Crystal structures of three halide salts of <small>L</small>-asparagine: an isostructural series
de Moraes, Lygia S.; Kennedy, Alan R.; Logan, Charlie R.; Acta Crystallographica Section E 74 (2018) 1619–1623; doi:10.1107/S2056989018014603

data_2242681
_publ_section_title
;
 Crystal structures of three halide salts of <small>L</small>-asparagine:
 an isostructural series
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1619
_journal_page_last               1623
_journal_paper_doi               10.1107/S2056989018014603
_journal_volume                  74
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C4 H9 N2 O3 -, Br +, H2 O'
_chemical_formula_moiety         'C4 H9 N2 O3 -, Br +, H2 O'
_chemical_formula_sum            'C4 H11 Br N2 O4'
_chemical_formula_weight         231.06
_chemical_name_systematic
;
<i>L</i>-Asparaginium bromide monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.606(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.2167(2)
_cell_length_b                   10.2784(5)
_cell_length_c                   8.3063(4)
_cell_measurement_reflns_used    3145
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.7542
_cell_measurement_theta_min      3.2022
_cell_volume                     432.88(4)
_computing_cell_refinement
;
Crysalis PRO (Agilent, 2014)
;
_computing_data_collection
;
Crysalis PRO (Agilent, 2014)
;
_computing_data_reduction
;
Crysalis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1994)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       'omega scans'
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4320
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.820
_diffrn_reflns_theta_min         3.209
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.723
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2014), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       tablet
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.384
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 908 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.022(11)
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2232
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                2118
_reflns_number_total             2232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7779sup1.cif
_cod_data_source_block           II
_cod_database_code               2242681
_cod_database_fobs_code          2242681
_shelx_hkl_checksum              52740
_shelx_res_checksum              13100