Dimethylammonium 2,4,5-tricarboxybenzoate: an example of the decarbonylation of <i>N</i>,<i>N</i>-dimethylformamide in the presence of a metal and a benzenepolycarboxylic acid. Is zirconium(IV) the <i>Tsotsi</i>?
Hulushe, S. T.; Hosten, E. C.; Watkins, G. M.; Acta Crystallographica Section E 72 (2016) 1521–1525; doi:10.1107/S2056989016014948

data_2241867
_publ_section_title
;
 Dimethylammonium 2,4,5-tricarboxybenzoate: an example of the
 decarbonylation of <i>N</i>,<i>N</i>-dimethylformamide in the presence of
 a metal and a benzenepolycarboxylic acid. Is zirconium(IV) the
 <i>Tsotsi</i>?
;
_journal_coeditor_code           SJ5505
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1521
_journal_page_last               1525
_journal_paper_doi               10.1107/S2056989016014948
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C2 H8 N +, C10 H5 O8 -'
_chemical_formula_moiety         'C2 H8 N +, C10 H5 O8 -'
_chemical_formula_sum            'C12 H13 N O8'
_chemical_formula_weight         299.23
_chemical_name_systematic
;
Dimethylammonium 2,4,5-tricarboxybenzoate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.6621(5)
_cell_length_b                   9.6621(5)
_cell_length_c                   27.8940(17)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.23
_cell_volume                     2604.1(2)
_computing_cell_refinement
;
APEX2 (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b) and
<i>ShelXle</i> (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47565
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         2.108
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9461
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2010)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.271
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2780 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.14(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6473
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+1.8024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                6118
_reflns_number_total             6473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5505sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2604.1(3)
_cod_database_code               2241867
_cod_database_fobs_code          2241867
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.974
_shelx_hkl_checksum              72543
_shelx_res_checksum              36619
_shelxl_version_number           2014/7