7 120(2) . . ? C9B C10B S8 120(2) . . ? C11 S11 C13 95.9(2) . . ? C11 S12 C14 95.8(2) . . ? C12 S13 C15 95.4(2) . . ? C12 S14 C16 95.1(2) . . ? C13 S15 C17B 103.1(8) . . ? C13 S15 C17A 100.2(3) . . ? C14 S16 C18A 102.5(3) . . ? C14 S16 C18B 100.0(8) . . ? C15 S17 C19B 103.5(5) . . ? C15 S17 C19A 101.6(5) . . ? C20A S18 C16 103.5(5) . . ? C16 S18 C20B 99.8(5) . . ? C12 C11 S11 123.5(4) . . ? C12 C11 S12 121.4(4) . . ? S11 C11 S12 115.0(3) . . ? C11 C12 S14 121.7(4) . . ? C11 C12 S13 122.7(4) . . ? S14 C12 S13 115.6(3) . . ? C14 C13 S15 127.3(4) . . ? C14 C13 S11 116.4(4) . . ? S15 C13 S11 116.2(3) . . ? C13 C14 S16 129.1(4) . . ? C13 C14 S12 116.6(4) . . ? S16 C14 S12 114.3(3) . . ? C16 C15 S17 129.1(4) . . ? C16 C15 S13 116.4(4) . . ? S17 C15 S13 114.5(3) . . ? C15 C16 S18 127.0(4) . . ? C15 C16 S14 117.4(4) . . ? S18 C16 S14 115.6(3) . . ? C18A C17A S15 112.6(6) . . ? C17A C18A S16 112.7(6) . . ? C18B C17B S15 113.9(19) . . ? C17B C18B S16 113.0(19) . . ? C20A C19A S17 112.3(10) . . ? C19A C20A S18 117.6(11) . . ? C20B C19B S17 112.1(10) . . ? C19B C20B S18 115.6(10) . . ? F4A S21 F5A 94.0(4) . . ? F3B S21 F2 87.6(6) . . ? F4A S21 F2 87.0(4) . . ? F5A S21 F2 88.6(3) . . ? F3B S21 F1 91.1(5) . . ? F4A S21 F1 92.6(4) . . ? F5A S21 F1 86.9(3) . . ? F2 S21 F1 175.4(3) . . ? F4A S21 F3A 178.0(4) . . ? F5A S21 F3A 87.0(4) . . ? F2 S21 F3A 91.4(4) . . ? F1 S21 F3A 89.1(3) . . ? F3B S21 F5B 89.3(6) . . ? F2 S21 F5B 86.4(4) . . ? F1 S21 F5B 89.2(4) . . ? F3B S21 F4B 164.3(7) . . ? F2 S21 F4B 101.2(5) . . ? F1 S21 F4B 79.1(5) . . ? F5B S21 F4B 78.5(6) . . ? F3B S21 C21B 94.0(7) . . ? F2 S21 C21B 98.2(5) . . ? F1 S21 C21B 86.3(5) . . ? F5B S21 C21B 174.5(6) . . ? F4B S21 C21B 97.5(7) . . ? F4A S21 C21A 91.6(4) . . ? F5A S21 C21A 171.3(4) . . ? F2 S21 C21A 85.0(3) . . ? F1 S21 C21A 99.6(3) . . ? F3A S21 C21A 87.2(4) . . ? F6A C21A C22A 112.8(7) . . ? F6A C21A S21 106.9(6) . . ? C22A C21A S21 114.0(6) . . ? F8A C22A F7A 103.4(7) . . ? F8A C22A C21A 112.8(7) . . ? F7A C22A C21A 111.2(7) . . ? F8A C22A S22 106.3(6) . . ? F7A C22A S22 109.8(6) . . ? C21A C22A S22 112.8(6) . . ? C22B C21B F6B 98.9(11) . . ? C22B C21B S21 123.8(11) . . ? F6B C21B S21 104.4(9) . . ? F7B C22B C21B 119.2(13) . . ? F7B C22B F8B 101.7(11) . . ? C21B C22B F8B 96.7(11) . . ? F7B C22B S22 107.7(9) . . ? C21B C22B S22 113.8(10) . . ? F8B C22B S22 117.2(9) . . ? O3A S22 O1A 113.5(5) . . ? O3A S22 O2 110.1(5) . . ? O1A S22 O2 113.8(4) . . ? O2 S22 O1B 115.8(6) . . ? O2 S22 O3B 128.4(7) . . ? O1B S22 O3B 109.3(8) . . ? O3A S22 C22A 112.0(5) . . ? O1A S22 C22A 106.3(4) . . ? O2 S22 C22A 100.4(3) . . ? O2 S22 C22B 106.2(5) . . ? O1B S22 C22B 103.2(7) . . ? O3B S22 C22B 86.0(8) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.887 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.093 data_chfsf5LT _database_code_CSD 158390 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethylenedithio)tetrathiafulvalenium 1-pentafluorothio-1,2,2-trifluoro-ethylsulfonate (2:1) ; _chemical_formula_moiety '2(C10 H8 S8)0.5+ (SF5CHFCF2SO3)-' _chemical_formula_sum 'C22 H17 F8 O3 S18' _chemical_formula_weight 1058.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'O' 'O' 0.0106 0.0060 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2462(4) _cell_length_b 11.3610(5) _cell_length_c 17.7145(8) _cell_angle_alpha 94.1210(10) _cell_angle_beta 94.9140(10) _cell_angle_gamma 103.1390(10) _cell_volume 1797.45(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 28.30 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1066 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.903 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.013 cm. Coverage of the unique set is over 98% complete to at least 28.28\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART with CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_reflns_number 16157 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8089 _reflns_number_gt 6797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL 5.10 (Sheldrick, 1997)' _computing_molecular_graphics ; SHELXTL 5.10 (Sheldrick, 1997) and ORTEP-II ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two components of the disordered anion were refined with isotropic atomic displacement parameters for those atoms that required split positions. Atoms S21, S22, F1, F2, and O2 were common (within experimental resolution) for the two disordered components, and these were refined with anisotropic displacement parameters, as were the non-hydrogen atoms of the radical cations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+5.9677P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8089 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.81987(10) 0.12458(8) 0.45931(5) 0.02507(19) Uani 1 1 d . . . S2 S 0.61805(10) -0.11715(8) 0.45488(5) 0.02506(19) Uani 1 1 d . . . S3 S 0.97338(10) 0.08416(8) 0.62587(5) 0.02531(19) Uani 1 1 d . . . S4 S 0.77293(9) -0.15923(7) 0.61588(4) 0.02078(18) Uani 1 1 d . . . S5 S 0.71209(11) 0.17610(8) 0.30751(5) 0.0296(2) Uani 1 1 d . . . S6 S 0.47296(12) -0.11430(9) 0.30027(6) 0.0370(3) Uani 1 1 d . . . S7 S 1.10539(11) 0.07713(8) 0.78381(5) 0.0272(2) Uani 1 1 d . . . S8 S 0.85550(10) -0.21049(8) 0.77175(5) 0.02420(19) Uani 1 1 d . . . C1 C 0.7673(4) -0.0086(3) 0.50368(18) 0.0198(6) Uani 1 1 d . . . C2 C 0.8323(4) -0.0261(3) 0.57259(18) 0.0195(6) Uani 1 1 d . . . C3 C 0.6990(4) 0.0720(3) 0.37581(18) 0.0204(6) Uani 1 1 d . . . C4 C 0.6073(4) -0.0391(3) 0.37368(19) 0.0233(7) Uani 1 1 d . . . C5 C 0.9810(4) 0.0023(3) 0.70628(18) 0.0203(6) Uani 1 1 d . . . C6 C 0.8868(4) -0.1092(3) 0.70170(18) 0.0193(6) Uani 1 1 d . . . C7 C 0.5831(5) 0.0916(4) 0.2289(2) 0.0336(9) Uani 1 1 d . . . H7A H 0.5552 0.1499 0.1947 0.040 Uiso 1 1 calc R . . H7B H 0.6351 0.0395 0.1995 0.040 Uiso 1 1 calc R . . C8 C 0.4430(4) 0.0133(4) 0.2517(2) 0.0323(8) Uani 1 1 d . . . H8A H 0.3724 -0.0171 0.2055 0.039 Uiso 1 1 calc R . . H8B H 0.3958 0.0636 0.2853 0.039 Uiso 1 1 calc R . . C9 C 1.0252(4) -0.0065(3) 0.86012(19) 0.0289(8) Uani 1 1 d . . . H9A H 1.0909 0.0219 0.9081 0.035 Uiso 1 1 calc R . . H9B H 0.9269 0.0112 0.8670 0.035 Uiso 1 1 calc R . . C10 C 1.0054(4) -0.1417(3) 0.84453(18) 0.0235(7) Uani 1 1 d . . . H10A H 0.9857 -0.1802 0.8922 0.028 Uiso 1 1 calc R . . H10B H 1.0997 -0.1582 0.8288 0.028 Uiso 1 1 calc R . . S11 S 0.97294(10) 0.59070(8) 0.62353(5) 0.02392(19) Uani 1 1 d . . . S12 S 0.77462(9) 0.34705(8) 0.61265(4) 0.02174(18) Uani 1 1 d . . . S13 S 0.82337(10) 0.62916(7) 0.45571(5) 0.02326(19) Uani 1 1 d . . . S14 S 0.61981(10) 0.38890(8) 0.45226(5) 0.0262(2) Uani 1 1 d . . . S15 S 1.11400(10) 0.57860(8) 0.77883(5) 0.02528(19) Uani 1 1 d . . . S16 S 0.86935(10) 0.29020(8) 0.76472(5) 0.02500(19) Uani 1 1 d . . . S17 S 0.71786(11) 0.67982(8) 0.30368(5) 0.0264(2) Uani 1 1 d . . . S18 S 0.47456(12) 0.39191(10) 0.29752(6) 0.0381(3) Uani 1 1 d . . . C11 C 0.8338(4) 0.4802(3) 0.56997(17) 0.0194(6) Uani 1 1 d . . . C12 C 0.7692(4) 0.4966(3) 0.50021(18) 0.0205(6) Uani 1 1 d . . . C13 C 0.9861(4) 0.5066(3) 0.70180(17) 0.0191(6) Uani 1 1 d . . . C14 C 0.8930(4) 0.3947(3) 0.69713(17) 0.0185(6) Uani 1 1 d . . . C15 C 0.7029(4) 0.5768(3) 0.37245(18) 0.0201(6) Uani 1 1 d . . . C16 C 0.6100(4) 0.4658(3) 0.37091(18) 0.0234(7) Uani 1 1 d . . . C17 C 1.0314(5) 0.4960(4) 0.8548(2) 0.0301(8) Uani 1 1 d . . . H17A H 1.0953 0.5254 0.9033 0.036 Uiso 1 1 calc R . . H17B H 0.9323 0.5130 0.8604 0.036 Uiso 1 1 calc R . . C18 C 1.0138(4) 0.3612(3) 0.84005(19) 0.0250(7) Uani 1 1 d . . . H18A H 0.9906 0.3230 0.8874 0.030 Uiso 1 1 calc R . . H18B H 1.1100 0.3455 0.8267 0.030 Uiso 1 1 calc R . . C19 C 0.5853(4) 0.5972(3) 0.2257(2) 0.0292(8) Uani 1 1 d . . . H19A H 0.5582 0.6558 0.1915 0.035 Uiso 1 1 calc R . . H19B H 0.6339 0.5428 0.1959 0.035 Uiso 1 1 calc R . . C20 C 0.4445(4) 0.5223(4) 0.2513(2) 0.0324(8) Uani 1 1 d . . . H20A H 0.3694 0.4943 0.2066 0.039 Uiso 1 1 calc R . . H20B H 0.4034 0.5742 0.2870 0.039 Uiso 1 1 calc R . . S21 S 0.65978(10) 0.20141(8) -0.02649(5) 0.0260(2) Uani 1 1 d . . . F1 F 0.5381(3) 0.0830(2) -0.05613(14) 0.0380(5) Uani 1 1 d . A . F2 F 0.7904(3) 0.3155(2) 0.00113(17) 0.0493(7) Uani 1 1 d . A . F3A F 0.6363(4) 0.2582(3) -0.1066(2) 0.0375(8) Uiso 0.723(4) 1 d P A 1 F4A F 0.6883(4) 0.1478(4) 0.0496(2) 0.0405(9) Uiso 0.723(4) 1 d P A 1 F5A F 0.7762(4) 0.1396(3) -0.0618(2) 0.0350(8) Uiso 0.723(4) 1 d P A 1 C21A C 0.5345(5) 0.2942(4) 0.0138(3) 0.0198(9) Uiso 0.723(4) 1 d P A 1 H21A H 0.5568 0.3753 -0.0068 0.024 Uiso 0.723(4) 1 calc PR A 1 F6A F 0.5689(4) 0.3109(3) 0.09059(17) 0.0288(7) Uiso 0.723(4) 1 d P A 1 C22A C 0.3670(5) 0.2376(4) -0.0037(3) 0.0198(9) Uiso 0.723(4) 1 d P A 1 F7A F 0.3262(3) 0.1361(3) 0.03288(18) 0.0282(7) Uiso 0.723(4) 1 d P A 1 F8A F 0.3343(4) 0.2048(3) -0.07959(17) 0.0283(7) Uiso 0.723(4) 1 d P A 1 O1A O 0.1029(5) 0.2709(4) -0.0028(2) 0.0306(9) Uiso 0.723(4) 1 d P A 1 O3A O 0.2802(5) 0.3753(5) 0.1002(3) 0.0420(11) Uiso 0.723(4) 1 d P A 1 F3B F 0.6763(11) 0.2255(9) -0.1089(5) 0.0375(8) Uiso 0.28 1 d P A 2 F4B F 0.6416(12) 0.1476(10) 0.0597(6) 0.0405(9) Uiso 0.28 1 d P A 2 F5B F 0.7884(10) 0.1249(8) -0.0300(5) 0.0350(8) Uiso 0.28 1 d P A 2 C21B C 0.4981(13) 0.2705(11) -0.0281(7) 0.0198(9) Uiso 0.28 1 d P A 2 H21B H 0.5350 0.3576 -0.0371 0.024 Uiso 0.277(4) 1 calc PR A 2 F6B F 0.3977(10) 0.2158(7) -0.0906(5) 0.0288(7) Uiso 0.28 1 d P A 2 C22B C 0.4128(13) 0.2682(11) 0.0413(7) 0.0198(9) Uiso 0.28 1 d P A 2 F7B F 0.3597(9) 0.1559(8) 0.0610(5) 0.0282(7) Uiso 0.28 1 d P A 2 F8B F 0.5070(10) 0.3280(7) 0.1019(4) 0.0283(7) Uiso 0.28 1 d P A 2 O1B O 0.1256(12) 0.2371(10) -0.0140(6) 0.0306(9) Uiso 0.28 1 d P A 2 O3B O 0.2268(15) 0.3698(12) 0.1038(7) 0.0420(11) Uiso 0.28 1 d P A 2 S22 S 0.25016(10) 0.34173(8) 0.02140(5) 0.02563(19) Uani 1 1 d . . . O2 O 0.3019(3) 0.4384(2) -0.02578(18) 0.0381(7) Uani 1 1 d . A . 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 S1 0.0350(5) 0.0177(4) 0.0171(4) 0.0026(3) -0.0072(3) -0.0017(3) S2 0.0283(4) 0.0226(4) 0.0184(4) 0.0073(3) -0.0059(3) -0.0047(3) S3 0.0348(5) 0.0188(4) 0.0165(4) 0.0031(3) -0.0073(3) -0.0024(3) S4 0.0241(4) 0.0201(4) 0.0144(4) 0.0029(3) -0.0035(3) -0.0007(3) S5 0.0424(5) 0.0199(4) 0.0215(4) 0.0079(3) -0.0075(4) -0.0009(4) S6 0.0373(5) 0.0320(5) 0.0303(5) 0.0112(4) -0.0187(4) -0.0101(4) S7 0.0366(5) 0.0183(4) 0.0207(4) 0.0030(3) -0.0123(3) -0.0006(3) S8 0.0267(4) 0.0228(4) 0.0189(4) 0.0061(3) -0.0066(3) -0.0007(3) C1 0.0214(16) 0.0187(16) 0.0166(15) 0.0022(12) -0.0013(12) 0.0001(12) C2 0.0234(16) 0.0174(15) 0.0152(14) 0.0012(11) -0.0025(12) 0.0017(12) C3 0.0230(16) 0.0211(16) 0.0151(14) 0.0022(12) -0.0038(12) 0.0028(13) C4 0.0231(16) 0.0233(17) 0.0190(15) 0.0052(13) -0.0079(13) -0.0015(13) C5 0.0268(17) 0.0183(15) 0.0149(14) 0.0024(12) -0.0040(12) 0.0056(13) C6 0.0215(16) 0.0203(16) 0.0156(14) 0.0021(12) -0.0029(12) 0.0056(13) C7 0.044(2) 0.033(2) 0.0206(17) 0.0054(15) -0.0074(16) 0.0034(17) C8 0.032(2) 0.037(2) 0.0260(18) 0.0035(15) -0.0050(15) 0.0077(17) C9 0.037(2) 0.0302(19) 0.0163(16) -0.0049(14) 0.0000(14) 0.0037(16) C10 0.0227(16) 0.0271(18) 0.0165(15) 0.0060(13) -0.0062(12) -0.0011(13) S11 0.0318(5) 0.0184(4) 0.0173(4) 0.0030(3) -0.0076(3) 0.0004(3) S12 0.0249(4) 0.0222(4) 0.0135(4) 0.0034(3) -0.0034(3) -0.0023(3) S13 0.0307(4) 0.0175(4) 0.0170(4) 0.0025(3) -0.0078(3) -0.0003(3) S14 0.0276(4) 0.0269(4) 0.0172(4) 0.0074(3) -0.0059(3) -0.0063(3) S15 0.0327(5) 0.0180(4) 0.0208(4) 0.0013(3) -0.0112(3) 0.0024(3) S16 0.0270(4) 0.0260(4) 0.0173(4) 0.0075(3) -0.0051(3) -0.0025(3) S17 0.0359(5) 0.0214(4) 0.0185(4) 0.0064(3) -0.0064(3) 0.0016(4) S18 0.0365(5) 0.0366(5) 0.0277(5) 0.0101(4) -0.0170(4) -0.0138(4) C11 0.0227(16) 0.0188(16) 0.0142(14) 0.0005(11) -0.0028(12) 0.0021(12) C12 0.0219(16) 0.0216(16) 0.0156(14) 0.0023(12) -0.0019(12) 0.0017(13) C13 0.0221(16) 0.0205(16) 0.0134(14) 0.0000(12) -0.0061(12) 0.0057(13) C14 0.0207(15) 0.0223(16) 0.0133(14) 0.0013(12) 0.0002(11) 0.0072(13) C15 0.0212(16) 0.0231(17) 0.0142(14) 0.0040(12) -0.0033(12) 0.0028(13) C16 0.0247(17) 0.0257(17) 0.0159(15) 0.0056(13) -0.0050(12) -0.0007(14) C17 0.038(2) 0.034(2) 0.0174(16) -0.0012(14) -0.0017(14) 0.0091(16) C18 0.0275(18) 0.0267(18) 0.0180(15) 0.0045(13) -0.0047(13) 0.0024(14) C19 0.037(2) 0.0285(19) 0.0184(16) 0.0019(14) -0.0099(14) 0.0059(16) C20 0.0302(19) 0.042(2) 0.0246(18) 0.0004(16) -0.0080(15) 0.0126(17) S21 0.0223(4) 0.0258(4) 0.0292(4) -0.0036(3) 0.0035(3) 0.0055(3) F1 0.0325(12) 0.0330(13) 0.0426(13) -0.0025(10) 0.0053(10) -0.0033(10) F2 0.0304(13) 0.0353(14) 0.0737(19) -0.0210(13) -0.0005(12) 0.0005(10) S22 0.0214(4) 0.0308(5) 0.0255(4) 0.0021(3) -0.0002(3) 0.0089(3) O2 0.0305(14) 0.0264(14) 0.0585(19) 0.0114(13) 0.0031(13) 0.0075(11) _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 S1 C1 1.745(3) . ? S1 C3 1.755(3) . ? S2 C1 1.744(3) . ? S2 C4 1.751(3) . ? S3 C2 1.743(3) . ? S3 C5 1.761(3) . ? S4 C2 1.743(3) . ? S4 C6 1.753(3) . ? S5 C3 1.744(3) . ? S5 C7 1.813(4) . ? S6 C4 1.745(3) . ? S6 C8 1.800(4) . ? S7 C5 1.746(3) . ? S7 C9 1.821(4) . ? S8 C6 1.750(3) . ? S8 C10 1.803(3) . ? C1 C2 1.362(4) . ? C3 C4 1.347(5) . ? C5 C6 1.356(5) . ? C7 C8 1.500(6) . ? C9 C10 1.508(5) . ? S11 C11 1.737(3) . ? S11 C13 1.751(3) . ? S12 C11 1.737(3) . ? S12 C14 1.750(3) . ? S13 C12 1.743(3) . ? S13 C15 1.750(3) . ? S14 C12 1.734(3) . ? S14 C16 1.744(3) . ? S15 C13 1.747(3) . ? S15 C17 1.819(4) . ? S16 C14 1.739(3) . ? S16 C18 1.807(3) . ? S17 C15 1.742(3) . ? S17 C19 1.815(4) . ? S18 C16 1.746(3) . ? S18 C20 1.806(4) . ? C11 C12 1.369(4) . ? C13 C14 1.356(5) . ? C15 C16 1.352(5) . ? C17 C18 1.504(5) . ? C19 C20 1.510(6) . ? S21 F3B 1.519(9) . ? S21 F4A 1.546(4) . ? S21 F5A 1.562(3) . ? S21 F1 1.568(2) . ? S21 F2 1.573(2) . ? S21 F3A 1.618(4) . ? S21 F5B 1.628(9) . ? S21 F4B 1.693(10) . ? S21 C21B 1.839(12) . ? S21 C21A 1.884(5) . ? C21A F6A 1.360(5) . ? C21A C22A 1.531(6) . ? C22A F7A 1.358(5) . ? C22A F8A 1.359(5) . ? C22A S22 1.830(5) . ? O1A S22 1.428(4) . ? O3A S22 1.408(5) . ? C21B F6B 1.391(14) . ? C21B C22B 1.515(16) . ? C22B F7B 1.342(14) . ? C22B F8B 1.356(14) . ? C22B S22 1.898(12) . ? S22 O1B 1.510(11) . ? S22 O3B 1.516(13) . ? S22 O2 1.447(3) . ? 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 C1 S1 C3 95.25(15) . . ? C1 S2 C4 95.39(16) . . ? C2 S3 C5 95.54(15) . . ? C2 S4 C6 95.58(15) . . ? C3 S5 C7 102.40(17) . . ? C4 S6 C8 99.89(17) . . ? C5 S7 C9 100.01(16) . . ? C6 S8 C10 101.61(16) . . ? C2 C1 S2 121.7(3) . . ? C2 C1 S1 123.4(3) . . ? S2 C1 S1 114.84(18) . . ? C1 C2 S4 121.8(3) . . ? C1 C2 S3 123.0(3) . . ? S4 C2 S3 115.12(18) . . ? C4 C3 S5 129.1(3) . . ? C4 C3 S1 117.0(2) . . ? S5 C3 S1 113.87(18) . . ? C3 C4 S6 127.8(3) . . ? C3 C4 S2 117.0(2) . . ? S6 C4 S2 115.12(19) . . ? C6 C5 S7 127.7(2) . . ? C6 C5 S3 116.6(2) . . ? S7 C5 S3 115.67(19) . . ? C5 C6 S8 129.0(2) . . ? C5 C6 S4 117.1(2) . . ? S8 C6 S4 113.84(18) . . ? C8 C7 S5 114.7(3) . . ? C7 C8 S6 113.9(3) . . ? C10 C9 S7 112.7(2) . . ? C9 C10 S8 113.4(2) . . ? C11 S11 C13 95.56(15) . . ? C11 S12 C14 95.46(15) . . ? C12 S13 C15 95.12(15) . . ? C12 S14 C16 95.30(16) . . ? C13 S15 C17 99.54(17) . . ? C14 S16 C18 102.52(16) . . ? C15 S17 C19 102.66(16) . . ? C16 S18 C20 99.26(17) . . ? C12 C11 S11 123.4(3) . . ? C12 C11 S12 121.3(3) . . ? S11 C11 S12 115.33(18) . . ? C11 C12 S14 121.8(3) . . ? C11 C12 S13 122.9(3) . . ? S14 C12 S13 115.20(18) . . ? C14 C13 S15 127.1(2) . . ? C14 C13 S11 116.7(2) . . ? S15 C13 S11 116.11(19) . . ? C13 C14 S16 129.3(2) . . ? C13 C14 S12 116.9(2) . . ? S16 C14 S12 113.81(18) . . ? C16 C15 S17 129.3(3) . . ? C16 C15 S13 116.8(2) . . ? S17 C15 S13 113.90(18) . . ? C15 C16 S14 117.1(2) . . ? C15 C16 S18 127.2(3) . . ? S14 C16 S18 115.58(19) . . ? C18 C17 S15 112.4(3) . . ? C17 C18 S16 113.8(2) . . ? C20 C19 S17 113.5(3) . . ? C19 C20 S18 113.0(3) . . ? F4A S21 F5A 90.28(19) . . ? F3B S21 F1 88.1(4) . . ? F4A S21 F1 90.27(18) . . ? F5A S21 F1 87.38(16) . . ? F3B S21 F2 90.6(4) . . ? F4A S21 F2 89.45(19) . . ? F5A S21 F2 88.53(16) . . ? F1 S21 F2 175.91(15) . . ? F4A S21 F3A 177.92(19) . . ? F5A S21 F3A 88.06(18) . . ? F1 S21 F3A 90.89(16) . . ? F2 S21 F3A 89.27(18) . . ? F3B S21 F5B 88.8(5) . . ? F1 S21 F5B 89.7(3) . . ? F2 S21 F5B 86.4(3) . . ? F3B S21 F4B 169.3(5) . . ? F1 S21 F4B 84.3(4) . . ? F2 S21 F4B 96.5(4) . . ? F5B S21 F4B 83.6(5) . . ? F3B S21 C21B 90.2(5) . . ? F1 S21 C21B 83.2(4) . . ? F2 S21 C21B 100.7(4) . . ? F5B S21 C21B 172.8(5) . . ? F4B S21 C21B 96.3(5) . . ? F4A S21 C21A 93.2(2) . . ? F5A S21 C21A 173.0(2) . . ? F1 S21 C21A 98.71(17) . . ? F2 S21 C21A 85.38(17) . . ? F3A S21 C21A 88.33(19) . . ? F6A C21A C22A 108.7(4) . . ? F6A C21A S21 107.7(3) . . ? C22A C21A S21 115.0(3) . . ? F7A C22A F8A 107.6(4) . . ? F7A C22A C21A 111.0(4) . . ? F8A C22A C21A 109.4(4) . . ? F7A C22A S22 108.7(3) . . ? F8A C22A S22 106.6(3) . . ? C21A C22A S22 113.4(3) . . ? F6B C21B C22B 108.0(9) . . ? F6B C21B S21 108.3(8) . . ? C22B C21B S21 118.8(9) . . ? F7B C22B F8B 105.6(9) . . ? F7B C22B C21B 113.4(10) . . ? F8B C22B C21B 108.9(10) . . ? F7B C22B S22 108.7(8) . . ? F8B C22B S22 111.4(8) . . ? C21B C22B S22 108.9(8) . . ? O3A S22 O1A 115.0(2) . . ? O3A S22 O2 114.7(2) . . ? O1A S22 O2 114.1(2) . . ? O2 S22 O1B 117.0(4) . . ? O2 S22 O3B 120.9(5) . . ? O1B S22 O3B 109.1(6) . . ? O3A S22 C22A 107.6(2) . . ? O1A S22 C22A 102.7(2) . . ? O2 S22 C22A 100.68(19) . . ? O2 S22 C22B 106.1(4) . . ? O1B S22 C22B 103.4(6) . . ? O3B S22 C22B 96.6(6) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 1.267 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.098 #===END