# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 177 loop_ _publ_author_name 'Howard Colquhoun' 'Abderrazak Ben-Haida' 'P Hodge' 'James Raftery' 'Andrew J. P. White' 'David Williams' _publ_contact_author_name 'Howard Colquhoun' _publ_contact_author_email H.M.COLQUHOUN@RDG.AC.UK _publ_section_title ; Macrocyclic aromatic polysulfones: synthesis and structural characterisation of molecular pentagons and rectangles ; # Attachment '2,3,5,6,7.CIF' data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 737298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 O10 S5, 3.75(C4 H9 N O)' _chemical_formula_sum 'C45 H53.75 N3.75 O13.75 S5' _chemical_formula_weight 1027.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.0349(4) _cell_length_b 20.6530(5) _cell_length_c 11.1727(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.111(2) _cell_angle_gamma 90.00 _cell_volume 2391.05(15) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.80 _cell_measurement_theta_max 27.99 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 2.824 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6530 _exptl_absorpt_correction_T_max 0.8602 _exptl_absorpt_process_details ; Bruker XPREP, version 5.1/NT Ellipsoidal absorption correction using psi-scans ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/RA' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3871 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 60.00 _reflns_number_total 3663 _reflns_number_gt 2905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. When refined using the space group P2(1)/m, with a mirror plane through the middle of the molecule, the thermal ellipsoids of the S(1) SO2 unit and the adjacent C(1)-C(6) phenyl ring showed noticeable elongation perpendicular to the plane of the mirror, suggesting disorder across the mirror plane. Using the lower symmetry space group P2(1), which does not have the mirror plane, did not remove this issue, so the refinements using the higher symmetry centrosymmetric space group were retained. ; _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^)+(0.0724P)^2^+0.5147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3663 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.89873(10) 0.2500 0.96710(9) 0.0717(4) Uani 1 2 d S . . O11 O 0.9907(3) 0.2500 0.9027(3) 0.0861(14) Uani 1 2 d S . . O12 O 0.9417(3) 0.2500 1.1036(3) 0.0893(14) Uani 1 2 d S . . S2 S 0.56558(7) 0.50130(5) 0.78913(6) 0.0575(3) Uani 1 1 d . . . O21 O 0.6105(2) 0.53323(14) 0.69710(18) 0.0673(7) Uani 1 1 d . . . O22 O 0.5690(2) 0.53478(13) 0.90202(19) 0.0700(7) Uani 1 1 d . . . S3 S 0.00126(6) 0.40139(3) 0.51615(7) 0.0410(2) Uani 1 1 d . . . O31 O -0.04344(19) 0.42236(10) 0.3858(2) 0.0572(6) Uani 1 1 d . . . O32 O -0.07242(19) 0.41633(9) 0.5975(2) 0.0569(6) Uani 1 1 d . . . C1 C 0.7976(3) 0.3187(2) 0.9132(2) 0.0602(9) Uani 1 1 d . . . C2 C 0.8030(3) 0.3518(2) 0.8071(3) 0.0715(12) Uani 1 1 d . . . H2A H 0.8568 0.3368 0.7623 0.086 Uiso 1 1 calc R . . C3 C 0.7294(3) 0.4061(2) 0.7679(3) 0.0716(12) Uani 1 1 d . . . H3A H 0.7288 0.4281 0.6930 0.086 Uiso 1 1 calc R . . C4 C 0.6557(3) 0.4293(2) 0.8370(2) 0.0569(9) Uani 1 1 d . . . C5 C 0.6506(3) 0.3948(2) 0.9433(3) 0.0712(11) Uani 1 1 d . . . H5A H 0.5971 0.4098 0.9885 0.085 Uiso 1 1 calc R . . C6 C 0.7223(3) 0.3398(2) 0.9823(3) 0.0687(11) Uani 1 1 d . . . H6A H 0.7204 0.3165 1.0550 0.082 Uiso 1 1 calc R . . C7 C 0.4058(3) 0.47456(14) 0.7104(2) 0.0421(6) Uani 1 1 d . . . C8 C 0.3606(3) 0.46728(18) 0.5797(3) 0.0557(8) Uani 1 1 d . . . H8A H 0.4145 0.4775 0.5319 0.067 Uiso 1 1 calc R . . C9 C 0.2358(3) 0.44490(18) 0.5182(3) 0.0559(8) Uani 1 1 d . . . H9A H 0.2029 0.4396 0.4283 0.067 Uiso 1 1 calc R . . C10 C 0.1606(2) 0.43052(11) 0.5919(2) 0.0361(5) Uani 1 1 d . . . C11 C 0.2038(3) 0.43954(15) 0.7202(3) 0.0519(7) Uani 1 1 d . . . H11A H 0.1485 0.4311 0.7675 0.062 Uiso 1 1 calc R . . C12 C 0.3291(3) 0.46112(16) 0.7819(3) 0.0527(8) Uani 1 1 d . . . H12A H 0.3613 0.4665 0.8718 0.063 Uiso 1 1 calc R . . C13 C 0.0177(2) 0.31609(11) 0.5168(2) 0.0316(5) Uani 1 1 d . . . C14 C -0.0091(2) 0.28372(13) 0.4027(2) 0.0375(5) Uani 1 1 d . . . H14A H -0.0274 0.3071 0.3252 0.045 Uiso 1 1 calc R . . C15 C 0.0481(3) 0.28324(13) 0.6334(2) 0.0381(5) Uani 1 1 d . . . H15A H 0.0684 0.3066 0.7110 0.046 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 S1 0.0342(5) 0.1496(13) 0.0266(5) 0.000 0.0046(4) 0.000 O11 0.0354(15) 0.180(4) 0.0439(16) 0.000 0.0148(13) 0.000 O12 0.0542(19) 0.178(4) 0.0279(15) 0.000 0.0045(13) 0.000 S2 0.0546(4) 0.0933(6) 0.0300(3) -0.0122(3) 0.0214(3) -0.0382(4) O21 0.0617(13) 0.1075(19) 0.0380(10) -0.0066(11) 0.0238(9) -0.0440(13) O22 0.0826(16) 0.0947(18) 0.0385(10) -0.0220(11) 0.0285(11) -0.0441(14) S3 0.0322(3) 0.0287(3) 0.0640(4) 0.0060(3) 0.0192(3) 0.0021(2) O31 0.0418(10) 0.0447(11) 0.0731(14) 0.0231(10) 0.0044(9) -0.0028(8) O32 0.0425(10) 0.0383(11) 0.1045(17) -0.0093(10) 0.0437(11) -0.0001(8) C1 0.0389(14) 0.111(3) 0.0289(13) -0.0012(15) 0.0091(11) -0.0117(17) C2 0.0406(16) 0.149(4) 0.0277(14) -0.0009(18) 0.0153(12) -0.009(2) C3 0.0479(17) 0.144(4) 0.0283(13) -0.0048(18) 0.0202(13) -0.027(2) C4 0.0374(14) 0.108(3) 0.0271(12) -0.0031(14) 0.0130(11) -0.0219(16) C5 0.0559(19) 0.132(4) 0.0366(15) -0.0026(18) 0.0295(14) -0.020(2) C6 0.0497(17) 0.128(3) 0.0347(14) 0.0104(18) 0.0228(13) -0.006(2) C7 0.0411(14) 0.0540(15) 0.0359(13) -0.0065(11) 0.0191(11) -0.0158(12) C8 0.0442(15) 0.096(2) 0.0331(13) 0.0032(14) 0.0209(12) -0.0205(16) C9 0.0440(15) 0.086(2) 0.0356(13) 0.0078(14) 0.0113(12) -0.0175(15) C10 0.0352(13) 0.0262(11) 0.0530(14) 0.0036(10) 0.0229(11) -0.0007(10) C11 0.0564(17) 0.0614(19) 0.0539(16) -0.0229(14) 0.0396(14) -0.0199(14) C12 0.0635(18) 0.068(2) 0.0382(13) -0.0240(13) 0.0320(13) -0.0264(15) C13 0.0272(11) 0.0299(12) 0.0394(13) 0.0043(10) 0.0136(10) 0.0029(9) C14 0.0388(13) 0.0436(13) 0.0272(11) 0.0048(10) 0.0076(9) -0.0024(11) C15 0.0506(14) 0.0369(12) 0.0325(12) -0.0042(10) 0.0218(11) -0.0029(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O11 1.432(3) . ? S1 O12 1.432(3) . ? S1 C1 1.778(4) 4_565 ? S1 C1 1.778(4) . ? S2 O22 1.428(2) . ? S2 O21 1.445(2) . ? S2 C7 1.766(3) . ? S2 C4 1.767(4) . ? S3 O31 1.435(2) . ? S3 O32 1.446(2) . ? S3 C13 1.771(2) . ? S3 C10 1.774(3) . ? C1 C6 1.385(5) . ? C1 C2 1.386(5) . ? C2 C3 1.367(6) . ? C3 C4 1.385(5) . ? C4 C5 1.402(5) . ? C5 C6 1.368(6) . ? C7 C12 1.378(4) . ? C7 C8 1.380(4) . ? C8 C9 1.390(4) . ? C9 C10 1.387(4) . ? C10 C11 1.359(4) . ? C11 C12 1.389(4) . ? C13 C14 1.379(4) . ? C13 C15 1.403(3) . ? C14 C14 1.393(5) 4_565 ? C15 C15 1.373(5) 4_565 ? 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 S1 O12 120.1(2) . . ? O11 S1 C1 107.48(12) . 4_565 ? O12 S1 C1 107.48(13) . 4_565 ? O11 S1 C1 107.48(12) . . ? O12 S1 C1 107.48(13) . . ? C1 S1 C1 106.0(2) 4_565 . ? O22 S2 O21 119.77(15) . . ? O22 S2 C7 108.05(14) . . ? O21 S2 C7 108.42(12) . . ? O22 S2 C4 107.41(15) . . ? O21 S2 C4 107.75(15) . . ? C7 S2 C4 104.42(14) . . ? O31 S3 O32 120.17(14) . . ? O31 S3 C13 107.66(12) . . ? O32 S3 C13 106.78(11) . . ? O31 S3 C10 108.67(12) . . ? O32 S3 C10 107.89(12) . . ? C13 S3 C10 104.59(11) . . ? C6 C1 C2 122.2(4) . . ? C6 C1 S1 119.3(3) . . ? C2 C1 S1 118.4(3) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C4 120.2(3) . . ? C3 C4 C5 120.0(4) . . ? C3 C4 S2 119.9(3) . . ? C5 C4 S2 120.1(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C1 118.4(3) . . ? C12 C7 C8 121.4(2) . . ? C12 C7 S2 118.8(2) . . ? C8 C7 S2 119.8(2) . . ? C7 C8 C9 119.7(2) . . ? C10 C9 C8 118.1(2) . . ? C11 C10 C9 122.2(2) . . ? C11 C10 S3 118.70(19) . . ? C9 C10 S3 119.1(2) . . ? C10 C11 C12 119.7(2) . . ? C7 C12 C11 118.8(2) . . ? C14 C13 C15 122.1(2) . . ? C14 C13 S3 119.30(18) . . ? C15 C13 S3 118.44(19) . . ? C13 C14 C14 119.00(14) . 4_565 ? C15 C15 C13 118.92(14) 4_565 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.471 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.049 # 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 0.000 -0.005 -0.004 1138 352 ' ' _platon_squeeze_details ; SQUEEZE suggests 352e/cell, which is 176e/macrocycle. Solvent was said to be dimethylacetamide (dma, C4H9NO), which has 48e. This is close to 3.75 dma/macrocycle (180e) so this was considered to be the solvent present. UNIT thus 7.5dma low = C30 H67.5 N7.5 O7.5 low, i.e. C60 H40 N0 O20 S10 ; #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 737299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 O8 S4, C Cl2 O, 2(C H Cl3)' _chemical_formula_sum 'C39 H26 Cl8 O9 S4' _chemical_formula_weight 1050.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8261(19) _cell_length_b 10.809(2) _cell_length_c 20.350(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.555(16) _cell_angle_gamma 90.00 _cell_volume 2157.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 4.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.87 _exptl_crystal_size_mid 0.77 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 7.052 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0833 _exptl_absorpt_correction_T_max 0.2821 _exptl_absorpt_process_details ; Bruker XPREP, version 5.1/NT Ellipsoidal absorption correction using psi-scans ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/RA' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3616 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 61.99 _reflns_number_total 3397 _reflns_number_gt 2739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3397 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.94172(7) 0.27850(6) -0.16234(3) 0.0397(2) Uani 1 1 d . . . O11 O 1.0626(2) 0.2293(2) -0.12910(10) 0.0479(5) Uani 1 1 d . . . O12 O 0.9123(2) 0.2519(2) -0.23097(10) 0.0483(5) Uani 1 1 d . . . S2 S 0.09305(7) 0.14655(7) 0.12215(3) 0.0405(2) Uani 1 1 d . . . O21 O -0.0242(2) 0.1022(2) 0.08283(10) 0.0474(5) Uani 1 1 d . . . O22 O 0.1279(2) 0.0894(2) 0.18521(10) 0.0495(5) Uani 1 1 d . . . C1 C 0.7987(3) 0.2350(3) -0.11846(14) 0.0407(6) Uani 1 1 d . . . C2 C 0.6674(3) 0.2553(3) -0.14510(14) 0.0461(7) Uani 1 1 d . . . H2A H 0.6523 0.2866 -0.1886 0.055 Uiso 1 1 calc R . . C3 C 0.5597(3) 0.2297(3) -0.10774(14) 0.0463(7) Uani 1 1 d . . . H3A H 0.4697 0.2442 -0.1259 0.056 Uiso 1 1 calc R . . C4 C 0.5780(3) 0.1829(3) -0.04370(14) 0.0390(6) Uani 1 1 d . . . C5 C 0.7115(3) 0.1611(3) -0.01831(14) 0.0432(6) Uani 1 1 d . . . H5A H 0.7269 0.1280 0.0247 0.052 Uiso 1 1 calc R . . C6 C 0.8212(3) 0.1874(3) -0.05538(14) 0.0423(6) Uani 1 1 d . . . H6A H 0.9116 0.1730 -0.0377 0.051 Uiso 1 1 calc R . . C7 C 0.4609(3) 0.1627(2) -0.00283(13) 0.0382(6) Uani 1 1 d . . . C8 C 0.3292(3) 0.1482(3) -0.03149(14) 0.0461(7) Uani 1 1 d . . . H8A H 0.3158 0.1443 -0.0781 0.055 Uiso 1 1 calc R . . C9 C 0.2175(3) 0.1394(3) 0.00645(15) 0.0447(7) Uani 1 1 d . . . H9A H 0.1283 0.1305 -0.0138 0.054 Uiso 1 1 calc R . . C10 C 0.2373(3) 0.1436(3) 0.07421(14) 0.0410(6) Uani 1 1 d . . . C11 C 0.3673(3) 0.1531(3) 0.10498(14) 0.0454(7) Uani 1 1 d . . . H11A H 0.3804 0.1524 0.1516 0.054 Uiso 1 1 calc R . . C12 C 0.4754(3) 0.1636(3) 0.06644(14) 0.0460(7) Uani 1 1 d . . . H12A H 0.5642 0.1718 0.0872 0.055 Uiso 1 1 calc R . . C13 C 0.0725(3) 0.3077(3) 0.13534(13) 0.0401(6) Uani 1 1 d . . . C14 C -0.0191(3) 0.3765(3) 0.09482(15) 0.0467(7) Uani 1 1 d . . . H14A H -0.0765 0.3369 0.0619 0.056 Uiso 1 1 calc R . . C15 C -0.0251(3) 0.5038(3) 0.10344(15) 0.0458(7) Uani 1 1 d . . . H15A H -0.0851 0.5528 0.0759 0.055 Uiso 1 1 calc R . . C16 C 0.0579(3) 0.5586(3) 0.15288(12) 0.0386(6) Uani 1 1 d . . . C17 C 0.1461(3) 0.4892(3) 0.19411(14) 0.0466(7) Uani 1 1 d . . . H17A H 0.2005 0.5284 0.2283 0.056 Uiso 1 1 calc R . . C18 C 0.1542(3) 0.3634(3) 0.18516(14) 0.0450(7) Uani 1 1 d . . . H18A H 0.2150 0.3150 0.2127 0.054 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 S1 0.0431(4) 0.0454(4) 0.0304(4) -0.0026(3) 0.0009(2) 0.0013(3) O11 0.0465(11) 0.0529(12) 0.0438(11) 0.0011(9) -0.0007(9) 0.0037(9) O12 0.0546(11) 0.0574(12) 0.0327(10) -0.0084(9) 0.0009(8) 0.0010(9) S2 0.0434(4) 0.0434(4) 0.0346(4) 0.0051(3) 0.0015(3) 0.0003(2) O21 0.0492(10) 0.0474(11) 0.0451(11) 0.0021(9) -0.0006(8) -0.0027(9) O22 0.0527(11) 0.0550(12) 0.0405(11) 0.0124(9) 0.0006(8) 0.0021(9) C1 0.0440(14) 0.0428(14) 0.0350(13) -0.0042(11) -0.0012(11) 0.0008(11) C2 0.0456(14) 0.0602(18) 0.0318(14) 0.0033(12) -0.0030(11) 0.0000(13) C3 0.0461(15) 0.0572(18) 0.0350(14) -0.0022(12) -0.0030(11) 0.0034(12) C4 0.0451(14) 0.0342(13) 0.0370(14) -0.0027(10) -0.0023(11) -0.0004(10) C5 0.0488(14) 0.0430(14) 0.0371(14) -0.0004(11) -0.0022(11) 0.0039(11) C6 0.0418(13) 0.0459(15) 0.0388(15) -0.0002(12) -0.0009(11) 0.0049(11) C7 0.0472(14) 0.0343(13) 0.0327(13) -0.0015(10) 0.0006(11) 0.0028(11) C8 0.0501(15) 0.0543(17) 0.0337(14) -0.0038(12) 0.0001(11) -0.0005(12) C9 0.0419(14) 0.0540(17) 0.0374(15) -0.0007(12) -0.0029(11) -0.0015(12) C10 0.0463(14) 0.0403(14) 0.0365(14) 0.0016(11) 0.0029(11) 0.0021(11) C11 0.0503(15) 0.0533(17) 0.0321(14) 0.0005(12) -0.0023(11) -0.0004(12) C12 0.0431(14) 0.0582(17) 0.0354(15) 0.0024(13) -0.0065(11) 0.0036(12) C13 0.0433(13) 0.0458(15) 0.0312(13) 0.0033(11) 0.0025(10) 0.0045(11) C14 0.0513(15) 0.0469(16) 0.0401(15) -0.0016(12) -0.0109(12) 0.0008(12) C15 0.0478(15) 0.0478(16) 0.0403(15) 0.0019(12) -0.0093(12) 0.0039(12) C16 0.0403(12) 0.0467(15) 0.0289(12) 0.0003(11) 0.0029(10) 0.0009(11) C17 0.0550(16) 0.0534(17) 0.0300(13) -0.0016(12) -0.0092(12) -0.0005(13) C18 0.0496(15) 0.0508(17) 0.0338(14) 0.0028(12) -0.0046(11) 0.0036(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O11 1.433(2) . ? S1 O12 1.438(2) . ? S1 C16 1.771(3) 3_665 ? S1 C1 1.775(3) . ? S2 O21 1.443(2) . ? S2 O22 1.446(2) . ? S2 C10 1.770(3) . ? S2 C13 1.776(3) . ? C1 C2 1.386(4) . ? C1 C6 1.388(4) . ? C2 C3 1.368(5) . ? C3 C4 1.399(4) . ? C4 C5 1.400(4) . ? C4 C7 1.477(4) . ? C5 C6 1.383(4) . ? C7 C8 1.395(4) . ? C7 C12 1.408(4) . ? C8 C9 1.384(4) . ? C9 C10 1.381(4) . ? C10 C11 1.391(4) . ? C11 C12 1.364(4) . ? C13 C18 1.391(4) . ? C13 C14 1.397(4) . ? C14 C15 1.389(5) . ? C15 C16 1.388(4) . ? C16 C17 1.388(4) . ? C16 S1 1.771(3) 3_665 ? C17 C18 1.376(5) . ? 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 S1 O12 119.68(13) . . ? O11 S1 C16 108.77(13) . 3_665 ? O12 S1 C16 107.65(13) . 3_665 ? O11 S1 C1 108.88(13) . . ? O12 S1 C1 108.57(13) . . ? C16 S1 C1 101.83(13) 3_665 . ? O21 S2 O22 119.17(13) . . ? O21 S2 C10 109.11(13) . . ? O22 S2 C10 109.14(13) . . ? O21 S2 C13 108.37(13) . . ? O22 S2 C13 107.91(13) . . ? C10 S2 C13 101.73(13) . . ? C2 C1 C6 120.8(3) . . ? C2 C1 S1 120.5(2) . . ? C6 C1 S1 118.5(2) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C4 122.1(3) . . ? C3 C4 C5 117.9(3) . . ? C3 C4 C7 121.2(2) . . ? C5 C4 C7 120.8(3) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C1 119.7(3) . . ? C8 C7 C12 116.9(3) . . ? C8 C7 C4 121.1(3) . . ? C12 C7 C4 121.9(3) . . ? C9 C8 C7 121.5(3) . . ? C10 C9 C8 119.2(3) . . ? C9 C10 C11 121.4(3) . . ? C9 C10 S2 118.9(2) . . ? C11 C10 S2 119.7(2) . . ? C12 C11 C10 118.3(3) . . ? C11 C12 C7 122.8(3) . . ? C18 C13 C14 121.4(3) . . ? C18 C13 S2 118.0(2) . . ? C14 C13 S2 120.5(2) . . ? C15 C14 C13 118.9(3) . . ? C16 C15 C14 119.1(3) . . ? C15 C16 C17 121.7(3) . . ? C15 C16 S1 120.0(2) . 3_665 ? C17 C16 S1 118.3(2) . 3_665 ? C18 C17 C16 119.5(3) . . ? C17 C18 C13 119.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 61.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.420 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.124 # 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 -0.112 0.042 0.388 760 308 ' ' _platon_squeeze_details ; SQUEEZE suggests 308e/cell. Before SQUEEZE, solvent looked like COCl2 inside the macrocycle and 2CHCl3 outside (per macrocycle). COCl2 = 48e, CHCl3 = 58e. 308e/cell = 154e/macrocycle. This is close to COCl2.2CHCl3 (48+58+58=164e) so this was considered to be the solvent present. asu thus C1.5 H O0.5 Cl4 low, so UNIT C6 H4 O2 Cl16 low, i.e. C72 H48 O16 S8 Cl0 ; #===END data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 737300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H24 O5 S5' _chemical_formula_weight 636.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8662(12) _cell_length_b 12.4037(8) _cell_length_c 11.9873(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.8050(10) _cell_angle_gamma 90.00 _cell_volume 2779.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7881 _cell_measurement_theta_min 2.373 _cell_measurement_theta_max 28.4355 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23723 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.62 _reflns_number_total 6643 _reflns_number_gt 5005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1234P)^2^+0.0697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6643 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.30876(15) 0.3528(2) 0.1367(3) 0.0222(6) Uani 1 1 d . . . C2 C 0.24495(16) 0.3426(2) 0.0645(3) 0.0234(6) Uani 1 1 d . . . H2 H 0.2452 0.3373 -0.0145 0.028 Uiso 1 1 calc R . . C3 C 0.18076(16) 0.3403(2) 0.1093(3) 0.0246(6) Uani 1 1 d . . . H3 H 0.1367 0.3340 0.0610 0.029 Uiso 1 1 calc R . . C4 C 0.18152(15) 0.3473(2) 0.2256(3) 0.0226(6) Uani 1 1 d . . . C5 C 0.24557(17) 0.3591(2) 0.2973(3) 0.0285(7) Uani 1 1 d . . . H5 H 0.2452 0.3651 0.3762 0.034 Uiso 1 1 calc R . . C6 C 0.31014(16) 0.3622(2) 0.2534(3) 0.0271(6) Uani 1 1 d . . . H6 H 0.3542 0.3706 0.3015 0.033 Uiso 1 1 calc R . . C7 C 0.09094(14) 0.4439(2) 0.3578(2) 0.0210(6) Uani 1 1 d . . . C8 C 0.10074(16) 0.4439(2) 0.4752(3) 0.0261(6) Uani 1 1 d . . . H8 H 0.1125 0.3789 0.5154 0.031 Uiso 1 1 calc R . . C9 C 0.09323(16) 0.5390(2) 0.5331(2) 0.0251(6) Uani 1 1 d . . . H9 H 0.1010 0.5399 0.6130 0.030 Uiso 1 1 calc R . . C10 C 0.07433(14) 0.6330(2) 0.4737(2) 0.0193(5) Uani 1 1 d . . . C11 C 0.06319(16) 0.6336(2) 0.3574(2) 0.0246(6) Uani 1 1 d . . . H11 H 0.0494 0.6981 0.3174 0.030 Uiso 1 1 calc R . . C12 C 0.07244(16) 0.5388(2) 0.2998(2) 0.0254(6) Uani 1 1 d . . . H12 H 0.0661 0.5388 0.2198 0.031 Uiso 1 1 calc R . . C13 C 0.11053(15) 0.8489(2) 0.4722(2) 0.0211(6) Uani 1 1 d . . . C14 C 0.07193(15) 0.9317(2) 0.4153(3) 0.0252(6) Uani 1 1 d . . . H14 H 0.0227 0.9409 0.4217 0.030 Uiso 1 1 calc R . . C15 C 0.10582(16) 1.0009(2) 0.3490(2) 0.0245(6) Uani 1 1 d . . . H15 H 0.0796 1.0578 0.3096 0.029 Uiso 1 1 calc R . . C16 C 0.17793(15) 0.9876(2) 0.3399(2) 0.0204(6) Uani 1 1 d . . . C17 C 0.21670(16) 0.9060(3) 0.4013(3) 0.0311(7) Uani 1 1 d . . . H17 H 0.2665 0.8983 0.3979 0.037 Uiso 1 1 calc R . . C18 C 0.18292(17) 0.8373(3) 0.4664(3) 0.0303(7) Uani 1 1 d . . . H18 H 0.2092 0.7816 0.5077 0.036 Uiso 1 1 calc R . . C19 C 0.28352(15) 1.0056(2) 0.1971(2) 0.0222(6) Uani 1 1 d . . . C20 C 0.27631(16) 0.8970(2) 0.1693(3) 0.0272(6) Uani 1 1 d . . . H20 H 0.2345 0.8588 0.1819 0.033 Uiso 1 1 calc R . . C21 C 0.33060(16) 0.8443(2) 0.1228(3) 0.0292(7) Uani 1 1 d . . . H21 H 0.3265 0.7695 0.1063 0.035 Uiso 1 1 calc R . . C22 C 0.39120(16) 0.9014(2) 0.1003(3) 0.0260(6) Uani 1 1 d . . . C23 C 0.39737(16) 1.0101(2) 0.1269(2) 0.0247(6) Uani 1 1 d . . . H23 H 0.4381 1.0494 0.1111 0.030 Uiso 1 1 calc R . . C24 C 0.34419(15) 1.0616(2) 0.1766(2) 0.0234(6) Uani 1 1 d . . . H24 H 0.3494 1.1355 0.1967 0.028 Uiso 1 1 calc R . . C25 C 0.44407(15) 0.7026(2) 0.0496(3) 0.0246(6) Uani 1 1 d . . . C26 C 0.41958(15) 0.6432(2) -0.0457(3) 0.0248(6) Uani 1 1 d . . . H26 H 0.4131 0.6772 -0.1174 0.030 Uiso 1 1 calc R . . C27 C 0.40442(15) 0.5338(2) -0.0369(2) 0.0222(6) Uani 1 1 d . . . H27 H 0.3878 0.4927 -0.1022 0.027 Uiso 1 1 calc R . . C28 C 0.41393(14) 0.4859(2) 0.0684(2) 0.0205(6) Uani 1 1 d . . . C29 C 0.44069(15) 0.5441(2) 0.1645(3) 0.0259(6) Uani 1 1 d . . . H29 H 0.4482 0.5098 0.2360 0.031 Uiso 1 1 calc R . . C30 C 0.45615(16) 0.6521(2) 0.1544(3) 0.0266(6) Uani 1 1 d . . . H30 H 0.4751 0.6922 0.2191 0.032 Uiso 1 1 calc R . . C31 C 0.2788(3) 0.8678(5) 0.8327(5) 0.0795(16) Uiso 1 1 d . . . H31A H 0.3216 0.9136 0.8414 0.119 Uiso 1 1 calc R . . H31B H 0.2926 0.7933 0.8525 0.119 Uiso 1 1 calc R . . H31C H 0.2454 0.8937 0.8825 0.119 Uiso 1 1 calc R . . O1 O 0.37647(13) 0.3031(2) -0.0317(2) 0.0379(6) Uani 1 1 d . . . O2 O 0.44167(12) 0.2992(2) 0.1625(2) 0.0409(6) Uani 1 1 d . . . O3 O 0.11086(13) 0.73822(18) 0.65750(18) 0.0339(5) Uani 1 1 d . . . O4 O -0.00472(12) 0.78547(17) 0.5458(2) 0.0337(5) Uani 1 1 d . . . O5 O 0.2456(2) 0.8717(4) 0.7199(4) 0.0879(12) Uiso 1 1 d . . . H5A H 0.2088 0.8330 0.7126 0.132 Uiso 1 1 calc R . . S1 S 0.39054(4) 0.34858(6) 0.08011(7) 0.0256(2) Uani 1 1 d . . . S2 S 0.10084(4) 0.32218(6) 0.28255(7) 0.0297(2) Uani 1 1 d . . . S3 S 0.06780(4) 0.75375(6) 0.54925(6) 0.02284(19) Uani 1 1 d . . . S4 S 0.21681(4) 1.08032(5) 0.25449(6) 0.02359(19) Uani 1 1 d . . . S5 S 0.46180(4) 0.84250(6) 0.03759(8) 0.0334(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0219(14) 0.0146(13) 0.0324(15) 0.0024(11) 0.0121(11) 0.0027(10) C2 0.0255(14) 0.0195(14) 0.0267(15) 0.0034(11) 0.0095(11) 0.0009(11) C3 0.0229(14) 0.0202(14) 0.0312(16) 0.0023(11) 0.0060(12) 0.0022(11) C4 0.0221(14) 0.0137(13) 0.0350(16) -0.0010(11) 0.0145(12) -0.0014(10) C5 0.0338(17) 0.0256(16) 0.0285(16) -0.0023(12) 0.0132(13) -0.0040(12) C6 0.0230(14) 0.0249(15) 0.0341(17) 0.0000(12) 0.0063(12) -0.0042(11) C7 0.0173(13) 0.0196(13) 0.0283(15) -0.0031(11) 0.0104(11) -0.0029(10) C8 0.0297(15) 0.0186(14) 0.0302(16) 0.0031(11) 0.0055(12) 0.0010(11) C9 0.0301(15) 0.0233(15) 0.0213(14) 0.0038(11) 0.0019(11) -0.0009(12) C10 0.0189(13) 0.0161(13) 0.0243(14) -0.0032(10) 0.0080(10) -0.0013(10) C11 0.0328(16) 0.0171(13) 0.0247(15) 0.0045(11) 0.0070(12) 0.0002(11) C12 0.0333(16) 0.0220(15) 0.0228(14) -0.0012(11) 0.0103(12) -0.0016(12) C13 0.0254(14) 0.0165(13) 0.0221(14) -0.0002(10) 0.0059(11) -0.0016(10) C14 0.0216(14) 0.0230(15) 0.0334(16) 0.0005(12) 0.0117(12) 0.0043(11) C15 0.0265(15) 0.0187(14) 0.0296(15) 0.0030(11) 0.0079(12) 0.0054(11) C16 0.0235(14) 0.0147(13) 0.0236(14) -0.0035(10) 0.0051(11) -0.0040(10) C17 0.0186(14) 0.0306(17) 0.0438(19) 0.0092(14) 0.0035(13) -0.0012(12) C18 0.0243(15) 0.0263(16) 0.0396(18) 0.0119(13) 0.0017(13) 0.0022(12) C19 0.0228(14) 0.0175(14) 0.0266(14) 0.0004(11) 0.0050(11) -0.0020(10) C20 0.0222(14) 0.0209(15) 0.0397(17) -0.0047(12) 0.0083(12) -0.0055(11) C21 0.0256(15) 0.0198(15) 0.0437(19) -0.0077(13) 0.0106(13) -0.0065(11) C22 0.0214(14) 0.0219(14) 0.0363(17) 0.0016(12) 0.0100(12) -0.0025(11) C23 0.0238(14) 0.0206(14) 0.0309(15) 0.0043(12) 0.0088(12) -0.0057(11) C24 0.0267(15) 0.0165(13) 0.0276(15) 0.0018(11) 0.0057(11) -0.0060(11) C25 0.0170(13) 0.0216(14) 0.0380(17) 0.0000(12) 0.0135(12) -0.0012(10) C26 0.0184(13) 0.0280(16) 0.0298(16) 0.0075(12) 0.0100(11) 0.0032(11) C27 0.0182(13) 0.0245(14) 0.0250(14) -0.0025(11) 0.0068(11) 0.0000(11) C28 0.0138(12) 0.0185(13) 0.0303(15) 0.0021(11) 0.0075(11) 0.0011(10) C29 0.0231(14) 0.0288(16) 0.0267(15) 0.0042(12) 0.0062(11) -0.0001(12) C30 0.0245(15) 0.0287(16) 0.0273(15) -0.0050(12) 0.0065(12) -0.0044(12) O1 0.0359(13) 0.0321(13) 0.0502(15) -0.0144(11) 0.0220(11) -0.0071(10) O2 0.0249(12) 0.0339(13) 0.0652(17) 0.0140(12) 0.0110(11) 0.0062(10) O3 0.0492(14) 0.0271(12) 0.0263(12) -0.0022(9) 0.0087(10) 0.0021(10) O4 0.0355(12) 0.0258(12) 0.0443(14) 0.0032(10) 0.0213(10) 0.0041(9) S1 0.0218(4) 0.0187(4) 0.0390(4) 0.0011(3) 0.0133(3) 0.0022(3) S2 0.0298(4) 0.0192(4) 0.0450(5) -0.0080(3) 0.0223(3) -0.0071(3) S3 0.0294(4) 0.0176(4) 0.0234(4) -0.0009(3) 0.0107(3) 0.0005(3) S4 0.0259(4) 0.0148(3) 0.0316(4) 0.0000(3) 0.0092(3) -0.0018(3) S5 0.0298(4) 0.0216(4) 0.0537(5) 0.0015(3) 0.0232(4) -0.0037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.390(4) . ? C1 C6 1.400(4) . ? C1 S1 1.769(3) . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 S2 1.778(3) . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(4) . ? C7 C8 1.394(4) . ? C7 S2 1.782(3) . ? C8 C9 1.386(4) . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 S3 1.763(3) . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.384(4) . ? C13 C18 1.384(4) . ? C13 S3 1.760(3) . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.389(4) . ? C15 H15 0.9500 . ? C16 C17 1.398(4) . ? C16 S4 1.764(3) . ? C17 C18 1.370(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.389(4) . ? C19 C20 1.390(4) . ? C19 S4 1.775(3) . ? C20 C21 1.393(4) . ? C20 H20 0.9500 . ? C21 C22 1.402(4) . ? C21 H21 0.9500 . ? C22 C23 1.386(4) . ? C22 S5 1.774(3) . ? C23 C24 1.390(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 C30 1.395(4) . ? C25 S5 1.777(3) . ? C26 C27 1.394(4) . ? C26 H26 0.9500 . ? C27 C28 1.385(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(4) . ? C28 S1 1.770(3) . ? C29 C30 1.380(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O5 1.412(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O1 S1 1.445(2) . ? O2 S1 1.422(2) . ? O3 S3 1.447(2) . ? O4 S3 1.419(2) . ? O5 H5A 0.8400 . ? 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 C2 C1 C6 121.8(3) . . ? C2 C1 S1 119.0(2) . . ? C6 C1 S1 119.1(2) . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 S2 119.9(2) . . ? C3 C4 S2 118.7(2) . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 118.5(3) . . ? C5 C6 H6 120.7 . . ? C1 C6 H6 120.7 . . ? C12 C7 C8 119.7(3) . . ? C12 C7 S2 120.1(2) . . ? C8 C7 S2 120.2(2) . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 121.1(3) . . ? C11 C10 S3 120.1(2) . . ? C9 C10 S3 118.8(2) . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C7 120.7(3) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C14 C13 C18 120.6(3) . . ? C14 C13 S3 120.5(2) . . ? C18 C13 S3 118.8(2) . . ? C15 C14 C13 119.3(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 S4 117.2(2) . . ? C17 C16 S4 123.3(2) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 119.9(3) . . ? C24 C19 S4 116.9(2) . . ? C20 C19 S4 123.2(2) . . ? C19 C20 C21 119.8(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.5(3) . . ? C23 C22 S5 117.0(2) . . ? C21 C22 S5 123.5(2) . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 120.4(3) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C30 120.0(3) . . ? C26 C25 S5 119.9(2) . . ? C30 C25 S5 120.1(2) . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 119.0(3) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 121.2(3) . . ? C27 C28 S1 118.8(2) . . ? C29 C28 S1 119.9(2) . . ? C30 C29 C28 119.2(3) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C25 120.3(3) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C31 O5 H5A 109.5 . . ? O2 S1 O1 119.87(16) . . ? O2 S1 C1 106.91(14) . . ? O1 S1 C1 107.91(14) . . ? O2 S1 C28 108.46(14) . . ? O1 S1 C28 108.57(14) . . ? C1 S1 C28 103.98(12) . . ? C4 S2 C7 101.55(13) . . ? O4 S3 O3 118.99(14) . . ? O4 S3 C13 107.90(13) . . ? O3 S3 C13 108.58(14) . . ? O4 S3 C10 110.79(14) . . ? O3 S3 C10 106.12(13) . . ? C13 S3 C10 103.34(13) . . ? C16 S4 C19 104.88(13) . . ? C22 S5 C25 101.99(13) . . ? 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 C6 C1 C2 C3 -0.9(4) . . . . ? S1 C1 C2 C3 176.7(2) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? C2 C3 C4 S2 -169.9(2) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? S2 C4 C5 C6 170.2(2) . . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? C2 C1 C6 C5 1.2(4) . . . . ? S1 C1 C6 C5 -176.3(2) . . . . ? C12 C7 C8 C9 -1.2(4) . . . . ? S2 C7 C8 C9 179.7(2) . . . . ? C7 C8 C9 C10 1.5(5) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C8 C9 C10 S3 -178.1(2) . . . . ? C9 C10 C11 C12 -1.2(4) . . . . ? S3 C10 C11 C12 176.5(2) . . . . ? C10 C11 C12 C7 1.6(5) . . . . ? C8 C7 C12 C11 -0.4(4) . . . . ? S2 C7 C12 C11 178.7(2) . . . . ? C18 C13 C14 C15 2.3(5) . . . . ? S3 C13 C14 C15 -175.5(2) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C17 -2.3(4) . . . . ? C14 C15 C16 S4 -179.5(2) . . . . ? C15 C16 C17 C18 2.6(5) . . . . ? S4 C16 C17 C18 179.6(3) . . . . ? C16 C17 C18 C13 -0.5(5) . . . . ? C14 C13 C18 C17 -2.0(5) . . . . ? S3 C13 C18 C17 175.9(3) . . . . ? C24 C19 C20 C21 1.2(5) . . . . ? S4 C19 C20 C21 178.9(2) . . . . ? C19 C20 C21 C22 -2.3(5) . . . . ? C20 C21 C22 C23 1.4(5) . . . . ? C20 C21 C22 S5 -178.1(3) . . . . ? C21 C22 C23 C24 0.7(5) . . . . ? S5 C22 C23 C24 -179.8(2) . . . . ? C20 C19 C24 C23 0.9(5) . . . . ? S4 C19 C24 C23 -177.0(2) . . . . ? C22 C23 C24 C19 -1.8(5) . . . . ? C30 C25 C26 C27 2.4(4) . . . . ? S5 C25 C26 C27 -179.0(2) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? C26 C27 C28 C29 -2.4(4) . . . . ? C26 C27 C28 S1 177.0(2) . . . . ? C27 C28 C29 C30 1.7(4) . . . . ? S1 C28 C29 C30 -177.6(2) . . . . ? C28 C29 C30 C25 1.0(4) . . . . ? C26 C25 C30 C29 -3.0(4) . . . . ? S5 C25 C30 C29 178.3(2) . . . . ? C2 C1 S1 O2 -146.9(2) . . . . ? C6 C1 S1 O2 30.7(3) . . . . ? C2 C1 S1 O1 -16.7(3) . . . . ? C6 C1 S1 O1 160.9(2) . . . . ? C2 C1 S1 C28 98.5(2) . . . . ? C6 C1 S1 C28 -83.9(2) . . . . ? C27 C28 S1 O2 142.2(2) . . . . ? C29 C28 S1 O2 -38.4(3) . . . . ? C27 C28 S1 O1 10.5(3) . . . . ? C29 C28 S1 O1 -170.2(2) . . . . ? C27 C28 S1 C1 -104.2(2) . . . . ? C29 C28 S1 C1 75.1(2) . . . . ? C5 C4 S2 C7 64.9(3) . . . . ? C3 C4 S2 C7 -123.5(2) . . . . ? C12 C7 S2 C4 71.4(3) . . . . ? C8 C7 S2 C4 -109.6(2) . . . . ? C14 C13 S3 O4 -4.3(3) . . . . ? C18 C13 S3 O4 177.8(2) . . . . ? C14 C13 S3 O3 -134.5(2) . . . . ? C18 C13 S3 O3 47.6(3) . . . . ? C14 C13 S3 C10 113.1(2) . . . . ? C18 C13 S3 C10 -64.8(3) . . . . ? C11 C10 S3 O4 74.0(3) . . . . ? C9 C10 S3 O4 -108.3(2) . . . . ? C11 C10 S3 O3 -155.5(2) . . . . ? C9 C10 S3 O3 22.2(3) . . . . ? C11 C10 S3 C13 -41.4(3) . . . . ? C9 C10 S3 C13 136.4(2) . . . . ? C15 C16 S4 C19 -148.0(2) . . . . ? C17 C16 S4 C19 35.0(3) . . . . ? C24 C19 S4 C16 -147.9(2) . . . . ? C20 C19 S4 C16 34.3(3) . . . . ? C23 C22 S5 C25 166.5(3) . . . . ? C21 C22 S5 C25 -14.0(3) . . . . ? C26 C25 S5 C22 109.3(2) . . . . ? C30 C25 S5 C22 -72.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O3 0.84 2.21 3.041(5) 168.6 . _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.646 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.122 #===END data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 737301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 O4 S4, C H2 Cl2' _chemical_formula_sum 'C37 H26 Cl2 O4 S4' _chemical_formula_weight 733.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5898(11) _cell_length_b 23.7421(19) _cell_length_c 20.4841(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.522(5) _cell_angle_gamma 90.00 _cell_volume 7082.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 49 _cell_measurement_theta_min 10.93 _cell_measurement_theta_max 22.50 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 4.170 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5820 _exptl_absorpt_correction_T_max 0.8577 _exptl_absorpt_process_details ; Bruker XPREP, version 5.1/NT Ellipsoidal absorption correction using psi-scans ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11255 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 61.99 _reflns_number_total 10688 _reflns_number_gt 6098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disorders in the C(1) to C(12) C6H4-C6H4 moiety, and in the C(1B) to C(6B) ring, were modelled by the inclusion of two partial occupancy orientations, with the geometries of the six-membered rings optimised in each case. Only the non-hydrogen atoms of the major occupancy orientations were refined anisotropically. ; _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^)+(0.1148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10688 _refine_ls_number_parameters 848 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2179 _refine_ls_wR_factor_gt 0.1937 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.64149(10) 0.27693(6) 0.74453(6) 0.0760(4) Uani 1 1 d . . . O11 O 0.7264(3) 0.2525(2) 0.7710(2) 0.0919(15) Uani 0.806(4) 1 d P A . O12 O 0.6098(4) 0.3279(2) 0.7655(2) 0.0925(15) Uani 0.806(4) 1 d P A . S2 S 0.63304(11) 0.24380(7) 0.23204(6) 0.0863(5) Uani 1 1 d . . . O21 O 0.7171(3) 0.2168(2) 0.2116(2) 0.0906(15) Uani 0.806(4) 1 d P A . O22 O 0.5944(4) 0.2890(2) 0.1985(2) 0.0975(16) Uani 0.806(4) 1 d P A . S3 S 0.34326(15) 0.04748(9) 0.23689(7) 0.1116(6) Uani 1 1 d . A . O31 O 0.3990(16) 0.0039(10) 0.2206(10) 0.099(7) Uiso 0.194(4) 1 d P . . O32 O 0.2659(17) 0.0752(11) 0.2045(12) 0.112(7) Uiso 0.194(4) 1 d P . . S4 S 0.33086(14) 0.09290(9) 0.75076(7) 0.1089(7) Uani 1 1 d . . . O41 O 0.3735(12) 0.0440(7) 0.7790(8) 0.069(5) Uiso 0.194(4) 1 d P . . O42 O 0.2521(13) 0.1183(8) 0.7692(8) 0.077(5) Uiso 0.194(4) 1 d P . . C1 C 0.6490(4) 0.2854(3) 0.6593(2) 0.068(4) Uani 0.670(15) 1 d PG A 1 C2 C 0.5819(5) 0.3127(4) 0.6199(3) 0.081(3) Uani 0.670(15) 1 d PG A 1 H2A H 0.5341 0.3313 0.6388 0.097 Uiso 0.670(15) 1 calc PR A 1 C3 C 0.5862(5) 0.3121(4) 0.5523(3) 0.076(2) Uani 0.670(15) 1 d PGD A 1 H3A H 0.5414 0.3304 0.5260 0.091 Uiso 0.670(15) 1 calc PR A 1 C4 C 0.6576(5) 0.2842(3) 0.5241(2) 0.071(9) Uani 0.670(15) 1 d PGD A 1 C5 C 0.7247(4) 0.2569(4) 0.5635(3) 0.076(2) Uani 0.670(15) 1 d PGD A 1 H5A H 0.7725 0.2383 0.5446 0.091 Uiso 0.670(15) 1 calc PR A 1 C6 C 0.7204(4) 0.2575(4) 0.6310(3) 0.071(2) Uani 0.670(15) 1 d PG A 1 H6A H 0.7653 0.2392 0.6574 0.085 Uiso 0.670(15) 1 calc PR A 1 C7 C 0.6582(5) 0.2791(3) 0.4492(2) 0.076(6) Uani 0.670(15) 1 d PGD A 1 C8 C 0.5895(5) 0.3044(4) 0.4093(3) 0.081(3) Uani 0.670(15) 1 d PGD A 1 H8A H 0.5470 0.3280 0.4275 0.097 Uiso 0.670(15) 1 calc PR A 1 C9 C 0.5842(5) 0.2943(5) 0.3424(3) 0.082(3) Uani 0.670(15) 1 d PG A 1 H9A H 0.5382 0.3112 0.3157 0.098 Uiso 0.670(15) 1 calc PR A 1 C10 C 0.6477(5) 0.2589(4) 0.3153(2) 0.080(6) Uani 0.670(15) 1 d PG A 1 C11 C 0.7164(6) 0.2337(4) 0.3552(3) 0.076(3) Uani 0.670(15) 1 d PG A 1 H11A H 0.7589 0.2101 0.3371 0.092 Uiso 0.670(15) 1 calc PR A 1 C12 C 0.7217(6) 0.2438(4) 0.4221(3) 0.075(3) Uani 0.670(15) 1 d PGD A 1 H12A H 0.7677 0.2269 0.4488 0.090 Uiso 0.670(15) 1 calc PR A 1 C1' C 0.6522(9) 0.2775(6) 0.6591(4) 0.056(7) Uiso 0.330(15) 1 d PG A 2 C2' C 0.6158(10) 0.3235(5) 0.6244(6) 0.057(5) Uiso 0.330(15) 1 d PG A 2 H2'A H 0.5890 0.3529 0.6463 0.069 Uiso 0.330(15) 1 calc PR A 2 C3' C 0.6195(10) 0.3254(5) 0.5567(6) 0.058(5) Uiso 0.330(15) 1 d PGD A 2 H3'A H 0.5951 0.3562 0.5335 0.069 Uiso 0.330(15) 1 calc PR A 2 C4' C 0.6595(9) 0.2815(6) 0.5239(4) 0.052(14) Uiso 0.330(15) 1 d PGD A 2 C5' C 0.6959(11) 0.2355(6) 0.5587(6) 0.074(6) Uiso 0.330(15) 1 d PGD A 2 H5'A H 0.7227 0.2061 0.5367 0.089 Uiso 0.330(15) 1 calc PR A 2 C6' C 0.6922(11) 0.2336(6) 0.6263(6) 0.068(5) Uiso 0.330(15) 1 d PG A 2 H6'A H 0.7166 0.2028 0.6495 0.081 Uiso 0.330(15) 1 calc PR A 2 C7' C 0.6571(9) 0.2774(6) 0.4538(5) 0.041(7) Uiso 0.330(15) 1 d PGD A 2 C8' C 0.6190(10) 0.3197(5) 0.4139(7) 0.061(5) Uiso 0.330(15) 1 d PGD A 2 H8'A H 0.5973 0.3525 0.4324 0.073 Uiso 0.330(15) 1 calc PR A 2 C9' C 0.6134(12) 0.3130(6) 0.3463(6) 0.082(7) Uiso 0.330(15) 1 d PG A 2 H9'A H 0.5879 0.3413 0.3196 0.099 Uiso 0.330(15) 1 calc PR A 2 C10' C 0.6458(11) 0.2640(7) 0.3187(5) 0.057(8) Uiso 0.330(15) 1 d PG A 2 C11' C 0.6839(13) 0.2216(6) 0.3586(7) 0.091(8) Uiso 0.330(15) 1 d PG A 2 H11D H 0.7056 0.1888 0.3402 0.110 Uiso 0.330(15) 1 calc PR A 2 C12' C 0.6896(12) 0.2283(6) 0.4262(7) 0.097(8) Uiso 0.330(15) 1 d PGD A 2 H12D H 0.7151 0.2000 0.4529 0.116 Uiso 0.330(15) 1 calc PR A 2 C13 C 0.5490(4) 0.1887(3) 0.2291(2) 0.0750(14) Uani 1 1 d . A . C14 C 0.4579(4) 0.2023(3) 0.2392(3) 0.0897(17) Uani 1 1 d . . . H14A H 0.4390 0.2392 0.2452 0.108 Uiso 1 1 calc R A . C15 C 0.3985(5) 0.1582(3) 0.2398(3) 0.0960(19) Uani 1 1 d . A . H15A H 0.3371 0.1658 0.2458 0.115 Uiso 1 1 calc R . . C16 C 0.4246(4) 0.1026(3) 0.2320(2) 0.0818(16) Uani 1 1 d . . . C17 C 0.5154(5) 0.0909(3) 0.2201(3) 0.0922(17) Uani 1 1 d . A . H17A H 0.5340 0.0540 0.2132 0.111 Uiso 1 1 calc R . . C18 C 0.5777(4) 0.1345(3) 0.2187(3) 0.0842(16) Uani 1 1 d . . . H18A H 0.6387 0.1273 0.2108 0.101 Uiso 1 1 calc R A . C19 C 0.3288(4) 0.0501(3) 0.3219(3) 0.0823(15) Uani 1 1 d . . . C20 C 0.3897(4) 0.0216(3) 0.3648(3) 0.0984(19) Uani 1 1 d . A . H20A H 0.4361 -0.0003 0.3488 0.118 Uiso 1 1 calc R . . C21 C 0.3809(4) 0.0260(3) 0.4308(3) 0.0897(17) Uani 1 1 d . . . H21A H 0.4224 0.0068 0.4589 0.108 Uiso 1 1 calc R A . C22 C 0.3129(4) 0.0578(2) 0.4577(2) 0.0686(12) Uani 1 1 d . A . C23 C 0.2487(4) 0.0819(3) 0.4139(3) 0.0876(16) Uani 1 1 d . . . H23A H 0.1996 0.1015 0.4299 0.105 Uiso 1 1 calc R A . C24 C 0.2552(5) 0.0777(3) 0.3463(3) 0.0955(18) Uani 1 1 d . A . H24A H 0.2102 0.0936 0.3179 0.115 Uiso 1 1 calc R . . C25 C 0.3090(4) 0.0644(2) 0.5291(2) 0.0708(13) Uani 1 1 d . . . C26 C 0.3604(4) 0.0285(3) 0.5715(3) 0.0882(17) Uani 1 1 d . A . H26A H 0.3924 -0.0013 0.5542 0.106 Uiso 1 1 calc R . . C27 C 0.3643(5) 0.0365(3) 0.6386(3) 0.0892(17) Uani 1 1 d . . . H27A H 0.3981 0.0117 0.6657 0.107 Uiso 1 1 calc R A . C28 C 0.3193(4) 0.0799(3) 0.6651(3) 0.0832(16) Uani 1 1 d . A . C29 C 0.2639(5) 0.1133(3) 0.6247(3) 0.106(2) Uani 1 1 d . . . H29A H 0.2286 0.1415 0.6423 0.127 Uiso 1 1 calc R A . C30 C 0.2605(4) 0.1051(3) 0.5577(3) 0.0957(18) Uani 1 1 d . A . H30A H 0.2232 0.1286 0.5312 0.115 Uiso 1 1 calc R . . C31 C 0.4201(4) 0.1440(2) 0.7520(2) 0.0745(14) Uani 1 1 d . . . C32 C 0.5110(4) 0.1298(2) 0.7621(2) 0.0792(15) Uani 1 1 d . A . H32A H 0.5271 0.0924 0.7701 0.095 Uiso 1 1 calc R . . C33 C 0.5786(4) 0.1701(2) 0.7604(2) 0.0771(14) Uani 1 1 d . . . H33A H 0.6401 0.1598 0.7662 0.093 Uiso 1 1 calc R A . C34 C 0.5554(3) 0.2259(2) 0.7499(2) 0.0648(12) Uani 1 1 d . A . C35 C 0.4646(4) 0.2417(2) 0.7411(2) 0.0772(14) Uani 1 1 d . . . H35A H 0.4486 0.2793 0.7347 0.093 Uiso 1 1 calc R A . C36 C 0.3966(4) 0.1997(3) 0.7421(3) 0.0855(16) Uani 1 1 d . A . H36A H 0.3351 0.2097 0.7360 0.103 Uiso 1 1 calc R . . S1A S 0.86526(11) 0.08627(6) 0.22563(6) 0.0816(4) Uani 1 1 d . . . O11A O 0.7760(5) 0.0654(3) 0.2000(3) 0.084(2) Uani 0.50 1 d P . . O12A O 0.9103(6) 0.1289(3) 0.1950(3) 0.089(2) Uani 0.50 1 d P . . S2A S 0.86110(11) 0.11780(7) 0.74002(6) 0.0816(4) Uani 1 1 d . . . O21A O 0.7714(5) 0.0951(3) 0.7586(3) 0.0771(19) Uani 0.50 1 d P . . O22A O 0.8980(6) 0.1630(3) 0.7647(3) 0.081(2) Uani 0.50 1 d P . . C1A C 0.8576(4) 0.1004(2) 0.3096(2) 0.0699(13) Uani 1 1 d . . . C2A C 0.9297(4) 0.1252(2) 0.3456(2) 0.0811(15) Uani 1 1 d . . . H2AA H 0.9811 0.1372 0.3248 0.097 Uiso 1 1 calc R . . C3A C 0.9261(4) 0.1327(2) 0.4127(2) 0.0772(14) Uani 1 1 d . . . H3AA H 0.9752 0.1496 0.4362 0.093 Uiso 1 1 calc R . . C4A C 0.8512(3) 0.11530(19) 0.4447(2) 0.0632(11) Uani 1 1 d . . . C5A C 0.7775(4) 0.0936(3) 0.4067(3) 0.0832(15) Uani 1 1 d . . . H5AA H 0.7239 0.0842 0.4266 0.100 Uiso 1 1 calc R . . C6A C 0.7814(4) 0.0854(3) 0.3405(3) 0.0898(17) Uani 1 1 d . . . H6AA H 0.7316 0.0695 0.3166 0.108 Uiso 1 1 calc R . . C7A C 0.8499(3) 0.11946(19) 0.5168(2) 0.0633(11) Uani 1 1 d . . . C8A C 0.9109(4) 0.1537(2) 0.5535(2) 0.0724(13) Uani 1 1 d . . . H8AA H 0.9507 0.1768 0.5318 0.087 Uiso 1 1 calc R . . C9A C 0.9144(4) 0.1545(2) 0.6212(3) 0.0785(14) Uani 1 1 d . . . H9AA H 0.9565 0.1773 0.6446 0.094 Uiso 1 1 calc R . . C10A C 0.8544(4) 0.1209(2) 0.6534(2) 0.0706(13) Uani 1 1 d . . . C11A C 0.7919(4) 0.0882(3) 0.6187(3) 0.0892(17) Uani 1 1 d . . . H11B H 0.7506 0.0663 0.6405 0.107 Uiso 1 1 calc R . . C12A C 0.7897(4) 0.0876(2) 0.5516(3) 0.0851(16) Uani 1 1 d . . . H12B H 0.7466 0.0651 0.5288 0.102 Uiso 1 1 calc R . . C13A C 0.9405(4) 0.0617(2) 0.7538(2) 0.0655(12) Uani 1 1 d . . . C14A C 1.0331(4) 0.0682(2) 0.7430(4) 0.100(2) Uani 1 1 d . . . H14B H 1.0556 0.1030 0.7305 0.121 Uiso 1 1 calc R . . C15A C 1.0906(4) 0.0228(2) 0.7509(4) 0.101(2) Uani 1 1 d . . . H15B H 1.1523 0.0269 0.7429 0.122 Uiso 1 1 calc R . . C16A C 1.0594(4) -0.0283(2) 0.7703(2) 0.0663(12) Uani 1 1 d . . . C17A C 0.9681(5) -0.0347(3) 0.7823(3) 0.0933(18) Uani 1 1 d . . . H17B H 0.9462 -0.0693 0.7958 0.112 Uiso 1 1 calc R . . C18A C 0.9100(4) 0.0102(2) 0.7743(3) 0.0834(16) Uani 1 1 d . . . H18B H 0.8485 0.0059 0.7829 0.100 Uiso 1 1 calc R . . S1B S 0.09169(12) -0.06100(8) 1.00536(12) 0.1162(7) Uani 1 1 d . . . O11B O 0.0498(6) -0.0635(4) 1.0620(6) 0.129(4) Uani 0.50 1 d P B . O12B O 0.0427(6) -0.0703(4) 0.9396(5) 0.120(3) Uani 0.50 1 d P B . S2B S 0.60681(12) 0.25075(8) 0.97881(12) 0.1117(6) Uani 1 1 d . . . O21B O 0.6192(7) 0.2794(4) 1.0405(6) 0.139(4) Uani 0.50 1 d P . . O22B O 0.6078(6) 0.2746(4) 0.9175(6) 0.130(4) Uani 0.50 1 d P . . C1B C 0.1633(4) -0.0012(3) 0.9938(5) 0.078(3) Uani 0.623(16) 1 d PG B 1 C2B C 0.2039(8) 0.0114(4) 0.9359(3) 0.104(4) Uani 0.623(16) 1 d PG B 1 H2BA H 0.1895 -0.0098 0.8985 0.124 Uiso 0.623(16) 1 calc PR B 1 C3B C 0.2659(8) 0.0558(4) 0.9339(3) 0.097(4) Uani 0.623(16) 1 d PG B 1 H3BA H 0.2930 0.0642 0.8952 0.116 Uiso 0.623(16) 1 calc PR B 1 C4B C 0.2873(5) 0.0874(3) 0.9899(4) 0.074(5) Uani 0.623(16) 1 d PG B 1 C5B C 0.2468(8) 0.0748(3) 1.0477(4) 0.093(4) Uani 0.623(16) 1 d PG B 1 H5BA H 0.2612 0.0960 1.0852 0.112 Uiso 0.623(16) 1 calc PR B 1 C6B C 0.1848(8) 0.0305(3) 1.0497(4) 0.100(4) Uani 0.623(16) 1 d PG B 1 H6BA H 0.1577 0.0220 1.0884 0.120 Uiso 0.623(16) 1 calc PR B 1 C1* C 0.1675(8) -0.0009(5) 1.0114(6) 0.079(6) Uiso 0.377(16) 1 d PG B 2 C2* C 0.1688(8) 0.0290(5) 0.9531(6) 0.072(5) Uiso 0.377(16) 1 d PG B 2 H2*A H 0.1281 0.0198 0.9181 0.086 Uiso 0.377(16) 1 calc PR B 2 C3* C 0.2310(9) 0.0728(5) 0.9472(6) 0.068(4) Uiso 0.377(16) 1 d PG B 2 H3*A H 0.2319 0.0928 0.9082 0.081 Uiso 0.377(16) 1 calc PR B 2 C4* C 0.2920(8) 0.0867(4) 0.9996(6) 0.056(6) Uiso 0.377(16) 1 d PG B 2 C5* C 0.2906(10) 0.0568(6) 1.0579(5) 0.084(5) Uiso 0.377(16) 1 d PG B 2 H5*A H 0.3314 0.0660 1.0929 0.101 Uiso 0.377(16) 1 calc PR B 2 C6* C 0.2284(11) 0.0130(6) 1.0638(5) 0.080(5) Uiso 0.377(16) 1 d PG B 2 H6*A H 0.2275 -0.0070 1.1027 0.096 Uiso 0.377(16) 1 calc PR B 2 C7B C 0.3628(4) 0.1310(2) 0.9904(2) 0.0677(13) Uani 1 1 d . . . C8B C 0.3895(5) 0.1511(3) 0.9322(3) 0.111(2) Uani 1 1 d . B . H8BA H 0.3593 0.1388 0.8935 0.133 Uiso 1 1 calc R . . C9B C 0.4614(5) 0.1897(4) 0.9296(3) 0.116(2) Uani 1 1 d . . . H9BA H 0.4763 0.2037 0.8891 0.139 Uiso 1 1 calc R B . C10B C 0.5098(4) 0.2073(2) 0.9839(3) 0.0783(14) Uani 1 1 d . B . C11B C 0.4819(6) 0.1892(4) 1.0423(3) 0.117(2) Uani 1 1 d . . . H11C H 0.5122 0.2020 1.0807 0.140 Uiso 1 1 calc R B . C12B C 0.4087(5) 0.1518(3) 1.0461(3) 0.109(2) Uani 1 1 d . B . H12C H 0.3905 0.1407 1.0869 0.131 Uiso 1 1 calc R . . C13B C 0.6962(4) 0.2003(2) 0.9835(2) 0.0782(14) Uani 1 1 d . . . C14B C 0.7293(5) 0.1782(3) 0.9277(3) 0.104(2) Uani 1 1 d . . . H14C H 0.7063 0.1911 0.8871 0.125 Uiso 1 1 calc R . . C15B C 0.7950(5) 0.1379(3) 0.9310(3) 0.114(2) Uani 1 1 d . . . H15C H 0.8183 0.1244 0.8927 0.136 Uiso 1 1 calc R . . C16B C 0.8272(4) 0.1171(3) 0.9899(3) 0.0838(16) Uani 1 1 d . . . C17B C 0.8011(5) 0.1413(3) 1.0455(3) 0.111(2) Uani 1 1 d . . . H17C H 0.8274 0.1299 1.0859 0.133 Uiso 1 1 calc R . . C18B C 0.7353(5) 0.1830(3) 1.0423(3) 0.110(2) Uani 1 1 d . . . H18C H 0.7174 0.1995 1.0807 0.132 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 S1 0.0760(9) 0.0874(9) 0.0643(7) -0.0027(6) 0.0027(6) -0.0202(7) O11 0.082(3) 0.120(4) 0.073(3) 0.014(3) -0.006(2) -0.017(3) O12 0.117(4) 0.086(3) 0.076(3) -0.023(2) 0.017(3) -0.026(3) S2 0.0827(10) 0.1207(12) 0.0563(7) 0.0127(7) 0.0121(6) -0.0116(9) O21 0.066(3) 0.128(4) 0.081(3) -0.010(3) 0.032(2) -0.011(3) O22 0.123(4) 0.093(3) 0.078(3) 0.018(3) 0.016(3) -0.013(3) S3 0.1312(15) 0.1330(15) 0.0706(9) -0.0056(9) 0.0058(9) -0.0379(13) S4 0.1232(14) 0.1350(15) 0.0712(8) -0.0104(9) 0.0279(9) -0.0634(12) C1 0.063(6) 0.067(6) 0.076(7) -0.008(4) 0.009(4) -0.026(4) C2 0.091(8) 0.073(5) 0.079(5) -0.008(4) 0.009(5) 0.003(6) C3 0.085(7) 0.074(5) 0.068(5) -0.001(4) 0.001(4) 0.007(6) C4 0.071(10) 0.061(9) 0.082(12) 0.003(4) 0.019(5) -0.017(4) C5 0.071(6) 0.086(6) 0.069(5) -0.007(4) -0.001(4) 0.005(5) C6 0.076(6) 0.074(6) 0.063(4) -0.001(4) 0.006(4) -0.003(5) C7 0.081(8) 0.068(7) 0.078(8) 0.011(4) 0.003(4) -0.012(4) C8 0.066(6) 0.082(6) 0.093(6) -0.010(5) -0.002(5) 0.018(6) C9 0.078(6) 0.109(7) 0.058(4) 0.001(4) -0.007(4) 0.010(7) C10 0.075(7) 0.102(10) 0.066(6) 0.016(4) 0.024(4) -0.008(5) C11 0.079(7) 0.097(6) 0.054(4) 0.001(4) 0.010(4) 0.006(6) C12 0.087(7) 0.075(5) 0.063(4) -0.005(4) 0.005(4) 0.023(6) C13 0.068(4) 0.100(4) 0.058(3) 0.010(3) 0.004(2) -0.002(3) C14 0.065(4) 0.104(4) 0.101(4) 0.014(3) 0.010(3) 0.017(3) C15 0.072(4) 0.122(5) 0.096(4) 0.015(4) 0.019(3) 0.019(4) C16 0.093(4) 0.098(4) 0.053(3) 0.007(2) -0.008(3) -0.014(3) C17 0.091(5) 0.106(5) 0.080(4) -0.006(3) 0.009(3) -0.005(4) C18 0.055(3) 0.126(5) 0.072(3) -0.005(3) 0.010(2) 0.015(3) C19 0.079(4) 0.093(4) 0.074(3) 0.001(3) -0.003(3) -0.013(3) C20 0.086(4) 0.119(5) 0.089(4) -0.013(4) 0.003(3) 0.007(4) C21 0.076(4) 0.120(5) 0.073(3) -0.004(3) -0.003(3) 0.002(4) C22 0.070(3) 0.062(3) 0.072(3) 0.005(2) -0.005(2) -0.010(3) C23 0.078(4) 0.095(4) 0.091(4) 0.009(3) 0.012(3) 0.019(3) C24 0.092(4) 0.112(5) 0.079(4) 0.021(3) -0.019(3) 0.014(4) C25 0.081(4) 0.065(3) 0.067(3) 0.002(2) 0.005(2) -0.011(3) C26 0.113(5) 0.080(4) 0.073(3) 0.009(3) 0.012(3) 0.001(3) C27 0.105(5) 0.090(4) 0.072(3) 0.004(3) 0.000(3) -0.009(4) C28 0.096(4) 0.082(4) 0.072(3) -0.004(3) 0.010(3) -0.036(3) C29 0.110(5) 0.124(5) 0.085(4) -0.033(4) 0.014(4) 0.013(4) C30 0.097(5) 0.102(5) 0.088(4) -0.002(3) -0.001(3) 0.023(4) C31 0.084(4) 0.084(4) 0.058(3) -0.008(2) 0.026(3) -0.019(3) C32 0.086(4) 0.078(3) 0.075(3) 0.003(3) 0.013(3) 0.001(3) C33 0.072(4) 0.087(4) 0.072(3) -0.001(3) 0.007(3) -0.003(3) C34 0.058(3) 0.077(3) 0.060(2) -0.005(2) 0.010(2) -0.009(2) C35 0.067(3) 0.084(3) 0.081(3) -0.009(3) 0.009(3) 0.003(3) C36 0.063(3) 0.115(5) 0.079(3) -0.015(3) 0.012(3) -0.006(3) S1A 0.0945(11) 0.0870(9) 0.0622(7) 0.0072(6) -0.0052(7) 0.0138(8) O11A 0.087(5) 0.100(5) 0.062(4) -0.003(3) -0.016(3) 0.023(4) O12A 0.135(7) 0.076(4) 0.057(4) 0.018(3) 0.017(4) 0.000(5) S2A 0.0887(10) 0.0896(10) 0.0685(7) -0.0018(7) 0.0197(7) 0.0149(8) O21A 0.060(4) 0.089(5) 0.084(4) 0.004(4) 0.027(3) 0.004(4) O22A 0.112(6) 0.063(4) 0.068(4) -0.007(3) 0.013(4) -0.001(4) C1A 0.081(4) 0.069(3) 0.060(3) 0.008(2) 0.001(3) 0.010(3) C2A 0.096(4) 0.086(4) 0.063(3) 0.004(3) 0.015(3) -0.015(3) C3A 0.083(4) 0.083(3) 0.066(3) 0.001(2) 0.009(3) -0.012(3) C4A 0.070(3) 0.057(3) 0.063(3) 0.007(2) 0.004(2) -0.003(2) C5A 0.073(4) 0.102(4) 0.075(3) 0.002(3) 0.006(3) -0.010(3) C6A 0.089(4) 0.105(4) 0.074(3) 0.002(3) -0.003(3) -0.004(4) C7A 0.071(3) 0.055(2) 0.064(3) 0.005(2) 0.004(2) 0.000(2) C8A 0.075(3) 0.063(3) 0.080(3) -0.002(2) 0.016(3) -0.017(3) C9A 0.082(4) 0.079(3) 0.075(3) -0.008(3) 0.009(3) -0.015(3) C10A 0.081(4) 0.070(3) 0.061(3) 0.000(2) 0.012(2) 0.007(3) C11A 0.097(4) 0.092(4) 0.078(3) 0.015(3) 0.005(3) -0.017(3) C12A 0.092(4) 0.088(4) 0.074(3) 0.016(3) -0.002(3) -0.024(3) C13A 0.074(3) 0.072(3) 0.051(2) -0.006(2) 0.005(2) 0.001(3) C14A 0.086(4) 0.061(3) 0.157(6) 0.006(3) 0.026(4) -0.009(3) C15A 0.069(4) 0.071(4) 0.166(6) 0.008(4) 0.016(4) -0.008(3) C16A 0.073(4) 0.072(3) 0.053(2) 0.003(2) -0.003(2) -0.002(3) C17A 0.096(5) 0.088(4) 0.097(4) 0.035(3) 0.012(3) 0.000(4) C18A 0.066(3) 0.088(4) 0.099(4) 0.027(3) 0.020(3) -0.004(3) S1B 0.0629(10) 0.1046(13) 0.181(2) 0.0313(13) 0.0084(11) 0.0080(9) O11B 0.091(6) 0.107(7) 0.198(10) 0.040(7) 0.076(7) 0.032(5) O12B 0.075(5) 0.104(6) 0.173(9) 0.031(6) -0.059(6) -0.007(5) S2B 0.0813(11) 0.0906(11) 0.1633(18) -0.0138(12) 0.0094(11) 0.0103(9) O21B 0.104(7) 0.096(6) 0.217(12) -0.075(7) 0.007(7) 0.016(5) O22B 0.088(6) 0.114(7) 0.192(10) 0.094(7) 0.029(6) 0.032(5) C1B 0.051(6) 0.092(7) 0.093(7) 0.017(5) 0.009(4) 0.022(4) C2B 0.127(10) 0.116(9) 0.066(5) 0.003(6) -0.011(6) 0.002(9) C3B 0.136(11) 0.097(8) 0.059(5) 0.004(5) 0.008(6) -0.005(8) C4B 0.065(7) 0.097(9) 0.062(6) 0.010(4) 0.014(4) 0.027(5) C5B 0.126(10) 0.108(8) 0.051(4) -0.002(5) 0.040(5) 0.015(8) C6B 0.099(9) 0.122(8) 0.085(7) 0.029(7) 0.056(6) 0.017(8) C7B 0.069(3) 0.081(3) 0.053(2) -0.004(2) 0.005(2) 0.016(3) C8B 0.125(6) 0.156(7) 0.051(3) -0.007(3) 0.006(3) -0.029(5) C9B 0.125(6) 0.155(7) 0.070(4) 0.001(4) 0.016(4) -0.007(5) C10B 0.073(4) 0.077(3) 0.085(4) -0.008(3) 0.006(3) 0.003(3) C11B 0.123(6) 0.146(7) 0.078(4) -0.012(4) -0.022(4) -0.002(5) C12B 0.133(6) 0.135(6) 0.059(3) 0.002(3) 0.003(3) -0.004(5) C13B 0.074(4) 0.092(4) 0.067(3) -0.011(3) 0.000(3) 0.005(3) C14B 0.111(5) 0.145(6) 0.056(3) 0.008(3) -0.006(3) 0.047(5) C15B 0.116(5) 0.158(7) 0.066(3) 0.004(4) 0.004(3) 0.060(5) C16B 0.074(4) 0.092(4) 0.086(4) 0.014(3) 0.010(3) 0.010(3) C17B 0.112(5) 0.159(7) 0.061(3) 0.026(4) -0.005(3) 0.042(5) C18B 0.117(6) 0.150(6) 0.063(3) -0.010(4) 0.010(3) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O12 1.374(5) . ? S1 O11 1.443(5) . ? S1 C34 1.754(5) . ? S1 C1' 1.766(9) . ? S1 C1 1.768(5) . ? S2 O22 1.376(5) . ? S2 O21 1.468(5) . ? S2 C10 1.743(5) . ? S2 C13 1.792(6) . ? S2 C10' 1.837(11) . ? S3 O31 1.37(2) . ? S3 O32 1.43(3) . ? S3 C19 1.768(6) . ? S3 C16 1.773(6) . ? S4 O42 1.371(19) . ? S4 O41 1.424(17) . ? S4 C28 1.779(5) . ? S4 C31 1.780(5) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 C7 1.539(7) . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C1' C2' 1.3900 . ? C1' C6' 1.3900 . ? C2' C3' 1.3900 . ? C3' C4' 1.3900 . ? C4' C5' 1.3900 . ? C4' C7' 1.438(14) . ? C5' C6' 1.3900 . ? C7' C8' 1.3900 . ? C7' C12' 1.3900 . ? C8' C9' 1.3900 . ? C9' C10' 1.3900 . ? C10' C11' 1.3900 . ? C11' C12' 1.3900 . ? C13 C18 1.373(8) . ? C13 C14 1.396(8) . ? C14 C15 1.358(9) . ? C15 C16 1.387(8) . ? C16 C17 1.390(8) . ? C17 C18 1.379(8) . ? C19 C24 1.377(8) . ? C19 C20 1.386(8) . ? C20 C21 1.371(8) . ? C21 C22 1.387(8) . ? C22 C23 1.381(7) . ? C22 C25 1.476(7) . ? C23 C24 1.398(8) . ? C25 C30 1.352(8) . ? C25 C26 1.402(7) . ? C26 C27 1.385(7) . ? C27 C28 1.354(8) . ? C28 C29 1.374(9) . ? C29 C30 1.384(8) . ? C31 C32 1.371(8) . ? C31 C36 1.378(8) . ? C32 C33 1.378(7) . ? C33 C34 1.379(7) . ? C34 C35 1.379(7) . ? C35 C36 1.407(8) . ? S1A O12A 1.378(7) . ? S1A O11A 1.460(8) . ? S1A C16A 1.760(5) 3_756 ? S1A C1A 1.763(5) . ? S2A O22A 1.291(7) . ? S2A O21A 1.487(7) . ? S2A C10A 1.772(5) . ? S2A C13A 1.776(5) . ? C1A C6A 1.360(8) . ? C1A C2A 1.379(7) . ? C2A C3A 1.389(7) . ? C3A C4A 1.373(7) . ? C4A C5A 1.388(7) . ? C4A C7A 1.482(6) . ? C5A C6A 1.376(7) . ? C7A C12A 1.388(7) . ? C7A C8A 1.391(7) . ? C8A C9A 1.385(7) . ? C9A C10A 1.382(7) . ? C10A C11A 1.364(8) . ? C11A C12A 1.373(7) . ? C13A C18A 1.375(7) . ? C13A C14A 1.391(8) . ? C14A C15A 1.370(8) . ? C15A C16A 1.364(7) . ? C16A C17A 1.379(8) . ? C16A S1A 1.760(5) 3_756 ? C17A C18A 1.366(8) . ? S1B O11B 1.345(10) . ? S1B O12B 1.502(9) . ? S1B C16B 1.781(6) 3_657 ? S1B C1B 1.787(6) . ? S1B C1* 1.806(9) . ? S2B O22B 1.378(9) . ? S2B O21B 1.437(10) . ? S2B C10B 1.760(6) . ? S2B C13B 1.768(6) . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C3B C4B 1.3900 . ? C4B C5B 1.3900 . ? C4B C7B 1.511(8) . ? C5B C6B 1.3900 . ? C1* C2* 1.3900 . ? C1* C6* 1.3900 . ? C2* C3* 1.3900 . ? C3* C4* 1.3900 . ? C4* C5* 1.3900 . ? C4* C7B 1.496(10) . ? C5* C6* 1.3900 . ? C7B C8B 1.363(7) . ? C7B C12B 1.378(8) . ? C8B C9B 1.397(10) . ? C9B C10B 1.349(8) . ? C10B C11B 1.355(9) . ? C11B C12B 1.395(10) . ? C13B C18B 1.365(8) . ? C13B C14B 1.372(7) . ? C14B C15B 1.352(8) . ? C15B C16B 1.361(8) . ? C16B C17B 1.353(8) . ? C16B S1B 1.781(6) 3_657 ? C17B C18B 1.376(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 S1 O11 122.3(3) . . ? O12 S1 C34 109.5(3) . . ? O11 S1 C34 107.4(3) . . ? O12 S1 C1' 110.7(5) . . ? O11 S1 C1' 104.5(5) . . ? C34 S1 C1' 100.1(5) . . ? O12 S1 C1 104.5(3) . . ? O11 S1 C1 108.3(3) . . ? C34 S1 C1 103.2(3) . . ? O22 S2 O21 121.6(3) . . ? O22 S2 C10 110.4(4) . . ? O21 S2 C10 108.3(3) . . ? O22 S2 C13 107.1(3) . . ? O21 S2 C13 104.7(3) . . ? C10 S2 C13 103.1(3) . . ? O22 S2 C10' 107.0(6) . . ? O21 S2 C10' 110.6(6) . . ? C13 S2 C10' 104.6(5) . . ? O31 S3 O32 134.1(14) . . ? O31 S3 C19 112.0(9) . . ? O32 S3 C19 107.6(10) . . ? O31 S3 C16 97.7(10) . . ? O32 S3 C16 98.4(10) . . ? C19 S3 C16 98.7(3) . . ? O42 S4 O41 126.8(10) . . ? O42 S4 C28 108.5(8) . . ? O41 S4 C28 105.7(7) . . ? O42 S4 C31 108.8(8) . . ? O41 S4 C31 104.4(7) . . ? C28 S4 C31 99.1(2) . . ? C2 C1 C6 120.0 . . ? C2 C1 S1 122.8(4) . . ? C6 C1 S1 116.8(4) . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C7 120.1(5) . . ? C5 C4 C7 119.6(5) . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 C4 120.3(5) . . ? C12 C7 C4 119.3(5) . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 S2 118.1(4) . . ? C11 C10 S2 121.8(4) . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? C2' C1' C6' 120.0 . . ? C2' C1' S1 117.4(8) . . ? C6' C1' S1 122.6(8) . . ? C1' C2' C3' 120.0 . . ? C4' C3' C2' 120.0 . . ? C3' C4' C5' 120.0 . . ? C3' C4' C7' 123.3(10) . . ? C5' C4' C7' 116.3(10) . . ? C6' C5' C4' 120.0 . . ? C5' C6' C1' 120.0 . . ? C8' C7' C12' 120.0 . . ? C8' C7' C4' 121.5(10) . . ? C12' C7' C4' 118.4(10) . . ? C9' C8' C7' 120.0 . . ? C8' C9' C10' 120.0 . . ? C11' C10' C9' 120.0 . . ? C11' C10' S2 113.2(9) . . ? C9' C10' S2 126.5(9) . . ? C10' C11' C12' 120.0 . . ? C11' C12' C7' 120.0 . . ? C18 C13 C14 122.8(6) . . ? C18 C13 S2 118.3(4) . . ? C14 C13 S2 118.8(5) . . ? C15 C14 C13 115.9(6) . . ? C14 C15 C16 123.6(6) . . ? C15 C16 C17 118.8(6) . . ? C15 C16 S3 120.5(5) . . ? C17 C16 S3 120.7(5) . . ? C18 C17 C16 119.3(6) . . ? C13 C18 C17 119.5(5) . . ? C24 C19 C20 119.1(5) . . ? C24 C19 S3 121.1(5) . . ? C20 C19 S3 119.7(5) . . ? C21 C20 C19 119.5(6) . . ? C20 C21 C22 123.1(6) . . ? C23 C22 C21 116.2(5) . . ? C23 C22 C25 122.2(5) . . ? C21 C22 C25 121.6(5) . . ? C22 C23 C24 122.0(6) . . ? C19 C24 C23 119.6(5) . . ? C30 C25 C26 116.2(5) . . ? C30 C25 C22 124.0(5) . . ? C26 C25 C22 119.8(5) . . ? C27 C26 C25 121.3(6) . . ? C28 C27 C26 120.7(6) . . ? C27 C28 C29 118.7(5) . . ? C27 C28 S4 120.6(5) . . ? C29 C28 S4 120.7(5) . . ? C28 C29 C30 120.0(6) . . ? C25 C30 C29 122.8(6) . . ? C32 C31 C36 119.3(5) . . ? C32 C31 S4 122.2(5) . . ? C36 C31 S4 118.5(5) . . ? C31 C32 C33 120.8(5) . . ? C32 C33 C34 120.1(5) . . ? C35 C34 C33 120.5(5) . . ? C35 C34 S1 119.3(4) . . ? C33 C34 S1 120.2(4) . . ? C34 C35 C36 118.5(5) . . ? C31 C36 C35 120.9(5) . . ? O12A S1A O11A 121.6(4) . . ? O12A S1A C16A 106.4(4) . 3_756 ? O11A S1A C16A 107.0(3) . 3_756 ? O12A S1A C1A 111.4(4) . . ? O11A S1A C1A 107.9(3) . . ? C16A S1A C1A 100.3(2) 3_756 . ? O22A S2A O21A 123.6(4) . . ? O22A S2A C10A 110.7(4) . . ? O21A S2A C10A 106.0(3) . . ? O22A S2A C13A 108.0(4) . . ? O21A S2A C13A 105.2(3) . . ? C10A S2A C13A 100.7(2) . . ? C6A C1A C2A 118.8(5) . . ? C6A C1A S1A 120.4(4) . . ? C2A C1A S1A 120.8(4) . . ? C1A C2A C3A 120.6(5) . . ? C4A C3A C2A 120.9(5) . . ? C3A C4A C5A 117.1(5) . . ? C3A C4A C7A 121.1(5) . . ? C5A C4A C7A 121.8(5) . . ? C6A C5A C4A 121.9(5) . . ? C1A C6A C5A 120.4(6) . . ? C12A C7A C8A 116.5(4) . . ? C12A C7A C4A 121.5(5) . . ? C8A C7A C4A 122.0(4) . . ? C9A C8A C7A 122.1(5) . . ? C10A C9A C8A 119.1(5) . . ? C11A C10A C9A 120.1(5) . . ? C11A C10A S2A 119.5(4) . . ? C9A C10A S2A 120.4(4) . . ? C10A C11A C12A 120.1(5) . . ? C11A C12A C7A 122.1(5) . . ? C18A C13A C14A 118.9(5) . . ? C18A C13A S2A 119.6(4) . . ? C14A C13A S2A 121.4(4) . . ? C15A C14A C13A 119.2(5) . . ? C16A C15A C14A 121.5(6) . . ? C15A C16A C17A 119.6(5) . . ? C15A C16A S1A 119.4(4) . 3_756 ? C17A C16A S1A 120.9(4) . 3_756 ? C18A C17A C16A 119.4(5) . . ? C17A C18A C13A 121.4(5) . . ? O11B S1B O12B 123.4(6) . . ? O11B S1B C16B 104.7(4) . 3_657 ? O12B S1B C16B 102.6(4) . 3_657 ? O11B S1B C1B 116.8(6) . . ? O12B S1B C1B 104.3(5) . . ? C16B S1B C1B 102.1(3) 3_657 . ? O11B S1B C1* 106.6(6) . . ? O12B S1B C1* 115.6(6) . . ? C16B S1B C1* 100.7(5) 3_657 . ? O22B S2B O21B 126.8(7) . . ? O22B S2B C10B 110.4(5) . . ? O21B S2B C10B 106.5(5) . . ? O22B S2B C13B 106.1(4) . . ? O21B S2B C13B 102.8(5) . . ? C10B S2B C13B 101.1(3) . . ? C2B C1B C6B 120.0 . . ? C2B C1B S1B 124.6(5) . . ? C6B C1B S1B 115.1(5) . . ? C3B C2B C1B 120.0 . . ? C4B C3B C2B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B C7B 119.4(5) . . ? C3B C4B C7B 120.2(5) . . ? C4B C5B C6B 120.0 . . ? C5B C6B C1B 120.0 . . ? C2* C1* C6* 120.0 . . ? C2* C1* S1B 112.7(7) . . ? C6* C1* S1B 126.9(7) . . ? C3* C2* C1* 120.0 . . ? C2* C3* C4* 120.0 . . ? C3* C4* C5* 120.0 . . ? C3* C4* C7B 118.9(8) . . ? C5* C4* C7B 120.9(8) . . ? C6* C5* C4* 120.0 . . ? C5* C6* C1* 120.0 . . ? C8B C7B C12B 116.7(6) . . ? C8B C7B C4* 126.4(7) . . ? C12B C7B C4* 116.8(7) . . ? C8B C7B C4B 118.7(5) . . ? C12B C7B C4B 124.6(6) . . ? C7B C8B C9B 121.3(6) . . ? C10B C9B C8B 121.9(6) . . ? C9B C10B C11B 117.3(6) . . ? C9B C10B S2B 121.0(5) . . ? C11B C10B S2B 121.7(5) . . ? C10B C11B C12B 121.6(6) . . ? C7B C12B C11B 121.1(6) . . ? C18B C13B C14B 118.0(6) . . ? C18B C13B S2B 121.3(5) . . ? C14B C13B S2B 120.7(4) . . ? C15B C14B C13B 121.0(5) . . ? C14B C15B C16B 120.3(6) . . ? C17B C16B C15B 119.6(6) . . ? C17B C16B S1B 119.5(5) . 3_657 ? C15B C16B S1B 120.8(5) . 3_657 ? C16B C17B C18B 119.7(5) . . ? C13B C18B C17B 120.8(6) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 61.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.303 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.050 # 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 -0.026 0.325 -0.011 176 44 ' ' 2 0.026 0.675 0.011 176 42 ' ' 3 0.000 0.500 0.500 198 51 ' ' 4 0.000 0.000 0.500 132 41 ' ' 5 0.474 0.175 0.489 176 44 ' ' 6 0.500 1.000 0.000 198 51 ' ' 7 0.500 0.500 1.000 132 41 ' ' 8 0.526 0.825 0.511 176 42 ' ' _platon_squeeze_details ; SQUEEZE suggests 357e/cell, which is 89.3e/asu. Solvent was said to be dcm (CH2Cl2), which has 42e. asu contains 2 macrocycles, so 89e/asu = 44.5e/macrocycle. This is close to 1 dcm/macrocycle so this was considered to be the solvent present. asu thus 2dcm low = C2 H4 Cl4, so UNIT C8 H16 Cl16 low, i.e. C288 H192 O32 S32 ; #===END data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 737302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H28 O4 S4, C H2 Cl2' _chemical_formula_sum 'C40 H30 Cl2 O4 S4' _chemical_formula_weight 773.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0673(10) _cell_length_b 17.1131(16) _cell_length_c 21.5403(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.428(7) _cell_angle_gamma 90.00 _cell_volume 3687.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 4.14 _cell_measurement_theta_max 21.11 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.034 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4897 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Bruker XPREP, version 5.1/NT Lamina [0 0 1] absorption correction using psi-scans ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6688 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5229 _reflns_number_gt 3419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5229 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.61330(12) 0.19962(8) 0.13779(6) 0.0637(3) Uani 1 1 d . . . O1 O 0.7347(4) 0.2142(3) 0.1105(2) 0.0841(11) Uani 1 1 d . . . O2 O 0.5456(4) 0.1258(2) 0.12709(19) 0.0758(10) Uani 1 1 d . . . C2 C 0.4980(4) 0.2750(3) 0.1151(2) 0.0543(10) Uani 1 1 d . . . C3 C 0.3613(5) 0.2601(3) 0.1168(2) 0.0574(10) Uani 1 1 d . . . H3A H 0.3314 0.2106 0.1266 0.069 Uiso 1 1 calc R . . C4 C 0.2731(4) 0.3206(3) 0.1036(2) 0.0524(10) Uani 1 1 d . . . C5 C 0.1218(4) 0.3200(3) 0.1062(2) 0.0596(11) Uani 1 1 d . . . C6 C 0.0898(4) 0.4053(3) 0.0938(2) 0.0542(10) Uani 1 1 d . . . C7 C -0.0309(4) 0.4431(3) 0.0968(2) 0.0564(10) Uani 1 1 d . . . H7A H -0.1067 0.4158 0.1052 0.068 Uiso 1 1 calc R . . C8 C -0.0347(5) 0.5223(3) 0.0868(2) 0.0595(11) Uani 1 1 d . . . C9 C 0.0761(5) 0.5643(3) 0.0720(2) 0.0609(11) Uani 1 1 d . . . H9A H 0.0691 0.6178 0.0644 0.073 Uiso 1 1 calc R . . C10 C 0.1960(5) 0.5266(3) 0.0684(2) 0.0570(10) Uani 1 1 d . . . H10A H 0.2704 0.5539 0.0583 0.068 Uiso 1 1 calc R . . C11 C 0.2034(4) 0.4472(3) 0.08036(19) 0.0515(9) Uani 1 1 d . . . C12 C 0.3188(4) 0.3937(3) 0.08734(19) 0.0519(10) Uani 1 1 d . . . C13 C 0.4531(4) 0.4069(3) 0.0824(2) 0.0568(10) Uani 1 1 d . . . H13A H 0.4822 0.4551 0.0692 0.068 Uiso 1 1 calc R . . C14 C 0.5426(5) 0.3470(3) 0.0975(2) 0.0600(11) Uani 1 1 d . . . H14A H 0.6334 0.3552 0.0958 0.072 Uiso 1 1 calc R . . S15 S -0.18279(12) 0.57357(8) 0.09927(6) 0.0674(3) Uani 1 1 d . . . O3 O -0.2974(3) 0.5308(3) 0.07169(18) 0.0841(11) Uani 1 1 d . . . O4 O -0.1649(5) 0.6532(3) 0.0826(2) 0.0915(13) Uani 1 1 d . . . C16 C -0.1836(5) 0.5682(3) 0.1814(2) 0.0613(11) Uani 1 1 d . . . C17 C -0.2923(6) 0.5411(5) 0.2066(3) 0.092(2) Uani 1 1 d . . . H17A H -0.3679 0.5255 0.1809 0.111 Uiso 1 1 calc R . . C18 C -0.2899(6) 0.5368(5) 0.2713(3) 0.093(2) Uani 1 1 d . . . H18A H -0.3646 0.5185 0.2886 0.112 Uiso 1 1 calc R . . C19 C -0.1805(5) 0.5589(3) 0.3092(2) 0.0619(11) Uani 1 1 d . . . C20 C -0.0696(6) 0.5856(4) 0.2840(3) 0.0821(16) Uani 1 1 d . . . H20A H 0.0066 0.6000 0.3100 0.099 Uiso 1 1 calc R . . C21 C -0.0721(6) 0.5912(4) 0.2199(3) 0.0791(15) Uani 1 1 d . . . H21A H 0.0020 0.6105 0.2027 0.095 Uiso 1 1 calc R . . S22 S -0.18244(12) 0.55352(8) 0.39226(6) 0.0643(3) Uani 1 1 d . . . C23 C -0.0260(5) 0.5058(3) 0.4131(2) 0.0566(10) Uani 1 1 d . . . C24 C 0.0888(5) 0.5477(3) 0.4333(2) 0.0601(11) Uani 1 1 d . . . H24A H 0.0844 0.6015 0.4386 0.072 Uiso 1 1 calc R . . C25 C 0.2099(5) 0.5092(3) 0.4457(2) 0.0628(11) Uani 1 1 d . . . H25A H 0.2867 0.5376 0.4588 0.075 Uiso 1 1 calc R . . C26 C 0.2180(4) 0.4287(3) 0.43870(19) 0.0521(9) Uani 1 1 d . . . C27 C 0.1007(5) 0.3873(3) 0.4207(3) 0.0682(13) Uani 1 1 d . . . H27A H 0.1034 0.3332 0.4176 0.082 Uiso 1 1 calc R . . C28 C -0.0202(5) 0.4262(3) 0.4075(3) 0.0665(12) Uani 1 1 d . . . H28A H -0.0975 0.3981 0.3947 0.080 Uiso 1 1 calc R . . C29 C 0.3479(5) 0.3868(3) 0.4466(2) 0.0561(10) Uani 1 1 d . . . C30 C 0.4653(5) 0.4239(3) 0.4355(2) 0.0634(12) Uani 1 1 d . . . H30A H 0.4655 0.4777 0.4295 0.076 Uiso 1 1 calc R . . C31 C 0.5813(5) 0.3822(3) 0.4332(2) 0.0644(12) Uani 1 1 d . . . H31A H 0.6590 0.4081 0.4255 0.077 Uiso 1 1 calc R . . C32 C 0.5837(5) 0.3026(3) 0.4422(2) 0.0630(11) Uani 1 1 d . . . C33 C 0.4704(6) 0.2661(3) 0.4582(2) 0.0679(13) Uani 1 1 d . . . H33A H 0.4729 0.2131 0.4677 0.081 Uiso 1 1 calc R . . C34 C 0.3546(5) 0.3070(3) 0.4604(2) 0.0667(12) Uani 1 1 d . . . H34A H 0.2791 0.2814 0.4712 0.080 Uiso 1 1 calc R . . S35 S 0.72972(13) 0.24831(9) 0.43023(6) 0.0733(4) Uani 1 1 d . . . C36 C 0.6968(5) 0.2331(3) 0.3480(2) 0.0646(12) Uani 1 1 d . . . C37 C 0.7938(5) 0.2440(4) 0.3107(3) 0.0861(17) Uani 1 1 d . . . H37A H 0.8789 0.2580 0.3285 0.103 Uiso 1 1 calc R . . C38 C 0.7707(6) 0.2348(4) 0.2471(3) 0.0856(17) Uani 1 1 d . . . H38A H 0.8389 0.2440 0.2222 0.103 Uiso 1 1 calc R . . C39 C 0.6469(4) 0.2121(3) 0.2204(2) 0.0611(11) Uani 1 1 d . . . C40 C 0.5493(6) 0.1964(5) 0.2577(3) 0.094(2) Uani 1 1 d . . . H40A H 0.4668 0.1777 0.2402 0.113 Uiso 1 1 calc R . . C41 C 0.5730(6) 0.2083(5) 0.3220(3) 0.093(2) Uani 1 1 d . . . H41A H 0.5053 0.1995 0.3472 0.111 Uiso 1 1 calc R . . C42 C 0.0501(5) 0.2672(3) 0.0550(3) 0.0779(16) Uani 1 1 d . . . H42A H 0.0723 0.2838 0.0148 0.117 Uiso 1 1 calc R . . H42B H -0.0448 0.2709 0.0560 0.117 Uiso 1 1 calc R . . H42C H 0.0782 0.2141 0.0622 0.117 Uiso 1 1 calc R . . C43 C 0.0893(6) 0.2956(4) 0.1716(4) 0.096(2) Uani 1 1 d . . . H43A H 0.1352 0.3295 0.2025 0.144 Uiso 1 1 calc R . . H43B H 0.1178 0.2426 0.1798 0.144 Uiso 1 1 calc R . . H43C H -0.0053 0.2993 0.1735 0.144 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 S1 0.0536(6) 0.0694(7) 0.0689(7) -0.0065(6) 0.0103(5) 0.0121(6) O1 0.060(2) 0.108(3) 0.088(2) -0.004(2) 0.0237(18) 0.018(2) O2 0.080(2) 0.0595(19) 0.086(2) -0.0107(17) -0.0004(19) 0.0096(18) C2 0.045(2) 0.066(3) 0.053(2) -0.0010(19) 0.0096(17) 0.001(2) C3 0.055(2) 0.052(2) 0.065(2) 0.005(2) 0.006(2) -0.004(2) C4 0.045(2) 0.057(2) 0.055(2) 0.0070(19) 0.0067(17) -0.0062(19) C5 0.047(2) 0.052(2) 0.082(3) 0.007(2) 0.015(2) -0.0011(19) C6 0.050(2) 0.056(2) 0.057(2) 0.0039(19) 0.0060(18) -0.0007(19) C7 0.044(2) 0.062(3) 0.064(2) 0.004(2) 0.0074(18) -0.0007(19) C8 0.057(2) 0.064(3) 0.058(2) 0.000(2) 0.0051(19) 0.003(2) C9 0.061(3) 0.056(3) 0.066(3) 0.006(2) 0.007(2) 0.004(2) C10 0.054(2) 0.052(2) 0.064(2) 0.005(2) 0.006(2) -0.010(2) C11 0.052(2) 0.051(2) 0.052(2) 0.0031(18) 0.0058(17) -0.0012(19) C12 0.049(2) 0.058(2) 0.049(2) -0.0010(19) 0.0066(17) -0.0082(19) C13 0.050(2) 0.056(2) 0.064(2) 0.006(2) 0.0082(19) -0.013(2) C14 0.046(2) 0.068(3) 0.067(3) -0.006(2) 0.009(2) -0.002(2) S15 0.0604(6) 0.0765(8) 0.0655(7) 0.0077(6) 0.0073(5) 0.0171(6) O3 0.0525(18) 0.126(3) 0.072(2) -0.002(2) -0.0021(16) 0.004(2) O4 0.097(3) 0.080(3) 0.101(3) 0.027(2) 0.026(2) 0.032(2) C16 0.055(2) 0.058(3) 0.071(3) -0.002(2) 0.004(2) 0.013(2) C17 0.055(3) 0.148(6) 0.073(3) -0.001(4) 0.004(2) 0.000(3) C18 0.055(3) 0.153(7) 0.074(3) -0.002(4) 0.018(3) -0.015(4) C19 0.055(2) 0.056(2) 0.075(3) -0.005(2) 0.012(2) 0.004(2) C20 0.073(3) 0.106(4) 0.069(3) -0.005(3) 0.013(3) -0.025(3) C21 0.072(3) 0.094(4) 0.072(3) 0.000(3) 0.013(3) -0.025(3) S22 0.0592(6) 0.0680(7) 0.0674(7) -0.0019(6) 0.0153(5) 0.0067(6) C23 0.061(3) 0.054(2) 0.057(2) -0.0009(19) 0.017(2) 0.002(2) C24 0.065(3) 0.052(2) 0.064(3) -0.008(2) 0.010(2) -0.001(2) C25 0.061(3) 0.061(3) 0.066(3) -0.008(2) 0.003(2) -0.005(2) C26 0.054(2) 0.053(2) 0.049(2) 0.0025(18) 0.0066(17) -0.0054(19) C27 0.060(3) 0.049(2) 0.096(4) -0.003(2) 0.013(2) -0.002(2) C28 0.049(2) 0.059(3) 0.091(3) -0.012(2) 0.009(2) -0.011(2) C29 0.061(3) 0.059(2) 0.049(2) -0.0038(19) 0.0069(18) -0.003(2) C30 0.062(3) 0.047(2) 0.080(3) -0.004(2) 0.007(2) -0.007(2) C31 0.051(2) 0.067(3) 0.073(3) -0.001(2) -0.003(2) -0.010(2) C32 0.060(3) 0.068(3) 0.058(2) -0.001(2) -0.005(2) 0.003(2) C33 0.077(3) 0.060(3) 0.067(3) 0.016(2) 0.009(2) 0.004(2) C34 0.068(3) 0.064(3) 0.070(3) 0.014(2) 0.014(2) -0.001(2) S35 0.0622(7) 0.0821(8) 0.0714(7) -0.0015(6) -0.0102(6) 0.0178(6) C36 0.052(2) 0.067(3) 0.073(3) 0.003(2) 0.000(2) 0.012(2) C37 0.053(3) 0.120(5) 0.084(4) -0.007(4) 0.000(3) -0.012(3) C38 0.056(3) 0.117(5) 0.085(4) 0.005(4) 0.017(3) -0.006(3) C39 0.044(2) 0.064(3) 0.075(3) -0.005(2) 0.005(2) 0.011(2) C40 0.058(3) 0.151(6) 0.073(3) -0.015(4) 0.004(3) -0.021(4) C41 0.066(3) 0.140(6) 0.074(3) -0.008(4) 0.013(3) -0.021(4) C42 0.057(3) 0.052(3) 0.121(5) 0.002(3) -0.007(3) -0.007(2) C43 0.070(3) 0.105(5) 0.120(5) 0.050(4) 0.039(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O1 1.436(4) . ? S1 O2 1.442(4) . ? S1 C2 1.766(5) . ? S1 C39 1.786(5) . ? C2 C14 1.380(7) . ? C2 C3 1.404(6) . ? C3 C4 1.373(7) . ? C4 C12 1.391(6) . ? C4 C5 1.530(6) . ? C5 C6 1.511(6) . ? C5 C43 1.541(8) . ? C5 C42 1.541(8) . ? C6 C7 1.384(6) . ? C6 C11 1.409(6) . ? C7 C8 1.372(7) . ? C8 C9 1.395(7) . ? C8 S15 1.776(5) . ? C9 C10 1.379(7) . ? C10 C11 1.382(6) . ? C11 C12 1.473(6) . ? C12 C13 1.386(6) . ? C13 C14 1.380(7) . ? S15 O4 1.426(5) . ? S15 O3 1.437(4) . ? S15 C16 1.772(5) . ? C16 C17 1.357(8) . ? C16 C21 1.376(7) . ? C17 C18 1.392(9) . ? C18 C19 1.349(8) . ? C19 C20 1.372(8) . ? C19 S22 1.794(5) . ? C20 C21 1.383(8) . ? S22 C23 1.786(5) . ? C23 C28 1.370(7) . ? C23 C24 1.387(7) . ? C24 C25 1.385(7) . ? C25 C26 1.390(7) . ? C26 C27 1.394(7) . ? C26 C29 1.484(7) . ? C27 C28 1.389(7) . ? C29 C30 1.386(7) . ? C29 C34 1.397(7) . ? C30 C31 1.374(7) . ? C31 C32 1.375(8) . ? C32 C33 1.378(8) . ? C32 S35 1.782(5) . ? C33 C34 1.365(8) . ? S35 C36 1.783(5) . ? C36 C37 1.345(8) . ? C36 C41 1.376(8) . ? C37 C38 1.374(9) . ? C38 C39 1.370(7) . ? C39 C40 1.364(8) . ? C40 C41 1.394(9) . ? 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 O1 S1 O2 119.7(3) . . ? O1 S1 C2 108.8(2) . . ? O2 S1 C2 108.1(2) . . ? O1 S1 C39 108.2(2) . . ? O2 S1 C39 107.3(2) . . ? C2 S1 C39 103.5(2) . . ? C14 C2 C3 121.3(4) . . ? C14 C2 S1 120.3(3) . . ? C3 C2 S1 118.4(4) . . ? C4 C3 C2 118.1(4) . . ? C3 C4 C12 120.4(4) . . ? C3 C4 C5 127.7(4) . . ? C12 C4 C5 111.9(4) . . ? C6 C5 C4 100.5(4) . . ? C6 C5 C43 111.1(5) . . ? C4 C5 C43 110.4(4) . . ? C6 C5 C42 111.5(4) . . ? C4 C5 C42 111.5(4) . . ? C43 C5 C42 111.4(5) . . ? C7 C6 C11 120.6(4) . . ? C7 C6 C5 127.9(4) . . ? C11 C6 C5 111.5(4) . . ? C8 C7 C6 117.6(4) . . ? C7 C8 C9 122.4(5) . . ? C7 C8 S15 118.3(4) . . ? C9 C8 S15 119.1(4) . . ? C10 C9 C8 119.9(4) . . ? C9 C10 C11 118.7(4) . . ? C10 C11 C6 120.7(4) . . ? C10 C11 C12 131.0(4) . . ? C6 C11 C12 108.1(4) . . ? C13 C12 C4 121.2(4) . . ? C13 C12 C11 130.9(4) . . ? C4 C12 C11 107.8(4) . . ? C14 C13 C12 118.5(4) . . ? C2 C14 C13 120.3(4) . . ? O4 S15 O3 120.0(3) . . ? O4 S15 C16 108.4(3) . . ? O3 S15 C16 107.0(2) . . ? O4 S15 C8 107.6(3) . . ? O3 S15 C8 109.5(2) . . ? C16 S15 C8 102.9(2) . . ? C17 C16 C21 119.7(5) . . ? C17 C16 S15 120.8(4) . . ? C21 C16 S15 119.5(4) . . ? C16 C17 C18 119.6(5) . . ? C19 C18 C17 120.8(5) . . ? C18 C19 C20 120.0(5) . . ? C18 C19 S22 119.3(4) . . ? C20 C19 S22 120.7(4) . . ? C19 C20 C21 119.5(5) . . ? C16 C21 C20 120.3(5) . . ? C23 S22 C19 99.6(2) . . ? C28 C23 C24 119.9(5) . . ? C28 C23 S22 118.5(4) . . ? C24 C23 S22 121.6(4) . . ? C25 C24 C23 120.0(4) . . ? C24 C25 C26 120.8(5) . . ? C25 C26 C27 118.4(5) . . ? C25 C26 C29 121.9(4) . . ? C27 C26 C29 119.7(4) . . ? C28 C27 C26 120.6(5) . . ? C23 C28 C27 120.3(5) . . ? C30 C29 C34 117.5(5) . . ? C30 C29 C26 121.1(4) . . ? C34 C29 C26 121.2(4) . . ? C31 C30 C29 120.9(5) . . ? C30 C31 C32 120.7(5) . . ? C31 C32 C33 118.8(5) . . ? C31 C32 S35 119.9(4) . . ? C33 C32 S35 121.2(4) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C29 121.0(5) . . ? C32 S35 C36 98.9(2) . . ? C37 C36 C41 119.0(5) . . ? C37 C36 S35 120.4(4) . . ? C41 C36 S35 120.6(4) . . ? C36 C37 C38 121.8(5) . . ? C39 C38 C37 119.7(5) . . ? C40 C39 C38 119.4(5) . . ? C40 C39 S1 119.7(4) . . ? C38 C39 S1 120.9(4) . . ? C39 C40 C41 120.2(5) . . ? C36 C41 C40 119.8(6) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.251 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.052 # 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 -0.233 0.087 0.766 150 38 ' ' 2 -0.233 0.413 0.266 150 38 ' ' 3 0.233 0.587 0.734 150 38 ' ' 4 0.233 0.913 0.234 150 38 ' ' _platon_squeeze_details ; SQUEEZE suggests 151e/cell. Before SQUEEZE, solvent looked like dcm and was full occupancy in the middle of the macrocycle. dcm = CH2Cl2 = 42e. 151e/cell = 37.8e/cell. This is close enough for the solvent to be considered as 1 dcm per macrocycle. asu thus C H2 Cl2 low, so UNIT C4 H8 Cl8 low, i.e. C156 H112 O16 S16 Cl0 ; #===END