# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Farrugia, L' _publ_contact_author_email louis@chem.gla.ac.uk _publ_section_title ; The first members of the octasubstituted naphthalene spider-host series with type I (abababab) conformation : gateway to new nano-host gas storage materials. ; loop_ _publ_author_name Farrugia D.MacNicol # Attachment '- archive_full.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-03-12 at 14:56:28 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : d:\my progs\wingx\files\archive.reqdat # CIF files read : ljf115 dreduc gaussian sortav struct data_3-tetraglyme _database_code_depnum_ccdc_archive 'CCDC 771696' #TrackingRef '- archive_full.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C74 H72 O8' _chemical_formula_sum 'C74 H72 O8' _chemical_formula_weight 1089.32 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' _symmetry_space_group_name_Hall '-P 4a 2ac' _symmetry_Int_Tables_number 130 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-y, -x, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' 'y, x, z-1/2' '-y-1/2, -x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' _cell_length_a 16.5680(2) _cell_length_b 16.5680(2) _cell_length_c 26.0484(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7150.25(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7167 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.22 0 0 -1 0.28 -1 -1 0 0.278 1 1 0 0.181 1 -1 0 0.153 -1 1 0 0.166 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst. (1965), 18, 1035-1038 ; _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.984 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.558394E-1 _diffrn_orient_matrix_ub_12 -0.180806E-1 _diffrn_orient_matrix_ub_13 -0.89513E-2 _diffrn_orient_matrix_ub_21 -0.201736E-1 _diffrn_orient_matrix_ub_22 0.563738E-1 _diffrn_orient_matrix_ub_23 0.48453E-2 _diffrn_orient_matrix_ub_31 0.108626E-1 _diffrn_orient_matrix_ub_32 0.117514E-1 _diffrn_orient_matrix_ub_33 -0.370161E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0186 _diffrn_reflns_number 86187 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3522 _reflns_number_gt 2644 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The reflection file used for refinement was prepared using the PLATON/SQUEEZE option. Residual density peaks prior to SQUEEEZE were of the order of 1.5 eA-3 and the (presumed) tetraglyme present in the cavities was highly disordered and normal atomic modelling was not possible. The SQUEEZE option recovered ~57 e per cavity, so that each cavity contained on average ~ 1/2 tetraglyme molecule.\"y ; _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^)+(0.1849P)^2^+0.8189P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3522 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2709 _refine_ls_wR_factor_gt 0.2507 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.498 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O11 O 0.56793(8) 0.12383(9) 0.18540(6) 0.0580(5) Uani 1 1 d . . . O21 O 0.76797(9) 0.12028(9) 0.09527(5) 0.0554(5) Uani 1 1 d . . . C1 C 0.69701(11) 0.18344(10) 0.20162(8) 0.0443(5) Uani 1 1 d . . . C2 C 0.72474(11) 0.21519(11) 0.15599(8) 0.0456(5) Uani 1 1 d . . . C9 C 0.71928(10) 0.21928(10) 0.25 0.0429(6) Uani 1 2 d S . . C11 C 0.65039(12) 0.10546(12) 0.19798(8) 0.0517(5) Uani 1 1 d . . . H11A H 0.6742 0.0705 0.1711 0.062 Uiso 1 1 calc R . . H11B H 0.6529 0.0763 0.2311 0.062 Uiso 1 1 calc R . . C21 C 0.70344(12) 0.17601(12) 0.10546(8) 0.0489(5) Uani 1 1 d . . . H21A H 0.6512 0.1473 0.108 0.059 Uiso 1 1 calc R . . H21B H 0.6996 0.2169 0.0779 0.059 Uiso 1 1 calc R . . C110 C 0.51618(13) 0.05884(15) 0.18130(8) 0.0593(6) Uani 1 1 d . . . C111 C 0.53895(16) -0.02072(15) 0.18666(9) 0.0679(7) Uani 1 1 d . . . H111 H 0.5941 -0.0336 0.1922 0.082 Uiso 1 1 calc R . . C112 C 0.4823(2) -0.08217(19) 0.18402(12) 0.0920(10) Uani 1 1 d . . . C113 C 0.4027(2) -0.0620(2) 0.17451(13) 0.0994(12) Uani 1 1 d . . . H113 H 0.3632 -0.1035 0.1723 0.119 Uiso 1 1 calc R . . C114 C 0.37954(17) 0.0176(2) 0.16818(11) 0.0926(11) Uani 1 1 d . . . H114 H 0.3247 0.0304 0.1612 0.111 Uiso 1 1 calc R . . C115 C 0.43614(14) 0.07849(18) 0.17194(9) 0.0712(7) Uani 1 1 d . . . H115 H 0.4204 0.1333 0.1682 0.085 Uiso 1 1 calc R . . C116 C 0.5086(3) -0.1680(2) 0.19350(16) 0.1288(16) Uani 1 1 d . . . H11C H 0.5564 -0.1683 0.2157 0.193 Uiso 1 1 calc R . . H11D H 0.5217 -0.1939 0.1607 0.193 Uiso 1 1 calc R . . H11E H 0.4648 -0.1978 0.2103 0.193 Uiso 1 1 calc R . . C210 C 0.76709(13) 0.08078(12) 0.04854(8) 0.0528(6) Uani 1 1 d . . . C211 C 0.83148(14) 0.02824(13) 0.04045(10) 0.0650(7) Uani 1 1 d . . . H211 H 0.8703 0.0198 0.0667 0.078 Uiso 1 1 calc R . . C212 C 0.83871(16) -0.01220(15) -0.00676(11) 0.0733(7) Uani 1 1 d . . . C213 C 0.78121(16) 0.00129(16) -0.04418(10) 0.0725(7) Uani 1 1 d . . . H213 H 0.786 -0.025 -0.0765 0.087 Uiso 1 1 calc R . . C214 C 0.71768(15) 0.05185(15) -0.03542(9) 0.0641(6) Uani 1 1 d . . . H214 H 0.6784 0.0595 -0.0616 0.077 Uiso 1 1 calc R . . C215 C 0.70920(13) 0.09249(13) 0.01115(8) 0.0556(6) Uani 1 1 d . . . H215 H 0.6646 0.1274 0.017 0.067 Uiso 1 1 calc R . . C216 C 0.9085(2) -0.0684(2) -0.01609(16) 0.1092(12) Uani 1 1 d . . . H21C H 0.8884 -0.1237 -0.0199 0.164 Uiso 1 1 calc R . . H21D H 0.9458 -0.0658 0.013 0.164 Uiso 1 1 calc R . . H21E H 0.9368 -0.0523 -0.0475 0.164 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O11 0.0436(8) 0.0556(9) 0.0748(10) 0.0000(7) -0.0050(6) -0.0100(6) O21 0.0533(9) 0.0485(8) 0.0644(9) -0.0059(6) -0.0044(6) 0.0113(6) C1 0.0373(9) 0.0353(9) 0.0603(12) -0.0013(8) -0.0026(8) 0.0022(7) C2 0.0377(9) 0.0373(9) 0.0619(12) -0.0017(8) -0.0009(8) 0.0045(7) C9 0.0343(8) 0.0343(8) 0.0600(15) 0.0005(7) -0.0005(7) 0.0050(9) C11 0.0483(11) 0.0425(10) 0.0645(12) -0.0009(8) -0.0025(9) -0.0053(8) C21 0.0435(10) 0.0428(10) 0.0604(12) -0.0009(8) -0.0009(8) 0.0027(8) C110 0.0529(12) 0.0750(15) 0.0498(11) -0.0021(9) -0.0024(8) -0.0219(10) C111 0.0741(15) 0.0614(14) 0.0683(14) -0.0026(10) -0.0078(11) -0.0228(12) C112 0.109(2) 0.0821(19) 0.0853(19) -0.0003(14) -0.0149(16) -0.0452(17) C113 0.087(2) 0.114(3) 0.097(2) 0.0049(19) -0.0121(17) -0.057(2) C114 0.0646(16) 0.140(3) 0.0729(17) 0.0018(17) -0.0105(12) -0.0324(19) C115 0.0546(13) 0.0948(19) 0.0643(13) 0.0039(12) -0.0057(10) -0.0153(12) C116 0.168(4) 0.081(2) 0.137(3) 0.008(2) -0.033(3) -0.057(3) C210 0.0536(12) 0.0395(10) 0.0654(12) -0.0048(9) 0.0040(9) -0.0025(8) C211 0.0608(13) 0.0494(12) 0.0849(16) -0.0091(11) 0.0030(11) 0.0067(10) C212 0.0697(16) 0.0550(13) 0.0952(19) -0.0184(12) 0.0148(13) 0.0051(11) C213 0.0783(17) 0.0651(15) 0.0741(16) -0.0206(12) 0.0105(12) -0.0077(12) C214 0.0695(14) 0.0559(13) 0.0670(13) -0.0077(11) 0.0051(10) -0.0131(11) C215 0.0555(12) 0.0458(11) 0.0654(13) -0.0013(9) 0.0041(9) -0.0060(9) C216 0.099(2) 0.097(2) 0.131(3) -0.047(2) 0.006(2) 0.0345(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O11 C110 1.381(2) . ? O11 C11 1.438(3) . ? O21 C210 1.382(2) . ? O21 C21 1.437(2) . ? C1 C2 1.379(3) . ? C1 C9 1.441(2) . ? C1 C11 1.508(3) . ? C2 C2 1.425(4) 2_655 ? C2 C21 1.510(3) . ? C9 C9 1.440(2) 2_655 ? C9 C1 1.441(2) 6_545 ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C110 C111 1.378(3) . ? C110 C115 1.387(3) . ? C111 C112 1.386(3) . ? C111 H111 0.95 . ? C112 C113 1.384(5) . ? C112 C116 1.508(5) . ? C113 C114 1.383(5) . ? C113 H113 0.95 . ? C114 C115 1.381(4) . ? C114 H114 0.95 . ? C115 H115 0.95 . ? C116 H11C 0.98 . ? C116 H11D 0.98 . ? C116 H11E 0.98 . ? C210 C215 1.381(3) . ? C210 C211 1.393(3) . ? C211 C212 1.406(3) . ? C211 H211 0.95 . ? C212 C213 1.381(4) . ? C212 C216 1.504(4) . ? C213 C214 1.364(4) . ? C213 H213 0.95 . ? C214 C215 1.394(3) . ? C214 H214 0.95 . ? C215 H215 0.95 . ? C216 H21C 0.98 . ? C216 H21D 0.98 . ? C216 H21E 0.98 . ? 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 C110 O11 C11 116.29(17) . . ? C210 O21 C21 117.31(15) . . ? C2 C1 C9 120.76(17) . . ? C2 C1 C11 116.32(17) . . ? C9 C1 C11 122.61(17) . . ? C1 C2 C2 120.30(11) . 2_655 ? C1 C2 C21 120.65(17) . . ? C2 C2 C21 119.04(11) 2_655 . ? C9 C9 C1 118.19(11) 2_655 6_545 ? C9 C9 C1 118.19(11) 2_655 . ? C1 C9 C1 123.6(2) 6_545 . ? O11 C11 C1 108.65(16) . . ? O11 C11 H11A 110 . . ? C1 C11 H11A 110 . . ? O11 C11 H11B 110 . . ? C1 C11 H11B 110 . . ? H11A C11 H11B 108.3 . . ? O21 C21 C2 105.27(15) . . ? O21 C21 H21A 110.7 . . ? C2 C21 H21A 110.7 . . ? O21 C21 H21B 110.7 . . ? C2 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C111 C110 O11 124.6(2) . . ? C111 C110 C115 120.3(2) . . ? O11 C110 C115 115.1(2) . . ? C110 C111 C112 120.8(3) . . ? C110 C111 H111 119.6 . . ? C112 C111 H111 119.6 . . ? C113 C112 C111 118.5(3) . . ? C113 C112 C116 122.2(3) . . ? C111 C112 C116 119.3(3) . . ? C114 C113 C112 121.0(3) . . ? C114 C113 H113 119.5 . . ? C112 C113 H113 119.5 . . ? C115 C114 C113 120.0(3) . . ? C115 C114 H114 120 . . ? C113 C114 H114 120 . . ? C114 C115 C110 119.3(3) . . ? C114 C115 H115 120.3 . . ? C110 C115 H115 120.3 . . ? C112 C116 H11C 109.5 . . ? C112 C116 H11D 109.5 . . ? H11C C116 H11D 109.5 . . ? C112 C116 H11E 109.5 . . ? H11C C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? C215 C210 O21 124.20(18) . . ? C215 C210 C211 120.9(2) . . ? O21 C210 C211 114.91(19) . . ? C210 C211 C212 119.7(2) . . ? C210 C211 H211 120.1 . . ? C212 C211 H211 120.1 . . ? C213 C212 C211 118.8(2) . . ? C213 C212 C216 121.1(3) . . ? C211 C212 C216 120.1(3) . . ? C214 C213 C212 120.9(2) . . ? C214 C213 H213 119.6 . . ? C212 C213 H213 119.6 . . ? C213 C214 C215 121.3(2) . . ? C213 C214 H214 119.3 . . ? C215 C214 H214 119.3 . . ? C210 C215 C214 118.4(2) . . ? C210 C215 H215 120.8 . . ? C214 C215 H215 120.8 . . ? C212 C216 H21C 109.5 . . ? C212 C216 H21D 109.5 . . ? H21C C216 H21D 109.5 . . ? C212 C216 H21E 109.5 . . ? H21C C216 H21E 109.5 . . ? H21D C216 H21E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C2 -0.7(3) . . . 2_655 ? C11 C1 C2 C2 -174.5(2) . . . 2_655 ? C9 C1 C2 C21 178.09(14) . . . . ? C11 C1 C2 C21 4.3(2) . . . . ? C2 C1 C9 C9 -9.51(18) . . . 2_655 ? C11 C1 C9 C9 163.89(13) . . . 2_655 ? C2 C1 C9 C1 170.49(18) . . . 6_545 ? C11 C1 C9 C1 -16.11(13) . . . 6_545 ? C110 O11 C11 C1 -179.09(16) . . . . ? C2 C1 C11 O11 -83.1(2) . . . . ? C9 C1 C11 O11 103.26(18) . . . . ? C210 O21 C21 C2 -174.56(16) . . . . ? C1 C2 C21 O21 -91.9(2) . . . . ? C2 C2 C21 O21 86.9(2) 2_655 . . . ? C11 O11 C110 C111 -2.3(3) . . . . ? C11 O11 C110 C115 176.60(19) . . . . ? O11 C110 C111 C112 177.3(2) . . . . ? C115 C110 C111 C112 -1.5(4) . . . . ? C110 C111 C112 C113 1.7(4) . . . . ? C110 C111 C112 C116 -176.0(3) . . . . ? C111 C112 C113 C114 -0.6(5) . . . . ? C116 C112 C113 C114 177.1(3) . . . . ? C112 C113 C114 C115 -0.8(5) . . . . ? C113 C114 C115 C110 1.0(4) . . . . ? C111 C110 C115 C114 0.2(3) . . . . ? O11 C110 C115 C114 -178.8(2) . . . . ? C21 O21 C210 C215 1.0(3) . . . . ? C21 O21 C210 C211 179.28(18) . . . . ? C215 C210 C211 C212 1.3(3) . . . . ? O21 C210 C211 C212 -177.0(2) . . . . ? C210 C211 C212 C213 -0.1(4) . . . . ? C210 C211 C212 C216 179.4(3) . . . . ? C211 C212 C213 C214 -1.1(4) . . . . ? C216 C212 C213 C214 179.5(3) . . . . ? C212 C213 C214 C215 1.0(4) . . . . ? O21 C210 C215 C214 176.71(19) . . . . ? C211 C210 C215 C214 -1.4(3) . . . . ? C213 C214 C215 C210 0.3(3) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 0.873 871 57 ' ' 2 -0.250 0.750 0.608 871 57 ' ' _platon_squeeze_details ; The electron count indicates that each void contains nearly half a solvent molecule of tetraglyme, i.e 0.25(C~10~H~22~O~5~) per molecule of host. ; #------------------ SECTION 2. ----------------------------------------------# data_3-CS2 _database_code_depnum_ccdc_archive 'CCDC 771697' #TrackingRef 'archive-full.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C74 H72 O8, 3.28(C S2)' _chemical_formula_sum 'C77.28 H72 O8 S6.56' _chemical_formula_weight 1339.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 15.7611(9) _cell_length_b 17.0636(9) _cell_length_c 26.4663(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7117.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6750 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.5 _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2817.8 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9432 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS, (Sheldrick 2008)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.77605E-2 _diffrn_orient_matrix_ub_12 -0.116454E-1 _diffrn_orient_matrix_ub_13 -0.367409E-1 _diffrn_orient_matrix_ub_21 -0.332184E-1 _diffrn_orient_matrix_ub_22 0.480217E-1 _diffrn_orient_matrix_ub_23 -0.88153E-2 _diffrn_orient_matrix_ub_31 0.534966E-1 _diffrn_orient_matrix_ub_32 0.315081E-1 _diffrn_orient_matrix_ub_33 -0.144E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_number 45331 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.08 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 6960 _reflns_number_gt 5658 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0711P)^2^+12.5278P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6960 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.2048 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.693 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O11 O 0.87594(15) 0.43139(12) 0.30409(8) 0.0358(5) Uani 1 1 d . . . O21 O 0.88496(14) 0.23299(12) 0.39157(8) 0.0344(5) Uani 1 1 d . . . O71 O 0.72675(14) 0.37565(13) 0.08559(8) 0.0340(5) Uani 1 1 d . . . O81 O 0.93099(14) 0.38553(12) 0.17571(8) 0.0359(5) Uani 1 1 d . . . C1 C 0.81762(19) 0.30431(16) 0.28728(11) 0.0271(6) Uani 1 1 d . . . C2 C 0.7854(2) 0.27570(16) 0.33204(11) 0.0286(6) Uani 1 1 d . . . C21 C 0.8270(2) 0.29635(17) 0.38201(11) 0.0305(7) Uani 1 1 d . . . H21A H 0.8577 0.3468 0.3795 0.037 Uiso 1 1 calc R . . H21B H 0.7842 0.3002 0.4092 0.037 Uiso 1 1 calc R . . C7 C 0.77432(19) 0.28511(16) 0.14724(11) 0.0277(6) Uani 1 1 d . . . C71 C 0.7962(2) 0.32412(17) 0.09743(11) 0.0299(6) Uani 1 1 d . . . H71A H 0.8496 0.3542 0.1005 0.036 Uiso 1 1 calc R . . H71B H 0.8032 0.2843 0.0706 0.036 Uiso 1 1 calc R . . C8 C 0.80065(19) 0.31796(16) 0.19201(11) 0.0278(6) Uani 1 1 d . . . C9 C 0.78024(18) 0.28141(16) 0.23939(11) 0.0266(6) Uani 1 1 d . . . C11 C 0.8981(2) 0.35233(17) 0.29062(12) 0.0307(7) Uani 1 1 d . . . H11A H 0.9364 0.3298 0.3165 0.037 Uiso 1 1 calc R . . H11B H 0.9279 0.3518 0.2577 0.037 Uiso 1 1 calc R . . C81 C 0.8436(2) 0.39735(17) 0.18912(12) 0.0307(6) Uani 1 1 d . . . H81A H 0.8152 0.4304 0.1634 0.037 Uiso 1 1 calc R . . H81B H 0.8397 0.4243 0.2222 0.037 Uiso 1 1 calc R . . C110 C 0.9419(2) 0.48315(18) 0.31306(12) 0.0379(8) Uani 1 1 d . . . C111 C 0.9181(3) 0.55929(19) 0.32327(13) 0.0445(9) Uani 1 1 d . . . H111 H 0.8596 0.5726 0.324 0.053 Uiso 1 1 calc R . . C112 C 0.9785(3) 0.6170(2) 0.33256(14) 0.0556(11) Uani 1 1 d . . . C113 C 1.0626(3) 0.5968(3) 0.33213(17) 0.0667(13) Uani 1 1 d . . . H113 H 1.1045 0.6353 0.3391 0.08 Uiso 1 1 calc R . . C114 C 1.0868(3) 0.5205(3) 0.32156(18) 0.0672(13) Uani 1 1 d . . . H114 H 1.1454 0.5074 0.3208 0.081 Uiso 1 1 calc R . . C115 C 1.0266(3) 0.4628(2) 0.31201(15) 0.0500(9) Uani 1 1 d . . . H115 H 1.0434 0.4104 0.3049 0.06 Uiso 1 1 calc R . . C116 C 0.9521(4) 0.7002(2) 0.3424(2) 0.0807(16) Uani 1 1 d . . . H11C H 0.9206 0.7029 0.3743 0.121 Uiso 1 1 calc R . . H11D H 0.916 0.7186 0.3147 0.121 Uiso 1 1 calc R . . H11E H 1.0027 0.7335 0.3447 0.121 Uiso 1 1 calc R . . C210 C 0.9251(2) 0.23047(18) 0.43783(11) 0.0308(7) Uani 1 1 d . . . C211 C 0.9784(2) 0.16635(18) 0.44497(12) 0.0346(7) Uani 1 1 d . . . H211 H 0.9869 0.1299 0.4183 0.042 Uiso 1 1 calc R . . C212 C 1.0193(2) 0.1555(2) 0.49095(13) 0.0410(8) Uani 1 1 d . . . C213 C 1.0072(2) 0.2106(2) 0.52891(13) 0.0439(8) Uani 1 1 d . . . H213 H 1.035 0.2042 0.5605 0.053 Uiso 1 1 calc R . . C214 C 0.9550(2) 0.2750(2) 0.52119(13) 0.0389(8) Uani 1 1 d . . . H214 H 0.9477 0.3121 0.5476 0.047 Uiso 1 1 calc R . . C215 C 0.9134(2) 0.28604(18) 0.47571(12) 0.0330(7) Uani 1 1 d . . . H215 H 0.8778 0.3303 0.4705 0.04 Uiso 1 1 calc R . . C216 C 1.0766(3) 0.0852(2) 0.49959(17) 0.0584(11) Uani 1 1 d . . . H21C H 1.0679 0.0469 0.4725 0.088 Uiso 1 1 calc R . . H21D H 1.0628 0.061 0.5322 0.088 Uiso 1 1 calc R . . H21E H 1.136 0.1022 0.4997 0.088 Uiso 1 1 calc R . . C710 C 0.7297(2) 0.41348(17) 0.03941(11) 0.0299(6) Uani 1 1 d . . . C711 C 0.6633(2) 0.46560(18) 0.03048(12) 0.0352(7) Uani 1 1 d . . . H711 H 0.6219 0.4746 0.0559 0.042 Uiso 1 1 calc R . . C712 C 0.6577(2) 0.50449(19) -0.01570(13) 0.0381(7) Uani 1 1 d . . . C713 C 0.7192(2) 0.49018(19) -0.05216(13) 0.0398(8) Uani 1 1 d . . . H713 H 0.7156 0.5157 -0.084 0.048 Uiso 1 1 calc R . . C714 C 0.7852(2) 0.43960(19) -0.04283(12) 0.0372(7) Uani 1 1 d . . . H714 H 0.8269 0.4311 -0.0681 0.045 Uiso 1 1 calc R . . C715 C 0.7917(2) 0.40052(17) 0.00341(11) 0.0315(7) Uani 1 1 d . . . H715 H 0.8376 0.3659 0.01 0.038 Uiso 1 1 calc R . . C716 C 0.5859(3) 0.5609(2) -0.02637(16) 0.0562(10) Uani 1 1 d . . . H71C H 0.609 0.6134 -0.0322 0.084 Uiso 1 1 calc R . . H71D H 0.5473 0.5622 0.0026 0.084 Uiso 1 1 calc R . . H71E H 0.5549 0.5436 -0.0564 0.084 Uiso 1 1 calc R . . C810 C 0.9841(2) 0.45070(18) 0.17721(11) 0.0340(7) Uani 1 1 d . . . C811 C 0.9565(2) 0.52582(18) 0.18855(11) 0.0348(7) Uani 1 1 d . . . H811 H 0.898 0.5356 0.1944 0.042 Uiso 1 1 calc R . . C812 C 1.0154(2) 0.5872(2) 0.19135(13) 0.0409(8) Uani 1 1 d . . . C813 C 1.0995(2) 0.5717(2) 0.18306(15) 0.0494(9) Uani 1 1 d . . . H813 H 1.1399 0.6128 0.1856 0.059 Uiso 1 1 calc R . . C814 C 1.1260(2) 0.4968(2) 0.17096(15) 0.0513(10) Uani 1 1 d . . . H814 H 1.1845 0.4872 0.1647 0.062 Uiso 1 1 calc R . . C815 C 1.0687(2) 0.4355(2) 0.16782(13) 0.0435(8) Uani 1 1 d . . . H815 H 1.0871 0.3841 0.1594 0.052 Uiso 1 1 calc R . . C816 C 0.9843(3) 0.6685(2) 0.20359(15) 0.0500(9) Uani 1 1 d . . . H81C H 1.0254 0.6947 0.2256 0.075 Uiso 1 1 calc R . . H81D H 0.9294 0.6652 0.2209 0.075 Uiso 1 1 calc R . . H81E H 0.9778 0.6985 0.1723 0.075 Uiso 1 1 calc R . . S11 S 0.28749(10) 0.39255(11) 0.38708(6) 0.0778(6) Uani 0.850(4) 1 d P . . S12 S 0.11332(12) 0.31973(10) 0.40832(7) 0.0866(6) Uani 0.850(4) 1 d P . . C100 C 0.2012(3) 0.3546(3) 0.39734(18) 0.0554(12) Uani 0.850(4) 1 d P . . S21 S 0.21254(12) 0.33304(12) 0.25417(7) 0.0934(8) Uani 0.889(6) 1 d P . . C200 C 0.25 0.25 0.2550(3) 0.069(2) Uani 0.889(6) 2 d SP . . S31 S 0.7602(4) 0.7005(5) 0.8829(2) 0.141(3) Uani 0.345(4) 1 d P . . S32 S 0.7489(14) 0.7574(9) 0.98957(17) 0.111(3) Uani 0.345(4) 1 d P . . C300 C 0.7525(11) 0.7332(7) 0.9354(4) 0.055(3) Uiso 0.345(4) 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 O11 0.0436(13) 0.0244(10) 0.0393(12) -0.0027(9) -0.0039(10) -0.0055(9) O21 0.0410(12) 0.0337(11) 0.0287(11) -0.0038(9) -0.0061(9) 0.0096(10) O71 0.0370(12) 0.0367(11) 0.0283(11) 0.0059(9) 0.0042(9) 0.0085(9) O81 0.0368(12) 0.0302(11) 0.0405(12) 0.0014(9) 0.0050(10) -0.0050(9) C1 0.0322(15) 0.0221(13) 0.0270(14) -0.0026(11) -0.0006(12) 0.0013(11) C2 0.0373(16) 0.0223(13) 0.0261(15) -0.0017(11) -0.0013(12) 0.0056(12) C21 0.0383(17) 0.0272(14) 0.0259(15) -0.0017(11) -0.0033(13) 0.0038(12) C7 0.0330(15) 0.0254(14) 0.0248(14) 0.0016(11) 0.0009(12) 0.0030(12) C71 0.0337(16) 0.0290(14) 0.0269(15) 0.0032(12) 0.0000(12) 0.0012(12) C8 0.0307(15) 0.0231(13) 0.0294(15) 0.0006(11) 0.0006(12) 0.0008(11) C9 0.0316(15) 0.0214(13) 0.0268(15) -0.0015(11) -0.0001(12) 0.0039(11) C11 0.0374(17) 0.0258(14) 0.0289(15) -0.0013(11) -0.0020(13) -0.0006(12) C81 0.0341(16) 0.0275(14) 0.0305(15) 0.0021(12) 0.0000(12) -0.0026(12) C110 0.056(2) 0.0303(16) 0.0278(16) 0.0031(12) -0.0095(15) -0.0120(15) C111 0.068(2) 0.0320(17) 0.0331(17) 0.0018(14) -0.0068(16) -0.0099(16) C112 0.094(3) 0.0351(19) 0.038(2) 0.0025(15) -0.015(2) -0.020(2) C113 0.078(3) 0.055(3) 0.067(3) 0.012(2) -0.026(2) -0.036(2) C114 0.057(3) 0.064(3) 0.081(3) 0.014(2) -0.021(2) -0.023(2) C115 0.050(2) 0.045(2) 0.055(2) 0.0075(17) -0.0106(18) -0.0111(17) C116 0.129(5) 0.043(2) 0.071(3) -0.007(2) -0.012(3) -0.024(3) C210 0.0312(16) 0.0350(16) 0.0262(15) 0.0025(12) 0.0005(12) -0.0031(13) C211 0.0339(16) 0.0329(16) 0.0370(17) -0.0002(13) -0.0010(13) -0.0001(13) C212 0.0378(18) 0.0406(18) 0.0445(19) 0.0087(15) -0.0048(15) -0.0011(14) C213 0.0437(19) 0.052(2) 0.0364(18) 0.0067(15) -0.0122(15) -0.0060(16) C214 0.0412(18) 0.0432(18) 0.0325(16) 0.0004(14) -0.0030(14) -0.0081(15) C215 0.0362(17) 0.0329(15) 0.0300(16) -0.0010(12) -0.0024(13) -0.0016(13) C216 0.055(2) 0.057(2) 0.063(3) 0.013(2) -0.012(2) 0.014(2) C710 0.0377(17) 0.0260(14) 0.0260(14) 0.0017(11) -0.0009(12) -0.0010(12) C711 0.0387(18) 0.0326(16) 0.0343(16) 0.0016(13) 0.0014(14) 0.0034(13) C712 0.0429(19) 0.0323(16) 0.0391(18) 0.0066(14) -0.0053(15) 0.0009(14) C713 0.049(2) 0.0379(17) 0.0329(16) 0.0094(14) -0.0020(15) -0.0012(15) C714 0.0412(18) 0.0386(17) 0.0319(16) 0.0053(13) 0.0041(14) -0.0021(14) C715 0.0339(16) 0.0302(15) 0.0305(15) 0.0034(12) 0.0005(13) 0.0003(13) C716 0.056(2) 0.056(2) 0.057(2) 0.0195(19) 0.0033(19) 0.0178(19) C810 0.0395(18) 0.0342(16) 0.0282(15) 0.0057(12) 0.0015(13) -0.0056(13) C811 0.0407(18) 0.0335(16) 0.0300(16) 0.0062(13) 0.0002(13) -0.0055(14) C812 0.050(2) 0.0394(18) 0.0335(17) 0.0087(14) -0.0030(15) -0.0118(15) C813 0.048(2) 0.048(2) 0.052(2) 0.0120(17) -0.0017(17) -0.0188(17) C814 0.040(2) 0.055(2) 0.059(2) 0.0169(18) 0.0047(17) -0.0073(17) C815 0.0422(19) 0.0433(19) 0.045(2) 0.0088(15) 0.0067(16) -0.0004(16) C816 0.064(2) 0.0371(18) 0.049(2) 0.0044(16) -0.0009(18) -0.0150(17) S11 0.0617(9) 0.0994(12) 0.0724(10) 0.0127(8) 0.0094(7) -0.0121(8) S12 0.0829(12) 0.0807(11) 0.0961(13) 0.0017(9) 0.0122(9) -0.0318(9) C100 0.069(3) 0.052(3) 0.046(3) 0.004(2) 0.002(2) 0.001(2) S21 0.0899(13) 0.1030(14) 0.0873(13) -0.0092(9) -0.0082(9) 0.0207(10) C200 0.058(4) 0.106(6) 0.042(4) 0 0 -0.001(4) S31 0.105(4) 0.229(8) 0.087(3) -0.054(4) 0.014(3) -0.019(5) S32 0.096(3) 0.147(7) 0.089(3) -0.059(6) 0.007(7) -0.004(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O11 C110 1.384(4) . ? O11 C11 1.438(3) . ? O21 C210 1.379(4) . ? O21 C21 1.438(4) . ? O71 C710 1.383(4) . ? O71 C71 1.438(4) . ? O81 C810 1.393(4) . ? O81 C81 1.437(4) . ? C1 C2 1.378(4) . ? C1 C9 1.451(4) . ? C1 C11 1.513(4) . ? C2 C2 1.420(6) 2_655 ? C2 C21 1.517(4) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C7 C8 1.375(4) . ? C7 C7 1.422(6) 2_655 ? C7 C71 1.517(4) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C8 C9 1.437(4) . ? C8 C81 1.516(4) . ? C9 C9 1.435(6) 2_655 ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C110 C111 1.379(5) . ? C110 C115 1.380(5) . ? C111 C112 1.392(5) . ? C111 H111 0.95 . ? C112 C113 1.369(7) . ? C112 C116 1.503(6) . ? C113 C114 1.386(7) . ? C113 H113 0.95 . ? C114 C115 1.392(5) . ? C114 H114 0.95 . ? C115 H115 0.95 . ? C116 H11C 0.98 . ? C116 H11D 0.98 . ? C116 H11E 0.98 . ? C210 C215 1.392(4) . ? C210 C211 1.392(4) . ? C211 C212 1.390(5) . ? C211 H211 0.95 . ? C212 C213 1.390(5) . ? C212 C216 1.519(5) . ? C213 C214 1.388(5) . ? C213 H213 0.95 . ? C214 C215 1.384(5) . ? C214 H214 0.95 . ? C215 H215 0.95 . ? C216 H21C 0.98 . ? C216 H21D 0.98 . ? C216 H21E 0.98 . ? C710 C715 1.383(4) . ? C710 C711 1.393(4) . ? C711 C712 1.393(4) . ? C711 H711 0.95 . ? C712 C713 1.390(5) . ? C712 C716 1.512(5) . ? C713 C714 1.373(5) . ? C713 H713 0.95 . ? C714 C715 1.398(4) . ? C714 H714 0.95 . ? C715 H715 0.95 . ? C716 H71C 0.98 . ? C716 H71D 0.98 . ? C716 H71E 0.98 . ? C810 C815 1.380(5) . ? C810 C811 1.386(5) . ? C811 C812 1.400(5) . ? C811 H811 0.95 . ? C812 C813 1.369(5) . ? C812 C816 1.507(5) . ? C813 C814 1.383(6) . ? C813 H813 0.95 . ? C814 C815 1.385(5) . ? C814 H814 0.95 . ? C815 H815 0.95 . ? C816 H81C 0.98 . ? C816 H81D 0.98 . ? C816 H81E 0.98 . ? S11 C100 1.531(5) . ? S12 C100 1.535(5) . ? S21 C200 1.5352(19) . ? C200 S21 1.5352(19) 2 ? S31 C300 1.502(12) . ? S31 C300 1.803(12) 2_665 ? S31 S31 1.721(16) 2_665 ? S32 S32 0.26(3) 2_665 ? S32 C300 1.444(12) 2_665 ? S32 C300 1.494(11) . ? C300 C300 0.58(2) 2_665 ? C300 S32 1.444(12) 2_665 ? C300 S31 1.803(12) 2_665 ? 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 C110 O11 C11 117.3(3) . . ? C210 O21 C21 118.1(2) . . ? C710 O71 C71 116.9(2) . . ? C810 O81 C81 117.2(2) . . ? C2 C1 C9 120.4(3) . . ? C2 C1 C11 116.8(3) . . ? C9 C1 C11 122.5(3) . . ? C1 C2 C2 120.56(18) . 2_655 ? C1 C2 C21 120.5(3) . . ? C2 C2 C21 118.89(17) 2_655 . ? O21 C21 C2 104.7(2) . . ? O21 C21 H21A 110.8 . . ? C2 C21 H21A 110.8 . . ? O21 C21 H21B 110.8 . . ? C2 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? C8 C7 C7 120.41(17) . 2_655 ? C8 C7 C71 120.1(3) . . ? C7 C7 C71 119.48(16) 2_655 . ? O71 C71 C7 106.6(2) . . ? O71 C71 H71A 110.4 . . ? C7 C71 H71A 110.4 . . ? O71 C71 H71B 110.4 . . ? C7 C71 H71B 110.4 . . ? H71A C71 H71B 108.6 . . ? C7 C8 C9 120.5(3) . . ? C7 C8 C81 117.1(3) . . ? C9 C8 C81 122.1(3) . . ? C9 C9 C8 118.24(17) 2_655 . ? C9 C9 C1 118.09(16) 2_655 . ? C8 C9 C1 123.7(3) . . ? O11 C11 C1 108.6(2) . . ? O11 C11 H11A 110 . . ? C1 C11 H11A 110 . . ? O11 C11 H11B 110 . . ? C1 C11 H11B 110 . . ? H11A C11 H11B 108.4 . . ? O81 C81 C8 108.3(2) . . ? O81 C81 H81A 110 . . ? C8 C81 H81A 110 . . ? O81 C81 H81B 110 . . ? C8 C81 H81B 110 . . ? H81A C81 H81B 108.4 . . ? C111 C110 C115 120.3(3) . . ? C111 C110 O11 115.5(3) . . ? C115 C110 O11 124.2(3) . . ? C110 C111 C112 121.1(4) . . ? C110 C111 H111 119.5 . . ? C112 C111 H111 119.5 . . ? C113 C112 C111 118.8(4) . . ? C113 C112 C116 120.5(4) . . ? C111 C112 C116 120.7(5) . . ? C112 C113 C114 120.3(4) . . ? C112 C113 H113 119.8 . . ? C114 C113 H113 119.8 . . ? C113 C114 C115 120.9(4) . . ? C113 C114 H114 119.5 . . ? C115 C114 H114 119.5 . . ? C110 C115 C114 118.6(4) . . ? C110 C115 H115 120.7 . . ? C114 C115 H115 120.7 . . ? C112 C116 H11C 109.5 . . ? C112 C116 H11D 109.5 . . ? H11C C116 H11D 109.5 . . ? C112 C116 H11E 109.5 . . ? H11C C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? O21 C210 C215 123.9(3) . . ? O21 C210 C211 115.0(3) . . ? C215 C210 C211 121.2(3) . . ? C212 C211 C210 120.2(3) . . ? C212 C211 H211 119.9 . . ? C210 C211 H211 119.9 . . ? C211 C212 C213 118.6(3) . . ? C211 C212 C216 120.9(3) . . ? C213 C212 C216 120.5(3) . . ? C214 C213 C212 120.7(3) . . ? C214 C213 H213 119.6 . . ? C212 C213 H213 119.6 . . ? C215 C214 C213 121.2(3) . . ? C215 C214 H214 119.4 . . ? C213 C214 H214 119.4 . . ? C214 C215 C210 118.1(3) . . ? C214 C215 H215 121 . . ? C210 C215 H215 121 . . ? C212 C216 H21C 109.5 . . ? C212 C216 H21D 109.5 . . ? H21C C216 H21D 109.5 . . ? C212 C216 H21E 109.5 . . ? H21C C216 H21E 109.5 . . ? H21D C216 H21E 109.5 . . ? O71 C710 C715 123.9(3) . . ? O71 C710 C711 115.0(3) . . ? C715 C710 C711 121.1(3) . . ? C710 C711 C712 120.0(3) . . ? C710 C711 H711 120 . . ? C712 C711 H711 120 . . ? C713 C712 C711 118.8(3) . . ? C713 C712 C716 120.3(3) . . ? C711 C712 C716 121.0(3) . . ? C714 C713 C712 120.9(3) . . ? C714 C713 H713 119.5 . . ? C712 C713 H713 119.5 . . ? C713 C714 C715 120.9(3) . . ? C713 C714 H714 119.6 . . ? C715 C714 H714 119.6 . . ? C710 C715 C714 118.3(3) . . ? C710 C715 H715 120.8 . . ? C714 C715 H715 120.8 . . ? C712 C716 H71C 109.5 . . ? C712 C716 H71D 109.5 . . ? H71C C716 H71D 109.5 . . ? C712 C716 H71E 109.5 . . ? H71C C716 H71E 109.5 . . ? H71D C716 H71E 109.5 . . ? C815 C810 C811 121.1(3) . . ? C815 C810 O81 115.2(3) . . ? C811 C810 O81 123.8(3) . . ? C810 C811 C812 119.7(3) . . ? C810 C811 H811 120.2 . . ? C812 C811 H811 120.2 . . ? C813 C812 C811 119.3(3) . . ? C813 C812 C816 121.7(3) . . ? C811 C812 C816 119.0(3) . . ? C812 C813 C814 120.5(3) . . ? C812 C813 H813 119.7 . . ? C814 C813 H813 119.7 . . ? C813 C814 C815 121.0(4) . . ? C813 C814 H814 119.5 . . ? C815 C814 H814 119.5 . . ? C810 C815 C814 118.5(3) . . ? C810 C815 H815 120.7 . . ? C814 C815 H815 120.7 . . ? C812 C816 H81C 109.5 . . ? C812 C816 H81D 109.5 . . ? H81C C816 H81D 109.5 . . ? C812 C816 H81E 109.5 . . ? H81C C816 H81E 109.5 . . ? H81D C816 H81E 109.5 . . ? S11 C100 S12 177.7(4) . . ? S21 C200 S21 178.4(5) . 2 ? S32 C300 S31 173.7(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C2 -0.8(5) . . . 2_655 ? C11 C1 C2 C2 -174.3(3) . . . 2_655 ? C9 C1 C2 C21 177.0(3) . . . . ? C11 C1 C2 C21 3.5(4) . . . . ? C210 O21 C21 C2 -172.3(2) . . . . ? C1 C2 C21 O21 -93.8(3) . . . . ? C2 C2 C21 O21 84.1(4) 2_655 . . . ? C710 O71 C71 C7 -175.2(2) . . . . ? C8 C7 C71 O71 -91.7(3) . . . . ? C7 C7 C71 O71 87.6(4) 2_655 . . . ? C7 C7 C8 C9 0.7(5) 2_655 . . . ? C71 C7 C8 C9 180.0(3) . . . . ? C7 C7 C8 C81 -173.3(3) 2_655 . . . ? C71 C7 C8 C81 6.0(4) . . . . ? C7 C8 C9 C9 -10.9(5) . . . 2_655 ? C81 C8 C9 C9 162.8(3) . . . 2_655 ? C7 C8 C9 C1 168.8(3) . . . . ? C81 C8 C9 C1 -17.5(4) . . . . ? C2 C1 C9 C9 -10.7(5) . . . 2_655 ? C11 C1 C9 C9 162.3(3) . . . 2_655 ? C2 C1 C9 C8 169.5(3) . . . . ? C11 C1 C9 C8 -17.4(4) . . . . ? C110 O11 C11 C1 174.9(2) . . . . ? C2 C1 C11 O11 -82.3(3) . . . . ? C9 C1 C11 O11 104.4(3) . . . . ? C810 O81 C81 C8 -172.3(2) . . . . ? C7 C8 C81 O81 -81.6(3) . . . . ? C9 C8 C81 O81 104.5(3) . . . . ? C11 O11 C110 C111 176.8(3) . . . . ? C11 O11 C110 C115 -2.9(4) . . . . ? C115 C110 C111 C112 0.2(5) . . . . ? O11 C110 C111 C112 -179.5(3) . . . . ? C110 C111 C112 C113 -0.9(6) . . . . ? C110 C111 C112 C116 178.5(4) . . . . ? C111 C112 C113 C114 1.3(6) . . . . ? C116 C112 C113 C114 -178.1(4) . . . . ? C112 C113 C114 C115 -1.0(7) . . . . ? C111 C110 C115 C114 0.1(5) . . . . ? O11 C110 C115 C114 179.8(3) . . . . ? C113 C114 C115 C110 0.3(6) . . . . ? C21 O21 C210 C215 -0.5(4) . . . . ? C21 O21 C210 C211 178.3(3) . . . . ? O21 C210 C211 C212 -177.0(3) . . . . ? C215 C210 C211 C212 1.8(5) . . . . ? C210 C211 C212 C213 -1.3(5) . . . . ? C210 C211 C212 C216 179.0(3) . . . . ? C211 C212 C213 C214 0.4(5) . . . . ? C216 C212 C213 C214 180.0(3) . . . . ? C212 C213 C214 C215 0.2(5) . . . . ? C213 C214 C215 C210 0.2(5) . . . . ? O21 C210 C215 C214 177.5(3) . . . . ? C211 C210 C215 C214 -1.2(5) . . . . ? C71 O71 C710 C715 4.4(4) . . . . ? C71 O71 C710 C711 -177.1(3) . . . . ? O71 C710 C711 C712 -177.2(3) . . . . ? C715 C710 C711 C712 1.3(5) . . . . ? C710 C711 C712 C713 0.0(5) . . . . ? C710 C711 C712 C716 179.6(3) . . . . ? C711 C712 C713 C714 -0.9(5) . . . . ? C716 C712 C713 C714 179.5(3) . . . . ? C712 C713 C714 C715 0.7(5) . . . . ? O71 C710 C715 C714 176.8(3) . . . . ? C711 C710 C715 C714 -1.6(5) . . . . ? C713 C714 C715 C710 0.6(5) . . . . ? C81 O81 C810 C815 175.2(3) . . . . ? C81 O81 C810 C811 -3.0(4) . . . . ? C815 C810 C811 C812 -1.0(5) . . . . ? O81 C810 C811 C812 177.2(3) . . . . ? C810 C811 C812 C813 -0.3(5) . . . . ? C810 C811 C812 C816 179.8(3) . . . . ? C811 C812 C813 C814 1.4(5) . . . . ? C816 C812 C813 C814 -178.8(3) . . . . ? C812 C813 C814 C815 -1.1(6) . . . . ? C811 C810 C815 C814 1.3(5) . . . . ? O81 C810 C815 C814 -177.1(3) . . . . ? C813 C814 C815 C810 -0.2(6) . . . . ? C300 S32 C300 S31 -2(2) 2_665 . . 2_665 ? S31 S31 C300 C300 -3(4) 2_665 . . 2_665 ? C300 S31 C300 S32 -174(9) 2_665 . . 2_665 ? S31 S31 C300 S32 -177(6) 2_665 . . 2_665 ? C300 S31 C300 S31 3(4) 2_665 . . 2_665 ? #------------------ SECTION 3. ----------------------------------------------# data_7-DMSO _database_code_depnum_ccdc_archive 'CCDC 771698' #TrackingRef '- archive_full.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C74 H72 O16 S8, 2(C2 H6 O S)' _chemical_formula_sum 'C78 H84 O18 S10' _chemical_formula_weight 1630.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3025(4) _cell_length_b 15.9172(6) _cell_length_c 17.7176(5) _cell_angle_alpha 92.3031(18) _cell_angle_beta 97.8882(19) _cell_angle_gamma 115.4395(16) _cell_volume 3836.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13899 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8644 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details ; R. H. Blessing, Acta Cryst. (1995), A51, 33-38 ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.684112E-1 _diffrn_orient_matrix_ub_12 0.139147E-1 _diffrn_orient_matrix_ub_13 -0.7101E-2 _diffrn_orient_matrix_ub_21 0.227593E-1 _diffrn_orient_matrix_ub_22 0.01642 _diffrn_orient_matrix_ub_23 0.565966E-1 _diffrn_orient_matrix_ub_31 -0.140302E-1 _diffrn_orient_matrix_ub_32 -0.666112E-1 _diffrn_orient_matrix_ub_33 0.57901E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_unetI/netI 0.0779 _diffrn_reflns_number 54852 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.11 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 14970 _reflns_number_gt 9618 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0994P)^2^+5.2159P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14970 _refine_ls_number_parameters 966 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.491 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.38033(8) 0.16883(8) 0.56388(6) 0.0396(3) Uani 1 1 d . . . S21 S 0.17053(8) 0.21486(9) 0.71265(8) 0.0497(3) Uani 1 1 d . . . S31 S 0.20155(8) -0.02687(9) 0.85892(8) 0.0500(3) Uani 1 1 d . . . S41 S 0.40939(8) 0.28351(8) 0.99982(6) 0.0396(3) Uani 1 1 d . . . S51 S 0.58129(8) 0.01780(7) 0.88583(6) 0.0338(2) Uani 1 1 d . . . S61 S 0.78866(8) 0.34083(8) 1.00041(6) 0.0371(3) Uani 1 1 d . . . S71 S 0.83670(7) 0.28675(8) 0.73622(6) 0.0371(3) Uani 1 1 d . . . S81 S 0.64406(8) 0.45131(8) 0.67927(6) 0.0372(3) Uani 1 1 d . . . O11 O 0.4733(2) 0.1725(2) 0.55374(16) 0.0435(7) Uani 1 1 d . . . O12 O 0.3013(2) 0.0787(2) 0.56942(17) 0.0442(7) Uani 1 1 d . . . O21 O 0.2174(3) 0.2901(3) 0.6683(3) 0.0702(11) Uani 1 1 d . . . O22 O 0.1710(2) 0.2366(2) 0.7919(2) 0.0577(9) Uani 1 1 d . . . O31 O 0.1738(3) -0.0623(2) 0.7789(2) 0.0653(10) Uani 1 1 d . . . O32 O 0.2793(2) -0.0395(2) 0.9048(2) 0.0553(9) Uani 1 1 d . . . O41 O 0.3055(2) 0.2588(2) 0.98490(18) 0.0459(8) Uani 1 1 d . . . O42 O 0.4593(3) 0.3078(3) 1.07831(17) 0.0553(9) Uani 1 1 d . . . O51 O 0.6840(2) 0.0430(2) 0.88749(16) 0.0401(7) Uani 1 1 d . . . O52 O 0.5242(2) -0.0647(2) 0.91958(16) 0.0433(7) Uani 1 1 d . . . O61 O 0.8230(2) 0.4291(2) 0.96912(17) 0.0457(8) Uani 1 1 d . . . O62 O 0.7023(2) 0.3108(2) 1.03615(16) 0.0455(8) Uani 1 1 d . . . O71 O 0.8270(2) 0.2072(2) 0.77563(18) 0.0445(7) Uani 1 1 d . . . O72 O 0.7912(2) 0.2695(3) 0.65665(17) 0.0554(9) Uani 1 1 d . . . O81 O 0.7219(2) 0.5056(2) 0.74166(18) 0.0453(8) Uani 1 1 d . . . O82 O 0.5519(2) 0.4556(2) 0.67540(17) 0.0441(7) Uani 1 1 d . . . C1 C 0.4104(3) 0.2160(3) 0.7246(2) 0.0317(9) Uani 1 1 d . . . C2 C 0.3243(3) 0.1653(3) 0.7535(2) 0.0335(9) Uani 1 1 d . . . C3 C 0.3263(3) 0.1469(3) 0.8315(2) 0.0350(9) Uani 1 1 d . . . C4 C 0.4160(3) 0.1724(3) 0.8773(2) 0.0320(9) Uani 1 1 d . . . C5 C 0.5853(3) 0.1920(3) 0.8837(2) 0.0294(8) Uani 1 1 d . . . C6 C 0.6773(3) 0.2452(3) 0.8677(2) 0.0289(8) Uani 1 1 d . . . C7 C 0.6862(3) 0.2958(3) 0.8020(2) 0.0292(8) Uani 1 1 d . . . C8 C 0.6034(3) 0.2863(3) 0.7505(2) 0.0303(9) Uani 1 1 d . . . C9 C 0.5051(3) 0.2361(3) 0.7701(2) 0.0296(8) Uani 1 1 d . . . C10 C 0.5024(3) 0.2013(3) 0.8434(2) 0.0288(8) Uani 1 1 d . . . C11 C 0.3969(3) 0.2487(3) 0.6457(2) 0.0358(9) Uani 1 1 d . . . H11A H 0.4551 0.3082 0.6435 0.043 Uiso 1 1 calc R . . H11B H 0.3392 0.2623 0.6409 0.043 Uiso 1 1 calc R . . C21 C 0.2234(3) 0.1333(3) 0.7040(3) 0.0402(10) Uani 1 1 d . . . H21A H 0.1781 0.0723 0.7185 0.048 Uiso 1 1 calc R . . H21B H 0.229 0.1236 0.6497 0.048 Uiso 1 1 calc R . . C31 C 0.2337(3) 0.0958(3) 0.8653(3) 0.0430(11) Uani 1 1 d . . . H31A H 0.1792 0.1059 0.837 0.052 Uiso 1 1 calc R . . H31B H 0.2448 0.1208 0.9196 0.052 Uiso 1 1 calc R . . C41 C 0.4293(3) 0.1859(3) 0.9648(2) 0.0343(9) Uani 1 1 d . . . H41A H 0.4967 0.1963 0.9867 0.041 Uiso 1 1 calc R . . H41B H 0.3827 0.1281 0.9828 0.041 Uiso 1 1 calc R . . C51 C 0.5662(3) 0.1125(3) 0.9328(2) 0.0330(9) Uani 1 1 d . . . H51A H 0.4985 0.0888 0.9439 0.04 Uiso 1 1 calc R . . H51B H 0.6122 0.136 0.9822 0.04 Uiso 1 1 calc R . . C61 C 0.7655(3) 0.2527(3) 0.9236(2) 0.0330(9) Uani 1 1 d . . . H61A H 0.8235 0.2706 0.8979 0.04 Uiso 1 1 calc R . . H61B H 0.7516 0.1919 0.9437 0.04 Uiso 1 1 calc R . . C71 C 0.7901(3) 0.3546(3) 0.7873(2) 0.0326(9) Uani 1 1 d . . . H71A H 0.8342 0.3834 0.837 0.039 Uiso 1 1 calc R . . H71B H 0.7902 0.4057 0.7572 0.039 Uiso 1 1 calc R . . C81 C 0.6238(3) 0.3308(3) 0.6764(2) 0.0330(9) Uani 1 1 d . . . H81A H 0.5676 0.2933 0.6352 0.04 Uiso 1 1 calc R . . H81B H 0.6824 0.3268 0.6623 0.04 Uiso 1 1 calc R . . C111 C 0.3397(4) 0.2182(4) 0.4864(3) 0.0515(13) Uani 1 1 d . . . C112 C 0.2399(5) 0.1937(4) 0.4686(3) 0.0671(16) Uani 1 1 d . . . H112 H 0.1956 0.1539 0.4987 0.08 Uiso 1 1 calc R . . C113 C 0.2054(6) 0.2284(5) 0.4057(4) 0.082(2) Uani 1 1 d . . . C114 C 0.2721(7) 0.2871(5) 0.3659(4) 0.086(2) Uani 1 1 d . . . H114 H 0.2494 0.312 0.3239 0.103 Uiso 1 1 calc R . . C115 C 0.3710(6) 0.3121(5) 0.3837(3) 0.080(2) Uani 1 1 d . . . H115 H 0.4155 0.3534 0.3545 0.096 Uiso 1 1 calc R . . C116 C 0.4051(5) 0.2760(4) 0.4453(3) 0.0609(14) Uani 1 1 d . . . H116 H 0.473 0.2916 0.4583 0.073 Uiso 1 1 calc R . . C117 C 0.0959(6) 0.1987(6) 0.3853(4) 0.121(3) Uani 1 1 d . . . H11C H 0.0785 0.2409 0.4149 0.181 Uiso 1 1 calc R . . H11D H 0.0598 0.1345 0.3976 0.181 Uiso 1 1 calc R . . H11E H 0.0786 0.2013 0.3304 0.181 Uiso 1 1 calc R . . C211 C 0.0486(3) 0.1481(4) 0.6659(3) 0.0590(14) Uani 1 1 d . . . C212 C -0.0206(4) 0.0975(4) 0.7092(4) 0.0697(17) Uani 1 1 d . . . H212 H -0.0035 0.0999 0.7631 0.084 Uiso 1 1 calc R . . C213 C -0.1201(4) 0.0408(4) 0.6703(5) 0.081(2) Uani 1 1 d . . . C214 C -0.1364(5) 0.0407(5) 0.5923(6) 0.095(3) Uani 1 1 d . . . H214 H -0.201 0.0027 0.5656 0.114 Uiso 1 1 calc R . . C215 C -0.0678(6) 0.0904(7) 0.5502(5) 0.111(3) Uani 1 1 d . . . H215 H -0.0844 0.0875 0.4962 0.133 Uiso 1 1 calc R . . C216 C 0.0264(5) 0.1450(5) 0.5875(4) 0.0815(19) Uani 1 1 d . . . H216 H 0.0761 0.1805 0.5593 0.098 Uiso 1 1 calc R . . C217 C -0.1944(4) -0.0154(5) 0.7174(6) 0.131(4) Uani 1 1 d . . . H21C H -0.2606 -0.0347 0.6885 0.196 Uiso 1 1 calc R . . H21D H -0.186 0.0227 0.7651 0.196 Uiso 1 1 calc R . . H21E H -0.1854 -0.0711 0.7294 0.196 Uiso 1 1 calc R . . C311 C 0.0967(4) -0.0747(4) 0.9037(4) 0.0615(15) Uani 1 1 d . . . C312 C 0.0041(4) -0.1087(5) 0.8592(5) 0.101(3) Uani 1 1 d . . . H312 H -0.0041 -0.1055 0.8054 0.121 Uiso 1 1 calc R . . C313 C -0.0778(5) -0.1483(6) 0.8972(7) 0.121(3) Uani 1 1 d . . . C314 C -0.0640(7) -0.1519(6) 0.9751(8) 0.123(4) Uani 1 1 d . . . H314 H -0.12 -0.1779 0.9995 0.148 Uiso 1 1 calc R . . C315 C 0.0266(6) -0.1197(5) 1.0182(5) 0.098(3) Uani 1 1 d . . . H315 H 0.0344 -0.1236 1.0719 0.117 Uiso 1 1 calc R . . C316 C 0.1091(4) -0.0800(4) 0.9813(4) 0.0729(17) Uani 1 1 d . . . H316 H 0.1734 -0.0571 1.0103 0.087 Uiso 1 1 calc R . . C317 C -0.1735(9) -0.1933(15) 0.8639(8) 0.280(11) Uani 1 1 d . . . H31C H -0.1781 -0.2058 0.8085 0.42 Uiso 1 1 calc R . . H31D H -0.2065 -0.1541 0.8735 0.42 Uiso 1 1 calc R . . H31E H -0.2051 -0.2527 0.8856 0.42 Uiso 1 1 calc R . . C411 C 0.4697(3) 0.3731(3) 0.9450(3) 0.0390(10) Uani 1 1 d . . . C412 C 0.4163(4) 0.3911(3) 0.8842(3) 0.0466(11) Uani 1 1 d . . . H412 H 0.3471 0.3553 0.8718 0.056 Uiso 1 1 calc R . . C413 C 0.4659(5) 0.4632(4) 0.8409(3) 0.0577(14) Uani 1 1 d . . . C414 C 0.5679(5) 0.5111(4) 0.8615(4) 0.0647(16) Uani 1 1 d . . . H414 H 0.6028 0.5602 0.8327 0.078 Uiso 1 1 calc R . . C415 C 0.6195(4) 0.4913(4) 0.9202(4) 0.0674(16) Uani 1 1 d . . . H415 H 0.689 0.5248 0.9313 0.081 Uiso 1 1 calc R . . C416 C 0.5712(4) 0.4232(4) 0.9631(3) 0.0535(13) Uani 1 1 d . . . H416 H 0.6065 0.4098 1.0055 0.064 Uiso 1 1 calc R . . C417 C 0.4146(5) 0.4916(5) 0.7801(4) 0.089(2) Uani 1 1 d . . . H41C H 0.3871 0.5303 0.8025 0.134 Uiso 1 1 calc R . . H41D H 0.3614 0.436 0.7496 0.134 Uiso 1 1 calc R . . H41E H 0.4606 0.5279 0.7471 0.134 Uiso 1 1 calc R . . C511 C 0.5253(3) 0.0064(3) 0.7896(2) 0.0325(9) Uani 1 1 d . . . C512 C 0.5842(3) 0.0333(3) 0.7335(2) 0.0336(9) Uani 1 1 d . . . H512 H 0.6537 0.06 0.7471 0.04 Uiso 1 1 calc R . . C513 C 0.5403(3) 0.0206(3) 0.6572(2) 0.0345(9) Uani 1 1 d . . . C514 C 0.4389(3) -0.0144(3) 0.6407(2) 0.0369(10) Uani 1 1 d . . . H514 H 0.4082 -0.022 0.5888 0.044 Uiso 1 1 calc R . . C515 C 0.3807(3) -0.0385(3) 0.6971(2) 0.0397(10) Uani 1 1 d . . . H515 H 0.3115 -0.0615 0.6837 0.048 Uiso 1 1 calc R . . C516 C 0.4232(3) -0.0293(3) 0.7722(2) 0.0379(10) Uani 1 1 d . . . H516 H 0.3842 -0.0466 0.8114 0.045 Uiso 1 1 calc R . . C517 C 0.6021(3) 0.0455(3) 0.5941(2) 0.0430(11) Uani 1 1 d . . . H51C H 0.5975 -0.0119 0.5676 0.064 Uiso 1 1 calc R . . H51D H 0.6708 0.0861 0.6165 0.064 Uiso 1 1 calc R . . H51E H 0.5779 0.0784 0.5574 0.064 Uiso 1 1 calc R . . C611 C 0.8864(3) 0.3422(3) 1.0676(2) 0.0411(10) Uani 1 1 d . . . C612 C 0.8656(4) 0.3070(3) 1.1367(3) 0.0483(12) Uani 1 1 d . . . H612 H 0.7995 0.2771 1.1448 0.058 Uiso 1 1 calc R . . C613 C 0.9413(4) 0.3154(4) 1.1940(3) 0.0555(13) Uani 1 1 d . . . C614 C 1.0355(4) 0.3568(4) 1.1779(4) 0.0692(17) Uani 1 1 d . . . H614 H 1.0885 0.3626 1.216 0.083 Uiso 1 1 calc R . . C615 C 1.0554(4) 0.3897(5) 1.1091(4) 0.0739(18) Uani 1 1 d . . . H615 H 1.1213 0.4167 1.1002 0.089 Uiso 1 1 calc R . . C616 C 0.9808(3) 0.3842(4) 1.0523(3) 0.0552(13) Uani 1 1 d . . . H616 H 0.9941 0.4083 1.0048 0.066 Uiso 1 1 calc R . . C617 C 0.9218(5) 0.2859(4) 1.2710(3) 0.0780(19) Uani 1 1 d . . . H61C H 0.972 0.2676 1.2944 0.117 Uiso 1 1 calc R . . H61D H 0.8568 0.2325 1.2658 0.117 Uiso 1 1 calc R . . H61E H 0.9236 0.338 1.3037 0.117 Uiso 1 1 calc R . . C711 C 0.9618(3) 0.3639(3) 0.7448(3) 0.0450(11) Uani 1 1 d . . . C712 C 1.0246(3) 0.3651(4) 0.8102(3) 0.0575(14) Uani 1 1 d . . . H712 H 0.999 0.323 0.8467 0.069 Uiso 1 1 calc R . . C713 C 1.1227(4) 0.4258(5) 0.8227(5) 0.085(2) Uani 1 1 d . . . C714 C 1.1545(5) 0.4840(6) 0.7665(8) 0.122(4) Uani 1 1 d . . . H714 H 1.2222 0.5268 0.7736 0.147 Uiso 1 1 calc R . . C715 C 1.0947(6) 0.4842(5) 0.7007(6) 0.111(3) Uani 1 1 d . . . H715 H 1.1212 0.5259 0.664 0.133 Uiso 1 1 calc R . . C716 C 0.9936(4) 0.4219(4) 0.6885(4) 0.0761(18) Uani 1 1 d . . . H716 H 0.95 0.4199 0.644 0.091 Uiso 1 1 calc R . . C717 C 1.1906(5) 0.4282(6) 0.8921(5) 0.128(4) Uani 1 1 d . . . H71C H 1.2564 0.478 0.8915 0.192 Uiso 1 1 calc R . . H71D H 1.1932 0.3678 0.8927 0.192 Uiso 1 1 calc R . . H71E H 1.1669 0.4405 0.9381 0.192 Uiso 1 1 calc R . . C811 C 0.6846(4) 0.4848(3) 0.5912(3) 0.0503(12) Uani 1 1 d . . . C812 C 0.7829(4) 0.5177(4) 0.5882(3) 0.0645(15) Uani 1 1 d . . . H812 H 0.8286 0.5198 0.6312 0.077 Uiso 1 1 calc R . . C813 C 0.8147(4) 0.5499(4) 0.5145(4) 0.0679(16) Uani 1 1 d . . . C814 C 0.7417(5) 0.5415(4) 0.4574(4) 0.0701(16) Uani 1 1 d . . . H814 H 0.7615 0.5611 0.41 0.084 Uiso 1 1 calc R . . C815 C 0.6480(6) 0.5102(5) 0.4589(4) 0.0780(18) Uani 1 1 d . . . H815 H 0.603 0.5075 0.4151 0.094 Uiso 1 1 calc R . . C816 C 0.6165(5) 0.4804(4) 0.5286(3) 0.0630(15) Uani 1 1 d . . . H816 H 0.5491 0.4575 0.5327 0.076 Uiso 1 1 calc R . . C817 C 0.9187(5) 0.5848(6) 0.5116(5) 0.104(3) Uani 1 1 d . . . H81C H 0.9301 0.5366 0.4843 0.156 Uiso 1 1 calc R . . H81D H 0.9561 0.6003 0.5639 0.156 Uiso 1 1 calc R . . H81E H 0.9403 0.641 0.4847 0.156 Uiso 1 1 calc R . . S10 S 0.45588(14) 0.76141(12) 0.71581(9) 0.0758(5) Uani 1 1 d . . . O100 O 0.4283(4) 0.6701(3) 0.6692(2) 0.0987(15) Uani 1 1 d . . . C100 C 0.5722(4) 0.7929(4) 0.7714(3) 0.0724(16) Uani 1 1 d . . . H10A H 0.6221 0.8117 0.7381 0.109 Uiso 1 1 calc R . . H10B H 0.5718 0.7392 0.7968 0.109 Uiso 1 1 calc R . . H10C H 0.5875 0.8451 0.8101 0.109 Uiso 1 1 calc R . . C101 C 0.3851(5) 0.7322(4) 0.7911(4) 0.0761(17) Uani 1 1 d . . . H10D H 0.3158 0.7124 0.7699 0.114 Uiso 1 1 calc R . . H10E H 0.4083 0.787 0.829 0.114 Uiso 1 1 calc R . . H10F H 0.3924 0.681 0.8158 0.114 Uiso 1 1 calc R . . S20A S 0.22935(18) 0.71857(18) 0.57954(15) 0.0681(10) Uani 0.695(6) 1 d P A 1 O20A O 0.1425(7) 0.6246(7) 0.5630(5) 0.112(2) Uiso 0.695(6) 1 d P A 1 C20A C 0.3180(4) 0.7244(4) 0.5237(3) 0.0671(15) Uani 0.695(6) 1 d P A 1 H2AA H 0.3507 0.6868 0.5438 0.101 Uiso 0.695(6) 1 calc PR A 1 H2AB H 0.3668 0.7897 0.5257 0.101 Uiso 0.695(6) 1 calc PR A 1 H2AC H 0.286 0.7001 0.4704 0.101 Uiso 0.695(6) 1 calc PR A 1 C21A C 0.1872(5) 0.7916(5) 0.5290(4) 0.0826(19) Uani 0.695(6) 1 d P A 1 H2AD H 0.1353 0.7969 0.5527 0.124 Uiso 0.695(6) 1 calc PR A 1 H2AE H 0.1611 0.7644 0.4755 0.124 Uiso 0.695(6) 1 calc PR A 1 H2AF H 0.2419 0.8538 0.5309 0.124 Uiso 0.695(6) 1 calc PR A 1 S20B S 0.1965(5) 0.6775(5) 0.5279(5) 0.088(3) Uiso 0.305(6) 1 d P A 2 O20B O 0.1888(15) 0.6575(15) 0.6116(13) 0.112(2) Uiso 0.305(6) 1 d P A 2 C20B C 0.3180(4) 0.7244(4) 0.5237(3) 0.0671(15) Uani 0.305(6) 1 d P A 2 H2BA H 0.3403 0.6752 0.5258 0.101 Uiso 0.305(6) 1 calc PR A 2 H2BB H 0.3547 0.7726 0.5671 0.101 Uiso 0.305(6) 1 calc PR A 2 H2BC H 0.3293 0.7526 0.4756 0.101 Uiso 0.305(6) 1 calc PR A 2 C21B C 0.1872(5) 0.7916(5) 0.5290(4) 0.0826(19) Uani 0.305(6) 1 d P A 2 H2BD H 0.1202 0.7805 0.534 0.124 Uiso 0.305(6) 1 calc PR A 2 H2BE H 0.203 0.8187 0.4812 0.124 Uiso 0.305(6) 1 calc PR A 2 H2BF H 0.2335 0.835 0.5725 0.124 Uiso 0.305(6) 1 calc PR A 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 S11 0.0401(6) 0.0411(7) 0.0358(6) 0.0007(5) -0.0029(5) 0.0192(5) S21 0.0278(6) 0.0475(8) 0.0705(9) -0.0025(6) -0.0023(6) 0.0173(5) S31 0.0362(6) 0.0367(7) 0.0728(9) 0.0042(6) 0.0263(6) 0.0074(5) S41 0.0403(6) 0.0419(7) 0.0416(6) 0.0038(5) 0.0144(5) 0.0207(5) S51 0.0399(6) 0.0355(6) 0.0311(5) 0.0076(4) 0.0101(4) 0.0197(5) S61 0.0329(6) 0.0435(7) 0.0335(5) -0.0003(5) 0.0018(4) 0.0171(5) S71 0.0264(5) 0.0431(7) 0.0383(6) 0.0020(5) 0.0083(4) 0.0113(5) S81 0.0377(6) 0.0325(6) 0.0400(6) 0.0077(5) 0.0112(5) 0.0126(5) O11 0.0440(18) 0.0461(19) 0.0407(17) -0.0019(14) 0.0040(14) 0.0214(15) O12 0.0387(17) 0.0388(18) 0.0501(18) 0.0002(14) -0.0024(14) 0.0157(15) O21 0.052(2) 0.058(2) 0.112(3) 0.029(2) 0.021(2) 0.0306(19) O22 0.0430(19) 0.058(2) 0.071(2) -0.0148(18) -0.0043(17) 0.0270(17) O31 0.057(2) 0.042(2) 0.081(3) -0.0061(19) 0.0232(19) 0.0045(17) O32 0.0412(18) 0.047(2) 0.084(2) 0.0179(18) 0.0312(17) 0.0188(16) O41 0.0384(17) 0.0435(19) 0.062(2) 0.0078(15) 0.0236(15) 0.0195(15) O42 0.075(2) 0.066(2) 0.0377(17) -0.0033(16) 0.0096(16) 0.044(2) O51 0.0424(17) 0.0510(19) 0.0358(16) 0.0054(14) 0.0075(13) 0.0284(15) O52 0.0566(19) 0.0389(18) 0.0403(16) 0.0122(14) 0.0164(14) 0.0234(15) O61 0.0480(18) 0.0422(19) 0.0455(18) 0.0011(15) 0.0000(15) 0.0211(15) O62 0.0372(17) 0.059(2) 0.0405(17) -0.0032(15) 0.0077(14) 0.0218(16) O71 0.0389(17) 0.0416(18) 0.0529(19) 0.0064(15) 0.0168(14) 0.0147(14) O72 0.053(2) 0.083(3) 0.0359(17) -0.0050(17) 0.0037(15) 0.0377(19) O81 0.0398(17) 0.0382(18) 0.0515(19) 0.0006(15) 0.0058(15) 0.0119(14) O82 0.0425(17) 0.0419(18) 0.0509(18) 0.0062(15) 0.0042(14) 0.0225(15) C1 0.027(2) 0.029(2) 0.035(2) -0.0019(17) -0.0001(17) 0.0099(17) C2 0.025(2) 0.028(2) 0.044(2) 0.0006(18) 0.0019(18) 0.0100(17) C3 0.029(2) 0.032(2) 0.044(2) 0.0044(19) 0.0116(18) 0.0116(18) C4 0.029(2) 0.026(2) 0.039(2) 0.0043(17) 0.0095(18) 0.0091(17) C5 0.029(2) 0.027(2) 0.030(2) 0.0018(17) 0.0058(16) 0.0103(17) C6 0.025(2) 0.029(2) 0.031(2) -0.0021(17) 0.0034(16) 0.0117(17) C7 0.0241(19) 0.028(2) 0.032(2) 0.0001(17) 0.0051(16) 0.0079(17) C8 0.028(2) 0.031(2) 0.031(2) 0.0017(17) 0.0052(17) 0.0125(18) C9 0.027(2) 0.026(2) 0.034(2) 0.0031(17) 0.0067(17) 0.0102(17) C10 0.0239(19) 0.026(2) 0.034(2) 0.0009(17) 0.0035(16) 0.0090(16) C11 0.029(2) 0.035(2) 0.040(2) 0.0036(19) 0.0009(18) 0.0138(19) C21 0.026(2) 0.040(3) 0.052(3) 0.003(2) 0.0030(19) 0.0127(19) C31 0.028(2) 0.039(3) 0.058(3) 0.004(2) 0.014(2) 0.009(2) C41 0.033(2) 0.037(2) 0.039(2) 0.0057(19) 0.0113(18) 0.0191(19) C51 0.034(2) 0.034(2) 0.032(2) 0.0033(18) 0.0089(18) 0.0161(19) C61 0.028(2) 0.042(3) 0.028(2) 0.0016(18) 0.0031(17) 0.0153(19) C71 0.0204(19) 0.037(2) 0.036(2) 0.0009(18) 0.0044(16) 0.0087(17) C81 0.030(2) 0.032(2) 0.035(2) 0.0057(18) 0.0075(17) 0.0101(18) C111 0.069(3) 0.051(3) 0.037(2) -0.005(2) -0.010(2) 0.034(3) C112 0.080(4) 0.079(4) 0.053(3) -0.004(3) -0.016(3) 0.053(4) C113 0.114(6) 0.087(5) 0.063(4) -0.016(4) -0.030(4) 0.074(5) C114 0.157(8) 0.069(5) 0.050(4) -0.005(3) -0.018(4) 0.077(5) C115 0.135(6) 0.066(4) 0.052(3) 0.010(3) 0.004(4) 0.060(4) C116 0.084(4) 0.060(4) 0.042(3) 0.007(3) 0.006(3) 0.036(3) C117 0.134(7) 0.137(7) 0.106(6) -0.030(5) -0.071(5) 0.102(6) C211 0.031(3) 0.061(4) 0.081(4) -0.010(3) -0.007(3) 0.023(2) C212 0.039(3) 0.058(4) 0.107(5) -0.019(3) 0.001(3) 0.023(3) C213 0.039(3) 0.066(4) 0.138(7) -0.020(4) 0.005(4) 0.029(3) C214 0.050(4) 0.087(5) 0.131(7) -0.040(5) -0.026(4) 0.031(4) C215 0.082(5) 0.146(8) 0.106(6) -0.016(6) -0.035(5) 0.067(6) C216 0.058(4) 0.110(6) 0.079(4) -0.002(4) -0.012(3) 0.048(4) C217 0.036(3) 0.068(5) 0.277(12) -0.007(6) 0.026(5) 0.014(3) C311 0.038(3) 0.037(3) 0.106(5) 0.004(3) 0.036(3) 0.007(2) C312 0.043(4) 0.092(5) 0.139(7) -0.024(5) 0.031(4) 0.001(3) C313 0.031(3) 0.102(6) 0.197(10) -0.025(7) 0.038(5) -0.004(3) C314 0.087(6) 0.080(5) 0.216(11) 0.025(6) 0.112(7) 0.022(5) C315 0.081(5) 0.070(5) 0.163(7) 0.032(5) 0.080(5) 0.033(4) C316 0.060(4) 0.071(4) 0.099(5) 0.027(4) 0.049(3) 0.028(3) C317 0.096(9) 0.48(3) 0.171(13) 0.000(15) -0.002(8) 0.053(13) C411 0.040(2) 0.033(2) 0.045(3) -0.001(2) 0.013(2) 0.016(2) C412 0.054(3) 0.043(3) 0.055(3) 0.009(2) 0.021(2) 0.029(2) C413 0.090(4) 0.055(3) 0.057(3) 0.015(3) 0.029(3) 0.053(3) C414 0.074(4) 0.032(3) 0.086(4) 0.003(3) 0.049(4) 0.011(3) C415 0.060(3) 0.052(4) 0.068(4) -0.009(3) 0.019(3) 0.002(3) C416 0.045(3) 0.051(3) 0.053(3) -0.008(2) 0.010(2) 0.012(2) C417 0.077(4) 0.104(6) 0.100(5) 0.029(4) 0.020(4) 0.050(4) C511 0.037(2) 0.030(2) 0.032(2) 0.0044(17) 0.0066(18) 0.0159(19) C512 0.032(2) 0.031(2) 0.037(2) 0.0036(18) 0.0086(18) 0.0132(18) C513 0.039(2) 0.032(2) 0.035(2) 0.0049(18) 0.0105(18) 0.0169(19) C514 0.036(2) 0.039(3) 0.033(2) 0.0040(19) 0.0006(18) 0.016(2) C515 0.034(2) 0.043(3) 0.041(2) 0.003(2) 0.0057(19) 0.016(2) C516 0.038(2) 0.038(3) 0.041(2) 0.008(2) 0.0137(19) 0.017(2) C517 0.044(3) 0.050(3) 0.033(2) 0.004(2) 0.009(2) 0.019(2) C611 0.037(2) 0.042(3) 0.037(2) -0.004(2) -0.0032(19) 0.014(2) C612 0.048(3) 0.049(3) 0.042(3) -0.002(2) 0.001(2) 0.017(2) C613 0.064(3) 0.051(3) 0.043(3) -0.003(2) -0.013(2) 0.024(3) C614 0.051(3) 0.063(4) 0.076(4) 0.005(3) -0.022(3) 0.019(3) C615 0.039(3) 0.081(4) 0.087(4) 0.019(4) -0.004(3) 0.016(3) C616 0.033(3) 0.063(3) 0.059(3) 0.015(3) 0.000(2) 0.013(2) C617 0.110(5) 0.067(4) 0.051(3) 0.006(3) -0.011(3) 0.041(4) C711 0.031(2) 0.042(3) 0.061(3) 0.003(2) 0.021(2) 0.011(2) C712 0.029(2) 0.059(3) 0.079(4) -0.022(3) 0.003(2) 0.018(2) C713 0.035(3) 0.059(4) 0.146(7) -0.046(4) 0.010(4) 0.015(3) C714 0.034(4) 0.057(5) 0.260(13) -0.032(6) 0.033(6) 0.008(3) C715 0.082(5) 0.054(4) 0.220(10) 0.048(5) 0.101(6) 0.026(4) C716 0.067(4) 0.064(4) 0.115(5) 0.034(4) 0.055(4) 0.031(3) C717 0.048(4) 0.152(8) 0.163(8) -0.110(6) -0.050(4) 0.055(4) C811 0.065(3) 0.030(3) 0.058(3) 0.008(2) 0.026(3) 0.018(2) C812 0.073(4) 0.043(3) 0.077(4) 0.008(3) 0.033(3) 0.018(3) C813 0.062(4) 0.040(3) 0.098(5) 0.004(3) 0.041(3) 0.011(3) C814 0.087(5) 0.064(4) 0.067(4) 0.016(3) 0.017(4) 0.039(4) C815 0.096(5) 0.078(5) 0.070(4) 0.008(3) 0.013(4) 0.048(4) C816 0.096(4) 0.061(4) 0.043(3) 0.020(3) 0.019(3) 0.042(3) C817 0.088(5) 0.091(6) 0.116(6) 0.013(5) 0.045(5) 0.015(4) S10 0.0999(13) 0.0651(10) 0.0598(9) 0.0077(8) 0.0114(8) 0.0345(9) O100 0.140(4) 0.078(3) 0.069(3) -0.014(2) -0.004(3) 0.048(3) C100 0.079(4) 0.064(4) 0.073(4) 0.004(3) 0.026(3) 0.027(3) C101 0.072(4) 0.062(4) 0.081(4) 0.006(3) 0.014(3) 0.017(3) S20A 0.0769(16) 0.0616(16) 0.0657(18) 0.0229(13) 0.0284(12) 0.0242(13) C20A 0.081(4) 0.073(4) 0.050(3) 0.006(3) 0.009(3) 0.036(3) C21A 0.069(4) 0.082(5) 0.100(5) 0.019(4) 0.031(4) 0.031(4) C20B 0.081(4) 0.073(4) 0.050(3) 0.006(3) 0.009(3) 0.036(3) C21B 0.069(4) 0.082(5) 0.100(5) 0.019(4) 0.031(4) 0.031(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S11 O11 1.436(3) . ? S11 O12 1.444(3) . ? S11 C111 1.778(5) . ? S11 C11 1.804(4) . ? S21 O22 1.430(4) . ? S21 O21 1.435(4) . ? S21 C211 1.760(5) . ? S21 C21 1.811(4) . ? S31 O32 1.439(4) . ? S31 O31 1.441(4) . ? S31 C311 1.770(5) . ? S31 C31 1.791(5) . ? S41 O42 1.442(3) . ? S41 O41 1.446(3) . ? S41 C411 1.749(5) . ? S41 C41 1.809(4) . ? S51 O52 1.438(3) . ? S51 O51 1.441(3) . ? S51 C511 1.765(4) . ? S51 C51 1.808(4) . ? S61 O61 1.437(3) . ? S61 O62 1.444(3) . ? S61 C611 1.772(4) . ? S61 C61 1.798(4) . ? S71 O71 1.433(3) . ? S71 O72 1.443(3) . ? S71 C711 1.755(4) . ? S71 C71 1.804(4) . ? S81 O82 1.433(3) . ? S81 O81 1.437(3) . ? S81 C811 1.775(5) . ? S81 C81 1.805(4) . ? C1 C2 1.397(6) . ? C1 C9 1.454(5) . ? C1 C11 1.530(6) . ? C2 C3 1.423(6) . ? C2 C21 1.526(5) . ? C3 C4 1.377(6) . ? C3 C31 1.520(5) . ? C4 C10 1.427(5) . ? C4 C41 1.530(6) . ? C5 C6 1.373(5) . ? C5 C10 1.437(5) . ? C5 C51 1.511(5) . ? C6 C7 1.430(5) . ? C6 C61 1.519(5) . ? C7 C8 1.402(5) . ? C7 C71 1.525(5) . ? C8 C9 1.468(5) . ? C8 C81 1.523(5) . ? C9 C10 1.430(5) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C111 C116 1.356(7) . ? C111 C112 1.389(7) . ? C112 C113 1.402(8) . ? C112 H112 0.95 . ? C113 C114 1.357(10) . ? C113 C117 1.517(10) . ? C114 C115 1.375(10) . ? C114 H114 0.95 . ? C115 C116 1.395(8) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 H11C 0.98 . ? C117 H11D 0.98 . ? C117 H11E 0.98 . ? C211 C212 1.378(8) . ? C211 C216 1.379(8) . ? C212 C213 1.445(8) . ? C212 H212 0.95 . ? C213 C214 1.370(11) . ? C213 C217 1.496(11) . ? C214 C215 1.354(11) . ? C214 H214 0.95 . ? C215 C216 1.374(10) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H21C 0.98 . ? C217 H21D 0.98 . ? C217 H21E 0.98 . ? C311 C316 1.373(8) . ? C311 C312 1.387(9) . ? C312 C313 1.418(10) . ? C312 H312 0.95 . ? C313 C317 1.355(13) . ? C313 C314 1.373(13) . ? C314 C315 1.355(13) . ? C314 H314 0.95 . ? C315 C316 1.413(8) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C317 H31C 0.98 . ? C317 H31D 0.98 . ? C317 H31E 0.98 . ? C411 C412 1.376(6) . ? C411 C416 1.389(6) . ? C412 C413 1.401(7) . ? C412 H412 0.95 . ? C413 C414 1.396(8) . ? C413 C417 1.447(8) . ? C414 C415 1.349(8) . ? C414 H414 0.95 . ? C415 C416 1.353(7) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C417 H41C 0.98 . ? C417 H41D 0.98 . ? C417 H41E 0.98 . ? C511 C512 1.391(6) . ? C511 C516 1.396(6) . ? C512 C513 1.390(6) . ? C512 H512 0.95 . ? C513 C514 1.387(6) . ? C513 C517 1.518(6) . ? C514 C515 1.386(6) . ? C514 H514 0.95 . ? C515 C516 1.372(6) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C517 H51C 0.98 . ? C517 H51D 0.98 . ? C517 H51E 0.98 . ? C611 C616 1.378(6) . ? C611 C612 1.386(6) . ? C612 C613 1.387(7) . ? C612 H612 0.95 . ? C613 C614 1.380(8) . ? C613 C617 1.489(8) . ? C614 C615 1.366(8) . ? C614 H614 0.95 . ? C615 C616 1.384(7) . ? C615 H615 0.95 . ? C616 H616 0.95 . ? C617 H61C 0.98 . ? C617 H61D 0.98 . ? C617 H61E 0.98 . ? C711 C716 1.381(7) . ? C711 C712 1.393(7) . ? C712 C713 1.372(8) . ? C712 H712 0.95 . ? C713 C714 1.381(13) . ? C713 C717 1.485(11) . ? C714 C715 1.382(13) . ? C714 H714 0.95 . ? C715 C716 1.413(10) . ? C715 H715 0.95 . ? C716 H716 0.95 . ? C717 H71C 0.98 . ? C717 H71D 0.98 . ? C717 H71E 0.98 . ? C811 C812 1.373(7) . ? C811 C816 1.392(7) . ? C812 C813 1.488(8) . ? C812 H812 0.95 . ? C813 C814 1.356(8) . ? C813 C817 1.454(9) . ? C814 C815 1.306(9) . ? C814 H814 0.95 . ? C815 C816 1.412(8) . ? C815 H815 0.95 . ? C816 H816 0.95 . ? C817 H81C 0.98 . ? C817 H81D 0.98 . ? C817 H81E 0.98 . ? S10 O100 1.502(5) . ? S10 C100 1.762(6) . ? S10 C101 1.784(6) . ? C100 H10A 0.98 . ? C100 H10B 0.98 . ? C100 H10C 0.98 . ? C101 H10D 0.98 . ? C101 H10E 0.98 . ? C101 H10F 0.98 . ? S20A O20A 1.497(11) . ? S20A C20A 1.760(6) . ? S20A C21A 1.771(7) . ? C20A H2AA 0.98 . ? C20A H2AB 0.98 . ? C20A H2AC 0.98 . ? C21A H2AD 0.98 . ? C21A H2AE 0.98 . ? C21A H2AF 0.98 . ? S20B O20B 1.54(2) . ? 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 O11 S11 O12 118.07(19) . . ? O11 S11 C111 108.2(2) . . ? O12 S11 C111 107.8(2) . . ? O11 S11 C11 109.86(18) . . ? O12 S11 C11 109.2(2) . . ? C111 S11 C11 102.6(2) . . ? O22 S21 O21 118.7(2) . . ? O22 S21 C211 109.3(3) . . ? O21 S21 C211 108.2(3) . . ? O22 S21 C21 109.2(2) . . ? O21 S21 C21 108.0(2) . . ? C211 S21 C21 102.1(2) . . ? O32 S31 O31 119.1(2) . . ? O32 S31 C311 107.9(3) . . ? O31 S31 C311 109.1(3) . . ? O32 S31 C31 108.2(2) . . ? O31 S31 C31 107.6(2) . . ? C311 S31 C31 104.0(2) . . ? O42 S41 O41 118.1(2) . . ? O42 S41 C411 109.8(2) . . ? O41 S41 C411 108.9(2) . . ? O42 S41 C41 104.85(19) . . ? O41 S41 C41 109.45(19) . . ? C411 S41 C41 104.8(2) . . ? O52 S51 O51 118.20(18) . . ? O52 S51 C511 108.45(19) . . ? O51 S51 C511 108.34(18) . . ? O52 S51 C51 106.02(18) . . ? O51 S51 C51 110.35(19) . . ? C511 S51 C51 104.63(19) . . ? O61 S61 O62 118.95(19) . . ? O61 S61 C611 108.1(2) . . ? O62 S61 C611 108.4(2) . . ? O61 S61 C61 107.00(19) . . ? O62 S61 C61 107.92(19) . . ? C611 S61 C61 105.8(2) . . ? O71 S71 O72 117.5(2) . . ? O71 S71 C711 109.0(2) . . ? O72 S71 C711 109.2(2) . . ? O71 S71 C71 109.13(19) . . ? O72 S71 C71 108.28(19) . . ? C711 S71 C71 102.5(2) . . ? O82 S81 O81 118.51(19) . . ? O82 S81 C811 106.4(2) . . ? O81 S81 C811 109.1(2) . . ? O82 S81 C81 109.48(19) . . ? O81 S81 C81 109.00(19) . . ? C811 S81 C81 103.3(2) . . ? C2 C1 C9 119.7(4) . . ? C2 C1 C11 115.9(3) . . ? C9 C1 C11 124.3(3) . . ? C1 C2 C3 121.8(3) . . ? C1 C2 C21 121.2(4) . . ? C3 C2 C21 116.9(4) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C31 118.5(4) . . ? C2 C3 C31 122.9(4) . . ? C3 C4 C10 119.6(4) . . ? C3 C4 C41 122.0(3) . . ? C10 C4 C41 117.7(3) . . ? C6 C5 C10 119.4(3) . . ? C6 C5 C51 121.5(3) . . ? C10 C5 C51 118.3(3) . . ? C5 C6 C7 118.9(3) . . ? C5 C6 C61 118.2(3) . . ? C7 C6 C61 122.8(3) . . ? C8 C7 C6 121.6(3) . . ? C8 C7 C71 121.5(3) . . ? C6 C7 C71 116.7(3) . . ? C7 C8 C9 119.7(3) . . ? C7 C8 C81 115.8(3) . . ? C9 C8 C81 124.5(3) . . ? C10 C9 C1 115.9(3) . . ? C10 C9 C8 115.5(3) . . ? C1 C9 C8 128.6(3) . . ? C4 C10 C9 120.8(3) . . ? C4 C10 C5 118.3(3) . . ? C9 C10 C5 120.9(3) . . ? C1 C11 S11 116.5(3) . . ? C1 C11 H11A 108.2 . . ? S11 C11 H11A 108.2 . . ? C1 C11 H11B 108.2 . . ? S11 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? C2 C21 S21 114.0(3) . . ? C2 C21 H21A 108.8 . . ? S21 C21 H21A 108.8 . . ? C2 C21 H21B 108.8 . . ? S21 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C3 C31 S31 109.7(3) . . ? C3 C31 H31A 109.7 . . ? S31 C31 H31A 109.7 . . ? C3 C31 H31B 109.7 . . ? S31 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C4 C41 S41 112.8(3) . . ? C4 C41 H41A 109 . . ? S41 C41 H41A 109 . . ? C4 C41 H41B 109 . . ? S41 C41 H41B 109 . . ? H41A C41 H41B 107.8 . . ? C5 C51 S51 111.5(3) . . ? C5 C51 H51A 109.3 . . ? S51 C51 H51A 109.3 . . ? C5 C51 H51B 109.3 . . ? S51 C51 H51B 109.3 . . ? H51A C51 H51B 108 . . ? C6 C61 S61 107.0(3) . . ? C6 C61 H61A 110.3 . . ? S61 C61 H61A 110.3 . . ? C6 C61 H61B 110.3 . . ? S61 C61 H61B 110.3 . . ? H61A C61 H61B 108.6 . . ? C7 C71 S71 112.6(3) . . ? C7 C71 H71A 109.1 . . ? S71 C71 H71A 109.1 . . ? C7 C71 H71B 109.1 . . ? S71 C71 H71B 109.1 . . ? H71A C71 H71B 107.8 . . ? C8 C81 S81 115.6(3) . . ? C8 C81 H81A 108.4 . . ? S81 C81 H81A 108.4 . . ? C8 C81 H81B 108.4 . . ? S81 C81 H81B 108.4 . . ? H81A C81 H81B 107.4 . . ? C116 C111 C112 121.9(5) . . ? C116 C111 S11 120.0(4) . . ? C112 C111 S11 118.0(4) . . ? C111 C112 C113 119.2(7) . . ? C111 C112 H112 120.4 . . ? C113 C112 H112 120.4 . . ? C114 C113 C112 118.0(6) . . ? C114 C113 C117 123.3(7) . . ? C112 C113 C117 118.7(8) . . ? C113 C114 C115 123.0(6) . . ? C113 C114 H114 118.5 . . ? C115 C114 H114 118.5 . . ? C114 C115 C116 118.9(7) . . ? C114 C115 H115 120.5 . . ? C116 C115 H115 120.5 . . ? C111 C116 C115 119.0(6) . . ? C111 C116 H116 120.5 . . ? C115 C116 H116 120.5 . . ? C113 C117 H11C 109.5 . . ? C113 C117 H11D 109.5 . . ? H11C C117 H11D 109.5 . . ? C113 C117 H11E 109.5 . . ? H11C C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C212 C211 C216 122.3(5) . . ? C212 C211 S21 118.4(5) . . ? C216 C211 S21 119.3(5) . . ? C211 C212 C213 118.2(6) . . ? C211 C212 H212 120.9 . . ? C213 C212 H212 120.9 . . ? C214 C213 C212 116.2(7) . . ? C214 C213 C217 125.9(7) . . ? C212 C213 C217 117.9(8) . . ? C215 C214 C213 125.3(7) . . ? C215 C214 H214 117.4 . . ? C213 C214 H214 117.4 . . ? C214 C215 C216 118.4(8) . . ? C214 C215 H215 120.8 . . ? C216 C215 H215 120.8 . . ? C215 C216 C211 119.6(7) . . ? C215 C216 H216 120.2 . . ? C211 C216 H216 120.2 . . ? C213 C217 H21C 109.5 . . ? C213 C217 H21D 109.5 . . ? H21C C217 H21D 109.5 . . ? C213 C217 H21E 109.5 . . ? H21C C217 H21E 109.5 . . ? H21D C217 H21E 109.5 . . ? C316 C311 C312 121.7(5) . . ? C316 C311 S31 119.1(4) . . ? C312 C311 S31 119.2(5) . . ? C311 C312 C313 117.2(8) . . ? C311 C312 H312 121.4 . . ? C313 C312 H312 121.4 . . ? C317 C313 C314 112.8(10) . . ? C317 C313 C312 126.6(12) . . ? C314 C313 C312 120.3(8) . . ? C315 C314 C313 122.2(7) . . ? C315 C314 H314 118.9 . . ? C313 C314 H314 118.9 . . ? C314 C315 C316 118.3(8) . . ? C314 C315 H315 120.9 . . ? C316 C315 H315 120.9 . . ? C311 C316 C315 120.2(7) . . ? C311 C316 H316 119.9 . . ? C315 C316 H316 119.9 . . ? C313 C317 H31C 109.5 . . ? C313 C317 H31D 109.5 . . ? H31C C317 H31D 109.5 . . ? C313 C317 H31E 109.5 . . ? H31C C317 H31E 109.5 . . ? H31D C317 H31E 109.5 . . ? C412 C411 C416 121.6(4) . . ? C412 C411 S41 119.6(4) . . ? C416 C411 S41 118.8(4) . . ? C411 C412 C413 118.8(5) . . ? C411 C412 H412 120.6 . . ? C413 C412 H412 120.6 . . ? C414 C413 C412 117.2(5) . . ? C414 C413 C417 120.4(6) . . ? C412 C413 C417 122.2(6) . . ? C415 C414 C413 123.3(5) . . ? C415 C414 H414 118.4 . . ? C413 C414 H414 118.4 . . ? C414 C415 C416 119.4(6) . . ? C414 C415 H415 120.3 . . ? C416 C415 H415 120.3 . . ? C415 C416 C411 119.7(5) . . ? C415 C416 H416 120.1 . . ? C411 C416 H416 120.1 . . ? C413 C417 H41C 109.5 . . ? C413 C417 H41D 109.5 . . ? H41C C417 H41D 109.5 . . ? C413 C417 H41E 109.5 . . ? H41C C417 H41E 109.5 . . ? H41D C417 H41E 109.5 . . ? C512 C511 C516 122.1(4) . . ? C512 C511 S51 119.0(3) . . ? C516 C511 S51 118.9(3) . . ? C513 C512 C511 119.3(4) . . ? C513 C512 H512 120.4 . . ? C511 C512 H512 120.4 . . ? C514 C513 C512 118.1(4) . . ? C514 C513 C517 121.2(4) . . ? C512 C513 C517 120.7(4) . . ? C515 C514 C513 122.4(4) . . ? C515 C514 H514 118.8 . . ? C513 C514 H514 118.8 . . ? C516 C515 C514 119.9(4) . . ? C516 C515 H515 120 . . ? C514 C515 H515 120 . . ? C515 C516 C511 118.2(4) . . ? C515 C516 H516 120.9 . . ? C511 C516 H516 120.9 . . ? C513 C517 H51C 109.5 . . ? C513 C517 H51D 109.5 . . ? H51C C517 H51D 109.5 . . ? C513 C517 H51E 109.5 . . ? H51C C517 H51E 109.5 . . ? H51D C517 H51E 109.5 . . ? C616 C611 C612 122.3(4) . . ? C616 C611 S61 119.3(4) . . ? C612 C611 S61 118.1(4) . . ? C611 C612 C613 120.0(5) . . ? C611 C612 H612 120 . . ? C613 C612 H612 120 . . ? C614 C613 C612 117.2(5) . . ? C614 C613 C617 121.7(5) . . ? C612 C613 C617 121.0(5) . . ? C615 C614 C613 122.5(5) . . ? C615 C614 H614 118.8 . . ? C613 C614 H614 118.8 . . ? C614 C615 C616 120.8(5) . . ? C614 C615 H615 119.6 . . ? C616 C615 H615 119.6 . . ? C611 C616 C615 117.1(5) . . ? C611 C616 H616 121.5 . . ? C615 C616 H616 121.5 . . ? C613 C617 H61C 109.5 . . ? C613 C617 H61D 109.5 . . ? H61C C617 H61D 109.5 . . ? C613 C617 H61E 109.5 . . ? H61C C617 H61E 109.5 . . ? H61D C617 H61E 109.5 . . ? C716 C711 C712 122.8(5) . . ? C716 C711 S71 119.5(4) . . ? C712 C711 S71 117.7(4) . . ? C713 C712 C711 121.4(6) . . ? C713 C712 H712 119.3 . . ? C711 C712 H712 119.3 . . ? C712 C713 C714 115.9(7) . . ? C712 C713 C717 122.0(8) . . ? C714 C713 C717 122.1(7) . . ? C713 C714 C715 124.4(6) . . ? C713 C714 H714 117.8 . . ? C715 C714 H714 117.8 . . ? C714 C715 C716 119.4(7) . . ? C714 C715 H715 120.3 . . ? C716 C715 H715 120.3 . . ? C711 C716 C715 116.2(7) . . ? C711 C716 H716 121.9 . . ? C715 C716 H716 121.9 . . ? C713 C717 H71C 109.5 . . ? C713 C717 H71D 109.5 . . ? H71C C717 H71D 109.5 . . ? C713 C717 H71E 109.5 . . ? H71C C717 H71E 109.5 . . ? H71D C717 H71E 109.5 . . ? C812 C811 C816 122.2(5) . . ? C812 C811 S81 118.8(4) . . ? C816 C811 S81 119.0(4) . . ? C811 C812 C813 117.1(6) . . ? C811 C812 H812 121.4 . . ? C813 C812 H812 121.4 . . ? C814 C813 C817 127.7(6) . . ? C814 C813 C812 115.4(5) . . ? C817 C813 C812 116.9(6) . . ? C815 C814 C813 128.6(6) . . ? C815 C814 H814 115.7 . . ? C813 C814 H814 115.7 . . ? C814 C815 C816 116.9(6) . . ? C814 C815 H815 121.6 . . ? C816 C815 H815 121.6 . . ? C811 C816 C815 119.8(6) . . ? C811 C816 H816 120.1 . . ? C815 C816 H816 120.1 . . ? C813 C817 H81C 109.5 . . ? C813 C817 H81D 109.5 . . ? H81C C817 H81D 109.5 . . ? C813 C817 H81E 109.5 . . ? H81C C817 H81E 109.5 . . ? H81D C817 H81E 109.5 . . ? O100 S10 C100 106.6(3) . . ? O100 S10 C101 105.4(3) . . ? C100 S10 C101 98.2(3) . . ? S10 C100 H10A 109.5 . . ? S10 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? S10 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? S10 C101 H10D 109.5 . . ? S10 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? S10 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? O20A S20A C20A 110.3(4) . . ? O20A S20A C21A 103.1(4) . . ? C20A S20A C21A 97.5(3) . . ? S20A C20A H2AA 109.5 . . ? S20A C20A H2AB 109.5 . . ? H2AA C20A H2AB 109.5 . . ? S20A C20A H2AC 109.5 . . ? H2AA C20A H2AC 109.5 . . ? H2AB C20A H2AC 109.5 . . ? S20A C21A H2AD 109.5 . . ? S20A C21A H2AE 109.5 . . ? H2AD C21A H2AE 109.5 . . ? S20A C21A H2AF 109.5 . . ? H2AD C21A H2AF 109.5 . . ? H2AE C21A H2AF 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C3 11.6(6) . . . . ? C11 C1 C2 C3 -167.2(4) . . . . ? C9 C1 C2 C21 -173.0(4) . . . . ? C11 C1 C2 C21 8.3(6) . . . . ? C1 C2 C3 C4 -6.2(6) . . . . ? C21 C2 C3 C4 178.2(4) . . . . ? C1 C2 C3 C31 177.2(4) . . . . ? C21 C2 C3 C31 1.6(6) . . . . ? C2 C3 C4 C10 -10.6(6) . . . . ? C31 C3 C4 C10 166.2(4) . . . . ? C2 C3 C4 C41 159.4(4) . . . . ? C31 C3 C4 C41 -23.8(6) . . . . ? C10 C5 C6 C7 -11.3(6) . . . . ? C51 C5 C6 C7 158.4(4) . . . . ? C10 C5 C6 C61 164.9(4) . . . . ? C51 C5 C6 C61 -25.4(5) . . . . ? C5 C6 C7 C8 -5.1(6) . . . . ? C61 C6 C7 C8 178.9(4) . . . . ? C5 C6 C7 C71 179.4(3) . . . . ? C61 C6 C7 C71 3.4(5) . . . . ? C6 C7 C8 C9 10.2(6) . . . . ? C71 C7 C8 C9 -174.5(4) . . . . ? C6 C7 C8 C81 -169.9(4) . . . . ? C71 C7 C8 C81 5.3(5) . . . . ? C2 C1 C9 C10 -0.2(5) . . . . ? C11 C1 C9 C10 178.5(4) . . . . ? C2 C1 C9 C8 178.9(4) . . . . ? C11 C1 C9 C8 -2.4(6) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C81 C8 C9 C10 -178.8(4) . . . . ? C7 C8 C9 C1 -178.0(4) . . . . ? C81 C8 C9 C1 2.1(6) . . . . ? C3 C4 C10 C9 22.4(6) . . . . ? C41 C4 C10 C9 -148.0(4) . . . . ? C3 C4 C10 C5 -155.8(4) . . . . ? C41 C4 C10 C5 33.7(5) . . . . ? C1 C9 C10 C4 -16.5(5) . . . . ? C8 C9 C10 C4 164.3(4) . . . . ? C1 C9 C10 C5 161.7(4) . . . . ? C8 C9 C10 C5 -17.5(5) . . . . ? C6 C5 C10 C4 -158.5(4) . . . . ? C51 C5 C10 C4 31.5(5) . . . . ? C6 C5 C10 C9 23.2(6) . . . . ? C51 C5 C10 C9 -146.8(4) . . . . ? C2 C1 C11 S11 -88.9(4) . . . . ? C9 C1 C11 S11 92.4(4) . . . . ? O11 S11 C11 C1 -78.1(3) . . . . ? O12 S11 C11 C1 52.9(3) . . . . ? C111 S11 C11 C1 167.1(3) . . . . ? C1 C2 C21 S21 -92.3(4) . . . . ? C3 C2 C21 S21 83.3(4) . . . . ? O22 S21 C21 C2 -52.8(4) . . . . ? O21 S21 C21 C2 77.7(4) . . . . ? C211 S21 C21 C2 -168.4(4) . . . . ? C4 C3 C31 S31 -83.9(4) . . . . ? C2 C3 C31 S31 92.8(4) . . . . ? O32 S31 C31 C3 63.2(4) . . . . ? O31 S31 C31 C3 -66.7(4) . . . . ? C311 S31 C31 C3 177.7(3) . . . . ? C3 C4 C41 S41 -65.6(5) . . . . ? C10 C4 C41 S41 104.6(4) . . . . ? O42 S41 C41 C4 -158.9(3) . . . . ? O41 S41 C41 C4 73.4(3) . . . . ? C411 S41 C41 C4 -43.3(3) . . . . ? C6 C5 C51 S51 -67.1(4) . . . . ? C10 C5 C51 S51 102.7(4) . . . . ? O52 S51 C51 C5 -156.5(3) . . . . ? O51 S51 C51 C5 74.4(3) . . . . ? C511 S51 C51 C5 -42.0(3) . . . . ? C5 C6 C61 S61 -81.8(4) . . . . ? C7 C6 C61 S61 94.2(4) . . . . ? O61 S61 C61 C6 -68.8(3) . . . . ? O62 S61 C61 C6 60.3(3) . . . . ? C611 S61 C61 C6 176.2(3) . . . . ? C8 C7 C71 S71 -91.8(4) . . . . ? C6 C7 C71 S71 83.6(4) . . . . ? O71 S71 C71 C7 -52.9(3) . . . . ? O72 S71 C71 C7 76.2(3) . . . . ? C711 S71 C71 C7 -168.4(3) . . . . ? C7 C8 C81 S81 -89.4(4) . . . . ? C9 C8 C81 S81 90.5(4) . . . . ? O82 S81 C81 C8 -76.2(3) . . . . ? O81 S81 C81 C8 54.9(3) . . . . ? C811 S81 C81 C8 170.8(3) . . . . ? O11 S11 C111 C116 -20.5(5) . . . . ? O12 S11 C111 C116 -149.2(4) . . . . ? C11 S11 C111 C116 95.6(4) . . . . ? O11 S11 C111 C112 157.8(4) . . . . ? O12 S11 C111 C112 29.1(5) . . . . ? C11 S11 C111 C112 -86.1(4) . . . . ? C116 C111 C112 C113 1.0(8) . . . . ? S11 C111 C112 C113 -177.3(4) . . . . ? C111 C112 C113 C114 -1.8(9) . . . . ? C111 C112 C113 C117 178.1(5) . . . . ? C112 C113 C114 C115 1.4(9) . . . . ? C117 C113 C114 C115 -178.5(6) . . . . ? C113 C114 C115 C116 -0.1(9) . . . . ? C112 C111 C116 C115 0.3(8) . . . . ? S11 C111 C116 C115 178.5(4) . . . . ? C114 C115 C116 C111 -0.8(8) . . . . ? O22 S21 C211 C212 -23.9(5) . . . . ? O21 S21 C211 C212 -154.5(4) . . . . ? C21 S21 C211 C212 91.7(5) . . . . ? O22 S21 C211 C216 158.7(5) . . . . ? O21 S21 C211 C216 28.1(5) . . . . ? C21 S21 C211 C216 -85.7(5) . . . . ? C216 C211 C212 C213 -1.0(8) . . . . ? S21 C211 C212 C213 -178.4(4) . . . . ? C211 C212 C213 C214 1.5(8) . . . . ? C211 C212 C213 C217 178.7(5) . . . . ? C212 C213 C214 C215 -1.4(11) . . . . ? C217 C213 C214 C215 -178.4(7) . . . . ? C213 C214 C215 C216 0.7(12) . . . . ? C214 C215 C216 C211 -0.1(11) . . . . ? C212 C211 C216 C215 0.3(10) . . . . ? S21 C211 C216 C215 177.6(6) . . . . ? O32 S31 C311 C316 25.5(5) . . . . ? O31 S31 C311 C316 156.1(5) . . . . ? C31 S31 C311 C316 -89.3(5) . . . . ? O32 S31 C311 C312 -152.3(5) . . . . ? O31 S31 C311 C312 -21.6(6) . . . . ? C31 S31 C311 C312 93.0(5) . . . . ? C316 C311 C312 C313 0.9(10) . . . . ? S31 C311 C312 C313 178.5(6) . . . . ? C311 C312 C313 C317 -173.1(14) . . . . ? C311 C312 C313 C314 0.1(13) . . . . ? C317 C313 C314 C315 173.1(12) . . . . ? C312 C313 C314 C315 -1.0(15) . . . . ? C313 C314 C315 C316 0.8(13) . . . . ? C312 C311 C316 C315 -1.0(9) . . . . ? S31 C311 C316 C315 -178.7(5) . . . . ? C314 C315 C316 C311 0.1(10) . . . . ? O42 S41 C411 C412 -147.4(4) . . . . ? O41 S41 C411 C412 -16.6(4) . . . . ? C41 S41 C411 C412 100.4(4) . . . . ? O42 S41 C411 C416 34.0(4) . . . . ? O41 S41 C411 C416 164.8(3) . . . . ? C41 S41 C411 C416 -78.2(4) . . . . ? C416 C411 C412 C413 -1.4(7) . . . . ? S41 C411 C412 C413 -179.9(3) . . . . ? C411 C412 C413 C414 1.5(7) . . . . ? C411 C412 C413 C417 -174.8(5) . . . . ? C412 C413 C414 C415 0.0(8) . . . . ? C417 C413 C414 C415 176.3(6) . . . . ? C413 C414 C415 C416 -1.6(9) . . . . ? C414 C415 C416 C411 1.7(8) . . . . ? C412 C411 C416 C415 -0.2(7) . . . . ? S41 C411 C416 C415 178.3(4) . . . . ? O52 S51 C511 C512 -137.6(3) . . . . ? O51 S51 C511 C512 -8.2(4) . . . . ? C51 S51 C511 C512 109.6(3) . . . . ? O52 S51 C511 C516 42.5(4) . . . . ? O51 S51 C511 C516 172.0(3) . . . . ? C51 S51 C511 C516 -70.3(4) . . . . ? C516 C511 C512 C513 -2.9(6) . . . . ? S51 C511 C512 C513 177.2(3) . . . . ? C511 C512 C513 C514 3.2(6) . . . . ? C511 C512 C513 C517 -177.5(4) . . . . ? C512 C513 C514 C515 -1.4(6) . . . . ? C517 C513 C514 C515 179.3(4) . . . . ? C513 C514 C515 C516 -0.8(7) . . . . ? C514 C515 C516 C511 1.1(6) . . . . ? C512 C511 C516 C515 0.7(6) . . . . ? S51 C511 C516 C515 -179.4(3) . . . . ? O61 S61 C611 C616 -38.3(5) . . . . ? O62 S61 C611 C616 -168.4(4) . . . . ? C61 S61 C611 C616 76.0(4) . . . . ? O61 S61 C611 C612 136.8(4) . . . . ? O62 S61 C611 C612 6.7(4) . . . . ? C61 S61 C611 C612 -108.9(4) . . . . ? C616 C611 C612 C613 1.5(8) . . . . ? S61 C611 C612 C613 -173.4(4) . . . . ? C611 C612 C613 C614 -2.1(8) . . . . ? C611 C612 C613 C617 174.6(5) . . . . ? C612 C613 C614 C615 0.8(9) . . . . ? C617 C613 C614 C615 -175.8(6) . . . . ? C613 C614 C615 C616 1.1(10) . . . . ? C612 C611 C616 C615 0.3(8) . . . . ? S61 C611 C616 C615 175.2(4) . . . . ? C614 C615 C616 C611 -1.6(9) . . . . ? O71 S71 C711 C716 152.2(4) . . . . ? O72 S71 C711 C716 22.6(5) . . . . ? C71 S71 C711 C716 -92.2(4) . . . . ? O71 S71 C711 C712 -29.2(4) . . . . ? O72 S71 C711 C712 -158.9(4) . . . . ? C71 S71 C711 C712 86.4(4) . . . . ? C716 C711 C712 C713 1.0(8) . . . . ? S71 C711 C712 C713 -177.5(4) . . . . ? C711 C712 C713 C714 -0.7(8) . . . . ? C711 C712 C713 C717 179.8(5) . . . . ? C712 C713 C714 C715 0.1(11) . . . . ? C717 C713 C714 C715 179.6(7) . . . . ? C713 C714 C715 C716 0.3(12) . . . . ? C712 C711 C716 C715 -0.5(8) . . . . ? S71 C711 C716 C715 177.9(5) . . . . ? C714 C715 C716 C711 -0.1(10) . . . . ? O82 S81 C811 C812 158.0(4) . . . . ? O81 S81 C811 C812 29.1(5) . . . . ? C81 S81 C811 C812 -86.7(4) . . . . ? O82 S81 C811 C816 -19.4(5) . . . . ? O81 S81 C811 C816 -148.4(4) . . . . ? C81 S81 C811 C816 95.8(4) . . . . ? C816 C811 C812 C813 0.6(7) . . . . ? S81 C811 C812 C813 -176.8(4) . . . . ? C811 C812 C813 C814 -1.1(7) . . . . ? C811 C812 C813 C817 179.9(5) . . . . ? C817 C813 C814 C815 179.8(7) . . . . ? C812 C813 C814 C815 1.0(10) . . . . ? C813 C814 C815 C816 -0.2(10) . . . . ? C812 C811 C816 C815 0.2(8) . . . . ? S81 C811 C816 C815 177.6(4) . . . . ? C814 C815 C816 C811 -0.5(9) . . . . ? # END of CIF