The suitability of anion-accelerated oxy-Cope rearrangement as a probe to study π-facial selectivity. An experimental study with (6-methyl-1-oxa-4-thiaspiro[4.5]dec-6-en-7-yl)(allyl)methanols †
Yadav, Veejendra K.; Jeyaraj, Duraiswamy A.; Parvez, Masood; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1423–; doi:10.1039/a909839i

data_7213247
_publ_contact_author
;
Masood Parvez
Department of Chemistry
University of Calgary
2500 University Drive N.W.
Calgary, Alberta
Canada
T2N 1N4
;
_publ_section_title
;
 The suitability of anion-accelerated oxy-Cope rearrangement as a probe to
 study \p-facial selectivity. An experimental study with
 (6-methyl-1-oxa-4-thiaspiro[4.5]dec-6-en-7-yl)(allyl)methanols&#x200A;&#x2020;
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1423
_journal_paper_doi               10.1039/a909839i
_journal_year                    2000
_chemical_formula_sum            'C19 H26 O2 S'
_chemical_formula_weight         318.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             1999-01-20
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                111.965(14)
_cell_angle_beta                 106.941(15)
_cell_angle_gamma                90.328(17)
_cell_formula_units_Z            4
_cell_length_a                   12.2879(19)
_cell_length_b                   13.883(3)
_cell_length_c                   11.625(2)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    170.2
_cell_measurement_theta_max      10.6
_cell_measurement_theta_min      9.0
_cell_volume                     1744.6(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      170.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01862
_diffrn_orient_matrix_UB_12      0.06530
_diffrn_orient_matrix_UB_13      0.06168
_diffrn_orient_matrix_UB_21      0.02629
_diffrn_orient_matrix_UB_22      -0.02578
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_diffrn_orient_matrix_UB_31      0.07951
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_diffrn_orient_matrix_UB_33      0.02405
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03499
_diffrn_reflns_av_sigmaI/netI    0.110
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8439
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0.20
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
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_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colorless
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_exptl_crystal_density_meas      ?
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_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.30
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_refine_ls_goodness_of_fit_obs   1.896
_refine_ls_hydrogen_treatment    noref
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_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.0038
_refine_ls_shift/esd_mean        0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00008|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0489
_refine_ls_wR_factor_obs         0.0489
_reflns_number_observed          3464
_reflns_number_total             8052
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            a909839isup1.cif
_cod_data_source_block           Y-10
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00008|Fo|^2^]' 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) + 0.00008|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1744.5(6)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C19 H26 O2 S '
_cod_database_code               7213247