#------------------------------------------------------------------------------ #$Date: 2017-10-13 07:09:21 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201973 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/05/2200507.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_2200507 loop_ _publ_author_name 'Subha Nandhini, M.' 'Krishnakumar, R. V.' 'S. Natarajan' _publ_section_title ; L-Alaninium oxalate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o633 _journal_page_last o635 _journal_paper_doi 10.1107/S1600536801010042 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C3 H8 N1 O2 1+, C2 H1 O4 1-' _chemical_formula_moiety 'C3 H8 N1 O2 1+, C2 H1 O4 1-' _chemical_formula_sum 'C5 H9 N O6' _chemical_formula_weight 179.13 _chemical_name_systematic ; L-alaninium oxalate ; _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' _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 5.6304(15) _cell_length_b 7.2353(15) _cell_length_c 19.597(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68 _cell_measurement_theta_min 4 _cell_volume 798.3(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 Software' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf-Nonius sealed tube' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0116 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 879 _diffrn_reflns_theta_full 67.91 _diffrn_reflns_theta_max 67.91 _diffrn_reflns_theta_min 4.51 _diffrn_standards_decay_% .1 _diffrn_standards_interval_count 25 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.229 _exptl_absorpt_correction_T_max .87 _exptl_absorpt_correction_T_min .79 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_meas 1.49 _exptl_crystal_density_method 'flotation in a mixture of carbon tetrachloride and bromoform' _exptl_crystal_description needle _exptl_crystal_F_000 376 _exptl_crystal_size_max .2 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .11 _refine_diff_density_max .143 _refine_diff_density_min -.143 _refine_ls_abs_structure_details 'see text' _refine_ls_extinction_coef .040(3) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 879 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all .0312 _refine_ls_R_factor_gt .0304 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.1739P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0826 _reflns_number_gt 853 _reflns_number_total 879 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob6056.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 798.3(2) _cod_database_code 2200507 _cod_database_fobs_code 2200507 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 .2644(3) .8562(2) .10946(7) .0359(4) Uani d . 1 . . N H1A .1867 .8789 .1481 .054 Uiso calc R 1 . . H H1B .4196 .8708 .1163 .054 Uiso calc R 1 . . H H1C .2356 .7408 .0962 .054 Uiso calc R 1 . . H O1 .1991(3) .9924(3) -.06326(7) .0511(5) Uani d . 1 . . O H1 .2798 .9719 -.0973 .077 Uiso calc R 1 . . H O2 .5153(3) .8816(2) -.00816(7) .0411(4) Uani d . 1 . . O O3 .4157(3) .5324(4) .21396(8) .0623(7) Uani d . 1 . . O H3 .5443 .5063 .2311 .093 Uiso calc R 1 . . H O4 .2719(3) .4667(3) .31722(7) .0489(5) Uani d . 1 . . O O5 -.0096(3) .5505(2) .16329(6) .0410(4) Uani d . 1 . . O O6 -.1695(3) .4814(4) .26207(8) .0760(8) Uani d . 1 . . O C1 .3174(3) .9450(3) -.00888(9) .0322(5) Uani d . 1 . . C C2 .1832(4) .9866(3) .05590(9) .0342(5) Uani d . 1 . . C H2 .0125 .9702 .0481 .041 Uiso calc R 1 . . H C3 .2320(7) 1.1841(3) .07866(13) .0664(9) Uani d . 1 . . C H3A .1459 1.2093 .1199 .100 Uiso calc R 1 . . H H3B .1820 1.2683 .0436 .100 Uiso calc R 1 . . H H3C .3990 1.1993 .0868 .100 Uiso calc R 1 . . H C4 .2478(4) .5021(4) .25784(10) .0344(4) Uani d . 1 . . C C5 .0000(3) .5137(3) .22394(9) .0314(5) 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 N1 .0392(10) .0462(9) .0223(7) -.0056(9) .0030(7) -.0009(7) O1 .0435(9) .0828(12) .0269(7) .0179(11) .0048(6) .0122(8) O2 .0390(8) .0535(8) .0308(7) .0133(7) .0067(6) .0025(7) O3 .0209(7) .1291(19) .0369(8) .0020(11) .0013(6) .0228(11) O4 .0315(7) .0865(12) .0286(7) .0002(9) -.0048(6) .0114(7) O5 .0320(7) .0665(10) .0246(6) -.0041(8) -.0033(6) .0080(6) O6 .0203(7) .172(2) .0361(8) -.0033(13) .0015(6) .0402(12) C1 .0353(10) .0340(9) .0271(9) .0027(8) .0044(8) .0029(8) C2 .0350(10) .0404(10) .0273(9) .0051(11) .0042(8) -.0018(8) C3 .105(3) .0392(11) .0552(14) .0083(17) .0140(18) -.0081(11) C4 .0212(8) .0548(11) .0273(9) -.0004(9) -.0006(8) .0063(9) C5 .0222(9) .0469(11) .0252(8) -.0011(10) -.0007(7) .0060(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 '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 _geom_angle_publ_flag C2 N1 H1A 109.5 ? C2 N1 H1B 109.5 ? H1A N1 H1B 109.5 ? C2 N1 H1C 109.5 ? H1A N1 H1C 109.5 ? H1B N1 H1C 109.5 ? C1 O1 H1 109.5 ? C4 O3 H3 109.5 ? O2 C1 O1 125.65(18) no O2 C1 C2 121.97(18) no O1 C1 C2 112.32(17) no N1 C2 C1 108.33(16) no N1 C2 C3 109.50(18) no C1 C2 C3 110.07(19) no N1 C2 H2 109.6 ? C1 C2 H2 109.6 ? C3 C2 H2 109.6 ? C2 C3 H3A 109.5 ? C2 C3 H3B 109.5 ? H3A C3 H3B 109.5 ? C2 C3 H3C 109.5 ? H3A C3 H3C 109.5 ? H3B C3 H3C 109.5 ? O4 C4 O3 126.7(2) no O4 C4 C5 122.01(18) no O3 C4 C5 111.32(15) no O5 C5 O6 126.65(19) no O5 C5 C4 118.05(17) no O6 C5 C4 115.29(15) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 . 1.483(3) yes N1 H1A . .8900 ? N1 H1B . .8900 ? N1 H1C . .8900 ? O1 C1 . 1.303(2) yes O1 H1 . .8200 ? O2 C1 . 1.205(2) yes O3 C4 . 1.297(2) yes O3 H3 . .8200 ? O4 C4 . 1.199(2) yes O5 C5 . 1.219(2) yes O6 C5 . 1.235(2) yes C1 C2 . 1.508(3) yes C2 C3 . 1.522(3) yes C2 H2 . .9800 ? C3 H3A . .9600 ? C3 H3B . .9600 ? C3 H3C . .9600 ? C4 C5 . 1.548(3) yes 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 N1 H1A O6 3 .89 1.91 2.728(2) 151.6 N1 H1B O4 3_655 .89 2.28 3.085(2) 150.4 N1 H1C O2 4_465 .89 2.30 2.978(2) 132.7 N1 H1C O5 . .89 2.35 2.896(2) 119.5 O1 H1 O5 4_565 .82 1.76 2.575(2) 170.4 O3 H3 O6 1_655 .82 1.73 2.545(2) 171.6 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 O2 C1 C2 N1 -29.3(3) yes O1 C1 C2 N1 153.29(18) yes O2 C1 C2 C3 90.4(3) yes O1 C1 C2 C3 -87.0(2) yes O4 C4 C5 O5 180.0(2) no O3 C4 C5 O5 -1.0(3) no O4 C4 C5 O6 -1.0(4) no O3 C4 C5 O6 178.1(3) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 30654624