# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 O6' _chemical_formula_sum 'C33 H30 O6' _chemical_formula_weight 522.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.6106(2) _cell_length_b 12.5495(2) _cell_length_c 18.7424(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2730.90(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 4.24 _cell_measurement_theta_max 71.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9017 _exptl_absorpt_correction_T_max 0.9523 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Incoatec micro-focus' _diffrn_source_monochromator 'MONTEL Multi-layer' _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method 'combination of \w and \f-scans ' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 28929 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 71.40 _reflns_number_total 5161 _reflns_number_gt 5060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2013-2.0' _computing_cell_refinement 'Bruker SAINT v8.27B' _computing_data_reduction 'Bruker SAINT v8.27B' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0878P)^2^+1.5716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2427 Friedel pairs' _refine_ls_abs_structure_Flack 0.2(2) _refine_ls_number_reflns 5161 _refine_ls_number_parameters 356 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 O1 O 0.46348(19) 0.11955(15) 0.93083(11) 0.0426(5) Uani 1 1 d . . . O2 O 0.3345(2) 0.13016(18) 1.02033(12) 0.0507(6) Uani 1 1 d . . . O3 O 0.5474(2) 0.26970(19) 1.05363(13) 0.0570(6) Uani 1 1 d . . . O4 O 0.4440(3) 0.3886(2) 1.11462(12) 0.0630(7) Uani 1 1 d . . . O5 O 0.21818(16) 0.63498(14) 0.88391(12) 0.0384(4) Uani 1 1 d . . . O6 O 0.40423(19) 0.65881(15) 0.85538(14) 0.0494(5) Uani 1 1 d . . . C1 C 0.3711(2) 0.28180(19) 0.94633(12) 0.0278(5) Uani 1 1 d . . . C2 C 0.4137(2) 0.3655(2) 0.98898(13) 0.0329(5) Uani 1 1 d . . . C3 C 0.3992(2) 0.4717(2) 0.96732(13) 0.0302(5) Uani 1 1 d . . . C4 C 0.34174(19) 0.49065(19) 0.90339(13) 0.0273(5) Uani 1 1 d . . . C5 C 0.29850(19) 0.40840(18) 0.86047(12) 0.0238(4) Uani 1 1 d . . . C6 C 0.31275(19) 0.30213(18) 0.88253(12) 0.0256(4) Uani 1 1 d . . . C7 C 0.3863(2) 0.1689(2) 0.97092(14) 0.0348(5) Uani 1 1 d . . . C8 C 0.4870(3) 0.0087(2) 0.9478(2) 0.0516(8) Uani 1 1 d . . . H8A H 0.4792 -0.0028 0.9998 0.062 Uiso 1 1 calc R . . H8B H 0.5670 -0.0093 0.9339 0.062 Uiso 1 1 calc R . . C9 C 0.4060(4) -0.0607(3) 0.9094(3) 0.0706(11) Uani 1 1 d . . . H9A H 0.4249 -0.1354 0.9190 0.106 Uiso 1 1 calc R . . H9B H 0.4117 -0.0470 0.8580 0.106 Uiso 1 1 calc R . . H9C H 0.3273 -0.0458 0.9255 0.106 Uiso 1 1 calc R . . C10 C 0.4689(3) 0.3441(2) 1.05974(16) 0.0420(6) Uani 1 1 d . . . C11 C 0.6014(6) 0.2326(4) 1.1197(3) 0.103(2) Uani 1 1 d . . . H11A H 0.6616 0.2838 1.1348 0.123 Uiso 1 1 calc R . . H11B H 0.5430 0.2281 1.1580 0.123 Uiso 1 1 calc R . . C12 C 0.6516(5) 0.1306(5) 1.1082(4) 0.104(2) Uani 1 1 d . . . H12A H 0.7069 0.1153 1.1463 0.156 Uiso 1 1 calc R . . H12B H 0.6913 0.1299 1.0621 0.156 Uiso 1 1 calc R . . H12C H 0.5910 0.0761 1.1083 0.156 Uiso 1 1 calc R . . C13 C 0.4475(3) 0.5634(2) 1.00858(15) 0.0378(6) Uani 1 1 d . . . C14 C 0.5664(3) 0.5760(3) 1.01212(18) 0.0501(7) Uani 1 1 d . . . H14 H 0.6160 0.5255 0.9902 0.060 Uiso 1 1 calc R . . C15 C 0.6121(3) 0.6637(3) 1.0483(2) 0.0620(10) Uani 1 1 d . . . H15 H 0.6932 0.6739 1.0500 0.074 Uiso 1 1 calc R . . C16 C 0.5397(3) 0.7360(3) 1.0818(2) 0.0618(10) Uani 1 1 d . . . H16 H 0.5711 0.7957 1.1062 0.074 Uiso 1 1 calc R . . C17 C 0.4229(4) 0.7213(3) 1.0795(2) 0.0668(10) Uani 1 1 d . . . H17 H 0.3735 0.7699 1.1035 0.080 Uiso 1 1 calc R . . C18 C 0.3764(3) 0.6358(3) 1.04251(19) 0.0533(8) Uani 1 1 d . . . H18 H 0.2952 0.6270 1.0404 0.064 Uiso 1 1 calc R . . C19 C 0.3274(2) 0.60496(18) 0.87800(14) 0.0318(5) Uani 1 1 d . . . C20 C 0.1867(3) 0.7396(2) 0.8551(2) 0.0518(8) Uani 1 1 d . . . H20A H 0.2551 0.7867 0.8554 0.062 Uiso 1 1 calc R . . H20B H 0.1270 0.7723 0.8858 0.062 Uiso 1 1 calc R . . C21 C 0.1423(5) 0.7300(3) 0.7813(2) 0.0775(13) Uani 1 1 d . . . H21A H 0.1037 0.7964 0.7677 0.116 Uiso 1 1 calc R . . H21B H 0.0874 0.6709 0.7787 0.116 Uiso 1 1 calc R . . H21C H 0.2066 0.7165 0.7486 0.116 Uiso 1 1 calc R . . C22 C 0.2425(2) 0.43465(16) 0.79122(12) 0.0244(4) Uani 1 1 d . . . C23 C 0.3070(2) 0.4793(2) 0.73610(15) 0.0338(5) Uani 1 1 d . . . H23 H 0.3868 0.4927 0.7429 0.041 Uiso 1 1 calc R . . C24 C 0.2558(3) 0.5042(2) 0.67156(15) 0.0420(6) Uani 1 1 d . . . H24 H 0.3009 0.5328 0.6339 0.050 Uiso 1 1 calc R . . C25 C 0.1394(3) 0.4877(3) 0.66182(16) 0.0465(7) Uani 1 1 d . . . H25 H 0.1038 0.5070 0.6181 0.056 Uiso 1 1 calc R . . C26 C 0.0749(3) 0.4429(2) 0.71592(16) 0.0415(6) Uani 1 1 d . . . H26 H -0.0050 0.4306 0.7090 0.050 Uiso 1 1 calc R . . C27 C 0.1256(2) 0.41583(19) 0.78019(13) 0.0296(5) Uani 1 1 d . . . H27 H 0.0806 0.3843 0.8169 0.036 Uiso 1 1 calc R . . C28 C 0.2644(2) 0.21334(17) 0.83879(13) 0.0274(5) Uani 1 1 d . . . C29 C 0.3022(2) 0.19544(19) 0.76971(14) 0.0325(5) Uani 1 1 d . . . H29 H 0.3621 0.2381 0.7504 0.039 Uiso 1 1 calc R . . C30 C 0.2528(3) 0.1154(2) 0.72858(16) 0.0386(6) Uani 1 1 d . . . H30 H 0.2794 0.1037 0.6813 0.046 Uiso 1 1 calc R . . C31 C 0.1649(2) 0.0523(2) 0.75596(17) 0.0409(6) Uani 1 1 d . . . H31 H 0.1306 -0.0018 0.7276 0.049 Uiso 1 1 calc R . . C32 C 0.1280(3) 0.0696(2) 0.82537(17) 0.0401(6) Uani 1 1 d . . . H32 H 0.0694 0.0258 0.8451 0.048 Uiso 1 1 calc R . . C33 C 0.1758(2) 0.1500(2) 0.86608(15) 0.0348(5) Uani 1 1 d . . . H33 H 0.1483 0.1623 0.9131 0.042 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 O1 0.0537(12) 0.0364(10) 0.0377(10) 0.0065(8) 0.0110(9) 0.0139(8) O2 0.0648(13) 0.0469(11) 0.0403(11) 0.0200(9) 0.0209(10) 0.0191(10) O3 0.0722(15) 0.0532(13) 0.0455(13) 0.0035(10) -0.0150(12) 0.0099(11) O4 0.105(2) 0.0563(14) 0.0280(11) -0.0080(9) -0.0112(12) 0.0144(13) O5 0.0365(9) 0.0277(8) 0.0509(11) -0.0049(8) -0.0029(8) -0.0004(7) O6 0.0447(10) 0.0294(9) 0.0740(15) 0.0042(10) 0.0044(11) -0.0078(8) C1 0.0309(11) 0.0314(12) 0.0211(11) 0.0045(9) 0.0057(9) 0.0038(9) C2 0.0281(11) 0.0457(14) 0.0249(12) -0.0021(10) 0.0000(9) -0.0029(10) C3 0.0279(11) 0.0401(13) 0.0225(11) -0.0043(10) 0.0029(9) -0.0027(10) C4 0.0261(10) 0.0281(11) 0.0277(12) -0.0031(9) 0.0039(9) -0.0028(8) C5 0.0250(10) 0.0252(10) 0.0211(10) -0.0003(8) 0.0015(8) -0.0007(8) C6 0.0280(10) 0.0274(11) 0.0216(11) -0.0018(9) 0.0014(9) 0.0020(8) C7 0.0421(13) 0.0343(13) 0.0282(12) 0.0071(10) 0.0050(11) 0.0083(11) C8 0.0650(19) 0.0350(14) 0.0547(19) 0.0037(13) 0.0104(16) 0.0131(14) C9 0.062(2) 0.0440(17) 0.105(3) -0.0035(19) 0.000(2) -0.0004(15) C10 0.0506(16) 0.0398(14) 0.0354(15) 0.0056(12) -0.0038(13) -0.0022(12) C11 0.158(5) 0.067(3) 0.083(3) 0.006(2) -0.074(4) 0.030(3) C12 0.074(3) 0.123(5) 0.116(5) 0.058(4) -0.014(3) 0.016(3) C13 0.0443(14) 0.0374(13) 0.0318(13) 0.0013(10) -0.0075(11) -0.0074(11) C14 0.0434(16) 0.0592(19) 0.0477(17) -0.0056(14) -0.0103(14) -0.0055(14) C15 0.056(2) 0.060(2) 0.070(2) -0.0109(18) -0.0230(19) -0.0126(16) C16 0.071(2) 0.0454(18) 0.069(2) -0.0126(16) -0.0248(19) -0.0100(16) C17 0.077(2) 0.054(2) 0.069(2) -0.0252(18) -0.015(2) 0.0058(18) C18 0.0515(18) 0.0556(19) 0.0529(19) -0.0178(15) -0.0080(15) -0.0034(14) C19 0.0354(12) 0.0231(11) 0.0368(14) -0.0057(10) -0.0003(10) -0.0045(9) C20 0.0561(17) 0.0251(12) 0.074(2) -0.0067(14) -0.0074(17) 0.0029(12) C21 0.131(4) 0.0465(19) 0.055(2) 0.0119(16) 0.003(2) 0.031(2) C22 0.0322(11) 0.0182(9) 0.0228(10) -0.0011(8) 0.0005(9) -0.0007(8) C23 0.0375(12) 0.0308(12) 0.0330(13) 0.0025(10) 0.0051(11) -0.0048(10) C24 0.0559(16) 0.0422(14) 0.0279(13) 0.0079(11) 0.0077(13) -0.0081(12) C25 0.0602(18) 0.0479(16) 0.0315(14) 0.0104(12) -0.0129(13) -0.0047(14) C26 0.0404(14) 0.0442(15) 0.0401(15) 0.0060(12) -0.0124(12) -0.0039(12) C27 0.0314(12) 0.0295(11) 0.0278(12) 0.0026(9) 0.0015(10) -0.0032(9) C28 0.0343(11) 0.0198(10) 0.0280(12) 0.0004(8) 0.0009(9) 0.0023(9) C29 0.0422(13) 0.0277(11) 0.0275(12) -0.0039(9) 0.0061(10) -0.0018(10) C30 0.0493(15) 0.0341(13) 0.0324(13) -0.0055(10) 0.0036(12) 0.0006(11) C31 0.0446(14) 0.0342(13) 0.0439(16) -0.0086(11) -0.0019(12) -0.0056(11) C32 0.0389(14) 0.0355(13) 0.0460(16) -0.0009(11) 0.0056(12) -0.0082(11) C33 0.0374(12) 0.0326(12) 0.0343(13) -0.0023(10) 0.0067(11) -0.0018(10) _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 O1 C7 1.323(3) . ? O1 C8 1.453(3) . ? O2 C7 1.206(3) . ? O3 C10 1.310(4) . ? O3 C11 1.464(5) . ? O4 C10 1.205(4) . ? O5 C19 1.327(3) . ? O5 C20 1.465(4) . ? O6 C19 1.197(3) . ? C1 C6 1.398(3) . ? C1 C2 1.410(4) . ? C1 C7 1.501(3) . ? C2 C3 1.404(4) . ? C2 C10 1.497(4) . ? C3 C4 1.392(4) . ? C3 C13 1.495(4) . ? C4 C5 1.402(3) . ? C4 C19 1.521(3) . ? C5 C6 1.406(3) . ? C5 C22 1.488(3) . ? C6 C28 1.493(3) . ? C8 C9 1.469(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.423(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.383(5) . ? C13 C14 1.391(4) . ? C14 C15 1.399(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(6) . ? C15 H15 0.9500 . ? C16 C17 1.369(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C20 C21 1.481(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.393(3) . ? C22 C27 1.394(3) . ? C23 C24 1.384(4) . ? C23 H23 0.9500 . ? C24 C25 1.379(5) . ? C24 H24 0.9500 . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 C33 1.396(4) . ? C29 C30 1.390(4) . ? C29 H29 0.9500 . ? C30 C31 1.390(4) . ? C30 H30 0.9500 . ? C31 C32 1.386(4) . ? C31 H31 0.9500 . ? C32 C33 1.381(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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 C7 O1 C8 116.8(2) . . ? C10 O3 C11 116.8(3) . . ? C19 O5 C20 117.5(2) . . ? C6 C1 C2 121.3(2) . . ? C6 C1 C7 119.5(2) . . ? C2 C1 C7 119.2(2) . . ? C3 C2 C1 120.1(2) . . ? C3 C2 C10 118.5(2) . . ? C1 C2 C10 121.3(2) . . ? C4 C3 C2 117.9(2) . . ? C4 C3 C13 119.6(2) . . ? C2 C3 C13 122.4(2) . . ? C3 C4 C5 122.7(2) . . ? C3 C4 C19 118.9(2) . . ? C5 C4 C19 118.4(2) . . ? C4 C5 C6 119.2(2) . . ? C4 C5 C22 119.6(2) . . ? C6 C5 C22 121.2(2) . . ? C1 C6 C5 118.8(2) . . ? C1 C6 C28 121.0(2) . . ? C5 C6 C28 120.1(2) . . ? O2 C7 O1 125.8(2) . . ? O2 C7 C1 123.9(2) . . ? O1 C7 C1 110.3(2) . . ? O1 C8 C9 109.8(3) . . ? O1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 O3 124.8(3) . . ? O4 C10 C2 124.8(3) . . ? O3 C10 C2 110.4(3) . . ? C12 C11 O3 109.5(5) . . ? C12 C11 H11A 109.8 . . ? O3 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? O3 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.7(3) . . ? C18 C13 C3 121.4(3) . . ? C14 C13 C3 118.9(3) . . ? C13 C14 C15 119.3(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.4(3) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? O6 C19 O5 125.6(2) . . ? O6 C19 C4 124.2(2) . . ? O5 C19 C4 110.3(2) . . ? O5 C20 C21 111.0(3) . . ? O5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? O5 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 118.8(2) . . ? C23 C22 C5 120.1(2) . . ? C27 C22 C5 121.1(2) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.1(2) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C29 C28 C33 118.9(2) . . ? C29 C28 C6 121.0(2) . . ? C33 C28 C6 120.0(2) . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C30 118.9(3) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C28 120.6(3) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? 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 -0.8(4) . . . . ? C7 C1 C2 C3 -179.3(2) . . . . ? C6 C1 C2 C10 175.7(2) . . . . ? C7 C1 C2 C10 -2.8(4) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C10 C2 C3 C4 -176.3(2) . . . . ? C1 C2 C3 C13 -177.0(2) . . . . ? C10 C2 C3 C13 6.4(4) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C13 C3 C4 C5 177.3(2) . . . . ? C2 C3 C4 C19 -178.7(2) . . . . ? C13 C3 C4 C19 -1.2(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C19 C4 C5 C6 178.9(2) . . . . ? C3 C4 C5 C22 -177.3(2) . . . . ? C19 C4 C5 C22 1.3(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? C7 C1 C6 C5 179.6(2) . . . . ? C2 C1 C6 C28 -177.9(2) . . . . ? C7 C1 C6 C28 0.6(3) . . . . ? C4 C5 C6 C1 -0.8(3) . . . . ? C22 C5 C6 C1 176.8(2) . . . . ? C4 C5 C6 C28 178.2(2) . . . . ? C22 C5 C6 C28 -4.2(3) . . . . ? C8 O1 C7 O2 0.5(5) . . . . ? C8 O1 C7 C1 -179.5(3) . . . . ? C6 C1 C7 O2 -107.3(3) . . . . ? C2 C1 C7 O2 71.3(4) . . . . ? C6 C1 C7 O1 72.7(3) . . . . ? C2 C1 C7 O1 -108.8(3) . . . . ? C7 O1 C8 C9 87.8(4) . . . . ? C11 O3 C10 O4 5.2(6) . . . . ? C11 O3 C10 C2 -174.3(4) . . . . ? C3 C2 C10 O4 46.8(4) . . . . ? C1 C2 C10 O4 -129.7(3) . . . . ? C3 C2 C10 O3 -133.7(3) . . . . ? C1 C2 C10 O3 49.8(3) . . . . ? C10 O3 C11 C12 159.7(5) . . . . ? C4 C3 C13 C18 69.5(4) . . . . ? C2 C3 C13 C18 -113.2(3) . . . . ? C4 C3 C13 C14 -109.9(3) . . . . ? C2 C3 C13 C14 67.4(4) . . . . ? C18 C13 C14 C15 -1.9(5) . . . . ? C3 C13 C14 C15 177.6(3) . . . . ? C13 C14 C15 C16 1.5(6) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? C15 C16 C17 C18 -1.6(7) . . . . ? C14 C13 C18 C17 0.5(5) . . . . ? C3 C13 C18 C17 -178.9(3) . . . . ? C16 C17 C18 C13 1.3(6) . . . . ? C20 O5 C19 O6 5.3(4) . . . . ? C20 O5 C19 C4 -174.0(2) . . . . ? C3 C4 C19 O6 71.7(4) . . . . ? C5 C4 C19 O6 -107.0(3) . . . . ? C3 C4 C19 O5 -109.0(2) . . . . ? C5 C4 C19 O5 72.4(3) . . . . ? C19 O5 C20 C21 94.5(4) . . . . ? C4 C5 C22 C23 65.6(3) . . . . ? C6 C5 C22 C23 -112.0(3) . . . . ? C4 C5 C22 C27 -114.1(2) . . . . ? C6 C5 C22 C27 68.3(3) . . . . ? C27 C22 C23 C24 -0.1(4) . . . . ? C5 C22 C23 C24 -179.8(2) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C23 C24 C25 C26 -2.1(5) . . . . ? C24 C25 C26 C27 0.9(5) . . . . ? C25 C26 C27 C22 0.7(4) . . . . ? C23 C22 C27 C26 -1.1(3) . . . . ? C5 C22 C27 C26 178.6(2) . . . . ? C1 C6 C28 C29 -118.5(3) . . . . ? C5 C6 C28 C29 62.5(3) . . . . ? C1 C6 C28 C33 64.5(3) . . . . ? C5 C6 C28 C33 -114.4(3) . . . . ? C33 C28 C29 C30 -0.2(4) . . . . ? C6 C28 C29 C30 -177.2(2) . . . . ? C28 C29 C30 C31 0.1(4) . . . . ? C29 C30 C31 C32 -0.8(4) . . . . ? C30 C31 C32 C33 1.6(5) . . . . ? C31 C32 C33 C28 -1.8(4) . . . . ? C29 C28 C33 C32 1.1(4) . . . . ? C6 C28 C33 C32 178.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 71.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.496 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.050 _iucr_refine_instructions_details ; TITL 2F in Pna2(1) CELL 1.54178 11.6106 12.5495 18.7424 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H O UNIT 132 120 24 TEMP -123 SIZE 0.15 0.10 0.07 acta REM Colorless block, ND DUO, ApexII rem 5-s low angle, 10-s high angle L.S. 5 conf twin mpla 6 c13 c14 c15 c16 c17 c18 mpla 6 c1 c2 c3 c4 c5 c6 mpla 6 c22 c23 c24 c25 c26 c27 mpla 6 c28 c29 c30 c31 c32 c33 mpla 6 c1 c2 c3 c4 c5 c6 mpla 4 c7 o1 o2 c8 mpla 4 c10 o3 o4 c11 mpla 6 c1 c2 c3 c4 c5 c6 mpla 4 c19 o5 o6 c20 FMAP 2 PLAN 5 WGHT 0.087800 1.571600 BASF 0.16353 FVAR 0.13197 O1 3 0.463477 0.119547 0.930828 11.00000 0.05372 0.03637 = 0.03768 0.00649 0.01101 0.01394 O2 3 0.334503 0.130160 1.020331 11.00000 0.06480 0.04691 = 0.04032 0.01999 0.02085 0.01908 O3 3 0.547369 0.269696 1.053633 11.00000 0.07223 0.05318 = 0.04555 0.00350 -0.01505 0.00987 O4 3 0.444028 0.388595 1.114623 11.00000 0.10478 0.05629 = 0.02797 -0.00804 -0.01123 0.01443 O5 3 0.218176 0.634980 0.883910 11.00000 0.03645 0.02772 = 0.05091 -0.00491 -0.00295 -0.00041 O6 3 0.404231 0.658810 0.855381 11.00000 0.04466 0.02945 = 0.07396 0.00424 0.00444 -0.00781 C1 1 0.371060 0.281796 0.946327 11.00000 0.03095 0.03142 = 0.02111 0.00450 0.00572 0.00376 C2 1 0.413682 0.365490 0.988980 11.00000 0.02812 0.04567 = 0.02485 -0.00214 -0.00001 -0.00291 C3 1 0.399249 0.471717 0.967316 11.00000 0.02791 0.04011 = 0.02254 -0.00435 0.00285 -0.00275 C4 1 0.341735 0.490646 0.903393 11.00000 0.02608 0.02813 = 0.02771 -0.00307 0.00392 -0.00282 C5 1 0.298500 0.408401 0.860470 11.00000 0.02504 0.02516 = 0.02105 -0.00035 0.00147 -0.00070 C6 1 0.312745 0.302134 0.882533 11.00000 0.02798 0.02737 = 0.02156 -0.00182 0.00144 0.00202 C7 1 0.386283 0.168873 0.970920 11.00000 0.04206 0.03432 = 0.02816 0.00713 0.00497 0.00835 C8 1 0.487022 0.008654 0.947768 11.00000 0.06502 0.03503 = 0.05467 0.00372 0.01036 0.01310 AFIX 23 H8A 2 0.479160 -0.002812 0.999801 11.00000 -1.20000 H8B 2 0.566971 -0.009311 0.933893 11.00000 -1.20000 AFIX 0 C9 1 0.405988 -0.060651 0.909399 11.00000 0.06224 0.04401 = 0.10544 -0.00351 0.00003 -0.00037 AFIX 137 H9A 2 0.424865 -0.135396 0.919019 11.00000 -1.50000 H9B 2 0.411729 -0.046956 0.858045 11.00000 -1.50000 H9C 2 0.327321 -0.045827 0.925543 11.00000 -1.50000 AFIX 0 C10 1 0.468885 0.344119 1.059736 11.00000 0.05065 0.03985 = 0.03536 0.00556 -0.00378 -0.00224 C11 1 0.601432 0.232599 1.119687 11.00000 0.15786 0.06698 = 0.08295 0.00558 -0.07366 0.03023 AFIX 23 H11A 2 0.661574 0.283756 1.134811 11.00000 -1.20000 H11B 2 0.542994 0.228057 1.158032 11.00000 -1.20000 AFIX 0 C12 1 0.651571 0.130551 1.108203 11.00000 0.07367 0.12309 = 0.11610 0.05796 -0.01379 0.01648 AFIX 137 H12A 2 0.706902 0.115320 1.146349 11.00000 -1.50000 H12B 2 0.691314 0.129918 1.062076 11.00000 -1.50000 H12C 2 0.591024 0.076143 1.108276 11.00000 -1.50000 AFIX 0 C13 1 0.447455 0.563362 1.008579 11.00000 0.04430 0.03743 = 0.03179 0.00131 -0.00747 -0.00743 C14 1 0.566379 0.575964 1.012121 11.00000 0.04340 0.05922 = 0.04775 -0.00558 -0.01033 -0.00554 AFIX 43 H14 2 0.615982 0.525458 0.990182 11.00000 -1.20000 AFIX 0 C15 1 0.612144 0.663747 1.048312 11.00000 0.05585 0.05977 = 0.07049 -0.01088 -0.02296 -0.01257 AFIX 43 H15 2 0.693181 0.673899 1.049988 11.00000 -1.20000 AFIX 0 C16 1 0.539707 0.736032 1.081760 11.00000 0.07103 0.04541 = 0.06911 -0.01255 -0.02481 -0.00999 AFIX 43 H16 2 0.571072 0.795686 1.106177 11.00000 -1.20000 AFIX 0 C17 1 0.422936 0.721294 1.079541 11.00000 0.07737 0.05362 = 0.06934 -0.02518 -0.01501 0.00583 AFIX 43 H17 2 0.373499 0.769862 1.103493 11.00000 -1.20000 AFIX 0 C18 1 0.376424 0.635831 1.042508 11.00000 0.05152 0.05562 = 0.05290 -0.01777 -0.00798 -0.00338 AFIX 43 H18 2 0.295226 0.627028 1.040443 11.00000 -1.20000 AFIX 0 C19 1 0.327393 0.604964 0.877997 11.00000 0.03536 0.02308 = 0.03684 -0.00571 -0.00032 -0.00452 C20 1 0.186681 0.739560 0.855103 11.00000 0.05614 0.02513 = 0.07415 -0.00666 -0.00736 0.00289 AFIX 23 H20A 2 0.255052 0.786696 0.855426 11.00000 -1.20000 H20B 2 0.126987 0.772332 0.885780 11.00000 -1.20000 AFIX 0 C21 1 0.142327 0.730014 0.781264 11.00000 0.13051 0.04647 = 0.05545 0.01187 0.00300 0.03149 AFIX 137 H21A 2 0.103702 0.796410 0.767661 11.00000 -1.50000 H21B 2 0.087374 0.670864 0.778702 11.00000 -1.50000 H21C 2 0.206565 0.716452 0.748584 11.00000 -1.50000 AFIX 0 C22 1 0.242546 0.434648 0.791220 11.00000 0.03225 0.01824 = 0.02284 -0.00109 0.00046 -0.00068 C23 1 0.307028 0.479295 0.736101 11.00000 0.03754 0.03080 = 0.03296 0.00247 0.00513 -0.00475 AFIX 43 H23 2 0.386805 0.492721 0.742882 11.00000 -1.20000 AFIX 0 C24 1 0.255786 0.504232 0.671564 11.00000 0.05591 0.04218 = 0.02791 0.00794 0.00766 -0.00811 AFIX 43 H24 2 0.300898 0.532841 0.633864 11.00000 -1.20000 AFIX 0 C25 1 0.139415 0.487671 0.661816 11.00000 0.06024 0.04786 = 0.03146 0.01037 -0.01287 -0.00471 AFIX 43 H25 2 0.103809 0.506990 0.618052 11.00000 -1.20000 AFIX 0 C26 1 0.074931 0.442914 0.715919 11.00000 0.04036 0.04421 = 0.04006 0.00604 -0.01239 -0.00394 AFIX 43 H26 2 -0.005011 0.430589 0.708951 11.00000 -1.20000 AFIX 0 C27 1 0.125604 0.415832 0.780192 11.00000 0.03143 0.02954 = 0.02784 0.00259 0.00149 -0.00316 AFIX 43 H27 2 0.080600 0.384340 0.816898 11.00000 -1.20000 AFIX 0 C28 1 0.264377 0.213342 0.838790 11.00000 0.03432 0.01985 = 0.02801 0.00042 0.00088 0.00232 C29 1 0.302173 0.195445 0.769708 11.00000 0.04223 0.02769 = 0.02746 -0.00392 0.00612 -0.00176 AFIX 43 H29 2 0.362123 0.238088 0.750353 11.00000 -1.20000 AFIX 0 C30 1 0.252780 0.115370 0.728575 11.00000 0.04926 0.03415 = 0.03241 -0.00552 0.00363 0.00059 AFIX 43 H30 2 0.279376 0.103655 0.681287 11.00000 -1.20000 AFIX 0 C31 1 0.164870 0.052291 0.755963 11.00000 0.04462 0.03417 = 0.04391 -0.00864 -0.00192 -0.00556 AFIX 43 H31 2 0.130584 -0.001819 0.727584 11.00000 -1.20000 AFIX 0 C32 1 0.128026 0.069613 0.825365 11.00000 0.03892 0.03545 = 0.04603 -0.00087 0.00562 -0.00815 AFIX 43 H32 2 0.069373 0.025820 0.845093 11.00000 -1.20000 AFIX 0 C33 1 0.175850 0.149986 0.866075 11.00000 0.03744 0.03259 = 0.03429 -0.00230 0.00670 -0.00179 AFIX 43 H33 2 0.148260 0.162280 0.913079 11.00000 -1.20000 HKLF 4 REM 13101 in Pna2(1) REM R1 = 0.0530 for 5060 Fo > 4sig(Fo) and 0.0539 for all 5161 data REM 356 parameters refined using 1 restraints END WGHT 0.0878 1.5716 REM Highest difference peak 0.496, deepest hole -0.212, 1-sigma level 0.050 Q1 1 0.4235 0.5747 1.0551 11.00000 0.05 0.50 Q2 1 0.4065 0.0772 0.9035 11.00000 0.05 0.47 Q3 1 0.5950 0.5035 1.0158 11.00000 0.05 0.40 Q4 1 0.4774 0.3226 1.1178 11.00000 0.05 0.37 Q5 1 0.4858 0.5034 1.0144 11.00000 0.05 0.34 ; _database_code_depnum_ccdc_archive 'CCDC 948437' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 O6' _chemical_formula_sum 'C30 H24 O6' _chemical_formula_weight 480.49 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.3776(2) _cell_length_b 15.9590(3) _cell_length_c 26.0724(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4734.10(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8607 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 70.99 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9136 _exptl_absorpt_correction_T_max 0.9774 _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_special_details ; loop, paratone ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Incoatec micro-focus' _diffrn_source_monochromator 'MONTEL Multi-layer' _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method 'combination of \w and \f-scans ' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 68457 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 71.63 _reflns_number_total 4563 _reflns_number_gt 3813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2013-2.0' _computing_cell_refinement 'Bruker SAINT v8.27B' _computing_data_reduction 'Bruker SAINT v8.27B' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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^)+(0.0523P)^2^+1.3577P] 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 4563 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 O1 O -0.35531(10) 0.47097(7) -0.20240(4) 0.0384(3) Uani 1 1 d . . . O2 O -0.44520(9) 0.37846(8) -0.15077(5) 0.0406(3) Uani 1 1 d . . . O3 O 0.27489(9) 0.21797(7) -0.31085(4) 0.0333(2) Uani 1 1 d . . . O4 O 0.10954(10) 0.14733(7) -0.29279(4) 0.0370(3) Uani 1 1 d . . . O5 O 0.82904(9) 0.33933(7) 0.08444(4) 0.0331(2) Uani 1 1 d . . . O6 O 0.76892(10) 0.44646(7) 0.13378(4) 0.0379(3) Uani 1 1 d . . . C1 C 0.08509(11) 0.38957(8) -0.05735(5) 0.0224(3) Uani 1 1 d . . . C2 C 0.18667(11) 0.36247(8) -0.08381(5) 0.0214(3) Uani 1 1 d . . . C3 C 0.29432(11) 0.36317(8) -0.05839(5) 0.0219(3) Uani 1 1 d . . . H3 H 0.3627 0.3459 -0.0764 0.026 Uiso 1 1 calc R . . C4 C 0.30544(11) 0.38840(8) -0.00724(5) 0.0219(3) Uani 1 1 d . . . C5 C 0.20342(12) 0.41227(9) 0.01884(5) 0.0245(3) Uani 1 1 d . . . H5 H 0.2081 0.4288 0.0538 0.029 Uiso 1 1 calc R . . C6 C 0.09548(12) 0.41210(9) -0.00580(5) 0.0248(3) Uani 1 1 d . . . H6 H 0.0271 0.4276 0.0128 0.030 Uiso 1 1 calc R . . C7 C -0.03054(11) 0.39897(8) -0.08340(5) 0.0222(3) Uani 1 1 d . . . C8 C -0.03722(11) 0.44365(8) -0.12950(5) 0.0239(3) Uani 1 1 d . . . H8 H 0.0317 0.4685 -0.1434 0.029 Uiso 1 1 calc R . . C9 C -0.14310(12) 0.45191(8) -0.15507(5) 0.0245(3) Uani 1 1 d . . . H9 H -0.1470 0.4832 -0.1860 0.029 Uiso 1 1 calc R . . C10 C -0.24426(11) 0.41423(8) -0.13535(5) 0.0239(3) Uani 1 1 d . . . C11 C -0.23869(12) 0.37155(9) -0.08885(5) 0.0262(3) Uani 1 1 d . . . H11 H -0.3077 0.3469 -0.0750 0.031 Uiso 1 1 calc R . . C12 C -0.13315(12) 0.36485(9) -0.06271(5) 0.0260(3) Uani 1 1 d . . . H12 H -0.1305 0.3369 -0.0306 0.031 Uiso 1 1 calc R . . C13 C -0.35893(12) 0.41800(9) -0.16278(5) 0.0283(3) Uani 1 1 d . . . C14 C -0.46076(16) 0.47618(14) -0.23322(7) 0.0516(5) Uani 1 1 d . . . H14A H -0.4488 0.5167 -0.2610 0.077 Uiso 1 1 calc R . . H14B H -0.5266 0.4944 -0.2117 0.077 Uiso 1 1 calc R . . H14C H -0.4783 0.4210 -0.2478 0.077 Uiso 1 1 calc R . . C15 C 0.18165(11) 0.32670(8) -0.13665(5) 0.0225(3) Uani 1 1 d . . . C16 C 0.26819(12) 0.34508(9) -0.17281(5) 0.0263(3) Uani 1 1 d . . . H16 H 0.3270 0.3853 -0.1650 0.032 Uiso 1 1 calc R . . C17 C 0.26938(12) 0.30517(9) -0.22018(5) 0.0275(3) Uani 1 1 d . . . H17 H 0.3290 0.3180 -0.2444 0.033 Uiso 1 1 calc R . . C18 C 0.18297(12) 0.24627(9) -0.23213(5) 0.0249(3) Uani 1 1 d . . . C19 C 0.09482(12) 0.22895(9) -0.19670(5) 0.0267(3) Uani 1 1 d . . . H19 H 0.0348 0.1898 -0.2049 0.032 Uiso 1 1 calc R . . C20 C 0.09432(11) 0.26855(9) -0.14958(5) 0.0247(3) Uani 1 1 d . . . H20 H 0.0339 0.2562 -0.1256 0.030 Uiso 1 1 calc R . . C21 C 0.18277(12) 0.19846(9) -0.28102(5) 0.0271(3) Uani 1 1 d . . . C22 C 0.28082(15) 0.17233(11) -0.35839(6) 0.0376(4) Uani 1 1 d . . . H22A H 0.2098 0.1833 -0.3786 0.056 Uiso 1 1 calc R . . H22B H 0.2866 0.1122 -0.3512 0.056 Uiso 1 1 calc R . . H22C H 0.3501 0.1904 -0.3778 0.056 Uiso 1 1 calc R . . C23 C 0.42181(11) 0.39027(8) 0.01850(5) 0.0219(3) Uani 1 1 d . . . C24 C 0.44661(12) 0.45214(8) 0.05503(5) 0.0246(3) Uani 1 1 d . . . H24 H 0.3891 0.4935 0.0626 0.029 Uiso 1 1 calc R . . C25 C 0.55371(12) 0.45392(9) 0.08019(5) 0.0254(3) Uani 1 1 d . . . H25 H 0.5685 0.4957 0.1053 0.030 Uiso 1 1 calc R . . C26 C 0.63989(12) 0.39484(8) 0.06894(5) 0.0242(3) Uani 1 1 d . . . C27 C 0.61733(12) 0.33374(9) 0.03199(5) 0.0247(3) Uani 1 1 d . . . H27 H 0.6760 0.2936 0.0237 0.030 Uiso 1 1 calc R . . C28 C 0.50937(12) 0.33149(8) 0.00734(5) 0.0238(3) Uani 1 1 d . . . H28 H 0.4946 0.2893 -0.0175 0.029 Uiso 1 1 calc R . . C29 C 0.75114(12) 0.39766(9) 0.09932(5) 0.0269(3) Uani 1 1 d . . . C30 C 0.93272(13) 0.33303(10) 0.11653(6) 0.0376(4) Uani 1 1 d . . . H30A H 0.9771 0.2826 0.1072 0.056 Uiso 1 1 calc R . . H30B H 0.9090 0.3296 0.1526 0.056 Uiso 1 1 calc R . . H30C H 0.9822 0.3826 0.1114 0.056 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 O1 0.0305(6) 0.0479(7) 0.0367(6) 0.0073(5) -0.0138(5) -0.0008(5) O2 0.0224(5) 0.0518(7) 0.0476(7) 0.0041(5) -0.0055(5) -0.0047(5) O3 0.0355(6) 0.0375(6) 0.0270(5) -0.0103(4) 0.0046(4) -0.0083(4) O4 0.0357(6) 0.0412(6) 0.0340(6) -0.0130(4) 0.0006(5) -0.0114(5) O5 0.0250(5) 0.0352(6) 0.0392(6) -0.0041(4) -0.0110(4) 0.0013(4) O6 0.0329(6) 0.0400(6) 0.0409(6) -0.0098(5) -0.0124(5) -0.0014(4) C1 0.0211(6) 0.0225(6) 0.0236(6) 0.0016(5) -0.0007(5) 0.0000(5) C2 0.0215(6) 0.0202(6) 0.0224(6) 0.0010(5) -0.0001(5) -0.0005(5) C3 0.0205(6) 0.0213(6) 0.0238(6) -0.0007(5) 0.0006(5) 0.0000(5) C4 0.0218(6) 0.0205(6) 0.0235(6) 0.0020(5) -0.0012(5) -0.0011(5) C5 0.0258(7) 0.0278(7) 0.0200(6) 0.0001(5) -0.0010(5) 0.0012(5) C6 0.0226(6) 0.0273(7) 0.0245(6) 0.0011(5) 0.0024(5) 0.0028(5) C7 0.0196(6) 0.0230(6) 0.0239(6) -0.0035(5) -0.0001(5) 0.0021(5) C8 0.0204(6) 0.0246(7) 0.0268(6) 0.0005(5) 0.0013(5) -0.0003(5) C9 0.0231(6) 0.0255(7) 0.0248(6) 0.0007(5) -0.0002(5) 0.0023(5) C10 0.0200(6) 0.0258(7) 0.0257(6) -0.0047(5) -0.0011(5) 0.0032(5) C11 0.0193(6) 0.0289(7) 0.0303(7) -0.0002(5) 0.0027(5) -0.0004(5) C12 0.0235(7) 0.0297(7) 0.0247(6) 0.0024(5) 0.0020(5) 0.0027(5) C13 0.0225(7) 0.0320(7) 0.0304(7) -0.0055(6) -0.0021(5) 0.0035(5) C14 0.0388(10) 0.0682(13) 0.0479(10) 0.0106(9) -0.0226(8) -0.0008(8) C15 0.0199(6) 0.0235(6) 0.0240(6) -0.0013(5) -0.0027(5) 0.0028(5) C16 0.0230(7) 0.0297(7) 0.0261(7) -0.0039(5) -0.0009(5) -0.0048(5) C17 0.0238(7) 0.0332(7) 0.0257(7) -0.0028(5) 0.0021(5) -0.0037(5) C18 0.0238(7) 0.0262(7) 0.0246(6) -0.0020(5) -0.0036(5) 0.0014(5) C19 0.0219(6) 0.0282(7) 0.0302(7) -0.0031(5) -0.0036(5) -0.0028(5) C20 0.0190(6) 0.0281(7) 0.0270(7) -0.0009(5) 0.0009(5) -0.0007(5) C21 0.0250(7) 0.0286(7) 0.0277(7) -0.0021(5) -0.0021(5) 0.0002(5) C22 0.0448(9) 0.0388(9) 0.0293(7) -0.0110(6) 0.0075(7) -0.0084(7) C23 0.0215(6) 0.0248(7) 0.0193(6) 0.0032(5) 0.0004(5) -0.0025(5) C24 0.0239(7) 0.0252(7) 0.0245(6) -0.0012(5) 0.0009(5) 0.0000(5) C25 0.0275(7) 0.0257(7) 0.0230(6) -0.0012(5) -0.0004(5) -0.0049(5) C26 0.0238(7) 0.0252(7) 0.0235(6) 0.0041(5) -0.0015(5) -0.0047(5) C27 0.0235(7) 0.0255(7) 0.0251(6) 0.0023(5) -0.0006(5) 0.0006(5) C28 0.0255(7) 0.0245(7) 0.0214(6) -0.0003(5) -0.0016(5) -0.0013(5) C29 0.0251(7) 0.0267(7) 0.0289(7) 0.0030(5) -0.0024(6) -0.0057(5) C30 0.0267(7) 0.0374(9) 0.0486(9) -0.0018(7) -0.0141(7) 0.0003(6) _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 O1 C13 1.3356(18) . ? O1 C14 1.4462(18) . ? O2 C13 1.2081(18) . ? O3 C21 1.3419(17) . ? O3 C22 1.4391(16) . ? O4 C21 1.2059(18) . ? O5 C29 1.3427(18) . ? O5 C30 1.4498(17) . ? O6 C29 1.2061(17) . ? C1 C6 1.3961(18) . ? C1 C2 1.4138(18) . ? C1 C7 1.4882(17) . ? C2 C3 1.3926(18) . ? C2 C15 1.4925(18) . ? C3 C4 1.3988(18) . ? C3 H3 0.9500 . ? C4 C5 1.3981(18) . ? C4 C23 1.4847(17) . ? C5 C6 1.3860(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.3966(18) . ? C7 C8 1.3996(18) . ? C8 C9 1.3832(18) . ? C8 H8 0.9500 . ? C9 C10 1.3966(19) . ? C9 H9 0.9500 . ? C10 C11 1.3921(19) . ? C10 C13 1.4890(18) . ? C11 C12 1.3849(19) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.3944(19) . ? C15 C20 1.4008(18) . ? C16 C17 1.3897(19) . ? C16 H16 0.9500 . ? C17 C18 1.3953(19) . ? C17 H17 0.9500 . ? C18 C19 1.391(2) . ? C18 C21 1.4856(18) . ? C19 C20 1.3814(19) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.3990(18) . ? C23 C24 1.4005(18) . ? C24 C25 1.3842(19) . ? C24 H24 0.9500 . ? C25 C26 1.3917(19) . ? C25 H25 0.9500 . ? C26 C27 1.3946(19) . ? C26 C29 1.4939(18) . ? C27 C28 1.3867(19) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 O1 C14 116.14(13) . . ? C21 O3 C22 114.73(11) . . ? C29 O5 C30 114.73(11) . . ? C6 C1 C2 118.64(12) . . ? C6 C1 C7 119.22(12) . . ? C2 C1 C7 122.06(12) . . ? C3 C2 C1 118.96(12) . . ? C3 C2 C15 118.43(11) . . ? C1 C2 C15 122.42(12) . . ? C2 C3 C4 122.39(12) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 117.83(12) . . ? C5 C4 C23 121.00(11) . . ? C3 C4 C23 121.16(12) . . ? C6 C5 C4 120.65(12) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 121.45(12) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C12 C7 C8 119.01(12) . . ? C12 C7 C1 121.56(12) . . ? C8 C7 C1 119.42(12) . . ? C9 C8 C7 120.65(12) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.95(12) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.59(12) . . ? C11 C10 C13 118.55(12) . . ? C9 C10 C13 121.86(12) . . ? C12 C11 C10 120.39(12) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.31(12) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? O2 C13 O1 123.79(13) . . ? O2 C13 C10 124.49(14) . . ? O1 C13 C10 111.72(12) . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.53(12) . . ? C16 C15 C2 121.10(12) . . ? C20 C15 C2 120.18(12) . . ? C17 C16 C15 120.74(12) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.03(13) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.57(13) . . ? C19 C18 C21 117.81(12) . . ? C17 C18 C21 122.60(12) . . ? C20 C19 C18 120.16(13) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 120.94(13) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? O4 C21 O3 123.31(13) . . ? O4 C21 C18 124.54(13) . . ? O3 C21 C18 112.15(12) . . ? O3 C22 H22A 109.5 . . ? O3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 118.08(12) . . ? C28 C23 C4 121.84(12) . . ? C24 C23 C4 120.08(12) . . ? C25 C24 C23 120.94(12) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.42(12) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 119.33(12) . . ? C25 C26 C29 117.69(12) . . ? C27 C26 C29 122.91(12) . . ? C28 C27 C26 120.08(13) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 121.14(12) . . ? C27 C28 H28 119.4 . . ? C23 C28 H28 119.4 . . ? O6 C29 O5 123.53(13) . . ? O6 C29 C26 123.82(13) . . ? O5 C29 C26 112.65(12) . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -3.19(19) . . . . ? C7 C1 C2 C3 173.57(12) . . . . ? C6 C1 C2 C15 171.85(12) . . . . ? C7 C1 C2 C15 -11.4(2) . . . . ? C1 C2 C3 C4 1.12(19) . . . . ? C15 C2 C3 C4 -174.12(12) . . . . ? C2 C3 C4 C5 1.02(19) . . . . ? C2 C3 C4 C23 -178.63(12) . . . . ? C3 C4 C5 C6 -1.1(2) . . . . ? C23 C4 C5 C6 178.58(12) . . . . ? C4 C5 C6 C1 -1.1(2) . . . . ? C2 C1 C6 C5 3.2(2) . . . . ? C7 C1 C6 C5 -173.65(12) . . . . ? C6 C1 C7 C12 -52.16(18) . . . . ? C2 C1 C7 C12 131.10(14) . . . . ? C6 C1 C7 C8 127.26(14) . . . . ? C2 C1 C7 C8 -49.48(18) . . . . ? C12 C7 C8 C9 -1.9(2) . . . . ? C1 C7 C8 C9 178.68(12) . . . . ? C7 C8 C9 C10 -1.1(2) . . . . ? C8 C9 C10 C11 2.7(2) . . . . ? C8 C9 C10 C13 -177.06(12) . . . . ? C9 C10 C11 C12 -1.3(2) . . . . ? C13 C10 C11 C12 178.45(12) . . . . ? C10 C11 C12 C7 -1.7(2) . . . . ? C8 C7 C12 C11 3.3(2) . . . . ? C1 C7 C12 C11 -177.30(12) . . . . ? C14 O1 C13 O2 -3.2(2) . . . . ? C14 O1 C13 C10 177.06(14) . . . . ? C11 C10 C13 O2 -9.1(2) . . . . ? C9 C10 C13 O2 170.72(14) . . . . ? C11 C10 C13 O1 170.63(12) . . . . ? C9 C10 C13 O1 -9.57(19) . . . . ? C3 C2 C15 C16 -43.41(18) . . . . ? C1 C2 C15 C16 141.52(14) . . . . ? C3 C2 C15 C20 131.56(13) . . . . ? C1 C2 C15 C20 -43.51(19) . . . . ? C20 C15 C16 C17 -1.5(2) . . . . ? C2 C15 C16 C17 173.58(13) . . . . ? C15 C16 C17 C18 0.3(2) . . . . ? C16 C17 C18 C19 1.1(2) . . . . ? C16 C17 C18 C21 -176.92(13) . . . . ? C17 C18 C19 C20 -1.3(2) . . . . ? C21 C18 C19 C20 176.75(13) . . . . ? C18 C19 C20 C15 0.2(2) . . . . ? C16 C15 C20 C19 1.2(2) . . . . ? C2 C15 C20 C19 -173.89(12) . . . . ? C22 O3 C21 O4 -0.5(2) . . . . ? C22 O3 C21 C18 178.80(12) . . . . ? C19 C18 C21 O4 2.2(2) . . . . ? C17 C18 C21 O4 -179.75(15) . . . . ? C19 C18 C21 O3 -177.10(12) . . . . ? C17 C18 C21 O3 0.92(19) . . . . ? C5 C4 C23 C28 145.95(13) . . . . ? C3 C4 C23 C28 -34.41(18) . . . . ? C5 C4 C23 C24 -34.16(18) . . . . ? C3 C4 C23 C24 145.48(13) . . . . ? C28 C23 C24 C25 -1.42(19) . . . . ? C4 C23 C24 C25 178.68(12) . . . . ? C23 C24 C25 C26 1.1(2) . . . . ? C24 C25 C26 C27 0.0(2) . . . . ? C24 C25 C26 C29 -177.01(12) . . . . ? C25 C26 C27 C28 -0.88(19) . . . . ? C29 C26 C27 C28 176.00(12) . . . . ? C26 C27 C28 C23 0.6(2) . . . . ? C24 C23 C28 C27 0.57(19) . . . . ? C4 C23 C28 C27 -179.54(12) . . . . ? C30 O5 C29 O6 6.2(2) . . . . ? C30 O5 C29 C26 -173.17(12) . . . . ? C25 C26 C29 O6 2.2(2) . . . . ? C27 C26 C29 O6 -174.78(14) . . . . ? C25 C26 C29 O5 -178.44(12) . . . . ? C27 C26 C29 O5 4.63(18) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 71.63 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.215 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.038 _iucr_refine_instructions_details ; TITL 2M in Pbca CELL 1.54178 11.3776 15.959 26.0724 90 90 90 ZERR 8 0.0002 0.0003 0.0004 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H O UNIT 240 192 48 TEMP -123 L.S. 5 SIZE 0.12 0.07 0.03 REM Colorless Plate, ND DUO, ApexII rem 10-s low angle, 15-s high angle acta conf bond $h mpla 6 c7 c8 c9 c10 c11 c12 mpla 6 c1 c2 c3 c4 c5 c6 mpla 6 c15 c16 c17 c18 c19 c20 mpla 6 c1 c2 c3 c4 c5 c6 mpla 6 c23 c24 c25 c26 c27 c28 fmap 2 PLAN 5 WGHT 0.052300 1.357700 FVAR 0.08157 O1 3 -0.355314 0.470973 -0.202403 11.00000 0.03054 0.04789 = 0.03671 0.00727 -0.01377 -0.00083 O2 3 -0.445198 0.378463 -0.150765 11.00000 0.02239 0.05183 = 0.04762 0.00410 -0.00550 -0.00468 O3 3 0.274894 0.217968 -0.310853 11.00000 0.03555 0.03746 = 0.02695 -0.01026 0.00461 -0.00827 O4 3 0.109538 0.147331 -0.292787 11.00000 0.03571 0.04121 = 0.03400 -0.01297 0.00062 -0.01139 O5 3 0.829037 0.339326 0.084435 11.00000 0.02501 0.03525 = 0.03916 -0.00408 -0.01102 0.00125 O6 3 0.768919 0.446465 0.133783 11.00000 0.03294 0.03998 = 0.04088 -0.00983 -0.01238 -0.00140 C1 1 0.085094 0.389575 -0.057348 11.00000 0.02113 0.02252 = 0.02360 0.00163 -0.00072 0.00001 C2 1 0.186673 0.362468 -0.083808 11.00000 0.02154 0.02025 = 0.02244 0.00100 -0.00010 -0.00046 C3 1 0.294317 0.363171 -0.058387 11.00000 0.02051 0.02131 = 0.02381 -0.00066 0.00055 0.00003 AFIX 43 H3 2 0.362674 0.345888 -0.076440 11.00000 -1.20000 AFIX 0 C4 1 0.305441 0.388399 -0.007238 11.00000 0.02178 0.02050 = 0.02350 0.00198 -0.00117 -0.00111 C5 1 0.203424 0.412274 0.018835 11.00000 0.02576 0.02780 = 0.01998 0.00005 -0.00097 0.00123 AFIX 43 H5 2 0.208135 0.428782 0.053783 11.00000 -1.20000 AFIX 0 C6 1 0.095483 0.412095 -0.005803 11.00000 0.02259 0.02731 = 0.02446 0.00114 0.00245 0.00283 AFIX 43 H6 2 0.027064 0.427637 0.012790 11.00000 -1.20000 AFIX 0 C7 1 -0.030541 0.398971 -0.083400 11.00000 0.01959 0.02299 = 0.02394 -0.00348 -0.00007 0.00215 C8 1 -0.037217 0.443650 -0.129500 11.00000 0.02041 0.02462 = 0.02679 0.00047 0.00130 -0.00035 AFIX 43 H8 2 0.031652 0.468544 -0.143365 11.00000 -1.20000 AFIX 0 C9 1 -0.143104 0.451915 -0.155070 11.00000 0.02308 0.02555 = 0.02481 0.00067 -0.00025 0.00228 AFIX 43 H9 2 -0.147018 0.483198 -0.186023 11.00000 -1.20000 AFIX 0 C10 1 -0.244259 0.414233 -0.135349 11.00000 0.01998 0.02584 = 0.02573 -0.00475 -0.00113 0.00316 C11 1 -0.238692 0.371551 -0.088847 11.00000 0.01926 0.02892 = 0.03029 -0.00024 0.00265 -0.00041 AFIX 43 H11 2 -0.307697 0.346879 -0.074963 11.00000 -1.20000 AFIX 0 C12 1 -0.133150 0.364847 -0.062709 11.00000 0.02350 0.02969 = 0.02471 0.00235 0.00195 0.00271 AFIX 43 H12 2 -0.130534 0.336908 -0.030555 11.00000 -1.20000 AFIX 0 C13 1 -0.358934 0.417999 -0.162775 11.00000 0.02250 0.03202 = 0.03036 -0.00554 -0.00214 0.00349 C14 1 -0.460756 0.476184 -0.233218 11.00000 0.03881 0.06819 = 0.04786 0.01064 -0.02265 -0.00079 AFIX 137 H14A 2 -0.448810 0.516676 -0.260991 11.00000 -1.50000 H14B 2 -0.526610 0.494396 -0.211707 11.00000 -1.50000 H14C 2 -0.478298 0.421011 -0.247836 11.00000 -1.50000 AFIX 0 C15 1 0.181645 0.326702 -0.136654 11.00000 0.01989 0.02351 = 0.02405 -0.00130 -0.00269 0.00282 C16 1 0.268194 0.345085 -0.172809 11.00000 0.02303 0.02975 = 0.02612 -0.00394 -0.00094 -0.00479 AFIX 43 H16 2 0.327012 0.385349 -0.164972 11.00000 -1.20000 AFIX 0 C17 1 0.269376 0.305166 -0.220177 11.00000 0.02381 0.03318 = 0.02566 -0.00278 0.00214 -0.00367 AFIX 43 H17 2 0.329040 0.317981 -0.244431 11.00000 -1.20000 AFIX 0 C18 1 0.182974 0.246273 -0.232131 11.00000 0.02384 0.02621 = 0.02463 -0.00197 -0.00357 0.00142 C19 1 0.094822 0.228946 -0.196697 11.00000 0.02188 0.02817 = 0.03018 -0.00307 -0.00363 -0.00281 AFIX 43 H19 2 0.034829 0.189784 -0.204924 11.00000 -1.20000 AFIX 0 C20 1 0.094320 0.268546 -0.149583 11.00000 0.01900 0.02806 = 0.02696 -0.00093 0.00093 -0.00066 AFIX 43 H20 2 0.033890 0.256161 -0.125608 11.00000 -1.20000 AFIX 0 C21 1 0.182768 0.198460 -0.281019 11.00000 0.02499 0.02857 = 0.02767 -0.00208 -0.00213 0.00025 C22 1 0.280816 0.172333 -0.358391 11.00000 0.04477 0.03878 = 0.02932 -0.01102 0.00748 -0.00837 AFIX 137 H22A 2 0.209794 0.183304 -0.378570 11.00000 -1.50000 H22B 2 0.286600 0.112209 -0.351177 11.00000 -1.50000 H22C 2 0.350086 0.190411 -0.377798 11.00000 -1.50000 AFIX 0 C23 1 0.421811 0.390275 0.018500 11.00000 0.02155 0.02484 = 0.01927 0.00319 0.00044 -0.00251 C24 1 0.446611 0.452139 0.055029 11.00000 0.02394 0.02522 = 0.02452 -0.00119 0.00089 0.00002 AFIX 43 H24 2 0.389110 0.493470 0.062645 11.00000 -1.20000 AFIX 0 C25 1 0.553707 0.453923 0.080193 11.00000 0.02755 0.02568 = 0.02299 -0.00116 -0.00045 -0.00485 AFIX 43 H25 2 0.568473 0.495749 0.105307 11.00000 -1.20000 AFIX 0 C26 1 0.639888 0.394835 0.068938 11.00000 0.02377 0.02519 = 0.02352 0.00408 -0.00151 -0.00472 C27 1 0.617334 0.333738 0.031986 11.00000 0.02354 0.02554 = 0.02514 0.00228 -0.00061 0.00062 AFIX 43 H27 2 0.676002 0.293610 0.023686 11.00000 -1.20000 AFIX 0 C28 1 0.509370 0.331489 0.007343 11.00000 0.02545 0.02448 = 0.02141 -0.00031 -0.00157 -0.00135 AFIX 43 H28 2 0.494610 0.289303 -0.017545 11.00000 -1.20000 AFIX 0 C29 1 0.751138 0.397659 0.099325 11.00000 0.02507 0.02665 = 0.02889 0.00297 -0.00237 -0.00571 C30 1 0.932716 0.333029 0.116530 11.00000 0.02668 0.03742 = 0.04861 -0.00177 -0.01414 0.00033 AFIX 137 H30A 2 0.977080 0.282628 0.107240 11.00000 -1.50000 H30B 2 0.908961 0.329596 0.152599 11.00000 -1.50000 H30C 2 0.982192 0.382604 0.111446 11.00000 -1.50000 HKLF 4 REM 13103b in Pbca REM R1 = 0.0362 for 3813 Fo > 4sig(Fo) and 0.0454 for all 4563 data REM 328 parameters refined using 0 restraints END WGHT 0.0524 1.3579 REM Highest difference peak 0.215, deepest hole -0.191, 1-sigma level 0.038 Q1 1 0.0271 0.3959 -0.0715 11.00000 0.05 0.22 Q2 1 -0.2966 0.4157 -0.1458 11.00000 0.05 0.21 Q3 1 0.3602 0.3823 0.0100 11.00000 0.05 0.21 Q4 1 -0.2013 0.4427 -0.1419 11.00000 0.05 0.19 Q5 1 0.1307 0.3617 -0.0693 11.00000 0.05 0.19 ; #eof data_2m =========================================== #eof =================================================== ________________________________________ From: #--------------------------------------------------------------- #--------------------------------------------------------------- #--------------------------------------------------------------- #--------------------------------------------------------------- #--------------------------------------------------------------- #--------------------------------------------------------------- #----- _database_code_depnum_ccdc_archive 'CCDC 948438'