Absolute configuration of the newly formed asymmetric centre in (1<i>R</i>,5<i>R</i>,8<i>S</i>)-8-benzyloxy-2,6-dioxabicyclo[3.2.1]octan-3-one
Koman, Marian; Babjak Matej; Gracza Tibor; Glowiak Tadeusz; Acta Crystallographica Section E 57 (2001) o360–o361; doi:10.1107/S1600536801004196

data_2200243
_publ_section_title
;Absolute configuration of the newly formed asymmetric centre in
 (1<i>R</i>,5<i>R</i>,8<i>S</i>)-8-benzyloxy-2,6-dioxabicyclo[3.2.1]octan-3-one
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o360
_journal_page_last               o361
_journal_paper_doi               10.1107/S1600536801004196
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C13 H14 O4'
_chemical_formula_moiety         'C13 H14 O4'
_chemical_formula_sum            'C13 H14 O4'
_chemical_formula_weight         234.24
_chemical_name_systematic
;
(1R,5R,8S)-8-benzyloxy-2,6-dioxabicyclo[3.2.1]octane-3-one
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7290(10)
_cell_length_b                   10.079(2)
_cell_length_c                   19.622(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      5.2
_cell_volume                     1133.0(4)
_computing_cell_refinement       'P2~1~ Software'
_computing_data_collection       'P2~1~ Software (Syntex, 1973)'
_computing_data_reduction        'XP21 (Pavel\<c\'ik, 1993)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'syntex P2~1~'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .056
_diffrn_reflns_av_sigmaI/netI    .051
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            2583
_diffrn_reflns_theta_max         80.1
_diffrn_reflns_theta_min         4.5
_diffrn_standards_decay_%        15
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .845
_exptl_absorpt_correction_T_max  .845
_exptl_absorpt_correction_T_min  .656
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .20
_refine_diff_density_max         .19
_refine_diff_density_min         -.26
_refine_ls_abs_structure_details '(Flack, 1983). No Fridel pairs.'
_refine_ls_abs_structure_Flack   -.03(19)
_refine_ls_extinction_coef       .0083(9)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_all   1.09
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_restrained_S_obs      1.13
_refine_ls_R_factor_all          .043
_refine_ls_R_factor_gt           .033
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0550P]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .091
_refine_ls_wR_factor_ref         .088
_reflns_number_gt                1969
_reflns_number_total             2259
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6004.cif
_cod_data_source_block           I
_cod_database_code               2200243