#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/37/2203711.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_2203711 loop_ _publ_author_name 'Netland, Kjetil Andreas' 'Andresen, Kim' 'G\"orbitz, Carl Henrik' 'Dalhus, Bj\/orn' _publ_section_title ; L-Alanyl-L-threonine ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o951 _journal_page_last o953 _journal_paper_doi 10.1107/S1600536804010578 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C7 H14 N2 O4' _chemical_formula_moiety 'C7 H14 N2 O4' _chemical_formula_sum 'C7 H14 N2 O4' _chemical_formula_weight 190.20 _chemical_name_systematic ; L-Alanyl-L-threonine ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.03990(10) _cell_length_b 9.7642(2) _cell_length_c 14.6820(4) _cell_measurement_reflns_used 8870 _cell_measurement_temperature 105(2) _cell_measurement_theta_max 35.0 _cell_measurement_theta_min 2.5 _cell_volume 865.87(3) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 105(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'Sets of exposures each taken over 0.3\% \w rotation' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11596 _diffrn_reflns_theta_full 34.99 _diffrn_reflns_theta_max 34.99 _diffrn_reflns_theta_min 2.51 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 408 _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.349 _refine_diff_density_min -0.187 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 2171 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.142 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0272 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0543P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.0753 _reflns_number_gt 2087 _reflns_number_total 2171 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6458.cif _cod_data_source_block I _cod_database_code 2203711 _cod_database_fobs_code 2203711 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 0.31462(11) 0.49629(10) 0.54567(5) 0.02228(15) Uani d . 1 O O2 -0.08708(10) 0.49939(7) 0.76669(4) 0.01676(12) Uani d . 1 O H5 -0.072(3) 0.5633(15) 0.8033(12) 0.025 Uiso d . 1 H O3 0.52447(11) 0.66402(7) 0.84564(4) 0.01663(12) Uani d . 1 O O4 0.15799(12) 0.69214(6) 0.86230(4) 0.01559(12) Uani d . 1 O N1 0.69505(12) 0.35868(8) 0.49325(5) 0.01407(12) Uani d . 1 N H1 0.712(3) 0.2794(15) 0.5309(10) 0.021 Uiso d . 1 H H2 0.807(3) 0.3587(17) 0.4490(11) 0.021 Uiso d . 1 H H3 0.565(3) 0.3539(17) 0.4639(11) 0.021 Uiso d . 1 H N2 0.48439(12) 0.54476(7) 0.68085(5) 0.01240(12) Uani d . 1 N H4 0.607(3) 0.5429(14) 0.7105(10) 0.015 Uiso d . 1 H C1 0.71079(13) 0.48608(9) 0.54955(5) 0.01445(14) Uani d . 1 C H11 0.821(3) 0.4768(15) 0.5950(10) 0.017 Uiso d . 1 H C2 0.77358(17) 0.60742(10) 0.48943(6) 0.01910(16) Uani d . 1 C H21 0.9193 0.5942 0.4660 0.029 Uiso calc R 1 H H22 0.7694 0.6896 0.5246 0.029 Uiso calc R 1 H H23 0.6713 0.6144 0.4401 0.029 Uiso calc R 1 H C3 0.48312(13) 0.50811(9) 0.59271(5) 0.01406(13) Uani d . 1 C C4 0.28098(13) 0.58214(8) 0.72729(5) 0.01114(12) Uani d . 1 C H41 0.2001 0.6457 0.6890 0.013 Uiso calc R 1 H C5 0.13295(12) 0.45530(8) 0.74426(5) 0.01227(13) Uani d . 1 C H51 0.1256 0.4057 0.6903 0.015 Uiso calc R 1 H C6 0.22662(15) 0.36179(8) 0.81750(6) 0.01552(14) Uani d . 1 C H61 0.1400 0.2796 0.8206 0.023 Uiso calc R 1 H H62 0.2221 0.4077 0.8752 0.023 Uiso calc R 1 H H63 0.3769 0.3390 0.8029 0.023 Uiso calc R 1 H C7 0.32871(13) 0.65284(8) 0.81904(5) 0.01180(12) Uani d . 1 C 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 0.0123(2) 0.0435(4) 0.0110(2) 0.0042(3) -0.0026(2) -0.0045(3) O2 0.0096(2) 0.0250(3) 0.0157(2) 0.0011(2) -0.0001(2) -0.0037(2) O3 0.0162(3) 0.0216(3) 0.0120(2) -0.0018(2) -0.0036(2) -0.0011(2) O4 0.0182(3) 0.0162(2) 0.0123(2) 0.0015(2) 0.0036(2) -0.0029(2) N1 0.0137(3) 0.0183(3) 0.0103(2) 0.0023(2) 0.0019(2) 0.0015(2) N2 0.0105(2) 0.0184(3) 0.0083(2) 0.0009(2) 0.0001(2) -0.0015(2) C1 0.0113(3) 0.0223(3) 0.0097(3) 0.0016(3) 0.0006(2) -0.0015(2) C2 0.0194(4) 0.0208(3) 0.0172(3) -0.0035(3) 0.0032(3) -0.0021(3) C3 0.0114(3) 0.0220(3) 0.0088(3) 0.0027(3) 0.0005(2) -0.0007(2) C4 0.0108(3) 0.0145(3) 0.0081(3) 0.0013(2) 0.0003(2) -0.0008(2) C5 0.0102(3) 0.0159(3) 0.0108(3) 0.0000(2) 0.0000(2) -0.0029(2) C6 0.0167(3) 0.0138(3) 0.0161(3) -0.0001(3) -0.0003(3) 0.0006(3) C7 0.0152(3) 0.0115(2) 0.0086(3) -0.0002(2) -0.0001(2) 0.0001(2) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C5 O2 H5 105.8(14) C1 N1 H1 110.3(9) C1 N1 H2 109.7(10) H1 N1 H2 108.9(14) C1 N1 H3 111.4(11) H1 N1 H3 109.3(14) H2 N1 H3 107.3(13) C3 N2 C4 120.99(7) C3 N2 H4 119.1(10) C4 N2 H4 119.8(10) N1 C1 C2 109.99(7) N1 C1 C3 106.78(7) C2 C1 C3 110.73(7) N1 C1 H11 110.8(9) C2 C1 H11 107.8(9) C3 C1 H11 110.8(9) C1 C2 H21 109.5 C1 C2 H22 109.5 H21 C2 H22 109.5 C1 C2 H23 109.5 H21 C2 H23 109.5 H22 C2 H23 109.5 O1 C3 N2 124.64(8) O1 C3 C1 119.74(7) N2 C3 C1 115.58(7) N2 C4 C7 111.40(6) N2 C4 C5 111.30(6) C7 C4 C5 109.02(6) N2 C4 H41 108.3 C7 C4 H41 108.3 C5 C4 H41 108.3 O2 C5 C6 111.25(7) O2 C5 C4 109.38(6) C6 C5 C4 112.31(6) O2 C5 H51 107.9 C6 C5 H51 107.9 C4 C5 H51 107.9 C5 C6 H61 109.5 C5 C6 H62 109.5 H61 C6 H62 109.5 C5 C6 H63 109.5 H61 C6 H63 109.5 H62 C6 H63 109.5 O3 C7 O4 125.82(7) O3 C7 C4 119.29(7) O4 C7 C4 114.87(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C3 1.2353(10) O2 C5 1.4352(10) O2 H5 0.828(16) O3 C7 1.2500(10) O4 C7 1.2704(10) N1 C1 1.4966(11) N1 H1 0.957(16) N1 H2 0.937(17) N1 H3 0.895(18) N2 C3 1.3427(10) N2 C4 1.4517(10) N2 H4 0.860(16) C1 C2 1.5254(13) C1 C3 1.5292(11) C1 H11 0.949(16) C2 H21 0.9540 C2 H22 0.9540 C2 H23 0.9540 C4 C7 1.5409(10) C4 C5 1.5477(11) C4 H41 0.9699 C5 C6 1.5199(11) C5 H51 0.9301 C6 H61 0.9586 C6 H62 0.9586 C6 H63 0.9586 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O4 3_646 0.957(16) 1.950(16) 2.8160(10) 149.5(14) y N1 H2 O3 2_664 0.937(18) 1.842(17) 2.7597(9) 166.0(15) y N1 H3 O4 2_564 0.895(18) 2.061(17) 2.9137(10) 158.9(15) y N2 H4 O2 1_655 0.860(16) 2.067(16) 2.9127(9) 167.6(13) y O2 H5 O4 1_555 0.828(16) 2.065(18) 2.7756(10) 143.6(18) y 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 N1 C1 C3 N2 136.81(7) yes C1 C3 N2 C4 173.74(7) yes C3 N2 C4 C7 -166.22(7) yes N2 C4 C7 O3 -3.67(10) yes N2 C4 C5 C6 71.62(8) yes N2 C4 C5 O2 -164.34(6) yes C4 C5 O2 H5 -44.0(11) yes C7 C4 C5 C6 -51.65(8) ? C7 C4 C5 O2 72.38(8) ? C4 N2 C3 O1 -3.75(14) ? N1 C1 C3 O1 -45.57(11) ? C2 C1 C3 O1 74.16(10) ? C2 C1 C3 N2 -103.47(9) ? C3 N2 C4 C5 71.88(9) ? C5 C4 C7 O3 119.55(8) ? N2 C4 C7 O4 178.01(7) ? C5 C4 C7 O4 -58.77(8) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 4932422 2 PubChem 7006473