Investigation of hydrogen-bond network in bis(glycinium) oxalate using single-crystal neutron diffraction and spectroscopic studies
Chitra, R.; Choudhury, R. R; Acta Crystallographica Section B 63 (2007) 497–504; doi:10.1107/S0108768107016965

data_2102809
_publ_section_title
;
 Investigation of hydrogen-bond network in bis(glycinium) oxalate using
 single-crystal neutron diffraction and spectroscopic studies
;
_journal_coeditor_code           AV5084
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              497
_journal_page_last               504
_journal_paper_doi               10.1107/S0108768107016965
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         '2(C2 H6 N O2), C2 O4'
_chemical_formula_sum            'C6 H12 N2 O8'
_chemical_formula_weight         240.16
_chemical_name_common            'Bis(glycinium) oxalate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.934(3)
_cell_length_b                   9.955(6)
_cell_length_c                   10.854(9)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    300
_cell_measurement_theta_max      76
_cell_measurement_theta_min      7
_cell_volume                     528.6(6)
_computing_cell_refinement       REFINE
_computing_data_collection       SCAD
_computing_data_reduction        DATRED
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Four circle diffractometer'
_diffrn_measurement_method       \q-\2q
_diffrn_radiation_monochromator  Cu
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'Dhruva Reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.99500
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1298
_diffrn_reflns_theta_full        41.79
_diffrn_reflns_theta_max         41.79
_diffrn_reflns_theta_min         3.90
_diffrn_standards_decay_%        '< 3%'
_diffrn_standards_interval_count 25
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.4091
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   datred
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle with six faces'
_exptl_crystal_F_000             120
_exptl_crystal_size_max          6
_exptl_crystal_size_mid          2.12
_exptl_crystal_size_min          1.06
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.817
_refine_ls_extinction_coef       0.071(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0841P)^2^+3.7730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                894
_reflns_number_total             1298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            av5084.cif
_cod_data_source_block           miss
_cod_depositor_comments
;

2019-10-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     'C2 H6 N O2, 0.5(C2 O4)'
_cod_original_formula_sum        'C3 H6 N O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     120.08
_cod_database_code               2102809