Supramolecular motifs in the first structures of organic carboxylate salts of 1-(diaminomethylene)thiourea (HATU)
Hołyńska, Małgorzata; Kubiak, Maria; Acta Crystallographica Section C 65 (2009) o410–o413; doi:10.1107/S0108270109026390

data_2017218
_publ_section_title
;
 Supramolecular motifs in the first structures of organic carboxylate
 salts of 1-(diaminomethylene)thiourea (HATU)
;
_journal_coeditor_code           FA3194
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o410
_journal_page_last               o413
_journal_paper_doi               10.1107/S0108270109026390
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '2C2 H7 N4 S + , C2 O4 2- , 2H2 O'
_chemical_formula_moiety         '2(C2 H7 N4 S +), C2 O4 2- , 2(H2 O)'
_chemical_formula_sum            'C6 H18 N8 O6 S2'
_chemical_formula_weight         362.40
_chemical_name_systematic
;
bis[1-(diaminomethylene)thiouron-1-ium] oxalate 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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                111.89(3)
_cell_angle_beta                 90.82(3)
_cell_angle_gamma                91.02(3)
_cell_formula_units_Z            1
_cell_length_a                   7.006(3)
_cell_length_b                   7.221(3)
_cell_length_c                   7.837(3)
_cell_measurement_reflns_used    3612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.87
_cell_measurement_theta_min      3.04
_cell_volume                     367.7(3)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlisRED (Oxford Diffraction, 2006)'
_computing_molecular_graphics
'DIAMOND (Brandenburg & Putz, 2005) and SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.571
_diffrn_measurement_device_type  'Kuma KM4 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0104
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4151
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         36.87
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlisRED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             190
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                1827
_reflns_number_total             2114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3194.cif
_cod_data_source_block           II
_cod_database_code               2017218
_cod_database_fobs_code          2017218