Bis-3-oxo-λ5-phosphole: Isolation, Structural Analyses, and Synthesis of Phosphorus-ylide Containing Conjugated Heterocycle
Yasunobu Nishimura; Yuka Kawamura; Yutaka Watanabe; Minoru Hayashi; Journal of Organic Chemistry 75 (2010) 3875–3877; doi:10.1021/jo1004235

data_4025450
_publ_contact_author_address
'Dept. of Mat. Sci. & Biotech., Ehime University, Matsuyama 790-8577, Japan'
_publ_contact_author_email       hayashi@eng.ehime-u.ac.jp
_publ_contact_author_fax         +81-89-927-9944
_publ_contact_author_name        'Dr. M. Hayashi'
_publ_contact_author_phone       +81-89-927-9917
_publ_section_title
;
 Bis-3-oxo-\l5-phosphole: Isolation, Structural Analyses, and Synthesis of
 Phosphorus-ylide Containing Conjugated Heterocycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3875
_journal_page_last               3877
_journal_paper_doi               10.1021/jo1004235
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C40 H32 O10 P2, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C44 H40 Cl4 O10 P2'
_chemical_formula_weight         932.50
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 114.524(15)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   13.15(3)
_cell_length_b                   12.75(3)
_cell_length_c                   14.29(3)
_cell_measurement_reflns_used    57
_cell_measurement_temperature    150.0500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1005
_cell_volume                     2180(8)
_computing_cell_refinement       'CrystalClear (Rigaku Corp.,2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp.,2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp.,2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0500
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16357
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9483
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.3000
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+3.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2438
_reflns_number_gt                3659
_reflns_number_total             4966
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo1004235_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4025450