Allyl Radical Nature of a Phenylcyclopentadienyl Radical Annelated with Two Homoadamantene Frameworks
Kohei Ogawa; Koichi Komatsu; Toshikazu Kitagawa; Journal of Organic Chemistry 76 (2011) 6095–6100; doi:10.1021/jo200748m

data_4026480
_publ_section_title
;
 Allyl Radical Nature of a Phenylcyclopentadienyl Radical Annelated with
 Two Homoadamantene Frameworks
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6095
_journal_page_last               6100
_journal_paper_doi               10.1021/jo200748m
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C29 H33 O, F6 Sb, C H2 Cl2'
_chemical_formula_sum            'C30 H35 Cl2 F6 O Sb'
_chemical_formula_weight         718.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 112.361(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.787(3)
_cell_length_b                   15.652(4)
_cell_length_c                   15.063(4)
_cell_measurement_temperature    100(2)
_cell_volume                     3006.1(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  '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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11076
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.8018
_exptl_absorpt_correction_T_min  0.7231
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+13.9364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                3812
_reflns_number_total             5173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200748m_si_003.cif
_cod_data_source_block           8+SbF6-
_cod_original_cell_volume        3006.2(12)
_cod_database_code               4026480