Low-temperature phase transition in glycine–glutaric acid co-crystals studied by single-crystal X-ray diffraction, Raman spectroscopy and differential scanning calorimetry
Zakharov, Boris A.; Losev, Evgeniy A.; Kolesov, Boris A.; Drebushchak, Valeri A.; Boldyreva, Elena V.; Acta Crystallographica Section B 68 (2012) 287–296; doi:10.1107/S0108768112015972

data_2105121
_publ_section_title
;
 Low-temperature phase transition in glycine--glutaric acid co-crystals
 studied by single-crystal X-ray diffraction, Raman spectroscopy and
 differential scanning calorimetry
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              287
_journal_page_last               296
_journal_paper_doi               10.1107/S0108768112015972
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C5 H8 O4, C2 H5 N O2'
_chemical_formula_sum            'C7 H13 N O6'
_chemical_formula_weight         207.18
_chemical_name_common            'glutaric acid--glycine (1/1)'
_chemical_name_systematic
;
Propane-1,3-dicarboxylic acid -- Aminoethanoic acid (1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.486(13)
_cell_angle_beta                 113.065(10)
_cell_angle_gamma                88.263(12)
_cell_formula_units_Z            4
_cell_length_a                   4.8884(7)
_cell_length_b                   20.136(3)
_cell_length_c                   10.1518(15)
_cell_measurement_reflns_used    8917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.06
_cell_volume                     914.5(2)
_computing_cell_refinement       'STOE X-AREA (Stoe & Cie, 2006)'
_computing_data_collection       'STOE X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'STOE X-RED (Stoe & Cie, 2006)'
_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, 2008) and X-STEP32
(Stoe & Cie, 2000)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8816
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                2766
_reflns_number_total             4247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gp5050.cif
_cod_data_source_block           100
_cod_database_code               2105121
_cod_database_fobs_code          2105121