The hetero-Diels–Alder addition of sulfur dioxide: structure of the first crystalline sultine. Quantum calculations on the conformations of 6-fluoro-3,6-dihydro-1,2-oxathiine 2-oxides
Roversi, Elena; Scopelliti, Rosario; Solari, Euro; Estoppey, Raphaël; Vogel, Pierre; Braña, Pedro; Menéndez, Bibiana; Sordo, JoséÁngel; Chemical Communications  (2001) 1214–; doi:10.1039/b103096p

data_7114670
_publ_section_title
;
 The hetero-Diels--Alder addition of sulfur dioxide: structure of the
 first crystalline sultine. Quantum calculations on the conformations of
 6-fluoro-3,6-dihydro-1,2-oxathiine 2-oxides
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1214
_journal_paper_doi               10.1039/b103096p
_journal_year                    2001
_chemical_formula_sum            'C12 H11 F O2 S'
_chemical_formula_weight         238.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.577(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8271(9)
_cell_length_b                   13.982(2)
_cell_length_c                   10.1237(15)
_cell_measurement_temperature    143(2)
_cell_volume                     1061.9(3)
_computing_cell_refinement       'CrysAlis RED, 1.6.7, 2000'
_computing_data_collection       'CrysAlis CCD, 1.6.7, 2000'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'KUMA CCD'
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5521
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.004(3)
_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_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0521P)^2^+1.5444P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                1648
_reflns_number_total             1795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103096p.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114670