A Frustrated Lewis Pair Based on a Cationic Aluminum Complex and Triphenylphosphine
Stennett, Tom E.; Pahl, Jürgen; Zijlstra, Harmen S.; Seidel, Falk W.; Harder, Sjoerd; Organometallics 35 (2016) 207–; doi:10.1021/acs.organomet.5b00927

data_4088200
_publ_section_title
;
 A Frustrated Lewis Pair Based on a Cationic Aluminum Complex and
 Triphenylphosphine
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              207
_journal_paper_doi               10.1021/acs.organomet.5b00927
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C61 H89 Al2 N4 O2, B C24 F20'
_chemical_formula_sum            'C85 H89 Al2 B F20 N4 O2'
_chemical_formula_weight         1643.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-19
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_angle_alpha                91.2573(15)
_cell_angle_beta                 104.8642(16)
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_cell_formula_units_Z            2
_cell_length_a                   14.6101(2)
_cell_length_b                   16.7664(3)
_cell_length_c                   18.2804(4)
_cell_measurement_reflns_used    22969
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4870
_cell_measurement_theta_min      3.5040
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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)
;
_computing_data_collection
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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)
;
_computing_data_reduction
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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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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega -112.00  -65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784 -138.0000  -93.0000 47

  2 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000  -30.0000 81

  3 omega -115.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  -38.0000 -180.0000 96

  4 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000 -180.0000 81

  5 omega   27.00  101.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8784 -131.0000   81.0000 74

  6 omega   35.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   30.0000 63

  7 omega   25.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -90.0000 84

  8 omega   25.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  150.0000 84

  9 omega   31.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  120.0000 60

 10 omega   34.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   90.0000 87

 11 omega   36.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000 -180.0000 98

 12 omega   36.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000  -60.0000 98

 13 omega   82.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  150.0000 95

 14 omega   26.00  151.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000  150.0000 125

 15 omega -116.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  -77.0000  -60.0000 106

 16 omega -112.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  -57.0000  120.0000 97

 17 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000 -120.0000 81

 18 omega -112.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  -57.0000   30.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0542842000
_diffrn_orient_matrix_UB_12      0.0881547000
_diffrn_orient_matrix_UB_13      0.0402040000
_diffrn_orient_matrix_UB_21      -0.0099238000
_diffrn_orient_matrix_UB_22      0.0353588000
_diffrn_orient_matrix_UB_23      -0.0778097000
_diffrn_orient_matrix_UB_31      -0.0995647000
_diffrn_orient_matrix_UB_32      0.0132316000
_diffrn_orient_matrix_UB_33      0.0023613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37200
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         3.266
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79699
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.2076
_exptl_crystal_size_mid          0.1626
_exptl_crystal_size_min          0.0955
_refine_diff_density_max         0.554
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_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         15030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0630P)^2^+1.6470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13530
_reflns_number_total             15030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_008.cif
_cod_data_source_block           exp_249
_cod_original_cell_volume        4146.89(14)
_cod_database_code               4088200
_chemical_oxdiff_formula         'C H N Al O P Si F B'
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_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C25(H25), C13(H13), C59(H59), C56(H56), C28(H28), C44(H44), C47(H47)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C11(H11), C4(H4), C23(H23), C10(H10), C35(H35), C21(H21), C22(H22),
 C9(H9), C54(H54), C53(H53), C52(H52), C42(H42), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C15(H15a,H15b,H15c), C2(H2a,H2b,H2c), C27(H27a,H27b,H27c),
 C18(H18a,H18b,H18c), C26(H26a,H26b,H26c), C32(H32a,H32b,H32c), C1(H1a,H1b,H1c),
  C17(H17a,H17b,H17c), C33(H33a,H33b,H33c), C37(H37a,H37b,H37c), C30(H30a,H30b,
 H30c), C57(H57a,H57b,H57c), C29(H29a,H29b,H29c), C58(H58a,H58b,H58c), C61(H61a,
 H61b,H61c), C60(H60a,H60b,H60c), C14(H14a,H14b,H14c), C45(H45a,H45b,H45c),
 C48(H48a,H48b,H48c), C49(H49a,H49b,H49c), C46(H46a,H46b,H46c)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-04-10
_olex2_submission_special_instructions 'No special instructions were received'