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_4088204
_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         'C19 H17 Cl P, B C24 F20'
_chemical_formula_sum            'C43 H17 B Cl F20 P'
_chemical_formula_weight         990.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-18
_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_length_b                   30.4115(2)
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_cell_measurement_reflns_used    17020
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5810
_cell_measurement_theta_min      3.7020
_cell_volume                     7688.88(10)
_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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_diffrn_ambient_environment      air
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_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -25.00   23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -30.0000 48

  2 omega  -29.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -120.0000 57

  3 omega   42.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000 -120.0000 42

  4 omega   35.00  116.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000 -120.0000 81

  5 omega   31.00   79.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 48

  6 omega   94.00  151.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000   60.0000 57

  7 omega   81.00  174.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -90.0000 93

  8 omega  142.00  178.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -150.0000 36

  9 omega   35.00  100.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000    0.0000 65

 10 omega  -47.00   18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  120.0000 65
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0303187000
_diffrn_orient_matrix_UB_12      0.0483419000
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_diffrn_orient_matrix_UB_21      -0.1112248000
_diffrn_orient_matrix_UB_22      0.0144791000
_diffrn_orient_matrix_UB_23      -0.0007182000
_diffrn_orient_matrix_UB_31      0.0317488000
_diffrn_orient_matrix_UB_32      0.0046470000
_diffrn_orient_matrix_UB_33      0.0806582000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26940
_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         2.906
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94148
_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    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.2049
_exptl_crystal_size_mid          0.1597
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0336
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+3.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12765
_reflns_number_total             13897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_010.cif
_cod_data_source_block           hajs150603a
_cod_database_code               4088204
_chemical_oxdiff_formula         'C H N Al P Cl O'
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1A(H1Aa,H1Ab), C1(H1a,H1b)
2.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C9(H9), C13A(H13A), C7A(H7A), C10A(H10A), C12A(H12A), C15(H15),
 C11A(H11A), C19(H19), C7(H7), C17(H17), C5(H5), C13(H13), C19A(H19A), C6(H6),
 C10(H10), C6A(H6A), C18(H18), C15A(H15A), C11(H11), C3A(H3A), C16(H16),
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 C4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-03
_olex2_submission_special_instructions 'No special instructions were received'