# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/448 # Paper Ref B002596H data_ph80i2 loop_ _publ_contact_author_name _publ_contact_author_address 'Pr Lorcy, Dominique' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; _publ_contact_author_email Dominique.Lorcy@univ-rennes1.fr _publ_requested_journal 'J. Chem. Soc. Perkin Trans. I' loop_ _publ_author_name _publ_author_address 'Lorcy, Dominique' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; 'Hascoat, Philippe' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; 'Boubekeur, Kamal' ; FRE 2068 CNRS-Universit\'e de Nantes Institut des Mat\'eriaux Jean Rouxel BP 32229, 2, rue de la Houssini\`ere 44322 Nantes Cedex 03, France ; 'Gu\'erin, David' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; 'Carlier, Roger' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; 'Tallec, Andr\'e' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; 'Robert, Albert' ; Synth\`ese et Electrosynth\`ese Organiques UMR 6510 CNRS-Universit\'e de Rennes 1 35042 Rennes Cedex, France ; _publ_section_title ; Electrochemical Oxidative Coupling of 1,4-(bis 1,4-dithiafulven-6-yl) benzene cyclophanes ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; 1,4-(bis 1,4-dithiafulven-6-yl)benzene cyclophane ; _chemical_formula_moiety 'C28 H36 S6' _chemical_formula_sum 'C28 H36 S6' _chemical_formula_weight 564.95 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 10.510(2) _cell_length_b 13.225(3) _cell_length_c 22.293(5) _cell_angle_alpha 88.29(3) _cell_angle_beta 89.88(3) _cell_angle_gamma 72.94(3) _cell_volume 2960.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 23.62 _exptl_crystal_description needdle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Rotation, \D\f=2\%' _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 23.62 _diffrn_reflns_number 17225 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.1306 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.62 _reflns_number_total 7734 _reflns_number_gt 3147 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'INTEGRATE (Stoe IPDS)' _computing_data_collection 'EXPOSE (Stoe IPDS)' _computing_cell_refinement 'SELECT (Stoe IPDS)' _computing_data_reduction 'INTEGRATE (Stoe IPDS)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7734 _refine_ls_number_parameters 610 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.845 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1A S 0.93079(15) 0.44133(10) 0.14646(6) 0.0720(5) Uani 1 1 d . . . S2A S 1.03365(16) 0.61603(11) 0.11164(7) 0.0862(5) Uani 1 1 d . . . S3A S 0.29096(17) 0.53722(13) 0.44548(7) 0.0916(5) Uani 1 1 d . . . S4A S 0.54821(16) 0.39459(11) 0.41144(7) 0.0853(5) Uani 1 1 d . . . S5A S 0.5491(2) 0.23816(13) 0.51223(9) 0.1249(7) Uani 1 1 d . . . S6A S 1.09785(18) 0.29446(13) 0.05755(7) 0.0953(6) Uani 1 1 d . . . S1B S 0.55600(14) 0.10449(10) 0.06724(6) 0.0712(5) Uani 1 1 d . . . S2B S 0.80263(16) -0.00352(11) 0.00754(7) 0.0865(5) Uani 1 1 d . . . S3B S 0.0983(2) -0.28124(13) 0.28475(10) 0.1146(7) Uani 1 1 d . . . S4B S 0.22494(17) -0.11488(11) 0.29975(8) 0.0889(5) Uani 1 1 d . . . S5B S 0.1037(3) -0.05509(19) 0.41925(10) 0.1479(8) Uani 1 1 d . D . S6B S 0.56257(15) 0.32027(10) 0.02538(7) 0.0765(5) Uani 1 1 d . . . C1A C 0.9267(5) 0.5724(4) 0.1595(2) 0.0630(15) Uani 1 1 d . . . C2A C 0.8499(6) 0.6362(4) 0.1994(3) 0.0665(16) Uani 1 1 d . . . H2A H 0.8604 0.7036 0.1998 0.080 Uiso 1 1 calc R . . C3A C 0.7544(5) 0.6194(4) 0.2418(2) 0.0597(15) Uani 1 1 d . . . C4A C 0.6710(6) 0.7058(4) 0.2700(3) 0.0766(18) Uani 1 1 d . . . H4A H 0.6807 0.7724 0.2615 0.092 Uiso 1 1 calc R . . C5A C 0.5765(6) 0.6973(4) 0.3090(3) 0.0791(18) Uani 1 1 d . . . H5A H 0.5248 0.7582 0.3270 0.095 Uiso 1 1 calc R . . C6A C 0.5530(5) 0.6014(4) 0.3237(2) 0.0588(14) Uani 1 1 d . . . C7A C 0.6383(6) 0.5140(4) 0.2963(2) 0.0739(17) Uani 1 1 d . . . H7A H 0.6293 0.4473 0.3053 0.089 Uiso 1 1 calc R . . C8A C 0.7340(6) 0.5225(4) 0.2569(2) 0.0714(17) Uani 1 1 d . . . H8A H 0.7875 0.4616 0.2395 0.086 Uiso 1 1 calc R . . C9A C 0.4464(6) 0.5972(5) 0.3641(2) 0.0739(17) Uani 1 1 d . . . H9A H 0.3761 0.6592 0.3651 0.089 Uiso 1 1 calc R . . C10A C 0.4327(5) 0.5187(4) 0.4001(2) 0.0681(16) Uani 1 1 d . . . C11A C 0.3471(7) 0.4199(5) 0.4864(3) 0.0837(19) Uani 1 1 d . . . C12A C 0.4644(7) 0.3542(4) 0.4723(2) 0.0783(18) Uani 1 1 d . . . C13A C 0.5679(11) 0.1374(6) 0.4575(4) 0.167(4) Uani 1 1 d . . . H13A H 0.6193 0.1533 0.4242 0.200 Uiso 1 1 calc R . . H13B H 0.6189 0.0702 0.4756 0.200 Uiso 1 1 calc R . . C14A C 0.4415(10) 0.1257(6) 0.4334(4) 0.153(3) Uani 1 1 d D B . H14A H 0.3900 0.1922 0.4147 0.184 Uiso 1 1 calc R . . H14B H 0.3897 0.1086 0.4661 0.184 Uiso 1 1 calc R . . C15A C 0.4681(12) 0.0375(7) 0.3867(4) 0.213(5) Uani 1 1 d D . . H15A H 0.5415 -0.0219 0.4007 0.255 Uiso 1 1 calc R A 1 H15B H 0.3900 0.0131 0.3835 0.255 Uiso 1 1 calc R A 1 C16A C 0.5017(13) 0.0749(10) 0.3238(6) 0.161(5) Uiso 0.70 1 d PD B 1 H16A H 0.4270 0.0826 0.2968 0.193 Uiso 0.70 1 calc PR B 1 H16B H 0.5174 0.1433 0.3264 0.193 Uiso 0.70 1 calc PR B 1 C160 C 0.595(3) 0.051(4) 0.3579(13) 0.30(3) Uiso 0.30 1 d PD B 2 H16C H 0.5886 0.1254 0.3533 0.360 Uiso 0.30 1 calc PR B 2 H16D H 0.6716 0.0170 0.3832 0.360 Uiso 0.30 1 calc PR B 2 C17A C 0.6105(11) 0.0047(7) 0.3019(5) 0.195(4) Uani 1 1 d D . . H17A H 0.5849 -0.0545 0.2867 0.234 Uiso 1 1 calc R B 1 H17B H 0.6732 -0.0222 0.3346 0.234 Uiso 1 1 calc R B 1 C18A C 0.6832(13) 0.0501(8) 0.2503(4) 0.196(5) Uani 1 1 d D B . H18A H 0.6211 0.0764 0.2173 0.235 Uiso 1 1 calc R . . H18B H 0.7088 0.1095 0.2653 0.235 Uiso 1 1 calc R . . C19A C 0.7920(13) -0.0214(8) 0.2295(5) 0.211(5) Uani 1 1 d D . . H19A H 0.7649 -0.0781 0.2118 0.253 Uiso 1 1 calc R B . H19B H 0.8503 -0.0519 0.2632 0.253 Uiso 1 1 calc R . . C20A C 0.8732(11) 0.0233(9) 0.1817(5) 0.195(5) Uani 1 1 d . B . H20A H 0.9279 -0.0370 0.1605 0.235 Uiso 1 1 calc R . . H20B H 0.8091 0.0654 0.1527 0.235 Uiso 1 1 calc R . . C21A C 0.9559(11) 0.0838(8) 0.1967(4) 0.178(4) Uani 1 1 d . . . H21A H 1.0164 0.0462 0.2282 0.213 Uiso 1 1 calc R B . H21B H 0.9015 0.1495 0.2130 0.213 Uiso 1 1 calc R . . C22A C 1.0354(8) 0.1094(7) 0.1468(4) 0.128(3) Uani 1 1 d . B . H22A H 0.9755 0.1479 0.1153 0.154 Uiso 1 1 calc R . . H22B H 1.0903 0.0441 0.1303 0.154 Uiso 1 1 calc R . . C23A C 1.1257(9) 0.1762(5) 0.1662(3) 0.123(3) Uani 1 1 d . . . H23A H 1.0717 0.2391 0.1854 0.148 Uiso 1 1 calc R B . H23B H 1.1901 0.1355 0.1955 0.148 Uiso 1 1 calc R . . C24A C 1.1974(7) 0.2083(5) 0.1151(4) 0.109(2) Uani 1 1 d . B . H24A H 1.2504 0.1446 0.0962 0.131 Uiso 1 1 calc R . . H24B H 1.2587 0.2432 0.1311 0.131 Uiso 1 1 calc R . . C25A C 1.0540(5) 0.4192(4) 0.0910(2) 0.0685(16) Uani 1 1 d . . . C26A C 1.1020(6) 0.4979(4) 0.0747(2) 0.0700(16) Uani 1 1 d . . . C27A C 0.2569(7) 0.3998(5) 0.5364(3) 0.119(2) Uani 1 1 d . . . H27A H 0.1770 0.4581 0.5374 0.178 Uiso 1 1 calc R . . H27B H 0.3025 0.3926 0.5742 0.178 Uiso 1 1 calc R . . H27C H 0.2344 0.3359 0.5289 0.178 Uiso 1 1 calc R . . C28A C 1.2047(6) 0.4992(4) 0.0286(2) 0.0907(19) Uani 1 1 d . . . H28A H 1.2172 0.5682 0.0260 0.136 Uiso 1 1 calc R . . H28B H 1.1757 0.4824 -0.0097 0.136 Uiso 1 1 calc R . . H28C H 1.2872 0.4478 0.0397 0.136 Uiso 1 1 calc R . . C1B C 0.6727(5) -0.0175(4) 0.0523(2) 0.0649(16) Uani 1 1 d . . . C2B C 0.6650(6) -0.1129(5) 0.0701(2) 0.0733(17) Uani 1 1 d . . . H2B H 0.7348 -0.1691 0.0572 0.088 Uiso 1 1 calc R . . C3B C 0.5675(6) -0.1439(4) 0.1059(2) 0.0656(16) Uani 1 1 d . . . C4B C 0.5662(7) -0.2494(5) 0.1071(3) 0.0816(19) Uani 1 1 d . . . H4B H 0.6301 -0.2980 0.0852 0.098 Uiso 1 1 calc R . . C5B C 0.4765(8) -0.2840(4) 0.1384(3) 0.0823(19) Uani 1 1 d . . . H5B H 0.4791 -0.3547 0.1367 0.099 Uiso 1 1 calc R . . C6B C 0.3807(7) -0.2168(5) 0.1732(3) 0.0734(17) Uani 1 1 d . . . C7B C 0.3812(6) -0.1116(4) 0.1740(3) 0.0842(19) Uani 1 1 d . . . H7B H 0.3193 -0.0641 0.1973 0.101 Uiso 1 1 calc R . . C8B C 0.4705(7) -0.0774(4) 0.1413(3) 0.0820(19) Uani 1 1 d . . . H8B H 0.4668 -0.0063 0.1425 0.098 Uiso 1 1 calc R . . C9B C 0.2854(7) -0.2561(4) 0.2061(3) 0.087(2) Uani 1 1 d . . . H9B H 0.2719 -0.3169 0.1909 0.105 Uiso 1 1 calc R . . C10B C 0.2133(6) -0.2201(4) 0.2548(3) 0.0787(18) Uani 1 1 d . . . C11B C 0.0610(7) -0.2120(6) 0.3484(3) 0.103(2) Uani 1 1 d . . . C12B C 0.1180(7) -0.1337(5) 0.3567(3) 0.095(2) Uani 1 1 d . . . C13B C -0.0248(13) 0.0670(9) 0.3850(5) 0.258(6) Uani 1 1 d D . . H13C H -0.0158 0.0770 0.3421 0.310 Uiso 1 1 calc R C 3 H13D H -0.1161 0.0727 0.3957 0.310 Uiso 1 1 calc R C 3 C14B C 0.038(3) 0.1296(15) 0.4218(12) 0.339(18) Uiso 0.60 1 d PD D 3 H14C H 0.0361 0.1089 0.4638 0.407 Uiso 0.60 1 calc PR D 3 H14D H 0.1299 0.1177 0.4101 0.407 Uiso 0.60 1 calc PR D 3 C140 C -0.089(3) 0.1688(17) 0.4055(15) 0.230(14) Uiso 0.40 1 d PD D 4 H14E H -0.1637 0.1982 0.3784 0.276 Uiso 0.40 1 calc PR D 4 H14F H -0.1269 0.1581 0.4440 0.276 Uiso 0.40 1 calc PR D 4 C15B C -0.0363(15) 0.2416(13) 0.4126(8) 0.311(8) Uani 1 1 d D . . H15C H -0.1298 0.2474 0.4073 0.374 Uiso 1 1 calc R D 3 H15D H -0.0280 0.2789 0.4485 0.374 Uiso 1 1 calc R D 3 C16B C 0.0057(15) 0.2920(8) 0.3630(5) 0.258(8) Uani 1 1 d D D . H16E H -0.0712 0.3257 0.3379 0.310 Uiso 1 1 calc R E 5 H16F H 0.0666 0.2384 0.3395 0.310 Uiso 1 1 calc R E 5 C17B C 0.070(2) 0.3702(16) 0.3780(7) 0.133(9) Uiso 0.50 1 d PD D 5 H17C H 0.1515 0.3374 0.4004 0.159 Uiso 0.50 1 calc PR D 5 H17D H 0.0120 0.4240 0.4023 0.159 Uiso 0.50 1 calc PR D 5 C170 C 0.023(3) 0.3926(16) 0.3682(10) 0.189(14) Uiso 0.50 1 d PD D 6 H17E H 0.0679 0.3949 0.4059 0.227 Uiso 0.50 1 calc PR D 6 H17F H -0.0634 0.4451 0.3690 0.227 Uiso 0.50 1 calc PR D 6 C18B C 0.1020(9) 0.4201(6) 0.3181(3) 0.146(3) Uani 1 1 d D . . H18C H 0.0375 0.4164 0.2878 0.175 Uiso 1 1 calc R D 5 H18D H 0.0941 0.4941 0.3237 0.175 Uiso 1 1 calc R D 5 C19B C 0.2315(8) 0.3678(6) 0.2979(3) 0.118(2) Uani 1 1 d D D . H19C H 0.2350 0.2952 0.2904 0.142 Uiso 1 1 calc R . . H19D H 0.2930 0.3658 0.3306 0.142 Uiso 1 1 calc R . . C20B C 0.2826(7) 0.4105(5) 0.2437(3) 0.103(2) Uani 1 1 d . . . H20C H 0.2208 0.4137 0.2110 0.123 Uiso 1 1 calc R D . H20D H 0.2812 0.4827 0.2514 0.123 Uiso 1 1 calc R . . C21B C 0.4178(7) 0.3529(5) 0.2231(3) 0.103(2) Uani 1 1 d . D . H21C H 0.4219 0.2793 0.2188 0.123 Uiso 1 1 calc R . . H21D H 0.4809 0.3554 0.2543 0.123 Uiso 1 1 calc R . . C22B C 0.4624(7) 0.3919(4) 0.1656(3) 0.096(2) Uani 1 1 d . . . H22C H 0.4547 0.4665 0.1689 0.116 Uiso 1 1 calc R D . H22D H 0.4031 0.3854 0.1336 0.116 Uiso 1 1 calc R . . C23B C 0.6046(7) 0.3335(5) 0.1485(3) 0.096(2) Uani 1 1 d . D . H23C H 0.6648 0.3485 0.1774 0.116 Uiso 1 1 calc R . . H23D H 0.6159 0.2580 0.1510 0.116 Uiso 1 1 calc R . . C24B C 0.6430(6) 0.3614(4) 0.0874(3) 0.0933(19) Uani 1 1 d . . . H24C H 0.7383 0.3306 0.0834 0.112 Uiso 1 1 calc R D . H24D H 0.6246 0.4376 0.0842 0.112 Uiso 1 1 calc R . . C25B C 0.6389(5) 0.1824(4) 0.0275(2) 0.0597(14) Uani 1 1 d . . . C26B C 0.7510(6) 0.1331(4) -0.0007(2) 0.0645(15) Uani 1 1 d . D . C27B C -0.0355(8) -0.2386(5) 0.3925(4) 0.150(3) Uani 1 1 d . . . H27D H -0.0658 -0.2947 0.3772 0.224 Uiso 1 1 calc R . . H27E H -0.1103 -0.1772 0.3977 0.224 Uiso 1 1 calc R . . H27F H 0.0084 -0.2607 0.4304 0.224 Uiso 1 1 calc R . . C28B C 0.8370(6) 0.1823(4) -0.0379(2) 0.0860(18) Uani 1 1 d . . . H28D H 0.9113 0.1278 -0.0527 0.129 Uiso 1 1 calc R D . H28E H 0.8687 0.2289 -0.0138 0.129 Uiso 1 1 calc R . . H28F H 0.7860 0.2218 -0.0711 0.129 Uiso 1 1 calc 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 S1A 0.0759(11) 0.0698(9) 0.0781(10) -0.0174(8) 0.0206(9) -0.0326(8) S2A 0.0830(13) 0.0721(10) 0.1040(13) 0.0096(9) 0.0248(10) -0.0249(9) S3A 0.0780(13) 0.1100(13) 0.0848(12) 0.0006(10) 0.0164(10) -0.0247(10) S4A 0.0953(13) 0.0750(10) 0.0860(12) -0.0049(8) 0.0181(10) -0.0255(9) S5A 0.174(2) 0.0882(13) 0.1104(15) 0.0092(11) -0.0032(14) -0.0358(13) S6A 0.1025(14) 0.1052(12) 0.0832(12) -0.0368(10) 0.0231(11) -0.0353(11) S1B 0.0627(11) 0.0665(9) 0.0812(11) -0.0130(8) 0.0099(8) -0.0129(8) S2B 0.0832(13) 0.0781(10) 0.0888(12) -0.0147(9) 0.0270(10) -0.0081(9) S3B 0.1049(15) 0.0976(12) 0.1559(19) 0.0037(12) 0.0043(14) -0.0533(11) S4B 0.0932(13) 0.0732(10) 0.1039(13) 0.0007(9) 0.0019(11) -0.0305(9) S5B 0.163(2) 0.1641(19) 0.1185(17) -0.0180(15) 0.0172(15) -0.0503(17) S6B 0.0742(12) 0.0704(10) 0.0807(11) -0.0107(8) 0.0058(9) -0.0136(8) C1A 0.062(4) 0.062(3) 0.067(4) 0.006(3) 0.003(3) -0.021(3) C2A 0.070(4) 0.054(3) 0.080(4) 0.004(3) 0.004(4) -0.024(3) C3A 0.063(4) 0.057(4) 0.061(4) -0.002(3) 0.005(3) -0.019(3) C4A 0.091(5) 0.047(4) 0.090(5) -0.003(3) 0.031(4) -0.019(3) C5A 0.098(5) 0.053(4) 0.075(4) -0.004(3) 0.023(4) -0.004(4) C6A 0.051(4) 0.068(4) 0.056(4) -0.002(3) 0.004(3) -0.015(3) C7A 0.094(5) 0.063(4) 0.073(4) -0.016(3) 0.020(4) -0.035(4) C8A 0.085(5) 0.061(4) 0.072(4) -0.022(3) 0.028(4) -0.026(3) C9A 0.070(5) 0.083(4) 0.057(4) -0.002(3) 0.003(4) -0.005(4) C10A 0.065(4) 0.081(4) 0.058(4) -0.004(3) 0.005(3) -0.021(3) C11A 0.095(5) 0.091(5) 0.077(5) -0.015(4) 0.010(4) -0.045(4) C12A 0.111(6) 0.075(4) 0.057(4) -0.002(3) 0.000(4) -0.041(4) C13A 0.228(12) 0.098(6) 0.168(9) 0.011(5) 0.021(8) -0.040(7) C14A 0.208(11) 0.133(7) 0.149(8) -0.003(6) -0.026(7) -0.097(7) C15A 0.332(16) 0.192(9) 0.167(9) -0.045(8) 0.080(9) -0.156(10) C17A 0.225(12) 0.166(8) 0.192(11) -0.043(8) 0.049(9) -0.052(8) C18A 0.279(15) 0.157(9) 0.114(8) 0.034(7) 0.025(8) -0.008(9) C19A 0.269(16) 0.178(10) 0.161(10) 0.043(8) 0.002(10) -0.032(10) C20A 0.168(11) 0.274(12) 0.182(11) 0.113(9) -0.040(8) -0.136(9) C21A 0.137(10) 0.233(11) 0.120(8) 0.058(8) -0.005(8) 0.006(8) C22A 0.085(6) 0.181(8) 0.103(6) 0.022(6) 0.008(5) -0.016(6) C23A 0.122(8) 0.102(5) 0.110(7) -0.025(5) -0.024(6) 0.027(5) C24A 0.080(5) 0.084(5) 0.157(7) -0.049(5) -0.004(5) -0.008(4) C25A 0.064(4) 0.086(4) 0.064(4) -0.010(3) 0.012(3) -0.033(3) C26A 0.054(4) 0.088(4) 0.064(4) 0.005(3) 0.008(3) -0.015(3) C27A 0.138(7) 0.152(6) 0.083(5) -0.011(4) 0.022(5) -0.068(5) C28A 0.077(5) 0.104(4) 0.083(4) 0.014(3) 0.024(4) -0.015(4) C1B 0.071(4) 0.065(4) 0.060(4) -0.012(3) -0.001(3) -0.022(3) C2B 0.079(5) 0.072(4) 0.067(4) -0.020(3) 0.009(4) -0.018(4) C3B 0.084(5) 0.047(4) 0.065(4) -0.010(3) -0.012(4) -0.018(4) C4B 0.101(6) 0.067(5) 0.073(4) -0.018(3) 0.005(4) -0.019(4) C5B 0.114(6) 0.052(4) 0.079(5) -0.016(4) -0.007(4) -0.022(4) C6B 0.086(5) 0.065(5) 0.077(4) 0.004(4) -0.017(4) -0.035(4) C7B 0.091(5) 0.058(4) 0.104(5) -0.003(3) 0.014(4) -0.023(4) C8B 0.096(5) 0.052(4) 0.099(5) -0.006(3) 0.021(4) -0.022(4) C9B 0.107(6) 0.062(4) 0.097(5) -0.005(4) -0.012(5) -0.031(4) C10B 0.080(5) 0.060(4) 0.104(5) 0.017(4) -0.021(4) -0.035(3) C11B 0.080(6) 0.092(5) 0.129(7) 0.034(5) 0.007(5) -0.017(4) C12B 0.092(6) 0.092(5) 0.091(5) 0.013(4) -0.003(4) -0.015(4) C13B 0.273(14) 0.256(12) 0.231(12) -0.158(11) 0.002(11) -0.040(11) C15B 0.251(16) 0.38(2) 0.35(2) -0.075(18) 0.164(16) -0.162(17) C16B 0.335(19) 0.178(10) 0.241(14) 0.030(9) 0.145(13) -0.046(11) C18B 0.132(8) 0.183(8) 0.119(7) -0.001(6) 0.039(6) -0.041(6) C19B 0.123(7) 0.157(6) 0.078(5) -0.013(5) 0.012(5) -0.044(6) C20B 0.120(7) 0.102(5) 0.086(5) -0.020(4) 0.023(5) -0.029(5) C21B 0.106(6) 0.119(5) 0.094(5) -0.022(4) -0.002(5) -0.048(5) C22B 0.105(6) 0.093(4) 0.100(6) -0.011(4) 0.026(5) -0.042(4) C23B 0.102(6) 0.108(5) 0.093(5) -0.024(4) -0.003(4) -0.050(4) C24B 0.092(5) 0.098(4) 0.098(5) -0.018(4) 0.020(4) -0.039(4) C25B 0.055(4) 0.071(4) 0.057(3) -0.004(3) 0.004(3) -0.024(3) C26B 0.057(4) 0.081(4) 0.052(4) -0.005(3) 0.000(3) -0.015(3) C27B 0.109(7) 0.158(7) 0.178(8) 0.054(6) 0.026(6) -0.041(5) C28B 0.077(5) 0.094(4) 0.082(4) -0.010(3) 0.016(4) -0.018(4) _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 S1A C1A 1.754(5) . ? S1A C25A 1.756(5) . ? S2A C26A 1.747(5) . ? S2A C1A 1.753(5) . ? S3A C11A 1.722(6) . ? S3A C10A 1.759(6) . ? S4A C10A 1.744(5) . ? S4A C12A 1.769(6) . ? S5A C12A 1.749(6) . ? S5A C13A 1.801(9) . ? S6A C25A 1.765(5) . ? S6A C24A 1.805(7) . ? S1B C25B 1.754(5) . ? S1B C1B 1.758(5) . ? S2B C26B 1.732(5) . ? S2B C1B 1.739(6) . ? S3B C11B 1.695(8) . ? S3B C10B 1.760(6) . ? S4B C12B 1.754(7) . ? S4B C10B 1.772(6) . ? S5B C12B 1.744(7) . ? S5B C13B 1.914(12) . ? S6B C25B 1.763(5) . ? S6B C24B 1.801(6) . ? C1A C2A 1.342(6) . ? C2A C3A 1.437(7) . ? C3A C4A 1.385(6) . ? C3A C8A 1.392(6) . ? C4A C5A 1.346(7) . ? C5A C6A 1.391(7) . ? C6A C7A 1.395(6) . ? C6A C9A 1.449(7) . ? C7A C8A 1.362(6) . ? C9A C10A 1.334(7) . ? C11A C12A 1.326(7) . ? C11A C27A 1.530(8) . ? C13A C14A 1.486(10) . ? C14A C15A 1.549(10) . ? C15A C160 1.535(19) . ? C15A C16A 1.548(11) . ? C16A C17A 1.344(10) . ? C160 C17A 1.393(18) . ? C17A C18A 1.579(10) . ? C18A C19A 1.344(10) . ? C19A C20A 1.573(13) . ? C20A C21A 1.390(12) . ? C21A C22A 1.480(11) . ? C22A C23A 1.543(10) . ? C23A C24A 1.484(9) . ? C25A C26A 1.325(7) . ? C26A C28A 1.492(7) . ? C1B C2B 1.337(7) . ? C2B C3B 1.442(7) . ? C3B C8B 1.395(7) . ? C3B C4B 1.399(7) . ? C4B C5B 1.347(7) . ? C5B C6B 1.385(7) . ? C6B C7B 1.393(7) . ? C6B C9B 1.445(8) . ? C7B C8B 1.359(7) . ? C9B C10B 1.339(8) . ? C11B C12B 1.356(8) . ? C11B C27B 1.517(9) . ? C13B C140 1.407(18) . ? C13B C14B 1.468(18) . ? C14B C15B 1.466(13) . ? C140 C15B 1.26(3) . ? C15B C16B 1.410(14) . ? C16B C170 1.404(16) . ? C16B C17B 1.440(15) . ? C17B C18B 1.549(14) . ? C170 C18B 1.487(15) . ? C18B C19B 1.414(8) . ? C19B C20B 1.483(8) . ? C20B C21B 1.482(8) . ? C21B C22B 1.492(8) . ? C22B C23B 1.521(7) . ? C23B C24B 1.485(7) . ? C25B C26B 1.333(6) . ? C26B C28B 1.496(7) . ? 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 C1A S1A C25A 96.1(3) . . ? C26A S2A C1A 97.9(3) . . ? C11A S3A C10A 96.5(3) . . ? C10A S4A C12A 95.9(3) . . ? C12A S5A C13A 103.2(3) . . ? C25A S6A C24A 102.8(3) . . ? C25B S1B C1B 95.8(3) . . ? C26B S2B C1B 98.0(3) . . ? C11B S3B C10B 98.3(4) . . ? C12B S4B C10B 96.7(3) . . ? C12B S5B C13B 96.4(3) . . ? C25B S6B C24B 101.7(3) . . ? C2A C1A S2A 121.7(4) . . ? C2A C1A S1A 126.2(4) . . ? S2A C1A S1A 112.1(3) . . ? C1A C2A C3A 131.7(5) . . ? C4A C3A C8A 115.3(5) . . ? C4A C3A C2A 119.0(5) . . ? C8A C3A C2A 125.7(5) . . ? C5A C4A C3A 122.7(5) . . ? C4A C5A C6A 122.8(5) . . ? C5A C6A C7A 114.6(5) . . ? C5A C6A C9A 120.7(5) . . ? C7A C6A C9A 124.7(5) . . ? C8A C7A C6A 122.6(5) . . ? C7A C8A C3A 121.9(5) . . ? C10A C9A C6A 130.5(5) . . ? C9A C10A S4A 126.6(5) . . ? C9A C10A S3A 120.4(4) . . ? S4A C10A S3A 112.9(3) . . ? C12A C11A C27A 125.0(6) . . ? C12A C11A S3A 118.0(5) . . ? C27A C11A S3A 117.0(5) . . ? C11A C12A S5A 126.0(5) . . ? C11A C12A S4A 116.3(5) . . ? S5A C12A S4A 117.4(4) . . ? C14A C13A S5A 115.2(7) . . ? C13A C14A C15A 111.3(9) . . ? C160 C15A C16A 46.0(15) . . ? C160 C15A C14A 99.9(12) . . ? C16A C15A C14A 112.9(8) . . ? C17A C16A C15A 110.4(10) . . ? C17A C160 C15A 108.5(18) . . ? C16A C17A C160 52.1(17) . . ? C16A C17A C18A 114.8(10) . . ? C160 C17A C18A 119.3(16) . . ? C19A C18A C17A 113.5(9) . . ? C18A C19A C20A 114.9(10) . . ? C21A C20A C19A 122.9(11) . . ? C20A C21A C22A 115.4(11) . . ? C21A C22A C23A 113.1(9) . . ? C24A C23A C22A 112.7(7) . . ? C23A C24A S6A 117.2(5) . . ? C26A C25A S1A 118.6(4) . . ? C26A C25A S6A 124.5(4) . . ? S1A C25A S6A 116.8(3) . . ? C25A C26A C28A 128.6(5) . . ? C25A C26A S2A 115.2(4) . . ? C28A C26A S2A 116.1(4) . . ? C2B C1B S2B 121.4(4) . . ? C2B C1B S1B 126.0(5) . . ? S2B C1B S1B 112.5(3) . . ? C1B C2B C3B 131.3(5) . . ? C8B C3B C4B 114.6(6) . . ? C8B C3B C2B 125.9(5) . . ? C4B C3B C2B 119.5(6) . . ? C5B C4B C3B 123.0(6) . . ? C4B C5B C6B 121.7(6) . . ? C5B C6B C7B 116.7(7) . . ? C5B C6B C9B 120.4(6) . . ? C7B C6B C9B 122.9(6) . . ? C8B C7B C6B 121.1(6) . . ? C7B C8B C3B 123.0(5) . . ? C10B C9B C6B 131.1(6) . . ? C9B C10B S3B 121.9(5) . . ? C9B C10B S4B 126.9(5) . . ? S3B C10B S4B 111.1(4) . . ? C12B C11B C27B 123.4(7) . . ? C12B C11B S3B 117.6(6) . . ? C27B C11B S3B 119.0(6) . . ? C11B C12B S5B 127.2(6) . . ? C11B C12B S4B 116.0(5) . . ? S5B C12B S4B 116.7(5) . . ? C140 C13B C14B 55.0(15) . . ? C140 C13B S5B 134.1(16) . . ? C14B C13B S5B 86.4(10) . . ? C15B C14B C13B 108.2(16) . . ? C15B C140 C13B 126(2) . . ? C140 C15B C16B 121(2) . . ? C140 C15B C14B 57.8(16) . . ? C16B C15B C14B 114.5(16) . . ? C170 C16B C15B 120.5(13) . . ? C170 C16B C17B 21.8(17) . . ? C15B C16B C17B 114.9(13) . . ? C16B C17B C18B 107.2(12) . . ? C16B C170 C18B 112.7(14) . . ? C19B C18B C170 130.7(13) . . ? C19B C18B C17B 111.7(11) . . ? C170 C18B C17B 20.3(16) . . ? C18B C19B C20B 119.0(7) . . ? C21B C20B C19B 117.6(6) . . ? C20B C21B C22B 116.6(6) . . ? C21B C22B C23B 114.2(6) . . ? C24B C23B C22B 114.3(6) . . ? C23B C24B S6B 116.5(4) . . ? C26B C25B S1B 117.9(4) . . ? C26B C25B S6B 125.1(4) . . ? S1B C25B S6B 116.9(3) . . ? C25B C26B C28B 127.5(5) . . ? C25B C26B S2B 115.8(5) . . ? C28B C26B S2B 116.7(4) . . ? _refine_diff_density_max 0.268 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.045 #=====END