A high-pressure single-crystal to single-crystal phase transition in <small>DL</small>-alaninium semi-oxalate monohydrate with switching-over hydrogen bonds
Zakharov, Boris A.; Boldyreva, Elena V.; Acta Crystallographica Section B 69 (2013) 271–280; doi:10.1107/S2052519213011676

data_2105447
_publ_section_title
;
 A high-pressure single-crystal to single-crystal phase transition in
 <small>DL</small>-alaninium semi-oxalate monohydrate with switching-over
 hydrogen bonds
;
_journal_coeditor_code           GP5064
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              271
_journal_page_last               280
_journal_paper_doi               10.1107/S2052519213011676
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C3 H8 N O2, C2 H O4, H2 O'
_chemical_formula_sum            'C5 H11 N O7'
_chemical_formula_weight         197.15
_chemical_name_common            'DL-alaninium semi-oxalate hydrate'
_chemical_name_systematic        'DL-alaninium semi-oxalate hydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.57(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.456(7)
_cell_length_b                   6.4891(4)
_cell_length_c                   11.338(3)
_cell_measurement_reflns_used    1215
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0343
_cell_measurement_theta_min      1.9557
_cell_volume                     840.0(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material
;
Mercury (Macrae et al., 2006),
PLATON (Spek, 2009),
enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.382
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4770
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'Absorb Angel (2004) J. Appl. Cryst. 37:486-492'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         788
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.3244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                508
_reflns_number_total             788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gp5064.cif
_cod_data_source_block           030
_cod_original_cell_volume        839.9(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105447
_cod_database_fobs_code          2105447