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_7119761
_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 O P3, C F3 O3 S, C6 H4 F2'
_chemical_formula_sum            'C56 H44 F5 O4 P3 S'
_chemical_formula_weight         1000.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-11-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6503(8)
_cell_length_b                   21.0918(7)
_cell_length_c                   19.7027(7)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.221
_cell_measurement_theta_min      2.196
_cell_volume                     9313.6(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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.603
_diffrn_reflns_theta_min         1.604
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0588 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9371.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       rod
_exptl_crystal_F_000             4144
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of o-difluorobenzene and dichloromethane by vapour diffusion'
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         14253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0545P)^2^+16.5621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10522
_reflns_number_total             14253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00982h2.cif
_cod_data_source_block           4OTf
_cod_database_code               7119761
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C49(H49), C13(H13), C45(H45), C27(H27), C43(H43), C21(H21), C7(H7),
 C39(H39), C25(H25), C24(H24), C15(H15), C22(H22), C33(H33), C31(H31), C19(H19),
  C23(H23), C9(H9), C36(H36), C12(H12), C28(H28), C46(H46), C16(H16), C40(H40),
 C42(H42), C18(H18), C35(H35), C48(H48), C29(H29), C6(H6), C34(H34), C17(H17),
 C11(H11), C41(H41), C30(H30), C10(H10), C4(H4), C5(H5), C3(H3), C47(H47),
 C53(H53), C56(H56), C54(H54), C55(H55)
;
_shelx_res_checksum              49239
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in oil'
_olex2_submission_original_sample_id jjw0312
_olex2_submission_special_instructions 'No special instructions were received'