# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jerry Atwood' _publ_contact_author_email ATWOODJ@MISSOURI.EDU _publ_section_title ; Dimeric Nanocapsule Induces Conformational Change ; loop_ _publ_author_name 'Andrew Maerz' 'Carol Deakyne' 'Andrew Maerz' 'Nicholas P. Power' 'Haunani Thomas' # Attachment 'PGPHDMSO.CIF' data_PgPhDMSO _database_code_depnum_ccdc_archive 'CCDC 752684' #TrackingRef 'PGPHDMSO.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H50 O11 S5' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour violet _diffrn_ambient_temperature 173(2) _chemical_formula_weight 819.06 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' 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6125(2) _cell_length_b 11.8904(2) _cell_length_c 16.1797(3) _cell_angle_alpha 80.9620(10) _cell_angle_beta 74.9120(10) _cell_angle_gamma 71.9090(10) _cell_volume 2043.31(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7369 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.6 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of G\"ottingen, Germany). ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 27263 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 30.58 _reflns_number_total 12161 _reflns_number_gt 8205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (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. The final model contains five DMSO molecules, two with significant disorder. The disordered DMSO molecules give a number of errors with CHECKCIF. ; _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12161 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1429 _refine_ls_R_factor_gt 0.1109 _refine_ls_wR_factor_ref 0.3908 _refine_ls_wR_factor_gt 0.3534 _refine_ls_goodness_of_fit_ref 1.492 _refine_ls_restrained_S_all 1.492 _refine_ls_shift/su_max 0.014 _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 S1S S 0.32310(9) 0.93257(9) 0.42142(8) 0.0539(3) Uani 1 1 d . . . S2S S 0.71471(15) 1.01822(12) 0.20458(9) 0.0763(4) Uani 1 1 d . . . C14 C 0.6858(2) 0.5513(2) 0.63724(16) 0.0237(5) Uani 1 1 d . . . H14 H 0.7119 0.6122 0.6584 0.028 Uiso 1 1 calc R . . C7 C 0.7665(2) 0.4549(2) 0.32524(16) 0.0245(5) Uani 1 1 d . . . H7 H 0.8229 0.4871 0.2759 0.029 Uiso 1 1 calc R . . C6 C 0.4434(2) 0.4445(2) 0.30827(15) 0.0233(5) Uani 1 1 d . . . O4 O 0.6392(2) 0.78984(18) 0.57246(14) 0.0357(5) Uani 1 1 d . . . H4 H 0.6153 0.8587 0.5492 0.043 Uiso 1 1 calc R . . C1 C 0.5399(2) 0.4559(2) 0.34052(15) 0.0225(5) Uani 1 1 d . . . H1 H 0.5236 0.4692 0.3994 0.027 Uiso 1 1 calc R . . O5 O 0.6602(2) 0.86380(19) 0.39763(15) 0.0407(5) Uani 1 1 d . . . H5 H 0.5871 0.9042 0.4171 0.049 Uiso 1 1 calc R . . O6 O 0.7115(2) 0.69754(19) 0.28201(13) 0.0370(5) Uani 1 1 d . . . H6 H 0.6997 0.7714 0.2742 0.044 Uiso 1 1 calc R . . C8 C 0.7173(2) 0.5080(2) 0.48105(16) 0.0233(5) Uani 1 1 d . . . H8 H 0.7323 0.4260 0.4997 0.028 Uiso 1 1 calc R . . C12 C 0.7027(2) 0.6628(2) 0.36713(17) 0.0270(5) Uani 1 1 d . . . C2 C 0.6592(2) 0.4485(2) 0.28969(16) 0.0242(5) Uani 1 1 d . . . O3 O 0.3768(2) 0.4183(2) 0.18722(13) 0.0400(5) Uani 1 1 d . . . H3 H 0.3977 0.4253 0.1333 0.048 Uiso 1 1 calc R . . C21 C 0.7841(2) 0.4339(3) 0.64882(17) 0.0279(5) Uani 1 1 d . . . O1 O 0.80054(19) 0.4161(3) 0.15474(13) 0.0427(6) Uani 1 1 d . . . H1A H 0.8058 0.3928 0.1071 0.051 Uiso 1 1 calc R . . C11 C 0.6736(2) 0.7464(2) 0.42725(18) 0.0279(5) Uani 1 1 d . . . C9 C 0.6872(2) 0.5895(2) 0.54243(16) 0.0233(5) Uani 1 1 d . . . C13 C 0.7261(2) 0.5425(2) 0.39339(16) 0.0233(5) Uani 1 1 d . . . C10 C 0.6655(2) 0.7094(2) 0.51429(17) 0.0260(5) Uani 1 1 d . . . C5 C 0.4687(3) 0.4283(3) 0.22036(17) 0.0298(6) Uani 1 1 d . . . C4 C 0.5872(3) 0.4212(3) 0.16838(17) 0.0340(6) Uani 1 1 d . . . C15 C 0.8454(3) 0.3323(3) 0.35404(18) 0.0317(6) Uani 1 1 d . . . O2 O 0.6100(2) 0.4006(3) 0.08346(14) 0.0478(6) Uani 1 1 d . . . H2 H 0.6374 0.4543 0.0521 0.057 Uiso 1 1 calc R . . C3 C 0.6828(2) 0.4279(3) 0.20413(17) 0.0300(6) Uani 1 1 d . . . O1S O 0.4187(3) 0.9691(2) 0.4507(2) 0.0517(7) Uani 1 1 d . . . C26 C 0.7604(3) 0.3373(3) 0.7021(2) 0.0425(7) Uani 1 1 d . . . H26 H 0.6779 0.3413 0.7332 0.051 Uiso 1 1 calc R . . C16 C 0.9597(3) 0.3231(4) 0.3703(3) 0.0516(10) Uani 1 1 d . . . H16 H 0.9877 0.3917 0.3642 0.062 Uiso 1 1 calc R . . C22 C 0.9071(3) 0.4244(4) 0.6043(2) 0.0449(8) Uani 1 1 d . . . H22 H 0.9263 0.4904 0.5682 0.054 Uiso 1 1 calc R . . O2S O 0.6667(5) 0.9175(3) 0.1987(2) 0.0844(12) Uani 1 1 d . . . C20 C 0.8091(4) 0.2308(3) 0.3615(3) 0.0494(8) Uani 1 1 d . . . H20 H 0.7322 0.2351 0.3490 0.059 Uiso 1 1 calc R . . C25 C 0.8553(4) 0.2344(4) 0.7109(3) 0.0612(11) Uani 1 1 d . . . H25 H 0.8371 0.1693 0.7487 0.073 Uiso 1 1 calc R . . C23 C 1.0014(3) 0.3206(5) 0.6120(3) 0.0607(12) Uani 1 1 d . . . H23 H 1.0840 0.3149 0.5803 0.073 Uiso 1 1 calc R . . C24 C 0.9744(4) 0.2252(4) 0.6659(3) 0.0645(13) Uani 1 1 d . . . H24 H 1.0385 0.1538 0.6717 0.077 Uiso 1 1 calc R . . C18 C 0.9963(5) 0.1107(4) 0.4035(3) 0.0727(15) Uani 1 1 d . . . H18 H 1.0477 0.0355 0.4199 0.087 Uiso 1 1 calc R . . C1S C 0.3745(5) 0.7743(4) 0.4262(4) 0.0676(13) Uani 1 1 d . . . H1S1 H 0.3654 0.7420 0.4864 0.101 Uiso 1 1 calc R . . H1S2 H 0.4620 0.7484 0.3962 0.101 Uiso 1 1 calc R . . H1S3 H 0.3242 0.7457 0.3987 0.101 Uiso 1 1 calc R . . C17 C 1.0338(4) 0.2112(5) 0.3958(3) 0.0762(17) Uani 1 1 d . . . H17 H 1.1114 0.2052 0.4079 0.091 Uiso 1 1 calc R . . C19 C 0.8855(5) 0.1205(4) 0.3874(4) 0.0712(13) Uani 1 1 d . . . H19 H 0.8582 0.0515 0.3936 0.085 Uiso 1 1 calc R . . C2S C 0.3484(6) 0.9668(6) 0.3092(4) 0.0836(16) Uani 1 1 d . . . H2S1 H 0.3235 1.0531 0.2965 0.125 Uiso 1 1 calc R . . H2S2 H 0.2990 0.9316 0.2858 0.125 Uiso 1 1 calc R . . H2S3 H 0.4368 0.9346 0.2829 0.125 Uiso 1 1 calc R . . C4S C 0.5959(6) 1.1222(5) 0.2665(4) 0.0878(17) Uani 1 1 d . . . H4S1 H 0.5818 1.0903 0.3267 0.132 Uiso 1 1 calc R . . H4S2 H 0.5194 1.1391 0.2460 0.132 Uiso 1 1 calc R . . H4S3 H 0.6198 1.1956 0.2614 0.132 Uiso 1 1 calc R . . C3S C 0.7212(12) 1.0984(8) 0.1010(5) 0.147(4) Uani 1 1 d . . . H3S1 H 0.7861 1.0502 0.0582 0.220 Uiso 1 1 calc R . . H3S2 H 0.7404 1.1727 0.1023 0.220 Uiso 1 1 calc R . . H3S3 H 0.6407 1.1163 0.0858 0.220 Uiso 1 1 calc R . . S3S S 0.1674(2) 0.1000(2) 0.09756(14) 0.1236(8) Uani 1 1 d . . . S4S S 0.8983(2) 0.3366(3) -0.08031(13) 0.0673(7) Uani 0.50 1 d P . . S4S' S 0.9562(3) 0.4055(4) -0.0616(2) 0.0820(11) Uani 0.40 1 d P A 1 O4S O 0.9026(5) 0.3285(6) 0.0031(3) 0.137(2) Uani 1 1 d . A . O3S O 0.2587(6) -0.0011(5) 0.1308(5) 0.141(2) Uani 1 1 d . . . C8S C 0.9156(9) 0.4447(11) -0.1553(6) 0.152(4) Uani 1 1 d . . . H8S1 H 0.8914 0.5315 -0.1653 0.227 Uiso 1 1 calc R A 1 H8S2 H 0.8453 0.4153 -0.1545 0.227 Uiso 1 1 calc R A 1 H8S3 H 0.9860 0.4106 -0.2013 0.227 Uiso 1 1 calc R A 1 C5S C 0.1361(15) 0.2184(9) 0.1575(7) 0.181(6) Uani 1 1 d . . . H5S1 H 0.2090 0.2484 0.1447 0.271 Uiso 1 1 calc R . . H5S2 H 0.1165 0.1923 0.2188 0.271 Uiso 1 1 calc R . . H5S3 H 0.0650 0.2816 0.1432 0.271 Uiso 1 1 calc R . . C7S C 1.0393(14) 0.2367(14) -0.1270(11) 0.104(4) Uiso 0.50 1 d P A . H7S1 H 1.0446 0.2372 -0.1885 0.156 Uiso 0.50 1 calc PR . . H7S2 H 1.0430 0.1566 -0.0994 0.156 Uiso 0.50 1 calc PR . . H7S3 H 1.1090 0.2607 -0.1192 0.156 Uiso 0.50 1 calc PR . . C7S' C 1.1104(13) 0.3453(13) -0.0781(10) 0.097(4) Uiso 0.50 1 d P A 1 H7S4 H 1.1496 0.4047 -0.0720 0.145 Uiso 0.50 1 calc PR A 1 H7S5 H 1.1428 0.3186 -0.1362 0.145 Uiso 0.50 1 calc PR A 1 H7S6 H 1.1292 0.2774 -0.0360 0.145 Uiso 0.50 1 calc PR A 1 C6S C 0.0221(11) 0.0872(16) 0.1405(10) 0.246(10) Uani 1 1 d . . . H6S1 H 0.0118 0.0201 0.1178 0.368 Uiso 1 1 calc R . . H6S2 H -0.0391 0.1604 0.1255 0.368 Uiso 1 1 calc R . . H6S3 H 0.0095 0.0736 0.2032 0.368 Uiso 1 1 calc R . . S5S S 0.4795(2) 0.2598(2) -0.01682(14) 0.0590(7) Uiso 0.566(5) 1 d P . . O5S O 0.3942(5) 0.3733(5) 0.0117(3) 0.0473(12) Uiso 0.566(5) 1 d P B . C9S C 0.6027(7) 0.2841(7) -0.0788(5) 0.106(2) Uiso 1 1 d . B . H9S1 H 0.6608 0.2088 -0.0985 0.159 Uiso 1 1 calc R . . H9S2 H 0.6416 0.3206 -0.0475 0.159 Uiso 1 1 calc R . . H9S3 H 0.5811 0.3377 -0.1285 0.159 Uiso 1 1 calc R . . C11S C 0.3241(16) 0.2942(16) -0.0797(11) 0.095(4) Uiso 0.434(5) 1 d P B 1 H11A H 0.3470 0.2137 -0.0977 0.143 Uiso 0.434(5) 1 calc PR B 1 H11B H 0.3402 0.3494 -0.1301 0.143 Uiso 0.434(5) 1 calc PR B 1 H11C H 0.2355 0.3180 -0.0515 0.143 Uiso 0.434(5) 1 calc PR B 1 S5S' S 0.4109(3) 0.2968(3) -0.00891(19) 0.0606(10) Uiso 0.434(5) 1 d P B 1 S4S" S 0.9776(9) 0.2956(9) -0.0785(6) 0.0442(18) Uiso 0.10 1 d P A 1 C10S C 0.4186(16) 0.2176(14) -0.0884(11) 0.121(5) Uiso 0.566(5) 1 d P . . H10A H 0.4490 0.1327 -0.0715 0.181 Uiso 0.566(5) 1 calc PR B 1 H10B H 0.4756 0.2391 -0.1405 0.181 Uiso 0.566(5) 1 calc PR B 1 H10C H 0.3356 0.2348 -0.0997 0.181 Uiso 0.566(5) 1 calc PR B 1 O5S' O 0.3665(6) 0.4208(7) 0.0186(4) 0.0481(16) Uiso 0.434(5) 1 d P B 1 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 S1S 0.0509(5) 0.0403(5) 0.0707(7) 0.0014(4) -0.0192(5) -0.0117(4) S2S 0.0997(10) 0.0576(7) 0.0646(8) 0.0011(6) -0.0019(7) -0.0288(7) C14 0.0275(11) 0.0244(12) 0.0195(11) -0.0040(9) -0.0040(9) -0.0078(9) C7 0.0233(11) 0.0272(12) 0.0204(11) -0.0040(9) -0.0037(8) -0.0033(9) C6 0.0284(11) 0.0243(12) 0.0161(11) -0.0023(8) -0.0037(8) -0.0065(9) O4 0.0510(12) 0.0231(10) 0.0302(11) -0.0072(8) -0.0065(9) -0.0064(9) C1 0.0265(11) 0.0225(11) 0.0161(10) -0.0014(8) -0.0041(8) -0.0042(9) O5 0.0573(13) 0.0222(10) 0.0360(12) 0.0007(8) -0.0049(10) -0.0079(9) O6 0.0560(13) 0.0286(10) 0.0215(10) 0.0020(8) -0.0056(9) -0.0096(9) C8 0.0258(11) 0.0225(11) 0.0218(11) -0.0018(9) -0.0056(9) -0.0069(9) C12 0.0287(12) 0.0279(13) 0.0212(12) -0.0020(9) -0.0045(9) -0.0045(10) C2 0.0256(11) 0.0259(12) 0.0186(11) -0.0034(9) -0.0042(9) -0.0036(9) O3 0.0362(11) 0.0651(16) 0.0228(10) -0.0058(10) -0.0073(8) -0.0184(10) C21 0.0257(11) 0.0349(14) 0.0243(12) -0.0035(10) -0.0089(9) -0.0072(10) O1 0.0298(10) 0.0780(18) 0.0198(10) -0.0135(10) 0.0032(8) -0.0172(10) C11 0.0319(12) 0.0208(12) 0.0267(13) -0.0003(9) -0.0039(10) -0.0044(9) C9 0.0229(10) 0.0262(12) 0.0194(11) -0.0023(9) -0.0016(8) -0.0073(9) C13 0.0225(10) 0.0264(12) 0.0196(11) -0.0031(9) -0.0029(8) -0.0059(9) C10 0.0282(11) 0.0260(12) 0.0222(12) -0.0063(9) -0.0015(9) -0.0069(9) C5 0.0319(13) 0.0389(15) 0.0192(12) -0.0029(10) -0.0067(9) -0.0100(11) C4 0.0329(13) 0.0514(18) 0.0164(12) -0.0040(11) -0.0029(10) -0.0116(12) C15 0.0334(13) 0.0323(14) 0.0245(12) -0.0110(10) -0.0083(10) 0.0032(10) O2 0.0428(12) 0.086(2) 0.0180(10) -0.0113(11) -0.0031(8) -0.0230(12) C3 0.0284(12) 0.0404(15) 0.0179(11) -0.0023(10) -0.0025(9) -0.0075(11) O1S 0.0585(15) 0.0280(12) 0.0697(18) -0.0088(11) -0.0227(13) -0.0048(10) C26 0.0398(16) 0.0326(16) 0.053(2) 0.0050(14) -0.0141(14) -0.0091(13) C16 0.0422(17) 0.053(2) 0.055(2) -0.0217(17) -0.0248(16) 0.0122(15) C22 0.0264(13) 0.073(3) 0.0328(16) -0.0065(15) -0.0066(11) -0.0102(14) O2S 0.160(4) 0.0492(18) 0.0505(19) -0.0015(14) -0.027(2) -0.037(2) C20 0.0514(19) 0.0305(17) 0.060(2) 0.0002(15) -0.0179(17) -0.0006(14) C25 0.065(2) 0.041(2) 0.080(3) -0.0005(19) -0.039(2) -0.0020(18) C23 0.0292(15) 0.092(3) 0.051(2) -0.023(2) -0.0130(14) 0.0076(17) C24 0.049(2) 0.064(3) 0.075(3) -0.025(2) -0.036(2) 0.0189(19) C18 0.079(3) 0.053(3) 0.054(2) -0.007(2) -0.020(2) 0.033(2) C1S 0.066(3) 0.042(2) 0.105(4) -0.008(2) -0.026(3) -0.0209(19) C17 0.058(2) 0.086(4) 0.065(3) -0.026(3) -0.035(2) 0.034(2) C19 0.079(3) 0.0305(19) 0.080(3) 0.0053(19) -0.009(2) 0.0057(19) C2S 0.103(4) 0.089(4) 0.076(4) 0.013(3) -0.035(3) -0.049(3) C4S 0.113(5) 0.054(3) 0.094(4) -0.003(3) -0.005(3) -0.037(3) C3S 0.261(12) 0.107(6) 0.082(5) 0.040(4) -0.033(6) -0.094(7) S3S 0.1448(19) 0.1087(16) 0.0802(12) 0.0014(10) -0.0109(12) 0.0002(13) S4S 0.0539(12) 0.117(2) 0.0351(10) -0.0195(11) -0.0049(8) -0.0270(13) S4S' 0.0689(18) 0.146(4) 0.0430(15) -0.0141(18) -0.0022(13) -0.053(2) O4S 0.095(3) 0.227(7) 0.043(2) -0.031(3) 0.018(2) 0.001(4) O3S 0.146(5) 0.098(4) 0.157(6) -0.033(4) -0.045(4) 0.015(3) C8S 0.121(6) 0.222(12) 0.129(7) 0.065(7) -0.074(6) -0.074(7) C5S 0.291(16) 0.101(7) 0.101(7) -0.002(5) -0.029(8) -0.001(8) C6S 0.135(9) 0.32(2) 0.224(17) 0.140(15) -0.049(10) -0.054(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 S1S O1S 1.511(3) . ? S1S C2S 1.765(6) . ? S1S C1S 1.784(5) . ? S2S O2S 1.494(4) . ? S2S C4S 1.745(7) . ? S2S C3S 1.789(7) . ? C14 C6 1.521(3) 2_666 ? C14 C21 1.525(4) . ? C14 C9 1.528(3) . ? C14 H14 1.0000 . ? C7 C13 1.519(3) . ? C7 C2 1.528(3) . ? C7 C15 1.536(4) . ? C7 H7 1.0000 . ? C6 C1 1.402(3) . ? C6 C5 1.407(3) . ? C6 C14 1.521(3) 2_666 ? O4 C10 1.359(3) . ? O4 H4 0.8400 . ? C1 C2 1.398(3) . ? C1 H1 0.9500 . ? O5 C11 1.377(3) . ? O5 H5 0.8400 . ? O6 C12 1.361(3) . ? O6 H6 0.8400 . ? C8 C13 1.399(3) . ? C8 C9 1.400(3) . ? C8 H8 0.9500 . ? C12 C13 1.388(4) . ? C12 C11 1.404(4) . ? C2 C3 1.385(3) . ? O3 C5 1.356(3) . ? O3 H3 0.8400 . ? C21 C26 1.378(4) . ? C21 C22 1.401(4) . ? O1 C3 1.369(3) . ? O1 H1A 0.8400 . ? C11 C10 1.396(4) . ? C9 C10 1.391(4) . ? C5 C4 1.399(4) . ? C4 O2 1.376(3) . ? C4 C3 1.405(4) . ? C15 C20 1.376(5) . ? C15 C16 1.387(4) . ? O2 H2 0.8400 . ? C26 C25 1.386(5) . ? C26 H26 0.9500 . ? C16 C17 1.409(6) . ? C16 H16 0.9500 . ? C22 C23 1.386(6) . ? C22 H22 0.9500 . ? C20 C19 1.407(5) . ? C20 H20 0.9500 . ? C25 C24 1.365(7) . ? C25 H25 0.9500 . ? C23 C24 1.383(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C18 C19 1.346(8) . ? C18 C17 1.372(8) . ? C18 H18 0.9500 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C17 H17 0.9500 . ? C19 H19 0.9500 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? S3S O3S 1.470(6) . ? S3S C6S 1.693(12) . ? S3S C5S 1.727(11) . ? S4S S4S" 0.904(10) . ? S4S S4S' 1.320(4) . ? S4S O4S 1.351(5) . ? S4S C7S 1.759(16) . ? S4S' S4S" 1.312(10) . ? S4S' O4S 1.426(7) . ? S4S' C8S 1.659(9) . ? S4S' C7S' 1.675(15) . ? O4S S4S" 1.417(10) . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C7S' H7S4 0.9800 . ? C7S' H7S5 0.9800 . ? C7S' H7S6 0.9800 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? S5S O5S 1.463(6) . ? S5S C9S 1.599(8) . ? S5S O5S' 2.026(8) . ? O5S O5S' 0.568(7) . ? O5S S5S' 0.964(6) . ? C9S H9S1 0.9800 . ? C9S H9S2 0.9800 . ? C9S H9S3 0.9800 . ? C11S S5S' 1.721(16) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? S5S' O5S' 1.501(8) . ? S5S' C10S 1.679(16) . ? C10S H10A 0.9800 . ? C10S H10B 0.9800 . ? C10S H10C 0.9800 . ? 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 O1S S1S C2S 106.5(2) . . ? O1S S1S C1S 105.61(18) . . ? C2S S1S C1S 100.3(3) . . ? O2S S2S C4S 108.5(3) . . ? O2S S2S C3S 104.6(4) . . ? C4S S2S C3S 99.9(4) . . ? C6 C14 C21 114.2(2) 2_666 . ? C6 C14 C9 113.08(19) 2_666 . ? C21 C14 C9 111.5(2) . . ? C6 C14 H14 105.7 2_666 . ? C21 C14 H14 105.7 . . ? C9 C14 H14 105.7 . . ? C13 C7 C2 113.2(2) . . ? C13 C7 C15 112.5(2) . . ? C2 C7 C15 113.0(2) . . ? C13 C7 H7 105.7 . . ? C2 C7 H7 105.7 . . ? C15 C7 H7 105.7 . . ? C1 C6 C5 117.6(2) . . ? C1 C6 C14 123.8(2) . 2_666 ? C5 C6 C14 118.6(2) . 2_666 ? C10 O4 H4 109.5 . . ? C2 C1 C6 122.8(2) . . ? C2 C1 H1 118.6 . . ? C6 C1 H1 118.6 . . ? C11 O5 H5 109.5 . . ? C12 O6 H6 109.5 . . ? C13 C8 C9 122.7(2) . . ? C13 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? O6 C12 C13 118.7(2) . . ? O6 C12 C11 120.8(2) . . ? C13 C12 C11 120.4(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 C7 118.4(2) . . ? C1 C2 C7 123.1(2) . . ? C5 O3 H3 109.5 . . ? C26 C21 C22 117.7(3) . . ? C26 C21 C14 124.3(2) . . ? C22 C21 C14 118.0(3) . . ? C3 O1 H1A 109.5 . . ? O5 C11 C10 121.3(2) . . ? O5 C11 C12 118.4(2) . . ? C10 C11 C12 120.2(2) . . ? C10 C9 C8 118.1(2) . . ? C10 C9 C14 119.2(2) . . ? C8 C9 C14 122.6(2) . . ? C12 C13 C8 118.1(2) . . ? C12 C13 C7 118.4(2) . . ? C8 C13 C7 123.4(2) . . ? O4 C10 C9 119.1(2) . . ? O4 C10 C11 120.3(2) . . ? C9 C10 C11 120.6(2) . . ? O3 C5 C4 120.6(2) . . ? O3 C5 C6 118.9(2) . . ? C4 C5 C6 120.4(2) . . ? O2 C4 C5 118.9(2) . . ? O2 C4 C3 121.0(2) . . ? C5 C4 C3 120.1(2) . . ? C20 C15 C16 118.7(3) . . ? C20 C15 C7 122.6(3) . . ? C16 C15 C7 118.6(3) . . ? C4 O2 H2 109.5 . . ? O1 C3 C2 118.7(2) . . ? O1 C3 C4 120.7(2) . . ? C2 C3 C4 120.6(2) . . ? C21 C26 C25 121.0(4) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C23 C22 C21 121.2(4) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C15 C20 C19 120.3(4) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C19 C18 C17 118.8(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? S1S C1S H1S1 109.5 . . ? S1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? S1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C18 C17 C16 121.4(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C18 C19 C20 121.4(5) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? S1S C2S H2S1 109.5 . . ? S1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? S1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? S2S C4S H4S1 109.5 . . ? S2S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? S2S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? S2S C3S H3S1 109.5 . . ? S2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? S2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O3S S3S C6S 109.7(5) . . ? O3S S3S C5S 108.4(5) . . ? C6S S3S C5S 90.2(9) . . ? S4S" S4S S4S' 69.4(6) . . ? S4S" S4S O4S 75.0(7) . . ? S4S' S4S O4S 64.5(3) . . ? S4S" S4S C7S 31.1(8) . . ? S4S' S4S C7S 92.2(6) . . ? O4S S4S C7S 103.8(6) . . ? S4S" S4S' S4S 40.2(4) . . ? S4S" S4S' O4S 62.2(5) . . ? S4S S4S' O4S 58.8(3) . . ? S4S" S4S' C8S 86.2(6) . . ? S4S S4S' C8S 65.9(4) . . ? O4S S4S' C8S 122.3(5) . . ? S4S" S4S' C7S' 73.8(7) . . ? S4S S4S' C7S' 113.1(6) . . ? O4S S4S' C7S' 106.0(6) . . ? C8S S4S' C7S' 109.6(7) . . ? S4S O4S S4S" 38.0(4) . . ? S4S O4S S4S' 56.7(3) . . ? S4S" O4S S4S' 54.9(4) . . ? S4S' C8S H8S1 109.5 . . ? S4S' C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? S4S' C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? S3S C5S H5S1 109.5 . . ? S3S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? S3S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? S4S C7S H7S1 109.5 . . ? S4S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? S4S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? S4S' C7S' H7S4 109.5 . . ? S4S' C7S' H7S5 109.5 . . ? H7S4 C7S' H7S5 109.5 . . ? S4S' C7S' H7S6 109.5 . . ? H7S4 C7S' H7S6 109.5 . . ? H7S5 C7S' H7S6 109.5 . . ? S3S C6S H6S1 109.5 . . ? S3S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? S3S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? O5S S5S C9S 108.5(4) . . ? O5S S5S O5S' 2.6(3) . . ? C9S S5S O5S' 105.9(4) . . ? O5S' O5S S5S' 156.1(12) . . ? O5S' O5S S5S 170.6(12) . . ? S5S' O5S S5S 28.4(3) . . ? S5S C9S H9S1 109.5 . . ? S5S C9S H9S2 109.5 . . ? H9S1 C9S H9S2 109.5 . . ? S5S C9S H9S3 109.5 . . ? H9S1 C9S H9S3 109.5 . . ? H9S2 C9S H9S3 109.5 . . ? S5S' C11S H11A 109.5 . . ? S5S' C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? S5S' C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? O5S S5S' O5S' 8.8(4) . . ? O5S S5S' C10S 148.7(7) . . ? O5S' S5S' C10S 142.4(7) . . ? O5S S5S' C11S 114.7(7) . . ? O5S' S5S' C11S 106.3(7) . . ? C10S S5S' C11S 40.6(7) . . ? S4S S4S" S4S' 70.4(7) . . ? S4S S4S" O4S 67.0(7) . . ? S4S' S4S" O4S 62.9(5) . . ? S5S' C10S H10A 109.5 . . ? S5S' C10S H10B 109.5 . . ? H10A C10S H10B 109.5 . . ? S5S' C10S H10C 109.5 . . ? H10A C10S H10C 109.5 . . ? H10B C10S H10C 109.5 . . ? O5S O5S' S5S' 15.1(8) . . ? O5S O5S' S5S 6.8(8) . . ? S5S' O5S' S5S 18.49(16) . . ? 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 C5 C6 C1 C2 -1.8(4) . . . . ? C14 C6 C1 C2 178.2(2) 2_666 . . . ? C6 C1 C2 C3 -0.6(4) . . . . ? C6 C1 C2 C7 -177.0(2) . . . . ? C13 C7 C2 C3 146.1(3) . . . . ? C15 C7 C2 C3 -84.4(3) . . . . ? C13 C7 C2 C1 -37.6(3) . . . . ? C15 C7 C2 C1 92.0(3) . . . . ? C6 C14 C21 C26 1.4(4) 2_666 . . . ? C9 C14 C21 C26 -128.4(3) . . . . ? C6 C14 C21 C22 -176.9(2) 2_666 . . . ? C9 C14 C21 C22 53.3(3) . . . . ? O6 C12 C11 O5 -3.2(4) . . . . ? C13 C12 C11 O5 175.2(2) . . . . ? O6 C12 C11 C10 -179.7(2) . . . . ? C13 C12 C11 C10 -1.3(4) . . . . ? C13 C8 C9 C10 0.0(4) . . . . ? C13 C8 C9 C14 -175.9(2) . . . . ? C6 C14 C9 C10 86.7(3) 2_666 . . . ? C21 C14 C9 C10 -142.9(2) . . . . ? C6 C14 C9 C8 -97.5(3) 2_666 . . . ? C21 C14 C9 C8 32.9(3) . . . . ? O6 C12 C13 C8 179.7(2) . . . . ? C11 C12 C13 C8 1.3(4) . . . . ? O6 C12 C13 C7 2.8(3) . . . . ? C11 C12 C13 C7 -175.6(2) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? C9 C8 C13 C7 176.1(2) . . . . ? C2 C7 C13 C12 -77.2(3) . . . . ? C15 C7 C13 C12 153.1(2) . . . . ? C2 C7 C13 C8 106.1(3) . . . . ? C15 C7 C13 C8 -23.6(3) . . . . ? C8 C9 C10 O4 -178.3(2) . . . . ? C14 C9 C10 O4 -2.3(3) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C14 C9 C10 C11 176.1(2) . . . . ? O5 C11 C10 O4 2.6(4) . . . . ? C12 C11 C10 O4 179.0(2) . . . . ? O5 C11 C10 C9 -175.8(2) . . . . ? C12 C11 C10 C9 0.6(4) . . . . ? C1 C6 C5 O3 -179.3(3) . . . . ? C14 C6 C5 O3 0.7(4) 2_666 . . . ? C1 C6 C5 C4 1.5(4) . . . . ? C14 C6 C5 C4 -178.5(3) 2_666 . . . ? O3 C5 C4 O2 -1.7(5) . . . . ? C6 C5 C4 O2 177.4(3) . . . . ? O3 C5 C4 C3 -177.9(3) . . . . ? C6 C5 C4 C3 1.2(5) . . . . ? C13 C7 C15 C20 118.7(3) . . . . ? C2 C7 C15 C20 -11.1(4) . . . . ? C13 C7 C15 C16 -63.6(3) . . . . ? C2 C7 C15 C16 166.5(3) . . . . ? C1 C2 C3 O1 -177.6(3) . . . . ? C7 C2 C3 O1 -1.0(4) . . . . ? C1 C2 C3 C4 3.4(4) . . . . ? C7 C2 C3 C4 180.0(3) . . . . ? O2 C4 C3 O1 1.1(5) . . . . ? C5 C4 C3 O1 177.2(3) . . . . ? O2 C4 C3 C2 -179.9(3) . . . . ? C5 C4 C3 C2 -3.8(5) . . . . ? C22 C21 C26 C25 -0.2(5) . . . . ? C14 C21 C26 C25 -178.4(3) . . . . ? C20 C15 C16 C17 -1.5(5) . . . . ? C7 C15 C16 C17 -179.3(3) . . . . ? C26 C21 C22 C23 1.4(5) . . . . ? C14 C21 C22 C23 179.8(3) . . . . ? C16 C15 C20 C19 1.7(6) . . . . ? C7 C15 C20 C19 179.4(4) . . . . ? C21 C26 C25 C24 -1.1(6) . . . . ? C21 C22 C23 C24 -1.4(6) . . . . ? C26 C25 C24 C23 1.1(7) . . . . ? C22 C23 C24 C25 0.1(6) . . . . ? C19 C18 C17 C16 -1.0(7) . . . . ? C15 C16 C17 C18 1.2(7) . . . . ? C17 C18 C19 C20 1.2(8) . . . . ? C15 C20 C19 C18 -1.6(7) . . . . ? O4S S4S S4S' S4S" 82.6(7) . . . . ? C7S S4S S4S' S4S" -21.6(8) . . . . ? S4S" S4S S4S' O4S -82.6(7) . . . . ? C7S S4S S4S' O4S -104.2(6) . . . . ? S4S" S4S S4S' C8S 114.6(8) . . . . ? O4S S4S S4S' C8S -162.7(6) . . . . ? C7S S4S S4S' C8S 93.0(7) . . . . ? S4S" S4S S4S' C7S' 12.6(9) . . . . ? O4S S4S S4S' C7S' 95.3(7) . . . . ? C7S S4S S4S' C7S' -9.0(8) . . . . ? S4S' S4S O4S S4S" -74.0(7) . . . . ? C7S S4S O4S S4S" 11.8(8) . . . . ? S4S" S4S O4S S4S' 74.0(7) . . . . ? C7S S4S O4S S4S' 85.8(6) . . . . ? S4S" S4S' O4S S4S -46.4(5) . . . . ? C8S S4S' O4S S4S 18.7(6) . . . . ? C7S' S4S' O4S S4S -107.7(6) . . . . ? S4S S4S' O4S S4S" 46.4(5) . . . . ? C8S S4S' O4S S4S" 65.1(8) . . . . ? C7S' S4S' O4S S4S" -61.4(8) . . . . ? C9S S5S O5S O5S' 11(7) . . . . ? C9S S5S O5S S5S' 137.4(6) . . . . ? O5S' S5S O5S S5S' 127(7) . . . . ? S5S O5S S5S' O5S' -161(3) . . . . ? O5S' O5S S5S' C10S 50(4) . . . . ? S5S O5S S5S' C10S -111.4(14) . . . . ? O5S' O5S S5S' C11S 18(3) . . . . ? S5S O5S S5S' C11S -142.9(9) . . . . ? O4S S4S S4S" S4S' -68.0(4) . . . . ? C7S S4S S4S" S4S' 134.5(16) . . . . ? S4S' S4S S4S" O4S 68.0(4) . . . . ? C7S S4S S4S" O4S -157.5(16) . . . . ? O4S S4S' S4S" S4S 73.5(6) . . . . ? C8S S4S' S4S" S4S -56.3(6) . . . . ? C7S' S4S' S4S" S4S -167.9(9) . . . . ? S4S S4S' S4S" O4S -73.5(6) . . . . ? C8S S4S' S4S" O4S -129.8(5) . . . . ? C7S' S4S' S4S" O4S 118.5(7) . . . . ? S4S' O4S S4S" S4S -78.9(6) . . . . ? S4S O4S S4S" S4S' 78.9(6) . . . . ? S5S O5S O5S' S5S' 110(8) . . . . ? S5S' O5S O5S' S5S -110(8) . . . . ? C10S S5S' O5S' O5S -139(3) . . . . ? C11S S5S' O5S' O5S -163(3) . . . . ? O5S S5S' O5S' S5S 21(3) . . . . ? C10S S5S' O5S' S5S -118.8(12) . . . . ? C11S S5S' O5S' S5S -142.2(8) . . . . ? C9S S5S O5S' O5S -169(7) . . . . ? O5S S5S O5S' S5S' -51(7) . . . . ? C9S S5S O5S' S5S' 139.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.366 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.124