2,4-Di-<i>tert</i>-butyl-6-[(<i>R</i>/<i>S</i>)-1-(3,5-di-<i>tert</i>-butyl-2-hydroxyphenyl)ethyl]phenyl [(1<i>R</i>,4<i>S</i>)-7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl]methanesulfonate
Wang, Cheng; Wu, Jincai; Acta Crystallographica Section E 68 (2012) o93–; doi:10.1107/S1600536811052664

data_2233225
_publ_section_title
;
 2,4-Di-<i>tert</i>-butyl-6-[(<i>R</i>/<i>S</i>)-1-(3,5-di-<i>tert</i>-butyl-2-hydroxyphenyl)ethyl]phenyl
 [(1<i>R</i>,4<i>S</i>)-7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl]methanesulfonate
;
_journal_coeditor_code           KP2372
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o93
_journal_paper_doi               10.1107/S1600536811052664
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C40 H60 O5 S1'
_chemical_formula_moiety         'C40 H60 O5 S1'
_chemical_formula_sum            'C40 H60 O5 S'
_chemical_formula_weight         652.98
_chemical_name_systematic
;
2,4-Di-<i>tert</i>-butyl-6-[(<i>R</i>/<i>S</i>)-1-(3,5-di-<i>tert</i>-butyl-2-
hydroxyphenyl)ethyl]phenyl
[(1<i>R</i>,4<i>S</i>)-7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-
yl]methanesulfonate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.003(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2082(19)
_cell_length_b                   10.6028(11)
_cell_length_c                   20.287(2)
_cell_measurement_reflns_used    5452
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.24
_cell_volume                     3911.2(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21496
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.348
_refine_ls_abs_structure_details 'Flack (1983), 5058 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.12(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13182
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.2034
_reflns_number_gt                7458
_reflns_number_total             13182
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kp2372.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C40 H60 O5 S1'
_cod_database_code               2233225
_cod_database_fobs_code          2233225