Bis-phosphoryl-bridged stilbenes synthesized by an intramolecular cascade cyclization.
Fukazawa, Aiko; Hara, Masanao; Okamoto, Toshihiro; Son, Eun-Cheol; Xu, Caihong; Tamao, Kohei; Yamaguchi, Shigehiro; Organic letters 10 (2008) 913–916; doi:10.1021/ol7030608

data_1504549
_publ_section_title
;
 Bis-phosphoryl-bridged stilbenes synthesized by an intramolecular cascade
 cyclization.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              913
_journal_page_last               916
_journal_paper_doi               10.1021/ol7030608
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C26 H18 O2 P2'
_chemical_formula_weight         424.34
_chemical_name_common            cis-1
_chemical_name_systematic
; 
 cis-P,P'-diphenyl-benzophospholo[3,2-b]benzophosphole-P,P'-dioxide 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.697(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.45(3)
_cell_length_b                   8.41(3)
_cell_length_c                   17.47(4)
_cell_measurement_temperature    123(2)
_cell_volume                     2071(10)
_computing_cell_refinement       'CrystalClear 1.3.5 (Rigaku Corp)'
_computing_data_collection       'CrystalClear 1.3.5 (Rigaku Corp)'
_computing_data_reduction        'CrystalClear 1.3.5 (Rigaku Corp)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, 2005)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13303
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_correction_T_min  0.9553
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+3.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                3013
_reflns_number_total             3623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7030608-file004.cif
_cod_data_source_block           hcis
_cod_original_cell_volume        2072(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1504549