X-ray diffraction and Raman study of <small>DL</small>-alanine at high pressure: revision of phase transitions
Tumanov, Nikolay A.; Boldyreva, Elena V.; Acta Crystallographica Section B 68 (2012) 412–423; doi:10.1107/S0108768112028972

data_2105152
_publ_section_title
;
 X-ray diffraction and Raman study of <small>DL</small>-alanine at high
 pressure: revision of phase transitions
;
_journal_coeditor_code           GP5051
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              412
_journal_page_last               423
_journal_paper_doi               10.1107/S0108768112028972
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C3 H7 N O2'
_chemical_formula_sum            'C3 H7 N O2'
_chemical_formula_weight         89.10
_chemical_name_common            DL-alanine
_chemical_name_systematic        'DL-2-Aminopropionic Acid '
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   11.572(4)
_cell_length_b                   5.567(5)
_cell_length_c                   5.6710(11)
_cell_measurement_reflns_used    988
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.9607
_cell_measurement_theta_min      3.5854
_cell_volume                     365.3(4)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction Ltd, 2010)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>, 2008),
PLATON (Spek, 2009),
enCIFer (Allen <i>et al.</i>, 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 0.462
_diffrn_measured_fraction_theta_max 0.462
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2420
_diffrn_reflns_theta_full        31.03
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         5.03
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Absorb6.1 (R. J. Angel, 2004)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         529
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                385
_reflns_number_total             529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gp5051.cif
_cod_data_source_block           dlala_45kbar
_cod_original_cell_volume        365.4(3)
_cod_database_code               2105152