#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/31/2003101.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_2003101 _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-Norleucine ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 N2 O4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 262.35 _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 10.012(2) _cell_length_b 4.7227(9) _cell_length_c 30.335(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.38(3) _cell_angle_gamma 90.00 _cell_volume 1419.1(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8192 _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 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Sheldrick (1996)' _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 0.986 _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 25110 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 40.41 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 49 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 14651 _reflns_number_observed 12393 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_obs 0.0482 _refine_ls_wR_factor_all 0.1183 _refine_ls_wR_factor_obs 0.1109 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_restrained_S_all 1.119 _refine_ls_restrained_S_obs 1.143 _refine_ls_number_reflns 14651 _refine_ls_number_parameters 399 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.2719P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.512 _refine_diff_density_min -0.262 _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 -0.2(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 0.57731(8) 0.3733(2) 0.03982(3) 0.01622(15) Uani d . 1 . O O2A 0.73624(7) 0.6764(2) 0.07098(3) 0.0190(2) Uani d . 1 . O N1A 0.37984(8) 0.7489(2) 0.04661(3) 0.01321(15) Uani d . 1 . N H1A 0.3439(18) 0.591(5) 0.0473(6) 0.024(5) Uiso d . 1 . H H2A 0.3208(16) 0.886(4) 0.0510(5) 0.017(4) Uiso d . 1 . H H3A 0.3986(16) 0.787(4) 0.0176(6) 0.024(4) Uiso d . 1 . H C1A 0.61585(10) 0.5921(2) 0.06153(3) 0.0126(2) Uani d . 1 . C C2A 0.50558(9) 0.7649(3) 0.07982(3) 0.0120(2) Uani d . 1 . C H4A 0.5331(5) 0.953(4) 0.08317(7) 0.014 Uiso calc R 1 . H C3A 0.48050(10) 0.6476(3) 0.12537(3) 0.0146(2) Uani d . 1 . C H5A 0.4680(2) 0.442(4) 0.12249(6) 0.018 Uiso calc R 1 . H C4A 0.60488(12) 0.7028(4) 0.16009(4) 0.0321(4) Uani d . 1 . C H6A 0.6145(8) 0.902(3) 0.1653(3) 0.048 Uiso calc R 1 . H H7A 0.6835(10) 0.632(3) 0.1493(2) 0.048 Uiso calc R 1 . H H8A 0.5942(6) 0.609(3) 0.1873(4) 0.048 Uiso calc R 1 . H C5A 0.35324(11) 0.7742(3) 0.14042(4) 0.0205(2) Uani d . 1 . C H9A 0.3627(2) 0.979(3) 0.14180(4) 0.025 Uiso calc R 1 . H H10A 0.2763(9) 0.7308(6) 0.1181(3) 0.025 Uiso calc R 1 . H C6A 0.32446(12) 0.6672(3) 0.18558(4) 0.0266(2) Uani d . 1 . C H11A 0.3267(12) 0.469(2) 0.18591(14) 0.040 Uiso calc R 1 . H H12A 0.2391(11) 0.729(2) 0.1904(2) 0.040 Uiso calc R 1 . H H13A 0.3899(10) 0.737(2) 0.2081(3) 0.040 Uiso calc R 1 . H O1B -0.06680(8) 0.3525(2) 0.46575(3) 0.01550(15) Uani d . 1 . O O2B -0.23338(7) 0.6571(2) 0.44202(3) 0.0189(2) Uani d . 1 . O N1B 0.12231(8) 0.7276(2) 0.44920(3) 0.0133(2) Uani d . 1 . N H1B 0.1562(19) 0.567(5) 0.4464(6) 0.027(5) Uiso d . 1 . H H2B 0.1737(16) 0.870(4) 0.4416(6) 0.015(4) Uiso d . 1 . H H3B 0.1147(19) 0.764(5) 0.4817(7) 0.041(5) Uiso d . 1 . H C1B -0.11286(10) 0.5720(2) 0.44573(3) 0.0118(2) Uani d . 1 . C C2B -0.01456(9) 0.7441(2) 0.42180(3) 0.0113(2) Uani d . 1 . C H4B -0.0425(5) 0.932(4) 0.41990(5) 0.014 Uiso calc R 1 . H C3B -0.01275(10) 0.6275(3) 0.37431(3) 0.0148(2) Uani d . 1 . C H5B 0.0019(3) 0.423(4) 0.37650(5) 0.018 Uiso calc R 1 . H C4B -0.14991(12) 0.6797(4) 0.34603(4) 0.0359(4) Uani d . 1 . C H6B -0.1635(6) 0.880(3) 0.3416(4) 0.054 Uiso calc R 1 . H H7B -0.2203(9) 0.604(3) 0.3611(3) 0.054 Uiso calc R 1 . H H8B -0.1523(5) 0.588(3) 0.3175(4) 0.054 Uiso calc R 1 . H C5B 0.10115(11) 0.7570(3) 0.35235(3) 0.0207(2) Uani d . 1 . C H9B 0.0884(2) 0.961(3) 0.35056(4) 0.025 Uiso calc R 1 . H H10B 0.1866(10) 0.7210(5) 0.3712(2) 0.025 Uiso calc R 1 . H C6B 0.10985(12) 0.6438(3) 0.30581(4) 0.0250(2) Uani d . 1 . C H11B 0.1158(11) 0.438(2) 0.30679(8) 0.038 Uiso calc R 1 . H H12B 0.1896(11) 0.721(2) 0.2953(2) 0.038 Uiso calc R 1 . H H13B 0.0297(10) 0.700(2) 0.2857(2) 0.038 Uiso calc R 1 . H O1C 0.06759(8) 0.5400(2) 0.03168(3) 0.01510(14) Uani d . 1 . O O2C 0.23620(7) 0.2430(2) 0.05654(3) 0.01771(15) Uani d . 1 . O N1C -0.12253(8) 0.1766(2) 0.05200(3) 0.0129(2) Uani d . 1 . N H1C -0.1598(17) 0.341(4) 0.0561(6) 0.018(4) Uiso d . 1 . H H2C -0.181(2) 0.041(5) 0.0608(7) 0.032(5) Uiso d . 1 . H H3C -0.1220(14) 0.149(4) 0.0222(5) 0.015(3) Uiso d . 1 . H C1C 0.11430(10) 0.3220(2) 0.05172(3) 0.0119(2) Uani d . 1 . C C2C 0.01808(9) 0.1480(2) 0.07577(3) 0.0117(2) Uani d . 1 . C H4C 0.0442(5) -0.046(4) 0.07606(3) 0.014 Uiso calc R 1 . H C3C 0.03029(10) 0.2567(3) 0.12376(3) 0.0156(2) Uani d . 1 . C H5C 0.1178(11) 0.2265(4) 0.1374(2) 0.019 Uiso calc R 1 . H H6C 0.0160(2) 0.450(2) 0.12287(3) 0.019 Uiso calc R 1 . H C4C -0.06530(11) 0.1248(3) 0.15284(3) 0.0188(2) Uani d . 1 . C H7C -0.1562(11) 0.1779(7) 0.14159(14) 0.023 Uiso calc R 1 . H H8C -0.05917(13) -0.077(3) 0.15141(4) 0.023 Uiso calc R 1 . H C5C -0.03172(12) 0.2200(3) 0.20110(3) 0.0252(2) Uani d . 1 . C H9C -0.02596(15) 0.424(3) 0.20195(4) 0.030 Uiso calc R 1 . H H10C 0.0555(11) 0.1459(10) 0.2133(2) 0.030 Uiso calc R 1 . H C6C -0.13517(13) 0.1242(4) 0.23011(4) 0.0290(3) Uani d . 1 . C H11C -0.1050(7) 0.178(2) 0.2608(3) 0.043 Uiso calc R 1 . H H12C -0.1450(9) -0.080(2) 0.2282(3) 0.043 Uiso calc R 1 . H H13C -0.2214(10) 0.213(2) 0.2198(3) 0.043 Uiso calc R 1 . H O1D 0.42787(8) 0.5241(2) 0.46106(3) 0.01604(15) Uani d . 1 . O O2D 0.26720(7) 0.2234(2) 0.43081(3) 0.0177(2) Uani d . 1 . O N1D 0.62596(8) 0.1515(2) 0.45482(3) 0.0139(2) Uani d . 1 . N H1D 0.6611(16) 0.327(4) 0.4528(5) 0.016(4) Uiso d . 1 . H H2D 0.687(2) 0.018(5) 0.4478(6) 0.031(5) Uiso d . 1 . H H3D 0.6124(16) 0.124(5) 0.4847(6) 0.026(4) Uiso d . 1 . H C1D 0.38825(10) 0.3031(2) 0.44027(3) 0.0122(2) Uani d . 1 . C C2D 0.49752(9) 0.1216(3) 0.42342(3) 0.0122(2) Uani d . 1 . C H4D 0.4708(5) -0.067(4) 0.42251(4) 0.015 Uiso calc R 1 . H C3D 0.52239(10) 0.2135(3) 0.37671(3) 0.0163(2) Uani d . 1 . C H5D 0.5325(2) 0.413(2) 0.37625(3) 0.020 Uiso calc R 1 . H H6D 0.6042(10) 0.1315(10) 0.37055(8) 0.020 Uiso calc R 1 . H C4D 0.40807(11) 0.1269(3) 0.34040(3) 0.0215(2) Uani d . 1 . C H7D 0.3249(10) 0.1967(9) 0.34805(10) 0.026 Uiso calc R 1 . H H8D 0.40265(13) -0.075(3) 0.33955(4) 0.026 Uiso calc R 1 . H C5D 0.42415(12) 0.2348(3) 0.29394(4) 0.0258(2) Uani d . 1 . C H9D 0.3457(10) 0.1742(8) 0.2729(3) 0.031 Uiso calc R 1 . H H10D 0.42458(12) 0.442(3) 0.29441(4) 0.031 Uiso calc R 1 . H C6D 0.55160(13) 0.1324(4) 0.27712(4) 0.0343(3) Uani d . 1 . C H11D 0.6301(10) 0.216(2) 0.2951(4) 0.052 Uiso calc R 1 . H H12D 0.5493(6) 0.189(3) 0.2462(4) 0.052 Uiso calc R 1 . H H13D 0.5569(7) -0.073(3) 0.2793(4) 0.052 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 0.0166(3) 0.0156(4) 0.0173(3) 0.0006(3) 0.0054(3) -0.0029(3) O2A 0.0104(3) 0.0182(4) 0.0290(4) -0.0010(3) 0.0054(3) -0.0001(3) N1A 0.0110(3) 0.0145(4) 0.0144(3) 0.0013(3) 0.0030(2) 0.0021(3) C1A 0.0117(4) 0.0119(4) 0.0149(4) 0.0013(3) 0.0047(3) 0.0018(3) C2A 0.0098(3) 0.0119(4) 0.0146(3) 0.0002(3) 0.0032(3) 0.0006(3) C3A 0.0137(4) 0.0164(4) 0.0140(3) 0.0008(4) 0.0031(3) 0.0004(4) C4A 0.0186(4) 0.0600(11) 0.0169(4) -0.0019(6) -0.0003(3) 0.0016(6) C5A 0.0192(4) 0.0245(5) 0.0199(4) 0.0027(4) 0.0098(3) 0.0010(4) C6A 0.0250(5) 0.0404(7) 0.0162(4) -0.0048(5) 0.0090(3) -0.0015(5) O1B 0.0161(3) 0.0147(4) 0.0163(3) 0.0005(3) 0.0046(3) 0.0031(3) O2B 0.0109(3) 0.0178(4) 0.0294(4) 0.0007(3) 0.0075(3) 0.0011(4) N1B 0.0099(3) 0.0153(4) 0.0149(3) -0.0011(3) 0.0025(2) -0.0015(3) C1B 0.0111(4) 0.0115(4) 0.0135(3) -0.0013(3) 0.0042(3) -0.0018(3) C2B 0.0090(3) 0.0113(4) 0.0140(3) -0.0001(3) 0.0028(3) 0.0009(3) C3B 0.0135(3) 0.0177(4) 0.0133(3) -0.0016(4) 0.0029(3) -0.0009(4) C4B 0.0170(4) 0.0717(11) 0.0182(4) -0.0009(6) -0.0001(3) -0.0027(6) C5B 0.0216(4) 0.0261(5) 0.0157(4) -0.0065(5) 0.0079(3) -0.0027(4) C6B 0.0224(5) 0.0379(6) 0.0159(4) -0.0006(5) 0.0067(3) -0.0013(5) O1C 0.0151(3) 0.0138(3) 0.0171(3) 0.0011(3) 0.0043(2) 0.0025(3) O2C 0.0103(3) 0.0162(4) 0.0276(4) 0.0015(3) 0.0059(2) 0.0019(3) N1C 0.0103(3) 0.0149(4) 0.0138(3) -0.0014(3) 0.0027(2) -0.0010(3) C1C 0.0108(3) 0.0122(4) 0.0132(3) -0.0007(3) 0.0034(3) -0.0014(3) C2C 0.0104(3) 0.0116(4) 0.0136(3) -0.0003(3) 0.0033(3) -0.0002(3) C3C 0.0153(4) 0.0186(5) 0.0134(3) -0.0030(4) 0.0033(3) -0.0015(4) C4C 0.0191(4) 0.0237(5) 0.0147(4) -0.0035(4) 0.0057(3) -0.0011(4) C5C 0.0251(5) 0.0370(6) 0.0144(4) -0.0053(5) 0.0060(3) -0.0031(4) C6C 0.0280(5) 0.0445(7) 0.0161(4) -0.0034(6) 0.0087(4) 0.0005(5) O1D 0.0164(3) 0.0137(3) 0.0186(3) -0.0005(3) 0.0046(3) -0.0035(3) O2D 0.0106(3) 0.0179(4) 0.0253(3) -0.0007(3) 0.0049(2) -0.0024(3) N1D 0.0108(3) 0.0149(4) 0.0163(3) 0.0016(3) 0.0027(2) 0.0015(3) C1D 0.0110(3) 0.0130(4) 0.0132(3) 0.0002(3) 0.0040(3) 0.0013(3) C2D 0.0108(3) 0.0118(4) 0.0144(3) 0.0001(4) 0.0031(3) -0.0004(3) C3D 0.0138(4) 0.0217(5) 0.0142(3) -0.0012(4) 0.0051(3) -0.0008(4) C4D 0.0161(4) 0.0328(6) 0.0159(4) -0.0026(4) 0.0035(3) 0.0000(4) C5D 0.0227(5) 0.0398(7) 0.0154(4) 0.0013(5) 0.0039(3) 0.0017(4) C6D 0.0265(5) 0.0592(9) 0.0191(4) -0.0020(6) 0.0093(4) -0.0048(6) _cod_database_code 2003101