Synthesis of the Phenoxonium Cation of an α-Tocopherol Model Compound Crystallized with Non-Nucleophilic [B(C6F5)4]-and (CB11H6Br6)- Anions
Stephen B. Lee; Anthony C. Willis; Richard D. Webster; Journal of the American Chemical Society 128 (2006) 9332–9333; doi:10.1021/ja0634268

data_4110733
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 Synthesis of the Phenoxonium Cation of an \a-Tocopherol Model Compound
 Crystallized with Non-Nucleophilic [B(C6F5)4]-and (CB11H6Br6)- Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9332
_journal_page_last               9333
_journal_paper_doi               10.1021/ja0634268
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        local
_chemical_formula_moiety
;
C14 H19 O2 +, C H5.98 B11 Br6.02 -, C2 H4 Cl2
;
_chemical_formula_sum            'C17 H28.98 B11 Br6.02 Cl2 O2'
_chemical_formula_weight         936.19
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-02-15
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2006-02-15 - Report on C17 H29 B11 Br6 Cl2 O2 
             by Anthony C. Willis
             for  Stephen B. Lee and Richard D. Webster

2006-02-15 - passes checkcif tests with minor warnings  

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.5677(2)
_cell_length_b                   20.2995(3)
_cell_length_c                   27.9851(6)
_cell_measurement_reflns_used    272638
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     6571.4(2)
_computing_cell_refinement       'Denzo/Scalepack '
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS '
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68824
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.767
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.536
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       plate
_exptl_crystal_F_000             3573.271
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.7283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5806
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.006837
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0716
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0716
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                3223
_reflns_number_total             5825
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.55
_oxford_diffrn_Wilson_scale      127.59
_oxford_refine_ls_scale          0.12598(3)
_oxford_structure_analysis_title '2061451 web0601'
_cod_data_source_file            ja0634268si20060516_092513.cif
_cod_data_source_block           web0601
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4110733