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_4026479
_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_sum            'C41 H57 K O3'
_chemical_formula_weight         636.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 93.433(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7713(12)
_cell_length_b                   18.247(2)
_cell_length_c                   17.767(2)
_cell_measurement_temperature    100(2)
_cell_volume                     3485.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10126
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.9630
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.453
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.464
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2369
_refine_ls_wR_factor_ref         0.3209
_reflns_number_gt                4706
_reflns_number_total             5410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200748m_si_002.cif
_cod_data_source_block           K+3-
_cod_original_cell_volume        3485.8(7)
_cod_database_code               4026479