Structural Aspects of the Nucleophilic Attack of Ketone Enolate on Dehydrodihydropyran
Ianelli, S.; Nardelli, M.; Belletti, D.; Jamart-Grégoire, B.; Mercier-Girardot, S.; Caubère, P.; Acta Crystallographica Section C 52 (1996) 237–244; doi:10.1107/S0108270195010134

data_2004446
_publ_section_title
;
 Structural Aspects of the Nucleophilic Attack of Ketone Enolate on
 Dehydrodihydropyran
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              237
_journal_page_last               244
_journal_paper_doi               10.1107/S0108270195010134
_journal_volume                  52
_journal_year                    1996
_chemical_formula_analytical     'C12 H18 O2 S'
_chemical_formula_sum            'C12 H18 O2 S'
_chemical_formula_weight         226.33
_chemical_name_systematic
;
(1SR,2RS,8RS)8-methylthio-3-oxatricyclo[6.4.0.0^2,7^]dodec-6-en-1-ol
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.370(10)
_cell_angle_beta                 93.660(10)
_cell_angle_gamma                98.310(10)
_cell_formula_units_Z            2
_cell_length_a                   11.031(2)
_cell_length_b                   8.3000(10)
_cell_length_c                   6.6250(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39
_cell_measurement_theta_min      25
_cell_volume                     583.44(16)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material
;
 PARST, Nardelli (1983); PARSTCIF (Nardelli, 1991)
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'fine focus X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0090
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2231
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_max         70.24
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
prisms
;
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.323
_refine_ls_extinction_coef       0.0118(16)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_obs          0.0322
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(F~o~^2^)+( 0.0626P)^2^] where P=(F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1007
_refine_ls_wR_factor_obs         0.0899
_reflns_number_observed          1913
_reflns_number_total             2218
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sz1044.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(F~o~^2^)+(
0.0626P)^2^] where P=(F~o~^2^+2F~c~^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^(F~o~^2^)+( 0.0626P)^2^] where
P=(F~o~^2^+2F~c~^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        583.4(2)
_cod_database_code               2004446