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_7119765
_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         'C49 H40 F P3, 2(C F3 O3 S), 1.727(C6 H4 F2)'
_chemical_formula_sum            'C61.36 H46.91 F10.45 O6 P3 S2'
_chemical_formula_weight         1235.90
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-14
_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                 102.320(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8033(11)
_cell_length_b                   19.1016(11)
_cell_length_c                   19.2535(13)
_cell_measurement_reflns_used    7174
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.615
_cell_measurement_theta_min      2.283
_cell_volume                     5678.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50279
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.607
_diffrn_reflns_theta_min         1.319
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0635 before and 0.0467 after correction. The Ratio of minimum to maximum transmission is 0.8962. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2536.7
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         13072
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0921P)^2^+5.4960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8661
_reflns_number_total             13072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00982h2.cif
_cod_data_source_block           8OTf2
_cod_database_code               7119765
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H41(0.053) H22(0.05) H45(0.039) H46(0.05) H37(0.051) H36(0.082)
 H47(0.054) H23(0.051) H7(0.037) H27(0.033) H19(0.05) H3(0.028) H4(0.033)
 H39(0.043) H25(0.037) H31(0.039) H24(0.045) H13(0.031) H28(0.041) H29(0.047)
 H18(0.07) H9(0.04) H49(0.037) H48(0.049) H15(0.057) H5(0.035) H21(0.038)
 H11(0.045) H6(0.041) H57(0.103) H54(0.061) H42(0.049) H33(0.057) H43(0.039)
 H12(0.04) H30(0.046) H40(0.055) H34(0.081) H16(0.081) H55(0.068) H56(0.089)
 H10(0.047) H17(0.086) H35(0.097) H60(0.104) H62(0.083) H61(0.093) H63(0.082)
 Fixed X: H41(0.3829) H22(0.4524) H45(0.0529) H46(-0.0742) H37(0.2274)
 H36(0.302) H47(-0.1314) H23(0.5383) H7(0.0814) H27(0.213) H19(0.102)
 H3(0.1035) H4(0.1356) H39(0.2683) H25(0.3971) H31(0.3114) H24(0.5097)
 H13(0.0821) H28(0.2025) H29(0.2474) H18(0.0147) H9(-0.0744) H49(0.0617) H48(-
 0.0651) H15(-0.1102) H5(0.1416) H21(0.3389) H11(-0.1228) H6(0.1121)
 H57(0.4811) H54(0.3883) H42(0.3159) H33(0.4173) H43(0.2279) H12(-0.0019)
 H30(0.3022) H40(0.3582) H34(0.4869) H16(-0.1962) H55(0.3557) H56(0.4052) H10(-
 0.1602) H17(-0.1327) H35(0.4291) H60(0.7094) H62(0.7627) H61(0.7955)
 H63(0.6743)
 Fixed Y: H41(0.0263) H22(0.3488) H45(0.3005) H46(0.2522) H37(0.2595)
 H36(0.227) H47(0.1492) H23(0.2569) H7(0.3051) H27(0.4394) H19(0.2089)
 H3(0.4859) H4(0.5459) H39(0.1805) H25(0.2454) H31(0.4792) H24(0.2039)
 H13(0.3942) H28(0.5596) H29(0.639) H18(0.1189) H9(0.4282) H49(0.1411)
 H48(0.095) H15(0.3099) H5(0.4854) H21(0.3908) H11(0.5243) H6(0.3661)
 H57(0.4933) H54(0.7233) H42(0.0668) H33(0.4019) H43(0.1654) H12(0.4707)
 H30(0.5995) H40(0.0826) H34(0.37) H16(0.2169) H55(0.6367) H56(0.5203)
 H10(0.5023) H17(0.1243) H35(0.2842) H60(0.3645) H62(0.2402) H61(0.2807)
 H63(0.3026)
 Fixed Z: H41(0.3334) H22(0.4741) H45(0.3939) H46(0.4189) H37(0.1161)
 H36(0.0271) H47(0.3622) H23(0.4498) H7(0.0399) H27(0.3371) H19(0.1275)
 H3(0.1535) H4(0.0568) H39(0.4236) H25(0.2488) H31(0.1626) H24(0.3382)
 H13(0.3285) H28(0.3557) H29(0.2789) H18(0.0705) H9(0.135) H49(0.2551)
 H48(0.2801) H15(0.1636) H5(-0.0475) H21(0.3856) H11(0.31) H6(-0.0566)
 H57(0.3781) H54(0.3988) H42(0.2204) H33(0.1894) H43(0.2082) H12(0.38)
 H30(0.1834) H40(0.4342) H34(0.0987) H16(0.1061) H55(0.4749) H56(0.4643)
 H10(0.1874) H17(0.0572) H35(0.0183) H60(0.179) H62(0.3499) H61(0.2465)
 H63(0.4036)
;
_shelx_res_checksum              5973
_olex2_submission_special_instructions 'No special instructions were received'