Electrophilic bis-fluorophosphonium dications: Lewis acid catalysts from diphosphines
Holthausen, Michael H.; Hiranandani, Rashi R.; Stephan, Douglas W.; Chem. Sci. 6 (2015) 2016–; doi:10.1039/C5SC00051C

data_1518603
_publ_section_title
;
 Electrophilic bis-fluorophosphonium dications: Lewis acid catalysts from
 diphosphines
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2016
_journal_paper_doi               10.1039/C5SC00051C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C24 B F20, C34 H26 F3 P2, C1.25, H2.5 Cl2.5'
_chemical_formula_sum            'C59.25 H28.5 B Cl2.5 F23 P2'
_chemical_formula_weight         1338.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-30 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.564(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8002(9)
_cell_length_b                   17.1372(10)
_cell_length_c                   17.8001(9)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      54.694
_cell_measurement_theta_min      4.689
_cell_volume                     5597.6(5)
_computing_cell_refinement
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_collection
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_molecular_graphics
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'
_computing_structure_refinement
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_solution
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50339
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2674
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The unit cell contains 5 methylene chloride molecules 
which have been treated as a diffuse contribution to the 
overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                8842
_reflns_number_total             12911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc00051c2.cif
_cod_data_source_block           4_[(C10H6)(Ph2PF2)(Ph2PF)][B(C6F5)4]
_cod_depositor_comments
'Adding full bibliography for 1518596--1518603.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C59.25 H28.50 B Cl2.50 F23 P2'
_cod_database_code               1518603
_cod_duplicate_entry 1518599