Synthesis and reactivity of electron poor allenes: formation of completely organic frustrated Lewis pairs.
Palomas, David; Holle, Sigrid; Inés, Blanca; Bruns, Hans; Goddard, Richard; Alcarazo, Manuel; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9073–9082; doi:10.1039/c2dt30195d

data_7019702
_publ_section_title
;
 Synthesis and reactivity of electron poor allenes: formation of
 completely organic frustrated Lewis pairs.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9073
_journal_page_last               9082
_journal_paper_doi               10.1039/c2dt30195d
_journal_volume                  41
_journal_year                    2012
_chemical_compound_source        'methylene chloride, pentane'
_chemical_formula_moiety         'C44 H37 P2 S, F6 P'
_chemical_formula_sum            'C44 H37 F6 P3 S'
_chemical_formula_weight         804.71
_chemical_name_systematic
;
1-(4-(methyl)phenylthio)-carbo-bis(triphenyl)phosphonium
hexafluorophosphate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                AVM-AB-777-01
_audit_creation_date             2012-01-18
_cell_angle_alpha                98.106(5)
_cell_angle_beta                 97.846(5)
_cell_angle_gamma                110.584(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4125(4)
_cell_length_b                   12.2494(14)
_cell_length_c                   16.5886(7)
_cell_measurement_reflns_used    53212
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.0973
_cell_measurement_theta_min      2.6885
_cell_volume                     1921.0(3)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program.
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26184
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.98476
_exptl_absorpt_correction_T_min  0.96522
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+1.1490P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                7538
_reflns_number_total             10957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30195d.txt
_cod_data_source_block           7000_28
_cod_original_cell_volume        1921.0(2)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7019702