Dispiroketals in synthesis. Part 25.1 Further reactions of dispiroketal protected glycolate to afford optically active 1,2,3,4-tetraols
Fujita, Morifumi; Lainé, Dramane; Ley, Steven V.; Journal of the Chemical Society, Perkin Transactions 1  (1999) 1647–; doi:10.1039/a900951e

data_7213032
_publ_section_title
;
 Dispiroketals in synthesis. Part 25.1 Further reactions of dispiroketal
 protected glycolate to afford optically active 1,2,3,4-tetraols
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1647
_journal_paper_doi               10.1039/a900951e
_journal_year                    1999
_chemical_formula_sum            'C19 H24 O6'
_chemical_formula_weight         348.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                112.210(10)
_cell_angle_beta                 117.65(2)
_cell_angle_gamma                75.36(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7660(10)
_cell_length_b                   11.5680(10)
_cell_length_c                   9.3670(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     864.0(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'R-AXIS IIc'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7486
_diffrn_reflns_theta_max         25.28
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       white
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.3050(175)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.203
_refine_ls_goodness_of_fit_obs   1.216
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_restrained_S_obs      1.216
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_obs          0.0527
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.2329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1252
_refine_ls_wR_factor_obs         0.1204
_reflns_number_observed          2666
_reflns_number_total             2850
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900951esup1.cif
_cod_data_source_block           sl9704
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.2329P] where P=(Fo^2^+2Fc^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^(Fo^2^)+(0.0521P)^2^+0.2329P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        863.95(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213032