An X-ray diffraction study of partially ordered electron density in clathrates of Dianin's compound that include simple carboxylic acids
Small, Ronald W. H.; Acta Crystallographica Section B 59 (2003) 141–148; doi:10.1107/S0108768102022395

data_2103819
_publ_section_title
;
 An X-ray diffraction study of partially ordered electron density in
 clathrates of Dianin's compound that include simple carboxylic acids
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              141
_journal_page_last               148
_journal_paper_doi               10.1107/S0108768102022395
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         '3(C18 H20 O2),(C2 F3 O2)'
_chemical_formula_structural     '(C18 H20 O2), 1/3(C2 F3 O2)'
_chemical_formula_sum            'C56 H61 F3 O8'
_chemical_formula_weight         919.02
_chemical_name_common            'Dianins compound-trifluoroacetic acid'
_chemical_name_systematic
;
[4-p-hydroxyphenyl-2,2,4-trimethylchroman]-trifluoroacetic acid
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   27.19(2)
_cell_length_b                   27.19(2)
_cell_length_c                   11.097(10)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      5
_cell_volume                     7105(10)
_computing_cell_refinement       local
_computing_data_collection       'Stoe STADI-2'
_computing_data_reduction        SMALL
_computing_molecular_graphics    SNOOPI
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  SHELX76
_computing_structure_solution    MULTAN87
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Stoe STADI-2 two circle diffractometer'
_diffrn_measurement_method
;
variable \w scan 2\q' fixed,  where the angle \q' is the projection
of \q on the equatorial plane
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.109
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4176
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        'maximum 5% corrected by intepolation'
_diffrn_standards_interval_count 20
_diffrn_standards_number         'one per layer'
_exptl_absorpt_coefficient_mu    0.09
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       'acicular, hexagonal prism'
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.81
_refine_ls_hydrogen_treatment    ' see text '
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1013
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.00019F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.083
_refine_ls_wR_factor_ref         0.083
_reflns_number_gt                1013
_reflns_number_total             1521
_reflns_threshold_expression     refl_obs_if_F_>_6.0_sigma(F)
_cod_data_source_file            bm0059.cif
_cod_data_source_block           DIT
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Trigonal' changed to 'trigonal' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2103819