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_4088197
_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         'C49 H59 Al N2 O2 P, B C24 F20'
_chemical_formula_sum            'C73 H59 Al B F20 N2 O2 P'
_chemical_formula_weight         1444.98
_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             2015-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                72.151(3)
_cell_angle_beta                 88.283(2)
_cell_angle_gamma                86.427(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0112(3)
_cell_length_b                   15.6917(4)
_cell_length_c                   19.6252(5)
_cell_measurement_reflns_used    13564
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.5490
_cell_measurement_theta_min      4.3080
_cell_volume                     3513.77(17)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -63.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000  -30.0000 91

  2 omega  -67.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000   90.0000 95

  3 omega -111.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000 -180.0000 93

  4 omega   44.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  150.0000 38

  5 omega   31.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 56

  6 omega   90.00  163.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000    0.0000 73

  7 omega   82.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  -90.0000 96

  8 omega   95.00  171.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -180.0000 76

  9 omega   31.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -120.0000 60

 10 omega   43.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000 -120.0000 78

 11 omega   39.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -180.0000 68

 12 omega   41.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   60.0000 80

 13 omega   34.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  150.0000 73
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0407280000
_diffrn_orient_matrix_UB_12      0.0129849000
_diffrn_orient_matrix_UB_13      0.0696655000
_diffrn_orient_matrix_UB_21      0.0096667000
_diffrn_orient_matrix_UB_22      0.1008045000
_diffrn_orient_matrix_UB_23      -0.0386820000
_diffrn_orient_matrix_UB_31      -0.1215108000
_diffrn_orient_matrix_UB_32      0.0184748000
_diffrn_orient_matrix_UB_33      0.0212696000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21306
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.358
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   gaussian
_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    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.2951
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.1775
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         12713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0540P)^2^+1.0310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11392
_reflns_number_total             12713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_007.cif
_cod_data_source_block           hasj150227a
_cod_original_cell_volume        3513.76(17)
_cod_database_code               4088197
_chemical_oxdiff_formula         'C H N P Al O B F Cl'
_reflns_odcompleteness_completeness 98.99
_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), C16(H16), C25(H25), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
  C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-02-27
_olex2_submission_special_instructions 'No special instructions were received'