Redetermination of ammonium oxalate oxalic acid dihydrate
Gustavo Portalone; Marcello Colapietro; Acta Crystallographica Section E 62 (2006) o4725–o4727; doi:10.1107/S1600536806038748

data_2210798
_publ_section_title
;
 Redetermination of ammonium oxalate oxalic acid dihydrate
;
_journal_coeditor_code           TK2071
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4725
_journal_page_last               o4727
_journal_paper_doi               10.1107/S1600536806038748
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'N1 H4 + , C2 H O4 - , C2 H2 O4 , 2H2 O'
_chemical_formula_moiety         'H4 N + , C2 H O4 - , C2 H2 O4 , 2H2 O'
_chemical_formula_sum            'C4 H11 N O10'
_chemical_formula_weight         233.14
_chemical_name_systematic
;
ammonium oxalate oxalic acid dihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                94.172(10)
_cell_angle_beta                 100.274(10)
_cell_angle_gamma                97.704(10)
_cell_formula_units_Z            2
_cell_length_a                   6.3387(8)
_cell_length_b                   7.2227(9)
_cell_length_c                   10.5527(11)
_cell_measurement_reflns_used    121
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      20
_cell_volume                     468.77(10)
_computing_cell_refinement       XCS
_computing_data_collection       'XCS (Colapietro <i>et al.</i>,  1992)'
_computing_data_reduction        XCS
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Huber CS four-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710689
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.011
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6934
_diffrn_reflns_theta_full        42.0
_diffrn_reflns_theta_max         42.0
_diffrn_reflns_theta_min         2.9
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.043
_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^)+(0.0705P)^2^+0.0474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.127
_refine_ls_wR_factor_ref         0.132
_reflns_number_gt                5265
_reflns_number_total             6283
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2071.cif
_cod_data_source_block           I
_cod_database_code               2210798
_cod_database_fobs_code          2210798