#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2000169.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_2000169 _journal_name_full 'Acta Cryst. C' _journal_year 1991 _journal_volume 47 _journal_page_first 2276 _journal_page_last 2277 _publ_section_title ; trans-3-Benzoyl-2-(tert-butyl)-4-(iso-butyl)-1,3-oxazolidin-5-one ; loop_ _publ_author_name 'Willis, Anthony C.' 'Beckwith, Athelstan L.J.' 'Tozer, Matthew J.' _chemical_name_systematic trans-3-Benzoyl-2-(tert-butyl)-4-(iso-butyl)-1,3-oxazolidin-5-one _chemical_formula_moiety 'C18 H25 N O3' _chemical_formula_sum 'C18 H25 N O3' _chemical_formula_weight 303.40 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall P_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 5.9590(10) _cell_length_b 14.9560(10) _cell_length_c 19.737(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1759.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 31 _cell_measurement_temperature 293 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_meas ? _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.59 _exptl_absorpt_correction_type 'shelx76 gaussian' _exptl_absorpt_correction_T_min .933 _exptl_absorpt_correction_T_max .824 _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Philips PW1100/20 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_reflns_number 1592 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI .027 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 61.97 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_reduction_process ? _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 2 4 1 9 1 3 0 10 _reflns_number_total 1592 _reflns_number_observed 1408 _reflns_observed_criterion refl_observed_if_F_>_6.0_sigma(F) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all .038 _refine_ls_R_factor_obs .034 _refine_ls_wR_factor_all .044 _refine_ls_wR_factor_obs .042 _refine_ls_goodness_of_fit_all 1.462 _refine_ls_goodness_of_fit_obs 1.515 _refine_ls_number_reflns 1408 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment 'refxyz except H332B noref' _refine_ls_weighting_scheme 'calc w=1/(\s^2^(F)+0.0004F^2^)' _refine_ls_shift/esd_max .535 _refine_ls_shift/esd_mean .044 _refine_diff_density_max .131 _refine_diff_density_min -.108 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 351E1(4) _refine_ls_abs_structure_details ; The absolute configuration was assigned to agree with the known chirality at C3 arising from its precursor l-leucine. ; _refine_ls_abs_structure_Flack 0 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C .017 .009 International_Tables_Vol_IV_Table_2.2B H 0 0 International_Tables_Vol_IV_Table_2.2B O .047 .032 International_Tables_Vol_IV_Table_2.2B N .029 .018 International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom O1 .4154(4) .56990(10) .3026000 .0600(10) Uani ? ? C2 .5630(5) .5087(2) .32460(10) .060(2) Uani ? ? C3 .5350(5) .4920(2) .39970(10) .0480(10) Uani ? ? N4 .3570(3) .55580(10) .4167000 .0390(10) Uani ? ? C5 .3000(5) .6122(2) .35810(10) .0450(10) Uani ? ? O21 .6958(5) .4738(2) .28740(10) .090(2) Uani ? ? C31 .4869(6) .3929(2) .4143(2) .059(2) Uani ? ? C32 .2552(7) .3558(2) .3953(2) .073(2) Uani ? ? C321 .2090(10) .3542(4) .3211(3) .111(4) Uani ? ? C322 .2300(10) .2626(3) .4264(3) .149(5) Uani ? ? C41 .2034(4) .5476(2) .46820(10) .0410(10) Uani ? ? O41 .0124(3) .57760(10) .4624000 .0540(10) Uani ? ? C411 .2826(4) .5093(2) .53340(10) .0430(10) Uani ? ? C412 .1315(5) .4613(2) .57250(10) .064(2) Uani ? ? C413 .1914(7) .4324(3) .6366(2) .086(2) Uani ? ? C414 .3987(6) .4522(3) .66200(10) .078(2) Uani ? ? C415 .5494(6) .4997(2) .62410(10) .065(2) Uani ? ? C416 .4920(5) .5279(2) .55940(10) .053(2) Uani ? ? C51 .3745(5) .7097(2) .36340(10) .052(2) Uani ? ? C511 .6299(6) .7166(3) .3669(2) .072(2) Uani ? ? C512 .2881(8) .7581(3) .3000(2) .079(2) Uani ? ? C513 .2757(7) .7522(2) .4267(2) .068(2) Uani ? ? H3 .679(5) .510(2) .4220(10) .06000 Uiso ? ? H5 .135(5) .608(2) .3500(10) .06000 Uiso ? ? H31A .507(5) .381(2) .461(2) .07000 Uiso ? ? H31B .593(6) .357(2) .390(2) .07000 Uiso ? ? H32 .129(6) .401(3) .417(2) .09000 Uiso ? ? H321A .330(9) .311(4) .306(3) .14000 Uiso ? ? H321B .220(10) .415(4) .298(2) .14000 Uiso ? ? H321C .040(10) .318(3) .320(2) .14000 Uiso ? ? H322A .250(10) .272(4) .475(3) .19000 Uiso ? ? H322B .34976 .22118 .40954 .19000 Uiso calc C322 H322C .080(10) .234(4) .397(3) .19000 Uiso ? ? H412 -.007(6) .447(2) .552(2) .08000 Uiso ? ? H513B .115(7) .757(3) .426(2) .09000 Uiso ? ? H513C .329(6) .817(2) .430(2) .09000 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 .0710(10) .0760(10) .0342(9) .0080(10) .0051(9) -.0030(9) C2 .060(2) .072(2) .0470(10) .002(2) .0130(10) -.0090(10) C3 .0380(10) .060(2) .0440(10) .0070(10) .0010(10) -.0050(10) N4 .0370(10) .0480(10) .0325(9) .0025(9) .0011(9) -.0011(9) C5 .0430(10) .0600(10) .0320(10) .0010(10) -.0010(10) .0010(10) O21 .094(2) .109(2) .0680(10) .023(2) .0380(10) -.0100(10) C31 .061(2) .056(2) .060(2) .015(2) .005(2) -.0020(10) C32 .075(2) .057(2) .087(2) -.005(2) .002(2) -.018(2) C321 .100(4) .127(4) .107(3) -.026(3) -.027(3) -.016(3) C322 .192(7) .084(3) .171(5) -.046(4) -.027(6) .017(3) C41 .0370(10) .0460(10) .0400(10) -.0040(10) .0010(10) -.0050(10) O41 .0360(9) .0710(10) .0540(10) .0066(9) .0028(8) .0015(9) C411 .0420(10) .0540(10) .0340(10) .0000(10) .0020(10) -.0030(10) C412 .048(2) .098(2) .0450(10) -.016(2) .0030(10) .007(2) C413 .074(2) .133(3) .052(2) -.022(2) .008(2) .031(2) C414 .075(2) .118(3) .040(2) -.002(2) -.004(2) .014(2) C415 .057(2) .096(2) .043(2) -.003(2) -.0080(10) -.0030(10) C416 .049(2) .069(2) .0410(10) -.010(2) -.0010(10) -.0020(10) C51 .048(2) .059(2) .0490(10) .0020(10) .0000(10) .0070(10) C511 .048(2) .071(2) .097(3) -.008(2) -.003(2) .010(2) C512 .078(2) .083(2) .075(2) .009(2) -.005(2) .033(2) C513 .074(2) .055(2) .075(2) .004(2) .001(2) -.010(2)