Carbodiphosphorane mediated synthesis of a triflyloxyphosphonium dication and its reactivity towards nucleophiles.
Yogendra, S.; Hennersdorf, F.; Bauzá, A; Frontera, A.; Fischer, R.; Weigand, J. J.; Chemical communications (Cambridge, England) 53 (2017) 2954–2957; doi:10.1039/c7cc00982h

data_7119760
_publ_section_title
;
 Carbodiphosphorane mediated synthesis of a triflyloxyphosphonium dication
 and its reactivity towards nucleophiles.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2954
_journal_page_last               2957
_journal_paper_doi               10.1039/c7cc00982h
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C50 H40 N P3, 2(C F3 O3 S), C3 H2 F'
_chemical_formula_sum            'C55 H42 F7 N O6 P3 S2'
_chemical_formula_weight         1102.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-11-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.93704(9)
_cell_length_b                   30.59463(14)
_cell_length_c                   18.10622(9)
_cell_measurement_reflns_used    60577
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4070
_cell_measurement_theta_min      3.7340
_cell_volume                     9936.28(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -55.00  32.00   1.00    2.60    --  -38.50  57.00 -60.00   87
  2  \w     45.00  87.00   1.00    2.60    --   42.50-125.00-180.00   42
  3  \w     44.00  81.00   1.00   10.40    --  111.00 -61.00-120.00   37
  4  \w    100.00 135.00   1.00   10.40    --  111.00 -61.00-120.00   35
  5  \w     82.00 130.00   1.00   10.40    --  111.00 -77.00 -60.00   48
  6  \w     83.00 120.00   1.00   10.40    --  111.00-125.00 -30.00   37
  7  \w     84.00 109.00   1.00   10.40    --  111.00 -94.00 -60.00   25
  8  \w     66.00 120.00   1.00   10.40    --  111.00-125.00-150.00   54
  9  \w     57.00  94.00   1.00    2.60    --   42.50-125.00 -30.00   37
 10  \w     55.00  83.00   1.00   10.40    --  111.00-125.00  60.00   28
 11  \w     93.00 118.00   1.00   10.40    --  111.00-125.00  60.00   25
 12  \w     77.00 121.00   1.00   10.40    --  111.00-125.00 120.00   44
 13  \w    114.00 139.00   1.00   10.40    --  111.00 -61.00  90.00   25
 14  \w     87.00 176.00   1.00   10.40    --  111.00  30.00 -30.00   89
 15  \w    132.00 158.00   1.00   10.40    --  111.00  45.00 -90.00   26
 16  \w    129.00 174.00   1.00   10.40    --  111.00  45.00   0.00   45
 17  \w    127.00 153.00   1.00   10.40    --  111.00 125.00   0.00   26
 18  \w     90.00 116.00   1.00   10.40    --  111.00  45.00   0.00   26
 19  \w     88.00 176.00   1.00   10.40    --  111.00  30.00  30.00   88
 20  \w     90.00 170.00   1.00   10.40    --  111.00  45.00  60.00   80
 21  \w     87.00 166.00   1.00   10.40    --  111.00  30.00 120.00   79
 22  \w     76.00 109.00   1.00   10.40    --  111.00 -94.00  90.00   33
 23  \w     61.00  87.00   1.00   10.40    --  111.00 -61.00  90.00   26
 24  \w     52.00 123.00   1.00   10.40    --  111.00 -30.00  60.00   71
 25  \w     50.00  94.00   1.00   10.40    --  111.00 -61.00  30.00   44
 26  \w     43.00  74.00   1.00   10.40    --  111.00 -77.00 -60.00   31
 27  \w     39.00 110.00   1.00   10.40    --  111.00-125.00-120.00   71
 28  \w     54.00 100.00   1.00   10.40    --  111.00-125.00 -90.00   46
 29  \w     39.00 120.00   1.00   10.40    --  111.00-125.00 -60.00   81
 30  \w     45.00  71.00   1.00   10.40    --  111.00 -94.00  90.00   26
 31  \w     43.00  89.00   1.00   10.40    --  111.00 -94.00 120.00   46
 32  \w     30.00  56.00   1.00   10.40    --  111.00 -94.00 -60.00   26
 33  \w   -105.00 -18.00   1.00    2.60    --  -38.50 -38.00 150.00   87
 34  \w   -101.00 -19.00   1.00    2.60    --  -38.50 -38.00 -30.00   82
 35  \w   -108.00 -16.00   1.00    2.60    --  -38.50 -38.00  60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0601778000
_diffrn_orient_matrix_UB_12      -0.0015330000
_diffrn_orient_matrix_UB_13      0.0606380000
_diffrn_orient_matrix_UB_21      0.0507998000
_diffrn_orient_matrix_UB_22      0.0268968000
_diffrn_orient_matrix_UB_23      0.0514091000
_diffrn_orient_matrix_UB_31      -0.0343152000
_diffrn_orient_matrix_UB_32      0.0425414000
_diffrn_orient_matrix_UB_33      -0.0302801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            102087
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.628
_diffrn_reflns_theta_min         2.856
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       needle
_exptl_crystal_F_000             4536
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+5.9905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9905
_reflns_number_total             10445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00982h2.cif
_cod_data_source_block           9OTf2
_cod_original_cell_volume        9936.28(9)
_cod_database_code               7119760
_chemical_oxdiff_formula         C55H42F7NO6P3S2
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C45(H45), C19(H19), C33(H33), C13(H13), C49(H49), C43(H43),
 C18(H18), C37(H37), C25(H25), C39(H39), C48(H48), C3(H3), C30(H30), C27(H27),
 C22(H22), C12(H12), C42(H42), C9(H9), C31(H31), C34(H34), C40(H40), C21(H21),
 C11(H11), C41(H41), C47(H47), C36(H36), C16(H16), C7(H7), C17(H17), C46(H46),
 C35(H35), C24(H24), C10(H10), C4(H4), C29(H29), C23(H23), C28(H28), C5(H5),
 C6(H6), C55(H55), C54(H54)
;
_shelx_res_checksum              59533
_shelx_shelxl_version_number     2014/7
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.698