Hydrogen-bonding synthons in lamotrigine salts: 3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazin-2-ium 2-[(2-carboxyphenyl)disulfanyl]benzoate in its monohydrate and anhydrous forms
Freire, Eleonora; Polla, Griselda; Baggio, Ricardo; Acta Crystallographica Section C 72 (2016) 910–916; doi:10.1107/S2053229616016090

data_2020637
_publ_section_title
;
 Hydrogen-bonding synthons in lamotrigine salts:
 3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazin-2-ium
 2-[(2-carboxyphenyl)disulfanyl]benzoate in its monohydrate and anhydrous
 forms
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              910
_journal_page_last               916
_journal_paper_doi               10.1107/S2053229616016090
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C9 H8 Cl2 N5 +, C14 H9 O4 S2 -, H2 O'
_chemical_formula_moiety         'C9 H8 Cl2 N5 +, C14 H9 O4 S2 -, H2 O'
_chemical_formula_sum            'C23 H19 Cl2 N5 O5 S2'
_chemical_formula_weight         580.45
_chemical_name_systematic
;
3,5-Diamino-6-(2,3-dichlorophenyl)-1,2,4-triazin-2-ium
2-[(2-carboxyphenyl)disulfanyl]benzoate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                100.996(7)
_cell_angle_beta                 98.101(7)
_cell_angle_gamma                103.659(8)
_cell_formula_units_Z            2
_cell_length_a                   8.0598(7)
_cell_length_b                   12.3474(13)
_cell_length_c                   13.4484(10)
_cell_measurement_reflns_used    1591
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.6290
_cell_measurement_theta_min      3.9560
_cell_volume                     1252.1(2)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) andPLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD S Ultra'
_diffrn_measurement_method       '\w scans, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11193
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.339
_diffrn_reflns_theta_min         3.699
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5794
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0716P)^2^+0.7292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1662
_reflns_number_gt                3744
_reflns_number_total             5794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3034sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-24

 Adding full bibliography for 2020637--2020638.cif.
;
_cod_database_code               2020637
_cod_database_fobs_code          2020637
_shelx_hkl_checksum              54027
_shelx_res_checksum              40746
_shelxl_version_number           2014/6