Stereoselective PCO/POC-Rearrangement of P-C-Cage Phosphorane in the Reaction of 4,5-Dimethyl-2-(2-oxo-1,2-diphenyl)ethoxy-1,3,2-dioxaphospholane with Hexafluoroacetone.
Mironov, Vladimir F.; Dimukhametov, Mudaris N.; Efimov, Sergey V.; Aminova, Roza M.; Karataeva, Farida Kh; Krivolapov, Dmitry B.; Mironova, Ekaterina V.; Klochkov, Vladimir V.; The Journal of organic chemistry 81 (2016) 5837–5850; doi:10.1021/acs.joc.6b00356

data_4036726
_publ_section_title
;
 Stereoselective PCO/POC-Rearrangement of P-C-Cage Phosphorane in the
 Reaction of
 4,5-Dimethyl-2-(2-oxo-1,2-diphenyl)ethoxy-1,3,2-dioxaphospholane with
 Hexafluoroacetone.
;
_journal_issue                   14
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5837
_journal_page_last               5850
_journal_paper_doi               10.1021/acs.joc.6b00356
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C21 H19 F6 O5 P'
_chemical_formula_sum            'C21 H19 F6 O5 P'
_chemical_formula_weight         496.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.259(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.079(5)
_cell_length_b                   9.051(3)
_cell_length_c                   15.770(5)
_cell_measurement_reflns_used    5864
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.58
_cell_volume                     2152.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4198
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.583
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Smart Apex2'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+1.7718P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3580
_reflns_number_total             4198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00356_si_005.cif
_cod_data_source_block           9_1451981
_cod_original_cell_volume        2152.2(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4036726
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2013-2
_shelx_res_checksum              6057
_shelx_hkl_checksum              55050