Crystal structure of propane-1,3-diaminium squarate dihydrate
Seidel, Rüdiger W.; Kolev, Tsonko M.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 973–975; doi:10.1107/S2056989024008235

data_2023244
_publ_section_title
;
 Crystal structure of propane-1,3-diaminium squarate dihydrate
;
_journal_coeditor_code           PK2708
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              973
_journal_page_last               975
_journal_paper_doi               10.1107/S2056989024008235
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C3 H12 N2 2+, C4 O4 2-, 2H2 O'
_chemical_formula_moiety         'C3 H12 N2 2+, C4 O4 2-, 2(H2 O)'
_chemical_formula_sum            'C7 H16 N2 O6'
_chemical_formula_weight         224.22
_chemical_name_common
;
Propane-1,3-diaminium squarate dihydrate
;
_chemical_name_systematic
;
Propane-1,3-diaminium 3,4-dioxocyclobutene-1,2-diolate dihydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_Hall           'P 4 -2ab'
_space_group_name_H-M_alt        'P 4 b m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2716(2)
_cell_length_b                   11.2716(2)
_cell_length_c                   4.33100(10)
_cell_measurement_reflns_used    5992
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.6740
_cell_measurement_theta_min      3.5970
_cell_volume                     550.249(19)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlis system (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      105(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            11463
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.857
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[ABSPACK in CrysAlisPro (Rigaku OD, 2023)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.131
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 298 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         745
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0450P)^2^+0.0625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                721
_reflns_number_total             745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2708.cif
_cod_data_source_block           I
_cod_original_cell_volume        550.25(2)
_cod_database_code               2023244
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              20697
_shelx_res_checksum              7890