Crystal structure of isobutylammonium hydrogen oxalate hemihydrate
Dziuk, Błażej; Zarychta, Bartosz; Ejsmont, Krzysztof; Acta Crystallographica Section E 70 (2014) o1175–; doi:10.1107/S1600536814022697

data_2240099
_publ_section_title
;
 Crystal structure of isobutylammonium hydrogen oxalate hemihydrate
;
_journal_coeditor_code           HB7298
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1175
_journal_paper_doi               10.1107/S1600536814022697
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '2C4 H12 N +, 2C2 H O4 -, H2 O'
_chemical_formula_moiety         'C4 H12 N +, C2 H O4 -, 0.5(H2 O)'
_chemical_formula_sum            'C6 H14 N O4.5'
_chemical_formula_weight         172.18
_chemical_name_systematic
;
Isobutylammonium hydrogen oxalate hemihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 119.141(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2425(9)
_cell_length_b                   5.63410(10)
_cell_length_c                   16.5372(6)
_cell_measurement_reflns_used    1696
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.78
_cell_volume                     1728.69(13)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w scan'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5536
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0414P)^2^+0.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                1370
_reflns_number_total             1696
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7298sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2017-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1728.69(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_moiety     '2(C4 H12 N +), 2(C2 H O4 -), H2 O'
_cod_original_formula_sum        'C12 H28 N2 O9'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     344.36
_cod_database_code               2240099
_cod_database_fobs_code          2240099