Preparation of Allenephosphoramide and Its Utility in the Preparation of 4,9-Dihydro-2H-benzo[f]isoindoles
Yin, Guangwei; Zhu, Yuanxun; Zhang, Li; Lu, Ping; Wang, Yanguang; Organic Letters 13 (2011) 940–943; doi:10.1021/ol102992n

data_1516230
_publ_section_title
;
 Preparation of Allenephosphoramide and Its Utility in the Preparation of
 4,9-Dihydro-2H-benzo[f]isoindoles
;
_journal_coden_ASTM              ORLEF7
_journal_issue                   5
_journal_name_full               'Organic Letters'
_journal_page_first              940
_journal_page_last               943
_journal_paper_doi               10.1021/ol102992n
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C32 H32 N O3 P'
_chemical_formula_weight         509.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 125.507(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   42.662(5)
_cell_length_b                   9.5733(6)
_cell_length_c                   33.755(4)
_cell_measurement_reflns_used    30725
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      3.21
_cell_volume                     11222(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30725
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                5089
_reflns_number_total             11572
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             1501944
_cod_data_source_file            ol102992n_si_002.cif
_cod_data_source_block           ygw560_174a
_cod_original_cell_volume        11222(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1516230