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_4088199
_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         'C56 H65 Al N2 P, B C24 F20'
_chemical_formula_sum            'C80 H65 Al B F20 N2 P'
_chemical_formula_weight         1503.10
_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
_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_angle_alpha                93.536(2)
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_cell_formula_units_Z            2
_cell_length_a                   11.0872(3)
_cell_length_b                   17.0047(4)
_cell_length_c                   19.8107(7)
_cell_measurement_reflns_used    13305
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.5110
_cell_measurement_theta_min      4.1350
_cell_volume                     3586.15(19)
_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_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_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  -66.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000   90.0000 94

  2 omega  -73.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   77.0000 -150.0000 98

  3 omega -112.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -60.0000 94

  4 omega   67.00  170.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   15.0000  -30.0000 103

  5 omega  103.00  171.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000  150.0000 68

  6 omega   35.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   60.0000 60

  7 omega   35.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  120.0000 86

  8 omega   31.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -90.0000 60

  9 omega   82.00  173.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000 -150.0000 91

 10 omega   39.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -90.0000 74

 11 omega   35.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -180.0000 51

 12 omega   31.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -180.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0872669000
_diffrn_orient_matrix_UB_12      -0.0720761000
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_diffrn_orient_matrix_UB_21      -0.0162560000
_diffrn_orient_matrix_UB_22      -0.0176653000
_diffrn_orient_matrix_UB_23      0.0724651000
_diffrn_orient_matrix_UB_31      -0.1139452000
_diffrn_orient_matrix_UB_32      0.0524343000
_diffrn_orient_matrix_UB_33      -0.0122175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21128
_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         68.112
_diffrn_reflns_theta_min         3.365
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.519
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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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2216
_exptl_crystal_size_mid          0.1397
_exptl_crystal_size_min          0.1083
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.044
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_refine_ls_number_reflns         12990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.2010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11715
_reflns_number_total             12990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_005.cif
_cod_data_source_block           hasj150227c
_cod_original_cell_volume        3586.17(17)
_cod_database_code               4088199
_chemical_oxdiff_formula         'C H N Al P B F O'
_reflns_odcompleteness_completeness 99.08
_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:
 C16(H16), C28(H28), C25(H25), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C31(H31), C9(H9), C11(H11), C10(H10), C21(H21), C22(H22), C23(H23),
 C38(H38), C52(H52), C46(H46), C34(H34), C50(H50), C44(H44), C40(H40), C37(H37),
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 C55(H55), C48(H48), C41(H41), C43(H43), C42(H42)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C18(H18A,H18B,H18C),
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 H30C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-02-27
_olex2_submission_special_instructions 'No special instructions were received'