Scope and limitation of the [1,2]-phenylsulfanyl (PhS) migration in the synthesis of tetrahydrofurans and tetrahydropyrans from common triol precursors
House, David; Kerr, Fraser; Warren, Stuart; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2652–; doi:10.1039/b208558e

data_7204526
_publ_section_title
;
 Scope and limitation of the [1,2]-phenylsulfanyl (PhS) migration in
 the synthesis of tetrahydrofurans and tetrahydropyrans from common
 triol precursors
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2652
_journal_paper_doi               10.1039/b208558e
_journal_year                    2002
_chemical_formula_sum            'C20 H34 O3 S Si'
_chemical_formula_weight         382.62
_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
_cell_angle_alpha                91.37(3)
_cell_angle_beta                 97.96(2)
_cell_angle_gamma                87.39(2)
_cell_formula_units_Z            2
_cell_length_a                   10.820(3)
_cell_length_b                   13.543(4)
_cell_length_c                   7.720(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1119.0(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    teXsan
_diffrn_ambient_temperature      230(2)
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2theta scans'
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.1059
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6366
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        +0.1%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_obs          0.0620
_refine_ls_shift/esd_max         0.052
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1359
_refine_ls_wR_factor_obs         0.1102
_reflns_number_observed          2219
_reflns_number_total             3924
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208558e.txt
_cod_data_source_block           sw9902
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0762P] 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^)+(0.0538P)^2^+0.0762P] 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      P-1
_cod_database_code               7204526