Synthesis of π-Extended Dibenzophospholes by Intramolecular Radical Cyclization and Their Properties.
Furukawa, Shunsuke; Haga, Shunsuke; Kobayashi, Junji; Kawashima, Takayuki; Organic letters 16 (2014) 3228–3231; doi:10.1021/ol501189u

data_1516499
_publ_section_title
;
 Synthesis of \p-Extended Dibenzophospholes by Intramolecular Radical
 Cyclization and Their Properties.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              3228
_journal_page_last               3231
_journal_paper_doi               10.1021/ol501189u
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C38 H36 P2 S2'
_chemical_formula_weight         618.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 98.7827(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.201(5)
_cell_length_b                   19.080(9)
_cell_length_c                   16.886(8)
_cell_measurement_reflns_used    5667
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0402
_cell_volume                     3248(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20685
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.9717
_exptl_absorpt_correction_T_min  0.8933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.6419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                4306
_reflns_number_total             5667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol501189u_si_003.cif
_cod_data_source_block           synPS_2
_cod_depositor_comments
'Adding full bibliography for 1516499--1516500.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1516499