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_2004445
_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     'C14 H16 O2'
_chemical_formula_sum            'C14 H16 O2'
_chemical_formula_weight         216.28
_chemical_name_systematic
;
(6SR,7RS,8SR)-7-methyl-8-phenyl-3-oxabicyclo[4.2.0]oct-1-en-8-ol
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   16.305(7)
_cell_length_b                   10.366(4)
_cell_length_c                   6.900(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      23
_cell_volume                     1166.2(10)
_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, 1983a); 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 scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5405620
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2508
_diffrn_reflns_reduction_process
;
Standard Lorentz & polarization correction
;
_diffrn_reflns_theta_max         70.12
_diffrn_reflns_theta_min         5.06
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablets
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.163
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_coef       0.107(5)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.280
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.369
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[\s^2^(F~o~^2^)+(0.0539P)^2^+0.1849P]
  where P=(F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1340
_refine_ls_wR_factor_obs         0.0975
_reflns_number_observed          1821
_reflns_number_total             2209
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sz1044.cif
_cod_data_source_block           8
_cod_original_cell_volume        1166.2(9)
_cod_database_code               2004445