# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1528 data_global _publ_contact_author 'Andrei S.Batsanov' _publ_contact_author_email a.s.batsanov@durham.ac.uk loop_ _publ_author_name 'Christensen, Christian A.' 'Bryce, Martin R.' 'Batsanov, Andrei S.' 'Becher, Jan' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2000' _ccdc_journal_depnumber '?' _publ_section_title ; A novel hexakis(tetrathiafulvalene) derivative: synthesis, structure and electrochemical properties. ; #==================================================================END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis{[tris(methylthio)tetrathiafulvalenyl]thiomethyl}benzene ; _chemical_name_common ? _chemical_melting_point '214-215 deg.C' _chemical_formula_moiety ? _chemical_formula_sum 'C66 H66 S48' _chemical_formula_weight 2398.07 _ccdc_compound_id '3' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; 3 of the methyl groups are disordered over 2 positions (A and B) each, with occupancies 85 and 15(1)% for C(20), 57 and 43(1)% for C(29), 84 and 16(1)% for C(39). ; _ccdc_comments '?' 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' _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 10.799(3) _cell_length_b 15.117(1) _cell_length_c 16.732(5) _cell_angle_alpha 69.56(1) _cell_angle_beta 76.88(1) _cell_angle_gamma 77.89(1) _cell_volume 2467(1) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 925 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.5907 _exptl_absorpt_correction_T_max 0.7197 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998); R(int)=0.064 before correction' _exptl_special_details ; Five sets of \w scans (each scan 0.3\% in \w, exposure time 15 s), each set at different \f and/or 2\q angles, nominally covered full sphere of reciprocal space. The first 50 scans were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22999 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8659 _reflns_number_gt 7731 _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^)+(0.0383P)^2^+2.4160P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8659 _refine_ls_number_parameters 541 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.018 _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 S11 S 0.26279(5) 0.42465(4) 0.44496(4) 0.02500(12) Uani 1 1 d . . . S12 S 0.18695(6) 0.24530(4) 0.57184(4) 0.02946(14) Uani 1 1 d . . . S13 S 0.09025(6) 0.54292(4) 0.57430(4) 0.02663(13) Uani 1 1 d . A . S14 S -0.00811(6) 0.36541(4) 0.69052(4) 0.03118(14) Uani 1 1 d . . . S15 S 0.50650(5) 0.32693(4) 0.36198(4) 0.02471(12) Uani 1 1 d . . . S16 S 0.42354(7) 0.12368(4) 0.50791(5) 0.03713(15) Uani 1 1 d . . . S17 S -0.00086(6) 0.64773(4) 0.70393(4) 0.03317(14) Uani 1 1 d . A . S18 S -0.12741(6) 0.44794(5) 0.83517(4) 0.03939(16) Uani 1 1 d . . . S21 S 0.68740(6) 0.78386(4) 0.10195(3) 0.02650(13) Uani 1 1 d . . . S22 S 0.75210(6) 0.65188(4) -0.00034(3) 0.02715(13) Uani 1 1 d . . . S23 S 0.82237(6) 0.94782(4) -0.06917(3) 0.02619(13) Uani 1 1 d . . . S24 S 0.90582(6) 0.80341(4) -0.15953(3) 0.02540(13) Uani 1 1 d . B . S25 S 0.69427(5) 0.62724(4) 0.27298(3) 0.02089(12) Uani 1 1 d . . . S26 S 0.74684(6) 0.47578(4) 0.15732(4) 0.02732(13) Uani 1 1 d . . . S27 S 0.97972(7) 1.09142(5) -0.20606(4) 0.04029(16) Uani 1 1 d D . . S28 S 1.08011(6) 0.92212(4) -0.30485(4) 0.03146(14) Uani 1 1 d . B . S31 S 0.35818(6) 0.90364(4) 0.23318(3) 0.02600(13) Uani 1 1 d . . . S32 S 0.27420(6) 1.03942(4) 0.33307(4) 0.02571(13) Uani 1 1 d . . . S33 S 0.52802(6) 1.06141(4) 0.08153(4) 0.03137(14) Uani 1 1 d . . . S34 S 0.42800(6) 1.19648(4) 0.18187(4) 0.03099(14) Uani 1 1 d . C . S35 S 0.27642(5) 0.73617(4) 0.38451(3) 0.02160(12) Uani 1 1 d . . . S36 S 0.17938(6) 0.89550(4) 0.49775(4) 0.03011(14) Uani 1 1 d . . . S37 S 0.72309(7) 1.18089(5) -0.04150(4) 0.03976(16) Uani 1 1 d . . . S38 S 0.61364(7) 1.33477(5) 0.07180(5) 0.03880(16) Uani 1 1 d . C . C1 C 0.55961(19) 0.43968(14) 0.45021(13) 0.0173(4) Uani 1 1 d . . . C2 C 0.52318(19) 0.53746(14) 0.40915(13) 0.0169(4) Uani 1 1 d . . . C3 C 0.46684(19) 0.59785(14) 0.45907(13) 0.0170(4) Uani 1 1 d . . . C11 C 0.1717(2) 0.37029(16) 0.54527(15) 0.0240(5) Uani 1 1 d . . . C12 C 0.3730(2) 0.31917(16) 0.44545(14) 0.0235(5) Uani 1 1 d . . . C13 C 0.3369(2) 0.23680(16) 0.50342(15) 0.0257(5) Uani 1 1 d . . . C14 C 0.0960(2) 0.41919(16) 0.59589(15) 0.0252(5) Uani 1 1 d . . . C15 C 0.0137(2) 0.54152(17) 0.67971(15) 0.0270(5) Uani 1 1 d . . . C16 C -0.0313(2) 0.46093(17) 0.73287(16) 0.0291(5) Uani 1 1 d . A . C17 C 0.6230(2) 0.37398(15) 0.39781(13) 0.0196(4) Uani 1 1 d . . . H171 H 0.6774 0.3197 0.4329 0.025 Uiso 1 1 d R . . H172 H 0.6798 0.4090 0.3461 0.025 Uiso 1 1 d R . . C18 C 0.3868(3) 0.05732(19) 0.6220(2) 0.0464(7) Uani 1 1 d . . . H181 H 0.4075 0.0910 0.6567 0.065(6) Uiso 1 1 d R . . H182 H 0.4377 -0.0063 0.6334 0.065(6) Uiso 1 1 d R . . H183 H 0.2951 0.0511 0.6374 0.065(6) Uiso 1 1 d R . . C19 C -0.1614(2) 0.70056(18) 0.68262(18) 0.0343(6) Uani 1 1 d . . . H191 H -0.1659 0.7084 0.6226 0.056(5) Uiso 1 1 d R A . H192 H -0.1820 0.7630 0.6916 0.056(5) Uiso 1 1 d R . . H193 H -0.2232 0.6590 0.7220 0.056(5) Uiso 1 1 d R . . C20A C -0.0493(3) 0.3385(2) 0.9025(2) 0.0398(9) Uani 0.850(7) 1 d P A 1 H201 H -0.0380 0.2881 0.8762 0.060 Uiso 0.850(7) 1 d PR A 1 H202 H -0.1026 0.3198 0.9599 0.060 Uiso 0.850(7) 1 d PR A 1 H203 H 0.0348 0.3483 0.9081 0.060 Uiso 0.850(7) 1 d PR A 1 C20B C -0.2844(18) 0.4322(13) 0.8026(12) 0.041(5) Uiso 0.150(7) 1 d P A 2 C21 C 0.7613(2) 0.76603(15) 0.00196(13) 0.0236(5) Uani 1 1 d . . . C22 C 0.7090(2) 0.66011(15) 0.16016(13) 0.0213(4) Uani 1 1 d . . . C23 C 0.7387(2) 0.59944(15) 0.11323(13) 0.0225(5) Uani 1 1 d . . . C24 C 0.8228(2) 0.82990(15) -0.06508(13) 0.0220(4) Uani 1 1 d . . . C25 C 0.9360(2) 0.97605(16) -0.16553(14) 0.0257(5) Uani 1 1 d . B . C26 C 0.9755(2) 0.90927(16) -0.20583(14) 0.0248(5) Uani 1 1 d . . . C27 C 0.5413(2) 0.57779(14) 0.31127(12) 0.0185(4) Uani 1 1 d . . . H271 H 0.4692 0.6285 0.2932 0.024 Uiso 1 1 d R . . H272 H 0.5435 0.5270 0.2861 0.024 Uiso 1 1 d R . . C28 C 0.8858(2) 0.43455(16) 0.08995(15) 0.0293(5) Uani 1 1 d . . . H281 H 0.8745 0.4627 0.0292 0.046(5) Uiso 1 1 d R . . H282 H 0.8961 0.3649 0.1062 0.046(5) Uiso 1 1 d R . . H283 H 0.9625 0.4537 0.0976 0.046(5) Uiso 1 1 d R . . C29A C 1.1331(5) 1.0673(7) -0.1706(4) 0.072(2) Uani 0.57 1 d PD B 1 H291 H 1.1698 1.1268 -0.1892 0.108 Uiso 0.57 1 d PR B 1 H292 H 1.1918 1.0214 -0.1958 0.108 Uiso 0.57 1 d PR B 1 H293 H 1.1206 1.0409 -0.1073 0.108 Uiso 0.57 1 d PR B 1 C29B C 1.0905(8) 1.0790(10) -0.1353(5) 0.072(2) Uani 0.43 1 d PD B 2 H294 H 1.1233 1.1396 -0.1506 0.108 Uiso 0.43 1 d PR B 2 H295 H 1.1625 1.0284 -0.1400 0.108 Uiso 0.43 1 d PR B 2 H296 H 1.0438 1.0631 -0.0757 0.108 Uiso 0.43 1 d PR B 2 C30 C 1.2126(3) 0.8291(2) -0.27185(18) 0.0430(7) Uani 1 1 d . . . H301 H 1.2431 0.8379 -0.2246 0.055(5) Uiso 1 1 d R B . H302 H 1.2828 0.8325 -0.3212 0.055(5) Uiso 1 1 d R . . H303 H 1.1834 0.7666 -0.2521 0.055(5) Uiso 1 1 d R . . C31 C 0.3652(2) 1.01693(15) 0.23827(14) 0.0237(5) Uani 1 1 d . . . C32 C 0.2849(2) 0.85915(15) 0.34218(13) 0.0210(4) Uani 1 1 d . . . C33 C 0.2479(2) 0.92070(15) 0.38769(14) 0.0223(4) Uani 1 1 d . . . C34 C 0.4325(2) 1.08164(15) 0.17577(14) 0.0253(5) Uani 1 1 d . . . C35 C 0.5985(2) 1.16697(17) 0.04832(16) 0.0293(5) Uani 1 1 d . C . C36 C 0.5531(2) 1.22820(16) 0.09354(15) 0.0281(5) Uani 1 1 d . . . C37 C 0.4377(2) 0.70362(14) 0.41515(13) 0.0185(4) Uani 1 1 d . . . H371 H 0.5030 0.7231 0.3626 0.024 Uiso 1 1 d R . . H372 H 0.4429 0.7383 0.4545 0.024 Uiso 1 1 d R . . C38 C 0.0265(2) 0.86335(18) 0.49921(17) 0.0353(6) Uani 1 1 d . . . H381 H -0.0144 0.9106 0.4520 0.059(6) Uiso 1 1 d R . . H382 H -0.0292 0.8617 0.5547 0.059(6) Uiso 1 1 d R . . H383 H 0.0403 0.8003 0.4918 0.059(6) Uiso 1 1 d R . . C39A C 0.6476(3) 1.2690(2) -0.1253(2) 0.0407(9) Uani 0.842(7) 1 d P C 1 H391 H 0.5734 1.2461 -0.1323 0.061 Uiso 0.842(7) 1 d PR C 1 H392 H 0.7091 1.2813 -0.1796 0.061 Uiso 0.842(7) 1 d PR C 1 H393 H 0.6188 1.3281 -0.1105 0.061 Uiso 0.842(7) 1 d PR C 1 C39B C 0.866(2) 1.1820(15) -0.0067(13) 0.052(6) Uiso 0.158(7) 1 d P C 2 C40 C 0.4755(3) 1.40815(18) 0.11278(18) 0.0361(6) Uani 1 1 d . . . H401 H 0.4017 1.4098 0.0871 0.050(5) Uiso 1 1 d R C . H402 H 0.4951 1.4731 0.0974 0.050(5) Uiso 1 1 d R . . H403 H 0.4551 1.3812 0.1759 0.050(5) Uiso 1 1 d R . . 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 S11 0.0239(3) 0.0237(3) 0.0266(3) -0.0092(2) -0.0042(2) 0.0003(2) S12 0.0285(3) 0.0264(3) 0.0343(3) -0.0133(2) 0.0018(2) -0.0071(2) S13 0.0268(3) 0.0247(3) 0.0270(3) -0.0088(2) -0.0059(2) 0.0018(2) S14 0.0278(3) 0.0310(3) 0.0369(3) -0.0171(3) 0.0038(2) -0.0079(2) S15 0.0267(3) 0.0282(3) 0.0216(3) -0.0139(2) -0.0006(2) -0.0021(2) S16 0.0435(4) 0.0239(3) 0.0428(4) -0.0157(3) -0.0020(3) 0.0009(3) S17 0.0352(3) 0.0278(3) 0.0415(4) -0.0178(3) -0.0125(3) 0.0034(2) S18 0.0347(3) 0.0443(4) 0.0368(4) -0.0193(3) 0.0070(3) -0.0034(3) S21 0.0397(3) 0.0170(3) 0.0164(3) -0.0036(2) 0.0045(2) -0.0034(2) S22 0.0448(3) 0.0190(3) 0.0147(3) -0.0034(2) -0.0007(2) -0.0063(2) S23 0.0372(3) 0.0191(3) 0.0177(3) -0.0047(2) 0.0032(2) -0.0048(2) S24 0.0344(3) 0.0194(3) 0.0170(3) -0.0049(2) 0.0031(2) -0.0019(2) S25 0.0228(3) 0.0235(3) 0.0133(2) -0.0031(2) 0.0002(2) -0.0052(2) S26 0.0374(3) 0.0166(3) 0.0211(3) -0.0031(2) 0.0047(2) -0.0047(2) S27 0.0526(4) 0.0302(3) 0.0352(3) -0.0081(3) 0.0079(3) -0.0199(3) S28 0.0307(3) 0.0332(3) 0.0194(3) -0.0025(2) 0.0043(2) -0.0004(2) S31 0.0396(3) 0.0154(3) 0.0173(3) -0.0029(2) 0.0004(2) -0.0013(2) S32 0.0352(3) 0.0163(3) 0.0205(3) -0.0048(2) 0.0016(2) -0.0012(2) S33 0.0413(3) 0.0205(3) 0.0267(3) -0.0081(2) 0.0086(3) -0.0069(2) S34 0.0399(3) 0.0203(3) 0.0280(3) -0.0089(2) 0.0080(3) -0.0069(2) S35 0.0239(3) 0.0145(2) 0.0219(3) -0.0011(2) -0.0046(2) -0.0002(2) S36 0.0375(3) 0.0305(3) 0.0191(3) -0.0071(2) 0.0038(2) -0.0087(2) S37 0.0367(4) 0.0408(4) 0.0380(4) -0.0162(3) 0.0134(3) -0.0124(3) S38 0.0401(4) 0.0324(3) 0.0459(4) -0.0170(3) 0.0073(3) -0.0173(3) C1 0.0171(10) 0.0172(10) 0.0154(10) -0.0042(8) -0.0001(8) -0.0023(8) C2 0.0167(10) 0.0167(10) 0.0143(9) -0.0022(8) -0.0016(8) -0.0021(8) C3 0.0163(10) 0.0148(10) 0.0166(10) -0.0015(8) -0.0017(8) -0.0024(8) C11 0.0217(11) 0.0251(11) 0.0275(12) -0.0101(9) -0.0064(9) -0.0024(9) C12 0.0234(11) 0.0241(11) 0.0251(11) -0.0118(9) -0.0043(9) -0.0009(9) C13 0.0259(12) 0.0255(12) 0.0294(12) -0.0141(10) -0.0047(9) -0.0018(9) C14 0.0219(11) 0.0276(12) 0.0275(12) -0.0101(10) -0.0063(9) -0.0016(9) C15 0.0231(11) 0.0277(12) 0.0318(12) -0.0136(10) -0.0067(10) 0.0027(9) C16 0.0224(11) 0.0315(13) 0.0346(13) -0.0163(11) -0.0024(10) 0.0013(9) C17 0.0213(10) 0.0181(10) 0.0162(10) -0.0047(8) -0.0002(8) -0.0008(8) C18 0.0446(16) 0.0281(14) 0.0535(18) -0.0019(12) -0.0043(14) -0.0010(12) C19 0.0322(13) 0.0292(13) 0.0424(15) -0.0181(11) -0.0064(11) 0.0054(10) C20A 0.0365(18) 0.048(2) 0.0335(17) -0.0119(14) 0.0056(13) -0.0161(14) C21 0.0321(12) 0.0195(11) 0.0151(10) -0.0046(8) 0.0000(9) -0.0006(9) C22 0.0261(11) 0.0182(10) 0.0151(10) -0.0018(8) 0.0016(8) -0.0051(8) C23 0.0287(12) 0.0179(10) 0.0157(10) -0.0013(8) 0.0004(9) -0.0037(9) C24 0.0284(12) 0.0185(10) 0.0157(10) -0.0044(8) -0.0015(9) -0.0002(9) C25 0.0307(12) 0.0230(11) 0.0191(11) -0.0021(9) 0.0002(9) -0.0072(9) C26 0.0266(12) 0.0237(11) 0.0177(10) -0.0015(9) -0.0010(9) -0.0020(9) C27 0.0215(10) 0.0175(10) 0.0133(10) -0.0024(8) -0.0004(8) -0.0031(8) C28 0.0358(13) 0.0213(11) 0.0241(12) -0.0053(9) 0.0015(10) 0.0000(9) C29A 0.106(5) 0.095(4) 0.039(4) -0.019(4) -0.016(4) -0.065(4) C29B 0.106(5) 0.095(4) 0.039(4) -0.019(4) -0.016(4) -0.065(4) C30 0.0371(15) 0.0453(16) 0.0326(14) -0.0069(12) 0.0036(12) 0.0044(12) C31 0.0302(12) 0.0173(10) 0.0197(11) -0.0052(9) -0.0012(9) 0.0009(9) C32 0.0251(11) 0.0157(10) 0.0171(10) -0.0002(8) -0.0049(8) 0.0007(8) C33 0.0256(11) 0.0175(10) 0.0188(10) -0.0005(8) -0.0038(9) -0.0016(8) C34 0.0318(12) 0.0173(11) 0.0228(11) -0.0050(9) -0.0009(9) -0.0008(9) C35 0.0302(12) 0.0245(12) 0.0295(12) -0.0078(10) 0.0032(10) -0.0059(10) C36 0.0290(12) 0.0243(12) 0.0274(12) -0.0053(9) 0.0003(10) -0.0067(9) C37 0.0218(10) 0.0143(10) 0.0160(10) -0.0023(8) -0.0016(8) -0.0014(8) C38 0.0279(13) 0.0337(14) 0.0341(14) -0.0039(11) 0.0024(10) -0.0031(10) C39A 0.0438(19) 0.047(2) 0.0325(17) -0.0112(14) 0.0033(14) -0.0211(15) C40 0.0456(15) 0.0261(13) 0.0397(14) -0.0121(11) -0.0086(12) -0.0073(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 S11 C11 1.757(2) . ? S11 C12 1.777(2) . ? S12 C11 1.764(2) . ? S12 C13 1.767(2) . ? S13 C15 1.765(2) . ? S13 C14 1.767(2) . ? S14 C14 1.763(2) . ? S14 C16 1.770(2) . ? S15 C12 1.757(2) . ? S15 C17 1.861(2) . ? S16 C13 1.754(2) . ? S16 C18 1.814(3) . ? S17 C15 1.757(2) . ? S17 C19 1.808(3) . ? S18 C16 1.758(2) . ? S18 C20A 1.806(3) . ? S18 C20B 1.977(19) . ? S21 C21 1.768(2) . ? S21 C22 1.775(2) . ? S22 C21 1.763(2) . ? S22 C23 1.770(2) . ? S23 C24 1.759(2) . ? S23 C25 1.769(2) . ? S24 C26 1.761(2) . ? S24 C24 1.763(2) . ? S25 C22 1.754(2) . ? S25 C27 1.844(2) . ? S26 C23 1.745(2) . ? S26 C28 1.801(2) . ? S27 C25 1.760(2) . ? S27 C29B 1.806(5) . ? S27 C29A 1.808(5) . ? S28 C26 1.754(2) . ? S28 C30 1.817(3) . ? S31 C31 1.762(2) . ? S31 C32 1.765(2) . ? S32 C33 1.757(2) . ? S32 C31 1.768(2) . ? S33 C34 1.764(2) . ? S33 C35 1.770(2) . ? S34 C36 1.763(2) . ? S34 C34 1.764(2) . ? S35 C32 1.757(2) . ? S35 C37 1.846(2) . ? S36 C33 1.759(2) . ? S36 C38 1.809(3) . ? S37 C35 1.759(2) . ? S37 C39B 1.77(2) . ? S37 C39A 1.779(3) . ? S38 C36 1.755(2) . ? S38 C40 1.816(3) . ? C1 C3 1.406(3) 2_666 ? C1 C2 1.408(3) . ? C1 C17 1.508(3) . ? C2 C3 1.404(3) . ? C2 C27 1.516(3) . ? C3 C1 1.406(3) 2_666 ? C3 C37 1.506(3) . ? C11 C14 1.342(3) . ? C12 C13 1.353(3) . ? C15 C16 1.344(3) . ? C21 C24 1.344(3) . ? C22 C23 1.351(3) . ? C25 C26 1.349(3) . ? C31 C34 1.348(3) . ? C32 C33 1.344(3) . ? C35 C36 1.342(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 C11 S11 C12 93.82(11) . . ? C11 S12 C13 93.87(11) . . ? C15 S13 C14 94.56(11) . . ? C14 S14 C16 94.74(11) . . ? C12 S15 C17 103.82(10) . . ? C13 S16 C18 102.07(12) . . ? C15 S17 C19 100.27(11) . . ? C16 S18 C20A 102.75(13) . . ? C16 S18 C20B 95.9(6) . . ? C20A S18 C20B 113.5(6) . . ? C21 S21 C22 93.22(10) . . ? C21 S22 C23 93.70(10) . . ? C24 S23 C25 95.39(10) . . ? C26 S24 C24 95.41(10) . . ? C22 S25 C27 102.61(10) . . ? C23 S26 C28 102.29(11) . . ? C25 S27 C29B 100.2(4) . . ? C25 S27 C29A 100.3(3) . . ? C29B S27 C29A 22.7(3) . . ? C26 S28 C30 101.00(12) . . ? C31 S31 C32 94.89(10) . . ? C33 S32 C31 95.11(10) . . ? C34 S33 C35 94.56(11) . . ? C36 S34 C34 95.02(11) . . ? C32 S35 C37 94.65(10) . . ? C33 S36 C38 101.77(12) . . ? C35 S37 C39B 107.9(7) . . ? C35 S37 C39A 102.54(14) . . ? C39B S37 C39A 128.5(7) . . ? C36 S38 C40 102.32(12) . . ? C3 C1 C2 119.75(18) 2_666 . ? C3 C1 C17 119.52(18) 2_666 . ? C2 C1 C17 120.70(18) . . ? C3 C2 C1 119.85(18) . . ? C3 C2 C27 119.62(18) . . ? C1 C2 C27 120.51(18) . . ? C2 C3 C1 120.31(18) . 2_666 ? C2 C3 C37 119.68(18) . . ? C1 C3 C37 119.99(18) 2_666 . ? C14 C11 S11 123.35(18) . . ? C14 C11 S12 123.31(18) . . ? S11 C11 S12 113.33(12) . . ? C13 C12 S15 124.92(17) . . ? C13 C12 S11 116.33(17) . . ? S15 C12 S11 118.05(13) . . ? C12 C13 S16 123.79(18) . . ? C12 C13 S12 116.89(17) . . ? S16 C13 S12 119.11(13) . . ? C11 C14 S14 122.81(18) . . ? C11 C14 S13 123.59(18) . . ? S14 C14 S13 113.59(12) . . ? C16 C15 S17 126.14(19) . . ? C16 C15 S13 117.40(18) . . ? S17 C15 S13 116.43(14) . . ? C15 C16 S18 125.26(19) . . ? C15 C16 S14 116.78(18) . . ? S18 C16 S14 117.49(14) . . ? C1 C17 S15 113.38(14) . . ? C24 C21 S22 122.32(17) . . ? C24 C21 S21 124.80(17) . . ? S22 C21 S21 112.83(12) . . ? C23 C22 S25 125.69(16) . . ? C23 C22 S21 116.91(16) . . ? S25 C22 S21 117.38(12) . . ? C22 C23 S26 124.50(16) . . ? C22 C23 S22 116.43(16) . . ? S26 C23 S22 118.68(13) . . ? C21 C24 S23 123.70(17) . . ? C21 C24 S24 122.24(17) . . ? S23 C24 S24 113.99(12) . . ? C26 C25 S27 124.80(17) . . ? C26 C25 S23 116.97(17) . . ? S27 C25 S23 118.04(13) . . ? C25 C26 S28 125.86(18) . . ? C25 C26 S24 117.10(17) . . ? S28 C26 S24 116.82(13) . . ? C2 C27 S25 108.00(14) . . ? C34 C31 S31 123.70(17) . . ? C34 C31 S32 122.41(17) . . ? S31 C31 S32 113.89(12) . . ? C33 C32 S35 125.17(17) . . ? C33 C32 S31 117.42(16) . . ? S35 C32 S31 117.25(12) . . ? C32 C33 S32 117.16(16) . . ? C32 C33 S36 127.32(17) . . ? S32 C33 S36 115.50(13) . . ? C31 C34 S34 121.44(17) . . ? C31 C34 S33 124.08(18) . . ? S34 C34 S33 114.47(12) . . ? C36 C35 S37 126.23(19) . . ? C36 C35 S33 117.63(18) . . ? S37 C35 S33 116.14(13) . . ? C35 C36 S38 124.00(18) . . ? C35 C36 S34 117.13(18) . . ? S38 C36 S34 118.84(14) . . ? C3 C37 S35 111.28(14) . . ? 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 C1 C17 S15 -85.4(2) . . . . ? C1 C17 S15 C12 -31.78(17) . . . . ? C17 S15 C12 C13 -108.4(2) . . . . ? S15 C12 C13 S16 3.5(3) . . . . ? C12 C13 S16 C18 150.1(2) . . . . ? C3 C2 C27 S25 85.3(2) . . . . ? C2 C27 S25 C22 174.59(14) . . . . ? C27 S25 C22 C23 -73.0(2) . . . . ? S25 C22 C23 S26 9.2(3) . . . . ? C22 C23 S26 C28 -139.8(2) . . . . ? C2 C3 C37 S35 88.3(2) . . . . ? C3 C37 S35 C32 178.00(15) . . . . ? C37 S35 C32 C33 -89.3(2) . . . . ? S35 C32 C33 S36 -1.8(3) . . . . ? C32 C33 S36 C38 -66.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.704 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.060 #=========================================================END