(1<i>RS</i>,3<i>SR</i>,4<i>RS</i>,5<i>RS</i>,7<i>SR</i>,9<i>SR</i>)-4,7-Diacetyl-9-hydroxy-1,3,5,9-tetramethyl-2,6,8-trioxatricyclo[3.2.1.1^3,7^]nonane: a Tricyclic System Formed Under Cathodic Conditions
Raabe, Gerhard; Hall, Sydney R.; .; Thomas, Hans Günter; .; Wellen, Ulrich; .; Simons, Josef; .; Acta Crystallographica Section C 53 (1997) 1107–1111; doi:10.1107/S0108270197005477

data_2006402
_publ_contact_author
;
  Dr. Gerhard Raabe
  Institut fuer Organische Chemie
  Prof.-Pirlet-Strasse 1
  D-52056 Aachen
  Germany
;
_publ_section_title
;(1<i>RS</i>,3<i>SR</i>,4<i>RS</i>,5<i>RS</i>,7<i>SR</i>,9<i>SR</i>)-4,7-Diacetyl-9-hydroxy-1,3,5,9-tetramethyl-2,6,8-trioxatricyclo[3.2.1.1^3,7^]nonane:
 a Tricyclic System Formed Under Cathodic Conditions
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1107
_journal_page_last               1111
_journal_paper_doi               10.1107/S0108270197005477
_journal_volume                  53
_journal_year                    1997
_chemical_formula_analytical     'C14 H20 O6'
_chemical_formula_moiety         'C14 H20 O6'
_chemical_formula_structural     '(C6 H O3) (CH3)4 (COCH3)2 (OH)'
_chemical_formula_sum            'C14 H20 O6'
_chemical_formula_weight         284.3
_chemical_melting_point          411
_chemical_name_systematic
;
(1RS,3SR,4RS,5RS,7SR,9SR)-4,7-diacetyl-9-hydroxy-1,3,5,9-tetramethyl
-2,6,8-trioxatricyclo[3.2.1.1^3,7^]nonane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 99.369(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            24
_cell_length_a                   8.6760(10)
_cell_length_b                   44.948(2)
_cell_length_c                   22.143(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      33.6
_cell_measurement_theta_min      13.3
_cell_volume                     8519.9(13)
_computing_cell_refinement       'CELDIM (Rettig, 1989)'
_computing_data_collection
'CAD4 (Schagen, Straver, Van Meurs & Williams (1989)'
_computing_data_reduction
;  DIFDAT (Stewart et al., 1992),
   SORTRF (Hall, Spadaccini & Stewart, 1992),
   ADDREF (Davenport & Hall, 1992)
;
_computing_molecular_graphics
'ORTEP (Davenport, Hall & Dreissig, 1992; Johnson, 1965)'
_computing_publication_material
; BONDLA (Dreissig, Doherty, Stewart & Hall, 1992),
  ATABLE (Englehardt & Hall, 1992),
  CIFIO (Hall, 1992b)
;
_computing_structure_refinement  'CRYLSQ  (Olthof-Hazekamp, 1992)'
_computing_structure_solution
'GENSIN (Subramanian & Hall, 1992), GENTAN (Hall, 1992a)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17485
_diffrn_reflns_reduction_process 'No monochromator, Lp applied'
_diffrn_reflns_theta_max         74.99
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3647.62
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.21
_refine_diff_density_max         .458
_refine_diff_density_min         -.65
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       42E2(3)
_refine_ls_extinction_method     'Zachariasen (Zachariasen, 1967; Larson, 1970)'
_refine_ls_goodness_of_fit_all   1.986
_refine_ls_goodness_of_fit_obs   2.529
_refine_ls_hydrogen_treatment    ' H-atom treatment: see text'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .105
_refine_ls_R_factor_obs          .059
_refine_ls_shift/esd_max         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .074
_refine_ls_wR_factor_obs         .067
_reflns_number_observed          9141
_reflns_number_total             16793
_reflns_observed_criterion       refl_observed_if_Inet_>_2.000_sigma(Inet)
_cod_data_source_file            ka1225.cif
_cod_data_source_block           gr0008
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8520.0(10)
_cod_original_sg_symbol_Hall     -P_2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006402