Chlorinated thiophenes. Part 2. Trihalogenated hydroxythiophenes; preparation, reactions and tautomeric properties
Skramstad, Jan; Lunde, Andreas; Hope, Håkon; Bjørnstad, Vidar; Frøyen, Paul; Journal of the Chemical Society, Perkin Transactions 2  (2000) 1453–; doi:10.1039/b001570i

data_7213288
_publ_section_title
;
 Chlorinated thiophenes. Part 2. Trihalogenated hydroxythiophenes;
 preparation, reactions and tautomeric properties
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1453
_journal_paper_doi               10.1039/b001570i
_journal_year                    2000
_chemical_formula_sum            'C8 Cl6 O2 S2'
_chemical_formula_weight         404.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 118.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.341(4)
_cell_length_b                   13.560(7)
_cell_length_c                   7.471(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    119(1)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     653.9(6)
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119(1)
_diffrn_measurement_device       'Siemens P4/RA'
_diffrn_measurement_method       theta/2theata
_diffrn_radiation_monochromator  'Ni filter'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            888
_diffrn_reflns_theta_max         55.05
_diffrn_reflns_theta_min         6.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    14.897
_exptl_absorpt_correction_T_max  0.068
_exptl_absorpt_correction_T_min  0.032
_exptl_absorpt_correction_type   'empirical XABS2'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0007(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_obs          0.0551
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+1.3175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1743
_refine_ls_wR_factor_obs         0.1653
_reflns_number_observed          727
_reflns_number_total             820
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001570isup1.cif
_cod_data_source_block           hh267
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+1.3175P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+1.3175P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7213288