4-Dimethylamino Pyridine-Promoted One-Pot Three-Component Regioselective Synthesis of Highly Functionalized 4H-Thiopyrans via Heteroannulation of β-Oxodithioesters.
Verma, Rajiv Kumar; Verma, Girijesh Kumar; Shukla, Gaurav; Nagaraju, Anugula; Singh, Maya Shankar; ACS combinatorial science 14 (2012) 224–230; doi:10.1021/co200203e

data_4505630
_publ_section_title
;
 4-Dimethylamino Pyridine-Promoted One-Pot Three-Component Regioselective
 Synthesis of Highly Functionalized 4H-Thiopyrans via Heteroannulation of
 \b-Oxodithioesters.
;
_journal_issue                   3
_journal_name_full               'ACS combinatorial science'
_journal_page_first              224
_journal_page_last               230
_journal_paper_doi               10.1021/co200203e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C16 H12 N2 O S4'
_chemical_formula_sum            'C16 H12 N2 O S4'
_chemical_formula_weight         376.52
_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                 90.843(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6868(3)
_cell_length_b                   12.0610(3)
_cell_length_c                   16.5857(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1737.52(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10835
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.550
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.6267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                2852
_reflns_number_total             3598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            co200203e_si_003.cif
_cod_data_source_block           bte_85r_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P12(1)/c1
_cod_database_code               4505630