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_4121186
_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_moiety         'C49 H74 P2'
_chemical_formula_sum            'C49 H74 P2'
_chemical_formula_weight         725.02
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 95.4413(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4396(3)
_cell_length_b                   23.2554(3)
_cell_length_c                   10.9080(1)
_cell_measurement_reflns_used    297358
_cell_measurement_temperature    90
_cell_measurement_theta_max      45.29
_cell_measurement_theta_min      1.46
_cell_volume                     4403.97(10)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    SV
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            294615
_diffrn_reflns_theta_full        45.29
_diffrn_reflns_theta_max         45.29
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.99292
_exptl_absorpt_correction_T_min  0.98632
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 N.W. Alcock (1970). Cryst. Computing, p271
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         36568
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                22982
_reflns_number_total             36568
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja409625x_si_007.cif
_cod_data_source_block           asymmetric-conventional
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4121186