Crystal structures of 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium benzoate and 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium picrate
Sagar, Belakavadi K.; Girisha, Marisiddaiah; Yathirajan, Hemmige S.; Rathore, Ravindranath S.; Glidewell, Christopher; Acta Crystallographica Section E 73 (2017) 1320–1325; doi:10.1107/S2056989017011446

data_2242274
_publ_section_title
;
 Crystal structures of
 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium
 benzoate and
 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium
 picrate
;
_journal_coeditor_code           LH5849
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1320
_journal_page_last               1325
_journal_paper_doi               10.1107/S2056989017011446
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C11 H19 N2 S +, C7 H5 O2 -'
_chemical_formula_moiety         'C11 H19 N2 S +, C7 H5 O2 -'
_chemical_formula_sum            'C18 H24 N2 O2 S'
_chemical_formula_weight         332.45
_chemical_name_systematic
'2-Amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium benzoate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 122.2110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6089(3)
_cell_length_b                   22.7141(5)
_cell_length_c                   8.8959(2)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.521
_cell_measurement_theta_min      7.655
_cell_volume                     1813.73(8)
_computing_cell_refinement
;
APEX2 (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2012)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material  'SHELXL2014 and PLATON'
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Kappa APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.521
_diffrn_reflns_theta_min         7.655
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.100
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1373 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.061(7)
_refine_ls_extinction_coef       0.0076(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0350P)^2^+0.3018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                3138
_reflns_number_total             3209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5849sup1.cif
_cod_data_source_block           I
_cod_database_code               2242274
_cod_database_fobs_code          2242274
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.825
_shelx_hkl_checksum              2077
_shelx_res_checksum              78179
_shelxl_version_number           2.014