Johnson orthoester Claisen rearrangement products of some (1-oxa-4-thiaspiro[4.5]dec-6-en-6-yl)alkanols
Parvez, Masood; Yadav, Veejendra K.; Senthil, Govindaraji; Acta Crystallographica Section C 57 (2001) 79–81; doi:10.1107/S0108270100013603

data_2011700
_publ_section_title
;
 Johnson orthoester Claisen rearrangement products of some
 (1-oxa-4-thiaspiro[4.5]dec-6-en-6-yl)alkanols
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              79
_journal_page_last               81
_journal_paper_doi               10.1107/S0108270100013603
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C19 H23 Br O3 S'
_chemical_formula_sum            'C19 H23 Br O3 S'
_chemical_formula_weight         411.34
_chemical_name_common
;
1-Oxa-4-thiaspiro[4.5]decane
;
_chemical_name_systematic
;
2-(6-ethylidene-1-oxa-4-thiaspiro[4.5]decan-7-yl)ethyl 4-bromobenzoate
;
_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'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.09(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.243(2)
_cell_length_b                   11.5410(10)
_cell_length_c                   22.180(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1849.3(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1994)'
_computing_molecular_graphics    TEXSAN
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  .03
_diffrn_reflns_av_sigmaI/netI    .05
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3651
_diffrn_reflns_theta_max         68
_diffrn_reflns_theta_min         5
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.20
_exptl_absorpt_correction_T_max  .68
_exptl_absorpt_correction_T_min  .37
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
via \y-scan (3 reflections; North et al., 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .10
_refine_diff_density_max         .43
_refine_diff_density_min         -.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          .091
_refine_ls_R_factor_gt           .054
_refine_ls_shift/su_max          <0.01
_refine_ls_shift/su_mean         .00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0736P)^2^+2.357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .164
_reflns_number_gt                2207
_reflns_number_total             3372
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1149.cif
_cod_data_source_block           VI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011700
_cod_database_fobs_code          2011700