#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/07/2200716.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_2200716 loop_ _publ_author_name 'B. Sridhar' 'N. Srinivasan' 'R. K. Rajaram' _publ_section_title ; Bis(\b-alanine) hydrogen nitrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1004 _journal_page_last o1006 _journal_paper_doi 10.1107/S1600536801015793 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '2C3 H7 N O2, H 1+, N O3 1-' _chemical_formula_moiety '2C3 H7 N O2, H 1+, N O3 1-' _chemical_formula_sum 'C6 H15 N3 O7' _chemical_formula_weight 241.21 _chemical_name_common 'bis(\b-Alanine) H+ nitrate' _chemical_name_systematic ; \b-Alanine \b-alaninium nitrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 113.923(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.7910(10) _cell_length_b 5.3220(3) _cell_length_c 10.9740(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.034 _cell_measurement_theta_min 11.307 _cell_volume 1056.57(13) _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, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .984 _diffrn_measured_fraction_theta_max .984 _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 MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0135 _diffrn_reflns_av_sigmaI/netI .0121 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 941 _diffrn_reflns_theta_full 24.97 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.25 _diffrn_standards_decay_% none _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .138 _exptl_absorpt_correction_T_max .9699 _exptl_absorpt_correction_T_min .8633 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_meas 1.502 _exptl_crystal_density_method 'flotation using a mixture of carbon tetrachloride and xylene' _exptl_crystal_description needle _exptl_crystal_F_000 512 _exptl_crystal_size_max .6 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .2 _refine_diff_density_max .314 _refine_diff_density_min -.182 _refine_ls_extinction_coef .103(7) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 914 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all .0400 _refine_ls_R_factor_gt .0334 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.6820P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0916 _reflns_number_gt 798 _reflns_number_total 914 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob6076.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2200716 _cod_database_fobs_code 2200716 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 O1A .19302(7) .4346(2) .27700(10) .0452(4) Uani d . 1 . . O O1B .21345(6) .1038(2) .41024(9) .0381(4) Uani d . 1 . . O H1B .2500 .2500 .5000 .116(14) Uiso d S 1 . . H C11 .18276(8) .2140(3) .29461(14) .0321(4) Uani d . 1 . . C C12 .13324(9) .0474(3) .18276(14) .0369(4) Uani d . 1 . . C H12A .0973(11) -.033(4) .2091(19) .050(5) Uiso d . 1 . . H H12B .1631(11) -.083(4) .1728(18) .045(5) Uiso d . 1 . . H C13 .09337(9) .1853(3) .05321(15) .0377(4) Uani d . 1 . . C H13A .0660(10) .324(4) .0621(17) .042(5) Uiso d . 1 . . H H13B .0597(11) .077(4) -.015(2) .050(5) Uiso d . 1 . . H N11 .14535(8) .2912(3) -.00011(14) .0389(4) Uani d . 1 . . N H1A .1805(12) .375(4) .062(2) .052(5) Uiso d . 1 . . H H2B .1670(11) .179(4) -.0288(19) .055(6) Uiso d . 1 . . H H3C .1196(13) .386(4) -.071(2) .061(6) Uiso d . 1 . . H N1 .5000 .0750(4) .7500 .0379(5) Uani d S 1 . . N O1 .45215(7) .1894(3) .65579(12) .0553(4) Uani d . 1 . . O O2 .5000 -.1571(4) .7500 .0753(7) Uani d S 1 . . O 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 .0592(8) .0348(7) .0367(6) -.0082(5) .0143(5) -.0005(5) O1B .0423(6) .0377(7) .0277(6) -.0011(5) .0074(4) .0007(4) C11 .0317(7) .0343(9) .0303(8) .0006(6) .0126(6) -.0012(6) C12 .0394(8) .0352(8) .0318(8) -.0027(7) .0100(7) -.0014(6) C13 .0314(8) .0471(10) .0316(8) -.0014(7) .0097(6) -.0003(7) N11 .0390(8) .0441(9) .0320(8) -.0008(7) .0127(6) -.0002(6) N1 .0377(10) .0440(11) .0341(9) .000 .0168(8) .000 O1 .0497(7) .0541(8) .0507(8) .0099(6) .0086(6) .0069(6) O2 .0956(16) .0438(11) .0539(12) .000 -.0034(11) .000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 '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 .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C11 O1B H1B . . 112.62(10) O1A C11 O1B . . 123.06(13) O1A C11 C12 . . 122.09(13) O1B C11 C12 . . 114.84(13) C13 C12 C11 . . 113.58(13) C13 C12 H12A . . 109.3(11) C11 C12 H12A . . 109.3(12) C13 C12 H12B . . 111.1(11) C11 C12 H12B . . 107.1(11) H12A C12 H12B . . 106.2(16) N11 C13 C12 . . 112.02(13) N11 C13 H13A . . 105.2(11) C12 C13 H13A . . 112.7(11) N11 C13 H13B . . 107.2(12) C12 C13 H13B . . 111.9(12) H13A C13 H13B . . 107.4(15) C13 N11 H1A . . 110.2(13) C13 N11 H2B . . 113.9(14) H1A N11 H2B . . 106.2(19) C13 N11 H3C . . 108.4(14) H1A N11 H3C . . 113(2) H2B N11 H3C . . 105.5(19) O2 N1 O1 . 2_656 119.35(10) O2 N1 O1 . . 119.35(10) O1 N1 O1 2_656 . 121.3(2) 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 O1A C11 . 1.2204(19) yes O1B C11 . 1.3030(17) yes O1B H1B . 1.2333(10) no C11 C12 . 1.509(2) ? C12 C13 . 1.507(2) ? C12 H12A . .97(2) ? C12 H12B . .94(2) ? C13 N11 . 1.486(2) ? C13 H13A . .94(2) ? C13 H13B . .96(2) ? N11 H1A . .87(2) ? N11 H2B . .87(2) ? N11 H3C . .89(2) ? N1 O2 . 1.235(3) yes N1 O1 2_656 1.2419(15) no N1 O1 . 1.2419(15) 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 O1B H1B O1B 7_556 1.2333(10) 1.2333(10) 2.467(2) 180.0 N11 H1A O1A . .87(2) 2.29(2) 2.8971(18) 126.5(17) N11 H1A O1B 4 .87(2) 2.34(2) 3.0517(18) 139.1(17) N11 H2B O1B 6 .87(2) 2.01(3) 2.877(2) 175(2) N11 H3C O1 4 .89(2) 2.10(3) 2.908(2) 150(2) N11 H3C O2 3_454 .89(2) 2.40(2) 3.0779(15) 133.2(18) 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 O1A C11 C12 C13 -5.2(2) yes O1B C11 C12 C13 174.93(13) yes C11 C12 C13 N11 63.60(19) yes