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_2004637
_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          'C7 H10 O6'
_chemical_formula_structural     HOOC.CH~2~.C(CH~3~)(COOH).CH~2~.COOH
_chemical_formula_sum            'C7 H10 O6'
_chemical_formula_weight         190.15
_chemical_name_common            '\b-methyl tricarballylic acid'
_chemical_name_systematic
;
2-methyl propane-1,2,3-tricarboxylic acid
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                86.770(5)
_cell_angle_beta                 88.663(8)
_cell_angle_gamma                84.456(13)
_cell_formula_units_Z            2
_cell_length_a                   6.8350(10)
_cell_length_b                   6.995(2)
_cell_length_c                   8.5400(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     405.68(14)
_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  0.047
_diffrn_reflns_av_sigmaI/netI    0.2034
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2233
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.408
_refine_ls_goodness_of_fit_obs   0.404
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.408
_refine_ls_restrained_S_obs      0.404
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_obs          0.036
_refine_ls_shift/esd_max         -0.03
_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^) + (0.0613P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.117
_refine_ls_wR_factor_obs         0.0896
_reflns_number_observed          1159
_reflns_number_total             1918
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1138.cif
_cod_data_source_block           bmetca
_cod_database_code               2004637