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_1516500
_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_moiety         'C38 H36 P2 S2'
_chemical_formula_sum            'C38 H36 P2 S2'
_chemical_formula_weight         618.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.378(6)
_cell_angle_beta                 91.446(5)
_cell_angle_gamma                107.726(6)
_cell_formula_units_Z            2
_cell_length_a                   9.151(5)
_cell_length_b                   12.814(8)
_cell_length_c                   15.408(9)
_cell_measurement_temperature    120(2)
_cell_volume                     1607.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.8923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0598P)^2^+0.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                4636
_reflns_number_total             5462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol501189u_si_002.cif
_cod_data_source_block           trpoles20128
_cod_depositor_comments
'Adding full bibliography for 1516499--1516500.cif.'
_cod_original_cell_volume        1607.3(16)
_cod_database_code               1516500