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_7128660
_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         'C20 H15 F6 O6 P'
_chemical_formula_sum            'C20 H15 F6 O6 P'
_chemical_formula_weight         496.29
_chemical_melting_point          418
_chemical_name_common
4',4'-dimethyl-5'-phenyl-4,5-bis(trifluoromethyl)-4',5'-dihydro-2?5-spiro[[1,3,2]dioxaphosphole-2,2'-[2,5]epoxybenzo[d][1,3,6,2]trioxaphosphocine]
_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   geom
_audit_creation_date             2021-03-12
_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                104.000(7)
_cell_angle_beta                 97.928(6)
_cell_angle_gamma                90.021(7)
_cell_formula_units_Z            4
_cell_length_a                   10.223(2)
_cell_length_b                   13.603(3)
_cell_length_c                   15.047(3)
_cell_measurement_reflns_used    5232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.33
_cell_volume                     2009.7(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16714
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.841
_diffrn_reflns_theta_min         1.544
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.745756
_exptl_absorpt_correction_T_min  0.614984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 48041 reflections, Rint = 0.1219
 (14399 with I > 3sig(I), Rint = 0.0810)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: penthane'
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0110(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         16714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0788P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10152
_reflns_number_total             16714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02941j2.cif
_cod_data_source_block           miro19t5
_cod_depositor_comments
'Adding full bibliography for 7128660--7128661.cif.'
_cod_original_cell_volume        2009.7(8)
_cod_database_code               7128660
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4562(10)
 0.5438(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Me refined with riding coordinates:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C23A(H23A,H23B,H23C), C23B(H23D,
 H23E,H23F)
3.b Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C12B(H12B), C13A(H13A), C13B(H13B), C14A(H14A), C14B(H14B),
 C15A(H15A), C15B(H15B), C17A(H17A), C17B(H17B), C18A(H18A), C18B(H18B),
 C19A(H19A), C19B(H19B), C20A(H20A), C20B(H20B), C21A(H21A), C21B(H21B)
;
_shelx_res_checksum              37918
_shelx_hkl_checksum              62226
_olex2_submission_special_instructions 'No special instructions were received'