Intramolecular Thia-anti-Michael Addition of a Sulfur Anion to Enones: A Regiospecific Approach to Multisubstituted Thiophene Derivatives
Yan Li; Fushun Liang; Xihe Bi; Qun Liu; Journal of Organic Chemistry 71 (2006) 8006–8010; doi:10.1021/jo0611420

data_4022007
_publ_section_title
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 Intramolecular Thia-anti-Michael Addition of a Sulfur Anion to Enones:
 A Regiospecific Approach to Multisubstituted Thiophene Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8006
_journal_page_last               8010
_journal_paper_doi               10.1021/jo0611420
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C25 H21 Cl N2 O2 S'
_chemical_formula_sum            'C25 H21 Cl N2 O2 S'
_chemical_formula_weight         448.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.741(5)
_cell_angle_beta                 94.709(5)
_cell_angle_gamma                109.103(5)
_cell_formula_units_Z            2
_cell_length_a                   6.656(5)
_cell_length_b                   8.686(5)
_cell_length_c                   20.105(5)
_cell_measurement_reflns_used    216
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.69
_cell_volume                     1084.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6113
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  10
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1351P)^2^+1.2842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2065
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                2667
_reflns_number_total             4184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0611420si20060605_083940.cif
_cod_depositor_comments
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The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4022007