Expected and unexpected products of reactions of 2-hydrazinylbenzothiazole with 3-nitrobenzenesulfonyl chloride in different solvents
Morscher, Alexandra; de Souza, Marcus V. N.; Wardell, James L.; Harrison, William T. A.; Acta Crystallographica Section E 74 (2018) 673–677; doi:10.1107/S2056989018005595

data_2242457
_publ_section_title
;
 Expected and unexpected products of reactions of
 2-hydrazinylbenzothiazole with 3-nitrobenzenesulfonyl chloride in
 different solvents
;
_journal_coeditor_code           SJ5555
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              673
_journal_page_last               677
_journal_paper_doi               10.1107/S2056989018005595
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C13 H11 N4 O4 S2 +, C6 H4 N O5 S -'
_chemical_formula_moiety         'C13 H11 N4 O4 S2 +, C6 H4 N O5 S -'
_chemical_formula_sum            'C19 H15 N5 O9 S3'
_chemical_formula_weight         553.54
_chemical_name_systematic
;
2-[2-(3-Nitrobenzenesulfonyl)hydrazinyl]-1,3-benzothiazol-3-ium;
3-nitrobenzenesulfonate
;
_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
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                85.607(4)
_cell_angle_beta                 71.369(5)
_cell_angle_gamma                77.115(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0399(5)
_cell_length_b                   10.7585(4)
_cell_length_c                   11.3372(6)
_cell_measurement_reflns_used    14254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.03
_cell_volume                     1131.17(10)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>FS_ABSCOR</i>; Rigaku, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.8265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                4880
_reflns_number_total             5159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5555sup1.cif
_cod_data_source_block           III
_cod_original_cell_volume        1131.16(10)
_cod_database_code               2242457
_cod_database_fobs_code          2242457
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              78897
_shelx_res_checksum              7604