Crystal structure studies and Hirshfeld surface analysis of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at 90 K
Anil Kumar, Haleyur G.; Mohan Kumar, Thaluru M.; Divakara, Thayamma R.; Geetha, Doreswamy; Yathirajan, Hemmige S.; Parkin, Sean; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S2056989023007223

data_2022844
_publ_section_title
;
 Crystal structure studies and Hirshfeld surface analysis of
 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at
 90&#x2005;K
;
_journal_coeditor_code           VM2289
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989023007223
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C8 H14 N2 O 2+, 2Cl -, H2 O'
_chemical_formula_moiety         'C8 H14 N2 O 2+, 2(Cl -), H2 O'
_chemical_formula_sum            'C8 H16 Cl2 N2 O2'
_chemical_formula_weight         243.13
_chemical_name_systematic
;
4-(Dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 117.188(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6493(7)
_cell_length_b                   13.0873(8)
_cell_length_c                   10.4634(7)
_cell_measurement_reflns_used    9459
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.38
_cell_volume                     1175.36(14)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            36719
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         2.382
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.218
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.2669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                2505
_reflns_number_total             2693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2289sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2022844
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.892
_shelx_hkl_checksum              33026
_shelx_res_checksum              65537
_cod_database_fobs_code 2022844