1,3,5-Tri-<i>tert</i>-butyl-5-(1,3,5-tri-<i>tert</i>-butyl-4-oxo-2,5-cyclohexadienyl)methylbicyclo[4.1.0]hept-3-en-2-one, a Highly Hindered Propane
Rieker, A.; Neumayer, M.; Hiller, W.; Acta Crystallographica Section C 52 (1996) 2351–2353; doi:10.1107/S0108270196004465

data_2005426
_publ_contact_author
;
   Prof. Dr. Wolfgang Hiller
   Anorganisch-Chemisches Institut der Technischen Universit\"at M\"unchen
   Lichtenbergstrasse 4
   D-85747 Garching
   Germany
;
_publ_section_title
;1,3,5-Tri-<i>tert</i>-butyl-5-(1,3,5-tri-<i>tert</i>-butyl-4-oxo-2,5-cyclohexadienyl)methylbicyclo[4.1.0]hept-3-en-2-one,
 a Highly Hindered Propane
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2351
_journal_page_last               2353
_journal_paper_doi               10.1107/S0108270196004465
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C38 H62 O2'
_chemical_formula_sum            'C38 H62 O2'
_chemical_formula_weight         550.88
_chemical_name_systematic
;
5-(1,3,5-Tri-tert.-butyl-4-hydroxybenzyl)-1,3,5,tri-tert.-butyl-2-oxo-
bicyclo[4.1.0]hept-3-en
;
_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 SHELXL93'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.73(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.757(2)
_cell_length_b                   11.099(2)
_cell_length_c                   20.165(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    211(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      8
_cell_volume                     3507.6(9)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CADSHEL (Kopf & R\"ubcke, 1993)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      211(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6847
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.011
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.0
_refine_ls_shift/esd_mean        0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.4863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1137
_refine_ls_wR_factor_obs         0.0940
_reflns_number_observed          3967
_reflns_number_total             6097
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            sk1019.cif
_cod_data_source_block           global
_cod_depositor_comments
;
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^)+(0.0372P)^2^+1.4863P] 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^)+(0.0372P)^2^+1.4863P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3507.6(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005426