#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005029.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005029 loop_ _publ_author_name 'Honda, T.' 'Fujii, I.' 'Hirayama, N.' 'Ishikawa, D.' 'Kawagishi, H.' 'Song, K.-S.' 'Yoo, I.-D.' _publ_section_title ; (14\a,22E)-14-Hydroxyergosta-4,7,22-triene-3,6-dione, C~28~H~40~O~3~ ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1550 _journal_page_last 1552 _journal_paper_doi 10.1107/S0108270196000030 _journal_volume 52 _journal_year 1996 _chemical_formula_sum 'C28 H40 O3' _chemical_formula_weight 424.62 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 93.51(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 21.900(7) _cell_length_b 6.368(2) _cell_length_c 8.939(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 35 _cell_measurement_theta_min 30 _cell_volume 1244.3(6) _computing_cell_refinement 'CAD-4 software' _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 software' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'TEXSAN (Molecular Structure Corporation, 1992)' _computing_structure_solution 'MITHRIL (Gilmore, 1984)' _diffrn_measurement_device 'Enraf-Nonius CAD-4 Turbo' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2875 _diffrn_reflns_theta_max 74.9 _diffrn_standards_decay_% -2.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_method none _exptl_crystal_description plate _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.23 _refine_diff_density_min -0.15 _refine_ls_extinction_coef 1.155E-5 _refine_ls_extinction_method |F~calc~|/(1+gI~calc~) _refine_ls_goodness_of_fit_obs 2.30 _refine_ls_hydrogen_treatment 'H atoms see text' _refine_ls_number_parameters 436 _refine_ls_number_reflns 2581 _refine_ls_R_factor_obs 0.039 _refine_ls_shift/esd_max 0.11 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w=1/\s^2^(F) _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.047 _reflns_number_observed 2581 _reflns_number_total 2832 _reflns_observed_criterion F>3\s(F) _[local]_cod_data_source_file kh1087.cif _[local]_cod_data_source_block kh1087a _[local]_cod_cif_authors_sg_H-M 'P 21' _[local]_cod_cif_authors_sg_Hall 'P 2y1' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value ' w=1/\s^2^(F)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/\s^2^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2005029 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv O3 .52949(7) .614 -0.4137(2) 5.04(4) O6 .49875(7) -.0515(4) -0.1319(2) 4.96(4) O14 .35584(6) .2720(3) .27050(10) 3.69(3) C1 .38020(10) .5734(4) -0.2741(2) 3.78(4) C2 .42060(10) .6030(4) -0.4068(2) 3.99(4) C3 .48420(9) .5260(4) -0.3698(2) 3.81(4) C4 .48956(9) .3347(4) -0.2787(2) 3.55(4) C5 .44327(8) .2556(4) -0.2060(2) 3.04(3) C6 .45418(8) .0583(4) -0.1172(2) 3.38(4) C7 .40956(9) .0083(4) -.0074(2) 3.24(3) C8 .36576(7) .1436(3) .0273(2) 2.83(3) C9 .35542(8) .3504(4) -.0536(2) 2.99(3) C10 .37955(8) .3479(4) -0.2143(2) 2.98(3) C11 .28900(10) .4287(4) -.0548(2) 3.99(4) C12 .25650(10) .3948(4) .0902(2) 3.85(4) C13 .26175(8) .1667(4) .1415(2) 3.23(3) C14 .33057(8) .1156(4) .1673(2) 3.05(3) C15 .33190(9) -.0963(4) .2457(2) 3.72(4) C16 .27590(9) -.0868(4) .3439(2) 3.88(4) C17 .23956(9) .1131(4) .2987(2) 3.60(4) C18 .23210(10) .0174(5) .0229(2) 4.05(4) C19 .34060(10) .2050(4) -0.3225(2) 3.74(4) C20 .17060(10) .0862(5) .3179(3) 4.91(5) C21 .13310(10) .2816(9) .2758(5) 8.00(10) C22 .16160(10) .0284(5) .4789(3) 5.08(5) C23 .12770(10) -0.1214(6) .5256(3) 5.66(6) C24 .12090(10) -0.1810(7) .6874(3) 6.14(7) C25 .1466(3) -0.4020(10) .7122(6) 11.5(2) C26 .05500(10) -0.1589(7) .7332(3) 6.85(8) C27 .0312(3) .0580(10) .7076(7) 10.8(2) C28 .0486(2) -0.2230(10) .8946(5) 10.80(10) H1a .3990(10) .668(4) -0.20(3) 4.2(5) H1b .3380(10) .612(5) -0.30(3) 4.7(5) H2a .4220(10) .758(6) -0.44(3) 7.2(8) H2b .4050(10) .517(5) -0.50(3) 4.9(6) H4 .5260(10) .273(4) -0.27(2) 3.6(4) H7 .4160(9) -0.113(4) .05(2) 3.4(4) H9 .3790(10) .456(4) .01(2) 3.7(5) H10a .3610(10) .195(4) -0.42(2) 4.0(5) H10b .2980(10) .256(5) -0.34(3) 5.5(6) H10c .3380(10) .060(5) -0.29(3) 5.4(6) H11a .2870(10) .575(4) -.08(3) 4.1(5) H11b .2630(10) .355(4) -0.14(3) 4.6(5) H12a .2750(10) .486(5) .17(3) 4.3(5) H12b .2130(10) .431(4) .07(3) 4.2(5) H14 .3950(10) .216(6) .29(3) 7.6(8) H15a .3730(10) -0.121(4) .31(3) 4.0(5) H15b .3300(10) -0.209(4) .17(2) 3.8(5) H16a .2880(10) -.094(5) .45(3) 4.9(5) H16b .2500(10) -0.209(5) .33(3) 4.7(5) H17 .2540(10) .233(5) .36(3) 4.2(5) H18a .2550(10) .022(5) -.08(3) 5.4(6) H18b .1910(10) .075(4) -.00(2) 4.6(5) H18c .2310(10) -0.129(6) .06(3) 6.2(7) H20 .1570(10) -.041(5) .26(3) 4.5(5) H21a .090(2) .262(7) .30(4) 9.0(10) H21b .132(2) .311(8) .18(4) 9.0(10) H21c .151(2) .404(7) .35(4) 9.0(10) H22 .1830(10) .114(6) .55(3) 5.7(6) H23 .1010(10) -0.197(6) .45(3) 5.9(6) H24 .1470(10) -.057(6) .75(3) 5.8(6) H25a .186(2) -0.413(8) .67(4) 10.0(10) H25b .143(2) -0.438(9) .83(5) 12.0(10) H25c .103(3) -0.490(10) .64(7) 8.0 H26 .0250(10) -0.259(5) .66(3) 5.9(6) H27a -.008(2) .076(8) .76(4) 9.0(10) H27b .067(2) .140(10) .76(5) 13.0(10) H27c .036(2) .120(10) .59(5) 14.0(10) H28a .004(2) -0.210(10) .93(5) 14.0(10) H28b .076(3) -0.17(2) .96(7) 8.0 H28c .056 -0.373 .903 8.0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 C1 C10 113.7(2) yes C1 C2 C3 111.3(2) yes O3 C3 C2 122.8(2) yes O3 C3 C4 121.2(2) yes C2 C3 C4 115.9(2) yes C3 C4 C5 123.1(2) yes C4 C5 C6 118.2(2) yes C4 C5 C10 123.8(2) yes C6 C5 C10 117.90(10) yes O6 C6 C5 121.9(2) yes O6 C6 C7 121.5(2) yes C5 C6 C7 116.5(2) yes C6 C7 C8 122.2(2) yes C7 C8 C9 122.5(2) yes C7 C8 C14 121.5(2) yes C9 C8 C14 115.20(10) yes C8 C9 C10 112.40(10) yes C8 C9 C11 113.5(2) yes C10 C9 C11 111.80(10) yes C1 C10 C5 110.7(2) yes C1 C10 C9 108.70(10) yes C1 C10 C19 110.5(2) yes C5 C10 C9 108.90(10) yes C5 C10 C19 105.9(2) yes C9 C10 C19 112.20(10) yes C11 C12 C13 111.0(2) yes C12 C13 C14 107.4(2) yes C12 C13 C17 117.3(2) yes C12 C13 C18 111.2(2) yes C14 C13 C17 100.10(10) yes C14 C13 C18 109.9(2) yes C17 C13 C18 110.2(2) yes O14 C14 C8 104.60(10) yes O14 C14 C13 106.40(10) yes O14 C14 C15 108.80(10) yes C8 C14 C13 113.10(10) yes C8 C14 C15 119.1(2) yes C13 C14 C15 104.20(10) yes C14 C15 C16 103.4(2) yes C15 C16 C17 107.3(2) yes C13 C17 C16 103.4(2) yes C13 C17 C20 119.3(2) yes C16 C17 C20 111.9(2) yes C17 C20 C21 113.5(2) yes C17 C20 C22 108.6(2) yes C21 C20 C22 109.5(2) yes C20 C22 C23 126.7(2) yes C22 C23 C24 125.9(3) yes C9 C11 C12 115.9(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O3 C3 1.224(2) yes O14 C14 1.446(2) yes C1 C10 1.532(3) yes C3 C4 1.464(3) yes C5 C6 1.497(3) yes C6 C7 1.462(2) yes C8 C9 1.512(3) yes C9 C10 1.561(2) yes C10 C19 1.547(3) yes C12 C13 1.525(3) yes C13 C17 1.552(2) yes C14 C15 1.519(3) yes C16 C17 1.541(3) yes C20 C21 1.525(5) yes C22 C23 1.293(4) yes O6 C6 1.214(2) yes C1 C2 1.534(3) yes C2 C3 1.495(3) yes C4 C5 1.336(3) yes C5 C10 1.511(3) yes C7 C8 1.340(3) yes C8 C14 1.519(2) yes C9 C11 1.538(3) yes C11 C12 1.530(3) yes C13 C14 1.545(3) yes C13 C18 1.539(3) yes C15 C16 1.553(3) yes C17 C20 1.540(3) yes C20 C22 1.509(3) yes C23 C24 1.511(4) yes 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_publ_flag C1 C2 C3 C4 38.2(3) yes C2 C1 C10 C5 42.6(2) yes C3 C2 C1 C10 -54.0(3) yes C5 C6 C7 C8 -8.6(3) yes C6 C5 C10 C9 46.3(2) yes C7 C6 C5 C10 -19.5(2) yes C8 C9 C11 C12 39.3(3) yes C1 C10 C5 C4 -17.4(2) yes C2 C3 C4 C5 -13.6(3) yes C3 C4 C5 C10 2.7(3) yes C5 C10 C9 C8 -47.1(2) yes C6 C7 C8 C9 5.5(3) yes C7 C8 C9 C10 23.9(2) yes C8 C14 C13 C12 -59.7(2) yes C9 C8 C14 C13 49.8(2) yes C11 C9 C8 C14 -37.9(2) yes C13 C14 C15 C16 -34.3(2) yes C14 C13 C17 C16 -39.7(2) yes C15 C14 C13 C17 46.5(2) yes C17 C20 C22 C23 -132.5(3) yes C22 C23 C24 C26 119.0(4) yes C9 C11 C12 C13 -51.7(3) yes C11 C12 C13 C14 59.6(2) yes C13 C17 C16 C15 19.7(2) yes C14 C15 C16 C17 8.8(2) yes C16 C17 C20 C22 57.4(3) yes C20 C22 C23 C24 178.0(3) yes