# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1823 data_global _publ_contact_author_name 'R.N. Lyubovskaya' _publ_contact_author_address ;Institute of Problems of Chemical Physics RAS Chernogolovka, 142432 Russia ; _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis and crystal structure of C60 complex with a bis(ethylenedithio)tetrathiafulvalene radical cation salt: (BEDT-TTF.I3)C60 ; data_eti3c60 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Bis(ethylenedithio)tetrathiafulvalene C60 complex' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C70 H8 I3 S8' _chemical_formula_sum 'C70 H8 I3 S8' _chemical_formula_weight 1485.94 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.590(2) _cell_length_b 9.9271(7) _cell_length_c 17.2881(12) _cell_angle_alpha 90.00 _cell_angle_beta 116.7350(10) _cell_angle_gamma 90.00 _cell_volume 4535.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 563 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860 _exptl_absorpt_coefficient_mu 2.492 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4356 _exptl_absorpt_correction_T_max 0.6356 _exptl_absorpt_process_details 'empirical, Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21257 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.66 _reflns_number_total 4228 _reflns_number_gt 3265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4228 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.02097(4) 1.09383(10) 0.31820(7) 0.0128(2) Uani 1 1 d . . . S2 S -0.01700(4) 1.38696(10) 0.33039(7) 0.0124(2) Uani 1 1 d . . . S3 S -0.06756(4) 1.05254(11) 0.43478(7) 0.0144(3) Uani 1 1 d . . . S4 S -0.06419(5) 1.40792(11) 0.44770(8) 0.0204(3) Uani 1 1 d . . . I1 I 0.0000 0.73005(4) 0.2500 0.01587(13) Uani 1 2 d S . . I2 I -0.082838(11) 0.73398(3) 0.29852(2) 0.01964(12) Uani 1 1 d . . . C1 C -0.00825(16) 1.2436(4) 0.2819(3) 0.0115(9) Uani 1 1 d . . . C2 C -0.04394(15) 1.1669(4) 0.3854(3) 0.0112(9) Uani 1 1 d . . . C3 C -0.04259(15) 1.3025(4) 0.3906(3) 0.0119(9) Uani 1 1 d . . . C4 C -0.05863(16) 1.1578(4) 0.5256(3) 0.0152(10) Uani 1 1 d . . . H4A H -0.0689 1.1074 0.5646 0.023(12) Uiso 1 1 calc R . . H4B H -0.0223 1.1804 0.5586 0.012(11) Uiso 1 1 calc R . . C5 C -0.08897(17) 1.2865(4) 0.4973(3) 0.0175(10) Uani 1 1 d . . . H5A H -0.0900 1.3288 0.5484 0.046(16) Uiso 1 1 calc R . . H5B H -0.1242 1.2639 0.4555 0.011(12) Uiso 1 1 calc R . . C6 C 0.19182(16) 1.5712(4) 0.4523(3) 0.0143(10) Uani 1 1 d . . . C7 C 0.24031(16) 1.5348(4) 0.3698(3) 0.0126(9) Uani 1 1 d . . . C8 C 0.20794(17) 0.9984(4) 0.3375(3) 0.0170(10) Uani 1 1 d . . . C9 C 0.21267(16) 1.0253(4) 0.6195(3) 0.0134(9) Uani 1 1 d . . . C10 C 0.23293(17) 1.0933(4) 0.3048(3) 0.0162(10) Uani 1 1 d U . . C11 C 0.21980(16) 0.9025(4) 0.4768(3) 0.0141(10) Uani 1 1 d . . . C12 C 0.17040(16) 1.0214(4) 0.5374(3) 0.0147(10) Uani 1 1 d . . . C13 C 0.21483(16) 1.3918(4) 0.6534(3) 0.0140(9) Uani 1 1 d U . . C14 C 0.18427(17) 1.4701(4) 0.5756(3) 0.0176(10) Uani 1 1 d . . . C15 C 0.20036(17) 1.2101(4) 0.2726(3) 0.0158(10) Uani 1 1 d U . . C16 C 0.15635(16) 1.1880(4) 0.2860(3) 0.0152(10) Uani 1 1 d . . . C17 C 0.19931(16) 1.4488(4) 0.3093(3) 0.0150(10) Uani 1 1 d . . . C18 C 0.23636(16) 1.5937(4) 0.4391(3) 0.0128(9) Uani 1 1 d . . . C19 C 0.22404(16) 1.1454(4) 0.6723(3) 0.0140(9) Uani 1 1 d . . . C20 C 0.17425(15) 0.9591(4) 0.4661(3) 0.0126(9) Uani 1 1 d . . . C21 C 0.23762(17) 0.9230(4) 0.4108(3) 0.0157(10) Uani 1 1 d . . . C22 C 0.20803(16) 1.5603(4) 0.5444(3) 0.0136(9) Uani 1 1 d . . . C23 C 0.12824(15) 1.3954(4) 0.4276(3) 0.0144(9) Uani 1 1 d . . . C24 C 0.11733(16) 1.2741(4) 0.3754(3) 0.0164(10) Uani 1 1 d . . . C25 C 0.12187(15) 1.1488(4) 0.4136(3) 0.0161(10) Uani 1 1 d . . . C26 C 0.13454(16) 1.2941(5) 0.3106(3) 0.0172(10) Uani 1 1 d . . . C27 C 0.14883(17) 1.2549(4) 0.5563(3) 0.0186(11) Uani 1 1 d . . . C28 C 0.13821(15) 1.1387(4) 0.5068(3) 0.0152(10) Uani 1 1 d . . . C29 C 0.22151(16) 1.3386(4) 0.2843(3) 0.0147(10) Uani 1 1 d . . . C30 C 0.14382(16) 1.0382(4) 0.3886(3) 0.0158(10) Uani 1 1 d . . . C31 C 0.19233(17) 1.2583(4) 0.6412(3) 0.0143(10) Uani 1 1 d U . . C32 C 0.15309(15) 1.4904(4) 0.3951(3) 0.0139(9) Uani 1 1 d . . . C33 C 0.15658(16) 1.4279(4) 0.3221(3) 0.0168(10) Uani 1 1 d . . . C34 C 0.16123(16) 1.0559(4) 0.3258(3) 0.0161(10) Uani 1 1 d . . . C35 C 0.14409(16) 1.3856(4) 0.5169(3) 0.0159(10) Uani 1 1 d . . . 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 0.0192(6) 0.0111(5) 0.0130(6) 0.0009(4) 0.0117(5) 0.0005(4) S2 0.0172(6) 0.0115(5) 0.0131(6) -0.0006(4) 0.0109(5) -0.0009(4) S3 0.0204(6) 0.0146(6) 0.0136(6) -0.0005(4) 0.0123(5) -0.0025(4) S4 0.0342(7) 0.0133(6) 0.0268(7) -0.0001(5) 0.0254(6) 0.0018(5) I1 0.0271(3) 0.0117(2) 0.0124(2) 0.000 0.0120(2) 0.000 I2 0.0248(2) 0.01770(19) 0.0213(2) -0.00411(12) 0.01467(16) -0.00343(12) C1 0.013(2) 0.012(2) 0.011(2) -0.0009(17) 0.0069(19) -0.0001(17) C2 0.009(2) 0.014(2) 0.009(2) -0.0004(17) 0.0038(18) 0.0016(17) C3 0.008(2) 0.022(2) 0.009(2) 0.0006(18) 0.0064(18) 0.0008(18) C4 0.019(2) 0.018(2) 0.013(2) 0.0016(19) 0.011(2) 0.0004(19) C5 0.020(3) 0.022(2) 0.018(3) 0.004(2) 0.015(2) 0.003(2) C6 0.018(2) 0.006(2) 0.021(3) 0.0037(18) 0.011(2) 0.0072(18) C7 0.023(2) 0.006(2) 0.012(2) 0.0058(17) 0.010(2) 0.0003(18) C8 0.030(3) 0.011(2) 0.012(2) -0.0099(18) 0.012(2) -0.0059(19) C9 0.023(2) 0.012(2) 0.011(2) 0.0049(18) 0.012(2) -0.0019(18) C10 0.0237(17) 0.0176(17) 0.0105(16) -0.0035(13) 0.0106(14) 0.0006(14) C11 0.024(3) 0.007(2) 0.015(2) -0.0033(17) 0.012(2) -0.0077(18) C12 0.016(2) 0.012(2) 0.022(3) 0.0025(19) 0.014(2) -0.0047(18) C13 0.0220(17) 0.0167(17) 0.0100(16) -0.0019(13) 0.0132(14) 0.0020(14) C14 0.026(3) 0.013(2) 0.021(3) -0.0038(19) 0.017(2) 0.008(2) C15 0.0194(17) 0.0194(17) 0.0089(16) -0.0032(13) 0.0065(14) -0.0003(14) C16 0.020(2) 0.019(2) 0.001(2) -0.0033(18) 0.0000(19) -0.0047(19) C17 0.019(2) 0.019(2) 0.005(2) 0.0082(18) 0.0038(19) 0.0044(19) C18 0.021(2) 0.003(2) 0.020(2) 0.0051(17) 0.013(2) 0.0029(17) C19 0.023(2) 0.016(2) 0.011(2) 0.0045(18) 0.015(2) 0.0019(19) C20 0.016(2) 0.008(2) 0.014(2) 0.0000(17) 0.0067(19) -0.0069(17) C21 0.033(3) 0.004(2) 0.017(2) -0.0052(18) 0.018(2) -0.0034(19) C22 0.024(3) 0.008(2) 0.015(2) -0.0008(18) 0.015(2) 0.0049(18) C23 0.010(2) 0.013(2) 0.023(3) 0.0040(19) 0.0102(19) 0.0049(17) C24 0.006(2) 0.026(3) 0.013(2) 0.0006(19) 0.0002(19) 0.0005(18) C25 0.007(2) 0.021(2) 0.018(2) -0.0001(19) 0.0039(19) -0.0064(18) C26 0.012(2) 0.023(3) 0.011(2) 0.0041(19) 0.000(2) 0.0003(19) C27 0.016(2) 0.019(3) 0.034(3) 0.005(2) 0.023(2) 0.0026(18) C28 0.012(2) 0.019(2) 0.020(3) 0.0019(19) 0.012(2) -0.0032(18) C29 0.025(3) 0.015(2) 0.007(2) 0.0043(17) 0.010(2) 0.0027(19) C30 0.015(2) 0.015(2) 0.015(2) -0.0025(18) 0.005(2) -0.0081(18) C31 0.0177(17) 0.0184(17) 0.0121(17) -0.0005(13) 0.0114(14) 0.0012(13) C32 0.015(2) 0.014(2) 0.014(2) 0.0047(18) 0.007(2) 0.0083(18) C33 0.016(2) 0.020(2) 0.009(2) 0.0099(18) 0.0005(19) 0.0082(19) C34 0.019(2) 0.015(2) 0.009(2) -0.0086(18) 0.0021(19) -0.0067(19) C35 0.016(2) 0.018(2) 0.024(3) 0.0071(19) 0.018(2) 0.0080(18) _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 1.720(4) . ? S1 C2 1.745(4) . ? S2 C1 1.729(4) . ? S2 C3 1.752(4) . ? S3 C2 1.744(4) . ? S3 C4 1.804(4) . ? S4 C3 1.745(4) . ? S4 C5 1.814(4) . ? I1 I2 2.9263(3) . ? I1 I2 2.9263(3) 2 ? C1 C1 1.393(9) 2 ? C2 C3 1.349(6) . ? C4 C5 1.511(6) . ? C6 C32 1.384(6) . ? C6 C22 1.446(6) . ? C6 C18 1.452(6) . ? C7 C18 1.383(6) . ? C7 C9 1.447(6) 7_576 ? C7 C17 1.467(6) . ? C8 C21 1.391(6) . ? C8 C34 1.423(6) . ? C8 C10 1.459(6) . ? C9 C12 1.407(6) . ? C9 C19 1.446(6) . ? C9 C7 1.447(6) 7_576 ? C10 C13 1.389(6) 7_576 ? C10 C15 1.449(6) . ? C11 C20 1.393(6) . ? C11 C18 1.450(6) 7_576 ? C11 C21 1.469(6) . ? C12 C20 1.429(6) . ? C12 C28 1.446(6) . ? C13 C10 1.389(6) 7_576 ? C13 C31 1.455(6) . ? C13 C14 1.462(6) . ? C14 C22 1.389(6) . ? C14 C35 1.436(6) . ? C15 C29 1.395(6) . ? C15 C16 1.439(6) . ? C16 C26 1.398(6) . ? C16 C34 1.457(6) . ? C17 C33 1.394(6) . ? C17 C29 1.439(6) . ? C18 C11 1.450(6) 7_576 ? C19 C31 1.404(6) . ? C19 C29 1.448(6) 7_576 ? C20 C30 1.462(6) . ? C21 C22 1.447(6) 7_576 ? C22 C21 1.447(6) 7_576 ? C23 C35 1.400(6) . ? C23 C24 1.451(6) . ? C23 C32 1.456(6) . ? C24 C25 1.387(6) . ? C24 C26 1.437(6) . ? C25 C30 1.438(6) . ? C25 C28 1.462(6) . ? C26 C33 1.453(6) . ? C27 C28 1.385(6) . ? C27 C35 1.443(6) . ? C27 C31 1.453(7) . ? C29 C19 1.448(6) 7_576 ? C30 C34 1.406(6) . ? C32 C33 1.451(6) . ? 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 C2 95.6(2) . . ? C1 S2 C3 95.3(2) . . ? C2 S3 C4 96.6(2) . . ? C3 S4 C5 101.4(2) . . ? I2 I1 I2 178.475(17) . 2 ? C1 C1 S1 120.08(14) 2 . ? C1 C1 S2 124.49(14) 2 . ? S1 C1 S2 115.4(2) . . ? C3 C2 S3 128.5(3) . . ? C3 C2 S1 116.8(3) . . ? S3 C2 S1 114.7(2) . . ? C2 C3 S4 129.0(3) . . ? C2 C3 S2 116.5(3) . . ? S4 C3 S2 114.5(2) . . ? C5 C4 S3 112.1(3) . . ? C4 C5 S4 114.0(3) . . ? C32 C6 C22 120.1(4) . . ? C32 C6 C18 119.7(4) . . ? C22 C6 C18 108.0(4) . . ? C18 C7 C9 120.9(4) . 7_576 ? C18 C7 C17 119.9(4) . . ? C9 C7 C17 106.9(4) 7_576 . ? C21 C8 C34 121.4(4) . . ? C21 C8 C10 118.5(4) . . ? C34 C8 C10 108.3(4) . . ? C12 C9 C19 120.5(4) . . ? C12 C9 C7 119.0(4) . 7_576 ? C19 C9 C7 108.8(4) . 7_576 ? C13 C10 C15 120.4(4) 7_576 . ? C13 C10 C8 120.4(4) 7_576 . ? C15 C10 C8 107.5(4) . . ? C20 C11 C18 119.9(4) . 7_576 ? C20 C11 C21 120.3(4) . . ? C18 C11 C21 107.7(3) 7_576 . ? C9 C12 C20 120.1(4) . . ? C9 C12 C28 119.2(4) . . ? C20 C12 C28 109.1(4) . . ? C10 C13 C31 120.2(4) 7_576 . ? C10 C13 C14 120.3(4) 7_576 . ? C31 C13 C14 107.3(4) . . ? C22 C14 C35 120.3(4) . . ? C22 C14 C13 119.2(4) . . ? C35 C14 C13 108.2(4) . . ? C29 C15 C16 119.7(4) . . ? C29 C15 C10 119.9(4) . . ? C16 C15 C10 108.0(4) . . ? C26 C16 C15 120.6(4) . . ? C26 C16 C34 119.8(4) . . ? C15 C16 C34 108.0(4) . . ? C33 C17 C29 120.2(4) . . ? C33 C17 C7 119.5(4) . . ? C29 C17 C7 108.3(4) . . ? C7 C18 C11 119.6(4) . 7_576 ? C7 C18 C6 120.4(4) . . ? C11 C18 C6 108.2(3) 7_576 . ? C31 C19 C29 120.4(4) . 7_576 ? C31 C19 C9 119.4(4) . . ? C29 C19 C9 107.8(4) 7_576 . ? C11 C20 C12 120.5(4) . . ? C11 C20 C30 119.9(4) . . ? C12 C20 C30 107.7(4) . . ? C8 C21 C22 121.3(4) . 7_576 ? C8 C21 C11 118.8(4) . . ? C22 C21 C11 107.5(4) 7_576 . ? C14 C22 C6 120.1(4) . . ? C14 C22 C21 120.1(4) . 7_576 ? C6 C22 C21 108.6(4) . 7_576 ? C35 C23 C24 119.9(4) . . ? C35 C23 C32 119.6(4) . . ? C24 C23 C32 107.8(4) . . ? C25 C24 C26 120.2(4) . . ? C25 C24 C23 120.0(4) . . ? C26 C24 C23 108.2(4) . . ? C24 C25 C30 120.1(4) . . ? C24 C25 C28 120.0(4) . . ? C30 C25 C28 108.0(4) . . ? C16 C26 C24 120.4(4) . . ? C16 C26 C33 119.3(4) . . ? C24 C26 C33 108.3(4) . . ? C28 C27 C35 120.7(4) . . ? C28 C27 C31 119.7(4) . . ? C35 C27 C31 108.0(4) . . ? C27 C28 C12 121.0(4) . . ? C27 C28 C25 119.6(4) . . ? C12 C28 C25 107.2(4) . . ? C15 C29 C17 120.2(4) . . ? C15 C29 C19 119.9(4) . 7_576 ? C17 C29 C19 108.2(4) . 7_576 ? C34 C30 C25 120.6(4) . . ? C34 C30 C20 119.1(4) . . ? C25 C30 C20 108.0(4) . . ? C19 C31 C27 120.2(4) . . ? C19 C31 C13 119.2(4) . . ? C27 C31 C13 107.9(4) . . ? C6 C32 C33 120.6(4) . . ? C6 C32 C23 119.9(4) . . ? C33 C32 C23 107.7(4) . . ? C17 C33 C32 119.9(4) . . ? C17 C33 C26 119.9(4) . . ? C32 C33 C26 107.9(4) . . ? C30 C34 C8 120.6(4) . . ? C30 C34 C16 118.9(4) . . ? C8 C34 C16 108.2(4) . . ? C23 C35 C14 119.9(4) . . ? C23 C35 C27 119.7(4) . . ? C14 C35 C27 108.6(4) . . ? 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 C2 S1 C1 C1 -175.0(5) . . . 2 ? C2 S1 C1 S2 5.4(3) . . . . ? C3 S2 C1 C1 174.6(5) . . . 2 ? C3 S2 C1 S1 -5.8(3) . . . . ? C4 S3 C2 C3 -26.3(4) . . . . ? C4 S3 C2 S1 155.8(2) . . . . ? C1 S1 C2 C3 -2.7(3) . . . . ? C1 S1 C2 S3 175.5(2) . . . . ? S3 C2 C3 S4 -0.3(6) . . . . ? S1 C2 C3 S4 177.5(3) . . . . ? S3 C2 C3 S2 -178.8(2) . . . . ? S1 C2 C3 S2 -1.0(4) . . . . ? C5 S4 C3 C2 -0.2(4) . . . . ? C5 S4 C3 S2 178.3(2) . . . . ? C1 S2 C3 C2 4.1(4) . . . . ? C1 S2 C3 S4 -174.6(2) . . . . ? C2 S3 C4 C5 61.4(3) . . . . ? S3 C4 C5 S4 -73.0(4) . . . . ? C3 S4 C5 C4 36.4(4) . . . . ? C21 C8 C10 C13 -0.5(6) . . . 7_576 ? C34 C8 C10 C13 143.1(4) . . . 7_576 ? C21 C8 C10 C15 -143.6(4) . . . . ? C34 C8 C10 C15 -0.1(5) . . . . ? C19 C9 C12 C20 138.8(4) . . . . ? C7 C9 C12 C20 -0.2(6) 7_576 . . . ? C19 C9 C12 C28 -0.4(6) . . . . ? C7 C9 C12 C28 -139.4(4) 7_576 . . . ? C10 C13 C14 C22 -0.4(6) 7_576 . . . ? C31 C13 C14 C22 -142.8(4) . . . . ? C10 C13 C14 C35 142.1(4) 7_576 . . . ? C31 C13 C14 C35 -0.4(5) . . . . ? C13 C10 C15 C29 -0.6(6) 7_576 . . . ? C8 C10 C15 C29 142.6(4) . . . . ? C13 C10 C15 C16 -142.7(4) 7_576 . . . ? C8 C10 C15 C16 0.5(5) . . . . ? C29 C15 C16 C26 0.1(6) . . . . ? C10 C15 C16 C26 142.2(4) . . . . ? C29 C15 C16 C34 -142.9(4) . . . . ? C10 C15 C16 C34 -0.7(5) . . . . ? C18 C7 C17 C33 0.3(6) . . . . ? C9 C7 C17 C33 142.8(4) 7_576 . . . ? C18 C7 C17 C29 -142.4(4) . . . . ? C9 C7 C17 C29 0.1(4) 7_576 . . . ? C9 C7 C18 C11 1.2(6) 7_576 . . 7_576 ? C17 C7 C18 C11 138.4(4) . . . 7_576 ? C9 C7 C18 C6 -137.4(4) 7_576 . . . ? C17 C7 C18 C6 -0.1(6) . . . . ? C32 C6 C18 C7 -0.1(6) . . . . ? C22 C6 C18 C7 142.4(4) . . . . ? C32 C6 C18 C11 -142.7(4) . . . 7_576 ? C22 C6 C18 C11 -0.3(4) . . . 7_576 ? C12 C9 C19 C31 0.3(6) . . . . ? C7 C9 C19 C31 143.0(4) 7_576 . . . ? C12 C9 C19 C29 -142.1(4) . . . 7_576 ? C7 C9 C19 C29 0.6(4) 7_576 . . 7_576 ? C18 C11 C20 C12 0.3(6) 7_576 . . . ? C21 C11 C20 C12 -137.6(4) . . . . ? C18 C11 C20 C30 138.3(4) 7_576 . . . ? C21 C11 C20 C30 0.5(6) . . . . ? C9 C12 C20 C11 -0.4(6) . . . . ? C28 C12 C20 C11 142.4(4) . . . . ? C9 C12 C20 C30 -143.0(4) . . . . ? C28 C12 C20 C30 -0.1(5) . . . . ? C34 C8 C21 C22 -137.1(4) . . . 7_576 ? C10 C8 C21 C22 1.6(6) . . . 7_576 ? C34 C8 C21 C11 0.3(6) . . . . ? C10 C8 C21 C11 139.0(4) . . . . ? C20 C11 C21 C8 -0.7(6) . . . . ? C18 C11 C21 C8 -143.0(4) 7_576 . . . ? C20 C11 C21 C22 142.0(4) . . . 7_576 ? C18 C11 C21 C22 -0.3(4) 7_576 . . 7_576 ? C35 C14 C22 C6 1.1(6) . . . . ? C13 C14 C22 C6 138.9(4) . . . . ? C35 C14 C22 C21 -138.6(4) . . . 7_576 ? C13 C14 C22 C21 -0.7(6) . . . 7_576 ? C32 C6 C22 C14 -1.0(6) . . . . ? C18 C6 C22 C14 -143.2(4) . . . . ? C32 C6 C22 C21 142.8(4) . . . 7_576 ? C18 C6 C22 C21 0.5(4) . . . 7_576 ? C35 C23 C24 C25 0.9(6) . . . . ? C32 C23 C24 C25 142.6(4) . . . . ? C35 C23 C24 C26 -142.4(4) . . . . ? C32 C23 C24 C26 -0.7(5) . . . . ? C26 C24 C25 C30 0.0(6) . . . . ? C23 C24 C25 C30 -139.0(4) . . . . ? C26 C24 C25 C28 138.3(4) . . . . ? C23 C24 C25 C28 -0.7(6) . . . . ? C15 C16 C26 C24 -138.1(4) . . . . ? C34 C16 C26 C24 0.6(6) . . . . ? C15 C16 C26 C33 0.3(6) . . . . ? C34 C16 C26 C33 139.0(4) . . . . ? C25 C24 C26 C16 -0.5(6) . . . . ? C23 C24 C26 C16 142.8(4) . . . . ? C25 C24 C26 C33 -143.0(4) . . . . ? C23 C24 C26 C33 0.3(5) . . . . ? C35 C27 C28 C12 137.4(4) . . . . ? C31 C27 C28 C12 -1.3(6) . . . . ? C35 C27 C28 C25 -0.2(6) . . . . ? C31 C27 C28 C25 -139.0(4) . . . . ? C9 C12 C28 C27 1.0(6) . . . . ? C20 C12 C28 C27 -142.3(4) . . . . ? C9 C12 C28 C25 143.1(4) . . . . ? C20 C12 C28 C25 -0.1(4) . . . . ? C24 C25 C28 C27 0.3(6) . . . . ? C30 C25 C28 C27 143.1(4) . . . . ? C24 C25 C28 C12 -142.5(4) . . . . ? C30 C25 C28 C12 0.3(4) . . . . ? C16 C15 C29 C17 -0.3(6) . . . . ? C10 C15 C29 C17 -138.0(4) . . . . ? C16 C15 C29 C19 138.4(4) . . . 7_576 ? C10 C15 C29 C19 0.7(6) . . . 7_576 ? C33 C17 C29 C15 0.1(6) . . . . ? C7 C17 C29 C15 142.4(4) . . . . ? C33 C17 C29 C19 -142.9(4) . . . 7_576 ? C7 C17 C29 C19 -0.5(4) . . . 7_576 ? C24 C25 C30 C34 0.5(6) . . . . ? C28 C25 C30 C34 -142.2(4) . . . . ? C24 C25 C30 C20 142.3(4) . . . . ? C28 C25 C30 C20 -0.4(4) . . . . ? C11 C20 C30 C34 0.0(6) . . . . ? C12 C20 C30 C34 142.8(4) . . . . ? C11 C20 C30 C25 -142.5(4) . . . . ? C12 C20 C30 C25 0.3(5) . . . . ? C29 C19 C31 C27 137.0(4) 7_576 . . . ? C9 C19 C31 C27 -0.7(6) . . . . ? C29 C19 C31 C13 -0.2(6) 7_576 . . . ? C9 C19 C31 C13 -137.8(4) . . . . ? C28 C27 C31 C19 1.2(6) . . . . ? C35 C27 C31 C19 -142.2(4) . . . . ? C28 C27 C31 C13 142.6(4) . . . . ? C35 C27 C31 C13 -0.8(5) . . . . ? C10 C13 C31 C19 0.1(6) 7_576 . . . ? C14 C13 C31 C19 142.6(4) . . . . ? C10 C13 C31 C27 -141.8(4) 7_576 . . . ? C14 C13 C31 C27 0.7(5) . . . . ? C22 C6 C32 C33 -137.9(4) . . . . ? C18 C6 C32 C33 0.1(6) . . . . ? C22 C6 C32 C23 0.7(6) . . . . ? C18 C6 C32 C23 138.6(4) . . . . ? C35 C23 C32 C6 -0.6(6) . . . . ? C24 C23 C32 C6 -142.4(4) . . . . ? C35 C23 C32 C33 142.7(4) . . . . ? C24 C23 C32 C33 0.9(5) . . . . ? C29 C17 C33 C32 137.9(4) . . . . ? C7 C17 C33 C32 -0.3(6) . . . . ? C29 C17 C33 C26 0.3(6) . . . . ? C7 C17 C33 C26 -137.9(4) . . . . ? C6 C32 C33 C17 0.1(6) . . . . ? C23 C32 C33 C17 -142.9(4) . . . . ? C6 C32 C33 C26 142.3(4) . . . . ? C23 C32 C33 C26 -0.7(5) . . . . ? C16 C26 C33 C17 -0.5(6) . . . . ? C24 C26 C33 C17 142.4(4) . . . . ? C16 C26 C33 C32 -142.7(4) . . . . ? C24 C26 C33 C32 0.3(5) . . . . ? C25 C30 C34 C8 137.4(4) . . . . ? C20 C30 C34 C8 -0.3(6) . . . . ? C25 C30 C34 C16 -0.5(6) . . . . ? C20 C30 C34 C16 -138.2(4) . . . . ? C21 C8 C34 C30 0.1(6) . . . . ? C10 C8 C34 C30 -142.2(4) . . . . ? C21 C8 C34 C16 142.0(4) . . . . ? C10 C8 C34 C16 -0.3(5) . . . . ? C26 C16 C34 C30 -0.1(6) . . . . ? C15 C16 C34 C30 143.2(4) . . . . ? C26 C16 C34 C8 -142.7(4) . . . . ? C15 C16 C34 C8 0.6(5) . . . . ? C24 C23 C35 C14 137.9(4) . . . . ? C32 C23 C35 C14 0.7(6) . . . . ? C24 C23 C35 C27 -0.8(6) . . . . ? C32 C23 C35 C27 -138.1(4) . . . . ? C22 C14 C35 C23 -0.9(6) . . . . ? C13 C14 C35 C23 -142.9(4) . . . . ? C22 C14 C35 C27 141.9(4) . . . . ? C13 C14 C35 C27 -0.1(5) . . . . ? C28 C27 C35 C23 0.5(6) . . . . ? C31 C27 C35 C23 143.4(4) . . . . ? C28 C27 C35 C14 -142.4(4) . . . . ? C31 C27 C35 C14 0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.797 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.797 _refine_diff_density_max 0.661 _refine_diff_density_min -1.416 _refine_diff_density_rms 0.158