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_4036729
_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         'C17 H12 F6 O2'
_chemical_formula_sum            'C17 H12 F6 O2'
_chemical_formula_weight         362.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                71.020(11)
_cell_angle_beta                 82.779(12)
_cell_angle_gamma                75.326(11)
_cell_formula_units_Z            2
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_cell_length_b                   11.279(12)
_cell_length_c                   11.328(12)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.07
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_computing_cell_refinement       'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8265
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'sealed tube'
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_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.489
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.489
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1873
_reflns_number_total             3180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00356_si_005.cif
_cod_data_source_block           14_1451980
_cod_original_cell_volume        813.0(14)
_cod_database_code               4036729
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-2
_shelx_res_checksum              35057
_shelx_hkl_checksum              11548