The formation of cage phosphoranes and their rearrangements in the reactions of substituted 2-(3-oxo-3-phenyl)ethoxybenzo[d]-1,3,2-dioxaphospholes with perfluorodiacetyl.
Mironov, Vladimir F.; Dimukhametov, Mudaris N.; Ivkova, Gulnara A.; Khayarov, Khasan R.; Islamov, Daut R.; Litvinov, Igor A.; Chemical communications (Cambridge, England) 57 (2021) 8516–8519; doi:10.1039/d1cc02941j

data_7128661
_publ_section_title
;
 The formation of cage phosphoranes and their rearrangements in the
 reactions of substituted
 2-(3-oxo-3-phenyl)ethoxybenzo[d]-1,3,2-dioxaphospholes with
 perfluorodiacetyl.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8516
_journal_page_last               8519
_journal_paper_doi               10.1039/d1cc02941j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C23 H19 F6 O6 P'
_chemical_formula_sum            'C23 H19 F6 O6 P'
_chemical_formula_weight         536.35
_chemical_melting_point          420
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.12410(10)
_cell_length_b                   13.5556(2)
_cell_length_c                   34.2865(4)
_cell_measurement_reflns_used    11563
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      76.0550
_cell_measurement_theta_min      2.5980
_cell_volume                     4658.35(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  19.00   0.50    0.19    --  -47.45  19.00  60.00   92
  2  \w    -63.00 -38.00   0.50    0.76    -- -105.86  61.00 120.00   50
  3  \w   -106.00 -41.00   0.50    0.76    -- -105.86  77.00 120.00  130
  4  \w    -74.00  -8.00   0.50    0.19    --  -47.45  93.00 -85.00  132
  5  \w    -24.00  78.00   0.50    0.19    --   47.45 -93.00 162.00  204
  6  \w     66.00 100.00   0.50    0.76    --  105.86 -93.00 162.00   68
  7  \w     35.00  69.00   0.50    0.76    --  105.86 -61.00  30.00   68
  8  \w     63.00 106.00   0.50    0.76    --  105.86 -94.00  30.00   86
  9  \w     37.00  71.00   0.50    0.76    --  105.86 -61.00  60.00   68
 10  \w     34.00  71.00   0.50    0.76    --  105.86 -61.00   0.00   74
 11  \w     33.00  71.00   0.50    0.76    --  105.86 -61.00 -60.00   76
 12  \w     33.00  71.00   0.50    0.76    --  105.86 -61.00-120.00   76
 13  \w     35.00  71.00   0.50    0.76    --  105.86 -61.00-150.00   72
 14  \w     33.00  71.00   0.50    0.76    --  105.86 -61.00-180.00   76
 15  \w     34.00  71.00   0.50    0.76    --  105.86 -61.00 -30.00   74
 16  \w    116.00 175.00   0.50    0.76    --  105.86  61.00-120.00  118
 17  \w     83.00 178.00   0.50    0.76    --  105.86  93.00 -85.00  190
 18  \w     76.00 120.00   0.50    0.19    --   47.45 125.00 120.00   88
 19  \w    -25.00  26.00   0.50    0.19    --   47.45 -19.00-120.00  102
 20  \w   -112.00 -75.00   0.50    0.19    --  -47.45-125.00-120.00   74
 21  \w    -66.00 -40.00   0.50    0.76    -- -105.86  61.00-120.00   52
 22  \w    -65.00 -39.00   0.50    0.76    -- -105.86  93.00 -85.00   52
 23  \w   -102.00 -69.00   0.50    0.76    -- -105.86  93.00 -85.00   66
 24  \w   -154.00-129.00   0.50    0.76    -- -105.86 -93.00 162.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0777011000
_diffrn_orient_matrix_UB_12      0.0825528000
_diffrn_orient_matrix_UB_13      0.0177183000
_diffrn_orient_matrix_UB_21      0.1255642000
_diffrn_orient_matrix_UB_22      0.0654609000
_diffrn_orient_matrix_UB_23      0.0047248000
_diffrn_orient_matrix_UB_31      -0.0425525000
_diffrn_orient_matrix_UB_32      0.0426585000
_diffrn_orient_matrix_UB_33      -0.0415193000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16879
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.466
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       needle
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+4.9793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4367
_reflns_number_total             4739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02941j2.cif
_cod_data_source_block           mir215_corr
_cod_depositor_comments
'Adding full bibliography for 7128660--7128661.cif.'
_cod_database_code               7128661
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H19F6O6P
_diffrn_oxdiff_digest_frames
;
01a6fd37ee132400441f39c2008aa09a3a000484745
;
_diffrn_oxdiff_digest_hkl
;
016bb0c61c0236d4c6806788e915ca9fb9e542
;
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21)
;
_shelx_res_checksum              78027
_shelx_hkl_checksum              26298
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.774