# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Manoj, K' 'Gonnade, Rajesh' 'Shashidhar, Mysore' 'Bhadbhade, Mohan' _publ_contact_author_name 'Dr Rajesh Gonnade' _publ_contact_author_email ms.shashidhar@ncl.res.in _publ_section_title ; Solvent Induced Crystallization of 1,2,3,4(6), 5-Penta-O-Acetyl-6(4)-O-[(1S)-10-Camphor-Sulfonyl]-myo-Inositol Diastereomers Associated via Weak Trifurcated C-H...O Interactions ; # Attachment '- KM_CIF.cif' data_1.1DCM _database_code_depnum_ccdc_archive 'CCDC 846743' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.1DCM ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 92 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT220_1.1DCM ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.1 Ratio RESPONSE: Higher anisotropies for the terminal C atoms of the host contribute to this alert. The high ratio could be due to their (C atoms) freedom of libration and their proximity to the cavity containing guest molecules with low occupancies. ; _vrf_PLAT221_1.1DCM ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.3 Ratio RESPONSE: The alert is due to the higher anisotropies of carbonyl O atoms of the host molecules, which are situated at the edge of the cavity containing disodered guest molecules. ; _vrf_PLAT340_1.1DCM ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0120 Ang RESPONSE: This type alerts do occur in the crystal structure of inclusion complexes where atoms or the group of atoms show statistical disorder due to their proximity to the disordered guest molecules. ; _vrf_PLAT241_1.1DCM ; PROBLEM: Check High Ueq as Compared to Neighbors for C19' RESPONSE: This alert could be due to proximity of this phenyl ring and particularly atom C19' near the vicinity of the cavity containing the guest molecule. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULPHONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S ,0.25(C H2 Cl2)' _chemical_formula_sum 'C26 H36.50 Cl0.50 O14 S' _chemical_formula_weight 622.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.499(5) _cell_length_b 11.793(5) _cell_length_c 12.374(5) _cell_angle_alpha 94.564(7) _cell_angle_beta 101.799(7) _cell_angle_gamma 105.126(7) _cell_volume 1569.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 2717 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 20.65 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9553 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14953 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.1343 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10787 _reflns_number_gt 7137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.1021P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(12) _refine_ls_number_reflns 10787 _refine_ls_number_parameters 780 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2207 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _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 0.09030(13) 0.12562(14) 0.34414(13) 0.0398(4) Uani 1 1 d . . . O1 O 0.1143(4) 0.2664(4) 0.9021(4) 0.0423(12) Uani 1 1 d . . . O2 O 0.2010(4) 0.1125(4) 0.7738(4) 0.0408(11) Uani 1 1 d . . . O3 O 0.0375(4) -0.0326(4) 0.5837(4) 0.0408(11) Uani 1 1 d . . . O4 O 0.0222(4) 0.1396(4) 0.4422(4) 0.0387(11) Uani 1 1 d . . . O5 O 0.1550(4) 0.3734(4) 0.5435(4) 0.0438(12) Uani 1 1 d . . . O6 O 0.1121(4) 0.4360(4) 0.7569(4) 0.0447(12) Uani 1 1 d . . . O7 O -0.0600(5) 0.2992(7) 0.9295(5) 0.091(2) Uani 1 1 d . . . O8 O 0.1534(6) -0.0746(5) 0.8114(5) 0.0652(15) Uani 1 1 d . . . O9 O -0.1357(6) -0.1276(5) 0.6333(5) 0.0756(18) Uani 1 1 d . . . O10 O -0.0015(6) 0.4502(6) 0.4814(6) 0.0831(19) Uani 1 1 d . . . O11 O 0.3122(5) 0.5121(6) 0.8355(7) 0.105(3) Uani 1 1 d . . . O12 O 0.2130(4) 0.1990(5) 0.3740(5) 0.0589(14) Uani 1 1 d . . . O13 O 0.0068(4) 0.1452(5) 0.2487(4) 0.0497(12) Uani 1 1 d . . . O14 O 0.1201(7) -0.2464(6) 0.3366(6) 0.0911(19) Uani 1 1 d . . . C1 C 0.0605(6) 0.2327(6) 0.7842(5) 0.0371(16) Uani 1 1 d . . . H1 H -0.0266 0.2324 0.7681 0.045 Uiso 1 1 calc R . . C2 C 0.0700(6) 0.1096(6) 0.7471(5) 0.0382(16) Uani 1 1 d . . . H2 H 0.0233 0.0508 0.7857 0.046 Uiso 1 1 calc R . . C3 C 0.0191(6) 0.0777(5) 0.6207(5) 0.0344(16) Uani 1 1 d . . . H3 H -0.0696 0.0716 0.6020 0.041 Uiso 1 1 calc R . . C4 C 0.0874(6) 0.1699(6) 0.5575(5) 0.0326(15) Uani 1 1 d . . . H4 H 0.1738 0.1690 0.5665 0.039 Uiso 1 1 calc R . . C5 C 0.0804(7) 0.2902(6) 0.5979(6) 0.0409(17) Uani 1 1 d . . . H5 H -0.0056 0.2931 0.5782 0.049 Uiso 1 1 calc R . . C6 C 0.1313(6) 0.3221(6) 0.7231(5) 0.0375(16) Uani 1 1 d . . . H6 H 0.2197 0.3272 0.7428 0.045 Uiso 1 1 calc R . . C7 C 0.0449(7) 0.3063(7) 0.9642(6) 0.0474(19) Uani 1 1 d . . . C8 C 0.1155(8) 0.3528(8) 1.0784(7) 0.068(2) Uani 1 1 d . . . H8A H 0.0608 0.3690 1.1229 0.103 Uiso 1 1 calc R . . H8B H 0.1784 0.4247 1.0786 0.103 Uiso 1 1 calc R . . H8C H 0.1535 0.2953 1.1089 0.103 Uiso 1 1 calc R . . C9 C 0.2279(7) 0.0149(8) 0.8036(6) 0.0494(19) Uani 1 1 d . . . C10 C 0.3671(9) 0.0309(10) 0.8268(11) 0.097(4) Uani 1 1 d . . . H10A H 0.4028 0.0551 0.9052 0.145 Uiso 1 1 calc R . . H10B H 0.4042 0.0904 0.7858 0.145 Uiso 1 1 calc R . . H10C H 0.3818 -0.0429 0.8042 0.145 Uiso 1 1 calc R . . C11 C -0.0497(9) -0.1337(7) 0.5948(7) 0.061(2) Uani 1 1 d . . . C12 C -0.0159(11) -0.2411(8) 0.5586(8) 0.085(3) Uani 1 1 d . . . H12A H 0.0431 -0.2564 0.6185 0.127 Uiso 1 1 calc R . . H12B H 0.0200 -0.2287 0.4953 0.127 Uiso 1 1 calc R . . H12C H -0.0887 -0.3077 0.5384 0.127 Uiso 1 1 calc R . . C13 C 0.1007(8) 0.4461(7) 0.4812(7) 0.0522(19) Uani 1 1 d . . . C14 C 0.1871(9) 0.5120(10) 0.4200(9) 0.092(3) Uani 1 1 d . . . H14A H 0.1550 0.5723 0.3877 0.139 Uiso 1 1 calc R . . H14B H 0.1965 0.4585 0.3620 0.139 Uiso 1 1 calc R . . H14C H 0.2661 0.5485 0.4704 0.139 Uiso 1 1 calc R . . C15 C 0.2098(8) 0.5253(7) 0.8117(7) 0.060(2) Uani 1 1 d . . . C16 C 0.1743(10) 0.6303(8) 0.8472(9) 0.084(3) Uani 1 1 d . . . H16A H 0.2396 0.6806 0.9060 0.125 Uiso 1 1 calc R . . H16B H 0.0999 0.6062 0.8737 0.125 Uiso 1 1 calc R . . H16C H 0.1599 0.6730 0.7852 0.125 Uiso 1 1 calc R . . C17 C 0.0881(7) -0.0235(6) 0.3384(6) 0.0425(17) Uani 1 1 d . . . H17A H 0.1558 -0.0289 0.3971 0.051 Uiso 1 1 calc R . . H17B H 0.0118 -0.0667 0.3561 0.051 Uiso 1 1 calc R . . C18 C 0.0979(6) -0.0895(5) 0.2281(5) 0.0406(14) Uani 1 1 d . . . C19 C -0.0261(6) -0.1291(7) 0.1343(6) 0.0593(17) Uani 1 1 d . . . H19A H -0.0873 -0.1931 0.1535 0.071 Uiso 1 1 calc R . . H19B H -0.0605 -0.0633 0.1212 0.071 Uiso 1 1 calc R . . C20 C 0.0169(7) -0.1709(6) 0.0325(6) 0.0645(18) Uani 1 1 d . . . H20A H 0.0044 -0.1223 -0.0260 0.077 Uiso 1 1 calc R . . H20B H -0.0279 -0.2530 0.0033 0.077 Uiso 1 1 calc R . . C21 C 0.1555(8) -0.1570(7) 0.0772(7) 0.066(2) Uani 1 1 d . . . H21 H 0.2030 -0.1563 0.0198 0.080 Uiso 1 1 calc R . . C22 C 0.1619(10) -0.2525(9) 0.1523(8) 0.079(3) Uani 1 1 d . . . H22A H 0.1035 -0.3283 0.1178 0.095 Uiso 1 1 calc R . . H22B H 0.2447 -0.2618 0.1716 0.095 Uiso 1 1 calc R . . C23 C 0.1266(8) -0.2019(7) 0.2529(7) 0.063(2) Uani 1 1 d . . . C24 C 0.1961(6) -0.0407(6) 0.1613(5) 0.0502(15) Uani 1 1 d . . . C25 C 0.1805(8) 0.0658(7) 0.1036(6) 0.073(2) Uani 1 1 d . . . H25A H 0.2058 0.1355 0.1581 0.109 Uiso 1 1 calc R . . H25B H 0.0952 0.0519 0.0663 0.109 Uiso 1 1 calc R . . H25C H 0.2308 0.0772 0.0500 0.109 Uiso 1 1 calc R . . C26 C 0.3270(7) -0.0120(9) 0.2312(8) 0.090(3) Uani 1 1 d . . . H26A H 0.3844 0.0060 0.1842 0.135 Uiso 1 1 calc R . . H26B H 0.3375 -0.0790 0.2672 0.135 Uiso 1 1 calc R . . H26C H 0.3423 0.0552 0.2866 0.135 Uiso 1 1 calc R . . S1' S 0.69249(14) 0.20672(14) 0.48618(13) 0.0421(4) Uani 1 1 d . . . O1' O 0.7523(4) 0.3730(4) 0.2525(4) 0.0428(11) Uani 1 1 d . . . O2' O 0.5922(4) 0.2323(4) 0.0619(4) 0.0425(12) Uani 1 1 d . . . O3' O 0.6789(4) 0.0785(4) -0.0656(4) 0.0471(13) Uani 1 1 d . . . O4' O 0.6658(4) -0.0960(4) 0.0739(4) 0.0480(13) Uani 1 1 d . . . O5' O 0.6306(4) -0.0375(4) 0.2879(4) 0.0438(12) Uani 1 1 d . . . O6' O 0.7644(4) 0.1975(4) 0.3912(4) 0.0425(12) Uani 1 1 d . . . O7' O 0.9232(5) 0.4708(5) 0.2024(5) 0.0691(16) Uani 1 1 d . . . O8' O 0.6459(6) 0.4183(5) 0.0235(5) 0.0629(14) Uani 1 1 d . . . O9' O 0.8484(6) 0.0223(6) -0.0841(5) 0.087(2) Uani 1 1 d . . . O10' O 0.7881(5) -0.1114(6) 0.3496(7) 0.088(2) Uani 1 1 d . . . O11' O 0.4619(6) -0.1714(6) 0.0113(8) 0.112(3) Uani 1 1 d . . . O12' O 0.5703(5) 0.1317(5) 0.4515(5) 0.0638(15) Uani 1 1 d . . . O13' O 0.7728(5) 0.1887(5) 0.5824(4) 0.0612(15) Uani 1 1 d . . . O14' O 0.6172(13) 0.5579(9) 0.4714(8) 0.185(6) Uani 1 1 d . . . C1' C 0.7704(6) 0.2623(6) 0.2138(5) 0.0405(17) Uani 1 1 d . . . H1' H 0.8589 0.2675 0.2331 0.049 Uiso 1 1 calc R . . C2' C 0.7198(6) 0.2312(6) 0.0863(6) 0.0401(17) Uani 1 1 d . . . H2' H 0.7680 0.2891 0.0479 0.048 Uiso 1 1 calc R . . C3' C 0.7257(6) 0.1102(6) 0.0507(5) 0.0396(17) Uani 1 1 d . . . H3' H 0.8127 0.1100 0.0686 0.047 Uiso 1 1 calc R . . C4' C 0.6532(6) 0.0157(6) 0.1082(5) 0.0408(17) Uani 1 1 d . . . H4' H 0.5655 0.0132 0.0900 0.049 Uiso 1 1 calc R . . C5' C 0.7051(6) 0.0461(6) 0.2344(5) 0.0345(16) Uani 1 1 d . . . H5' H 0.7908 0.0420 0.2532 0.041 Uiso 1 1 calc R . . C6' C 0.7010(6) 0.1708(6) 0.2734(6) 0.0407(17) Uani 1 1 d . . . H6' H 0.6150 0.1733 0.2637 0.049 Uiso 1 1 calc R . . C7' C 0.8352(7) 0.4712(6) 0.2385(6) 0.0462(18) Uani 1 1 d . . . C8' C 0.8009(9) 0.5770(7) 0.2767(8) 0.074(3) Uani 1 1 d . . . H8D H 0.8721 0.6329 0.3255 0.111 Uiso 1 1 calc R . . H8E H 0.7365 0.5542 0.3160 0.111 Uiso 1 1 calc R . . H8F H 0.7719 0.6128 0.2135 0.111 Uiso 1 1 calc R . . C9' C 0.5679(8) 0.3359(7) 0.0334(7) 0.0489(19) Uani 1 1 d . . . C10' C 0.4338(8) 0.3228(8) 0.0186(9) 0.072(2) Uani 1 1 d . . . H10D H 0.4124 0.3187 0.0895 0.108 Uiso 1 1 calc R . . H10E H 0.3873 0.2515 -0.0312 0.108 Uiso 1 1 calc R . . H10F H 0.4147 0.3899 -0.0122 0.108 Uiso 1 1 calc R . . C11' C 0.7482(8) 0.0325(7) -0.1256(7) 0.058(2) Uani 1 1 d . . . C12' C 0.6771(8) -0.0117(8) -0.2432(7) 0.065(2) Uani 1 1 d . . . H12D H 0.6934 0.0508 -0.2880 0.098 Uiso 1 1 calc R . . H12E H 0.5901 -0.0369 -0.2455 0.098 Uiso 1 1 calc R . . H12F H 0.7020 -0.0775 -0.2717 0.098 Uiso 1 1 calc R . . C13' C 0.6845(9) -0.1075(7) 0.3455(8) 0.065(2) Uani 1 1 d . . . C14' C 0.5961(10) -0.1789(11) 0.4065(11) 0.105(4) Uani 1 1 d . . . H14D H 0.5490 -0.2526 0.3605 0.158 Uiso 1 1 calc R . . H14E H 0.5408 -0.1350 0.4229 0.158 Uiso 1 1 calc R . . H14F H 0.6422 -0.1946 0.4747 0.158 Uiso 1 1 calc R . . C15' C 0.5624(8) -0.1821(7) 0.0230(8) 0.064(2) Uani 1 1 d . . . C16' C 0.5967(11) -0.2925(9) -0.0069(12) 0.118(5) Uani 1 1 d . . . H16D H 0.5308 -0.3607 -0.0038 0.177 Uiso 1 1 calc R . . H16E H 0.6711 -0.2930 0.0449 0.177 Uiso 1 1 calc R . . H16F H 0.6103 -0.2946 -0.0810 0.177 Uiso 1 1 calc R . . C17' C 0.6927(7) 0.3544(7) 0.4989(6) 0.0511(19) Uani 1 1 d . . . H17C H 0.7784 0.4025 0.5216 0.061 Uiso 1 1 calc R . . H17D H 0.6591 0.3710 0.4253 0.061 Uiso 1 1 calc R . . C18' C 0.6228(6) 0.3971(6) 0.5785(5) 0.0471(15) Uani 1 1 d . . . C19' C 0.4939(8) 0.3238(11) 0.5763(10) 0.118(4) Uani 1 1 d . . . H19C H 0.4916 0.2418 0.5828 0.142 Uiso 1 1 calc R . . H19D H 0.4363 0.3265 0.5080 0.142 Uiso 1 1 calc R . . C20' C 0.4621(9) 0.3831(10) 0.6802(11) 0.123(4) Uani 1 1 d . . . H20C H 0.3928 0.4154 0.6582 0.148 Uiso 1 1 calc R . . H20D H 0.4431 0.3271 0.7319 0.148 Uiso 1 1 calc R . . C21' C 0.5804(8) 0.4799(8) 0.7302(8) 0.076(3) Uani 1 1 d . . . H21' H 0.5915 0.5078 0.8095 0.091 Uiso 1 1 calc R . . C22' C 0.5809(13) 0.5747(11) 0.6567(10) 0.109(4) Uani 1 1 d . . . H22C H 0.6449 0.6477 0.6901 0.131 Uiso 1 1 calc R . . H22D H 0.5011 0.5908 0.6389 0.131 Uiso 1 1 calc R . . C23' C 0.6092(13) 0.5161(11) 0.5546(10) 0.115(4) Uani 1 1 d . . . C24' C 0.6831(7) 0.4307(7) 0.7040(6) 0.0653(19) Uani 1 1 d . . . C25' C 0.6840(14) 0.3179(12) 0.7643(9) 0.146(6) Uani 1 1 d . . . H25D H 0.7284 0.2721 0.7307 0.219 Uiso 1 1 calc R . . H25E H 0.6003 0.2705 0.7569 0.219 Uiso 1 1 calc R . . H25F H 0.7237 0.3425 0.8418 0.219 Uiso 1 1 calc R . . C26' C 0.8067(10) 0.5178(14) 0.7313(12) 0.180(9) Uani 1 1 d . . . H26D H 0.8002 0.5907 0.7047 0.270 Uiso 1 1 calc R . . H26E H 0.8615 0.4872 0.6963 0.270 Uiso 1 1 calc R . . H26F H 0.8387 0.5321 0.8107 0.270 Uiso 1 1 calc R . . Cl1 Cl 0.3732(9) 0.9625(12) 0.5516(7) 0.119(4) Uani 0.25 1 d PDU . . Cl2 Cl 0.3563(13) 0.7480(11) 0.6638(11) 0.133(4) Uani 0.25 1 d PDU . . C27 C 0.282(3) 0.830(2) 0.579(3) 0.138(17) Uani 0.25 1 d PDU . . H27A H 0.2403 0.7809 0.5077 0.166 Uiso 0.25 1 calc PR . . H27B H 0.2188 0.8485 0.6123 0.166 Uiso 0.25 1 calc PR . . 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 0.0400(10) 0.0549(11) 0.0270(9) 0.0041(8) 0.0072(7) 0.0185(8) O1 0.039(2) 0.064(3) 0.025(3) 0.000(2) 0.007(2) 0.020(2) O2 0.035(2) 0.053(3) 0.041(3) 0.007(2) 0.009(2) 0.024(2) O3 0.050(3) 0.043(3) 0.027(3) 0.006(2) 0.009(2) 0.009(2) O4 0.039(2) 0.056(3) 0.028(3) 0.003(2) 0.010(2) 0.024(2) O5 0.043(3) 0.054(3) 0.038(3) 0.012(2) 0.009(2) 0.019(2) O6 0.045(3) 0.045(3) 0.043(3) -0.001(2) 0.007(2) 0.016(2) O7 0.050(3) 0.172(7) 0.058(4) -0.015(4) 0.021(3) 0.045(4) O8 0.069(4) 0.070(4) 0.060(4) 0.017(3) 0.008(3) 0.028(3) O9 0.078(4) 0.074(4) 0.073(4) 0.004(3) 0.032(4) 0.007(3) O10 0.077(4) 0.103(5) 0.093(5) 0.058(4) 0.027(4) 0.048(4) O11 0.055(4) 0.081(4) 0.154(7) -0.045(4) -0.015(4) 0.023(3) O12 0.040(3) 0.078(4) 0.057(4) 0.002(3) 0.018(3) 0.013(3) O13 0.058(3) 0.069(3) 0.034(3) 0.016(2) 0.011(2) 0.036(3) O14 0.144(5) 0.090(4) 0.069(4) 0.032(3) 0.038(4) 0.068(4) C1 0.038(4) 0.052(4) 0.021(3) -0.002(3) 0.002(3) 0.018(3) C2 0.042(4) 0.050(4) 0.030(4) 0.013(3) 0.018(3) 0.019(3) C3 0.033(3) 0.038(4) 0.032(4) -0.002(3) 0.009(3) 0.012(3) C4 0.034(3) 0.046(4) 0.020(3) 0.005(3) 0.004(3) 0.015(3) C5 0.040(4) 0.048(4) 0.034(4) 0.012(3) 0.011(3) 0.008(3) C6 0.036(3) 0.048(4) 0.034(4) 0.002(3) 0.004(3) 0.025(3) C7 0.043(4) 0.073(5) 0.039(4) 0.010(4) 0.021(3) 0.028(4) C8 0.084(6) 0.090(7) 0.034(5) -0.005(4) 0.013(4) 0.035(5) C9 0.056(5) 0.063(5) 0.032(4) 0.005(3) 0.003(3) 0.028(4) C10 0.070(6) 0.096(7) 0.130(10) -0.003(6) 0.005(6) 0.052(5) C11 0.078(6) 0.061(6) 0.032(5) -0.008(4) 0.001(4) 0.011(5) C12 0.143(9) 0.068(6) 0.052(6) 0.011(5) 0.035(6) 0.037(6) C13 0.059(5) 0.053(5) 0.048(5) 0.018(4) 0.011(4) 0.020(4) C14 0.097(7) 0.104(8) 0.092(8) 0.061(6) 0.028(6) 0.038(6) C15 0.056(5) 0.063(5) 0.052(5) -0.008(4) -0.001(4) 0.018(4) C16 0.101(7) 0.062(6) 0.085(7) -0.020(5) 0.006(5) 0.040(5) C17 0.052(4) 0.054(4) 0.030(4) 0.013(3) 0.014(3) 0.024(3) C18 0.045(3) 0.046(3) 0.035(3) 0.002(2) 0.012(3) 0.017(3) C19 0.048(4) 0.070(4) 0.055(4) 0.001(3) 0.004(3) 0.018(3) C20 0.080(5) 0.059(4) 0.045(4) -0.007(3) 0.008(4) 0.012(4) C21 0.099(6) 0.070(5) 0.045(4) 0.003(3) 0.029(4) 0.042(4) C22 0.109(7) 0.093(6) 0.062(5) 0.008(4) 0.032(5) 0.066(5) C23 0.081(5) 0.065(5) 0.049(5) 0.012(4) 0.015(4) 0.030(4) C24 0.045(4) 0.070(4) 0.044(4) 0.006(3) 0.021(3) 0.024(3) C25 0.110(6) 0.071(5) 0.051(5) 0.015(4) 0.050(4) 0.024(4) C26 0.035(4) 0.137(8) 0.098(7) -0.002(6) 0.019(4) 0.027(4) S1' 0.0440(10) 0.0545(11) 0.0325(10) 0.0069(8) 0.0132(8) 0.0183(8) O1' 0.053(3) 0.041(3) 0.037(3) 0.000(2) 0.012(2) 0.019(2) O2' 0.042(3) 0.055(3) 0.029(3) 0.003(2) 0.004(2) 0.015(2) O3' 0.045(3) 0.070(3) 0.031(3) -0.006(2) 0.008(2) 0.029(2) O4' 0.045(3) 0.052(3) 0.045(3) -0.008(2) 0.003(2) 0.021(2) O5' 0.052(3) 0.039(3) 0.045(3) 0.012(2) 0.016(2) 0.014(2) O6' 0.043(3) 0.061(3) 0.023(3) -0.003(2) 0.005(2) 0.017(2) O7' 0.067(4) 0.066(4) 0.076(4) 0.010(3) 0.036(3) 0.007(3) O8' 0.078(4) 0.067(4) 0.051(3) 0.019(3) 0.016(3) 0.030(3) O9' 0.085(4) 0.145(6) 0.051(3) -0.009(3) 0.014(3) 0.073(4) O10' 0.051(4) 0.106(5) 0.124(6) 0.050(4) 0.023(4) 0.039(3) O11' 0.058(4) 0.088(5) 0.170(8) -0.038(5) 0.005(4) 0.018(3) O12' 0.064(4) 0.070(4) 0.050(3) -0.005(3) 0.021(3) 0.002(3) O13' 0.086(4) 0.085(4) 0.025(3) 0.018(3) 0.011(3) 0.043(3) O14' 0.385(16) 0.189(9) 0.113(7) 0.096(7) 0.133(9) 0.230(11) C1' 0.049(4) 0.050(4) 0.024(4) 0.005(3) 0.004(3) 0.020(3) C2' 0.032(4) 0.052(4) 0.034(4) -0.003(3) 0.005(3) 0.013(3) C3' 0.032(3) 0.061(5) 0.032(4) 0.003(3) 0.009(3) 0.023(3) C4' 0.043(4) 0.050(4) 0.027(4) -0.002(3) 0.008(3) 0.013(3) C5' 0.031(3) 0.045(4) 0.027(4) -0.003(3) 0.002(3) 0.016(3) C6' 0.038(4) 0.055(4) 0.025(4) 0.001(3) -0.003(3) 0.016(3) C7' 0.062(5) 0.043(4) 0.032(4) 0.011(3) 0.013(4) 0.009(4) C8' 0.090(6) 0.035(4) 0.091(7) 0.011(4) 0.022(5) 0.007(4) C9' 0.060(5) 0.048(4) 0.044(4) 0.003(4) 0.017(4) 0.021(4) C10' 0.053(4) 0.081(5) 0.088(6) 0.020(5) 0.006(4) 0.035(4) C11' 0.066(5) 0.065(5) 0.050(5) -0.005(4) 0.027(4) 0.027(4) C12' 0.078(6) 0.087(6) 0.038(5) -0.004(4) 0.020(4) 0.034(5) C13' 0.077(6) 0.056(5) 0.070(6) 0.022(5) 0.019(5) 0.024(5) C14' 0.095(8) 0.116(9) 0.125(11) 0.077(8) 0.049(7) 0.029(7) C15' 0.061(5) 0.053(5) 0.071(6) -0.012(4) 0.001(4) 0.024(4) C16' 0.103(8) 0.075(7) 0.149(12) -0.044(7) 0.000(8) 0.021(6) C17' 0.042(4) 0.083(5) 0.033(4) 0.007(4) 0.008(3) 0.028(4) C18' 0.046(4) 0.059(4) 0.037(3) 0.001(3) 0.009(3) 0.018(3) C19' 0.051(5) 0.169(10) 0.119(9) -0.049(7) 0.037(5) 0.011(6) C20' 0.086(6) 0.141(9) 0.145(10) -0.042(8) 0.070(7) 0.023(6) C21' 0.082(6) 0.099(6) 0.061(5) 0.002(5) 0.042(5) 0.034(5) C22' 0.160(10) 0.119(8) 0.090(8) 0.022(6) 0.055(7) 0.089(8) C23' 0.209(12) 0.131(9) 0.082(7) 0.051(7) 0.071(8) 0.141(9) C24' 0.059(5) 0.103(5) 0.039(4) -0.008(4) 0.014(3) 0.035(4) C25' 0.240(16) 0.221(14) 0.050(6) 0.049(7) 0.047(8) 0.175(13) C26' 0.079(7) 0.258(18) 0.157(13) -0.134(13) 0.025(8) 0.019(9) Cl1 0.081(6) 0.199(10) 0.048(5) 0.031(6) -0.001(4) -0.003(6) Cl2 0.147(10) 0.140(9) 0.110(9) 0.009(7) 0.008(8) 0.057(8) C27 0.22(5) 0.08(2) 0.06(2) -0.016(14) -0.04(2) 0.017(16) _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 O12 1.405(5) . ? S1 O13 1.437(5) . ? S1 O4 1.593(5) . ? S1 C17 1.748(7) . ? O1 C7 1.354(8) . ? O1 C1 1.442(7) . ? O2 C9 1.328(9) . ? O2 C2 1.465(8) . ? O3 C11 1.381(10) . ? O3 C3 1.427(7) . ? O4 C4 1.439(7) . ? O5 C13 1.381(9) . ? O5 C5 1.432(8) . ? O6 C15 1.337(9) . ? O6 C6 1.460(7) . ? O7 C7 1.173(8) . ? O8 C9 1.199(10) . ? O9 C11 1.198(10) . ? O10 C13 1.188(9) . ? O11 C15 1.208(9) . ? O14 C23 1.205(10) . ? C1 C6 1.509(10) . ? C1 C2 1.526(9) . ? C1 H1 0.9800 . ? C2 C3 1.533(9) . ? C2 H2 0.9800 . ? C3 C4 1.534(9) . ? C3 H3 0.9800 . ? C4 C5 1.493(9) . ? C4 H4 0.9800 . ? C5 C6 1.519(10) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.460(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.524(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.480(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.471(12) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.465(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.555(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.488(10) . ? C18 C24 1.552(8) . ? C18 C19 1.577(9) . ? C19 C20 1.535(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.536(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.523(12) . ? C21 C24 1.557(10) . ? C21 H21 0.9800 . ? C22 C23 1.512(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C26 1.512(10) . ? C24 C25 1.526(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O12' 1.409(5) . ? S1' O13' 1.418(5) . ? S1' O6' 1.582(5) . ? S1' C17' 1.735(8) . ? O1' C7' 1.342(8) . ? O1' C1' 1.435(8) . ? O2' C9' 1.380(9) . ? O2' C2' 1.440(8) . ? O3' C11' 1.373(8) . ? O3' C3' 1.411(8) . ? O4' C15' 1.343(9) . ? O4' C4' 1.404(8) . ? O5' C13' 1.324(10) . ? O5' C5' 1.428(8) . ? O6' C6' 1.458(8) . ? O7' C7' 1.188(8) . ? O8' C9' 1.172(9) . ? O9' C11' 1.202(10) . ? O10' C13' 1.195(10) . ? O11' C15' 1.176(9) . ? O14' C23' 1.186(13) . ? C1' C6' 1.505(10) . ? C1' C2' 1.544(9) . ? C1' H1' 0.9800 . ? C2' C3' 1.483(9) . ? C2' H2' 0.9800 . ? C3' C4' 1.526(10) . ? C3' H3' 0.9800 . ? C4' C5' 1.530(9) . ? C4' H4' 0.9800 . ? C5' C6' 1.527(9) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.475(11) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.480(11) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C12' 1.493(11) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.510(13) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.497(12) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.525(9) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.498(12) . ? C18' C19' 1.502(11) . ? C18' C24' 1.539(9) . ? C19' C20' 1.568(13) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.507(13) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.496(14) . ? C21' C24' 1.525(10) . ? C21' H21' 0.9800 . ? C22' C23' 1.525(14) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C26' 1.474(14) . ? C24' C25' 1.577(13) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? Cl1 C27 1.733(19) . ? Cl2 C27 1.736(19) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? 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 O12 S1 O13 118.7(3) . . ? O12 S1 O4 110.3(3) . . ? O13 S1 O4 102.9(3) . . ? O12 S1 C17 110.3(4) . . ? O13 S1 C17 111.5(3) . . ? O4 S1 C17 101.4(3) . . ? C7 O1 C1 116.9(5) . . ? C9 O2 C2 117.3(6) . . ? C11 O3 C3 116.3(6) . . ? C4 O4 S1 122.5(4) . . ? C13 O5 C5 118.7(6) . . ? C15 O6 C6 118.9(5) . . ? O1 C1 C6 108.3(5) . . ? O1 C1 C2 109.9(5) . . ? C6 C1 C2 109.6(5) . . ? O1 C1 H1 109.7 . . ? C6 C1 H1 109.7 . . ? C2 C1 H1 109.7 . . ? O2 C2 C1 108.4(5) . . ? O2 C2 C3 108.8(5) . . ? C1 C2 C3 109.3(5) . . ? O2 C2 H2 110.1 . . ? C1 C2 H2 110.1 . . ? C3 C2 H2 110.1 . . ? O3 C3 C2 109.8(5) . . ? O3 C3 C4 106.4(5) . . ? C2 C3 C4 111.6(5) . . ? O3 C3 H3 109.7 . . ? C2 C3 H3 109.7 . . ? C4 C3 H3 109.7 . . ? O4 C4 C5 107.9(5) . . ? O4 C4 C3 106.7(5) . . ? C5 C4 C3 109.7(5) . . ? O4 C4 H4 110.8 . . ? C5 C4 H4 110.8 . . ? C3 C4 H4 110.8 . . ? O5 C5 C4 107.1(6) . . ? O5 C5 C6 108.7(5) . . ? C4 C5 C6 111.4(6) . . ? O5 C5 H5 109.9 . . ? C4 C5 H5 109.9 . . ? C6 C5 H5 109.9 . . ? O6 C6 C1 106.8(5) . . ? O6 C6 C5 107.9(5) . . ? C1 C6 C5 110.8(5) . . ? O6 C6 H6 110.4 . . ? C1 C6 H6 110.4 . . ? C5 C6 H6 110.4 . . ? O7 C7 O1 122.9(7) . . ? O7 C7 C8 125.4(7) . . ? O1 C7 C8 111.6(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 125.0(7) . . ? O8 C9 C10 123.8(8) . . ? O2 C9 C10 111.2(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 121.0(8) . . ? O9 C11 C12 128.4(9) . . ? O3 C11 C12 110.6(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 121.6(7) . . ? O10 C13 C14 128.4(8) . . ? O5 C13 C14 110.0(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 121.1(7) . . ? O11 C15 C16 126.3(8) . . ? O6 C15 C16 112.3(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 118.8(5) . . ? C18 C17 H17A 107.6 . . ? S1 C17 H17A 107.6 . . ? C18 C17 H17B 107.6 . . ? S1 C17 H17B 107.6 . . ? H17A C17 H17B 107.0 . . ? C23 C18 C24 100.4(5) . . ? C23 C18 C17 108.0(6) . . ? C24 C18 C17 124.4(5) . . ? C23 C18 C19 104.9(5) . . ? C24 C18 C19 102.2(5) . . ? C17 C18 C19 114.5(5) . . ? C20 C19 C18 102.5(5) . . ? C20 C19 H19A 111.3 . . ? C18 C19 H19A 111.3 . . ? C20 C19 H19B 111.3 . . ? C18 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? C19 C20 C21 104.4(5) . . ? C19 C20 H20A 110.9 . . ? C21 C20 H20A 110.9 . . ? C19 C20 H20B 110.9 . . ? C21 C20 H20B 110.9 . . ? H20A C20 H20B 108.9 . . ? C22 C21 C20 105.8(7) . . ? C22 C21 C24 103.3(6) . . ? C20 C21 C24 101.8(6) . . ? C22 C21 H21 114.8 . . ? C20 C21 H21 114.8 . . ? C24 C21 H21 114.8 . . ? C23 C22 C21 101.3(7) . . ? C23 C22 H22A 111.5 . . ? C21 C22 H22A 111.5 . . ? C23 C22 H22B 111.5 . . ? C21 C22 H22B 111.5 . . ? H22A C22 H22B 109.3 . . ? O14 C23 C18 126.4(8) . . ? O14 C23 C22 126.0(8) . . ? C18 C23 C22 107.5(7) . . ? C26 C24 C25 109.1(6) . . ? C26 C24 C18 112.3(6) . . ? C25 C24 C18 115.5(5) . . ? C26 C24 C21 114.1(6) . . ? C25 C24 C21 112.0(6) . . ? C18 C24 C21 93.3(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12' S1' O13' 119.6(4) . . ? O12' S1' O6' 110.0(3) . . ? O13' S1' O6' 103.7(3) . . ? O12' S1' C17' 110.5(4) . . ? O13' S1' C17' 108.8(3) . . ? O6' S1' C17' 102.8(3) . . ? C7' O1' C1' 115.9(5) . . ? C9' O2' C2' 117.2(5) . . ? C11' O3' C3' 118.0(6) . . ? C15' O4' C4' 117.7(5) . . ? C13' O5' C5' 117.4(6) . . ? C6' O6' S1' 122.0(4) . . ? O1' C1' C6' 106.2(6) . . ? O1' C1' C2' 110.2(5) . . ? C6' C1' C2' 110.8(5) . . ? O1' C1' H1' 109.8 . . ? C6' C1' H1' 109.8 . . ? C2' C1' H1' 109.8 . . ? O2' C2' C3' 108.9(5) . . ? O2' C2' C1' 107.6(5) . . ? C3' C2' C1' 109.0(6) . . ? O2' C2' H2' 110.4 . . ? C3' C2' H2' 110.4 . . ? C1' C2' H2' 110.4 . . ? O3' C3' C2' 110.5(6) . . ? O3' C3' C4' 108.1(5) . . ? C2' C3' C4' 113.1(6) . . ? O3' C3' H3' 108.4 . . ? C2' C3' H3' 108.4 . . ? C4' C3' H3' 108.4 . . ? O4' C4' C3' 110.3(5) . . ? O4' C4' C5' 108.4(6) . . ? C3' C4' C5' 109.1(5) . . ? O4' C4' H4' 109.7 . . ? C3' C4' H4' 109.7 . . ? C5' C4' H4' 109.7 . . ? O5' C5' C6' 109.3(5) . . ? O5' C5' C4' 108.7(5) . . ? C6' C5' C4' 109.7(6) . . ? O5' C5' H5' 109.7 . . ? C6' C5' H5' 109.7 . . ? C4' C5' H5' 109.7 . . ? O6' C6' C1' 107.4(5) . . ? O6' C6' C5' 106.1(5) . . ? C1' C6' C5' 112.0(6) . . ? O6' C6' H6' 110.4 . . ? C1' C6' H6' 110.4 . . ? C5' C6' H6' 110.4 . . ? O7' C7' O1' 124.2(7) . . ? O7' C7' C8' 126.2(7) . . ? O1' C7' C8' 109.6(7) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 122.2(7) . . ? O8' C9' C10' 128.4(8) . . ? O2' C9' C10' 109.5(7) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? O9' C11' O3' 122.9(7) . . ? O9' C11' C12' 126.2(7) . . ? O3' C11' C12' 110.6(7) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O10' C13' O5' 124.8(8) . . ? O10' C13' C14' 125.6(9) . . ? O5' C13' C14' 109.6(8) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O4' 123.9(7) . . ? O11' C15' C16' 127.0(8) . . ? O4' C15' C16' 108.9(7) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 118.9(6) . . ? C18' C17' H17C 107.6 . . ? S1' C17' H17C 107.6 . . ? C18' C17' H17D 107.6 . . ? S1' C17' H17D 107.6 . . ? H17C C17' H17D 107.0 . . ? C23' C18' C19' 104.8(9) . . ? C23' C18' C17' 108.9(6) . . ? C19' C18' C17' 118.8(6) . . ? C23' C18' C24' 98.0(7) . . ? C19' C18' C24' 103.0(7) . . ? C17' C18' C24' 120.4(5) . . ? C18' C19' C20' 104.0(7) . . ? C18' C19' H19C 111.0 . . ? C20' C19' H19C 111.0 . . ? C18' C19' H19D 111.0 . . ? C20' C19' H19D 111.0 . . ? H19C C19' H19D 109.0 . . ? C21' C20' C19' 102.1(7) . . ? C21' C20' H20C 111.4 . . ? C19' C20' H20C 111.4 . . ? C21' C20' H20D 111.4 . . ? C19' C20' H20D 111.4 . . ? H20C C20' H20D 109.2 . . ? C22' C21' C20' 105.5(10) . . ? C22' C21' C24' 102.2(7) . . ? C20' C21' C24' 105.0(7) . . ? C22' C21' H21' 114.3 . . ? C20' C21' H21' 114.3 . . ? C24' C21' H21' 114.3 . . ? C21' C22' C23' 100.4(8) . . ? C21' C22' H22C 111.7 . . ? C23' C22' H22C 111.7 . . ? C21' C22' H22D 111.7 . . ? C23' C22' H22D 111.7 . . ? H22C C22' H22D 109.5 . . ? O14' C23' C18' 126.9(9) . . ? O14' C23' C22' 125.5(9) . . ? C18' C23' C22' 107.6(9) . . ? C26' C24' C21' 114.3(8) . . ? C26' C24' C18' 114.7(8) . . ? C21' C24' C18' 94.4(6) . . ? C26' C24' C25' 111.5(10) . . ? C21' C24' C25' 108.8(7) . . ? C18' C24' C25' 112.0(7) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? Cl1 C27 Cl2 117.3(17) . . ? Cl1 C27 H27A 108.0 . . ? Cl2 C27 H27A 108.0 . . ? Cl1 C27 H27B 108.0 . . ? Cl2 C27 H27B 108.0 . . ? H27A C27 H27B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.478 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.084 #===END data_1.2AN _database_code_depnum_ccdc_archive 'CCDC 846744' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.2AN ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 97 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT113_1.2AN ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P-1 RESPONSE: Since the host molecule has a chiral camphorsulfonyl group, the crystals can not belong to a centro-symmetric space group. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULFONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, C2 H3 N, 0.5 (H2 O)' _chemical_formula_sum 'C28 H39 N O14.50 S' _chemical_formula_weight 653.66 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.404(4) _cell_length_b 12.492(4) _cell_length_c 13.331(4) _cell_angle_alpha 99.188(5) _cell_angle_beta 109.620(5) _cell_angle_gamma 116.837(4) _cell_volume 1612.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5356 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.26 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9050 _exptl_absorpt_correction_T_max 0.9430 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15615 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11129 _reflns_number_gt 10662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.0560P)^2^+0.2701P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 11129 _refine_ls_number_parameters 817 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.50471(5) 0.69917(5) 0.92969(4) 0.02714(14) Uani 1 1 d . . . O1 O 0.60770(18) 1.30246(17) 1.05030(16) 0.0321(4) Uani 1 1 d . . . O2 O 0.40129(17) 1.05227(17) 0.90632(16) 0.0337(4) Uani 1 1 d . . . O3 O 0.45074(17) 0.89879(17) 0.76952(14) 0.0305(4) Uani 1 1 d . . . O4 O 0.59545(16) 0.84576(16) 0.94511(15) 0.0284(4) Uani 1 1 d . . . O5 O 0.65175(17) 0.97594(17) 1.16792(15) 0.0306(4) Uani 1 1 d . . . O6 O 0.75665(19) 1.24469(18) 1.22175(16) 0.0345(4) Uani 1 1 d . . . O7 O 0.8230(2) 1.4657(2) 1.1071(2) 0.0485(5) Uani 1 1 d . . . O8 O 0.2944(2) 1.0295(2) 0.72266(18) 0.0464(5) Uani 1 1 d . . . O9 O 0.5534(2) 1.0203(2) 0.68279(17) 0.0462(5) Uani 1 1 d . . . O10 O 0.8752(2) 1.0492(2) 1.2488(2) 0.0503(5) Uani 1 1 d . . . O11 O 0.6197(2) 1.2546(3) 1.29274(19) 0.0629(7) Uani 1 1 d . . . O12 O 0.4336(2) 0.69010(18) 0.99577(17) 0.0386(4) Uani 1 1 d . . . O13 O 0.60038(18) 0.66071(18) 0.95535(16) 0.0342(4) Uani 1 1 d . . . O14 O 0.1939(2) 0.5021(2) 0.55418(18) 0.0477(5) Uani 1 1 d . . . C1 C 0.6392(3) 1.2079(2) 1.0237(2) 0.0293(5) Uani 1 1 d . . . H1 H 0.7286 1.2496 1.0252 0.035 Uiso 1 1 calc R . . C2 C 0.5302(2) 1.1070(2) 0.9047(2) 0.0288(5) Uani 1 1 d . . . H2 H 0.5300 1.1466 0.8468 0.035 Uiso 1 1 calc R . . C3 C 0.5578(3) 1.0005(2) 0.8793(2) 0.0291(5) Uani 1 1 d . . . H3 H 0.6460 1.0369 0.8788 0.035 Uiso 1 1 calc R . . C4 C 0.5569(3) 0.9372(2) 0.9677(2) 0.0275(5) Uani 1 1 d . . . H4 H 0.4665 0.8935 0.9640 0.033 Uiso 1 1 calc R . . C5 C 0.6643(2) 1.0388(2) 1.0869(2) 0.0271(5) Uani 1 1 d . . . H5 H 0.7553 1.0734 1.0925 0.033 Uiso 1 1 calc R . . C6 C 0.6426(2) 1.1477(2) 1.1138(2) 0.0290(5) Uani 1 1 d . . . H6 H 0.5576 1.1158 1.1196 0.035 Uiso 1 1 calc R . . C7 C 0.7121(3) 1.4292(3) 1.0985(2) 0.0327(6) Uani 1 1 d . . . C8 C 0.6677(3) 1.5122(3) 1.1402(3) 0.0458(7) Uani 1 1 d . . . H8A H 0.7332 1.6009 1.1573 0.069 Uiso 1 1 calc R . . H8B H 0.6609 1.5024 1.2082 0.069 Uiso 1 1 calc R . . H8C H 0.5804 1.4868 1.0820 0.069 Uiso 1 1 calc R . . C9 C 0.2911(3) 1.0201(3) 0.8101(3) 0.0389(7) Uani 1 1 d . . . C10 C 0.1693(3) 0.9709(4) 0.8285(3) 0.0576(9) Uani 1 1 d . . . H10A H 0.0920 0.9477 0.7596 0.086 Uiso 1 1 calc R . . H10B H 0.1843 1.0368 0.8897 0.086 Uiso 1 1 calc R . . H10C H 0.1525 0.8963 0.8483 0.086 Uiso 1 1 calc R . . C11 C 0.4627(3) 0.9230(3) 0.6771(2) 0.0356(6) Uani 1 1 d . . . C12 C 0.3474(4) 0.8130(3) 0.5678(3) 0.0513(8) Uani 1 1 d . . . H12A H 0.2906 0.8397 0.5265 0.077 Uiso 1 1 calc R . . H12B H 0.2946 0.7414 0.5851 0.077 Uiso 1 1 calc R . . H12C H 0.3832 0.7876 0.5218 0.077 Uiso 1 1 calc R . . C13 C 0.7655(3) 0.9870(3) 1.2429(2) 0.0355(6) Uani 1 1 d . . . C14 C 0.7313(4) 0.9087(4) 1.3149(3) 0.0581(9) Uani 1 1 d . . . H14A H 0.7992 0.8893 1.3453 0.087 Uiso 1 1 calc R . . H14B H 0.6437 0.8298 1.2686 0.087 Uiso 1 1 calc R . . H14C H 0.7290 0.9572 1.3770 0.087 Uiso 1 1 calc R . . C15 C 0.7321(3) 1.2927(3) 1.3040(2) 0.0392(7) Uani 1 1 d . . . C16 C 0.8616(4) 1.3969(4) 1.4038(3) 0.0622(10) Uani 1 1 d . . . H16A H 0.8442 1.4221 1.4655 0.093 Uiso 1 1 calc R . . H16B H 0.9037 1.4697 1.3833 0.093 Uiso 1 1 calc R . . H16C H 0.9212 1.3668 1.4276 0.093 Uiso 1 1 calc R . . C17 C 0.3877(3) 0.6245(2) 0.7816(2) 0.0295(5) Uani 1 1 d . . . H17A H 0.3146 0.6387 0.7710 0.035 Uiso 1 1 calc R . . H17B H 0.4341 0.6686 0.7412 0.035 Uiso 1 1 calc R . . C18 C 0.3236(2) 0.4802(2) 0.72414(19) 0.0290(5) Uani 1 1 d . . . C19 C 0.4195(2) 0.4425(2) 0.7007(2) 0.0336(5) Uani 1 1 d . . . H19A H 0.4392 0.4699 0.6415 0.040 Uiso 1 1 calc R . . H19B H 0.5046 0.4811 0.7698 0.040 Uiso 1 1 calc R . . C20 C 0.3376(3) 0.2942(2) 0.6610(2) 0.0406(6) Uani 1 1 d . . . H20A H 0.3236 0.2547 0.5851 0.049 Uiso 1 1 calc R . . H20B H 0.3834 0.2659 0.7141 0.049 Uiso 1 1 calc R . . C21 C 0.2020(3) 0.2615(2) 0.6599(2) 0.0398(6) Uani 1 1 d . . . H21 H 0.1483 0.1753 0.6604 0.048 Uiso 1 1 calc R . . C22 C 0.1255(3) 0.2876(3) 0.5589(2) 0.0397(6) Uani 1 1 d . . . H22A H 0.1254 0.2501 0.4893 0.048 Uiso 1 1 calc R . . H22B H 0.0323 0.2548 0.5448 0.048 Uiso 1 1 calc R . . C23 C 0.2110(3) 0.4344(3) 0.6038(2) 0.0351(6) Uani 1 1 d . . . C24 C 0.2475(2) 0.3746(2) 0.7667(2) 0.0355(5) Uani 1 1 d . . . C25 C 0.3362(3) 0.3729(3) 0.8776(2) 0.0441(7) Uani 1 1 d . . . H25A H 0.3639 0.4441 0.9416 0.066 Uiso 1 1 calc R . . H25B H 0.4154 0.3802 0.8745 0.066 Uiso 1 1 calc R . . H25C H 0.2850 0.2933 0.8862 0.066 Uiso 1 1 calc R . . C26 C 0.1296(3) 0.3774(3) 0.7779(3) 0.0495(7) Uani 1 1 d . . . H26A H 0.0732 0.2997 0.7865 0.074 Uiso 1 1 calc R . . H26B H 0.0763 0.3836 0.7104 0.074 Uiso 1 1 calc R . . H26C H 0.1657 0.4508 0.8439 0.074 Uiso 1 1 calc R . . S1' S 0.00213(5) 1.14758(5) 0.02672(4) 0.02851(14) Uani 1 1 d . . . O1' O 0.05063(18) 0.94195(16) 0.18637(14) 0.0301(4) Uani 1 1 d . . . O2' O 0.10060(16) 0.79025(16) 0.04952(15) 0.0300(4) Uani 1 1 d . . . O3' O -0.11140(17) 0.54009(17) -0.09914(15) 0.0302(4) Uani 1 1 d . . . O4' O -0.24971(17) 0.60556(17) -0.26900(15) 0.0301(4) Uani 1 1 d . . . O5' O -0.14480(17) 0.87477(17) -0.20973(15) 0.0311(4) Uani 1 1 d . . . O6' O -0.08852(17) 1.00232(17) 0.01486(15) 0.0296(4) Uani 1 1 d . . . O7' O -0.0585(2) 0.81985(19) 0.26914(17) 0.0449(5) Uani 1 1 d . . . O8' O 0.2029(2) 0.8063(2) 0.23108(19) 0.0464(5) Uani 1 1 d . . . O9' O -0.3304(2) 0.38215(19) -0.16032(19) 0.0462(5) Uani 1 1 d . . . O10' O -0.3685(2) 0.8013(3) -0.2936(2) 0.0547(6) Uani 1 1 d . . . O11' O -0.1101(2) 0.5890(2) -0.33386(18) 0.0543(6) Uani 1 1 d . . . O12' O 0.0768(2) 1.15494(19) -0.03590(17) 0.0429(5) Uani 1 1 d . . . O13' O -0.0931(2) 1.18466(19) -0.00234(19) 0.0432(5) Uani 1 1 d . . . O14' O 0.3125(2) 1.3400(2) 0.40333(17) 0.0454(5) Uani 1 1 d . . . C1' C -0.0555(2) 0.8441(2) 0.0772(2) 0.0259(5) Uani 1 1 d . . . H1' H -0.1438 0.8088 0.0776 0.031 Uiso 1 1 calc R . . C2' C -0.0311(2) 0.7356(2) 0.0490(2) 0.0275(5) Uani 1 1 d . . . H2' H -0.0335 0.6937 0.1051 0.033 Uiso 1 1 calc R . . C3' C -0.1389(2) 0.6378(2) -0.0710(2) 0.0270(5) Uani 1 1 d . . . H3' H -0.2289 0.5977 -0.0737 0.032 Uiso 1 1 calc R . . C4' C -0.1382(2) 0.7007(2) -0.1601(2) 0.0273(5) Uani 1 1 d . . . H4' H -0.0518 0.7335 -0.1636 0.033 Uiso 1 1 calc R . . C5' C -0.1598(2) 0.8102(2) -0.1313(2) 0.0264(5) Uani 1 1 d . . . H5' H -0.2513 0.7754 -0.1378 0.032 Uiso 1 1 calc R . . C6' C -0.0526(2) 0.9090(2) -0.0101(2) 0.0258(5) Uani 1 1 d . . . H6' H 0.0383 0.9522 -0.0056 0.031 Uiso 1 1 calc R . . C7' C 0.0376(3) 0.9171(3) 0.2790(2) 0.0340(6) Uani 1 1 d . . . C8' C 0.1542(4) 1.0235(3) 0.3875(3) 0.0511(8) Uani 1 1 d . . . H8D H 0.1282 1.0219 0.4477 0.077 Uiso 1 1 calc R . . H8E H 0.1803 1.1047 0.3780 0.077 Uiso 1 1 calc R . . H8F H 0.2297 1.0130 0.4071 0.077 Uiso 1 1 calc R . . C9' C 0.2086(3) 0.8203(3) 0.1464(2) 0.0357(6) Uani 1 1 d . . . C10' C 0.3342(3) 0.8716(4) 0.1300(3) 0.0610(10) Uani 1 1 d . . . H10D H 0.4044 0.9553 0.1886 0.091 Uiso 1 1 calc R . . H10E H 0.3133 0.8785 0.0561 0.091 Uiso 1 1 calc R . . H10F H 0.3652 0.8138 0.1349 0.091 Uiso 1 1 calc R . . C11' C -0.2186(3) 0.4150(3) -0.1495(2) 0.0333(6) Uani 1 1 d . . . C12' C -0.1768(3) 0.3281(3) -0.1878(3) 0.0456(7) Uani 1 1 d . . . H12F H -0.2530 0.2548 -0.2550 0.068 Uiso 1 1 calc R . . H12D H -0.1468 0.2992 -0.1278 0.068 Uiso 1 1 calc R . . H12E H -0.1037 0.3741 -0.2053 0.068 Uiso 1 1 calc R . . C13' C -0.2576(3) 0.8664(3) -0.2845(3) 0.0380(6) Uani 1 1 d . . . C14' C -0.2209(4) 0.9496(4) -0.3519(3) 0.0616(10) Uani 1 1 d . . . H14D H -0.2955 0.9098 -0.4277 0.092 Uiso 1 1 calc R . . H14E H -0.1416 0.9595 -0.3565 0.092 Uiso 1 1 calc R . . H14F H -0.2022 1.0328 -0.3146 0.092 Uiso 1 1 calc R . . C15' C -0.2223(3) 0.5548(3) -0.3466(2) 0.0371(6) Uani 1 1 d . . . C16' C -0.3527(3) 0.4474(3) -0.4490(3) 0.0540(8) Uani 1 1 d . . . H16D H -0.3674 0.4751 -0.5128 0.081 Uiso 1 1 calc R . . H16E H -0.4273 0.4249 -0.4315 0.081 Uiso 1 1 calc R . . H16F H -0.3470 0.3734 -0.4683 0.081 Uiso 1 1 calc R . . C17' C 0.1146(3) 1.2255(3) 0.1760(2) 0.0309(6) Uani 1 1 d . . . H17C H 0.0604 1.2189 0.2156 0.037 Uiso 1 1 calc R . . H17D H 0.1560 1.1775 0.1976 0.037 Uiso 1 1 calc R . . C18' C 0.2290(2) 1.3673(2) 0.22083(19) 0.0296(5) Uani 1 1 d . . . C19' C 0.3417(3) 1.4012(3) 0.1813(2) 0.0419(6) Uani 1 1 d . . . H19C H 0.3991 1.3709 0.2156 0.050 Uiso 1 1 calc R . . H19D H 0.3017 1.3638 0.0985 0.050 Uiso 1 1 calc R . . C20' C 0.4238(3) 1.5513(3) 0.2252(2) 0.0509(7) Uani 1 1 d . . . H20C H 0.5193 1.5883 0.2755 0.061 Uiso 1 1 calc R . . H20D H 0.4161 1.5812 0.1619 0.061 Uiso 1 1 calc R . . C21' C 0.3557(3) 1.5859(2) 0.2906(2) 0.0410(6) Uani 1 1 d . . . H21' H 0.3751 1.6736 0.3044 0.049 Uiso 1 1 calc R . . C22' C 0.3950(3) 1.5563(3) 0.3992(3) 0.0421(7) Uani 1 1 d . . . H22C H 0.4920 1.5911 0.4381 0.051 Uiso 1 1 calc R . . H22D H 0.3695 1.5898 0.4517 0.051 Uiso 1 1 calc R . . C23' C 0.3125(3) 1.4110(3) 0.3509(2) 0.0329(6) Uani 1 1 d . . . C24' C 0.2027(3) 1.4776(2) 0.2159(2) 0.0363(5) Uani 1 1 d . . . C25' C 0.1470(4) 1.4830(3) 0.0965(3) 0.0543(8) Uani 1 1 d . . . H25D H 0.0502 1.4216 0.0554 0.081 Uiso 1 1 calc R . . H25E H 0.1897 1.4624 0.0553 0.081 Uiso 1 1 calc R . . H25F H 0.1661 1.5682 0.1041 0.081 Uiso 1 1 calc R . . C26' C 0.1113(3) 1.4778(3) 0.2687(2) 0.0461(6) Uani 1 1 d . . . H26D H 0.1155 1.5577 0.2796 0.069 Uiso 1 1 calc R . . H26E H 0.1417 1.4687 0.3413 0.069 Uiso 1 1 calc R . . H26F H 0.0191 1.4071 0.2184 0.069 Uiso 1 1 calc R . . N1 N 0.7702(6) 0.7093(6) 0.4691(5) 0.1167(17) Uani 1 1 d . . . C27 C 1.0056(4) 0.7513(4) 0.5042(4) 0.0778(12) Uani 1 1 d . . . H27A H 1.0744 0.8398 0.5533 0.117 Uiso 1 1 calc R . . H27B H 1.0090 0.7343 0.4329 0.117 Uiso 1 1 calc R . . H27C H 1.0214 0.6958 0.5407 0.117 Uiso 1 1 calc R . . C28 C 0.8740(5) 0.7274(4) 0.4829(4) 0.0771(12) Uani 1 1 d . . . N2 N 0.7553(6) 0.1592(5) 0.5102(4) 0.1010(13) Uani 1 1 d . . . C29 C 0.6476(6) 0.1289(4) 0.4851(4) 0.0743(12) Uani 1 1 d . . . C30 C 0.5116(5) 0.0931(5) 0.4552(4) 0.0959(17) Uani 1 1 d . . . H30A H 0.4522 0.0007 0.4226 0.144 Uiso 1 1 calc R . . H30B H 0.4841 0.1286 0.4002 0.144 Uiso 1 1 calc R . . H30C H 0.5066 0.1260 0.5225 0.144 Uiso 1 1 calc R . . O1W O 0.1693(6) 0.6967(6) 0.8343(5) 0.0518(14) Uiso 0.35 1 d P . . O2W O 0.329(2) 0.121(2) 0.1368(18) 0.092(6) Uiso 0.15 1 d P . . 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 0.0287(3) 0.0231(3) 0.0251(3) 0.0076(2) 0.0116(3) 0.0118(3) O1 0.0302(9) 0.0246(10) 0.0388(10) 0.0083(8) 0.0163(8) 0.0138(8) O2 0.0294(9) 0.0320(10) 0.0364(11) 0.0117(8) 0.0158(8) 0.0143(8) O3 0.0298(9) 0.0255(9) 0.0236(9) 0.0048(7) 0.0082(7) 0.0101(7) O4 0.0284(9) 0.0215(9) 0.0305(9) 0.0062(7) 0.0137(8) 0.0112(7) O5 0.0329(9) 0.0304(10) 0.0278(9) 0.0132(8) 0.0147(8) 0.0156(8) O6 0.0338(9) 0.0299(10) 0.0301(10) 0.0043(8) 0.0132(8) 0.0137(8) O7 0.0374(11) 0.0301(10) 0.0671(15) 0.0151(10) 0.0223(10) 0.0127(9) O8 0.0393(11) 0.0440(12) 0.0429(13) 0.0174(10) 0.0096(10) 0.0194(9) O9 0.0555(13) 0.0421(12) 0.0354(11) 0.0161(9) 0.0239(10) 0.0200(11) O10 0.0376(11) 0.0674(15) 0.0512(13) 0.0336(12) 0.0198(10) 0.0292(11) O11 0.0519(14) 0.089(2) 0.0394(13) 0.0061(12) 0.0243(11) 0.0354(14) O12 0.0443(11) 0.0304(10) 0.0388(11) 0.0124(8) 0.0248(9) 0.0150(9) O13 0.0334(9) 0.0299(10) 0.0304(10) 0.0084(8) 0.0072(8) 0.0170(8) O14 0.0479(12) 0.0444(12) 0.0356(11) 0.0176(10) 0.0083(10) 0.0208(10) C1 0.0276(12) 0.0250(13) 0.0331(14) 0.0103(11) 0.0145(11) 0.0127(11) C2 0.0281(12) 0.0245(13) 0.0283(13) 0.0092(10) 0.0130(11) 0.0105(10) C3 0.0270(12) 0.0265(13) 0.0273(13) 0.0095(11) 0.0117(11) 0.0106(11) C4 0.0323(12) 0.0243(13) 0.0266(13) 0.0090(10) 0.0153(11) 0.0148(11) C5 0.0284(12) 0.0288(13) 0.0251(12) 0.0123(11) 0.0150(11) 0.0136(11) C6 0.0266(12) 0.0261(13) 0.0261(13) 0.0040(10) 0.0114(11) 0.0108(11) C7 0.0342(14) 0.0256(13) 0.0286(13) 0.0106(11) 0.0094(11) 0.0127(11) C8 0.0520(17) 0.0313(16) 0.0563(19) 0.0154(14) 0.0220(15) 0.0267(14) C9 0.0324(14) 0.0264(14) 0.0496(18) 0.0137(13) 0.0146(13) 0.0132(12) C10 0.0340(16) 0.067(2) 0.066(2) 0.0237(19) 0.0214(16) 0.0248(17) C11 0.0425(15) 0.0333(15) 0.0370(16) 0.0161(12) 0.0201(13) 0.0228(13) C12 0.064(2) 0.0458(18) 0.0278(15) 0.0087(13) 0.0094(14) 0.0273(16) C13 0.0421(16) 0.0393(15) 0.0311(14) 0.0147(12) 0.0182(12) 0.0251(13) C14 0.063(2) 0.074(2) 0.059(2) 0.0445(19) 0.0338(19) 0.0423(19) C15 0.0459(17) 0.0426(17) 0.0315(15) 0.0107(13) 0.0208(13) 0.0247(14) C16 0.056(2) 0.062(2) 0.0391(18) -0.0081(16) 0.0177(16) 0.0228(18) C17 0.0292(12) 0.0235(13) 0.0257(13) 0.0064(10) 0.0078(11) 0.0112(11) C18 0.0267(11) 0.0272(11) 0.0254(11) 0.0073(9) 0.0102(9) 0.0111(10) C19 0.0334(12) 0.0311(12) 0.0277(11) 0.0059(9) 0.0122(9) 0.0143(10) C20 0.0445(14) 0.0328(13) 0.0348(13) 0.0047(10) 0.0129(11) 0.0203(12) C21 0.0412(14) 0.0255(12) 0.0361(13) 0.0075(10) 0.0140(11) 0.0101(11) C22 0.0337(13) 0.0309(14) 0.0291(14) 0.0023(11) 0.0042(11) 0.0094(12) C23 0.0318(13) 0.0370(14) 0.0314(14) 0.0110(12) 0.0148(11) 0.0154(12) C24 0.0369(12) 0.0276(12) 0.0330(12) 0.0106(9) 0.0164(10) 0.0111(10) C25 0.0552(16) 0.0316(14) 0.0322(14) 0.0144(11) 0.0166(13) 0.0155(12) C26 0.0429(15) 0.0475(17) 0.0495(16) 0.0155(14) 0.0292(13) 0.0136(13) S1' 0.0325(3) 0.0220(3) 0.0255(3) 0.0082(2) 0.0120(3) 0.0119(3) O1' 0.0356(9) 0.0240(9) 0.0252(9) 0.0083(7) 0.0121(8) 0.0139(8) O2' 0.0243(8) 0.0269(9) 0.0319(10) 0.0078(8) 0.0116(8) 0.0109(7) O3' 0.0298(9) 0.0241(9) 0.0317(9) 0.0079(7) 0.0118(8) 0.0136(8) O4' 0.0278(8) 0.0274(9) 0.0239(9) 0.0021(7) 0.0089(7) 0.0114(7) O5' 0.0351(9) 0.0310(10) 0.0278(9) 0.0141(8) 0.0163(8) 0.0161(8) O6' 0.0311(9) 0.0258(9) 0.0309(10) 0.0097(7) 0.0159(8) 0.0139(8) O7' 0.0508(12) 0.0363(12) 0.0341(11) 0.0128(9) 0.0198(10) 0.0139(10) O8' 0.0387(11) 0.0528(13) 0.0416(12) 0.0180(10) 0.0114(10) 0.0253(10) O9' 0.0331(10) 0.0285(10) 0.0568(13) 0.0084(9) 0.0143(9) 0.0089(8) O10' 0.0444(12) 0.0774(17) 0.0537(14) 0.0397(13) 0.0233(11) 0.0359(12) O11' 0.0452(13) 0.0745(17) 0.0394(12) 0.0079(11) 0.0200(10) 0.0338(12) O12' 0.0528(12) 0.0288(10) 0.0359(11) 0.0082(8) 0.0265(10) 0.0111(9) O13' 0.0397(10) 0.0295(10) 0.0489(12) 0.0139(9) 0.0104(10) 0.0176(9) O14' 0.0440(11) 0.0388(11) 0.0330(11) 0.0153(9) 0.0073(9) 0.0143(9) C1' 0.0240(12) 0.0219(12) 0.0211(12) 0.0027(10) 0.0077(10) 0.0084(10) C2' 0.0246(11) 0.0268(13) 0.0297(13) 0.0113(10) 0.0126(10) 0.0126(10) C3' 0.0266(12) 0.0187(12) 0.0284(13) 0.0046(10) 0.0113(10) 0.0092(10) C4' 0.0247(12) 0.0244(13) 0.0259(13) 0.0074(10) 0.0103(10) 0.0098(10) C5' 0.0269(12) 0.0221(12) 0.0247(12) 0.0076(10) 0.0104(10) 0.0106(10) C6' 0.0227(11) 0.0232(13) 0.0289(13) 0.0082(10) 0.0119(10) 0.0110(10) C7' 0.0460(15) 0.0310(15) 0.0223(13) 0.0096(11) 0.0131(12) 0.0211(13) C8' 0.065(2) 0.0352(16) 0.0283(15) 0.0071(13) 0.0114(15) 0.0183(15) C9' 0.0284(13) 0.0337(15) 0.0352(15) 0.0055(12) 0.0086(12) 0.0165(12) C10' 0.0328(16) 0.072(2) 0.068(2) 0.0208(19) 0.0207(16) 0.0240(17) C11' 0.0375(15) 0.0253(13) 0.0298(13) 0.0103(11) 0.0117(11) 0.0145(12) C12' 0.0502(16) 0.0297(15) 0.0396(17) 0.0039(13) 0.0110(14) 0.0188(13) C13' 0.0435(16) 0.0438(17) 0.0361(15) 0.0201(13) 0.0204(13) 0.0276(14) C14' 0.071(2) 0.082(3) 0.064(2) 0.055(2) 0.040(2) 0.049(2) C15' 0.0427(16) 0.0407(16) 0.0302(15) 0.0101(12) 0.0158(13) 0.0261(14) C16' 0.0551(19) 0.052(2) 0.0347(17) -0.0029(14) 0.0118(15) 0.0268(17) C17' 0.0321(13) 0.0326(14) 0.0263(13) 0.0114(11) 0.0129(11) 0.0166(12) C18' 0.0299(11) 0.0276(11) 0.0260(11) 0.0080(9) 0.0130(10) 0.0125(10) C19' 0.0406(14) 0.0364(14) 0.0428(14) 0.0132(11) 0.0252(12) 0.0128(12) C20' 0.0466(15) 0.0375(14) 0.0439(15) 0.0120(12) 0.0233(13) 0.0043(12) C21' 0.0496(16) 0.0245(12) 0.0346(13) 0.0083(10) 0.0163(12) 0.0129(11) C22' 0.0380(14) 0.0351(15) 0.0338(15) 0.0060(12) 0.0113(12) 0.0116(12) C23' 0.0270(12) 0.0336(14) 0.0264(13) 0.0103(11) 0.0085(10) 0.0110(11) C24' 0.0420(13) 0.0290(12) 0.0299(12) 0.0098(10) 0.0117(11) 0.0173(11) C25' 0.069(2) 0.0321(15) 0.0387(16) 0.0144(12) 0.0116(14) 0.0195(15) C26' 0.0447(15) 0.0413(15) 0.0475(16) 0.0100(13) 0.0161(13) 0.0256(13) N1 0.099(3) 0.129(4) 0.128(4) 0.074(3) 0.043(3) 0.064(3) C27 0.063(2) 0.070(3) 0.066(3) 0.029(2) 0.015(2) 0.020(2) C28 0.071(3) 0.068(3) 0.065(3) 0.032(2) 0.018(2) 0.025(2) N2 0.112(4) 0.111(4) 0.107(3) 0.064(3) 0.058(3) 0.067(3) C29 0.087(3) 0.063(3) 0.060(2) 0.031(2) 0.027(2) 0.033(2) C30 0.093(3) 0.080(3) 0.066(3) 0.035(3) 0.029(3) 0.014(3) _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 O12 1.4251(19) . ? S1 O13 1.432(2) . ? S1 O4 1.5893(18) . ? S1 C17 1.772(3) . ? O1 C7 1.365(3) . ? O1 C1 1.432(3) . ? O2 C9 1.355(3) . ? O2 C2 1.438(3) . ? O3 C11 1.353(3) . ? O3 C3 1.448(3) . ? O4 C4 1.451(3) . ? O5 C13 1.357(3) . ? O5 C5 1.442(3) . ? O6 C15 1.354(3) . ? O6 C6 1.439(3) . ? O7 C7 1.194(3) . ? O8 C9 1.203(4) . ? O9 C11 1.195(3) . ? O10 C13 1.191(4) . ? O11 C15 1.196(4) . ? O14 C23 1.202(4) . ? C1 C6 1.514(4) . ? C1 C2 1.523(4) . ? C1 H1 0.9800 . ? C2 C3 1.531(4) . ? C2 H2 0.9800 . ? C3 C4 1.520(3) . ? C3 H3 0.9800 . ? C4 C5 1.523(3) . ? C4 H4 0.9800 . ? C5 C6 1.514(4) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.493(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.475(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.498(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.502(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.472(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.525(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.527(4) . ? C18 C24 1.558(3) . ? C18 C19 1.563(3) . ? C19 C20 1.539(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.536(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.543(4) . ? C21 C24 1.561(3) . ? C21 H21 0.9800 . ? C22 C23 1.521(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.528(4) . ? C24 C26 1.534(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O13' 1.416(2) . ? S1' O12' 1.425(2) . ? S1' O6' 1.5903(18) . ? S1' C17' 1.773(3) . ? O1' C7' 1.364(3) . ? O1' C1' 1.427(3) . ? O2' C9' 1.354(3) . ? O2' C2' 1.455(3) . ? O3' C11' 1.360(3) . ? O3' C3' 1.436(3) . ? O4' C15' 1.346(3) . ? O4' C4' 1.432(3) . ? O5' C13' 1.364(3) . ? O5' C5' 1.429(3) . ? O6' C6' 1.453(3) . ? O7' C7' 1.204(3) . ? O8' C9' 1.190(4) . ? O9' C11' 1.202(3) . ? O10' C13' 1.189(4) . ? O11' C15' 1.195(4) . ? O14' C23' 1.214(3) . ? C1' C6' 1.523(3) . ? C1' C2' 1.535(4) . ? C1' H1' 0.9800 . ? C2' C3' 1.517(3) . ? C2' H2' 0.9800 . ? C3' C4' 1.526(4) . ? C3' H3' 0.9800 . ? C4' C5' 1.524(4) . ? C4' H4' 0.9800 . ? C5' C6' 1.529(3) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.482(4) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.503(4) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C12' 1.489(4) . ? C12' H12F 0.9600 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C13' C14' 1.496(4) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.501(4) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.526(3) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.535(3) . ? C18' C24' 1.560(3) . ? C18' C19' 1.562(3) . ? C19' C20' 1.555(4) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.538(4) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.525(4) . ? C21' C24' 1.551(4) . ? C21' H21' 0.9800 . ? C22' C23' 1.504(4) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C26' 1.522(4) . ? C24' C25' 1.533(4) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? N1 C28 1.143(7) . ? C27 C28 1.434(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N2 C29 1.115(6) . ? C29 C30 1.419(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? 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 O12 S1 O13 119.27(12) . . ? O12 S1 O4 109.56(11) . . ? O13 S1 O4 102.85(10) . . ? O12 S1 C17 109.87(13) . . ? O13 S1 C17 111.08(12) . . ? O4 S1 C17 102.71(11) . . ? C7 O1 C1 117.4(2) . . ? C9 O2 C2 117.6(2) . . ? C11 O3 C3 115.1(2) . . ? C4 O4 S1 122.09(15) . . ? C13 O5 C5 117.5(2) . . ? C15 O6 C6 118.7(2) . . ? O1 C1 C6 107.9(2) . . ? O1 C1 C2 108.8(2) . . ? C6 C1 C2 111.1(2) . . ? O1 C1 H1 109.7 . . ? C6 C1 H1 109.7 . . ? C2 C1 H1 109.7 . . ? O2 C2 C1 107.3(2) . . ? O2 C2 C3 109.0(2) . . ? C1 C2 C3 109.0(2) . . ? O2 C2 H2 110.5 . . ? C1 C2 H2 110.5 . . ? C3 C2 H2 110.5 . . ? O3 C3 C4 106.1(2) . . ? O3 C3 C2 110.3(2) . . ? C4 C3 C2 111.1(2) . . ? O3 C3 H3 109.8 . . ? C4 C3 H3 109.8 . . ? C2 C3 H3 109.8 . . ? O4 C4 C3 108.4(2) . . ? O4 C4 C5 107.0(2) . . ? C3 C4 C5 109.6(2) . . ? O4 C4 H4 110.6 . . ? C3 C4 H4 110.6 . . ? C5 C4 H4 110.6 . . ? O5 C5 C6 109.08(19) . . ? O5 C5 C4 107.4(2) . . ? C6 C5 C4 111.3(2) . . ? O5 C5 H5 109.7 . . ? C6 C5 H5 109.7 . . ? C4 C5 H5 109.7 . . ? O6 C6 C5 107.1(2) . . ? O6 C6 C1 108.3(2) . . ? C5 C6 C1 111.4(2) . . ? O6 C6 H6 110.0 . . ? C5 C6 H6 110.0 . . ? C1 C6 H6 110.0 . . ? O7 C7 O1 123.8(3) . . ? O7 C7 C8 126.0(3) . . ? O1 C7 C8 110.2(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 123.7(3) . . ? O8 C9 C10 126.0(3) . . ? O2 C9 C10 110.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 124.0(3) . . ? O9 C11 C12 124.7(3) . . ? O3 C11 C12 111.3(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 124.1(3) . . ? O10 C13 C14 125.9(3) . . ? O5 C13 C14 110.0(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 123.0(3) . . ? O11 C15 C16 126.9(3) . . ? O6 C15 C16 110.1(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 117.52(18) . . ? C18 C17 H17A 107.9 . . ? S1 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? S1 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 C23 107.7(2) . . ? C17 C18 C24 125.0(2) . . ? C23 C18 C24 100.69(19) . . ? C17 C18 C19 115.26(19) . . ? C23 C18 C19 102.95(19) . . ? C24 C18 C19 102.32(19) . . ? C20 C19 C18 103.99(19) . . ? C20 C19 H19A 111.0 . . ? C18 C19 H19A 111.0 . . ? C20 C19 H19B 111.0 . . ? C18 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C21 C20 C19 103.1(2) . . ? C21 C20 H20A 111.1 . . ? C19 C20 H20A 111.1 . . ? C21 C20 H20B 111.1 . . ? C19 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? C20 C21 C22 107.2(2) . . ? C20 C21 C24 102.85(19) . . ? C22 C21 C24 102.7(2) . . ? C20 C21 H21 114.3 . . ? C22 C21 H21 114.3 . . ? C24 C21 H21 114.3 . . ? C23 C22 C21 101.0(2) . . ? C23 C22 H22A 111.6 . . ? C21 C22 H22A 111.6 . . ? C23 C22 H22B 111.6 . . ? C21 C22 H22B 111.6 . . ? H22A C22 H22B 109.4 . . ? O14 C23 C22 126.7(3) . . ? O14 C23 C18 126.2(3) . . ? C22 C23 C18 107.1(2) . . ? C25 C24 C26 108.8(2) . . ? C25 C24 C18 116.1(2) . . ? C26 C24 C18 112.6(2) . . ? C25 C24 C21 111.2(2) . . ? C26 C24 C21 114.4(2) . . ? C18 C24 C21 93.21(18) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O13' S1' O12' 120.26(14) . . ? O13' S1' O6' 102.65(11) . . ? O12' S1' O6' 110.04(11) . . ? O13' S1' C17' 109.95(13) . . ? O12' S1' C17' 110.16(13) . . ? O6' S1' C17' 102.02(11) . . ? C7' O1' C1' 115.65(19) . . ? C9' O2' C2' 117.6(2) . . ? C11' O3' C3' 117.4(2) . . ? C15' O4' C4' 118.3(2) . . ? C13' O5' C5' 117.43(19) . . ? C6' O6' S1' 121.62(14) . . ? O1' C1' C6' 106.63(19) . . ? O1' C1' C2' 110.3(2) . . ? C6' C1' C2' 110.5(2) . . ? O1' C1' H1' 109.8 . . ? C6' C1' H1' 109.8 . . ? C2' C1' H1' 109.8 . . ? O2' C2' C3' 107.41(19) . . ? O2' C2' C1' 108.87(19) . . ? C3' C2' C1' 109.5(2) . . ? O2' C2' H2' 110.3 . . ? C3' C2' H2' 110.3 . . ? C1' C2' H2' 110.3 . . ? O3' C3' C2' 109.2(2) . . ? O3' C3' C4' 107.9(2) . . ? C2' C3' C4' 111.4(2) . . ? O3' C3' H3' 109.4 . . ? C2' C3' H3' 109.4 . . ? C4' C3' H3' 109.4 . . ? O4' C4' C5' 107.7(2) . . ? O4' C4' C3' 108.2(2) . . ? C5' C4' C3' 110.4(2) . . ? O4' C4' H4' 110.1 . . ? C5' C4' H4' 110.1 . . ? C3' C4' H4' 110.1 . . ? O5' C5' C4' 108.6(2) . . ? O5' C5' C6' 107.85(19) . . ? C4' C5' C6' 110.7(2) . . ? O5' C5' H5' 109.9 . . ? C4' C5' H5' 109.9 . . ? C6' C5' H5' 109.9 . . ? O6' C6' C1' 107.89(19) . . ? O6' C6' C5' 107.25(19) . . ? C1' C6' C5' 110.6(2) . . ? O6' C6' H6' 110.4 . . ? C1' C6' H6' 110.4 . . ? C5' C6' H6' 110.4 . . ? O7' C7' O1' 122.1(2) . . ? O7' C7' C8' 126.9(2) . . ? O1' C7' C8' 111.1(2) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 124.2(2) . . ? O8' C9' C10' 125.7(3) . . ? O2' C9' C10' 110.1(3) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? O9' C11' O3' 123.4(3) . . ? O9' C11' C12' 126.1(3) . . ? O3' C11' C12' 110.5(2) . . ? C11' C12' H12F 109.5 . . ? C11' C12' H12D 109.5 . . ? H12F C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12F C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? O10' C13' O5' 123.8(3) . . ? O10' C13' C14' 125.9(3) . . ? O5' C13' C14' 110.3(3) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O4' 124.5(3) . . ? O11' C15' C16' 125.5(3) . . ? O4' C15' C16' 110.0(3) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 118.03(18) . . ? C18' C17' H17C 107.8 . . ? S1' C17' H17C 107.8 . . ? C18' C17' H17D 107.8 . . ? S1' C17' H17D 107.8 . . ? H17C C17' H17D 107.1 . . ? C17' C18' C23' 107.9(2) . . ? C17' C18' C24' 123.1(2) . . ? C23' C18' C24' 100.25(19) . . ? C17' C18' C19' 117.7(2) . . ? C23' C18' C19' 101.51(19) . . ? C24' C18' C19' 103.03(19) . . ? C20' C19' C18' 103.2(2) . . ? C20' C19' H19C 111.1 . . ? C18' C19' H19C 111.1 . . ? C20' C19' H19D 111.1 . . ? C18' C19' H19D 111.1 . . ? H19C C19' H19D 109.1 . . ? C21' C20' C19' 103.1(2) . . ? C21' C20' H20C 111.1 . . ? C19' C20' H20C 111.1 . . ? C21' C20' H20D 111.1 . . ? C19' C20' H20D 111.1 . . ? H20C C20' H20D 109.1 . . ? C22' C21' C20' 106.7(2) . . ? C22' C21' C24' 103.4(2) . . ? C20' C21' C24' 102.9(2) . . ? C22' C21' H21' 114.2 . . ? C20' C21' H21' 114.2 . . ? C24' C21' H21' 114.2 . . ? C23' C22' C21' 101.4(2) . . ? C23' C22' H22C 111.5 . . ? C21' C22' H22C 111.5 . . ? C23' C22' H22D 111.5 . . ? C21' C22' H22D 111.5 . . ? H22C C22' H22D 109.3 . . ? O14' C23' C22' 127.1(3) . . ? O14' C23' C18' 125.5(2) . . ? C22' C23' C18' 107.4(2) . . ? C26' C24' C25' 108.8(2) . . ? C26' C24' C21' 114.5(2) . . ? C25' C24' C21' 111.3(2) . . ? C26' C24' C18' 113.0(2) . . ? C25' C24' C18' 115.4(2) . . ? C21' C24' C18' 93.38(19) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 C27 178.1(6) . . ? N2 C29 C30 178.6(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.282 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.048 #===END data_1.2NM _database_code_depnum_ccdc_archive 'CCDC 846745' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.2NM ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 95 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT340_1.2NM ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0111 Ang. RESPONSE: This type alerts do occur in the crystal structure of inclusion complexes where atoms or the group of molecules show statistical disorder due to their proximity to the guest molecules. ; _vrf_PLAT413_1.2NM ; PROBLEM: Short Inter XH3 .. XHn H16A .. H27B .. 2.08 Ang. RESPONSE: This is due to H atoms attached to the disordered guest molecule. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULFONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, C H3 N O2, 0.25(H2 O)' _chemical_formula_sum 'C27 H39 N O16 S' _chemical_formula_weight 665.65 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' N N 0.0061 0.0033 '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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.401(4) _cell_length_b 12.587(4) _cell_length_c 13.250(4) _cell_angle_alpha 98.697(5) _cell_angle_beta 108.729(5) _cell_angle_gamma 117.919(4) _cell_volume 1614.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8994 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.3 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8892 _exptl_absorpt_correction_T_max 0.9777 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14464 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10685 _reflns_number_gt 10051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.1074P)^2^+3.4485P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(13) _refine_ls_number_reflns 10685 _refine_ls_number_parameters 816 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2352 _refine_ls_wR_factor_gt 0.2324 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.004 _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 0.74139(13) 0.27060(12) 0.23896(11) 0.0193(3) Uani 1 1 d . . . O1 O 0.8483(4) 0.8697(4) 0.3584(4) 0.0222(9) Uani 1 1 d . . . O2 O 0.6435(4) 0.6229(4) 0.2128(4) 0.0258(10) Uani 1 1 d . . . O3 O 0.6978(4) 0.4739(4) 0.0801(4) 0.0204(9) Uani 1 1 d . . . O4 O 0.8339(4) 0.4176(4) 0.2526(4) 0.0209(9) Uani 1 1 d . . . O5 O 0.8877(5) 0.5431(4) 0.4762(4) 0.0255(10) Uani 1 1 d . . . O6 O 0.9916(5) 0.8113(5) 0.5298(4) 0.0259(10) Uani 1 1 d . . . O7 O 1.0656(5) 1.0357(5) 0.4160(5) 0.0357(12) Uani 1 1 d . . . O8 O 0.5446(5) 0.6022(5) 0.0285(5) 0.0358(12) Uani 1 1 d . . . O9 O 0.8048(5) 0.5999(5) -0.0045(4) 0.0333(11) Uani 1 1 d . . . O10 O 1.1130(5) 0.6248(5) 0.5611(5) 0.0393(13) Uani 1 1 d . . . O11 O 0.8503(6) 0.7965(7) 0.6069(5) 0.0524(17) Uani 1 1 d . . . O12 O 0.6673(5) 0.2587(4) 0.3040(4) 0.0275(10) Uani 1 1 d . . . O13 O 0.8349(4) 0.2313(4) 0.2642(4) 0.0233(9) Uani 1 1 d . . . O14 O 0.4325(5) 0.0748(5) -0.1343(5) 0.0362(12) Uani 1 1 d . . . C1 C 0.8806(6) 0.7778(6) 0.3329(6) 0.0207(13) Uani 1 1 d . . . H1 H 0.9712 0.8216 0.3351 0.025 Uiso 1 1 calc R . . C2 C 0.7746(6) 0.6780(6) 0.2131(5) 0.0184(12) Uani 1 1 d . . . H2 H 0.7779 0.7191 0.1559 0.022 Uiso 1 1 calc R . . C3 C 0.8025(6) 0.5732(6) 0.1888(6) 0.0229(13) Uani 1 1 d . . . H3 H 0.8919 0.6105 0.1890 0.027 Uiso 1 1 calc R . . C4 C 0.7968(7) 0.5063(6) 0.2757(6) 0.0223(13) Uani 1 1 d . . . H4 H 0.7051 0.4616 0.2711 0.027 Uiso 1 1 calc R . . C5 C 0.9018(7) 0.6070(6) 0.3948(6) 0.0224(13) Uani 1 1 d . . . H5 H 0.9936 0.6421 0.4005 0.027 Uiso 1 1 calc R . . C6 C 0.8829(6) 0.7176(6) 0.4236(5) 0.0192(12) Uani 1 1 d . . . H6 H 0.7967 0.6845 0.4287 0.023 Uiso 1 1 calc R . . C7 C 0.9513(7) 0.9967(7) 0.4041(6) 0.0241(14) Uani 1 1 d . . . C8 C 0.9029(8) 1.0787(7) 0.4366(7) 0.0368(17) Uani 1 1 d . . . H8A H 0.9773 1.1556 0.5007 0.055 Uiso 1 1 calc R . . H8B H 0.8310 1.0318 0.4567 0.055 Uiso 1 1 calc R . . H8C H 0.8691 1.1015 0.3733 0.055 Uiso 1 1 calc R . . C9 C 0.5362(7) 0.5913(6) 0.1174(6) 0.0268(15) Uani 1 1 d . . . C10 C 0.4108(8) 0.5454(8) 0.1316(8) 0.0410(19) Uani 1 1 d . . . H10B H 0.3948 0.6131 0.1414 0.061 Uiso 1 1 calc R . . H10A H 0.4209 0.5211 0.1977 0.061 Uiso 1 1 calc R . . H10C H 0.3348 0.4722 0.0651 0.061 Uiso 1 1 calc R . . C11 C 0.7116(7) 0.4989(7) -0.0129(6) 0.0293(15) Uani 1 1 d . . . C12 C 0.6008(7) 0.3901(7) -0.1215(6) 0.0332(16) Uani 1 1 d . . . H12A H 0.5403 0.4132 -0.1616 0.050 Uiso 1 1 calc R . . H12B H 0.5506 0.3153 -0.1051 0.050 Uiso 1 1 calc R . . H12C H 0.6397 0.3717 -0.1681 0.050 Uiso 1 1 calc R . . C13 C 1.0000(7) 0.5552(6) 0.5507(5) 0.0231(13) Uani 1 1 d . . . C14 C 0.9645(9) 0.4722(9) 0.6208(8) 0.043(2) Uani 1 1 d . . . H14A H 1.0254 0.4438 0.6406 0.065 Uiso 1 1 calc R . . H14B H 0.8722 0.3987 0.5772 0.065 Uiso 1 1 calc R . . H14C H 0.9732 0.5213 0.6893 0.065 Uiso 1 1 calc R . . C15 C 0.9658(8) 0.8451(7) 0.6155(6) 0.0326(16) Uani 1 1 d . . . C16 C 1.0946(9) 0.9512(9) 0.7197(7) 0.046(2) Uani 1 1 d . . . H16A H 1.1044 1.0322 0.7232 0.069 Uiso 1 1 calc R . . H16B H 1.1718 0.9545 0.7152 0.069 Uiso 1 1 calc R . . H16C H 1.0898 0.9347 0.7870 0.069 Uiso 1 1 calc R . . C17 C 0.6276(6) 0.1975(6) 0.0899(6) 0.0228(13) Uani 1 1 d . . . H17A H 0.5562 0.2137 0.0780 0.027 Uiso 1 1 calc R . . H17B H 0.6778 0.2409 0.0502 0.027 Uiso 1 1 calc R . . C18 C 0.5591(5) 0.0520(5) 0.0331(5) 0.0198(11) Uani 1 1 d . . . C19 C 0.6548(6) 0.0151(6) 0.0097(5) 0.0249(12) Uani 1 1 d . . . H19A H 0.6755 0.0423 -0.0501 0.030 Uiso 1 1 calc R . . H19B H 0.7395 0.0536 0.0783 0.030 Uiso 1 1 calc R . . C20 C 0.5705(6) -0.1332(6) -0.0283(5) 0.0303(13) Uani 1 1 d . . . H20A H 0.5557 -0.1730 -0.1043 0.036 Uiso 1 1 calc R . . H20B H 0.6154 -0.1616 0.0246 0.036 Uiso 1 1 calc R . . C21 C 0.4351(6) -0.1649(6) -0.0269(5) 0.0266(13) Uani 1 1 d . . . H21 H 0.3806 -0.2505 -0.0246 0.032 Uiso 1 1 calc R . . C22 C 0.3616(7) -0.1409(6) -0.1249(6) 0.0298(15) Uani 1 1 d . . . H22A H 0.2687 -0.1734 -0.1370 0.036 Uiso 1 1 calc R . . H22B H 0.3598 -0.1807 -0.1947 0.036 Uiso 1 1 calc R . . C23 C 0.4467(7) 0.0059(6) -0.0868(5) 0.0218(13) Uani 1 1 d . . . C24 C 0.4822(6) -0.0514(5) 0.0785(5) 0.0242(12) Uani 1 1 d . . . C25 C 0.5680(7) -0.0538(6) 0.1881(6) 0.0286(14) Uani 1 1 d . . . H25A H 0.5901 0.0130 0.2522 0.043 Uiso 1 1 calc R . . H25B H 0.6507 -0.0400 0.1873 0.043 Uiso 1 1 calc R . . H25C H 0.5177 -0.1361 0.1943 0.043 Uiso 1 1 calc R . . C26 C 0.3645(7) -0.0493(7) 0.0906(7) 0.0420(17) Uani 1 1 d . . . H26A H 0.3049 -0.1287 0.0965 0.063 Uiso 1 1 calc R . . H26B H 0.3143 -0.0392 0.0248 0.063 Uiso 1 1 calc R . . H26C H 0.4004 0.0215 0.1580 0.063 Uiso 1 1 calc R . . S1' S 0.24889(14) 0.72771(13) 0.34221(12) 0.0216(3) Uani 1 1 d . . . O1' O 0.2831(5) 0.5172(4) 0.4998(4) 0.0251(10) Uani 1 1 d . . . O2' O 0.3378(4) 0.3690(4) 0.3648(4) 0.0223(9) Uani 1 1 d . . . O3' O 0.1270(4) 0.1211(4) 0.2133(4) 0.0236(9) Uani 1 1 d . . . O4' O -0.0061(4) 0.1871(4) 0.0446(4) 0.0243(10) Uani 1 1 d . . . O5' O 0.1029(4) 0.4594(4) 0.1067(4) 0.0249(10) Uani 1 1 d . . . O6' O 0.1532(4) 0.5816(4) 0.3288(4) 0.0250(10) Uani 1 1 d . . . O7' O 0.1697(5) 0.3898(5) 0.5802(4) 0.0318(11) Uani 1 1 d . . . O8' O 0.4310(5) 0.3804(5) 0.5471(5) 0.0365(12) Uani 1 1 d . . . O9' O -0.0932(5) -0.0385(4) 0.1516(5) 0.0344(12) Uani 1 1 d . . . O10' O 0.1389(6) 0.1939(7) -0.0253(5) 0.0522(16) Uani 1 1 d . . . O11' O -0.1221(5) 0.3822(6) 0.0173(5) 0.0392(13) Uani 1 1 d . . . O12' O 0.3270(5) 0.7354(5) 0.2805(5) 0.0329(11) Uani 1 1 d . . . O13' O 0.1556(5) 0.7653(5) 0.3108(5) 0.0361(12) Uani 1 1 d . . . O14' O 0.5520(5) 0.9130(5) 0.7187(4) 0.0339(12) Uani 1 1 d . . . C1' C 0.1820(6) 0.4208(6) 0.3902(5) 0.0198(12) Uani 1 1 d . . . H1' H 0.0920 0.3848 0.3886 0.024 Uiso 1 1 calc R . . C2' C 0.2023(6) 0.3112(7) 0.3614(7) 0.0268(15) Uani 1 1 d . . . H2' H 0.1961 0.2674 0.4164 0.032 Uiso 1 1 calc R . . C3' C 0.0988(6) 0.2172(6) 0.2416(6) 0.0223(13) Uani 1 1 d . . . H3' H 0.0070 0.1755 0.2369 0.027 Uiso 1 1 calc R . . C4' C 0.1061(6) 0.2852(6) 0.1551(6) 0.0244(14) Uani 1 1 d . . . H4' H 0.1940 0.3193 0.1528 0.029 Uiso 1 1 calc R . . C5' C 0.0834(6) 0.3917(6) 0.1828(5) 0.0207(13) Uani 1 1 d . . . H5' H -0.0091 0.3556 0.1757 0.025 Uiso 1 1 calc R . . C6' C 0.1882(6) 0.4861(6) 0.3033(6) 0.0205(13) Uani 1 1 d . . . H6' H 0.2800 0.5295 0.3082 0.025 Uiso 1 1 calc R . . C7' C 0.2654(7) 0.4898(6) 0.5913(6) 0.0237(14) Uani 1 1 d . . . C8' C 0.3768(8) 0.5959(7) 0.7009(7) 0.0355(16) Uani 1 1 d . . . H8D H 0.3491 0.5853 0.7605 0.053 Uiso 1 1 calc R . . H8E H 0.3962 0.6770 0.6940 0.053 Uiso 1 1 calc R . . H8F H 0.4573 0.5942 0.7193 0.053 Uiso 1 1 calc R . . C9' C 0.4416(7) 0.3948(7) 0.4643(6) 0.0281(15) Uani 1 1 d . . . C10' C 0.5710(7) 0.4476(9) 0.4492(8) 0.042(2) Uani 1 1 d . . . H10D H 0.6449 0.4668 0.5181 0.064 Uiso 1 1 calc R . . H10E H 0.5925 0.5248 0.4327 0.064 Uiso 1 1 calc R . . H10F H 0.5573 0.3846 0.3871 0.064 Uiso 1 1 calc R . . C11' C 0.0187(7) -0.0053(6) 0.1651(6) 0.0245(14) Uani 1 1 d . . . C12' C 0.0658(8) -0.0891(7) 0.1334(7) 0.0345(16) Uani 1 1 d . . . H12D H 0.1530 -0.0591 0.1936 0.052 Uiso 1 1 calc R . . H12E H 0.0738 -0.0857 0.0641 0.052 Uiso 1 1 calc R . . H12F H 0.0008 -0.1763 0.1222 0.052 Uiso 1 1 calc R . . C13' C 0.0235(7) 0.1450(7) -0.0357(7) 0.0319(16) Uani 1 1 d . . . C14' C -0.1017(9) 0.0382(9) -0.1364(8) 0.047(2) Uani 1 1 d . . . H14D H -0.1553 0.0693 -0.1728 0.070 Uiso 1 1 calc R . . H14E H -0.1537 -0.0286 -0.1129 0.070 Uiso 1 1 calc R . . H14F H -0.0776 0.0044 -0.1892 0.070 Uiso 1 1 calc R . . C15' C -0.0093(7) 0.4511(7) 0.0300(6) 0.0306(16) Uani 1 1 d . . . C16' C 0.0351(9) 0.5407(9) -0.0308(8) 0.043(2) Uani 1 1 d . . . H16D H -0.0376 0.5071 -0.1059 0.064 Uiso 1 1 calc R . . H16E H 0.1138 0.5494 -0.0367 0.064 Uiso 1 1 calc R . . H16F H 0.0579 0.6235 0.0110 0.064 Uiso 1 1 calc R . . C17' C 0.3572(7) 0.8027(7) 0.4915(6) 0.0285(15) Uani 1 1 d . . . H17C H 0.3010 0.7966 0.5300 0.034 Uiso 1 1 calc R . . H17D H 0.3956 0.7534 0.5138 0.034 Uiso 1 1 calc R . . C18' C 0.4761(6) 0.9453(6) 0.5366(5) 0.0230(12) Uani 1 1 d . . . C19' C 0.5903(6) 0.9775(6) 0.4974(6) 0.0320(14) Uani 1 1 d . . . H19C H 0.5516 0.9408 0.4149 0.038 Uiso 1 1 calc R . . H19D H 0.6449 0.9455 0.5317 0.038 Uiso 1 1 calc R . . C20' C 0.6770(7) 1.1281(7) 0.5413(6) 0.0378(15) Uani 1 1 d . . . H20C H 0.7718 1.1635 0.5918 0.045 Uiso 1 1 calc R . . H20D H 0.6726 1.1590 0.4783 0.045 Uiso 1 1 calc R . . C21' C 0.6072(7) 1.1627(6) 0.6064(6) 0.0295(14) Uani 1 1 d . . . H21' H 0.6291 1.2508 0.6203 0.035 Uiso 1 1 calc R . . C22' C 0.6417(8) 1.1307(7) 0.7161(5) 0.0295(15) Uani 1 1 d . . . H22C H 0.7382 1.1647 0.7559 0.035 Uiso 1 1 calc R . . H22D H 0.6144 1.1631 0.7677 0.035 Uiso 1 1 calc R . . C23' C 0.5556(7) 0.9841(7) 0.6656(6) 0.0285(15) Uani 1 1 d . . . C24' C 0.4528(6) 1.0560(6) 0.5314(5) 0.0268(12) Uani 1 1 d . . . C25' C 0.4013(8) 1.0646(7) 0.4124(6) 0.0373(17) Uani 1 1 d . . . H25D H 0.3053 0.9998 0.3687 0.056 Uiso 1 1 calc R . . H25E H 0.4497 1.0510 0.3736 0.056 Uiso 1 1 calc R . . H25F H 0.4167 1.1483 0.4206 0.056 Uiso 1 1 calc R . . C26' C 0.3590(7) 1.0555(7) 0.5811(6) 0.0333(14) Uani 1 1 d . . . H26D H 0.3653 1.1357 0.5918 0.050 Uiso 1 1 calc R . . H26E H 0.3853 1.0447 0.6534 0.050 Uiso 1 1 calc R . . H26F H 0.2668 0.9857 0.5298 0.050 Uiso 1 1 calc R . . N1 N 0.1226(16) 0.2888(17) 0.7772(12) 0.036(3) Uiso 0.50 1 d P A 1 O15 O 0.097(2) 0.3604(19) 0.8262(16) 0.088(5) Uiso 0.50 1 d P A 1 O16 O 0.0221(15) 0.1763(16) 0.7061(13) 0.064(4) Uiso 0.50 1 d P A 1 C27 C 0.254(3) 0.302(3) 0.789(3) 0.069(10) Uiso 0.50 1 d P A 1 H27A H 0.2623 0.3062 0.7200 0.104 Uiso 0.50 1 calc PR A 1 H27B H 0.2528 0.2289 0.8027 0.104 Uiso 0.50 1 calc PR A 1 H27C H 0.3297 0.3794 0.8520 0.104 Uiso 0.50 1 calc PR A 1 N1' N 0.142(2) 0.337(2) 0.7923(17) 0.058(5) Uiso 0.50 1 d P B 2 O15' O 0.1639(15) 0.4264(14) 0.8368(12) 0.055(3) Uiso 0.50 1 d P B 2 O16' O 0.0317(18) 0.2285(18) 0.7324(14) 0.062(4) Uiso 0.50 1 d P B 2 C27' C 0.2613(18) 0.3249(19) 0.8104(17) 0.028(4) Uiso 0.50 1 d P B 2 H27D H 0.3444 0.4049 0.8637 0.042 Uiso 0.50 1 calc PR B 2 H27E H 0.2641 0.3044 0.7389 0.042 Uiso 0.50 1 calc PR B 2 H27F H 0.2514 0.2576 0.8401 0.042 Uiso 0.50 1 calc PR B 2 N2 N 0.8403(9) 0.6690(8) 0.7933(7) 0.054(2) Uiso 1 1 d . . . O18 O 0.7927(14) 0.5367(14) 0.7385(11) 0.051(3) Uiso 0.50 1 d P C 1 O17 O 0.9569(15) 0.7398(15) 0.8452(12) 0.058(4) Uiso 0.50 1 d P C 1 O17' O 0.9538(11) 0.7811(12) 0.8629(10) 0.037(3) Uiso 0.50 1 d P C 2 O18' O 0.8405(15) 0.5894(15) 0.7453(12) 0.051(3) Uiso 0.50 1 d P C 2 C28 C 0.7243(11) 0.6767(11) 0.7752(9) 0.059(3) Uiso 1 1 d . C . H28A H 0.7173 0.7234 0.7250 0.088 Uiso 1 1 calc R . . H28B H 0.7349 0.7206 0.8470 0.088 Uiso 1 1 calc R . . H28C H 0.6430 0.5914 0.7413 0.088 Uiso 1 1 calc R . . O1W O 0.4095(19) 0.2732(18) 0.1432(16) 0.038(4) Uiso 0.25 1 d P . . 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 0.0187(7) 0.0170(7) 0.0190(7) 0.0066(6) 0.0090(6) 0.0072(6) O1 0.018(2) 0.016(2) 0.030(2) 0.0057(18) 0.0126(19) 0.0072(18) O2 0.015(2) 0.020(2) 0.040(3) 0.009(2) 0.014(2) 0.0073(19) O3 0.017(2) 0.022(2) 0.018(2) 0.0069(17) 0.0079(17) 0.0076(18) O4 0.021(2) 0.016(2) 0.022(2) 0.0071(18) 0.0091(19) 0.0084(19) O5 0.028(2) 0.023(2) 0.033(3) 0.013(2) 0.019(2) 0.015(2) O6 0.026(2) 0.028(2) 0.020(2) 0.0033(19) 0.011(2) 0.014(2) O7 0.023(2) 0.026(2) 0.053(3) 0.017(2) 0.018(2) 0.009(2) O8 0.028(3) 0.036(3) 0.037(3) 0.014(2) 0.010(2) 0.017(2) O9 0.032(3) 0.025(3) 0.036(3) 0.009(2) 0.018(2) 0.010(2) O10 0.024(3) 0.047(3) 0.040(3) 0.022(3) 0.012(2) 0.014(2) O11 0.026(3) 0.073(4) 0.037(3) -0.001(3) 0.015(3) 0.018(3) O12 0.032(3) 0.020(2) 0.028(2) 0.0086(19) 0.021(2) 0.008(2) O13 0.024(2) 0.018(2) 0.027(2) 0.0086(18) 0.0108(19) 0.0101(19) O14 0.035(3) 0.036(3) 0.034(3) 0.019(2) 0.011(2) 0.017(2) C1 0.019(3) 0.016(3) 0.023(3) 0.007(2) 0.012(3) 0.006(2) C2 0.019(3) 0.016(3) 0.015(3) 0.003(2) 0.007(2) 0.006(2) C3 0.016(3) 0.021(3) 0.035(4) 0.017(3) 0.015(3) 0.008(3) C4 0.023(3) 0.022(3) 0.024(3) 0.010(3) 0.012(3) 0.012(3) C5 0.027(3) 0.021(3) 0.027(3) 0.012(3) 0.015(3) 0.016(3) C6 0.017(3) 0.016(3) 0.018(3) 0.003(2) 0.011(2) 0.004(2) C7 0.023(3) 0.026(3) 0.018(3) 0.013(3) 0.006(2) 0.011(3) C8 0.038(4) 0.028(4) 0.037(4) 0.003(3) 0.008(3) 0.020(3) C9 0.025(3) 0.019(3) 0.038(4) 0.011(3) 0.012(3) 0.014(3) C10 0.025(4) 0.041(5) 0.049(5) 0.013(4) 0.013(4) 0.017(4) C11 0.029(3) 0.035(4) 0.034(4) 0.015(3) 0.015(3) 0.024(3) C12 0.031(4) 0.031(4) 0.024(3) 0.003(3) 0.004(3) 0.014(3) C13 0.025(3) 0.027(3) 0.021(3) 0.007(3) 0.012(3) 0.017(3) C14 0.042(4) 0.063(5) 0.046(5) 0.038(4) 0.023(4) 0.036(4) C15 0.042(4) 0.035(4) 0.025(4) 0.013(3) 0.012(3) 0.026(4) C16 0.044(5) 0.053(5) 0.023(4) -0.006(3) 0.007(3) 0.025(4) C17 0.019(3) 0.016(3) 0.022(3) 0.005(3) 0.003(3) 0.006(3) C18 0.015(3) 0.016(3) 0.024(3) 0.007(2) 0.012(2) 0.004(2) C19 0.024(3) 0.020(3) 0.024(3) 0.003(2) 0.010(2) 0.009(2) C20 0.030(3) 0.018(3) 0.027(3) -0.002(2) 0.005(3) 0.010(3) C21 0.029(3) 0.017(3) 0.022(3) 0.003(2) 0.011(3) 0.006(2) C22 0.022(3) 0.018(3) 0.035(4) 0.002(3) 0.013(3) 0.003(3) C23 0.025(3) 0.026(3) 0.020(3) 0.013(3) 0.014(3) 0.014(3) C24 0.020(3) 0.022(3) 0.022(3) 0.009(2) 0.013(2) 0.004(2) C25 0.032(3) 0.020(3) 0.024(3) 0.006(2) 0.015(3) 0.007(3) C26 0.027(3) 0.033(4) 0.062(5) 0.019(4) 0.029(3) 0.008(3) S1' 0.0207(7) 0.0158(7) 0.0255(8) 0.0083(6) 0.0111(6) 0.0073(6) O1' 0.024(2) 0.015(2) 0.032(3) 0.0064(19) 0.012(2) 0.0086(18) O2' 0.016(2) 0.023(2) 0.020(2) 0.0044(18) 0.0071(18) 0.0070(19) O3' 0.019(2) 0.017(2) 0.029(2) 0.0078(18) 0.0089(19) 0.0079(18) O4' 0.019(2) 0.018(2) 0.025(2) 0.0024(18) 0.0087(19) 0.0051(18) O5' 0.020(2) 0.028(2) 0.025(2) 0.013(2) 0.0109(19) 0.011(2) O6' 0.020(2) 0.018(2) 0.040(3) 0.010(2) 0.019(2) 0.0101(19) O7' 0.036(3) 0.029(3) 0.030(3) 0.014(2) 0.020(2) 0.013(2) O8' 0.032(3) 0.041(3) 0.029(3) 0.014(2) 0.008(2) 0.018(2) O9' 0.019(2) 0.018(2) 0.050(3) 0.004(2) 0.009(2) 0.0050(19) O10' 0.036(3) 0.076(4) 0.034(3) 0.005(3) 0.018(3) 0.026(3) O11' 0.030(3) 0.051(3) 0.047(3) 0.029(3) 0.019(2) 0.024(3) O12' 0.033(3) 0.023(2) 0.040(3) 0.010(2) 0.023(2) 0.009(2) O13' 0.029(3) 0.028(3) 0.040(3) 0.014(2) 0.004(2) 0.015(2) O14' 0.034(3) 0.027(3) 0.029(3) 0.014(2) 0.007(2) 0.012(2) C1' 0.019(3) 0.019(3) 0.013(3) 0.001(2) 0.005(2) 0.007(2) C2' 0.014(3) 0.026(3) 0.045(4) 0.022(3) 0.016(3) 0.010(3) C3' 0.016(3) 0.011(3) 0.038(4) 0.007(3) 0.012(3) 0.006(2) C4' 0.014(3) 0.021(3) 0.029(4) 0.008(3) 0.004(3) 0.007(3) C5' 0.013(3) 0.020(3) 0.022(3) 0.009(3) 0.010(2) 0.002(2) C6' 0.021(3) 0.012(3) 0.035(4) 0.010(3) 0.017(3) 0.010(2) C7' 0.033(4) 0.017(3) 0.022(3) 0.006(3) 0.013(3) 0.014(3) C8' 0.045(4) 0.029(4) 0.029(4) 0.012(3) 0.017(3) 0.018(3) C9' 0.025(3) 0.026(3) 0.027(4) 0.007(3) 0.007(3) 0.013(3) C10' 0.016(3) 0.048(5) 0.052(5) 0.018(4) 0.012(3) 0.012(3) C11' 0.026(3) 0.010(3) 0.021(3) -0.001(2) 0.003(3) 0.006(3) C12' 0.032(4) 0.024(3) 0.039(4) 0.008(3) 0.011(3) 0.014(3) C13' 0.029(4) 0.031(4) 0.039(4) 0.012(3) 0.020(3) 0.017(3) C14' 0.037(4) 0.043(5) 0.049(5) 0.005(4) 0.017(4) 0.019(4) C15' 0.028(4) 0.032(4) 0.037(4) 0.018(3) 0.017(3) 0.017(3) C16' 0.048(5) 0.065(5) 0.047(5) 0.039(4) 0.035(4) 0.039(4) C17' 0.021(3) 0.029(4) 0.039(4) 0.021(3) 0.020(3) 0.009(3) C18' 0.019(3) 0.021(3) 0.027(3) 0.009(2) 0.015(2) 0.006(2) C19' 0.022(3) 0.026(3) 0.038(3) 0.008(3) 0.017(3) 0.004(3) C20' 0.025(3) 0.027(3) 0.044(4) 0.009(3) 0.018(3) 0.002(3) C21' 0.028(3) 0.019(3) 0.033(3) 0.009(2) 0.011(3) 0.009(3) C22' 0.037(4) 0.027(3) 0.012(3) 0.007(2) 0.004(3) 0.014(3) C23' 0.018(3) 0.024(3) 0.032(4) 0.004(3) 0.011(3) 0.006(3) C24' 0.025(3) 0.022(3) 0.024(3) 0.006(2) 0.008(3) 0.010(3) C25' 0.044(4) 0.026(3) 0.034(4) 0.012(3) 0.013(3) 0.017(3) C26' 0.029(3) 0.028(3) 0.038(4) 0.004(3) 0.014(3) 0.016(3) _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 O12 1.424(5) . ? S1 O13 1.429(5) . ? S1 O4 1.597(4) . ? S1 C17 1.784(6) . ? O1 C7 1.361(8) . ? O1 C1 1.420(8) . ? O2 C9 1.341(9) . ? O2 C2 1.436(7) . ? O3 C11 1.359(8) . ? O3 C3 1.435(8) . ? O4 C4 1.421(8) . ? O5 C13 1.345(8) . ? O5 C5 1.445(8) . ? O6 C15 1.338(9) . ? O6 C6 1.407(8) . ? O7 C7 1.206(9) . ? O8 C9 1.237(9) . ? O9 C11 1.209(9) . ? O10 C13 1.201(9) . ? O11 C15 1.221(10) . ? O14 C23 1.190(8) . ? C1 C6 1.515(9) . ? C1 C2 1.529(9) . ? C1 H1 0.9800 . ? C2 C3 1.528(9) . ? C2 H2 0.9800 . ? C3 C4 1.526(9) . ? C3 H3 0.9800 . ? C4 C5 1.524(9) . ? C4 H4 0.9800 . ? C5 C6 1.531(9) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.491(10) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.474(11) . ? C10 H10B 0.9600 . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.486(10) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.507(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.507(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.536(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.531(8) . ? C18 C24 1.552(7) . ? C18 C19 1.558(8) . ? C19 C20 1.542(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.540(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.492(10) . ? C21 C24 1.557(8) . ? C21 H21 0.9800 . ? C22 C23 1.527(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.515(9) . ? C24 C26 1.531(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O13' 1.413(5) . ? S1' O12' 1.436(5) . ? S1' O6' 1.595(5) . ? S1' C17' 1.775(8) . ? O1' C7' 1.365(8) . ? O1' C1' 1.423(7) . ? O2' C9' 1.374(8) . ? O2' C2' 1.467(7) . ? O3' C11' 1.373(8) . ? O3' C3' 1.438(7) . ? O4' C13' 1.345(9) . ? O4' C4' 1.464(8) . ? O5' C15' 1.379(8) . ? O5' C5' 1.422(8) . ? O6' C6' 1.485(7) . ? O7' C7' 1.203(8) . ? O8' C9' 1.176(9) . ? O9' C11' 1.187(9) . ? O10' C13' 1.212(9) . ? O11' C15' 1.186(9) . ? O14' C23' 1.212(9) . ? C1' C6' 1.513(9) . ? C1' C2' 1.530(9) . ? C1' H1' 0.9800 . ? C2' C3' 1.506(10) . ? C2' H2' 0.9800 . ? C3' C4' 1.532(9) . ? C3' H3' 0.9800 . ? C4' C5' 1.511(9) . ? C4' H4' 0.9800 . ? C5' C6' 1.516(9) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.483(10) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.518(10) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C12' 1.493(10) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.473(11) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.484(11) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.544(9) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.532(9) . ? C18' C24' 1.557(8) . ? C18' C19' 1.562(8) . ? C19' C20' 1.563(9) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.551(9) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.548(9) . ? C21' C24' 1.557(8) . ? C21' H21' 0.9800 . ? C22' C23' 1.521(10) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C26' 1.506(9) . ? C24' C25' 1.542(9) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? N1 O15 1.25(2) . ? N1 O16 1.28(2) . ? N1 C27 1.51(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1' O15' 1.05(3) . ? N1' O16' 1.26(3) . ? N1' C27' 1.51(3) . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? N2 O18' 1.105(15) . ? N2 O17 1.152(16) . ? N2 O17' 1.317(15) . ? N2 C28 1.433(13) . ? N2 O18 1.445(16) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 O12 S1 O13 119.0(3) . . ? O12 S1 O4 110.6(3) . . ? O13 S1 O4 103.6(2) . . ? O12 S1 C17 110.2(3) . . ? O13 S1 C17 110.3(3) . . ? O4 S1 C17 101.6(3) . . ? C7 O1 C1 117.8(5) . . ? C9 O2 C2 118.3(5) . . ? C11 O3 C3 115.9(5) . . ? C4 O4 S1 121.6(4) . . ? C13 O5 C5 117.7(5) . . ? C15 O6 C6 119.9(5) . . ? O1 C1 C6 107.9(5) . . ? O1 C1 C2 109.0(5) . . ? C6 C1 C2 112.2(5) . . ? O1 C1 H1 109.3 . . ? C6 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? O2 C2 C3 109.7(5) . . ? O2 C2 C1 106.8(5) . . ? C3 C2 C1 109.1(5) . . ? O2 C2 H2 110.4 . . ? C3 C2 H2 110.4 . . ? C1 C2 H2 110.4 . . ? O3 C3 C4 105.5(5) . . ? O3 C3 C2 109.7(5) . . ? C4 C3 C2 111.7(5) . . ? O3 C3 H3 109.9 . . ? C4 C3 H3 109.9 . . ? C2 C3 H3 109.9 . . ? O4 C4 C5 108.1(5) . . ? O4 C4 C3 108.2(5) . . ? C5 C4 C3 108.8(5) . . ? O4 C4 H4 110.6 . . ? C5 C4 H4 110.6 . . ? C3 C4 H4 110.6 . . ? O5 C5 C4 107.8(5) . . ? O5 C5 C6 109.0(5) . . ? C4 C5 C6 112.8(5) . . ? O5 C5 H5 109.1 . . ? C4 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? O6 C6 C1 109.5(5) . . ? O6 C6 C5 108.7(5) . . ? C1 C6 C5 110.9(5) . . ? O6 C6 H6 109.2 . . ? C1 C6 H6 109.2 . . ? C5 C6 H6 109.2 . . ? O7 C7 O1 123.8(6) . . ? O7 C7 C8 125.5(7) . . ? O1 C7 C8 110.7(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 122.7(6) . . ? O8 C9 C10 124.7(7) . . ? O2 C9 C10 112.7(7) . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? C9 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? O9 C11 O3 122.0(7) . . ? O9 C11 C12 125.7(7) . . ? O3 C11 C12 112.4(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 124.3(6) . . ? O10 C13 C14 125.0(7) . . ? O5 C13 C14 110.7(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 122.8(7) . . ? O11 C15 C16 125.4(7) . . ? O6 C15 C16 111.8(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 117.5(4) . . ? C18 C17 H17A 107.9 . . ? S1 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? S1 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C23 C18 C17 108.3(5) . . ? C23 C18 C24 101.1(4) . . ? C17 C18 C24 124.7(5) . . ? C23 C18 C19 103.3(4) . . ? C17 C18 C19 114.0(5) . . ? C24 C18 C19 103.0(5) . . ? C20 C19 C18 103.4(5) . . ? C20 C19 H19A 111.1 . . ? C18 C19 H19A 111.1 . . ? C20 C19 H19B 111.1 . . ? C18 C19 H19B 111.1 . . ? H19A C19 H19B 109.1 . . ? C21 C20 C19 103.1(5) . . ? C21 C20 H20A 111.1 . . ? C19 C20 H20A 111.1 . . ? C21 C20 H20B 111.1 . . ? C19 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? C22 C21 C20 107.2(5) . . ? C22 C21 C24 102.9(5) . . ? C20 C21 C24 102.9(5) . . ? C22 C21 H21 114.2 . . ? C20 C21 H21 114.2 . . ? C24 C21 H21 114.2 . . ? C21 C22 C23 102.9(5) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? O14 C23 C22 130.2(7) . . ? O14 C23 C18 124.9(6) . . ? C22 C23 C18 104.9(5) . . ? C25 C24 C26 108.5(5) . . ? C25 C24 C18 116.8(5) . . ? C26 C24 C18 113.3(5) . . ? C25 C24 C21 111.0(5) . . ? C26 C24 C21 113.9(5) . . ? C18 C24 C21 92.9(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O13' S1' O12' 119.7(3) . . ? O13' S1' O6' 102.4(3) . . ? O12' S1' O6' 109.8(3) . . ? O13' S1' C17' 110.6(3) . . ? O12' S1' C17' 110.4(3) . . ? O6' S1' C17' 102.1(3) . . ? C7' O1' C1' 116.3(5) . . ? C9' O2' C2' 116.1(5) . . ? C11' O3' C3' 117.0(5) . . ? C13' O4' C4' 118.9(5) . . ? C15' O5' C5' 117.6(5) . . ? C6' O6' S1' 121.3(4) . . ? O1' C1' C6' 107.4(5) . . ? O1' C1' C2' 112.6(5) . . ? C6' C1' C2' 110.5(5) . . ? O1' C1' H1' 108.7 . . ? C6' C1' H1' 108.7 . . ? C2' C1' H1' 108.7 . . ? O2' C2' C3' 107.5(6) . . ? O2' C2' C1' 107.0(5) . . ? C3' C2' C1' 110.3(5) . . ? O2' C2' H2' 110.6 . . ? C3' C2' H2' 110.6 . . ? C1' C2' H2' 110.6 . . ? O3' C3' C2' 109.2(5) . . ? O3' C3' C4' 108.1(5) . . ? C2' C3' C4' 111.0(5) . . ? O3' C3' H3' 109.5 . . ? C2' C3' H3' 109.5 . . ? C4' C3' H3' 109.5 . . ? O4' C4' C5' 108.3(5) . . ? O4' C4' C3' 105.8(5) . . ? C5' C4' C3' 111.0(5) . . ? O4' C4' H4' 110.5 . . ? C5' C4' H4' 110.5 . . ? C3' C4' H4' 110.5 . . ? O5' C5' C4' 109.1(5) . . ? O5' C5' C6' 107.9(5) . . ? C4' C5' C6' 109.2(5) . . ? O5' C5' H5' 110.2 . . ? C4' C5' H5' 110.2 . . ? C6' C5' H5' 110.2 . . ? O6' C6' C1' 107.9(5) . . ? O6' C6' C5' 106.6(5) . . ? C1' C6' C5' 111.9(5) . . ? O6' C6' H6' 110.1 . . ? C1' C6' H6' 110.1 . . ? C5' C6' H6' 110.1 . . ? O7' C7' O1' 122.0(6) . . ? O7' C7' C8' 126.2(6) . . ? O1' C7' C8' 111.8(6) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 125.2(6) . . ? O8' C9' C10' 126.6(7) . . ? O2' C9' C10' 108.2(6) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? O9' C11' O3' 123.6(6) . . ? O9' C11' C12' 127.3(6) . . ? O3' C11' C12' 109.1(6) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O10' C13' O4' 122.9(7) . . ? O10' C13' C14' 126.0(7) . . ? O4' C13' C14' 111.1(6) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O5' 123.7(7) . . ? O11' C15' C16' 127.0(7) . . ? O5' C15' C16' 109.3(6) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 117.4(5) . . ? C18' C17' H17C 108.0 . . ? S1' C17' H17C 108.0 . . ? C18' C17' H17D 108.0 . . ? S1' C17' H17D 108.0 . . ? H17C C17' H17D 107.2 . . ? C23' C18' C17' 106.7(5) . . ? C23' C18' C24' 101.5(5) . . ? C17' C18' C24' 122.6(5) . . ? C23' C18' C19' 101.7(5) . . ? C17' C18' C19' 117.5(5) . . ? C24' C18' C19' 103.8(5) . . ? C18' C19' C20' 103.2(5) . . ? C18' C19' H19C 111.1 . . ? C20' C19' H19C 111.1 . . ? C18' C19' H19D 111.1 . . ? C20' C19' H19D 111.1 . . ? H19C C19' H19D 109.1 . . ? C21' C20' C19' 102.5(5) . . ? C21' C20' H20C 111.3 . . ? C19' C20' H20C 111.3 . . ? C21' C20' H20D 111.3 . . ? C19' C20' H20D 111.3 . . ? H20C C20' H20D 109.2 . . ? C22' C21' C20' 106.9(6) . . ? C22' C21' C24' 103.2(5) . . ? C20' C21' C24' 103.3(5) . . ? C22' C21' H21' 114.1 . . ? C20' C21' H21' 114.1 . . ? C24' C21' H21' 114.1 . . ? C23' C22' C21' 100.7(5) . . ? C23' C22' H22C 111.6 . . ? C21' C22' H22C 111.6 . . ? C23' C22' H22D 111.6 . . ? C21' C22' H22D 111.6 . . ? H22C C22' H22D 109.4 . . ? O14' C23' C22' 125.8(7) . . ? O14' C23' C18' 127.3(6) . . ? C22' C23' C18' 106.9(6) . . ? C26' C24' C25' 107.7(5) . . ? C26' C24' C18' 113.5(5) . . ? C25' C24' C18' 115.9(5) . . ? C26' C24' C21' 115.5(5) . . ? C25' C24' C21' 111.1(5) . . ? C18' C24' C21' 92.8(5) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? O15 N1 O16 117.8(18) . . ? O15 N1 C27 133(2) . . ? O16 N1 C27 108.8(18) . . ? O15' N1' O16' 133(2) . . ? O15' N1' C27' 117(2) . . ? O16' N1' C27' 110(2) . . ? N1' C27' H27D 109.5 . . ? N1' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? N1' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? O18' N2 O17 97.4(13) . . ? O18' N2 O17' 122.2(12) . . ? O17 N2 O17' 25.1(8) . . ? O18' N2 C28 126.6(11) . . ? O17 N2 C28 135.3(12) . . ? O17' N2 C28 110.2(9) . . ? O18' N2 O18 23.4(9) . . ? O17 N2 O18 115.8(12) . . ? O17' N2 O18 140.7(10) . . ? C28 N2 O18 108.7(9) . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.799 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.113 #===END data_1.2AC _database_code_depnum_ccdc_archive 'CCDC 846746' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.2AC ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 92 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT112_1.2AC ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... n RESPONSE: Since the host molecule has a chiral camphorsulfonyl group, the crystals can not belong to a centro-symmetric space group. ; _vrf_PLAT220_1.2AC ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.50 Ratio RESPONSE: This alert is due to the higher anisotropies of carbonyl O atoms of the host molecule, which are situated at the edge of the cavity containing disordered guest molecules. ; _vrf_PLAT222_1.2AC ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.25 Ratio RESPONSE: The alert for H atoms is because their thermal parameters come from C atoms to which they are attached having higher thermal anisotropies. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1,2,3,4(6),5-O-PENTA ACETYL 6(4)-O-CAMPHORSULFONYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, 0.75 (C3 H6 O)' _chemical_formula_sum 'C28.25 H40.50 O14.75 S' _chemical_formula_weight 648.17 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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.597(4) _cell_length_b 14.351(4) _cell_length_c 17.818(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.466(5) _cell_angle_gamma 90.00 _cell_volume 3475.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7605 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.15 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9091 _exptl_absorpt_correction_T_max 0.9429 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17415 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11744 _reflns_number_gt 9729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.1152P)^2^+1.3878P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(10) _refine_ls_number_reflns 11744 _refine_ls_number_parameters 801 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _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 0.36290(7) 0.55644(7) 0.38732(5) 0.0339(3) Uani 1 1 d . . . O1 O 0.3738(3) 0.1902(2) 0.14114(18) 0.0466(8) Uani 1 1 d . . . O2 O 0.5074(2) 0.2952(3) 0.22931(17) 0.0432(8) Uani 1 1 d . . . O3 O 0.5008(2) 0.4885(2) 0.22317(16) 0.0378(7) Uani 1 1 d . . . O4 O 0.33064(19) 0.5142(2) 0.30786(15) 0.0305(7) Uani 1 1 d . . . O5 O 0.2333(2) 0.3493(2) 0.34683(15) 0.0330(7) Uani 1 1 d . . . O6 O 0.2073(2) 0.2198(2) 0.22331(17) 0.0364(7) Uani 1 1 d . . . O7 O 0.3585(5) 0.2342(4) 0.0230(2) 0.1037(19) Uani 1 1 d . . . O8 O 0.6303(3) 0.3130(5) 0.1498(3) 0.123(3) Uani 1 1 d . . . O9 O 0.4977(3) 0.5268(3) 0.10135(18) 0.0601(10) Uani 1 1 d . . . O10 O 0.0799(2) 0.3741(3) 0.30058(19) 0.0541(9) Uani 1 1 d . . . O11 O 0.2397(3) 0.1162(3) 0.3147(2) 0.0587(10) Uani 1 1 d . . . O12 O 0.3845(2) 0.4828(3) 0.43791(17) 0.0478(9) Uani 1 1 d . . . O13 O 0.2868(2) 0.6194(3) 0.40312(17) 0.0470(8) Uani 1 1 d . . . O14 O 0.5640(4) 0.7889(4) 0.3423(3) 0.0927(15) Uani 1 1 d . . . C1 C 0.3493(3) 0.2808(3) 0.1662(2) 0.0339(10) Uani 1 1 d . . . H1 H 0.3042 0.3099 0.1294 0.041 Uiso 1 1 calc R . . C2 C 0.4414(3) 0.3411(3) 0.1757(3) 0.0367(10) Uani 1 1 d . . . H2 H 0.4734 0.3492 0.1275 0.044 Uiso 1 1 calc R . . C3 C 0.4144(3) 0.4348(3) 0.2086(2) 0.0312(10) Uani 1 1 d . . . H3 H 0.3709 0.4683 0.1732 0.037 Uiso 1 1 calc R . . C4 C 0.3637(3) 0.4243(3) 0.2840(2) 0.0298(9) Uani 1 1 d . . . H4 H 0.4090 0.3972 0.3216 0.036 Uiso 1 1 calc R . . C5 C 0.2731(3) 0.3629(3) 0.2732(2) 0.0312(10) Uani 1 1 d . . . H5 H 0.2245 0.3948 0.2407 0.037 Uiso 1 1 calc R . . C6 C 0.2976(3) 0.2689(3) 0.2398(2) 0.0313(10) Uani 1 1 d . . . H6 H 0.333(3) 0.237(3) 0.271(2) 0.020(9) Uiso 1 1 d . . . C7 C 0.3681(5) 0.1744(4) 0.0674(3) 0.0640(17) Uani 1 1 d . . . C8 C 0.3860(6) 0.0761(5) 0.0480(4) 0.088(2) Uani 1 1 d . . . H8A H 0.3434 0.0583 0.0067 0.131 Uiso 1 1 calc R . . H8B H 0.3731 0.0374 0.0906 0.131 Uiso 1 1 calc R . . H8C H 0.4533 0.0685 0.0341 0.131 Uiso 1 1 calc R . . C9 C 0.6016(4) 0.2820(5) 0.2078(4) 0.0640(16) Uani 1 1 d . . . C10 C 0.6581(4) 0.2349(6) 0.2696(4) 0.090(2) Uani 1 1 d . . . H10A H 0.7134 0.2030 0.2494 0.135 Uiso 1 1 calc R . . H10B H 0.6164 0.1909 0.2940 0.135 Uiso 1 1 calc R . . H10C H 0.6808 0.2805 0.3054 0.135 Uiso 1 1 calc R . . C11 C 0.5359(3) 0.5339(4) 0.1619(3) 0.0477(12) Uani 1 1 d . . . C12 C 0.6244(4) 0.5910(5) 0.1815(4) 0.0670(17) Uani 1 1 d . . . H12A H 0.6441 0.6253 0.1381 0.101 Uiso 1 1 calc R . . H12B H 0.6771 0.5508 0.1979 0.101 Uiso 1 1 calc R . . H12C H 0.6091 0.6337 0.2210 0.101 Uiso 1 1 calc R . . C13 C 0.1344(3) 0.3563(4) 0.3529(3) 0.0396(11) Uani 1 1 d . . . C14 C 0.1057(4) 0.3391(5) 0.4309(3) 0.0607(16) Uani 1 1 d . . . H14A H 0.0365 0.3502 0.4353 0.091 Uiso 1 1 calc R . . H14B H 0.1417 0.3802 0.4640 0.091 Uiso 1 1 calc R . . H14C H 0.1202 0.2757 0.4441 0.091 Uiso 1 1 calc R . . C15 C 0.1883(4) 0.1432(3) 0.2630(3) 0.0398(11) Uani 1 1 d . . . C16 C 0.0964(4) 0.0970(4) 0.2334(3) 0.0604(15) Uani 1 1 d . . . H16A H 0.0940 0.0340 0.2515 0.091 Uiso 1 1 calc R . . H16B H 0.0963 0.0967 0.1795 0.091 Uiso 1 1 calc R . . H16C H 0.0400 0.1306 0.2503 0.091 Uiso 1 1 calc R . . C17 C 0.4693(3) 0.6188(4) 0.3665(2) 0.0366(10) Uani 1 1 d . . . H17A H 0.5157 0.5760 0.3446 0.044 Uiso 1 1 calc R . . H17B H 0.4521 0.6647 0.3284 0.044 Uiso 1 1 calc R . . C18 C 0.5218(3) 0.6694(4) 0.4319(3) 0.0458(12) Uani 1 1 d . . . C19 C 0.4617(4) 0.7098(6) 0.4968(3) 0.082(2) Uani 1 1 d . . . H19A H 0.4254 0.7647 0.4805 0.099 Uiso 1 1 calc R . . H19B H 0.4157 0.6640 0.5151 0.099 Uiso 1 1 calc R . . C20 C 0.5387(5) 0.7351(8) 0.5583(4) 0.112(4) Uani 1 1 d . . . H20A H 0.5361 0.8009 0.5706 0.135 Uiso 1 1 calc R . . H20B H 0.5294 0.6988 0.6034 0.135 Uiso 1 1 calc R . . C21 C 0.6347(4) 0.7104(6) 0.5217(3) 0.085(2) Uani 1 1 d . . . H21 H 0.6898 0.7024 0.5576 0.102 Uiso 1 1 calc R . . C22 C 0.6538(4) 0.7799(5) 0.4623(3) 0.0766(17) Uani 1 1 d . . . H22A H 0.7201 0.7744 0.4441 0.092 Uiso 1 1 calc R . . H22B H 0.6433 0.8430 0.4801 0.092 Uiso 1 1 calc R . . C23 C 0.5780(4) 0.7529(4) 0.4025(3) 0.0584(13) Uani 1 1 d . . . C24 C 0.6074(4) 0.6197(5) 0.4771(3) 0.0710(17) Uani 1 1 d . . . C25 C 0.5783(5) 0.5382(6) 0.5254(4) 0.097(2) Uani 1 1 d . . . H25A H 0.5577 0.4872 0.4939 0.145 Uiso 1 1 calc R . . H25B H 0.5252 0.5563 0.5567 0.145 Uiso 1 1 calc R . . H25C H 0.6336 0.5193 0.5563 0.145 Uiso 1 1 calc R . . C26 C 0.6886(4) 0.5859(6) 0.4239(4) 0.083(2) Uani 1 1 d . . . H26A H 0.7448 0.5653 0.4531 0.125 Uiso 1 1 calc R . . H26B H 0.7074 0.6362 0.3918 0.125 Uiso 1 1 calc R . . H26C H 0.6638 0.5351 0.3938 0.125 Uiso 1 1 calc R . . S1' S 0.13535(7) 0.52680(7) 0.11021(5) 0.0295(2) Uani 1 1 d . . . O1' O -0.0017(2) 0.5890(2) 0.27619(16) 0.0383(8) Uani 1 1 d . . . O2' O -0.0116(2) 0.7818(2) 0.27241(17) 0.0412(8) Uani 1 1 d . . . O3' O 0.1169(2) 0.8911(2) 0.35460(16) 0.0403(7) Uani 1 1 d . . . O4' O 0.2910(2) 0.8579(2) 0.27904(16) 0.0351(7) Uani 1 1 d . . . O5' O 0.2642(2) 0.7326(2) 0.15322(14) 0.0311(7) Uani 1 1 d . . . O6' O 0.16730(19) 0.5657(2) 0.19132(15) 0.0317(7) Uani 1 1 d . . . O7' O 0.0044(3) 0.5469(3) 0.39715(19) 0.0641(11) Uani 1 1 d . . . O8' O -0.1304(4) 0.7668(8) 0.3530(4) 0.171(4) Uani 1 1 d . . . O9' O 0.1488(5) 0.8604(4) 0.4744(2) 0.110(2) Uani 1 1 d . . . O10' O 0.4149(2) 0.6930(4) 0.19536(19) 0.0635(12) Uani 1 1 d . . . O11' O 0.2714(3) 0.9536(3) 0.1810(2) 0.0607(11) Uani 1 1 d . . . O12' O 0.1208(2) 0.6013(2) 0.05937(17) 0.0463(8) Uani 1 1 d . . . O13' O 0.2080(2) 0.4588(3) 0.09566(18) 0.0484(9) Uani 1 1 d . . . O14' O -0.1717(3) 0.5296(4) 0.0885(3) 0.0830(14) Uani 1 1 d . . . C1' C 0.0861(3) 0.6445(3) 0.2907(2) 0.0330(10) Uani 1 1 d . . . H1' H 0.1308 0.6115 0.3256 0.040 Uiso 1 1 calc R . . C2' C 0.0583(3) 0.7381(3) 0.3234(2) 0.0372(11) Uani 1 1 d . . . H2' H 0.0281 0.7286 0.3722 0.045 Uiso 1 1 calc R . . C3' C 0.1471(3) 0.7984(3) 0.3332(2) 0.0341(10) Uani 1 1 d . . . H3' H 0.1917 0.7722 0.3718 0.041 Uiso 1 1 calc R . . C4' C 0.2009(3) 0.8108(3) 0.2601(2) 0.0302(10) Uani 1 1 d . . . H4' H 0.1613 0.8482 0.2247 0.036 Uiso 1 1 calc R . . C5' C 0.2251(3) 0.7175(3) 0.2258(2) 0.0292(9) Uani 1 1 d . . . H5' H 0.2741 0.6853 0.2577 0.035 Uiso 1 1 calc R . . C6' C 0.1341(3) 0.6569(3) 0.2162(2) 0.0297(10) Uani 1 1 d . . . H6' H 0.0878 0.6842 0.1793 0.036 Uiso 1 1 calc R . . C7' C -0.0344(3) 0.5426(4) 0.3362(3) 0.0457(12) Uani 1 1 d . . . C8' C -0.1242(4) 0.4859(5) 0.3141(4) 0.0616(16) Uani 1 1 d . . . H8D H -0.1658 0.4797 0.3566 0.092 Uiso 1 1 calc R . . H8E H -0.1041 0.4252 0.2978 0.092 Uiso 1 1 calc R . . H8F H -0.1597 0.5167 0.2741 0.092 Uiso 1 1 calc R . . C9' C -0.1041(5) 0.7894(7) 0.2940(4) 0.087(2) Uani 1 1 d . . . C10' C -0.1686(5) 0.8351(8) 0.2370(5) 0.116(3) Uani 1 1 d . . . H10D H -0.2343 0.8392 0.2554 0.173 Uiso 1 1 calc R . . H10F H -0.1692 0.7993 0.1915 0.173 Uiso 1 1 calc R . . H10E H -0.1444 0.8966 0.2271 0.173 Uiso 1 1 calc R . . C11' C 0.1208(4) 0.9141(4) 0.4286(3) 0.0490(12) Uani 1 1 d . . . C12' C 0.0875(4) 1.0103(4) 0.4376(3) 0.0564(14) Uani 1 1 d . . . H12D H 0.0740 1.0217 0.4894 0.085 Uiso 1 1 calc R . . H12E H 0.0287 1.0202 0.4076 0.085 Uiso 1 1 calc R . . H12F H 0.1379 1.0522 0.4217 0.085 Uiso 1 1 calc R . . C13' C 0.3614(3) 0.7169(4) 0.1451(3) 0.0416(11) Uani 1 1 d . . . C14' C 0.3908(4) 0.7367(5) 0.0657(3) 0.0687(19) Uani 1 1 d . . . H14D H 0.4210 0.7971 0.0634 0.103 Uiso 1 1 calc R . . H14E H 0.3335 0.7355 0.0331 0.103 Uiso 1 1 calc R . . H14F H 0.4367 0.6902 0.0499 0.103 Uiso 1 1 calc R . . C15' C 0.3183(3) 0.9292(4) 0.2343(3) 0.0404(11) Uani 1 1 d . . . C16' C 0.4141(4) 0.9697(4) 0.2622(3) 0.0543(13) Uani 1 1 d . . . H16D H 0.4588 0.9202 0.2755 0.082 Uiso 1 1 calc R . . H16E H 0.4030 1.0078 0.3055 0.082 Uiso 1 1 calc R . . H16F H 0.4420 1.0071 0.2234 0.082 Uiso 1 1 calc R . . C17' C 0.0219(3) 0.4747(4) 0.1285(2) 0.0434(12) Uani 1 1 d . . . H17C H 0.0328 0.4278 0.1670 0.052 Uiso 1 1 calc R . . H17D H -0.0205 0.5220 0.1493 0.052 Uiso 1 1 calc R . . C18' C -0.0336(3) 0.4288(3) 0.0624(3) 0.0392(10) Uani 1 1 d . . . C19' C -0.0002(4) 0.4489(4) -0.0197(3) 0.0611(13) Uani 1 1 d . . . H19C H -0.0209 0.5103 -0.0365 0.073 Uiso 1 1 calc R . . H19D H 0.0706 0.4434 -0.0238 0.073 Uiso 1 1 calc R . . C20' C -0.0553(4) 0.3702(5) -0.0649(3) 0.0676(17) Uani 1 1 d . . . H20C H -0.0972 0.3964 -0.1044 0.081 Uiso 1 1 calc R . . H20D H -0.0090 0.3275 -0.0871 0.081 Uiso 1 1 calc R . . C21' C -0.1146(4) 0.3224(4) -0.0080(3) 0.0545(13) Uani 1 1 d . . . H21' H -0.1380 0.2604 -0.0232 0.065 Uiso 1 1 calc R . . C22' C -0.1964(3) 0.3898(4) 0.0135(3) 0.0592(13) Uani 1 1 d . . . H22C H -0.2272 0.4183 -0.0306 0.071 Uiso 1 1 calc R . . H22D H -0.2463 0.3589 0.0424 0.071 Uiso 1 1 calc R . . C23' C -0.1402(4) 0.4605(4) 0.0601(3) 0.0533(12) Uani 1 1 d . . . C24' C -0.0461(4) 0.3223(3) 0.0628(3) 0.0563(13) Uani 1 1 d . . . C25' C 0.0495(5) 0.2700(5) 0.0521(4) 0.094(2) Uani 1 1 d . . . H25D H 0.0878 0.3016 0.0154 0.140 Uiso 1 1 calc R . . H25E H 0.0353 0.2078 0.0352 0.140 Uiso 1 1 calc R . . H25F H 0.0859 0.2675 0.0990 0.140 Uiso 1 1 calc R . . C26' C -0.0951(5) 0.2885(5) 0.1339(4) 0.095(2) Uani 1 1 d . . . H26D H -0.0525 0.3006 0.1766 0.142 Uiso 1 1 calc R . . H26E H -0.1074 0.2228 0.1301 0.142 Uiso 1 1 calc R . . H26F H -0.1562 0.3209 0.1397 0.142 Uiso 1 1 calc R . . O15' O 0.8725(10) 0.1134(12) 0.3178(8) 0.052(3) Uiso 0.25 1 d P A 1 O15 O 0.8679(7) 0.0680(8) 0.3138(5) 0.071(2) Uiso 0.50 1 d P A 2 C27 C 0.8459(8) 0.1581(8) 0.4299(6) 0.101(3) Uiso 0.75 1 d P A . H27A H 0.8987 0.1986 0.4162 0.152 Uiso 0.75 1 calc PR . . H27B H 0.8619 0.1288 0.4771 0.152 Uiso 0.75 1 calc PR . . H27C H 0.7866 0.1939 0.4344 0.152 Uiso 0.75 1 calc PR . . C28 C 0.8318(6) 0.0896(6) 0.3743(5) 0.068(2) Uiso 0.75 1 d P . . C29 C 0.7538(9) 0.0224(11) 0.3895(7) 0.123(4) Uiso 0.75 1 d P A . H29A H 0.7020 0.0286 0.3522 0.184 Uiso 0.75 1 calc PR . . H29B H 0.7282 0.0343 0.4383 0.184 Uiso 0.75 1 calc PR . . H29C H 0.7801 -0.0396 0.3880 0.184 Uiso 0.75 1 calc PR . . O16 O 0.6383(8) 1.0029(8) 0.1907(6) 0.063(3) Uiso 0.38 1 d P B 1 O16' O 0.6111(10) 1.0453(11) 0.1688(8) 0.094(4) Uiso 0.38 1 d P B 2 C30 C 0.7505(10) 1.0570(11) 0.1071(7) 0.130(5) Uiso 0.75 1 d P B . H30A H 0.7422 1.0894 0.0602 0.196 Uiso 0.75 1 calc PR . . H30B H 0.8055 1.0153 0.1044 0.196 Uiso 0.75 1 calc PR . . H30C H 0.7623 1.1013 0.1467 0.196 Uiso 0.75 1 calc PR . . C31 C 0.6636(8) 1.0050(8) 0.1219(6) 0.090(3) Uiso 0.75 1 d P . . C32 C 0.6434(11) 0.9271(13) 0.0807(8) 0.154(6) Uiso 0.75 1 d P B . H32A H 0.6083 0.8833 0.1107 0.231 Uiso 0.75 1 calc PR . . H32B H 0.7038 0.8995 0.0650 0.231 Uiso 0.75 1 calc PR . . H32C H 0.6038 0.9435 0.0373 0.231 Uiso 0.75 1 calc PR . . 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 0.0316(6) 0.0445(7) 0.0253(5) -0.0002(5) -0.0030(4) -0.0055(5) O1 0.054(2) 0.044(2) 0.0416(18) -0.0021(16) 0.0104(15) 0.0055(16) O2 0.0290(16) 0.055(2) 0.0451(19) 0.0006(16) 0.0016(13) 0.0086(14) O3 0.0259(15) 0.051(2) 0.0371(17) 0.0005(14) 0.0021(13) -0.0048(13) O4 0.0269(14) 0.0362(18) 0.0280(14) -0.0010(12) -0.0034(11) 0.0001(13) O5 0.0259(14) 0.0444(19) 0.0288(15) 0.0062(13) 0.0034(11) -0.0022(13) O6 0.0309(15) 0.0401(18) 0.0381(17) 0.0043(14) -0.0029(13) -0.0027(13) O7 0.198(6) 0.069(3) 0.045(2) 0.001(2) 0.032(3) 0.002(3) O8 0.053(3) 0.186(7) 0.133(5) 0.073(5) 0.047(3) 0.040(3) O9 0.069(2) 0.077(3) 0.0348(18) 0.0024(18) 0.0175(16) -0.027(2) O10 0.0302(16) 0.088(3) 0.044(2) 0.0070(18) -0.0002(15) 0.0072(17) O11 0.062(2) 0.062(2) 0.051(2) 0.0209(18) -0.0130(17) -0.0107(19) O12 0.058(2) 0.055(2) 0.0297(16) 0.0092(15) -0.0103(14) -0.0131(17) O13 0.0359(17) 0.061(2) 0.0443(18) -0.0154(17) 0.0011(14) 0.0040(17) O14 0.096(3) 0.086(3) 0.095(3) 0.026(3) -0.019(3) -0.037(3) C1 0.031(2) 0.036(3) 0.035(2) -0.005(2) 0.0025(18) 0.0021(19) C2 0.034(2) 0.043(3) 0.034(2) 0.002(2) 0.0053(19) 0.001(2) C3 0.027(2) 0.039(3) 0.027(2) 0.0019(18) 0.0019(17) -0.0036(19) C4 0.026(2) 0.036(3) 0.028(2) 0.0051(18) 0.0016(17) -0.0003(18) C5 0.027(2) 0.039(3) 0.028(2) 0.0063(19) 0.0019(17) -0.0035(18) C6 0.026(2) 0.036(3) 0.032(2) 0.0040(19) -0.0018(18) -0.0023(19) C7 0.102(5) 0.053(3) 0.039(3) -0.008(3) 0.033(3) -0.008(3) C8 0.136(6) 0.059(4) 0.071(4) -0.018(3) 0.057(4) -0.023(4) C9 0.032(3) 0.080(4) 0.080(4) 0.011(3) 0.014(3) 0.013(3) C10 0.047(3) 0.115(6) 0.107(5) 0.025(5) -0.003(3) 0.030(4) C11 0.034(2) 0.067(4) 0.043(3) 0.005(3) 0.013(2) -0.006(2) C12 0.040(3) 0.079(4) 0.084(4) 0.006(3) 0.015(3) -0.019(3) C13 0.028(2) 0.053(3) 0.039(2) 0.001(2) 0.005(2) -0.001(2) C14 0.041(3) 0.096(5) 0.045(3) 0.014(3) 0.008(2) 0.011(3) C15 0.045(3) 0.038(3) 0.036(2) 0.003(2) 0.006(2) -0.003(2) C16 0.055(3) 0.058(3) 0.068(4) 0.011(3) -0.005(3) -0.009(3) C17 0.031(2) 0.047(3) 0.032(2) -0.0003(19) -0.0015(17) -0.0068(19) C18 0.037(2) 0.067(3) 0.033(2) -0.010(2) -0.0018(19) -0.010(2) C19 0.059(3) 0.124(6) 0.064(3) -0.049(4) 0.013(3) -0.019(3) C20 0.079(5) 0.193(10) 0.067(4) -0.067(5) 0.018(3) -0.047(5) C21 0.067(4) 0.144(6) 0.042(3) -0.024(4) -0.004(3) -0.050(4) C22 0.057(3) 0.098(5) 0.076(4) -0.030(3) 0.007(3) -0.029(3) C23 0.053(3) 0.054(3) 0.068(3) -0.005(3) -0.005(2) -0.011(2) C24 0.066(3) 0.102(5) 0.044(3) 0.010(3) -0.026(3) -0.024(3) C25 0.080(4) 0.144(6) 0.064(4) 0.035(4) -0.037(3) -0.017(4) C26 0.052(3) 0.111(6) 0.087(4) -0.002(4) -0.009(3) 0.014(4) S1' 0.0282(5) 0.0329(5) 0.0272(5) -0.0018(4) -0.0025(4) -0.0005(4) O1' 0.0316(16) 0.0446(19) 0.0390(18) -0.0036(14) 0.0066(13) -0.0111(14) O2' 0.0332(17) 0.0459(19) 0.0447(19) -0.0014(15) 0.0034(14) 0.0066(14) O3' 0.0506(19) 0.0401(18) 0.0300(15) -0.0090(14) 0.0008(13) 0.0023(15) O4' 0.0373(16) 0.0367(18) 0.0311(15) -0.0026(13) -0.0025(13) -0.0077(14) O5' 0.0293(15) 0.0417(18) 0.0221(14) -0.0017(12) -0.0004(11) 0.0003(13) O6' 0.0293(15) 0.0348(17) 0.0306(14) 0.0000(13) -0.0058(12) 0.0007(13) O7' 0.080(3) 0.071(3) 0.042(2) -0.0051(19) 0.0186(18) -0.024(2) O8' 0.075(4) 0.335(12) 0.106(4) 0.062(6) 0.049(3) 0.090(6) O9' 0.208(6) 0.092(4) 0.029(2) -0.002(2) -0.009(3) 0.060(4) O10' 0.0325(18) 0.119(4) 0.0393(19) 0.011(2) 0.0015(15) 0.019(2) O11' 0.069(2) 0.066(3) 0.047(2) 0.0190(18) -0.0094(18) -0.032(2) O12' 0.063(2) 0.044(2) 0.0313(16) 0.0003(14) -0.0083(15) -0.0036(16) O13' 0.0401(18) 0.057(2) 0.0481(19) -0.0191(17) -0.0062(15) 0.0078(17) O14' 0.055(2) 0.091(3) 0.102(3) -0.040(3) -0.019(2) 0.029(2) C1' 0.027(2) 0.041(3) 0.031(2) -0.0017(19) -0.0026(18) -0.0057(19) C2' 0.034(2) 0.050(3) 0.027(2) 0.000(2) 0.0035(19) -0.001(2) C3' 0.042(3) 0.036(3) 0.024(2) 0.0006(18) 0.0008(18) 0.001(2) C4' 0.031(2) 0.035(3) 0.024(2) 0.0003(17) -0.0043(17) 0.0008(18) C5' 0.027(2) 0.037(2) 0.024(2) 0.0004(18) -0.0026(17) 0.0003(18) C6' 0.028(2) 0.033(2) 0.027(2) -0.0030(17) -0.0064(17) -0.0002(17) C7' 0.044(3) 0.046(3) 0.048(3) -0.011(2) 0.021(2) -0.008(2) C8' 0.040(3) 0.065(4) 0.080(4) -0.007(3) 0.017(3) -0.013(3) C9' 0.057(4) 0.122(7) 0.083(5) 0.005(5) 0.013(4) 0.034(4) C10' 0.056(4) 0.178(10) 0.113(6) 0.019(6) -0.002(4) 0.050(5) C11' 0.058(3) 0.054(3) 0.035(2) -0.009(2) 0.007(2) 0.002(2) C12' 0.071(3) 0.058(3) 0.040(2) -0.020(2) 0.017(2) 0.007(2) C13' 0.035(2) 0.053(3) 0.036(2) 0.006(2) 0.005(2) 0.008(2) C14' 0.049(3) 0.116(6) 0.042(3) 0.023(3) 0.018(2) 0.012(3) C15' 0.041(3) 0.047(3) 0.033(2) -0.005(2) 0.005(2) -0.012(2) C16' 0.043(3) 0.062(3) 0.058(3) 0.001(3) 0.001(2) -0.022(2) C17' 0.035(2) 0.061(3) 0.034(2) -0.006(2) -0.0048(18) -0.014(2) C18' 0.032(2) 0.043(2) 0.042(2) -0.0074(19) -0.0103(18) -0.0034(18) C19' 0.063(3) 0.074(3) 0.046(3) -0.015(2) -0.011(2) -0.016(3) C20' 0.060(3) 0.085(4) 0.057(3) -0.036(3) -0.021(3) -0.002(3) C21' 0.053(3) 0.046(3) 0.063(3) -0.011(2) -0.018(2) -0.006(2) C22' 0.042(2) 0.075(3) 0.059(3) -0.017(3) -0.019(2) -0.003(2) C23' 0.046(3) 0.059(3) 0.055(3) -0.010(2) -0.012(2) 0.003(2) C24' 0.061(3) 0.042(3) 0.064(3) -0.005(2) -0.025(2) -0.001(2) C25' 0.082(4) 0.072(4) 0.124(6) -0.037(4) -0.048(4) 0.035(3) C26' 0.108(5) 0.079(4) 0.095(5) 0.031(4) -0.034(4) -0.050(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 S1 O13 1.408(3) . ? S1 O12 1.415(3) . ? S1 O4 1.591(3) . ? S1 C17 1.749(4) . ? O1 C7 1.334(6) . ? O1 C1 1.417(6) . ? O2 C9 1.360(6) . ? O2 C2 1.451(5) . ? O3 C11 1.368(6) . ? O3 C3 1.423(5) . ? O4 C4 1.435(5) . ? O5 C13 1.355(5) . ? O5 C5 1.445(5) . ? O6 C15 1.336(6) . ? O6 C6 1.439(5) . ? O7 C7 1.171(7) . ? O8 C9 1.200(8) . ? O9 C11 1.190(6) . ? O10 C13 1.203(6) . ? O11 C15 1.206(6) . ? O14 C23 1.201(7) . ? C1 C6 1.514(6) . ? C1 C2 1.528(6) . ? C1 H1 0.9800 . ? C2 C3 1.516(7) . ? C2 H2 0.9800 . ? C3 C4 1.532(6) . ? C3 H3 0.9800 . ? C4 C5 1.522(6) . ? C4 H4 0.9800 . ? C5 C6 1.515(7) . ? C5 H5 0.9800 . ? C6 H6 0.85(4) . ? C7 C8 1.475(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.488(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.490(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.474(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.499(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.534(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.521(8) . ? C18 C19 1.546(7) . ? C18 C24 1.570(7) . ? C19 C20 1.538(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.515(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.481(10) . ? C21 C24 1.565(9) . ? C21 H21 0.9800 . ? C22 C23 1.514(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.511(9) . ? C24 C26 1.550(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O12' 1.412(3) . ? S1' O13' 1.417(3) . ? S1' O6' 1.599(3) . ? S1' C17' 1.752(5) . ? O1' C7' 1.345(6) . ? O1' C1' 1.453(5) . ? O2' C9' 1.328(7) . ? O2' C2' 1.443(5) . ? O3' C11' 1.358(5) . ? O3' C3' 1.446(6) . ? O4' C15' 1.354(6) . ? O4' C4' 1.432(5) . ? O5' C13' 1.353(5) . ? O5' C5' 1.426(5) . ? O6' C6' 1.458(5) . ? O7' C7' 1.197(6) . ? O8' C9' 1.164(9) . ? O9' C11' 1.178(7) . ? O10' C13' 1.190(5) . ? O11' C15' 1.183(6) . ? O14' C23' 1.198(6) . ? C1' C6' 1.505(6) . ? C1' C2' 1.515(7) . ? C1' H1' 0.9800 . ? C2' C3' 1.492(6) . ? C2' H2' 0.9800 . ? C3' C4' 1.520(6) . ? C3' H3' 0.9800 . ? C4' C5' 1.511(6) . ? C4' H4' 0.9800 . ? C5' C6' 1.519(6) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.511(7) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.480(10) . ? C10' H10D 0.9600 . ? C10' H10F 0.9600 . ? C10' H10E 0.9600 . ? C11' C12' 1.463(8) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.508(6) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.500(6) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.531(6) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.518(7) . ? C18' C24' 1.537(7) . ? C18' C19' 1.571(7) . ? C19' C20' 1.567(7) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.480(9) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.530(7) . ? C21' C24' 1.548(6) . ? C21' H21' 0.9800 . ? C22' C23' 1.508(6) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C25' 1.518(8) . ? C24' C26' 1.525(9) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? O15' C28 1.210(15) . ? O15 C28 1.235(12) . ? C27 C28 1.406(13) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.463(15) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O16 C31 1.282(14) . ? O16' C31 1.254(16) . ? C30 C31 1.428(16) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.362(18) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 O13 S1 O12 119.6(2) . . ? O13 S1 O4 103.60(16) . . ? O12 S1 O4 109.29(18) . . ? O13 S1 C17 109.2(2) . . ? O12 S1 C17 111.0(2) . . ? O4 S1 C17 102.52(18) . . ? C7 O1 C1 117.2(4) . . ? C9 O2 C2 116.7(4) . . ? C11 O3 C3 114.6(3) . . ? C4 O4 S1 121.7(2) . . ? C13 O5 C5 117.2(3) . . ? C15 O6 C6 118.0(3) . . ? O1 C1 C6 106.7(4) . . ? O1 C1 C2 110.9(4) . . ? C6 C1 C2 111.4(4) . . ? O1 C1 H1 109.3 . . ? C6 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? O2 C2 C3 107.4(4) . . ? O2 C2 C1 107.9(4) . . ? C3 C2 C1 109.9(4) . . ? O2 C2 H2 110.5 . . ? C3 C2 H2 110.5 . . ? C1 C2 H2 110.5 . . ? O3 C3 C2 110.1(4) . . ? O3 C3 C4 106.4(3) . . ? C2 C3 C4 111.7(4) . . ? O3 C3 H3 109.5 . . ? C2 C3 H3 109.5 . . ? C4 C3 H3 109.5 . . ? O4 C4 C5 107.4(3) . . ? O4 C4 C3 108.8(3) . . ? C5 C4 C3 109.1(3) . . ? O4 C4 H4 110.5 . . ? C5 C4 H4 110.5 . . ? C3 C4 H4 110.5 . . ? O5 C5 C6 109.1(3) . . ? O5 C5 C4 106.5(3) . . ? C6 C5 C4 112.3(3) . . ? O5 C5 H5 109.6 . . ? C6 C5 H5 109.6 . . ? C4 C5 H5 109.6 . . ? O6 C6 C1 106.9(3) . . ? O6 C6 C5 108.7(3) . . ? C1 C6 C5 110.6(4) . . ? O6 C6 H6 109(2) . . ? C1 C6 H6 110(2) . . ? C5 C6 H6 111(2) . . ? O7 C7 O1 122.9(5) . . ? O7 C7 C8 124.0(5) . . ? O1 C7 C8 112.8(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 121.3(5) . . ? O8 C9 C10 129.3(5) . . ? O2 C9 C10 109.1(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 122.0(5) . . ? O9 C11 C12 126.2(5) . . ? O3 C11 C12 111.8(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 123.1(4) . . ? O10 C13 C14 126.4(4) . . ? O5 C13 C14 110.5(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 123.6(5) . . ? O11 C15 C16 126.0(5) . . ? O6 C15 C16 110.4(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 116.9(3) . . ? C18 C17 H17A 108.1 . . ? S1 C17 H17A 108.1 . . ? C18 C17 H17B 108.1 . . ? S1 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C23 C18 C17 109.8(4) . . ? C23 C18 C19 104.0(5) . . ? C17 C18 C19 120.1(4) . . ? C23 C18 C24 99.4(4) . . ? C17 C18 C24 120.0(5) . . ? C19 C18 C24 100.7(4) . . ? C20 C19 C18 104.9(5) . . ? C20 C19 H19A 110.8 . . ? C18 C19 H19A 110.8 . . ? C20 C19 H19B 110.8 . . ? C18 C19 H19B 110.8 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 102.5(5) . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C20 108.5(7) . . ? C22 C21 C24 104.0(4) . . ? C20 C21 C24 102.6(5) . . ? C22 C21 H21 113.6 . . ? C20 C21 H21 113.6 . . ? C24 C21 H21 113.6 . . ? C21 C22 C23 101.6(5) . . ? C21 C22 H22A 111.4 . . ? C23 C22 H22A 111.4 . . ? C21 C22 H22B 111.4 . . ? C23 C22 H22B 111.4 . . ? H22A C22 H22B 109.3 . . ? O14 C23 C22 127.4(5) . . ? O14 C23 C18 125.3(5) . . ? C22 C23 C18 107.3(5) . . ? C25 C24 C26 107.9(6) . . ? C25 C24 C21 114.6(5) . . ? C26 C24 C21 114.1(5) . . ? C25 C24 C18 116.3(5) . . ? C26 C24 C18 111.0(4) . . ? C21 C24 C18 92.6(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12' S1' O13' 119.4(2) . . ? O12' S1' O6' 110.27(18) . . ? O13' S1' O6' 103.34(17) . . ? O12' S1' C17' 109.4(2) . . ? O13' S1' C17' 111.2(3) . . ? O6' S1' C17' 101.58(18) . . ? C7' O1' C1' 114.6(3) . . ? C9' O2' C2' 117.8(4) . . ? C11' O3' C3' 118.3(4) . . ? C15' O4' C4' 117.6(3) . . ? C13' O5' C5' 117.3(3) . . ? C6' O6' S1' 120.6(2) . . ? O1' C1' C6' 106.3(3) . . ? O1' C1' C2' 110.0(4) . . ? C6' C1' C2' 110.7(4) . . ? O1' C1' H1' 109.9 . . ? C6' C1' H1' 109.9 . . ? C2' C1' H1' 109.9 . . ? O2' C2' C3' 109.8(4) . . ? O2' C2' C1' 108.1(4) . . ? C3' C2' C1' 110.5(4) . . ? O2' C2' H2' 109.5 . . ? C3' C2' H2' 109.5 . . ? C1' C2' H2' 109.5 . . ? O3' C3' C2' 109.3(4) . . ? O3' C3' C4' 105.4(3) . . ? C2' C3' C4' 111.9(3) . . ? O3' C3' H3' 110.1 . . ? C2' C3' H3' 110.1 . . ? C4' C3' H3' 110.1 . . ? O4' C4' C5' 108.7(3) . . ? O4' C4' C3' 106.3(3) . . ? C5' C4' C3' 111.0(4) . . ? O4' C4' H4' 110.3 . . ? C5' C4' H4' 110.3 . . ? C3' C4' H4' 110.3 . . ? O5' C5' C4' 108.8(3) . . ? O5' C5' C6' 107.8(3) . . ? C4' C5' C6' 111.6(3) . . ? O5' C5' H5' 109.5 . . ? C4' C5' H5' 109.5 . . ? C6' C5' H5' 109.5 . . ? O6' C6' C1' 107.9(3) . . ? O6' C6' C5' 106.9(3) . . ? C1' C6' C5' 109.8(3) . . ? O6' C6' H6' 110.7 . . ? C1' C6' H6' 110.7 . . ? C5' C6' H6' 110.7 . . ? O7' C7' O1' 123.3(4) . . ? O7' C7' C8' 126.8(5) . . ? O1' C7' C8' 109.9(4) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 123.7(7) . . ? O8' C9' C10' 123.5(7) . . ? O2' C9' C10' 112.7(7) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? H10F C10' H10E 109.5 . . ? O9' C11' O3' 121.2(5) . . ? O9' C11' C12' 129.5(5) . . ? O3' C11' C12' 109.3(5) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O10' C13' O5' 123.3(4) . . ? O10' C13' C14' 126.1(4) . . ? O5' C13' C14' 110.6(4) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O4' 123.1(4) . . ? O11' C15' C16' 126.7(5) . . ? O4' C15' C16' 110.3(4) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 117.4(3) . . ? C18' C17' H17C 108.0 . . ? S1' C17' H17C 108.0 . . ? C18' C17' H17D 108.0 . . ? S1' C17' H17D 108.0 . . ? H17C C17' H17D 107.2 . . ? C23' C18' C17' 110.1(4) . . ? C23' C18' C24' 101.1(4) . . ? C17' C18' C24' 118.5(4) . . ? C23' C18' C19' 102.6(4) . . ? C17' C18' C19' 119.3(4) . . ? C24' C18' C19' 102.7(4) . . ? C20' C19' C18' 101.6(4) . . ? C20' C19' H19C 111.5 . . ? C18' C19' H19C 111.5 . . ? C20' C19' H19D 111.5 . . ? C18' C19' H19D 111.5 . . ? H19C C19' H19D 109.3 . . ? C21' C20' C19' 104.1(4) . . ? C21' C20' H20C 110.9 . . ? C19' C20' H20C 110.9 . . ? C21' C20' H20D 110.9 . . ? C19' C20' H20D 110.9 . . ? H20C C20' H20D 109.0 . . ? C20' C21' C22' 106.9(5) . . ? C20' C21' C24' 103.4(4) . . ? C22' C21' C24' 102.9(4) . . ? C20' C21' H21' 114.2 . . ? C22' C21' H21' 114.2 . . ? C24' C21' H21' 114.2 . . ? C23' C22' C21' 101.6(4) . . ? C23' C22' H22C 111.5 . . ? C21' C22' H22C 111.5 . . ? C23' C22' H22D 111.5 . . ? C21' C22' H22D 111.5 . . ? H22C C22' H22D 109.3 . . ? O14' C23' C22' 127.4(5) . . ? O14' C23' C18' 126.0(4) . . ? C22' C23' C18' 106.5(4) . . ? C25' C24' C26' 109.9(6) . . ? C25' C24' C18' 113.3(5) . . ? C26' C24' C18' 111.7(5) . . ? C25' C24' C21' 113.4(5) . . ? C26' C24' C21' 114.2(5) . . ? C18' C24' C21' 93.5(4) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O15' C28 O15 31.2(7) . . ? O15' C28 C27 109.4(11) . . ? O15 C28 C27 137.8(10) . . ? O15' C28 C29 133.6(11) . . ? O15 C28 C29 107.6(9) . . ? C27 C28 C29 114.6(9) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O16' C31 O16 37.1(8) . . ? O16' C31 C32 128.9(13) . . ? O16 C31 C32 116.2(12) . . ? O16' C31 C30 111.7(12) . . ? O16 C31 C30 115.6(11) . . ? C32 C31 C30 119.1(12) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.604 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.070 #===END data_1.2CF _database_code_depnum_ccdc_archive 'CCDC 846747' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.2CF ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 90 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT214_1.2CF ; PROBLEM: Atom C28' (Anion/Solvent) ADP max/min Ratio 5.1 oblat RESPONSE: This is due to the disordered solvent molecule which has free space in the crystal ordered chlorine atom Cl3' close to C9 atom. ; _vrf_PLAT220_1.2CF ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.2 Ratio RESPONSE: The alert for H atoms is because their thermal parameters come from C atoms to which they are attached having higher thermal anisotropies. ; _vrf_PLAT230_1.2CF ; PROBLEM: Hirshfeld Test Diff for O7' -- C7' ... 7.3 su RESPONSE: This alert is due to the abnormal anisotropic displacement parameters of the C=O group due to its proximity to the disordered chloroform molecule. ; _vrf_PLAT241_1.2CF ; PROBLEM: Check High Ueq as Compared to Neighbors for C19 RESPONSE: This alert is because thermal anisotropies from C atom attached to camphor moiety of the host molecule. ; _vrf_PLAT245_1.2CF ; PROBLEM: U(iso) H28 Smaller than U(eq) Cl4' by ... 0.11 AngSq RESPONSE: This is due to H atoms attached to the disordered guest molecule. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULFONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, 0.75 (C H Cl3)' _chemical_formula_sum 'C26.75 H36.75 Cl2.50 O14 S' _chemical_formula_weight 703.00 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.857(3) _cell_length_b 14.298(3) _cell_length_c 17.717(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.651(4) _cell_angle_gamma 90.00 _cell_volume 3510.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5887 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.51 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1471 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8128 _exptl_absorpt_correction_T_max 0.9100 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42287 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12340 _reflns_number_gt 9723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.1235P)^2^+0.8943P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(8) _refine_ls_number_reflns 12340 _refine_ls_number_parameters 867 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1894 _refine_ls_wR_factor_gt 0.1726 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _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 0.13623(7) 0.80754(7) 0.38867(6) 0.0434(3) Uani 1 1 d . . . O1 O 0.1321(3) 1.1644(3) 0.1284(2) 0.0641(9) Uani 1 1 d . . . O2 O -0.0021(2) 1.0740(3) 0.22112(19) 0.0611(9) Uani 1 1 d . . . O3 O -0.0066(2) 0.8793(3) 0.22571(17) 0.0551(8) Uani 1 1 d . . . O4 O 0.16530(19) 0.8488(2) 0.30846(14) 0.0418(6) Uani 1 1 d . . . O5 O 0.2634(2) 1.0150(2) 0.34801(15) 0.0470(7) Uani 1 1 d . . . O6 O 0.2881(2) 1.1431(2) 0.22404(19) 0.0558(9) Uani 1 1 d . . . O7 O 0.2084(4) 1.1213(4) 0.0240(2) 0.1076(16) Uani 1 1 d . . . O8 O -0.1264(4) 1.0560(7) 0.1417(3) 0.166(4) Uani 1 1 d . . . O9 O -0.0231(3) 0.8374(4) 0.1072(2) 0.0966(15) Uani 1 1 d . . . O10 O 0.4139(2) 0.9939(4) 0.3052(2) 0.0775(12) Uani 1 1 d . . . O11 O 0.2556(3) 1.2451(3) 0.3156(2) 0.0823(12) Uani 1 1 d . . . O12 O 0.1100(3) 0.8817(2) 0.43712(17) 0.0601(9) Uani 1 1 d . . . O13 O 0.2145(2) 0.7488(3) 0.40741(19) 0.0695(10) Uani 1 1 d . . . O14 O -0.0699(4) 0.5788(4) 0.3304(3) 0.1142(17) Uani 1 1 d . . . C1 C 0.1516(4) 1.0764(4) 0.1623(3) 0.0523(11) Uani 1 1 d . . . H1 H 0.1951 1.0412 0.1296 0.063 Uiso 1 1 calc R . . C2 C 0.0597(3) 1.0215(3) 0.1714(2) 0.0495(11) Uani 1 1 d . . . H2 H 0.0279 1.0119 0.1223 0.059 Uiso 1 1 calc R . . C3 C 0.0808(3) 0.9286(3) 0.2090(2) 0.0465(11) Uani 1 1 d . . . H3 H 0.1197 0.8903 0.1750 0.056 Uiso 1 1 calc R . . C4 C 0.1341(3) 0.9396(3) 0.2830(2) 0.0403(10) Uani 1 1 d . . . H4 H 0.0916 0.9678 0.3204 0.048 Uiso 1 1 calc R . . C5 C 0.2239(3) 0.9993(3) 0.2740(2) 0.0426(10) Uani 1 1 d . . . H5 H 0.2710 0.9654 0.2435 0.051 Uiso 1 1 calc R . . C6 C 0.2007(3) 1.0919(3) 0.2366(3) 0.0457(10) Uani 1 1 d . . . H6 H 0.1584 1.1284 0.2694 0.055 Uiso 1 1 calc R . . C7 C 0.1677(4) 1.1798(4) 0.0588(3) 0.0607(13) Uani 1 1 d . . . C8 C 0.1562(5) 1.2759(4) 0.0342(3) 0.0767(16) Uani 1 1 d . . . H8A H 0.1956 1.2869 -0.0091 0.115 Uiso 1 1 calc R . . H8B H 0.1756 1.3173 0.0743 0.115 Uiso 1 1 calc R . . H8C H 0.0898 1.2873 0.0212 0.115 Uiso 1 1 calc R . . C9 C -0.0943(4) 1.0867(7) 0.1989(4) 0.094(2) Uani 1 1 d . . . C10 C -0.1458(5) 1.1483(8) 0.2538(4) 0.122(3) Uani 1 1 d . . . H10A H -0.2076 1.1656 0.2331 0.182 Uiso 1 1 calc R . . H10B H -0.1082 1.2035 0.2631 0.182 Uiso 1 1 calc R . . H10C H -0.1547 1.1151 0.3003 0.182 Uiso 1 1 calc R . . C11 C -0.0500(4) 0.8328(5) 0.1690(3) 0.0717(17) Uani 1 1 d . . . C12 C -0.1352(5) 0.7787(6) 0.1935(4) 0.101(3) Uani 1 1 d . . . H12A H -0.1601 0.7429 0.1517 0.151 Uiso 1 1 calc R . . H12B H -0.1841 0.8208 0.2109 0.151 Uiso 1 1 calc R . . H12C H -0.1167 0.7371 0.2337 0.151 Uiso 1 1 calc R . . C13 C 0.3603(4) 1.0100(4) 0.3572(3) 0.0628(14) Uani 1 1 d . . . C14 C 0.3854(4) 1.0241(7) 0.4376(3) 0.093(2) Uani 1 1 d . . . H14A H 0.4462 0.9946 0.4487 0.140 Uiso 1 1 calc R . . H14B H 0.3363 0.9969 0.4685 0.140 Uiso 1 1 calc R . . H14C H 0.3901 1.0898 0.4480 0.140 Uiso 1 1 calc R . . C15 C 0.3065(4) 1.2192(4) 0.2652(4) 0.0699(15) Uani 1 1 d . . . C16 C 0.3960(5) 1.2658(5) 0.2394(5) 0.106(3) Uani 1 1 d . . . H16A H 0.4195 1.3071 0.2781 0.159 Uiso 1 1 calc R . . H16B H 0.3822 1.3010 0.1944 0.159 Uiso 1 1 calc R . . H16C H 0.4440 1.2194 0.2289 0.159 Uiso 1 1 calc R . . C17 C 0.0335(3) 0.7408(4) 0.3643(2) 0.0561(12) Uani 1 1 d . . . H17A H -0.0149 0.7825 0.3431 0.067 Uiso 1 1 calc R . . H17B H 0.0512 0.6969 0.3251 0.067 Uiso 1 1 calc R . . C18 C -0.0119(4) 0.6861(5) 0.4290(3) 0.0648(14) Uani 1 1 d . . . C19 C 0.0489(5) 0.6422(8) 0.4906(5) 0.157(5) Uani 1 1 d . . . H19A H 0.0929 0.6875 0.5126 0.188 Uiso 1 1 calc R . . H19B H 0.0859 0.5900 0.4711 0.188 Uiso 1 1 calc R . . C20 C -0.0266(6) 0.6080(8) 0.5502(5) 0.150(5) Uani 1 1 d . . . H20A H -0.0205 0.5414 0.5599 0.180 Uiso 1 1 calc R . . H20B H -0.0199 0.6418 0.5974 0.180 Uiso 1 1 calc R . . C21 C -0.1175(6) 0.6299(8) 0.5122(4) 0.147(5) Uani 1 1 d . . . H21 H -0.1698 0.6345 0.5488 0.176 Uiso 1 1 calc R . . C22 C -0.1445(4) 0.5740(6) 0.4532(4) 0.100(2) Uani 1 1 d . . . H22A H -0.2106 0.5855 0.4373 0.120 Uiso 1 1 calc R . . H22B H -0.1364 0.5082 0.4651 0.120 Uiso 1 1 calc R . . C23 C -0.0735(4) 0.6061(4) 0.3947(4) 0.0797(16) Uani 1 1 d . . . C24 C -0.0940(6) 0.7327(7) 0.4760(4) 0.117(3) Uani 1 1 d . . . C25 C -0.0584(8) 0.8127(9) 0.5317(6) 0.171(5) Uani 1 1 d . . . H25A H -0.0005 0.7929 0.5573 0.256 Uiso 1 1 calc R . . H25B H -0.1075 0.8253 0.5680 0.256 Uiso 1 1 calc R . . H25C H -0.0454 0.8685 0.5033 0.256 Uiso 1 1 calc R . . C26 C -0.1759(7) 0.7757(10) 0.4264(6) 0.158(4) Uani 1 1 d . . . H26A H -0.2281 0.7950 0.4581 0.238 Uiso 1 1 calc R . . H26B H -0.1988 0.7299 0.3909 0.238 Uiso 1 1 calc R . . H26C H -0.1515 0.8289 0.3997 0.238 Uiso 1 1 calc R . . S1' S 0.36488(7) 0.84625(7) 0.10626(5) 0.0418(3) Uani 1 1 d . . . O1' O 0.5009(2) 0.7837(2) 0.2741(2) 0.0606(9) Uani 1 1 d . . . O2' O 0.5054(2) 0.5887(3) 0.27783(19) 0.0592(9) Uani 1 1 d . A . O3' O 0.3762(3) 0.4870(3) 0.36109(19) 0.0669(10) Uani 1 1 d . . . O4' O 0.2101(2) 0.5165(2) 0.27396(17) 0.0504(8) Uani 1 1 d . . . O5' O 0.2358(2) 0.6423(2) 0.14795(14) 0.0413(7) Uani 1 1 d . . . O6' O 0.33259(19) 0.8087(2) 0.18683(15) 0.0418(6) Uani 1 1 d . . . O7' O 0.5033(4) 0.8263(4) 0.3980(3) 0.118(2) Uani 1 1 d . . . O8' O 0.6261(4) 0.6218(7) 0.3587(5) 0.158(3) Uani 1 1 d . A . O9' O 0.3070(7) 0.5177(5) 0.4704(3) 0.163(3) Uani 1 1 d . . . O10' O 0.2365(4) 0.4144(3) 0.1799(2) 0.0940(15) Uani 1 1 d . . . O11' O 0.0872(2) 0.6762(4) 0.18802(18) 0.0766(13) Uani 1 1 d . . . O12' O 0.3894(3) 0.7709(3) 0.05979(18) 0.0679(10) Uani 1 1 d . . . O13' O 0.2880(2) 0.9064(3) 0.0845(2) 0.0706(10) Uani 1 1 d . . . O14' O 0.6524(3) 0.8402(3) 0.0942(3) 0.1005(14) Uani 1 1 d . . . C1' C 0.4139(3) 0.7319(3) 0.2898(3) 0.0488(11) Uani 1 1 d . . . H1' H 0.3722 0.7675 0.3237 0.059 Uiso 1 1 calc R . . C2' C 0.4400(3) 0.6369(4) 0.3248(3) 0.0517(12) Uani 1 1 d . . . H2' H 0.4700 0.6468 0.3744 0.062 Uiso 1 1 calc R . . C3' C 0.3488(3) 0.5786(3) 0.3337(2) 0.0483(11) Uani 1 1 d . . . H3' H 0.3050 0.6088 0.3692 0.058 Uiso 1 1 calc R . . C4' C 0.2981(3) 0.5637(3) 0.2576(2) 0.0431(10) Uani 1 1 d . . . H4' H 0.3382 0.5262 0.2238 0.052 Uiso 1 1 calc R . . C5' C 0.2743(3) 0.6574(3) 0.2226(2) 0.0399(10) Uani 1 1 d . . . H5' H 0.2270 0.6904 0.2535 0.048 Uiso 1 1 calc R . . C6' C 0.3640(3) 0.7172(3) 0.2135(2) 0.0419(10) Uani 1 1 d . . . H6' H 0.4084 0.6884 0.1776 0.050 Uiso 1 1 calc R . . C7' C 0.5401(5) 0.8281(4) 0.3342(5) 0.099(3) Uani 1 1 d . . . C8' C 0.6297(5) 0.8820(6) 0.3086(5) 0.117(3) Uani 1 1 d . . . H8D H 0.6386 0.8726 0.2555 0.175 Uiso 1 1 calc R . . H8E H 0.6854 0.8597 0.3358 0.175 Uiso 1 1 calc R . . H8F H 0.6211 0.9475 0.3185 0.175 Uiso 1 1 calc R . . C9' C 0.5965(6) 0.5837(10) 0.3023(6) 0.135(4) Uani 1 1 d . . . C10' C 0.6612(15) 0.5690(16) 0.2277(15) 0.132(8) Uani 0.50 1 d P A 1 H10D H 0.6749 0.6287 0.2055 0.197 Uiso 0.50 1 calc PR A 1 H10E H 0.6264 0.5310 0.1920 0.197 Uiso 0.50 1 calc PR A 1 H10F H 0.7206 0.5385 0.2414 0.197 Uiso 0.50 1 calc PR A 1 C10" C 0.6499(16) 0.514(2) 0.2510(11) 0.146(12) Uani 0.50 1 d P A 2 H10J H 0.6421 0.5329 0.1993 0.220 Uiso 0.50 1 calc PR A 2 H10G H 0.6235 0.4526 0.2576 0.220 Uiso 0.50 1 calc PR A 2 H10M H 0.7172 0.5136 0.2642 0.220 Uiso 0.50 1 calc PR A 2 C11' C 0.3485(7) 0.4639(5) 0.4308(4) 0.095(2) Uani 1 1 d . . . C12' C 0.3837(6) 0.3637(5) 0.4454(4) 0.122(3) Uani 1 1 d . . . H12D H 0.3692 0.3461 0.4963 0.183 Uiso 1 1 calc R . . H12E H 0.4522 0.3607 0.4381 0.183 Uiso 1 1 calc R . . H12F H 0.3519 0.3218 0.4109 0.183 Uiso 1 1 calc R . . C13' C 0.1409(3) 0.6563(4) 0.1385(2) 0.0511(12) Uani 1 1 d . . . C14' C 0.1088(4) 0.6374(5) 0.0574(3) 0.0763(18) Uani 1 1 d . . . H14D H 0.1265 0.5749 0.0436 0.114 Uiso 1 1 calc R . . H14E H 0.1396 0.6811 0.0243 0.114 Uiso 1 1 calc R . . H14F H 0.0400 0.6444 0.0532 0.114 Uiso 1 1 calc R . . C15' C 0.1873(4) 0.4410(4) 0.2287(3) 0.0583(13) Uani 1 1 d . . . C16' C 0.0921(4) 0.3994(5) 0.2534(4) 0.0852(18) Uani 1 1 d . . . H16D H 0.0867 0.3364 0.2350 0.128 Uiso 1 1 calc R . . H16E H 0.0398 0.4362 0.2334 0.128 Uiso 1 1 calc R . . H16F H 0.0893 0.3991 0.3075 0.128 Uiso 1 1 calc R . . C17' C 0.4670(4) 0.9137(5) 0.1297(2) 0.0699(17) Uani 1 1 d . . . H17C H 0.4462 0.9661 0.1602 0.084 Uiso 1 1 calc R . . H17D H 0.5096 0.8758 0.1609 0.084 Uiso 1 1 calc R . . C18' C 0.5255(4) 0.9520(4) 0.0638(3) 0.0576(12) Uani 1 1 d . . . C19' C 0.4884(5) 0.9359(6) -0.0191(3) 0.097(2) Uani 1 1 d . . . H19C H 0.5032 0.8732 -0.0364 0.117 Uiso 1 1 calc R . . H19D H 0.4193 0.9462 -0.0233 0.117 Uiso 1 1 calc R . . C20' C 0.5450(5) 1.0101(6) -0.0639(3) 0.092(2) Uani 1 1 d . . . H20C H 0.5803 0.9815 -0.1048 0.111 Uiso 1 1 calc R . . H20D H 0.5020 1.0573 -0.0845 0.111 Uiso 1 1 calc R . . C21' C 0.6132(4) 1.0519(4) -0.0060(3) 0.0639(13) Uani 1 1 d . . . H21' H 0.6419 1.1117 -0.0207 0.077 Uiso 1 1 calc R . . C22' C 0.6850(4) 0.9778(4) 0.0163(3) 0.0725(14) Uani 1 1 d . . . H22C H 0.7381 1.0041 0.0454 0.087 Uiso 1 1 calc R . . H22D H 0.7104 0.9463 -0.0277 0.087 Uiso 1 1 calc R . . C23' C 0.6259(4) 0.9121(4) 0.0635(3) 0.0673(13) Uani 1 1 d . . . C24' C 0.5473(4) 1.0570(3) 0.0646(3) 0.0667(14) Uani 1 1 d . . . C25' C 0.4599(4) 1.1210(4) 0.0563(3) 0.127(3) Uani 1 1 d . . . H25D H 0.4146 1.1073 0.0953 0.191 Uiso 1 1 calc R . . H25E H 0.4299 1.1110 0.0078 0.191 Uiso 1 1 calc R . . H25F H 0.4802 1.1850 0.0604 0.191 Uiso 1 1 calc R . . C26' C 0.6031(4) 1.0854(4) 0.1375(3) 0.0913(19) Uani 1 1 d R . . H26D H 0.6294 1.1469 0.1314 0.137 Uiso 1 1 d R . . H26E H 0.6545 1.0417 0.1469 0.137 Uiso 1 1 d R . . H26F H 0.5598 1.0850 0.1795 0.137 Uiso 1 1 d R . . C27 C 0.8298(5) 0.4446(5) 0.0791(4) 0.0692(18) Uani 0.75 1 d PDU . . H27 H 0.7865 0.4861 0.0506 0.083 Uiso 0.75 1 calc PR B 1 Cl1 Cl 0.87842(18) 0.5100(3) 0.15201(15) 0.1149(10) Uani 0.75 1 d PDU C 1 Cl2 Cl 0.7573(2) 0.3513(2) 0.11441(14) 0.1078(8) Uani 0.75 1 d PDU C . Cl3 Cl 0.91706(16) 0.4078(2) 0.01745(13) 0.0967(7) Uani 0.75 1 d PDU C . C28 C 0.6786(8) 0.1992(10) 0.4311(6) 0.066(4) Uani 0.50 1 d PDU D 1 H28 H 0.7238 0.1612 0.4611 0.079 Uiso 0.50 1 calc PR D 1 Cl4 Cl 0.6289(3) 0.1322(4) 0.3556(2) 0.1154(16) Uani 0.50 1 d PDU D 1 Cl5 Cl 0.5837(2) 0.2387(3) 0.48709(16) 0.0917(11) Uani 0.50 1 d PDU D 1 Cl6 Cl 0.7370(4) 0.2973(4) 0.3947(3) 0.1135(14) Uani 0.50 1 d PDU D 1 C28' C 0.6810(13) 0.3006(13) 0.3579(9) 0.101(6) Uani 0.25 1 d PDU E 2 H28' H 0.6732 0.2882 0.3038 0.121 Uiso 0.25 1 calc PR E 2 Cl4' Cl 0.6604(12) 0.1984(11) 0.4103(9) 0.185(7) Uani 0.25 1 d PDU E 2 Cl5' Cl 0.5929(12) 0.3844(11) 0.3889(8) 0.212(6) Uani 0.25 1 d PDU E 2 Cl6' Cl 0.7903(11) 0.3385(11) 0.3769(10) 0.206(6) Uani 0.25 1 d PDU E 2 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 0.0435(6) 0.0483(6) 0.0385(5) 0.0007(4) 0.0087(4) -0.0014(5) O1 0.077(2) 0.051(2) 0.065(2) 0.0093(16) 0.0093(17) 0.0038(17) O2 0.0527(19) 0.068(2) 0.063(2) 0.0024(17) 0.0014(16) 0.0076(17) O3 0.0454(17) 0.070(2) 0.0495(17) 0.0123(16) -0.0045(14) -0.0117(16) O4 0.0407(15) 0.0484(17) 0.0366(13) -0.0009(13) 0.0089(11) -0.0026(14) O5 0.0428(16) 0.059(2) 0.0395(15) -0.0124(14) 0.0055(12) -0.0045(15) O6 0.0537(19) 0.0440(19) 0.070(2) -0.0084(16) 0.0222(16) -0.0113(16) O7 0.169(5) 0.087(3) 0.067(2) 0.009(2) 0.035(3) 0.004(3) O8 0.094(4) 0.283(10) 0.121(4) -0.079(5) -0.062(3) 0.078(5) O9 0.118(3) 0.116(4) 0.056(2) 0.011(2) -0.022(2) -0.056(3) O10 0.0449(19) 0.126(3) 0.062(2) -0.016(2) 0.0075(17) -0.008(2) O11 0.078(2) 0.074(3) 0.095(3) -0.039(2) 0.027(2) -0.017(2) O12 0.086(2) 0.051(2) 0.0440(16) -0.0041(15) 0.0165(16) -0.0061(18) O13 0.0532(19) 0.089(3) 0.067(2) 0.030(2) 0.0115(15) 0.015(2) O14 0.136(4) 0.108(4) 0.099(3) -0.008(3) 0.008(3) -0.059(3) C1 0.058(3) 0.046(3) 0.052(3) 0.003(2) 0.003(2) 0.003(2) C2 0.054(3) 0.058(3) 0.036(2) -0.002(2) -0.0014(19) 0.005(2) C3 0.047(2) 0.055(3) 0.038(2) -0.0004(19) 0.0083(18) -0.006(2) C4 0.041(2) 0.040(2) 0.040(2) -0.0030(18) 0.0111(18) -0.0043(19) C5 0.038(2) 0.049(3) 0.041(2) -0.0126(19) 0.0153(18) -0.002(2) C6 0.042(2) 0.043(3) 0.052(2) -0.008(2) 0.0090(19) -0.002(2) C7 0.073(3) 0.060(3) 0.049(3) 0.006(2) -0.004(2) -0.009(3) C8 0.096(4) 0.066(3) 0.068(3) 0.012(3) -0.024(3) -0.008(3) C9 0.061(4) 0.142(6) 0.079(4) 0.007(4) -0.013(3) 0.020(4) C10 0.078(4) 0.173(9) 0.114(5) -0.027(6) -0.012(4) 0.063(5) C11 0.071(3) 0.095(5) 0.048(3) 0.021(3) -0.023(2) -0.026(3) C12 0.071(4) 0.114(6) 0.117(5) 0.032(5) -0.041(4) -0.045(4) C13 0.052(3) 0.073(4) 0.063(3) -0.019(3) 0.004(2) -0.012(3) C14 0.062(3) 0.162(7) 0.056(3) -0.023(4) -0.010(3) -0.020(4) C15 0.060(3) 0.054(3) 0.096(4) -0.013(3) 0.008(3) -0.003(3) C16 0.089(4) 0.065(4) 0.165(7) -0.040(4) 0.056(5) -0.024(3) C17 0.057(3) 0.060(3) 0.051(2) 0.008(2) 0.010(2) -0.005(2) C18 0.060(3) 0.088(4) 0.047(2) 0.012(2) 0.009(2) -0.010(3) C19 0.105(5) 0.200(10) 0.164(8) 0.140(8) -0.058(5) -0.071(6) C20 0.128(7) 0.223(11) 0.098(5) 0.089(7) -0.040(5) -0.095(8) C21 0.114(6) 0.244(12) 0.083(5) 0.061(6) 0.015(4) -0.100(7) C22 0.069(3) 0.136(6) 0.095(4) 0.048(4) -0.010(3) -0.045(4) C23 0.074(3) 0.074(4) 0.091(4) 0.013(3) 0.009(3) -0.021(3) C24 0.121(6) 0.158(7) 0.072(4) -0.013(5) 0.040(4) -0.051(6) C25 0.176(9) 0.192(10) 0.147(8) -0.072(7) 0.101(7) -0.066(8) C26 0.113(6) 0.208(12) 0.155(8) -0.011(9) 0.030(6) 0.047(8) S1' 0.0463(6) 0.0395(5) 0.0399(5) 0.0024(4) 0.0064(4) -0.0009(5) O1' 0.0518(18) 0.053(2) 0.076(2) 0.0104(17) -0.0160(16) -0.0145(16) O2' 0.0399(17) 0.074(2) 0.0634(19) 0.0117(17) 0.0035(15) 0.0096(17) O3' 0.077(2) 0.063(2) 0.0609(19) 0.0249(17) -0.0008(17) -0.0002(19) O4' 0.0505(17) 0.0450(19) 0.0559(18) 0.0041(15) 0.0145(15) -0.0032(15) O5' 0.0412(16) 0.0490(17) 0.0338(13) 0.0015(12) 0.0058(12) -0.0020(13) O6' 0.0430(15) 0.0376(15) 0.0450(14) 0.0016(13) 0.0102(12) 0.0023(13) O7' 0.184(5) 0.097(4) 0.071(3) 0.020(3) -0.061(3) -0.061(3) O8' 0.066(3) 0.242(9) 0.166(6) 0.003(6) -0.028(4) 0.029(4) O9' 0.310(10) 0.117(5) 0.063(3) 0.025(3) 0.050(4) -0.034(6) O10' 0.128(4) 0.081(3) 0.073(3) -0.026(2) 0.041(3) -0.044(3) O11' 0.0382(18) 0.144(4) 0.0476(18) -0.021(2) 0.0046(15) 0.012(2) O12' 0.108(3) 0.049(2) 0.0475(18) -0.0047(15) 0.0219(18) -0.003(2) O13' 0.058(2) 0.082(3) 0.072(2) 0.028(2) 0.0089(16) 0.015(2) O14' 0.116(3) 0.084(3) 0.103(3) 0.026(2) 0.031(3) 0.032(3) C1' 0.046(3) 0.047(3) 0.053(3) 0.003(2) -0.007(2) -0.007(2) C2' 0.049(3) 0.055(3) 0.051(3) 0.009(2) -0.004(2) -0.002(2) C3' 0.061(3) 0.047(3) 0.037(2) 0.010(2) 0.010(2) 0.003(2) C4' 0.048(2) 0.044(3) 0.038(2) 0.0034(18) 0.0103(18) -0.004(2) C5' 0.040(2) 0.043(2) 0.037(2) 0.0030(18) 0.0004(18) -0.0020(19) C6' 0.039(2) 0.045(3) 0.041(2) 0.0033(18) 0.0017(17) 0.0069(19) C7' 0.109(5) 0.060(4) 0.126(6) 0.025(4) -0.075(5) -0.033(4) C8' 0.075(4) 0.112(6) 0.163(7) 0.036(6) -0.047(5) -0.035(4) C9' 0.072(5) 0.222(12) 0.112(6) -0.001(7) -0.009(5) 0.066(6) C10' 0.077(10) 0.133(17) 0.19(2) 0.040(14) 0.021(12) 0.037(11) C10" 0.113(15) 0.23(3) 0.098(11) 0.036(16) 0.039(10) 0.11(2) C11' 0.157(7) 0.080(4) 0.047(3) 0.026(3) -0.033(4) -0.047(5) C12' 0.175(8) 0.086(5) 0.104(5) 0.055(4) -0.075(5) -0.037(5) C13' 0.041(3) 0.070(3) 0.043(2) 0.000(2) 0.002(2) -0.004(2) C14' 0.060(3) 0.116(5) 0.053(3) -0.023(3) -0.001(2) 0.013(3) C15' 0.066(3) 0.051(3) 0.057(3) 0.007(2) 0.003(2) -0.019(3) C16' 0.063(3) 0.087(4) 0.107(4) 0.016(4) 0.001(3) -0.030(3) C17' 0.072(3) 0.097(4) 0.040(2) -0.002(3) 0.010(2) -0.047(3) C18' 0.053(3) 0.060(3) 0.060(3) 0.010(2) 0.018(2) -0.018(2) C19' 0.102(4) 0.132(6) 0.059(3) 0.011(3) 0.015(3) -0.049(4) C20' 0.089(4) 0.127(6) 0.062(3) 0.028(3) 0.020(3) -0.014(4) C21' 0.060(3) 0.055(3) 0.077(3) 0.015(2) 0.018(2) -0.002(2) C22' 0.060(3) 0.076(3) 0.082(3) 0.013(3) 0.031(2) 0.010(2) C23' 0.087(4) 0.052(3) 0.063(3) 0.007(2) 0.023(3) 0.010(3) C24' 0.064(3) 0.052(3) 0.085(4) 0.016(3) 0.029(3) 0.002(2) C25' 0.110(5) 0.116(6) 0.157(7) 0.056(5) 0.072(5) 0.062(5) C26' 0.107(5) 0.065(3) 0.103(4) -0.020(3) 0.035(4) -0.032(3) C27 0.086(5) 0.069(4) 0.053(3) 0.000(3) 0.004(3) 0.025(4) Cl1 0.0749(13) 0.175(3) 0.0951(16) -0.0630(18) -0.0051(12) 0.0174(15) Cl2 0.135(2) 0.0970(17) 0.0911(14) 0.0207(14) 0.0099(13) 0.0035(16) Cl3 0.0811(13) 0.1218(19) 0.0877(13) -0.0243(13) 0.0191(10) 0.0258(14) C28 0.037(5) 0.122(10) 0.037(5) -0.024(5) -0.014(4) -0.013(6) Cl4 0.100(2) 0.173(4) 0.074(2) -0.055(3) 0.0089(18) -0.039(3) Cl5 0.0780(18) 0.135(3) 0.0619(15) 0.0012(17) 0.0132(13) 0.049(2) Cl6 0.132(4) 0.108(3) 0.100(3) 0.005(2) 0.005(3) -0.032(3) C28' 0.106(12) 0.179(17) 0.018(7) 0.019(10) -0.024(9) 0.034(10) Cl4' 0.202(13) 0.178(11) 0.178(14) 0.066(11) 0.089(11) 0.104(9) Cl5' 0.262(13) 0.189(11) 0.184(11) -0.001(10) -0.025(11) 0.111(12) Cl6' 0.204(10) 0.160(11) 0.252(16) -0.028(10) -0.127(11) 0.027(8) _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 O13 1.409(4) . ? S1 O12 1.414(3) . ? S1 O4 1.595(3) . ? S1 C17 1.763(5) . ? O1 C7 1.351(6) . ? O1 C1 1.419(6) . ? O2 C9 1.344(7) . ? O2 C2 1.446(5) . ? O3 C11 1.342(6) . ? O3 C3 1.434(5) . ? O4 C4 1.439(5) . ? O5 C13 1.353(6) . ? O5 C5 1.433(5) . ? O6 C15 1.333(6) . ? O6 C6 1.434(5) . ? O7 C7 1.186(7) . ? O8 C9 1.186(8) . ? O9 C11 1.163(6) . ? O10 C13 1.211(6) . ? O11 C15 1.203(6) . ? O14 C23 1.207(8) . ? C1 C6 1.491(7) . ? C1 C2 1.507(7) . ? C1 H1 0.9800 . ? C2 C3 1.513(7) . ? C2 H2 0.9800 . ? C3 C4 1.506(6) . ? C3 H3 0.9800 . ? C4 C5 1.518(6) . ? C4 H4 0.9800 . ? C5 C6 1.513(7) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.449(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.499(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.481(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.476(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.484(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.530(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.507(8) . ? C18 C23 1.547(9) . ? C18 C24 1.567(10) . ? C19 C20 1.574(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.457(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.364(12) . ? C21 C24 1.638(13) . ? C21 H21 0.9800 . ? C22 C23 1.508(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C26 1.554(13) . ? C24 C25 1.586(12) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O12' 1.400(4) . ? S1' O13' 1.419(4) . ? S1' O6' 1.594(3) . ? S1' C17' 1.758(5) . ? O1' C7' 1.349(8) . ? O1' C1' 1.444(5) . ? O2' C9' 1.332(9) . ? O2' C2' 1.415(6) . ? O3' C11' 1.339(8) . ? O3' C3' 1.446(6) . ? O4' C15' 1.379(6) . ? O4' C4' 1.427(5) . ? O5' C13' 1.339(5) . ? O5' C5' 1.437(5) . ? O6' C6' 1.456(5) . ? O7' C7' 1.245(10) . ? O8' C9' 1.206(12) . ? O9' C11' 1.193(10) . ? O10' C15' 1.171(6) . ? O11' C13' 1.191(5) . ? O14' C23' 1.217(7) . ? C1' C6' 1.526(6) . ? C1' C2' 1.535(7) . ? C1' H1' 0.9800 . ? C2' C3' 1.523(7) . ? C2' H2' 0.9800 . ? C3' C4' 1.529(6) . ? C3' H3' 0.9800 . ? C4' C5' 1.511(6) . ? C4' H4' 0.9800 . ? C5' C6' 1.519(6) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.534(10) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10" 1.54(2) . ? C9' C10' 1.62(2) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C10" H10J 0.9600 . ? C10" H10G 0.9600 . ? C10" H10M 0.9600 . ? C11' C12' 1.534(11) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.524(6) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.516(7) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.530(6) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.504(8) . ? C18' C24' 1.530(7) . ? C18' C19' 1.569(8) . ? C19' C20' 1.545(8) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.511(9) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.503(7) . ? C21' C24' 1.559(7) . ? C21' H21' 0.9800 . ? C22' C23' 1.506(7) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C25' 1.524(7) . ? C24' C26' 1.552(8) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9588 . ? C26' H26E 0.9599 . ? C26' H26F 0.9605 . ? C27 Cl3 1.721(7) . ? C27 Cl1 1.726(7) . ? C27 Cl2 1.787(8) . ? C27 H27 0.9800 . ? C28 Cl6 1.746(13) . ? C28 Cl5 1.750(13) . ? C28 Cl4 1.777(9) . ? C28 H28 0.9800 . ? C28' Cl6' 1.640(16) . ? C28' Cl4' 1.755(16) . ? C28' Cl5' 1.802(17) . ? C28' H28' 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 O13 S1 O12 120.4(2) . . ? O13 S1 O4 103.25(17) . . ? O12 S1 O4 109.44(18) . . ? O13 S1 C17 110.6(3) . . ? O12 S1 C17 110.0(2) . . ? O4 S1 C17 101.15(18) . . ? C7 O1 C1 117.5(4) . . ? C9 O2 C2 117.4(5) . . ? C11 O3 C3 117.5(4) . . ? C4 O4 S1 122.4(2) . . ? C13 O5 C5 118.1(3) . . ? C15 O6 C6 119.2(4) . . ? O1 C1 C6 109.0(4) . . ? O1 C1 C2 110.5(4) . . ? C6 C1 C2 111.1(4) . . ? O1 C1 H1 108.7 . . ? C6 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? O2 C2 C1 107.6(4) . . ? O2 C2 C3 107.5(4) . . ? C1 C2 C3 110.2(4) . . ? O2 C2 H2 110.5 . . ? C1 C2 H2 110.5 . . ? C3 C2 H2 110.5 . . ? O3 C3 C4 106.2(3) . . ? O3 C3 C2 111.3(4) . . ? C4 C3 C2 112.4(4) . . ? O3 C3 H3 109.0 . . ? C4 C3 H3 109.0 . . ? C2 C3 H3 109.0 . . ? O4 C4 C3 108.7(3) . . ? O4 C4 C5 107.3(3) . . ? C3 C4 C5 111.3(3) . . ? O4 C4 H4 109.8 . . ? C3 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? O5 C5 C6 109.9(3) . . ? O5 C5 C4 107.3(3) . . ? C6 C5 C4 111.6(3) . . ? O5 C5 H5 109.3 . . ? C6 C5 H5 109.3 . . ? C4 C5 H5 109.3 . . ? O6 C6 C1 108.4(4) . . ? O6 C6 C5 109.8(3) . . ? C1 C6 C5 110.4(4) . . ? O6 C6 H6 109.4 . . ? C1 C6 H6 109.4 . . ? C5 C6 H6 109.4 . . ? O7 C7 O1 122.7(5) . . ? O7 C7 C8 124.3(5) . . ? O1 C7 C8 112.8(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 123.1(7) . . ? O8 C9 C10 126.5(6) . . ? O2 C9 C10 110.3(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 122.2(5) . . ? O9 C11 C12 124.7(5) . . ? O3 C11 C12 113.1(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 122.3(5) . . ? O10 C13 C14 128.3(5) . . ? O5 C13 C14 109.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 123.2(5) . . ? O11 C15 C16 126.1(5) . . ? O6 C15 C16 110.7(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 115.5(3) . . ? C18 C17 H17A 108.4 . . ? S1 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? S1 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 121.6(5) . . ? C19 C18 C23 106.1(6) . . ? C17 C18 C23 108.2(4) . . ? C19 C18 C24 101.3(6) . . ? C17 C18 C24 119.2(6) . . ? C23 C18 C24 97.0(5) . . ? C18 C19 C20 104.2(6) . . ? C18 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? C18 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C19 101.5(5) . . ? C21 C20 H20A 111.5 . . ? C19 C20 H20A 111.5 . . ? C21 C20 H20B 111.5 . . ? C19 C20 H20B 111.5 . . ? H20A C20 H20B 109.3 . . ? C22 C21 C20 117.2(11) . . ? C22 C21 C24 106.3(6) . . ? C20 C21 C24 101.5(7) . . ? C22 C21 H21 110.5 . . ? C20 C21 H21 110.5 . . ? C24 C21 H21 110.5 . . ? C21 C22 C23 99.9(5) . . ? C21 C22 H22A 111.8 . . ? C23 C22 H22A 111.8 . . ? C21 C22 H22B 111.8 . . ? C23 C22 H22B 111.8 . . ? H22A C22 H22B 109.5 . . ? O14 C23 C22 125.7(6) . . ? O14 C23 C18 125.6(5) . . ? C22 C23 C18 108.5(6) . . ? C26 C24 C18 113.5(6) . . ? C26 C24 C25 106.6(10) . . ? C18 C24 C25 114.5(6) . . ? C26 C24 C21 115.4(8) . . ? C18 C24 C21 88.5(7) . . ? C25 C24 C21 117.8(7) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12' S1' O13' 119.6(2) . . ? O12' S1' O6' 109.88(18) . . ? O13' S1' O6' 103.29(18) . . ? O12' S1' C17' 111.1(3) . . ? O13' S1' C17' 109.4(3) . . ? O6' S1' C17' 101.93(19) . . ? C7' O1' C1' 114.8(5) . . ? C9' O2' C2' 116.5(6) . . ? C11' O3' C3' 117.1(5) . . ? C15' O4' C4' 116.3(3) . . ? C13' O5' C5' 116.5(3) . . ? C6' O6' S1' 120.5(2) . . ? O1' C1' C6' 105.7(4) . . ? O1' C1' C2' 109.7(4) . . ? C6' C1' C2' 109.7(4) . . ? O1' C1' H1' 110.5 . . ? C6' C1' H1' 110.5 . . ? C2' C1' H1' 110.5 . . ? O2' C2' C3' 109.4(4) . . ? O2' C2' C1' 110.1(4) . . ? C3' C2' C1' 109.5(4) . . ? O2' C2' H2' 109.3 . . ? C3' C2' H2' 109.3 . . ? C1' C2' H2' 109.3 . . ? O3' C3' C2' 108.4(4) . . ? O3' C3' C4' 106.6(4) . . ? C2' C3' C4' 110.9(3) . . ? O3' C3' H3' 110.3 . . ? C2' C3' H3' 110.3 . . ? C4' C3' H3' 110.3 . . ? O4' C4' C5' 108.6(4) . . ? O4' C4' C3' 105.8(3) . . ? C5' C4' C3' 109.5(4) . . ? O4' C4' H4' 110.9 . . ? C5' C4' H4' 110.9 . . ? C3' C4' H4' 110.9 . . ? O5' C5' C4' 108.8(3) . . ? O5' C5' C6' 106.4(3) . . ? C4' C5' C6' 111.5(3) . . ? O5' C5' H5' 110.0 . . ? C4' C5' H5' 110.0 . . ? C6' C5' H5' 110.0 . . ? O6' C6' C5' 107.3(3) . . ? O6' C6' C1' 107.1(4) . . ? C5' C6' C1' 110.3(3) . . ? O6' C6' H6' 110.7 . . ? C5' C6' H6' 110.7 . . ? C1' C6' H6' 110.7 . . ? O7' C7' O1' 122.7(6) . . ? O7' C7' C8' 128.3(6) . . ? O1' C7' C8' 108.9(7) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 124.0(8) . . ? O8' C9' C10" 128.2(12) . . ? O2' C9' C10" 107.6(13) . . ? O8' C9' C10' 123.2(13) . . ? O2' C9' C10' 105.8(11) . . ? C10" C9' C10' 33.0(11) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? C9' C10" H10J 109.5 . . ? C9' C10" H10G 109.5 . . ? H10J C10" H10G 109.5 . . ? C9' C10" H10M 109.5 . . ? H10J C10" H10M 109.5 . . ? H10G C10" H10M 109.5 . . ? O9' C11' O3' 121.9(6) . . ? O9' C11' C12' 131.1(7) . . ? O3' C11' C12' 107.0(8) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O11' C13' O5' 124.4(4) . . ? O11' C13' C14' 124.0(4) . . ? O5' C13' C14' 111.5(4) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O10' C15' O4' 123.4(5) . . ? O10' C15' C16' 127.0(5) . . ? O4' C15' C16' 109.5(5) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 116.7(3) . . ? C18' C17' H17C 108.1 . . ? S1' C17' H17C 108.1 . . ? C18' C17' H17D 108.1 . . ? S1' C17' H17D 108.1 . . ? H17C C17' H17D 107.3 . . ? C23' C18' C17' 111.4(5) . . ? C23' C18' C24' 101.0(4) . . ? C17' C18' C24' 116.8(5) . . ? C23' C18' C19' 103.5(5) . . ? C17' C18' C19' 119.4(4) . . ? C24' C18' C19' 102.5(5) . . ? C20' C19' C18' 102.5(5) . . ? C20' C19' H19C 111.3 . . ? C18' C19' H19C 111.3 . . ? C20' C19' H19D 111.3 . . ? C18' C19' H19D 111.3 . . ? H19C C19' H19D 109.2 . . ? C21' C20' C19' 103.9(5) . . ? C21' C20' H20C 111.0 . . ? C19' C20' H20C 111.0 . . ? C21' C20' H20D 111.0 . . ? C19' C20' H20D 111.0 . . ? H20C C20' H20D 109.0 . . ? C22' C21' C20' 107.8(5) . . ? C22' C21' C24' 102.3(4) . . ? C20' C21' C24' 101.3(4) . . ? C22' C21' H21' 114.6 . . ? C20' C21' H21' 114.6 . . ? C24' C21' H21' 114.6 . . ? C21' C22' C23' 103.0(4) . . ? C21' C22' H22C 111.2 . . ? C23' C22' H22C 111.2 . . ? C21' C22' H22D 111.2 . . ? C23' C22' H22D 111.2 . . ? H22C C22' H22D 109.1 . . ? O14' C23' C18' 126.4(5) . . ? O14' C23' C22' 127.7(5) . . ? C18' C23' C22' 105.9(4) . . ? C25' C24' C18' 115.6(5) . . ? C25' C24' C26' 108.2(4) . . ? C18' C24' C26' 111.1(4) . . ? C25' C24' C21' 115.0(4) . . ? C18' C24' C21' 93.7(4) . . ? C26' C24' C21' 112.9(4) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.4 . . ? C24' C26' H26E 109.6 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.4 . . ? H26D C26' H26F 109.6 . . ? H26E C26' H26F 109.4 . . ? Cl3 C27 Cl1 111.7(4) . . ? Cl3 C27 Cl2 113.3(4) . . ? Cl1 C27 Cl2 111.0(4) . . ? Cl3 C27 H27 106.8 . . ? Cl1 C27 H27 106.8 . . ? Cl2 C27 H27 106.8 . . ? Cl6 C28 Cl5 107.7(8) . . ? Cl6 C28 Cl4 109.4(7) . . ? Cl5 C28 Cl4 108.2(6) . . ? Cl6 C28 H28 110.5 . . ? Cl5 C28 H28 110.5 . . ? Cl4 C28 H28 110.5 . . ? Cl6' C28' Cl4' 108.8(13) . . ? Cl6' C28' Cl5' 110.2(14) . . ? Cl4' C28' Cl5' 106.1(11) . . ? Cl6' C28' H28' 110.5 . . ? Cl4' C28' H28' 110.5 . . ? Cl5' C28' H28' 110.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.687 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.076 #===END data_1.2DCE _database_code_depnum_ccdc_archive 'CCDC 846748' #TrackingRef '- KM_CIF.cif' _vrf_PLAT029_1.2DCE ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: This is due to the weakly diffracting inclusion crystals, which did not diffracted at high angle. ; _vrf_PLAT213_1.2DCE ; PROBLEM: Atom O8 has ADP max/min Ratio ..... 4.5 prola RESPONSE: The higher anisotropies of terminal carbonyl group of the host contribute to this alert. ; _vrf_PLAT220_1.2DCE ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.78 Ratio RESPONSE: Higher anisotropies for the terminal C atoms of the host contribute to this alert. The high ratio could be due to their (C atoms) freedom of libration and their proximity to the cavity containing guest molecules with low occupancies. ; _vrf_PLAT222_1.2DCE ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.32 Ratio RESPONSE: The alert for H atoms is because their thermal parameters come from C atoms to which they are attached having higher thermal anisotropies. ; _vrf_PLAT230_1.2DCE ; PROBLEM: Hirshfeld Test Diff for O14 -- C23 ... 2 su RESPONSE: This alert could be due to its proximity towards the disordered dichloroethane molecule. ; _vrf_PLAT432_1.2DCE ; PROBLEM: Short Inter X...Y Contact C9 .. Cl3' .. 2.75 Ang. RESPONSE: This is due to the disordered solvent molecule which has free space in the crystal lattice. Because of this, the C-Cl bond is free to rotate and the minor postion of the disordered chlorine atom Cl3' close to C9 atom. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULFONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, C2 H4 cl2' _chemical_formula_sum 'C28 H40 Cl2 O14 S' _chemical_formula_weight 703.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.39(2) _cell_length_b 14.35(3) _cell_length_c 17.54(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.55(2) _cell_angle_gamma 90.00 _cell_volume 3372(11) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 13.82 _cell_measurement_theta_max 22.03 _exptl_crystal_description FLAT _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.319 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8593 _exptl_absorpt_correction_T_max 0.9448 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26497 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10755 _reflns_number_gt 8320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.0829P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(6) _refine_ls_number_reflns 10755 _refine_ls_number_parameters 843 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.003 _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 0.64090(8) 0.15596(7) 0.10445(6) 0.0312(3) Uani 1 1 d . . . O1 O 0.6316(2) -0.1975(2) 0.36043(16) 0.0350(7) Uani 1 1 d . . . O2 O 0.4952(2) -0.0943(2) 0.27260(16) 0.0328(7) Uani 1 1 d . . . O3 O 0.5007(2) 0.0989(2) 0.27708(15) 0.0296(7) Uani 1 1 d . . . O4 O 0.6681(2) 0.12248(19) 0.18863(15) 0.0255(6) Uani 1 1 d . . . O5 O 0.7671(2) -0.04190(19) 0.14969(14) 0.0248(6) Uani 1 1 d . . . O6 O 0.7961(2) -0.1698(2) 0.27456(16) 0.0284(7) Uani 1 1 d . . . O7 O 0.6551(4) -0.1495(3) 0.4786(2) 0.0853(16) Uani 1 1 d . . . O8 O 0.3849(5) -0.1080(9) 0.3604(3) 0.231(6) Uani 1 1 d . . . O9 O 0.5079(2) 0.1397(3) 0.39967(17) 0.0442(8) Uani 1 1 d . . . O10 O 0.9222(2) -0.0168(2) 0.19387(18) 0.0385(8) Uani 1 1 d . . . O11 O 0.7601(3) -0.2727(2) 0.18344(19) 0.0470(9) Uani 1 1 d . . . O13 O 0.7326(3) 0.1879(3) 0.07778(19) 0.0677(12) Uani 1 1 d . . . O12 O 0.5896(3) 0.0860(2) 0.06489(16) 0.0407(8) Uani 1 1 d . . . O14 O 0.5918(3) 0.2479(3) -0.0491(2) 0.0675(11) Uani 1 1 d . . . C1 C 0.6552(3) -0.1071(3) 0.3342(2) 0.0278(10) Uani 1 1 d . . . H1 H 0.7026 -0.0774 0.3701 0.033 Uiso 1 1 calc R . . C2 C 0.5634(3) -0.0478(3) 0.3250(2) 0.0274(9) Uani 1 1 d . . . H2 H 0.5322 -0.0394 0.3744 0.033 Uiso 1 1 calc R . . C3 C 0.5895(3) 0.0454(3) 0.2917(2) 0.0255(10) Uani 1 1 d . . . H3 H 0.6355 0.0792 0.3262 0.031 Uiso 1 1 calc R . . C4 C 0.6361(3) 0.0317(3) 0.2141(2) 0.0247(9) Uani 1 1 d . . . H4 H 0.5883 0.0037 0.1775 0.030 Uiso 1 1 calc R . . C5 C 0.7295(3) -0.0287(3) 0.2243(2) 0.0236(9) Uani 1 1 d . . . H5 H 0.7793 0.0032 0.2568 0.028 Uiso 1 1 calc R . . C6 C 0.7041(3) -0.1210(3) 0.2578(2) 0.0285(10) Uani 1 1 d . . . H6 H 0.6609 -0.1570 0.2229 0.034 Uiso 1 1 calc R . . C7 C 0.6381(5) -0.2108(4) 0.4364(3) 0.0472(14) Uani 1 1 d . . . C8 C 0.6236(5) -0.3101(4) 0.4557(3) 0.0603(17) Uani 1 1 d . . . H8A H 0.6550 -0.3231 0.5044 0.090 Uiso 1 1 calc R . . H8B H 0.6530 -0.3485 0.4175 0.090 Uiso 1 1 calc R . . H8C H 0.5535 -0.3233 0.4578 0.090 Uiso 1 1 calc R . . C9 C 0.4071(5) -0.1198(7) 0.2978(4) 0.101(3) Uani 1 1 d . . . C10 C 0.3463(5) -0.1620(9) 0.2347(4) 0.137(5) Uani 1 1 d . . . H10A H 0.3014 -0.2071 0.2551 0.205 Uiso 1 1 calc R . . H10B H 0.3896 -0.1920 0.1995 0.205 Uiso 1 1 calc R . . H10C H 0.3087 -0.1142 0.2086 0.205 Uiso 1 1 calc R . . C11 C 0.4671(3) 0.1458(4) 0.3391(3) 0.0371(11) Uani 1 1 d . . . C12 C 0.3761(3) 0.1996(4) 0.3193(3) 0.0443(12) Uani 1 1 d . . . H12A H 0.3183 0.1639 0.3319 0.067 Uiso 1 1 calc R . . H12B H 0.3743 0.2129 0.2656 0.067 Uiso 1 1 calc R . . H12C H 0.3766 0.2570 0.3474 0.067 Uiso 1 1 calc R . . C13 C 0.8665(3) -0.0347(3) 0.1419(3) 0.0296(10) Uani 1 1 d . . . C14 C 0.8938(4) -0.0460(4) 0.0617(3) 0.0463(13) Uani 1 1 d . . . H14A H 0.9648 -0.0532 0.0589 0.069 Uiso 1 1 calc R . . H14B H 0.8731 0.0081 0.0332 0.069 Uiso 1 1 calc R . . H14C H 0.8612 -0.1001 0.0407 0.069 Uiso 1 1 calc R . . C15 C 0.8140(4) -0.2463(3) 0.2345(2) 0.0295(10) Uani 1 1 d . . . C16 C 0.9051(4) -0.2934(3) 0.2609(3) 0.0440(12) Uani 1 1 d . . . H16A H 0.9030 -0.3574 0.2449 0.066 Uiso 1 1 calc R . . H16B H 0.9102 -0.2905 0.3155 0.066 Uiso 1 1 calc R . . H16C H 0.9619 -0.2633 0.2396 0.066 Uiso 1 1 calc R . . C17 C 0.5650(4) 0.2504(4) 0.1232(3) 0.0577(15) Uani 1 1 d . . . H17A H 0.5300 0.2371 0.1696 0.069 Uiso 1 1 calc R . . H17B H 0.6080 0.3036 0.1336 0.069 Uiso 1 1 calc R . . C18 C 0.4881(4) 0.2794(3) 0.0630(3) 0.0437(13) Uani 1 1 d . . . C19 C 0.3914(4) 0.2193(4) 0.0578(3) 0.0495(13) Uani 1 1 d . . . H19A H 0.4022 0.1629 0.0286 0.059 Uiso 1 1 calc R . . H19B H 0.3695 0.2022 0.1082 0.059 Uiso 1 1 calc R . . C20 C 0.3160(4) 0.2817(4) 0.0179(3) 0.0515(14) Uani 1 1 d . . . H20A H 0.2612 0.2965 0.0508 0.062 Uiso 1 1 calc R . . H20B H 0.2897 0.2531 -0.0285 0.062 Uiso 1 1 calc R . . C21 C 0.3786(4) 0.3702(4) 0.0000(3) 0.0391(12) Uani 1 1 d . . . H21 H 0.3386 0.4262 -0.0104 0.047 Uiso 1 1 calc R . . C22 C 0.4444(5) 0.3435(5) -0.0624(3) 0.0622(17) Uani 1 1 d . . . H22A H 0.4759 0.3977 -0.0844 0.075 Uiso 1 1 calc R . . H22B H 0.4077 0.3100 -0.1022 0.075 Uiso 1 1 calc R . . C23 C 0.5192(4) 0.2825(4) -0.0233(3) 0.0483(13) Uani 1 1 d . . . C24 C 0.4498(4) 0.3782(4) 0.0709(3) 0.0528(14) Uani 1 1 d . . . C25 C 0.3996(5) 0.3909(4) 0.1440(3) 0.0573(15) Uani 1 1 d . . . H25A H 0.3556 0.3393 0.1523 0.086 Uiso 1 1 calc R . . H25B H 0.3618 0.4477 0.1424 0.086 Uiso 1 1 calc R . . H25C H 0.4487 0.3940 0.1847 0.086 Uiso 1 1 calc R . . C26 C 0.5297(5) 0.4527(4) 0.0599(4) 0.0667(17) Uani 1 1 d . . . H26A H 0.4983 0.5124 0.0534 0.100 Uiso 1 1 calc R . . H26B H 0.5671 0.4383 0.0155 0.100 Uiso 1 1 calc R . . H26C H 0.5739 0.4543 0.1039 0.100 Uiso 1 1 calc R . . S1' S 0.86476(7) 0.13191(6) 0.39117(5) 0.0226(2) Uani 1 1 d . . . O1' O 1.0000(2) 0.1897(2) 0.22362(15) 0.0293(7) Uani 1 1 d . . . O2' O 1.0109(2) 0.3828(2) 0.22918(16) 0.0327(7) Uani 1 1 d . . . O3' O 0.8768(2) 0.4870(2) 0.13492(17) 0.0382(8) Uani 1 1 d . . . O4' O 0.7097(2) 0.46386(19) 0.22117(16) 0.0291(7) Uani 1 1 d . . . O5' O 0.7339(2) 0.33691(19) 0.34779(14) 0.0241(6) Uani 1 1 d . . . O6' O 0.82957(19) 0.17031(18) 0.31078(14) 0.0229(6) Uani 1 1 d . . . O7' O 1.0001(2) 0.1542(3) 0.09975(17) 0.0448(9) Uani 1 1 d . . . O8' O 1.1412(2) 0.3277(2) 0.1667(2) 0.0527(9) Uani 1 1 d . . . O9' O 0.8039(5) 0.4523(3) 0.0247(2) 0.103(2) Uani 1 1 d . . . O10' O 0.5786(3) 0.3128(3) 0.30184(19) 0.0496(9) Uani 1 1 d . . . O11' O 0.7396(3) 0.5618(2) 0.31909(18) 0.0431(8) Uani 1 1 d . . . O12' O 0.8861(2) 0.2062(2) 0.44080(15) 0.0371(7) Uani 1 1 d . . . O13' O 0.7909(2) 0.0660(2) 0.40913(15) 0.0348(7) Uani 1 1 d . . . O14' O 1.1676(3) 0.1363(2) 0.4112(2) 0.0587(9) Uani 1 1 d . . . C1' C 0.9138(3) 0.2460(3) 0.2089(2) 0.0257(10) Uani 1 1 d . . . H1' H 0.8684 0.2137 0.1730 0.031 Uiso 1 1 calc R . . C2' C 0.9437(4) 0.3382(3) 0.1757(2) 0.0313(10) Uani 1 1 d . . . H2' H 0.9762 0.3288 0.1269 0.038 Uiso 1 1 calc R . . C3' C 0.8513(4) 0.3983(3) 0.1646(2) 0.0299(10) Uani 1 1 d . . . H3' H 0.8052 0.3673 0.1284 0.036 Uiso 1 1 calc R . . C4' C 0.7991(3) 0.4132(3) 0.2381(2) 0.0216(9) Uani 1 1 d . . . H4' H 0.8420 0.4494 0.2732 0.026 Uiso 1 1 calc R . . C5' C 0.7738(3) 0.3204(3) 0.2743(2) 0.0244(9) Uani 1 1 d . . . H5' H 0.7233 0.2887 0.2422 0.029 Uiso 1 1 calc R . . C6' C 0.8634(3) 0.2593(3) 0.2831(2) 0.0207(9) Uani 1 1 d . . . H6' H 0.9106 0.2868 0.3204 0.025 Uiso 1 1 calc R . . C7' C 1.0379(3) 0.1472(3) 0.1622(2) 0.0331(10) Uani 1 1 d . . . C8' C 1.1305(4) 0.0949(4) 0.1823(3) 0.0494(14) Uani 1 1 d . . . H8D H 1.1607 0.0734 0.1366 0.074 Uiso 1 1 calc R . . H8E H 1.1144 0.0426 0.2137 0.074 Uiso 1 1 calc R . . H8F H 1.1762 0.1351 0.2097 0.074 Uiso 1 1 calc R . . C9' C 1.1094(4) 0.3663(3) 0.2203(3) 0.0461(13) Uani 1 1 d . . . C10' C 1.1676(4) 0.4026(4) 0.2853(4) 0.0636(16) Uani 1 1 d . . . H10D H 1.1778 0.3540 0.3224 0.095 Uiso 1 1 calc R . . H10E H 1.1322 0.4533 0.3079 0.095 Uiso 1 1 calc R . . H10F H 1.2311 0.4243 0.2684 0.095 Uiso 1 1 calc R . . C11' C 0.8453(5) 0.5076(4) 0.0638(3) 0.0484(15) Uani 1 1 d . . . C12' C 0.8696(5) 0.6031(4) 0.0435(3) 0.0611(17) Uani 1 1 d . . . H12D H 0.9268 0.6034 0.0118 0.092 Uiso 1 1 calc R . . H12E H 0.8841 0.6383 0.0891 0.092 Uiso 1 1 calc R . . H12F H 0.8138 0.6307 0.0164 0.092 Uiso 1 1 calc R . . C13' C 0.6342(3) 0.3287(3) 0.3548(2) 0.0320(11) Uani 1 1 d . . . C14' C 0.6060(4) 0.3474(4) 0.4343(3) 0.0437(13) Uani 1 1 d . . . H14D H 0.6052 0.4135 0.4430 0.066 Uiso 1 1 calc R . . H14E H 0.6536 0.3187 0.4688 0.066 Uiso 1 1 calc R . . H14F H 0.5408 0.3223 0.4427 0.066 Uiso 1 1 calc R . . C15' C 0.6894(4) 0.5393(3) 0.2648(3) 0.0333(11) Uani 1 1 d . . . C16' C 0.5962(4) 0.5853(4) 0.2356(3) 0.0421(12) Uani 1 1 d . . . H16D H 0.5771 0.6332 0.2706 0.063 Uiso 1 1 calc R . . H16E H 0.5437 0.5399 0.2309 0.063 Uiso 1 1 calc R . . H16F H 0.6077 0.6124 0.1867 0.063 Uiso 1 1 calc R . . C17' C 0.9759(3) 0.0755(3) 0.3695(2) 0.0346(10) Uani 1 1 d . . . H17C H 0.9606 0.0269 0.3325 0.042 Uiso 1 1 calc R . . H17D H 1.0193 0.1200 0.3454 0.042 Uiso 1 1 calc R . . C18' C 1.0331(3) 0.0317(3) 0.4366(2) 0.0310(10) Uani 1 1 d . . . C19' C 0.9961(4) 0.0462(4) 0.5188(3) 0.0549(15) Uani 1 1 d . . . H19C H 0.9247 0.0362 0.5214 0.066 Uiso 1 1 calc R . . H19D H 1.0123 0.1080 0.5376 0.066 Uiso 1 1 calc R . . C20' C 1.0557(4) -0.0302(4) 0.5637(3) 0.0473(13) Uani 1 1 d . . . H20C H 1.0952 -0.0029 0.6051 0.057 Uiso 1 1 calc R . . H20D H 1.0110 -0.0763 0.5844 0.057 Uiso 1 1 calc R . . C21' C 1.1218(4) -0.0731(4) 0.5053(3) 0.0440(13) Uani 1 1 d . . . H21' H 1.1492 -0.1340 0.5201 0.053 Uiso 1 1 calc R . . C22' C 1.1987(4) -0.0026(4) 0.4870(3) 0.0432(12) Uani 1 1 d . . . H22C H 1.2521 -0.0297 0.4580 0.052 Uiso 1 1 calc R . . H22D H 1.2269 0.0259 0.5329 0.052 Uiso 1 1 calc R . . C23' C 1.1387(4) 0.0664(4) 0.4401(3) 0.0418(11) Uani 1 1 d . . . C24' C 1.0513(4) -0.0758(3) 0.4332(3) 0.0406(12) Uani 1 1 d . . . C25' C 0.9587(5) -0.1315(4) 0.4409(4) 0.073(2) Uani 1 1 d . . . H25D H 0.9144 -0.1196 0.3981 0.109 Uiso 1 1 calc R . . H25E H 0.9266 -0.1144 0.4871 0.109 Uiso 1 1 calc R . . H25F H 0.9753 -0.1966 0.4424 0.109 Uiso 1 1 calc R . . C26' C 1.1049(5) -0.1027(5) 0.3605(3) 0.0675(19) Uani 1 1 d . . . H26D H 1.1222 -0.1676 0.3624 0.101 Uiso 1 1 calc R . . H26E H 1.1645 -0.0661 0.3564 0.101 Uiso 1 1 calc R . . H26F H 1.0617 -0.0913 0.3169 0.101 Uiso 1 1 calc R . . Cl1 Cl 0.12080(17) 0.57910(13) 0.13559(11) 0.0861(6) Uani 1 1 d . . . Cl2 Cl 0.09668(13) 0.80875(13) 0.13697(10) 0.0737(5) Uani 1 1 d . . . C27 C 0.2096(5) 0.6590(5) 0.1030(4) 0.0690(17) Uani 1 1 d . . . H27A H 0.2528 0.6779 0.1454 0.083 Uiso 1 1 calc R . . H27B H 0.2507 0.6286 0.0656 0.083 Uiso 1 1 calc R . . C28 C 0.1626(4) 0.7428(4) 0.0680(3) 0.0544(14) Uani 1 1 d . . . H28A H 0.1166 0.7239 0.0272 0.065 Uiso 1 1 calc R . . H28B H 0.2138 0.7816 0.0461 0.065 Uiso 1 1 calc R . . Cl3 Cl 0.19985(17) 0.64442(13) 0.34305(12) 0.0868(6) Uani 0.88 1 d P A 1 Cl4 Cl 0.4012(10) 0.5158(13) 0.3645(7) 0.171(5) Uani 0.50 1 d P A 1 Cl3' Cl 0.3619(10) 0.7163(7) 0.3703(6) 0.060(3) Uani 0.13 1 d PD A 2 Cl4' Cl 0.4089(4) 0.5111(6) 0.3640(3) 0.0652(15) Uani 0.50 1 d P A 2 C29 C 0.2869(6) 0.6475(5) 0.4172(4) 0.094(3) Uani 1 1 d D . . H29A H 0.3379 0.6924 0.4044 0.112 Uiso 1 1 calc R A 1 H29B H 0.2541 0.6707 0.4620 0.112 Uiso 1 1 calc R A 1 C30 C 0.3369(5) 0.5592(5) 0.4377(3) 0.0722(19) Uani 1 1 d . A . H30A H 0.2872 0.5141 0.4528 0.087 Uiso 1 1 calc R B 1 H30B H 0.3822 0.5695 0.4809 0.087 Uiso 1 1 calc R 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 S1 0.0344(6) 0.0352(6) 0.0235(5) 0.0063(5) -0.0082(5) -0.0013(5) O1 0.051(2) 0.0295(16) 0.0241(15) 0.0034(13) 0.0038(14) -0.0067(15) O2 0.0233(17) 0.0431(18) 0.0318(16) -0.0075(14) -0.0011(13) -0.0088(14) O3 0.0195(15) 0.0438(18) 0.0255(15) -0.0042(13) 0.0014(12) 0.0050(13) O4 0.0295(16) 0.0230(14) 0.0237(14) 0.0012(12) -0.0051(12) 0.0001(13) O5 0.0262(16) 0.0284(15) 0.0196(14) -0.0025(12) -0.0004(12) 0.0022(13) O6 0.0289(17) 0.0248(15) 0.0311(15) -0.0008(13) -0.0039(13) 0.0039(13) O7 0.169(5) 0.059(3) 0.0283(19) -0.0048(18) 0.015(2) -0.007(3) O8 0.104(5) 0.503(17) 0.091(4) -0.153(7) 0.066(4) -0.180(8) O9 0.051(2) 0.052(2) 0.0294(17) -0.0035(17) -0.0003(15) 0.0197(18) O10 0.0284(18) 0.054(2) 0.0329(18) -0.0090(16) 0.0014(15) -0.0082(16) O11 0.050(2) 0.049(2) 0.042(2) -0.0150(17) -0.0029(17) 0.0103(18) O13 0.052(2) 0.106(3) 0.0445(19) 0.034(2) -0.0089(16) -0.025(2) O12 0.060(2) 0.0331(17) 0.0282(15) -0.0027(13) -0.0119(14) 0.0010(15) O14 0.071(3) 0.082(3) 0.050(2) 0.0022(19) -0.0005(19) 0.013(2) C1 0.037(3) 0.019(2) 0.028(2) 0.0017(18) -0.004(2) -0.0063(19) C2 0.025(2) 0.033(2) 0.024(2) 0.0001(18) 0.0012(18) -0.0041(19) C3 0.020(2) 0.031(2) 0.026(2) -0.0039(18) 0.0033(19) 0.0032(18) C4 0.024(2) 0.030(2) 0.020(2) 0.0012(18) -0.0044(18) 0.0003(18) C5 0.023(2) 0.025(2) 0.023(2) 0.0004(18) -0.0017(18) 0.0000(18) C6 0.027(2) 0.029(2) 0.030(2) -0.0008(19) 0.002(2) 0.0002(19) C7 0.067(4) 0.043(3) 0.033(3) 0.011(2) 0.023(3) 0.006(3) C8 0.094(5) 0.042(3) 0.046(3) 0.022(3) 0.032(3) 0.020(3) C9 0.048(4) 0.193(9) 0.063(4) -0.065(5) 0.029(3) -0.064(5) C10 0.060(5) 0.249(12) 0.102(5) -0.079(7) 0.028(4) -0.096(6) C11 0.027(2) 0.045(3) 0.040(3) -0.002(2) 0.010(2) 0.005(2) C12 0.030(3) 0.053(3) 0.050(3) 0.003(3) 0.014(2) 0.012(2) C13 0.024(3) 0.028(2) 0.037(3) 0.002(2) 0.000(2) -0.0033(19) C14 0.030(3) 0.070(4) 0.039(3) -0.013(2) 0.010(2) 0.006(3) C15 0.034(3) 0.029(2) 0.025(2) 0.0000(19) 0.003(2) -0.004(2) C16 0.044(3) 0.032(3) 0.055(3) -0.010(2) -0.002(2) 0.002(2) C17 0.067(4) 0.050(3) 0.054(3) -0.012(2) -0.034(3) 0.031(3) C18 0.042(3) 0.035(2) 0.054(3) 0.005(2) -0.021(2) 0.001(2) C19 0.055(3) 0.042(3) 0.052(3) 0.004(2) -0.008(2) -0.007(2) C20 0.037(3) 0.056(3) 0.061(3) 0.004(3) -0.005(2) -0.007(2) C21 0.040(3) 0.040(3) 0.037(3) -0.002(2) -0.015(2) 0.008(2) C22 0.059(4) 0.074(4) 0.053(3) 0.016(3) -0.008(3) 0.003(3) C23 0.041(3) 0.055(3) 0.049(3) 0.011(2) 0.009(2) 0.013(2) C24 0.044(3) 0.050(3) 0.064(3) 0.000(3) -0.015(3) 0.011(3) C25 0.058(4) 0.056(3) 0.058(3) 0.012(3) 0.001(3) 0.009(3) C26 0.062(4) 0.054(4) 0.082(4) 0.019(3) -0.030(3) -0.013(3) S1' 0.0236(5) 0.0225(5) 0.0215(5) 0.0012(4) -0.0033(4) -0.0005(4) O1' 0.0262(16) 0.0316(16) 0.0300(15) 0.0058(13) 0.0008(13) 0.0063(13) O2' 0.0277(18) 0.0342(17) 0.0365(17) 0.0006(14) 0.0035(14) -0.0059(14) O3' 0.0411(19) 0.0345(17) 0.0392(18) 0.0147(15) 0.0038(15) -0.0034(15) O4' 0.0326(17) 0.0247(16) 0.0294(15) 0.0020(13) -0.0089(13) 0.0003(13) O5' 0.0211(16) 0.0290(15) 0.0225(14) 0.0006(12) 0.0036(12) 0.0002(12) O6' 0.0224(15) 0.0252(15) 0.0207(13) -0.0001(11) -0.0054(11) 0.0001(12) O7' 0.050(2) 0.056(2) 0.0300(17) -0.0022(17) 0.0167(15) 0.0088(18) O8' 0.0354(18) 0.0481(19) 0.076(2) -0.0094(18) 0.0218(18) -0.0033(15) O9' 0.215(6) 0.056(3) 0.036(2) 0.017(2) -0.041(3) -0.014(3) O10' 0.0285(19) 0.083(3) 0.0369(19) -0.0051(19) -0.0025(16) -0.0009(19) O11' 0.051(2) 0.0408(19) 0.0363(18) -0.0118(16) -0.0106(16) 0.0128(17) O12' 0.054(2) 0.0343(16) 0.0219(14) -0.0026(13) -0.0109(13) 0.0041(15) O13' 0.0328(16) 0.0379(16) 0.0332(15) 0.0125(13) -0.0066(12) -0.0096(13) O14' 0.059(2) 0.050(2) 0.067(2) 0.0281(18) -0.0073(17) -0.0174(18) C1' 0.029(2) 0.028(2) 0.020(2) 0.0007(17) -0.0072(18) -0.0012(19) C2' 0.035(3) 0.034(2) 0.025(2) -0.0038(19) 0.004(2) -0.003(2) C3' 0.034(3) 0.035(2) 0.021(2) 0.0081(19) 0.000(2) 0.001(2) C4' 0.022(2) 0.024(2) 0.0182(19) 0.0000(17) -0.0100(17) 0.0024(18) C5' 0.026(2) 0.030(2) 0.0170(19) -0.0070(18) -0.0006(18) 0.0002(19) C6' 0.023(2) 0.0170(19) 0.022(2) 0.0012(17) 0.0039(18) -0.0037(17) C7' 0.039(3) 0.033(2) 0.028(2) 0.006(2) 0.011(2) 0.004(2) C8' 0.036(3) 0.054(3) 0.058(3) -0.003(3) 0.002(3) 0.008(3) C9' 0.030(3) 0.030(2) 0.079(4) 0.000(2) 0.006(3) -0.0034(19) C10' 0.033(3) 0.070(4) 0.088(4) -0.015(3) -0.011(3) -0.004(3) C11' 0.076(4) 0.044(3) 0.026(3) 0.009(2) 0.015(3) 0.025(3) C12' 0.081(4) 0.049(3) 0.055(3) 0.016(3) 0.027(3) 0.018(3) C13' 0.026(3) 0.043(3) 0.027(2) -0.005(2) -0.002(2) 0.002(2) C14' 0.031(3) 0.066(3) 0.034(2) -0.011(2) 0.009(2) -0.010(2) C15' 0.035(3) 0.031(3) 0.034(3) 0.004(2) 0.005(2) 0.008(2) C16' 0.037(3) 0.045(3) 0.045(3) 0.001(2) 0.001(2) 0.011(3) C17' 0.024(2) 0.050(3) 0.0297(19) 0.003(2) -0.0001(16) 0.0099(19) C18' 0.031(2) 0.037(2) 0.025(2) 0.0068(17) -0.0061(18) 0.0058(19) C19' 0.053(3) 0.076(4) 0.036(3) 0.014(2) -0.002(2) 0.032(3) C20' 0.047(3) 0.067(3) 0.028(2) 0.023(2) -0.013(2) 0.000(2) C21' 0.040(3) 0.040(3) 0.051(3) 0.019(2) -0.018(3) -0.002(2) C22' 0.036(3) 0.046(3) 0.046(3) 0.010(2) -0.020(2) 0.000(2) C23' 0.048(3) 0.036(3) 0.041(2) 0.009(2) -0.004(2) -0.002(2) C24' 0.047(3) 0.034(3) 0.041(3) 0.007(2) -0.016(2) -0.006(2) C25' 0.078(4) 0.060(4) 0.078(4) 0.022(3) -0.042(3) -0.037(3) C26' 0.084(5) 0.061(4) 0.056(3) -0.015(3) -0.028(3) 0.041(4) Cl1 0.1081(14) 0.0741(11) 0.0764(11) 0.0071(10) 0.0105(10) -0.0295(11) Cl2 0.0631(10) 0.0861(11) 0.0730(10) -0.0059(8) 0.0236(8) 0.0137(9) C27 0.055(3) 0.071(4) 0.080(4) -0.001(3) 0.012(3) -0.003(3) C28 0.054(3) 0.058(3) 0.052(3) 0.001(3) 0.011(3) -0.001(3) Cl3 0.1119(15) 0.0528(10) 0.0957(13) 0.0007(9) 0.0068(11) 0.0040(10) Cl4 0.120(8) 0.267(14) 0.126(8) -0.034(8) 0.019(6) 0.048(8) Cl3' 0.115(10) 0.031(5) 0.034(5) 0.025(4) -0.004(5) -0.018(6) Cl4' 0.033(2) 0.125(4) 0.038(2) -0.009(2) 0.0159(19) 0.003(2) C29 0.121(6) 0.078(5) 0.085(5) 0.000(4) 0.061(5) -0.032(5) C30 0.078(5) 0.089(5) 0.050(3) 0.011(3) 0.023(3) -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 S1 O12 1.392(4) . ? S1 O13 1.403(4) . ? S1 O4 1.586(4) . ? S1 C17 1.731(5) . ? O1 C7 1.347(6) . ? O1 C1 1.415(6) . ? O2 C9 1.323(7) . ? O2 C2 1.441(5) . ? O3 C11 1.366(5) . ? O3 C3 1.433(5) . ? O4 C4 1.445(5) . ? O5 C13 1.347(6) . ? O5 C5 1.427(5) . ? O6 C15 1.329(6) . ? O6 C6 1.440(6) . ? O7 C7 1.168(7) . ? O8 C9 1.158(7) . ? O9 C11 1.185(5) . ? O10 C13 1.190(5) . ? O11 C15 1.196(5) . ? O14 C23 1.191(6) . ? C1 C2 1.500(7) . ? C1 C6 1.520(6) . ? C1 H1 0.9800 . ? C2 C3 1.504(6) . ? C2 H2 0.9800 . ? C3 C4 1.526(6) . ? C3 H3 0.9800 . ? C4 C5 1.530(6) . ? C4 H4 0.9800 . ? C5 C6 1.492(6) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.479(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.486(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.476(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.472(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.460(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.513(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C24 1.515(8) . ? C18 C19 1.557(7) . ? C18 C23 1.582(8) . ? C19 C20 1.509(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.558(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.474(8) . ? C21 C24 1.551(7) . ? C21 H21 0.9800 . ? C22 C23 1.484(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.475(8) . ? C24 C26 1.529(8) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O12' 1.401(4) . ? S1' O13' 1.411(3) . ? S1' O6' 1.575(4) . ? S1' C17' 1.745(5) . ? O1' C7' 1.349(5) . ? O1' C1' 1.426(5) . ? O2' C9' 1.354(6) . ? O2' C2' 1.434(6) . ? O3' C11' 1.340(6) . ? O3' C3' 1.421(6) . ? O4' C15' 1.358(6) . ? O4' C4' 1.426(5) . ? O5' C13' 1.349(6) . ? O5' C5' 1.429(5) . ? O6' C6' 1.444(5) . ? O7' C7' 1.199(5) . ? O8' C9' 1.181(6) . ? O9' C11' 1.178(7) . ? O10' C13' 1.198(6) . ? O11' C15' 1.196(6) . ? O14' C23' 1.194(6) . ? C1' C6' 1.495(6) . ? C1' C2' 1.505(7) . ? C1' H1' 0.9800 . ? C2' C3' 1.517(7) . ? C2' H2' 0.9800 . ? C3' C4' 1.499(6) . ? C3' H3' 0.9800 . ? C4' C5' 1.518(6) . ? C4' H4' 0.9800 . ? C5' C6' 1.492(6) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.483(7) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.460(8) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C12' 1.455(8) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.479(6) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.490(7) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.523(6) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.499(7) . ? C18' C19' 1.551(7) . ? C18' C24' 1.564(7) . ? C19' C20' 1.557(7) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.504(8) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.485(7) . ? C21' C24' 1.558(7) . ? C21' H21' 0.9800 . ? C22' C23' 1.507(7) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C25' 1.484(8) . ? C24' C26' 1.531(8) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? Cl1 C27 1.759(7) . ? Cl2 C28 1.788(6) . ? C27 C28 1.484(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? Cl3 C29 1.724(9) . ? Cl4 C30 1.685(14) . ? Cl3' C29 1.646(11) . ? Cl4' C30 1.774(9) . ? C29 C30 1.473(11) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? 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 O12 S1 O13 119.6(3) . . ? O12 S1 O4 110.1(2) . . ? O13 S1 O4 103.2(2) . . ? O12 S1 C17 112.0(3) . . ? O13 S1 C17 109.3(3) . . ? O4 S1 C17 100.5(2) . . ? C7 O1 C1 116.3(4) . . ? C9 O2 C2 118.1(4) . . ? C11 O3 C3 114.3(3) . . ? C4 O4 S1 119.9(3) . . ? C13 O5 C5 117.2(3) . . ? C15 O6 C6 117.3(3) . . ? O1 C1 C2 111.4(4) . . ? O1 C1 C6 105.8(3) . . ? C2 C1 C6 110.5(4) . . ? O1 C1 H1 109.7 . . ? C2 C1 H1 109.7 . . ? C6 C1 H1 109.7 . . ? O2 C2 C1 108.0(4) . . ? O2 C2 C3 108.3(4) . . ? C1 C2 C3 110.4(4) . . ? O2 C2 H2 110.0 . . ? C1 C2 H2 110.0 . . ? C3 C2 H2 110.0 . . ? O3 C3 C2 110.2(4) . . ? O3 C3 C4 105.4(3) . . ? C2 C3 C4 109.7(3) . . ? O3 C3 H3 110.5 . . ? C2 C3 H3 110.5 . . ? C4 C3 H3 110.5 . . ? O4 C4 C3 107.0(3) . . ? O4 C4 C5 107.4(3) . . ? C3 C4 C5 108.7(3) . . ? O4 C4 H4 111.2 . . ? C3 C4 H4 111.2 . . ? C5 C4 H4 111.2 . . ? O5 C5 C6 109.5(3) . . ? O5 C5 C4 106.0(3) . . ? C6 C5 C4 110.8(3) . . ? O5 C5 H5 110.1 . . ? C6 C5 H5 110.1 . . ? C4 C5 H5 110.1 . . ? O6 C6 C5 108.0(4) . . ? O6 C6 C1 105.7(3) . . ? C5 C6 C1 109.9(4) . . ? O6 C6 H6 111.0 . . ? C5 C6 H6 111.0 . . ? C1 C6 H6 111.0 . . ? O7 C7 O1 121.7(5) . . ? O7 C7 C8 127.2(5) . . ? O1 C7 C8 111.0(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 122.0(5) . . ? O8 C9 C10 128.1(6) . . ? O2 C9 C10 109.9(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 121.6(4) . . ? O9 C11 C12 127.4(4) . . ? O3 C11 C12 111.0(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 122.6(4) . . ? O10 C13 C14 126.1(4) . . ? O5 C13 C14 111.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 123.0(4) . . ? O11 C15 C16 124.9(4) . . ? O6 C15 C16 112.1(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 118.4(4) . . ? C18 C17 H17A 107.7 . . ? S1 C17 H17A 107.7 . . ? C18 C17 H17B 107.7 . . ? S1 C17 H17B 107.7 . . ? H17A C17 H17B 107.1 . . ? C17 C18 C24 114.8(4) . . ? C17 C18 C19 116.0(4) . . ? C24 C18 C19 103.9(4) . . ? C17 C18 C23 118.9(5) . . ? C24 C18 C23 99.2(4) . . ? C19 C18 C23 101.5(4) . . ? C20 C19 C18 104.1(4) . . ? C20 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? C20 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 109.0 . . ? C19 C20 C21 102.8(4) . . ? C19 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? C19 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? C22 C21 C24 104.4(5) . . ? C22 C21 C20 105.8(5) . . ? C24 C21 C20 102.8(4) . . ? C22 C21 H21 114.2 . . ? C24 C21 H21 114.2 . . ? C20 C21 H21 114.2 . . ? C21 C22 C23 102.7(5) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? O14 C23 C22 128.1(5) . . ? O14 C23 C18 126.2(5) . . ? C22 C23 C18 105.5(4) . . ? C25 C24 C18 111.0(5) . . ? C25 C24 C26 111.1(5) . . ? C18 C24 C26 113.8(5) . . ? C25 C24 C21 114.9(5) . . ? C18 C24 C21 93.5(4) . . ? C26 C24 C21 111.6(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12' S1' O13' 120.3(2) . . ? O12' S1' O6' 110.0(2) . . ? O13' S1' O6' 103.88(18) . . ? O12' S1' C17' 109.1(2) . . ? O13' S1' C17' 110.2(2) . . ? O6' S1' C17' 101.77(18) . . ? C7' O1' C1' 115.6(3) . . ? C9' O2' C2' 116.3(4) . . ? C11' O3' C3' 117.8(4) . . ? C15' O4' C4' 118.0(3) . . ? C13' O5' C5' 117.6(3) . . ? C6' O6' S1' 121.4(3) . . ? O1' C1' C6' 107.2(3) . . ? O1' C1' C2' 110.2(4) . . ? C6' C1' C2' 110.8(4) . . ? O1' C1' H1' 109.5 . . ? C6' C1' H1' 109.5 . . ? C2' C1' H1' 109.5 . . ? O2' C2' C1' 108.0(4) . . ? O2' C2' C3' 109.0(4) . . ? C1' C2' C3' 109.0(4) . . ? O2' C2' H2' 110.3 . . ? C1' C2' H2' 110.3 . . ? C3' C2' H2' 110.3 . . ? O3' C3' C4' 108.0(4) . . ? O3' C3' C2' 110.7(4) . . ? C4' C3' C2' 111.7(3) . . ? O3' C3' H3' 108.8 . . ? C4' C3' H3' 108.8 . . ? C2' C3' H3' 108.8 . . ? O4' C4' C3' 107.6(3) . . ? O4' C4' C5' 109.8(3) . . ? C3' C4' C5' 110.4(3) . . ? O4' C4' H4' 109.7 . . ? C3' C4' H4' 109.7 . . ? C5' C4' H4' 109.7 . . ? O5' C5' C6' 108.8(3) . . ? O5' C5' C4' 109.0(3) . . ? C6' C5' C4' 111.8(3) . . ? O5' C5' H5' 109.1 . . ? C6' C5' H5' 109.1 . . ? C4' C5' H5' 109.1 . . ? O6' C6' C5' 107.2(3) . . ? O6' C6' C1' 109.4(3) . . ? C5' C6' C1' 111.4(3) . . ? O6' C6' H6' 109.6 . . ? C5' C6' H6' 109.6 . . ? C1' C6' H6' 109.6 . . ? O7' C7' O1' 122.2(4) . . ? O7' C7' C8' 126.1(4) . . ? O1' C7' C8' 111.7(4) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 123.2(5) . . ? O8' C9' C10' 126.4(5) . . ? O2' C9' C10' 110.4(5) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? O9' C11' O3' 121.6(5) . . ? O9' C11' C12' 126.7(5) . . ? O3' C11' C12' 111.6(6) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O10' C13' O5' 122.8(4) . . ? O10' C13' C14' 126.6(5) . . ? O5' C13' C14' 110.5(4) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O4' 123.2(4) . . ? O11' C15' C16' 127.0(4) . . ? O4' C15' C16' 109.8(4) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 116.0(3) . . ? C18' C17' H17C 108.3 . . ? S1' C17' H17C 108.3 . . ? C18' C17' H17D 108.3 . . ? S1' C17' H17D 108.3 . . ? H17C C17' H17D 107.4 . . ? C23' C18' C17' 110.4(4) . . ? C23' C18' C19' 104.1(4) . . ? C17' C18' C19' 119.8(4) . . ? C23' C18' C24' 100.5(4) . . ? C17' C18' C24' 116.9(4) . . ? C19' C18' C24' 102.8(4) . . ? C18' C19' C20' 101.8(4) . . ? C18' C19' H19C 111.4 . . ? C20' C19' H19C 111.4 . . ? C18' C19' H19D 111.4 . . ? C20' C19' H19D 111.4 . . ? H19C C19' H19D 109.3 . . ? C21' C20' C19' 104.2(4) . . ? C21' C20' H20C 110.9 . . ? C19' C20' H20C 110.9 . . ? C21' C20' H20D 110.9 . . ? C19' C20' H20D 110.9 . . ? H20C C20' H20D 108.9 . . ? C22' C21' C20' 107.0(5) . . ? C22' C21' C24' 104.6(4) . . ? C20' C21' C24' 102.0(4) . . ? C22' C21' H21' 114.0 . . ? C20' C21' H21' 114.0 . . ? C24' C21' H21' 114.0 . . ? C21' C22' C23' 101.7(4) . . ? C21' C22' H22C 111.4 . . ? C23' C22' H22C 111.4 . . ? C21' C22' H22D 111.4 . . ? C23' C22' H22D 111.4 . . ? H22C C22' H22D 109.3 . . ? O14' C23' C18' 125.4(5) . . ? O14' C23' C22' 127.6(5) . . ? C18' C23' C22' 107.0(4) . . ? C25' C24' C26' 110.6(5) . . ? C25' C24' C21' 115.5(4) . . ? C26' C24' C21' 113.3(5) . . ? C25' C24' C18' 113.4(5) . . ? C26' C24' C18' 111.0(4) . . ? C21' C24' C18' 92.1(4) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C28 C27 Cl1 112.3(5) . . ? C28 C27 H27A 109.1 . . ? Cl1 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? Cl1 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 Cl2 111.2(4) . . ? C27 C28 H28A 109.4 . . ? Cl2 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? Cl2 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 Cl3' 111.0(7) . . ? C30 C29 Cl3 117.1(6) . . ? Cl3' C29 Cl3 92.7(6) . . ? C30 C29 H29A 108.0 . . ? Cl3' C29 H29A 16.7 . . ? Cl3 C29 H29A 108.0 . . ? C30 C29 H29B 108.0 . . ? Cl3' C29 H29B 119.7 . . ? Cl3 C29 H29B 108.0 . . ? H29A C29 H29B 107.3 . . ? C29 C30 Cl4 111.8(7) . . ? C29 C30 Cl4' 114.1(5) . . ? Cl4 C30 Cl4' 2.8(7) . . ? C29 C30 H30A 109.3 . . ? Cl4 C30 H30A 109.3 . . ? Cl4' C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? Cl4 C30 H30B 109.3 . . ? Cl4' C30 H30B 106.8 . . ? H30A C30 H30B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.496 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.062 #===END data_1.2DCM _database_code_depnum_ccdc_archive 'CCDC 846749' #TrackingRef '- KM_CIF.cif' # start Validation Reply Form _vrf_PLAT111_1.2DCM ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 93 PerFi RESPONSE: The host molecule has a chiral camphorsulfonyl group, so there can never be the presence of centre of symmetry. The centrosymmetric relation is detected by ADDSYM for the diastereomers excluding camphorsulfonyl moiety. ; _vrf_PLAT220_1.2DCM ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.02 Ratio RESPONSE: Higher anisotropies for the terminal C atoms of the host contribute to this alert. The high ratio could be due to their (C atoms) freedom of libration and their proximity to the cavity containing guest molecules with low occupancies. ; _vrf_PLAT222_1.2DCM ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.43 Ratio RESPONSE: The alert for H atoms is because their thermal parameters come from C atoms to which they are attached having higher thermal anisotropies. ; _vrf_PLAT230_1.2DCM ; PROBLEM: Hirshfeld Test Diff for C18 -- C24 .. 9.6 su RESPONSE: This alert could be due to the high ADP of the other atoms in this camphorsulphonyl moiety which is contaminating components of ADP along C18-C24 bond. ; _vrf_PLAT241_1.2DCM ; PROBLEM: Check High Ueq as Compared to Neighbors for C19 RESPONSE: This alert could be due to proximity of the camphor sulphonyl moiety to the edge of the void containing DCM molecule. ; _vrf_PLAT340_1.2DCM ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0109 Ang RESPONSE: This type alerts do occur in the crystal structure of inclusion complexes where atoms or the group of atoms show statistical disorder due to their proximity to the guest molecules or disordered guest molecules. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; '6(4)-O-CAMPHORSULFONYL 1,2,3,4(6),5-O-PENTA ACETYL MYO-INOSITOL' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 O14 S, C H2 Cl2' _chemical_formula_sum 'C27 H38 Cl2 O14 S' _chemical_formula_weight 689.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.463(2) _cell_length_b 14.451(3) _cell_length_c 17.848(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.363(3) _cell_angle_gamma 90.00 _cell_volume 3471.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5442 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.46 _exptl_crystal_description FLAT _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8892 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'CCD Area Detector' _diffrn_measurement_device 'BRUKER SMART APEX' _diffrn_measurement_method 'Omega and phi Scan' _diffrn_detector_area_resol_mean ? _chemical_absolute_configuration SYN _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25077 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11847 _reflns_number_gt 9192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, ORTEP3,MERCURY1.2.1' _computing_publication_material 'SHELXTL, PLATON' _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^)+(0.1310P)^2^+2.4768P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(11) _refine_ls_number_reflns 11847 _refine_ls_number_parameters 807 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 0.13584(9) 0.68615(10) 0.11352(7) 0.0276(3) Uani 1 1 d . . . O1 O 0.1278(3) 0.3172(3) 0.3569(2) 0.0406(11) Uani 1 1 d . . . O2 O -0.0094(3) 0.4211(3) 0.2703(2) 0.0381(10) Uani 1 1 d . . . O3 O -0.0046(3) 0.6160(3) 0.2769(2) 0.0325(10) Uani 1 1 d . . . O4 O 0.1677(3) 0.6427(3) 0.1928(2) 0.0250(8) Uani 1 1 d . . . O5 O 0.2642(2) 0.4802(3) 0.1500(2) 0.0261(9) Uani 1 1 d . . . O6 O 0.2932(3) 0.3484(3) 0.2727(2) 0.0282(9) Uani 1 1 d . . . O7 O 0.1584(7) 0.3632(5) 0.4740(3) 0.101(3) Uani 1 1 d . . . O8 O -0.1263(5) 0.4164(10) 0.3544(4) 0.159(5) Uani 1 1 d . . . O9 O -0.0057(3) 0.6460(4) 0.4000(2) 0.0520(13) Uani 1 1 d . . . O10 O 0.4210(3) 0.5050(4) 0.1933(3) 0.0484(12) Uani 1 1 d . . . O11 O 0.2583(4) 0.2447(4) 0.1810(3) 0.0553(14) Uani 1 1 d . . . O12 O 0.1091(4) 0.6156(3) 0.0638(2) 0.0448(12) Uani 1 1 d . . . O13 O 0.2173(3) 0.7453(3) 0.0970(2) 0.0407(11) Uani 1 1 d . . . O14 O -0.0653(5) 0.9189(5) 0.1706(4) 0.096(2) Uani 1 1 d . . . C1 C 0.1507(4) 0.4101(4) 0.3309(3) 0.0297(13) Uani 1 1 d . . . H1 H 0.1962 0.4403 0.3669 0.036 Uiso 1 1 calc R . . C2 C 0.0583(4) 0.4658(4) 0.3222(3) 0.0307(14) Uani 1 1 d . . . H2 H 0.0271 0.4730 0.3710 0.037 Uiso 1 1 calc R . . C3 C 0.0827(4) 0.5619(4) 0.2893(3) 0.0270(13) Uani 1 1 d . . . H3 H 0.1273 0.5948 0.3244 0.032 Uiso 1 1 calc R . . C4 C 0.1334(4) 0.5516(4) 0.2154(3) 0.0247(12) Uani 1 1 d . . . H4 H 0.0873 0.5260 0.1775 0.030 Uiso 1 1 calc R . . C5 C 0.2259(4) 0.4908(4) 0.2233(3) 0.0259(13) Uani 1 1 d . . . H5 H 0.2754 0.5223 0.2554 0.031 Uiso 1 1 calc R . . C6 C 0.2025(4) 0.3965(4) 0.2570(3) 0.0295(14) Uani 1 1 d . . . H6 H 0.1603 0.3605 0.2222 0.035 Uiso 1 1 calc R . . C7 C 0.1374(7) 0.3022(6) 0.4315(5) 0.067(3) Uani 1 1 d . . . C8 C 0.1231(8) 0.2076(6) 0.4527(5) 0.082(3) Uani 1 1 d . . . H8A H 0.1472 0.1985 0.5032 0.124 Uiso 1 1 calc R . . H8B H 0.1590 0.1680 0.4196 0.124 Uiso 1 1 calc R . . H8C H 0.0537 0.1927 0.4494 0.124 Uiso 1 1 calc R . . C9 C -0.1023(5) 0.4024(8) 0.2933(5) 0.070(3) Uani 1 1 d . . . C10 C -0.1591(6) 0.3493(10) 0.2359(6) 0.107(4) Uani 1 1 d . . . H10A H -0.2225 0.3323 0.2552 0.161 Uiso 1 1 calc R . . H10B H -0.1229 0.2944 0.2234 0.161 Uiso 1 1 calc R . . H10C H -0.1688 0.3866 0.1918 0.161 Uiso 1 1 calc R . . C11 C -0.0422(4) 0.6588(5) 0.3391(3) 0.0359(14) Uani 1 1 d . . . C12 C -0.1303(5) 0.7166(6) 0.3197(5) 0.057(2) Uani 1 1 d . . . H12A H -0.1831 0.7023 0.3529 0.086 Uiso 1 1 calc R . . H12B H -0.1516 0.7042 0.2690 0.086 Uiso 1 1 calc R . . H12C H -0.1131 0.7808 0.3246 0.086 Uiso 1 1 calc R . . C13 C 0.3638(4) 0.4904(5) 0.1407(3) 0.0338(14) Uani 1 1 d . . . C14 C 0.3884(5) 0.4792(6) 0.0602(4) 0.0506(19) Uani 1 1 d . . . H14A H 0.4589 0.4850 0.0546 0.076 Uiso 1 1 calc R . . H14B H 0.3550 0.5263 0.0311 0.076 Uiso 1 1 calc R . . H14C H 0.3671 0.4193 0.0430 0.076 Uiso 1 1 calc R . . C15 C 0.3125(5) 0.2693(5) 0.2318(4) 0.0361(15) Uani 1 1 d . . . C16 C 0.4049(5) 0.2244(5) 0.2608(4) 0.0443(17) Uani 1 1 d . . . H16A H 0.4055 0.2249 0.3146 0.066 Uiso 1 1 calc R . . H16B H 0.4616 0.2577 0.2434 0.066 Uiso 1 1 calc R . . H16C H 0.4074 0.1617 0.2433 0.066 Uiso 1 1 calc R . . C17 C 0.0323(4) 0.7558(5) 0.1364(3) 0.0307(13) Uani 1 1 d . . . H17A H -0.0175 0.7158 0.1579 0.037 Uiso 1 1 calc R . . H17B H 0.0536 0.7988 0.1752 0.037 Uiso 1 1 calc R . . C18 C -0.0167(5) 0.8101(5) 0.0748(4) 0.0476(18) Uani 1 1 d . . . C19 C 0.0503(8) 0.8571(11) 0.0156(7) 0.172(7) Uani 1 1 d U . . H19A H 0.0895 0.9064 0.0383 0.207 Uiso 1 1 calc R . . H19B H 0.0949 0.8123 -0.0062 0.207 Uiso 1 1 calc R . . C20 C -0.0222(11) 0.8961(14) -0.0447(7) 0.198(7) Uani 1 1 d U . . H20A H -0.0164 0.9628 -0.0487 0.238 Uiso 1 1 calc R . . H20B H -0.0111 0.8684 -0.0932 0.238 Uiso 1 1 calc R . . C21 C -0.1213(9) 0.8685(11) -0.0147(6) 0.142(4) Uani 1 1 d U . . H21 H -0.1744 0.8675 -0.0532 0.170 Uiso 1 1 calc R . . C22 C -0.1438(5) 0.9294(7) 0.0499(5) 0.085(3) Uani 1 1 d U . . H22A H -0.2127 0.9238 0.0641 0.102 Uiso 1 1 calc R . . H22B H -0.1293 0.9937 0.0390 0.102 Uiso 1 1 calc R . . C23 C -0.0742(5) 0.8915(6) 0.1098(5) 0.0610(19) Uani 1 1 d U . . C24 C -0.1000(8) 0.7667(9) 0.0232(5) 0.107(3) Uani 1 1 d U . . C25 C -0.0723(10) 0.6825(13) -0.0280(7) 0.189(8) Uani 1 1 d U . . H25A H -0.0608 0.6287 0.0026 0.283 Uiso 1 1 calc R . . H25B H -0.0132 0.6968 -0.0548 0.283 Uiso 1 1 calc R . . H25C H -0.1259 0.6705 -0.0630 0.283 Uiso 1 1 calc R . . C26 C -0.1835(7) 0.7300(11) 0.0681(8) 0.135(4) Uani 1 1 d U . . H26A H -0.2396 0.7175 0.0355 0.202 Uiso 1 1 calc R . . H26B H -0.2016 0.7751 0.1049 0.202 Uiso 1 1 calc R . . H26C H -0.1629 0.6740 0.0928 0.202 Uiso 1 1 calc R . . S1' S 0.36491(9) 0.65043(9) 0.39036(7) 0.0269(3) Uani 1 1 d . . . O1' O 0.5057(3) 0.7160(3) 0.2246(2) 0.0328(10) Uani 1 1 d . . . O2' O 0.5137(3) 0.9093(3) 0.2294(2) 0.0373(10) Uani 1 1 d . . . O3' O 0.3809(3) 1.0143(3) 0.1459(2) 0.0397(10) Uani 1 1 d . . . O4' O 0.2070(3) 0.9827(3) 0.2252(2) 0.0323(10) Uani 1 1 d . . . O5' O 0.2372(3) 0.8580(3) 0.3513(2) 0.0263(9) Uani 1 1 d . . . O6' O 0.3340(3) 0.6903(3) 0.30999(19) 0.0268(8) Uani 1 1 d . . . O7' O 0.5014(4) 0.6785(4) 0.1025(2) 0.0509(12) Uani 1 1 d . . . O8' O 0.6366(4) 0.8836(7) 0.1496(5) 0.128(4) Uani 1 1 d . . . O9' O 0.3438(6) 0.9796(5) 0.0278(3) 0.093(2) Uani 1 1 d . . . O10' O 0.0858(3) 0.8109(4) 0.3115(3) 0.0551(15) Uani 1 1 d . . . O11' O 0.2331(3) 1.0843(4) 0.3182(2) 0.0498(12) Uani 1 1 d . . . O12' O 0.3871(4) 0.7251(3) 0.4410(2) 0.0454(12) Uani 1 1 d . . . O13' O 0.2875(3) 0.5868(4) 0.4062(2) 0.0429(11) Uani 1 1 d . . . O14' O 0.6681(4) 0.6523(4) 0.4127(3) 0.0734(16) Uani 1 1 d . . . C1' C 0.4158(4) 0.7705(4) 0.2106(3) 0.0288(13) Uani 1 1 d . . . H1' H 0.3708 0.7377 0.1758 0.035 Uiso 1 1 calc R . . C2' C 0.4442(4) 0.8621(4) 0.1784(3) 0.0308(14) Uani 1 1 d . . . H2' H 0.4751 0.8529 0.1298 0.037 Uiso 1 1 calc R . . C3' C 0.3519(4) 0.9237(4) 0.1685(3) 0.0315(14) Uani 1 1 d . . . H3' H 0.3060 0.8968 0.1311 0.038 Uiso 1 1 calc R . . C4' C 0.2994(4) 0.9361(4) 0.2436(3) 0.0248(12) Uani 1 1 d . . . H4' H 0.3401 0.9734 0.2784 0.030 Uiso 1 1 calc R . . C5' C 0.2759(4) 0.8422(4) 0.2777(3) 0.0254(13) Uani 1 1 d . . . H5' H 0.2258 0.8105 0.2464 0.030 Uiso 1 1 calc R . . C6' C 0.3677(4) 0.7816(4) 0.2862(3) 0.0275(13) Uani 1 1 d . . . H6' H 0.4148 0.8079 0.3231 0.033 Uiso 1 1 calc R . . C7' C 0.5403(4) 0.6711(5) 0.1644(4) 0.0412(16) Uani 1 1 d . . . C8' C 0.6283(5) 0.6136(6) 0.1841(4) 0.053(2) Uani 1 1 d . . . H8D H 0.6091 0.5648 0.2173 0.080 Uiso 1 1 calc R . . H8E H 0.6780 0.6514 0.2084 0.080 Uiso 1 1 calc R . . H8F H 0.6547 0.5873 0.1394 0.080 Uiso 1 1 calc R . . C9' C 0.6065(7) 0.9191(9) 0.2055(6) 0.091(4) Uani 1 1 d . . . C10' C 0.6674(6) 0.9739(10) 0.2630(5) 0.101(4) Uani 1 1 d . . . H10D H 0.7360 0.9563 0.2605 0.152 Uiso 1 1 calc R . . H10E H 0.6438 0.9612 0.3123 0.152 Uiso 1 1 calc R . . H10F H 0.6609 1.0389 0.2526 0.152 Uiso 1 1 calc R . . C11' C 0.3717(5) 1.0348(5) 0.0719(4) 0.0452(17) Uani 1 1 d . . . C12' C 0.4067(6) 1.1330(5) 0.0604(4) 0.0524(18) Uani 1 1 d . . . H12D H 0.4096 1.1457 0.0077 0.079 Uiso 1 1 calc R . . H12E H 0.4715 1.1406 0.0831 0.079 Uiso 1 1 calc R . . H12F H 0.3611 1.1751 0.0830 0.079 Uiso 1 1 calc R . . C13' C 0.1413(5) 0.8371(5) 0.3610(3) 0.0371(15) Uani 1 1 d . . . C14' C 0.1140(5) 0.8484(7) 0.4415(4) 0.054(2) Uani 1 1 d . . . H14D H 0.0526 0.8170 0.4501 0.081 Uiso 1 1 calc R . . H14E H 0.1066 0.9130 0.4526 0.081 Uiso 1 1 calc R . . H14F H 0.1655 0.8226 0.4733 0.081 Uiso 1 1 calc R . . C15' C 0.1835(5) 1.0569(4) 0.2666(3) 0.0338(14) Uani 1 1 d . . . C16' C 0.0894(5) 1.0993(5) 0.2390(4) 0.0489(18) Uani 1 1 d . . . H16D H 0.0680 1.1450 0.2743 0.073 Uiso 1 1 calc R . . H16E H 0.0393 1.0523 0.2335 0.073 Uiso 1 1 calc R . . H16F H 0.0997 1.1282 0.1914 0.073 Uiso 1 1 calc R . . C17' C 0.4759(5) 0.5928(6) 0.3692(3) 0.0471(18) Uani 1 1 d . . . H17C H 0.4607 0.5449 0.3325 0.057 Uiso 1 1 calc R . . H17D H 0.5202 0.6367 0.3460 0.057 Uiso 1 1 calc R . . C18' C 0.5316(4) 0.5478(4) 0.4369(3) 0.0359(14) Uani 1 1 d . . . C19' C 0.4934(6) 0.5638(6) 0.5204(4) 0.064(2) Uani 1 1 d . . . H19C H 0.5114 0.6248 0.5390 0.077 Uiso 1 1 calc R . . H19D H 0.4221 0.5557 0.5231 0.077 Uiso 1 1 calc R . . C20' C 0.5510(5) 0.4858(6) 0.5639(4) 0.060(2) Uani 1 1 d . . . H20C H 0.5908 0.5114 0.6049 0.072 Uiso 1 1 calc R . . H20D H 0.5055 0.4404 0.5836 0.072 Uiso 1 1 calc R . . C21' C 0.6158(4) 0.4435(5) 0.5057(4) 0.0455(16) Uani 1 1 d . . . H21' H 0.6430 0.3830 0.5202 0.055 Uiso 1 1 calc R . . C22' C 0.6948(5) 0.5142(5) 0.4869(4) 0.0561(17) Uani 1 1 d . . . H22C H 0.7227 0.5429 0.5318 0.067 Uiso 1 1 calc R . . H22D H 0.7478 0.4865 0.4586 0.067 Uiso 1 1 calc R . . C23' C 0.6365(5) 0.5820(4) 0.4406(4) 0.0445(14) Uani 1 1 d . . . C24' C 0.5493(5) 0.4405(5) 0.4345(4) 0.0571(18) Uani 1 1 d . . . C25' C 0.4514(6) 0.3853(6) 0.4453(6) 0.090(3) Uani 1 1 d . . . H25D H 0.4251 0.3994 0.4935 0.135 Uiso 1 1 calc R . . H25E H 0.4649 0.3202 0.4423 0.135 Uiso 1 1 calc R . . H25F H 0.4038 0.4022 0.4068 0.135 Uiso 1 1 calc R . . C26' C 0.6019(6) 0.4121(6) 0.3646(4) 0.074(2) Uani 1 1 d . . . H26D H 0.5644 0.4329 0.3214 0.110 Uiso 1 1 calc R . . H26E H 0.6078 0.3460 0.3633 0.110 Uiso 1 1 calc R . . H26F H 0.6668 0.4395 0.3647 0.110 Uiso 1 1 calc R . . C27 C 0.1553(8) 0.5651(8) 0.5562(5) 0.094(3) Uani 1 1 d . . . H27A H 0.2055 0.5253 0.5352 0.113 Uiso 1 1 calc R . . H27B H 0.1106 0.5842 0.5157 0.113 Uiso 1 1 calc R . . Cl1 Cl 0.0882(2) 0.5025(3) 0.62244(19) 0.1170(11) Uani 1 1 d . . . Cl2 Cl 0.2120(4) 0.6615(3) 0.5945(2) 0.1538(16) Uani 1 1 d . . . C28 C 0.3463(7) 0.7753(8) 0.9433(6) 0.089(3) Uani 1 1 d . . . H28A H 0.2986 0.8171 0.9651 0.106 Uiso 1 1 calc R . . H28B H 0.3928 0.7565 0.9828 0.106 Uiso 1 1 calc R . . Cl3 Cl 0.4088(2) 0.8324(2) 0.87667(18) 0.1048(10) Uani 1 1 d . . . Cl4 Cl 0.2826(3) 0.6761(3) 0.90891(18) 0.1170(11) 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 0.0299(7) 0.0329(8) 0.0198(7) -0.0004(6) -0.0018(5) 0.0030(6) O1 0.059(3) 0.036(2) 0.028(2) 0.008(2) 0.009(2) -0.003(2) O2 0.031(2) 0.046(3) 0.038(3) -0.004(2) 0.0029(18) -0.008(2) O3 0.027(2) 0.045(3) 0.025(2) -0.0078(19) -0.0038(17) 0.0079(18) O4 0.0275(18) 0.025(2) 0.0229(19) -0.0002(17) -0.0038(15) -0.0011(17) O5 0.0241(18) 0.031(2) 0.023(2) -0.0037(18) 0.0041(16) 0.0004(16) O6 0.031(2) 0.026(2) 0.027(2) -0.0009(18) -0.0016(17) 0.0040(17) O7 0.213(8) 0.058(4) 0.034(3) -0.004(3) 0.027(4) -0.012(5) O8 0.072(4) 0.313(14) 0.093(5) -0.099(7) 0.055(4) -0.097(7) O9 0.060(3) 0.064(3) 0.033(3) -0.007(3) 0.016(2) 0.020(3) O10 0.027(2) 0.078(3) 0.041(3) -0.005(2) 0.0039(19) -0.004(2) O11 0.062(3) 0.050(3) 0.052(3) -0.031(3) -0.016(2) 0.014(2) O12 0.072(3) 0.034(2) 0.027(2) -0.0089(19) -0.017(2) 0.000(2) O13 0.037(2) 0.046(3) 0.038(2) 0.017(2) 0.0048(19) -0.002(2) O14 0.100(4) 0.093(5) 0.095(5) -0.032(4) -0.024(4) 0.048(4) C1 0.039(3) 0.026(3) 0.024(3) 0.004(3) 0.002(2) -0.003(3) C2 0.037(3) 0.033(3) 0.023(3) 0.000(3) 0.006(3) -0.006(3) C3 0.027(3) 0.035(3) 0.019(3) 0.000(3) 0.004(2) 0.001(3) C4 0.022(3) 0.027(3) 0.025(3) 0.002(3) -0.004(2) 0.000(2) C5 0.026(3) 0.028(3) 0.023(3) 0.000(3) -0.004(2) 0.002(2) C6 0.030(3) 0.032(3) 0.027(3) -0.013(3) -0.001(2) -0.003(3) C7 0.113(7) 0.050(5) 0.042(5) 0.010(4) 0.036(5) 0.008(5) C8 0.146(9) 0.046(5) 0.057(5) 0.010(4) 0.047(5) 0.009(5) C9 0.032(4) 0.108(7) 0.070(6) -0.020(5) 0.014(4) -0.020(4) C10 0.055(5) 0.169(11) 0.099(7) -0.033(8) 0.011(5) -0.061(6) C11 0.037(3) 0.038(4) 0.033(3) 0.010(3) 0.010(3) 0.007(3) C12 0.039(4) 0.069(5) 0.065(5) 0.014(4) 0.009(3) -0.002(4) C13 0.023(3) 0.043(4) 0.035(4) -0.006(3) 0.003(3) -0.006(3) C14 0.040(3) 0.066(5) 0.046(4) -0.006(4) 0.018(3) -0.006(3) C15 0.037(3) 0.042(4) 0.030(3) -0.002(3) 0.009(3) 0.000(3) C16 0.050(4) 0.040(4) 0.043(4) -0.008(3) -0.002(3) 0.009(3) C17 0.023(2) 0.039(3) 0.029(3) 0.008(3) -0.002(2) 0.003(2) C18 0.043(3) 0.064(5) 0.035(3) 0.009(3) -0.005(3) 0.015(3) C19 0.107(6) 0.257(16) 0.158(10) 0.164(11) 0.089(7) 0.127(9) C20 0.175(9) 0.301(16) 0.121(9) 0.140(11) 0.072(8) 0.157(10) C21 0.132(7) 0.239(10) 0.054(5) 0.046(6) 0.003(5) 0.124(8) C22 0.056(4) 0.099(6) 0.101(6) 0.062(5) 0.019(4) 0.039(4) C23 0.048(4) 0.056(5) 0.078(5) 0.031(4) 0.003(4) 0.008(3) C24 0.115(6) 0.153(7) 0.051(5) -0.019(5) -0.024(4) 0.087(6) C25 0.162(10) 0.275(14) 0.124(9) -0.132(11) -0.106(8) 0.134(12) C26 0.071(6) 0.135(10) 0.198(12) -0.058(8) -0.028(6) -0.009(7) S1' 0.0306(7) 0.0296(7) 0.0203(7) 0.0027(6) -0.0054(6) 0.0011(6) O1' 0.030(2) 0.035(2) 0.034(2) 0.0019(19) 0.0046(17) 0.0037(18) O2' 0.031(2) 0.043(3) 0.038(3) -0.001(2) 0.0019(18) -0.008(2) O3' 0.059(3) 0.029(2) 0.031(2) 0.0066(19) 0.010(2) -0.001(2) O4' 0.030(2) 0.033(2) 0.034(2) -0.001(2) -0.0039(18) 0.0055(18) O5' 0.028(2) 0.035(2) 0.0161(19) -0.0002(17) -0.0022(15) -0.0047(17) O6' 0.0311(19) 0.030(2) 0.0187(19) 0.0035(18) -0.0072(15) -0.0014(18) O7' 0.066(3) 0.056(3) 0.032(2) -0.001(2) 0.012(2) 0.016(3) O8' 0.048(3) 0.201(10) 0.136(7) -0.086(7) 0.045(4) -0.038(4) O9' 0.171(7) 0.079(5) 0.029(3) 0.013(3) -0.016(4) -0.030(5) O10' 0.037(2) 0.100(4) 0.029(2) -0.007(3) -0.004(2) -0.022(3) O11' 0.056(3) 0.055(3) 0.038(3) -0.011(2) -0.002(2) 0.017(2) O12' 0.077(3) 0.036(2) 0.022(2) -0.0009(19) -0.010(2) 0.007(2) O13' 0.036(2) 0.052(3) 0.040(2) 0.011(2) -0.0090(19) -0.008(2) O14' 0.069(3) 0.074(4) 0.077(3) 0.028(3) -0.005(3) -0.026(3) C1' 0.027(3) 0.030(3) 0.030(3) 0.001(3) -0.006(2) 0.007(3) C2' 0.030(3) 0.037(3) 0.025(3) -0.004(3) 0.003(3) 0.001(3) C3' 0.039(3) 0.033(3) 0.022(3) 0.003(3) -0.001(3) -0.002(3) C4' 0.025(3) 0.028(3) 0.021(3) 0.008(3) -0.003(2) 0.007(2) C5' 0.025(3) 0.032(3) 0.019(3) -0.006(3) 0.000(2) -0.001(2) C6' 0.029(3) 0.027(3) 0.026(3) 0.002(3) -0.003(2) 0.000(2) C7' 0.032(3) 0.050(4) 0.042(4) -0.009(4) 0.014(3) 0.003(3) C8' 0.039(4) 0.057(4) 0.065(5) -0.017(4) 0.012(3) 0.018(3) C9' 0.057(5) 0.130(10) 0.086(7) -0.034(7) 0.020(5) -0.044(6) C10' 0.051(5) 0.166(12) 0.088(7) -0.035(8) 0.001(5) -0.040(6) C11' 0.063(4) 0.050(4) 0.023(3) 0.004(3) 0.012(3) 0.017(3) C12' 0.072(4) 0.046(4) 0.040(4) 0.017(3) 0.024(3) 0.001(3) C13' 0.042(4) 0.041(4) 0.028(3) 0.004(3) 0.006(3) 0.003(3) C14' 0.045(4) 0.088(6) 0.029(4) -0.016(4) 0.007(3) -0.008(4) C15' 0.045(3) 0.026(3) 0.030(3) 0.001(3) 0.001(3) 0.002(3) C16' 0.042(4) 0.051(4) 0.054(4) 0.003(4) 0.006(3) 0.014(3) C17' 0.039(3) 0.069(5) 0.032(3) 0.003(3) -0.001(3) 0.027(3) C18' 0.034(3) 0.043(3) 0.029(3) 0.005(3) -0.014(2) 0.003(2) C19' 0.059(4) 0.075(5) 0.059(4) 0.010(4) -0.009(3) 0.019(4) C20' 0.056(4) 0.085(5) 0.039(4) 0.033(4) -0.012(3) 0.001(4) C21' 0.048(3) 0.045(3) 0.044(4) 0.017(3) -0.016(3) 0.005(3) C22' 0.045(3) 0.067(4) 0.055(4) 0.020(3) -0.021(3) -0.003(3) C23' 0.043(3) 0.040(3) 0.050(4) 0.006(3) -0.004(3) -0.003(3) C24' 0.059(4) 0.045(4) 0.066(5) 0.025(4) -0.022(4) -0.008(3) C25' 0.079(5) 0.069(5) 0.120(8) 0.047(5) -0.052(5) -0.040(4) C26' 0.079(5) 0.079(6) 0.062(5) -0.014(4) -0.025(4) 0.034(4) C27 0.134(9) 0.101(8) 0.047(5) -0.019(6) 0.012(5) 0.007(7) Cl1 0.114(2) 0.130(3) 0.110(2) -0.014(2) 0.0380(19) -0.008(2) Cl2 0.240(4) 0.125(3) 0.097(2) -0.016(2) -0.001(3) -0.032(3) C28 0.068(5) 0.100(8) 0.098(8) 0.001(7) 0.009(5) 0.006(6) Cl3 0.0968(19) 0.114(2) 0.104(2) 0.0075(19) 0.0265(17) -0.0107(18) Cl4 0.137(2) 0.107(3) 0.107(2) 0.008(2) 0.0105(18) -0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O12 1.393(4) . ? S1 O13 1.426(4) . ? S1 O4 1.597(4) . ? S1 C17 1.775(6) . ? O1 C7 1.352(9) . ? O1 C1 1.456(7) . ? O2 C9 1.352(8) . ? O2 C2 1.438(7) . ? O3 C11 1.377(7) . ? O3 C3 1.424(7) . ? O4 C4 1.455(7) . ? O5 C13 1.362(7) . ? O5 C5 1.427(6) . ? O6 C15 1.386(8) . ? O6 C6 1.427(7) . ? O7 C7 1.193(11) . ? O8 C9 1.163(10) . ? O9 C11 1.197(7) . ? O10 C13 1.218(7) . ? O11 C15 1.204(7) . ? O14 C23 1.159(10) . ? C1 C2 1.486(8) . ? C1 C6 1.519(8) . ? C1 H1 0.9800 . ? C2 C3 1.547(8) . ? C2 H2 0.9800 . ? C3 C4 1.506(8) . ? C3 H3 0.9800 . ? C4 C5 1.527(7) . ? C4 H4 0.9800 . ? C5 C6 1.525(8) . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C7 C8 1.432(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.479(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.485(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.490(9) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.485(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.491(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.549(11) . ? C18 C19 1.562(12) . ? C18 C24 1.565(13) . ? C19 C20 1.541(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.503(19) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.488(15) . ? C21 C24 1.641(18) . ? C21 H21 0.9800 . ? C22 C23 1.508(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C26 1.493(17) . ? C24 C25 1.572(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S1' O13' 1.423(5) . ? S1' O12' 1.435(5) . ? S1' O6' 1.592(4) . ? S1' C17' 1.759(6) . ? O1' C7' 1.348(7) . ? O1' C1' 1.461(7) . ? O2' C9' 1.337(9) . ? O2' C2' 1.460(7) . ? O3' C11' 1.356(7) . ? O3' C3' 1.427(8) . ? O4' C15' 1.344(7) . ? O4' C4' 1.445(7) . ? O5' C13' 1.341(7) . ? O5' C5' 1.443(6) . ? O6' C6' 1.461(7) . ? O7' C7' 1.216(8) . ? O8' C9' 1.200(11) . ? O9' C11' 1.175(9) . ? O10' C13' 1.206(7) . ? O11' C15' 1.191(7) . ? O14' C23' 1.214(8) . ? C1' C2' 1.497(9) . ? C1' C6' 1.519(8) . ? C1' H1' 0.9800 . ? C2' C3' 1.536(8) . ? C2' H2' 0.9800 . ? C3' C4' 1.540(8) . ? C3' H3' 0.9800 . ? C4' C5' 1.524(8) . ? C4' H4' 0.9800 . ? C5' C6' 1.519(7) . ? C5' H5' 0.9800 . ? C6' H6' 0.9800 . ? C7' C8' 1.483(9) . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9' C10' 1.522(13) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C12' 1.511(10) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' C14' 1.500(8) . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.482(9) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' C18' 1.551(8) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C23' 1.496(9) . ? C18' C24' 1.569(10) . ? C18' C19' 1.603(10) . ? C19' C20' 1.564(10) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' C21' 1.502(10) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.517(9) . ? C21' C24' 1.538(9) . ? C21' H21' 0.9800 . ? C22' C23' 1.493(8) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C24' C26' 1.506(11) . ? C24' C25' 1.557(10) . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27 Cl2 1.721(11) . ? C27 Cl1 1.757(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 Cl3 1.689(10) . ? C28 Cl4 1.772(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? 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 O12 S1 O13 119.7(3) . . ? O12 S1 O4 109.6(2) . . ? O13 S1 O4 103.1(2) . . ? O12 S1 C17 111.6(3) . . ? O13 S1 C17 108.7(3) . . ? O4 S1 C17 102.4(2) . . ? C7 O1 C1 116.5(6) . . ? C9 O2 C2 118.1(5) . . ? C11 O3 C3 116.1(4) . . ? C4 O4 S1 121.5(3) . . ? C13 O5 C5 118.6(4) . . ? C15 O6 C6 117.9(4) . . ? O1 C1 C2 110.4(5) . . ? O1 C1 C6 105.2(5) . . ? C2 C1 C6 112.4(5) . . ? O1 C1 H1 109.6 . . ? C2 C1 H1 109.6 . . ? C6 C1 H1 109.6 . . ? O2 C2 C1 109.9(5) . . ? O2 C2 C3 107.2(5) . . ? C1 C2 C3 109.9(5) . . ? O2 C2 H2 109.9 . . ? C1 C2 H2 109.9 . . ? C3 C2 H2 109.9 . . ? O3 C3 C4 108.0(4) . . ? O3 C3 C2 111.7(5) . . ? C4 C3 C2 110.4(5) . . ? O3 C3 H3 108.9 . . ? C4 C3 H3 108.9 . . ? C2 C3 H3 108.9 . . ? O4 C4 C3 107.9(5) . . ? O4 C4 C5 106.4(4) . . ? C3 C4 C5 111.2(4) . . ? O4 C4 H4 110.4 . . ? C3 C4 H4 110.4 . . ? C5 C4 H4 110.4 . . ? O5 C5 C6 110.3(5) . . ? O5 C5 C4 106.8(4) . . ? C6 C5 C4 112.0(4) . . ? O5 C5 H5 109.2 . . ? C6 C5 H5 109.2 . . ? C4 C5 H5 109.2 . . ? O6 C6 C1 107.5(5) . . ? O6 C6 C5 109.2(5) . . ? C1 C6 C5 109.2(5) . . ? O6 C6 H6 110.3 . . ? C1 C6 H6 110.3 . . ? C5 C6 H6 110.3 . . ? O7 C7 O1 121.5(8) . . ? O7 C7 C8 124.7(8) . . ? O1 C7 C8 113.8(8) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 O2 122.0(7) . . ? O8 C9 C10 126.1(8) . . ? O2 C9 C10 111.1(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 O3 120.8(5) . . ? O9 C11 C12 127.4(6) . . ? O3 C11 C12 111.8(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O10 C13 O5 122.0(6) . . ? O10 C13 C14 127.6(5) . . ? O5 C13 C14 110.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C15 O6 121.5(6) . . ? O11 C15 C16 128.5(6) . . ? O6 C15 C16 110.0(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S1 117.7(4) . . ? C18 C17 H17A 107.9 . . ? S1 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? S1 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 C23 108.6(6) . . ? C17 C18 C19 118.4(6) . . ? C23 C18 C19 104.2(8) . . ? C17 C18 C24 121.4(7) . . ? C23 C18 C24 100.5(6) . . ? C19 C18 C24 101.1(9) . . ? C20 C19 C18 105.4(9) . . ? C20 C19 H19A 110.7 . . ? C18 C19 H19A 110.7 . . ? C20 C19 H19B 110.7 . . ? C18 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 102.0(9) . . ? C21 C20 H20A 111.4 . . ? C19 C20 H20A 111.4 . . ? C21 C20 H20B 111.4 . . ? C19 C20 H20B 111.4 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C20 108.5(14) . . ? C22 C21 C24 104.3(7) . . ? C20 C21 C24 103.7(9) . . ? C22 C21 H21 113.2 . . ? C20 C21 H21 113.2 . . ? C24 C21 H21 113.2 . . ? C21 C22 C23 101.5(7) . . ? C21 C22 H22A 111.5 . . ? C23 C22 H22A 111.5 . . ? C21 C22 H22B 111.5 . . ? C23 C22 H22B 111.5 . . ? H22A C22 H22B 109.3 . . ? O14 C23 C22 126.1(8) . . ? O14 C23 C18 126.5(6) . . ? C22 C23 C18 107.4(7) . . ? C26 C24 C18 111.4(7) . . ? C26 C24 C25 103.2(13) . . ? C18 C24 C25 118.4(8) . . ? C26 C24 C21 114.4(9) . . ? C18 C24 C21 90.0(10) . . ? C25 C24 C21 119.7(10) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O13' S1' O12' 120.3(3) . . ? O13' S1' O6' 103.6(2) . . ? O12' S1' O6' 110.0(2) . . ? O13' S1' C17' 111.5(4) . . ? O12' S1' C17' 109.0(3) . . ? O6' S1' C17' 100.5(3) . . ? C7' O1' C1' 115.1(5) . . ? C9' O2' C2' 116.1(6) . . ? C11' O3' C3' 117.2(5) . . ? C15' O4' C4' 117.3(4) . . ? C13' O5' C5' 116.9(4) . . ? C6' O6' S1' 120.8(3) . . ? O1' C1' C2' 108.9(5) . . ? O1' C1' C6' 105.9(4) . . ? C2' C1' C6' 111.5(5) . . ? O1' C1' H1' 110.2 . . ? C2' C1' H1' 110.2 . . ? C6' C1' H1' 110.2 . . ? O2' C2' C1' 109.8(5) . . ? O2' C2' C3' 107.8(5) . . ? C1' C2' C3' 110.0(5) . . ? O2' C2' H2' 109.7 . . ? C1' C2' H2' 109.7 . . ? C3' C2' H2' 109.7 . . ? O3' C3' C2' 109.8(5) . . ? O3' C3' C4' 105.9(5) . . ? C2' C3' C4' 110.8(5) . . ? O3' C3' H3' 110.1 . . ? C2' C3' H3' 110.1 . . ? C4' C3' H3' 110.1 . . ? O4' C4' C5' 108.6(4) . . ? O4' C4' C3' 105.5(4) . . ? C5' C4' C3' 110.4(5) . . ? O4' C4' H4' 110.7 . . ? C5' C4' H4' 110.7 . . ? C3' C4' H4' 110.7 . . ? O5' C5' C6' 108.1(4) . . ? O5' C5' C4' 107.8(5) . . ? C6' C5' C4' 112.2(4) . . ? O5' C5' H5' 109.6 . . ? C6' C5' H5' 109.6 . . ? C4' C5' H5' 109.6 . . ? O6' C6' C1' 107.8(5) . . ? O6' C6' C5' 107.0(4) . . ? C1' C6' C5' 109.5(4) . . ? O6' C6' H6' 110.8 . . ? C1' C6' H6' 110.8 . . ? C5' C6' H6' 110.8 . . ? O7' C7' O1' 122.2(6) . . ? O7' C7' C8' 126.1(6) . . ? O1' C7' C8' 111.7(6) . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? O8' C9' O2' 123.8(8) . . ? O8' C9' C10' 126.6(8) . . ? O2' C9' C10' 109.4(8) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? O9' C11' O3' 121.6(7) . . ? O9' C11' C12' 129.9(7) . . ? O3' C11' C12' 108.4(6) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O10' C13' O5' 123.9(6) . . ? O10' C13' C14' 125.1(6) . . ? O5' C13' C14' 111.0(5) . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? O11' C15' O4' 123.7(6) . . ? O11' C15' C16' 125.3(6) . . ? O4' C15' C16' 111.0(6) . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C18' C17' S1' 115.3(5) . . ? C18' C17' H17C 108.4 . . ? S1' C17' H17C 108.4 . . ? C18' C17' H17D 108.4 . . ? S1' C17' H17D 108.4 . . ? H17C C17' H17D 107.5 . . ? C23' C18' C17' 109.5(5) . . ? C23' C18' C24' 100.6(5) . . ? C17' C18' C24' 117.7(6) . . ? C23' C18' C19' 103.6(5) . . ? C17' C18' C19' 120.3(5) . . ? C24' C18' C19' 102.8(6) . . ? C20' C19' C18' 101.0(6) . . ? C20' C19' H19C 111.6 . . ? C18' C19' H19C 111.6 . . ? C20' C19' H19D 111.6 . . ? C18' C19' H19D 111.6 . . ? H19C C19' H19D 109.4 . . ? C21' C20' C19' 103.9(5) . . ? C21' C20' H20C 111.0 . . ? C19' C20' H20C 111.0 . . ? C21' C20' H20D 111.0 . . ? C19' C20' H20D 111.0 . . ? H20C C20' H20D 109.0 . . ? C20' C21' C22' 107.5(6) . . ? C20' C21' C24' 104.2(5) . . ? C22' C21' C24' 103.6(5) . . ? C20' C21' H21' 113.6 . . ? C22' C21' H21' 113.6 . . ? C24' C21' H21' 113.6 . . ? C23' C22' C21' 101.6(5) . . ? C23' C22' H22C 111.4 . . ? C21' C22' H22C 111.4 . . ? C23' C22' H22D 111.4 . . ? C21' C22' H22D 111.4 . . ? H22C C22' H22D 109.3 . . ? O14' C23' C22' 126.3(6) . . ? O14' C23' C18' 126.8(6) . . ? C22' C23' C18' 106.9(5) . . ? C26' C24' C21' 114.6(6) . . ? C26' C24' C25' 112.3(7) . . ? C21' C24' C25' 113.0(6) . . ? C26' C24' C18' 111.5(6) . . ? C21' C24' C18' 92.0(5) . . ? C25' C24' C18' 111.9(7) . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? Cl2 C27 Cl1 112.3(5) . . ? Cl2 C27 H27A 109.1 . . ? Cl1 C27 H27A 109.1 . . ? Cl2 C27 H27B 109.1 . . ? Cl1 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? Cl3 C28 Cl4 113.4(6) . . ? Cl3 C28 H28A 108.9 . . ? Cl4 C28 H28A 108.9 . . ? Cl3 C28 H28B 108.9 . . ? Cl4 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.802 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.087 #===END