Donor-substituted phosphanes - surprisingly weak Lewis donors for phosphenium cation stabilisation.
Clark, Ewan R.; Borys, Andryj M.; Pearce, Kyle; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16125–16129; doi:10.1039/c6dt03478k

data_7040679
_publ_section_title
;
 Donor-substituted phosphanes - surprisingly weak Lewis donors for
 phosphenium cation stabilisation.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16125
_journal_page_last               16129
_journal_paper_doi               10.1039/c6dt03478k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C33 H32 N P2, C32 H12 B F24'
_chemical_formula_sum            'C65 H44 B F24 N P2'
_chemical_formula_weight         1367.76
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-08-21
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-02 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.8699(11)
_cell_angle_beta                 107.3045(11)
_cell_angle_gamma                91.5968(10)
_cell_formula_units_Z            2
_cell_length_a                   13.06366(17)
_cell_length_b                   13.20669(16)
_cell_length_c                   19.4224(2)
_cell_measurement_reflns_used    25932
_cell_measurement_temperature    150(1)
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
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(compiled Aug 13 2014,18:06:01)
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  2 omega   18.00   77.00   1.0000    3.6450
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  3 omega   94.00  170.00   1.0000   14.5850
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  7 omega   77.00  157.00   1.0000   14.5850
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  8 omega   78.00  138.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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  9 omega   78.00  114.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 10 omega   75.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 11 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 12 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 13 omega   77.00  103.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 14 omega   77.00  104.00   1.0000   14.5850
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 15 omega   75.00  100.00   1.0000   14.5850
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 16 omega   74.00  141.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 17 omega   77.00  105.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 18 omega   77.00  177.00   1.0000   14.5850
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 19 omega  104.00  177.00   1.0000   14.5850
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 20 omega   74.00  105.00   1.0000   14.5850
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 21 omega   77.00  169.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 22 omega   77.00  104.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 23 omega   77.00  175.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 24 omega   77.00  173.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 25 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 26 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 27 omega   74.00  178.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000  -90.0000 104

 28 omega   74.00  101.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   77.0000  -30.0000 27

 29 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 30 omega   77.00  106.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
    -      106.3614   61.0000  -90.0000 29

 31 omega   77.00  103.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 32 omega   74.00  100.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 33 omega   30.00  139.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 34 omega   36.00  122.00   1.0000   14.5850
omega____ theta____ kappa____ phi______ frames
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 35 omega   24.00   99.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 36 omega   24.00   98.00   1.0000   14.5850
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 37 omega   24.00  109.00   1.0000   14.5850
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 38 omega    2.00   56.00   1.0000    3.6450
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 39 omega  -60.00  -11.00   1.0000    3.6450
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 40 omega  -57.00  -10.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 41 omega  -64.00  -10.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 42 omega  -93.00   -5.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 43 omega -106.00  -65.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 44 omega -119.00  -10.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 45 omega -114.00  -81.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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 46 omega  -72.00  -10.00   1.0000    3.6450
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 47 omega  -48.00   25.00   1.0000    3.6450
omega____ theta____ kappa____ phi______ frames
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_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, hexane'
_exptl_crystal_size_max          0.1
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+4.3577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03478k2.cif
_cod_data_source_block           xstr0487
_cod_depositor_comments          'Adding full bibliography for 7040679.cif.'
_cod_database_code               7040679
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C65 H44 N1 P2 B1 F24'
_chemical_oxdiff_usercomment     KP010
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_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F7(0.75) F8(0.75) F9(0.75) F9A(0.25) F8A(0.25) F7A(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C35(H35), C37(H37), C39(H39), C43(H43), C45(H45), C47(H47), C51(H51),
  C53(H53), C55(H55), C59(H59), C61(H61), C63(H63)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              79503
_olex2_date_sample_data_collection 2015-08-20
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id 'XSTR0487 KP010'
_olex2_submission_special_instructions 'No special instructions were received'