Hydrogen Bonding in 2-Methyl-1,2,3-propanetricarboxylic Acid, Ammonium Dihydrogen 1,2,3-Propanetricarboxylate Hemihydrate and Tetraammonium 1,2,3,4-Butanetetracarboxylate Monohydrate
Barnes, H. A.; Barnes, J. C.; Acta Crystallographica Section C 52 (1996) 731–736; doi:10.1107/S0108270195013527

data_2004638
_publ_section_title
;
 Hydrogen Bonding in 2-Methyl-1,2,3-propanetricarboxylic Acid, Ammonium
 Dihydrogen 1,2,3-Propanetricarboxylate Hemihydrate and Tetraammonium
 1,2,3,4-Butanetetracarboxylate Monohydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              731
_journal_page_last               736
_journal_paper_doi               10.1107/S0108270195013527
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'N H4 1+, C6 H7 O6 1-, 1/2H2 O1'
_chemical_formula_structural     C~3~H~5~(COOH)~2~(COO^-^).NH~4~^+^.0.5H~2~O
_chemical_formula_sum            'C6 H12 N O6.5'
_chemical_formula_weight         202.17
_chemical_name_common            'ammonium tricarballylate hydrate (1:1:0.5)'
_chemical_name_systematic
;
propane-1,2,3-tricarboxylic acid, mono-ammonium salt hemi-hydrate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 93.565(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.9331(12)
_cell_length_b                   7.8035(14)
_cell_length_c                   7.4103(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1785.3(3)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1991)'
_computing_data_reduction        MADNES
_computing_molecular_graphics
'PLATON92 (Spek, 1992a) and PLUTON92 (Spek, 1992b)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 FAST'
_diffrn_measurement_method       'Measurement method: area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3797
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.889
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_restrained_S_obs      1.038
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_obs          0.040
_refine_ls_shift/esd_max         0.09
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0437P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.100
_refine_ls_wR_factor_obs         0.0866
_reflns_number_observed          975
_reflns_number_total             1386
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1138.cif
_cod_data_source_block           aca
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C6 H12 N O6.50'
_cod_database_code               2004638