Visible light-mediated dehydrogenative β-arylsulfonylation of tertiary aliphatic amines with arylsulfonyl chlorides.
Chen, Min; Huang, Zhi-Tang; Zheng, Qi-Yu; Organic & biomolecular chemistry 12 (2014) 9337–; doi:10.1039/c4ob01713g

data_7154159
_publ_section_title
;
 Visible light-mediated dehydrogenative \b-arylsulfonylation of tertiary
 aliphatic amines with arylsulfonyl chlorides.
;
_journal_issue                   46
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9337
_journal_paper_doi               10.1039/c4ob01713g
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C22 H29 N O2 S2'
_chemical_formula_sum            'C22 H29 N O2 S2'
_chemical_formula_weight         403.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 111.581(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.737(4)
_cell_length_b                   14.565(3)
_cell_length_c                   20.694(5)
_cell_measurement_reflns_used    18694
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.7742
_cell_measurement_theta_min      1.3981
_cell_volume                     4410.7(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31620
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         10025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+4.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                8956
_reflns_number_total             10025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01713g2.cif
_cod_data_source_block           cm_obc_1a
_cod_depositor_comments
'Adding full bibliography for 7154159--7154160.cif.'
_cod_original_cell_volume        4410.6(18)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7154159