#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003490.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003490 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 958 _journal_page_last 960 _publ_section_title ; 3-Hydroxyimino-5\a,13\a,14\b,17\a-lanosta-8,24-dien-20-oic Acid ; _chemical_formula_moiety 'C30 H47 N1 O3' _chemical_formula_sum 'C30 H47 N1 O3' _chemical_formula_weight 469.69 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _symmetry_space_group_name_H-M 'P 21' _cell_length_a 12.995(1) _cell_length_b 7.161(1) _cell_length_c 16.187(1) _cell_angle_alpha 90.00 _cell_angle_beta 112.37(1) _cell_angle_gamma 90.00 _cell_volume 1393.0(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 43.96 _cell_measurement_theta_max 46.16 _exptl_absorpt_coefficient_mu 0.547 _cell_measurement_temperature 293(2) _exptl_crystal_description 'transparent blocks' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.40 _exptl_crystal_colour colourless _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method 2\q/\w _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 6630 _reflns_number_total 5757 _reflns_number_observed 5684 _reflns_observed_criterion >2\s(I) _diffrn_reflns_av_R_equivalents 0.0081 _diffrn_reflns_theta_max 75.57 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'none' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0337 _refine_ls_wR_factor_obs 0.0968 _refine_ls_wR_factor_all 0.1024 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_goodness_of_fit_all 1.117 _refine_ls_number_reflns 5757 _refine_ls_number_parameters 316 _refine_ls_hydrogen_treatment ;H-atom parameters refined using a riding model ; _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0616P)^2^ + 0.1052P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.012 _refine_diff_density_max 0.204 _refine_diff_density_min -0.147 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef 0.0048(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 _refine_ls_abs_structure_details 'Flack (1983), h=?' _refine_ls_abs_structure_Flack 0.02(16) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.22063(11) 1.0000 0.60864(9) 0.0451(3) H1A 1 0.20087(11) 1.1250 0.58474(9) 0.059 H1B 1 0.15247(11) 0.9284 0.59290(9) 0.059 C2 1 0.27744(13) 1.0112(3) 0.71077(9) 0.0496(3) H2A 1 0.34495(13) 1.0849(3) 0.72761(9) 0.064 H2B 1 0.22818(13) 1.0698(3) 0.73546(9) 0.064 C3 1 0.30450(11) 0.8164(3) 0.74582(8) 0.0426(3) N3 1 0.25738(10) 0.7344(3) 0.79196(7) 0.0453(2) O3 1 0.18243(11) 0.8491(2) 0.81233(8) 0.0594(3) H3 1 0.1495(13) 0.7869(7) 0.8371(13) 0.077 C4 1 0.38394(11) 0.7060(3) 0.71550(9) 0.0444(3) C41 1 0.38977(14) 0.5009(3) 0.74442(10) 0.0563(3) H41A 1 0.4475(7) 0.4383(5) 0.7318(7) 0.073 H41B 1 0.3197(3) 0.4413(5) 0.7122(6) 0.073 H41C 1 0.4058(10) 0.4947(3) 0.8074(2) 0.073 C42 1 0.50272(12) 0.7877(4) 0.76061(11) 0.0637(4) H42A 1 0.5514(3) 0.7285(14) 0.7364(7) 0.083 H42B 1 0.5296(5) 0.7657(18) 0.8238(2) 0.083 H42C 1 0.5008(2) 0.9197(5) 0.7496(8) 0.083 C5 1 0.33519(10) 0.7151(3) 0.61076(8) 0.0405(2) H5 1 0.26759(10) 0.6387(3) 0.59225(8) 0.053 C6 1 0.40827(12) 0.6202(3) 0.56869(10) 0.0564(4) H6A 1 0.47105(12) 0.6999(3) 0.57462(10) 0.073 H6B 1 0.43681(12) 0.5036(3) 0.59934(10) 0.073 C7 1 0.34091(13) 0.5824(3) 0.47061(10) 0.0601(4) H7A 1 0.39200(13) 0.5646(3) 0.44049(10) 0.078 H7B 1 0.30048(13) 0.4664(3) 0.46577(10) 0.078 C8 1 0.26028(10) 0.7305(3) 0.42310(8) 0.0445(3) C9 1 0.23237(11) 0.8747(3) 0.46507(9) 0.0452(3) C10 1 0.29527(10) 0.9090(3) 0.56565(8) 0.0406(3) C11 1 0.14680(13) 1.0188(3) 0.41379(9) 0.0536(3) H11A 1 0.18304(13) 1.1398(3) 0.42459(9) 0.070 H11B 1 0.09006(13) 1.0224(3) 0.43905(9) 0.070 C12 1 0.08790(13) 0.9941(3) 0.31216(9) 0.0523(3) H12A 1 0.01137(13) 1.0357(3) 0.29357(9) 0.068 H12B 1 0.12439(13) 1.0712(3) 0.28218(9) 0.068 C13 1 0.08971(10) 0.7903(3) 0.28431(8) 0.0393(3) C14 1 0.21247(10) 0.7217(3) 0.32213(9) 0.0460(3) C14A 1 0.29067(13) 0.8416(4) 0.29173(11) 0.0692(5) H14A 1 0.2856(9) 0.9700(5) 0.3069(9) 0.090 H14B 1 0.2690(8) 0.8303(17) 0.2283(2) 0.090 H14C 1 0.3659(2) 0.7989(14) 0.3212(8) 0.090 C15 1 0.2020(2) 0.5302(3) 0.27737(11) 0.0675(5) H15A 1 0.1766(2) 0.4366(3) 0.30865(11) 0.088 H15B 1 0.2726(2) 0.4908(3) 0.27572(11) 0.088 C16 1 0.11439(13) 0.5626(3) 0.18174(10) 0.0576(4) H16A 1 0.06062(13) 0.4616(3) 0.16479(10) 0.075 H16B 1 0.15033(13) 0.5679(3) 0.13911(10) 0.075 C17 1 0.05567(10) 0.7511(3) 0.18297(8) 0.0420(3) H17 1 0.09079(10) 0.8470(3) 0.15925(8) 0.055 C18 1 0.01816(12) 0.6722(3) 0.32160(9) 0.0526(3) H18A 1 0.0088(8) 0.5492(6) 0.2962(6) 0.068 H18B 1 -0.0534(4) 0.7300(9) 0.3064(7) 0.068 H18C 1 0.0544(5) 0.6638(14) 0.38539(12) 0.068 C19 1 0.38958(13) 1.0466(3) 0.57331(11) 0.0609(4) H19A 1 0.4401(6) 0.9889(7) 0.5505(8) 0.079 H19B 1 0.4288(7) 1.0796(15) 0.63485(15) 0.079 H19C 1 0.3586(2) 1.1570(8) 0.5393(7) 0.079 C20 1 -0.06877(10) 0.7441(3) 0.12138(8) 0.0418(3) H20 1 -0.10389(10) 0.6357(3) 0.13683(8) 0.054 C21 1 -0.08122(12) 0.7299(3) 0.02281(8) 0.0499(3) H21A 1 -0.05271(12) 0.8437(3) 0.00680(8) 0.065 H21B 1 -0.03568(12) 0.6273(3) 0.01712(8) 0.065 C22 1 -0.20097(14) 0.6998(3) -0.04353(9) 0.0565(4) H22A 1 -0.25008(14) 0.7811(3) -0.02742(9) 0.073 H22B 1 -0.20595(14) 0.7355(3) -0.10275(9) 0.073 C23 1 -0.24002(12) 0.5037(3) -0.04643(9) 0.0500(3) H23 1 -0.19928(12) 0.4148(3) -0.06295(9) 0.065 C24 1 -0.32470(12) 0.4382(3) -0.02876(9) 0.0543(3) C25 1 -0.3542(2) 0.2333(4) -0.04188(14) 0.0766(5) H25A 1 -0.4284(5) 0.2195(4) -0.0856(7) 0.100 H25B 1 -0.3500(12) 0.1800(6) 0.0137(3) 0.100 H25C 1 -0.3029(8) 0.1701(5) -0.0621(10) 0.100 C26 1 -0.3960(2) 0.5518(4) 0.00540(13) 0.0788(6) H26A 1 -0.3872(10) 0.5088(15) 0.0639(5) 0.102 H26B 1 -0.4725(2) 0.5393(18) -0.0342(6) 0.102 H26C 1 -0.3743(9) 0.6806(5) 0.0086(10) 0.102 C30 1 -0.12621(10) 0.9203(3) 0.13182(8) 0.0424(3) O31 1 -0.10347(9) 1.0745(2) 0.11244(7) 0.0544(2) O32 1 -0.20319(9) 0.8921(2) 0.16563(7) 0.0530(2) H32 1 -0.2327(12) 0.9917(5) 0.1685(13) 0.069 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0511(7) 0.0046(5) 0.0171(5) 0.0373(6) 0.0036(5) 0.0457(6) C2 0.0645(8) 0.0013(6) 0.0222(6) 0.0385(7) 0.0010(5) 0.0466(7) C3 0.0489(6) -0.0014(5) 0.0120(5) 0.0387(6) -0.0001(5) 0.0364(5) N3 0.0535(6) 0.0030(5) 0.0181(4) 0.0418(6) -0.0009(4) 0.0408(5) O3 0.0797(7) 0.0143(5) 0.0430(6) 0.0490(6) 0.0062(5) 0.0634(6) C4 0.0430(6) 0.0024(5) 0.0121(5) 0.0447(7) 0.0059(5) 0.0419(6) C41 0.0665(9) 0.0141(7) 0.0254(7) 0.0482(8) 0.0116(7) 0.0559(8) C42 0.0445(7) -0.0027(7) 0.0043(6) 0.0798(11) 0.0072(8) 0.0541(8) C5 0.0345(5) 0.0030(5) 0.0127(4) 0.0436(6) 0.0022(5) 0.0418(6) C6 0.0441(7) 0.0209(7) 0.0169(6) 0.0724(10) 0.0062(7) 0.0515(7) C7 0.0533(7) 0.0267(8) 0.0203(6) 0.0763(11) 0.0002(7) 0.0512(7) C8 0.0369(5) 0.0058(6) 0.0170(5) 0.0550(7) 0.0020(6) 0.0431(6) C9 0.0453(6) 0.0039(5) 0.0127(5) 0.0449(7) 0.0026(5) 0.0420(6) C10 0.0384(5) -0.0016(5) 0.0129(4) 0.0420(6) 0.0030(5) 0.0397(6) C11 0.0647(8) 0.0103(6) 0.0092(6) 0.0432(7) -0.0005(6) 0.0427(6) C12 0.0600(8) 0.0094(6) 0.0100(6) 0.0460(7) -0.0007(6) 0.0426(6) C13 0.0378(6) 0.0017(5) 0.0167(4) 0.0438(7) 0.0006(5) 0.0382(6) C14 0.0401(6) 0.0063(6) 0.0190(5) 0.0576(8) 0.0001(6) 0.0431(6) C14A 0.0459(7) -0.0079(9) 0.0231(6) 0.111(2) 0.0075(9) 0.0547(8) C15 0.0704(10) 0.0268(8) 0.0180(7) 0.0712(11) -0.0093(8) 0.0556(8) C16 0.0599(8) 0.0136(7) 0.0208(6) 0.0611(9) -0.0112(7) 0.0514(7) C17 0.0427(6) 0.0006(5) 0.0188(5) 0.0457(7) -0.0017(5) 0.0403(6) C18 0.0473(7) -0.0075(6) 0.0193(5) 0.0671(9) 0.0047(6) 0.0449(6) C19 0.0547(8) -0.0184(7) 0.0177(6) 0.0673(10) 0.0071(7) 0.0575(8) C20 0.0450(6) -0.0030(5) 0.0172(5) 0.0433(6) -0.0010(5) 0.0383(5) C21 0.0564(7) -0.0067(6) 0.0206(5) 0.0555(8) -0.0043(6) 0.0398(6) C22 0.0657(9) -0.0038(7) 0.0122(6) 0.0564(8) 0.0023(6) 0.0403(6) C23 0.0535(7) -0.0016(6) 0.0178(5) 0.0550(8) -0.0049(6) 0.0412(6) C24 0.0485(7) 0.0010(7) 0.0124(5) 0.0685(10) 0.0058(6) 0.0418(6) C25 0.0682(10) -0.0147(9) 0.0197(9) 0.0738(12) 0.0072(10) 0.0803(12) C26 0.0572(9) 0.0169(10) 0.0270(8) 0.117(2) 0.0073(11) 0.0656(10) C30 0.0418(6) -0.0011(5) 0.0124(5) 0.0470(7) 0.0009(5) 0.0361(6) O31 0.0622(6) 0.0029(4) 0.0306(5) 0.0459(5) 0.0085(4) 0.0614(6) O32 0.0556(5) -0.0009(4) 0.0344(5) 0.0466(5) -0.0028(5) 0.0666(6)