Stereochemistry of Hydroxylation Reactions on Polycyclic Pyrans
Ianelli, S.; Nardelli, M.; Belletti, D.; Jamart-Grégoire, B.; Mercier-Girardot, S.; Caubère, P.; Acta Crystallographica Section C 51 (1995) 1885–1889; doi:10.1107/S0108270195001442

data_2003927
_publ_section_title
;
 Stereochemistry of Hydroxylation Reactions on Polycyclic Pyrans
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1885
_journal_page_last               1889
_journal_paper_doi               10.1107/S0108270195001442
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;
chemical synthesis
;
_chemical_formula_analytical     'C15 H26 O6'
_chemical_formula_sum            'C15 H26 O6'
_chemical_formula_weight         302.37
_chemical_name_systematic
;(1SR,2RS,9RS,10RS,14SR)-9-acetoxy-11-oxatricyclo[8.4.0.0^2,9^]tetradec-6,7-diol
monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 97.14(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.355(7)
_cell_length_b                   16.648(5)
_cell_length_c                   9.181(2)
_cell_measurement_radiation      'Cu K\a~1~'
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39
_cell_measurement_theta_min      20
_cell_measurement_wavelength     1.540562
_cell_volume                     3087.0(16)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics
'ORTEP (Johnson, 1965); PLUTO (Motherwell & Clegg, 1976)'
_computing_publication_material
'PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR88 (Burla, et al., 1988)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'fine focus X-ray tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5405620
_diffrn_reflns_av_R_equivalents  .0291
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -024
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -020
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -011
_diffrn_reflns_number            5759
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_max         70.21
_diffrn_reflns_theta_min         3.44
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    .787
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
small prisms
;
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          .51
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .29
_refine_diff_density_max         .30
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       .0090(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_obs          .0374
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(F~o~^2^)+(0.0679P)^2^] where P=(F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1071
_refine_ls_wR_factor_obs         .1024
_reflns_number_observed          2282
_reflns_number_total             2939
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            mu1167.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(F~o~^2^)+(0.0679P)^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^)+(0.0679P)^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        3087(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2003927