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_4088201
_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         'C48 H59 Al N2 P, B C24 F20'
_chemical_formula_sum            'C72 H59 Al B F20 N2 P'
_chemical_formula_weight         1400.97
_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             2015-11-03
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_formula_units_Z            2
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_cell_length_b                   14.7992(4)
_cell_length_c                   18.4930(5)
_cell_measurement_reflns_used    12117
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5410
_cell_measurement_theta_min      3.4540
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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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   19.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8784   38.0000  120.0000 96

  2 omega   31.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   30.0000 60

  3 omega   31.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 59

  4 omega   32.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000   30.0000 104

  5 omega   43.00  119.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   30.0000 76

  6 omega   34.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000 -120.0000 87

  7 omega   53.00  134.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000 -180.0000 81

  8 omega   27.00  142.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000  -90.0000 115

  9 omega   27.00  151.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000  150.0000 124

 10 omega  -96.00   -3.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  125.0000  -60.0000 93

 11 omega -116.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784  -77.0000 -150.0000 106
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0733424000
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_diffrn_orient_matrix_UB_13      0.0793518000
_diffrn_orient_matrix_UB_21      -0.0972463000
_diffrn_orient_matrix_UB_22      0.0368753000
_diffrn_orient_matrix_UB_23      -0.0357145000
_diffrn_orient_matrix_UB_31      -0.0234216000
_diffrn_orient_matrix_UB_32      -0.0979229000
_diffrn_orient_matrix_UB_33      -0.0094809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20392
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.092
_diffrn_reflns_theta_min         3.079
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78002
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_exptl_absorpt_process_details
;
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    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.1741
_exptl_crystal_size_mid          0.1325
_exptl_crystal_size_min          0.0826
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         11948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0450P)^2^+0.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10537
_reflns_number_total             11948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_004.cif
_cod_data_source_block           hasj150417a
_cod_original_cell_volume        3298.82(16)
_cod_database_code               4088201
_chemical_oxdiff_formula         'C H N Al P O B F '
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
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:
 C13(H13), C25(H25), C28(H28), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C32(H32), C48(H48), C44(H44), C36(H36), C42(H42), C46(H46), C35(H35),
 C47(H47), C33(H33), C11(H11), C34(H34), C45(H45), C9(H9), C23(H23), C10(H10),
 C21(H21), C38(H38), C41(H41), C22(H22), C40(H40), C39(H39)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C6(H6a,H6b,H6c), C15(H15a,H15b,H15c),
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;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-04-17
_olex2_submission_special_instructions 'No special instructions were received'