#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/31/2003103.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_2003103 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 424 _journal_page_last 431 _chemical_name_systematic ; L-Isoleucine:D-Valine ; _chemical_name_common ? _chemical_formula_moiety 'C6 H13 N1 O2,C5 H11 N1 O2' _chemical_formula_sum 'C11 H24 N2 O4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 248.32 _chemical_melting_point ? _symmetry_cell_setting monoclinic _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.25280(10) _cell_length_b 23.9809(6) _cell_length_c 5.42000(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.4200(10) _cell_angle_gamma 90.00 _cell_volume 639.84(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6101 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 150(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Sheldrick (1996)' _exptl_absorpt_correction_T_min 0.939 _exptl_absorpt_correction_T_max 0.990 _diffrn_ambient_temperature 150(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD area-detector diffractometer' _diffrn_measurement_method '\w' _diffrn_reflns_number 10296 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 40.26 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 6854 _reflns_number_observed 6220 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_obs 0.0458 _refine_ls_wR_factor_all 0.1114 _refine_ls_wR_factor_obs 0.1066 _refine_ls_goodness_of_fit_all 1.140 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_restrained_S_all 1.140 _refine_ls_restrained_S_obs 1.145 _refine_ls_number_reflns 6854 _refine_ls_number_parameters 191 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.1323P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.252 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(6) 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' 'N' 'N' 0.0061 0.0033 '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' 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol O1A 0.8903(2) 0.22269(4) 0.59890(14) 0.01742(14) Uani d . 1 . O O2A 0.4438(2) 0.20401(4) 0.4632(2) 0.01708(13) Uani d . 1 . O N1A 0.9007(2) 0.22898(4) 0.1102(2) 0.01386(13) Uani d . 1 . N H2A 0.888(4) 0.2268(8) -0.071(4) 0.022(4) Uiso d . 1 . H H3A 0.889(4) 0.2642(8) 0.142(4) 0.016(4) Uiso d . 1 . H H1A 1.059(4) 0.2167(8) 0.219(4) 0.019(4) Uiso d . 1 . H C1A 0.6663(2) 0.20966(4) 0.4264(2) 0.01249(14) Uani d . 1 . C C2A 0.6661(2) 0.19912(4) 0.1459(2) 0.01233(14) Uani d . 1 . C H4A 0.489(3) 0.2156(3) 0.014(2) 0.015 Uiso calc R 1 . H C3A 0.6767(2) 0.13645(4) 0.0817(2) 0.01466(15) Uani d . 1 . C H5A 0.7435(13) 0.13369(6) -0.068(3) 0.018 Uiso calc R 1 . H C4A 0.8768(2) 0.10439(5) 0.3132(2) 0.0215(2) Uani d . 1 . C H6A 1.045(3) 0.1252(4) 0.3831(19) 0.032 Uiso calc R 1 . H H7A 0.913(2) 0.0681(5) 0.2531(10) 0.032 Uiso calc R 1 . H H8A 0.7989(15) 0.0996(5) 0.450(2) 0.032 Uiso calc R 1 . H C5A 0.3918(2) 0.11065(5) -0.0075(3) 0.0225(2) Uani d . 1 . C H9A 0.3326(10) 0.10831(6) 0.140(2) 0.027 Uiso calc R 1 . H H10A 0.2685(19) 0.1346(4) -0.136(2) 0.027 Uiso calc R 1 . H C6A 0.3818(3) 0.05255(6) -0.1264(3) 0.0336(3) Uani d . 1 . C H11A 0.199(3) 0.0393(3) -0.188(3) 0.050 Uiso calc R 1 . H H12A 0.493(3) 0.0277(4) 0.005(2) 0.050 Uiso calc R 1 . H H13A 0.447(3) 0.05435(13) -0.270(3) 0.050 Uiso calc R 1 . H O1B 0.3033(2) 0.32034(4) 0.13077(15) 0.01766(14) Uani d . 1 . O O2B 0.7500(2) 0.33844(3) 0.2660(2) 0.01739(14) Uani d . 1 . O N1B 0.2935(2) 0.31423(4) 0.6203(2) 0.01439(13) Uani d . 1 . N H2B 0.291(4) 0.3171(9) 0.783(4) 0.027(5) Uiso d . 1 . H H1B 0.131(4) 0.3273(9) 0.512(4) 0.024(4) Uiso d . 1 . H H3B 0.305(4) 0.2782(9) 0.587(4) 0.028(5) Uiso d . 1 . H C1B 0.5272(2) 0.33311(4) 0.3032(2) 0.01265(14) Uani d . 1 . C C2B 0.5281(2) 0.34390(4) 0.5837(2) 0.01315(14) Uani d . 1 . C H4B 0.686(3) 0.3293(3) 0.702(2) 0.016 Uiso calc R 1 . H C3B 0.5175(2) 0.40683(4) 0.6446(2) 0.0179(2) Uani d . 1 . C H5B 0.4561(12) 0.41015(8) 0.795(3) 0.021 Uiso calc R 1 . H C4B 0.8006(3) 0.43227(7) 0.7244(3) 0.0331(3) Uani d . 1 . C H6B 0.926(2) 0.4112(5) 0.874(3) 0.050 Uiso calc R 1 . H H7B 0.7936(7) 0.4716(6) 0.776(3) 0.050 Uiso calc R 1 . H H8B 0.8658(17) 0.4305(6) 0.574(3) 0.050 Uiso calc R 1 . H C5B 0.3160(3) 0.43878(5) 0.4146(3) 0.0251(2) Uani d . 1 . C H9B 0.145(3) 0.4198(4) 0.356(2) 0.038 Uiso calc R 1 . H H10B 0.3846(16) 0.4409(5) 0.273(2) 0.038 Uiso calc R 1 . H H11B 0.292(2) 0.4756(6) 0.4708(11) 0.038 Uiso calc R 1 . H 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 O1A 0.0159(3) 0.0258(4) 0.0107(3) -0.0034(3) 0.0048(2) -0.0027(2) O2A 0.0142(3) 0.0233(3) 0.0165(3) 0.0008(3) 0.0089(2) -0.0002(3) N1A 0.0151(3) 0.0174(3) 0.0102(3) -0.0028(3) 0.0059(2) -0.0008(2) C1A 0.0139(3) 0.0144(4) 0.0106(3) 0.0009(3) 0.0060(3) 0.0002(3) C2A 0.0129(3) 0.0151(3) 0.0098(3) -0.0001(3) 0.0050(2) 0.0000(3) C3A 0.0163(4) 0.0150(4) 0.0138(4) -0.0004(3) 0.0066(3) -0.0020(3) C4A 0.0217(5) 0.0203(5) 0.0216(5) 0.0036(4) 0.0064(4) 0.0015(4) C5A 0.0188(4) 0.0224(5) 0.0252(5) -0.0047(4) 0.0064(4) -0.0054(4) C6A 0.0389(7) 0.0207(5) 0.0336(6) -0.0069(5) 0.0033(5) -0.0052(5) O1B 0.0167(3) 0.0258(4) 0.0113(3) -0.0040(3) 0.0058(2) -0.0027(2) O2B 0.0160(3) 0.0229(4) 0.0164(3) 0.0011(3) 0.0096(2) 0.0003(3) N1B 0.0165(3) 0.0171(3) 0.0108(3) -0.0026(3) 0.0064(3) -0.0008(3) C1B 0.0155(3) 0.0131(3) 0.0108(3) 0.0008(3) 0.0065(3) -0.0004(3) C2B 0.0137(3) 0.0171(4) 0.0092(3) -0.0011(3) 0.0048(2) -0.0013(3) C3B 0.0207(4) 0.0181(4) 0.0179(4) -0.0037(3) 0.0106(3) -0.0046(3) C4B 0.0284(6) 0.0336(7) 0.0393(7) -0.0162(5) 0.0143(5) -0.0161(6) C5B 0.0315(6) 0.0179(5) 0.0295(6) 0.0041(4) 0.0151(5) 0.0040(4) _cod_database_code 2003103