A Trimer from 5,5-Dimethylcyclohexan-1,3-dione Containing an O-Protonated Furan Ring
Barnes, J. C.; Acta Crystallographica Section C 52 (1996) 262–264; doi:10.1107/S0108270195009279

data_2004406
_publ_section_title
;
 A Trimer from 5,5-Dimethylcyclohexan-1,3-dione Containing an
 O-Protonated Furan Ring
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              262
_journal_page_last               264
_journal_paper_doi               10.1107/S0108270195009279
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C24 H31.5 O5.43'
_chemical_formula_weight         406.79
_chemical_melting_point          ' 235\% C with decomposition'
_chemical_name_systematic
;
 1,2,3,4,6,7,8,9,11,12,13,14-dodecahydro-1,6,14-trioxo-
benzo[b]benzo[4,5]furo[3,2-d]oxoninium hydroxide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.722(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9030(10)
_cell_length_b                   22.275(2)
_cell_length_c                   14.6622(9)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2243.3(4)
_computing_cell_refinement       'FAST-MADNESS system'
_computing_data_collection       'FAST-MADNESS system (Enraf-Nonius, 1990)'
_computing_data_reduction        'FAST-MADNESS system'
_computing_molecular_graphics    'PLATON93 (Spek, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measurement_device
;
Enraf-Nonius CAD-4 FAST area-detector diffractometer
;
_diffrn_measurement_method       area-detector
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7873
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        insignificant
_diffrn_standards_number
;
Intensity  standards  were  not  measured  by  the  area  detector.
Possible  variations were checked by comparing the intensities of common
or   symmetry   related  reflections  as  they  occur  during  data
collection.  In this case no variation was noted.
;
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.85
_refine_ls_goodness_of_fit_obs   1.006
_refine_ls_hydrogen_treatment    'riding model, refine H12, H30'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_restrained_S_obs      1.006
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_obs          0.056
_refine_ls_shift/esd_max         -0.04
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0921P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.157
_refine_ls_wR_factor_obs         0.1328
_reflns_number_observed          2306
_reflns_number_total             3481
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1137.cif
_cod_data_source_block           ndk55b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0921P)^2^] 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^)+(0.0921P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C24 H31.50 O5.43'
_cod_database_code               2004406