Electrochemical Method for the Synthesis of Disulfides of 2-(Benzo[d]thiazol(or oxazol)-2-ylamino)-5-morpholinobenzenethiol
Roya Esmaili; Davood Nematollahi; Journal of Organic Chemistry 78 (2013) 5018–5021; doi:10.1021/jo302647r

data_4028218
_publ_section_title
;
 Electrochemical Method for the Synthesis of Disulfides of
 2-(Benzo[d]thiazol(or oxazol)-2-ylamino)-5-morpholinobenzenethiol
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5018
_journal_page_last               5021
_journal_paper_doi               10.1021/jo302647r
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C36 H34 Cl6 N6 O2 S4'
_chemical_formula_weight         923.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.912(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.735(2)
_cell_length_b                   5.5440(3)
_cell_length_c                   22.2598(15)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.35
_cell_volume                     4010.4(4)
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.1103
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9629
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'shape of crystal determined optically'
_exptl_crystal_colour            Yelloqw
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+10.0860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                2483
_reflns_number_total             3932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302647r_si_003.cif
_cod_data_source_block           d:\determination\solution\c302\khc302
_cod_original_cell_volume        4010.5(4)
_cod_database_code               4028218