Phosphonium-Iodonium Ylides with Heteroatomic Groups in the Synthesis of Annelated P-Containing Heterocycles
Elena D. Matveeva; Tatyana A. Podrugina; Marina A. Taranova; Dmitriy S. Vinogradov; Rolf Gleiter; Nikolay S. Zefirov; Journal of Organic Chemistry 78 (2013) 11691–11697; doi:10.1021/jo401514d

data_4028772
_publ_section_title
;
 Phosphonium-Iodonium Ylides with Heteroatomic Groups in the Synthesis of
 Annelated P-Containing Heterocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11691
_journal_page_last               11697
_journal_paper_doi               10.1021/jo401514d
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C31 H30 O3 P2'
_chemical_formula_weight         512.49
_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                 94.720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.170(2)
_cell_length_b                   12.496(2)
_cell_length_c                   23.338(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2665.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0929P)^2^+1.8963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                3463
_reflns_number_total             4662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401514d_si_001.cif
_cod_data_source_block           z2
_cod_database_code               4028772