Direct Arylations for Study of the Air-Stable P-Heterocyclic Biradical: From Wide Electronic Tuning to Characterization of the Localized Radicalic Electrons
Shigekazu Ito; Yasuhiro Ueta; Trang Thi Thu Ngo; Makoto Kobayashi; Daisuke Hashizume; Jun-ichi Nishida; Yoshiro Yamashita; Koichi Mikami; Journal of the American Chemical Society 135 (2013) 17610–17616; doi:10.1021/ja409625x

data_4121182
_publ_section_title
;
 Direct Arylations for Study of the Air-Stable P-Heterocyclic Biradical:
 From Wide Electronic Tuning to Characterization of the Localized
 Radicalic Electrons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17610
_journal_page_last               17616
_journal_paper_doi               10.1021/ja409625x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C57.5 H78 Cl N3 P2'
_chemical_formula_weight         908.62
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.3701(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.9518(12)
_cell_length_b                   21.0329(8)
_cell_length_c                   19.4833(6)
_cell_measurement_temperature    123(2)
_cell_volume                     10827.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46914
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.9689
_exptl_absorpt_correction_T_min  0.9376
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         12368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                8673
_reflns_number_total             12368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409625x_si_002.cif
_cod_data_source_block           ueta
_cod_original_formula_sum        'C57.50 H78 Cl N3 P2'
_cod_database_code               4121182