Spontaneous oxidation of organic donors to their cation radicals using Brønsted acids. Identification of the elusive oxidant †
Rathore, Rajendra; Zhu, Chengjian; Lindeman, Sergey V.; Kochi, Jay K.; Journal of the Chemical Society, Perkin Transactions 2  (2000) 1837–; doi:10.1039/b003860l

data_7213371
_publ_section_title
;
 Spontaneous oxidation of organic donors to their cation radicals using
 Br\/onsted acids. Identification of the elusive oxidant&#x200A;&#x2020;
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1837
_journal_paper_doi               10.1039/b003860l
_journal_year                    2000
_chemical_compound_source        'chemical synthesis'
_chemical_formula_sum            'C20 H30'
_chemical_formula_weight         270.44
_chemical_name_systematic
; 
 2,2'-Biadamantane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2428(5)
_cell_length_b                   9.0959(11)
_cell_length_c                   18.4539(13)
_cell_measurement_reflns_used    4247
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1507.7(2)
_computing_cell_refinement       'SAINT V6.01 (BruckerAXS, 1997-99)'
_computing_data_collection       'SMART V5.054 (BruckerAXS, 1997-98)'
_computing_data_reduction        'SAINT & SADABS (Sheldrick, 1998)'
_computing_molecular_graphics    'XP V5.06 (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 & XCIF V5.05 (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Siemens SMART 1K'
_diffrn_measurement_method
;
\w-scan, frame range 0.3 deg, hemisphere
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10681
_diffrn_reflns_theta_max         35.49
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.5
_diffrn_standards_number         201
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.1621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1349
_refine_ls_wR_factor_obs         0.1039
_reflns_number_observed          2493
_reflns_number_total             3308
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003860lsup1.cif
_cod_data_source_block           rajxtsx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.1621P] 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^)+(0.0623P)^2^+0.1621P] 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      C2/c
_cod_database_code               7213371