Twinned Crystal Structure of Bis(2-hydroxy-4,4-dimethyl-6-oxo-1-cyclohexenyl)phenylmethane at 150K
Bolte, M.; Degen, A.; Rühl, S.; Acta Crystallographica Section C 53 (1997) 340–342; doi:10.1107/S0108270196013078

data_2006016
_publ_section_title
;
 Twinned Crystal Structure of
 Bis(2-hydroxy-4,4-dimethyl-6-oxo-1-cyclohexenyl)phenylmethane at 150K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              340
_journal_page_last               342
_journal_paper_doi               10.1107/S0108270196013078
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C23 H28 O4'
_chemical_formula_weight         368.45
_chemical_name_systematic
;
[Bis-(2-Hydroxy-4,4-dimethyl-6-oxo-1-cyclohexenyl)]-phenyl-methane
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   20.7727(2)
_cell_length_b                   20.7727(2)
_cell_length_c                   36.6751(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.00
_cell_volume                     15825.5(2)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device       'Siemens CCD three-circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            74624
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  480
_diffrn_standards_number         1049
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.180
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_obs          0.0392
_refine_ls_shift/esd_max         0.119
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0292P)^2^+9.3976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0855
_refine_ls_wR_factor_obs         0.0825
_reflns_number_observed          7442
_reflns_number_total             7940
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1062.cif
_cod_data_source_block           p1twin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0292P)^2^+9.3976P] 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^)+(0.0292P)^2^+9.3976P] 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      'I 41/a'
_cod_database_code               2006016
_cod_database_fobs_code          2006016