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_4088202
_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         'C54 H71 Al N2 P, B C24 F20'
_chemical_formula_sum            'C78 H71 Al B F20 N2 P'
_chemical_formula_weight         1485.12
_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
_audit_creation_date             2015-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0147(3)
_cell_length_b                   31.3266(7)
_cell_length_c                   20.4013(4)
_cell_measurement_reflns_used    20635
_cell_measurement_temperature    293.53(10)
_cell_measurement_theta_max      73.4860
_cell_measurement_theta_min      3.5450
_cell_volume                     7673.9(3)
_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      air
_diffrn_ambient_temperature      293.53(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -39.00    8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  120.0000 47

  2 omega  -39.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -120.0000 70

  3 omega  -62.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -180.0000 77

  4 omega   31.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -90.0000 60

  5 omega   55.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -30.0000 70

  6 omega   42.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000 -150.0000 75

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

  8 omega   31.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 60

  9 omega   95.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000    0.0000 81

 10 omega  -92.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9409  125.0000  -90.0000 85

 11 omega   23.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9409   57.0000  -60.0000 86

 12 omega   97.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   90.0000 31

 13 omega   42.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   90.0000 34

 14 omega  123.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  -90.0000 51

 15 omega   46.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -60.0000 63

 16 omega   31.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000   90.0000 87

 17 omega   31.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   30.0000 41
;
_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      -0.0637402000
_diffrn_orient_matrix_UB_12      -0.0426083000
_diffrn_orient_matrix_UB_13      -0.0032300000
_diffrn_orient_matrix_UB_21      -0.1051354000
_diffrn_orient_matrix_UB_22      0.0236438000
_diffrn_orient_matrix_UB_23      -0.0259962000
_diffrn_orient_matrix_UB_31      0.0365122000
_diffrn_orient_matrix_UB_32      -0.0066779000
_diffrn_orient_matrix_UB_33      -0.0708951000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            13988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.110
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.966
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.285
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.3439
_exptl_crystal_size_mid          0.2465
_exptl_crystal_size_min          0.1604
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         13988
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+23.1898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12157
_reflns_number_total             13988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_006.cif
_cod_data_source_block           hasj151029b
_cod_database_code               4088202
_chemical_oxdiff_formula         'C H N Al P Cl B F'
_reflns_odcompleteness_completeness 99.85
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C74A-F16A
 1.35 with sigma of 0.01
3. Rigid bond restraints
 C73, C78A, F20A, C77A, F19A, C76A, F18A, C75A, F17A, C74A, F16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C73 \\sim C78A \\sim F20A \\sim C77A \\sim F19A \\sim C76A \\sim F18A \\sim
C75A \\sim F17A \\sim C74A \\sim F16A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C67A, C68A, C69A, C70A, C71A, C72A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C78A, F20A, C77A, F19A, C76A, F18A, C75A, F17A, C74A, F16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F13A)=Sof(F14A)=Sof(F12A)=Sof(F15A)=Sof(F11A)=Sof(C72A)=Sof(C67A)=
 Sof(C68A)=Sof(C69A)=Sof(C70A)=Sof(C71A)=1-FVAR(1)
 Sof(F11)=Sof(F15)=Sof(F12)=Sof(F14)=Sof(F13)=Sof(C67)=Sof(C68)=Sof(C72)=
 Sof(C71)=Sof(C69)=Sof(C70)=FVAR(1)
 Sof(C78A)=Sof(C77A)=Sof(C76A)=Sof(C75A)=Sof(C74A)=Sof(F18A)=Sof(F19A)=
 Sof(F20A)=Sof(F17A)=Sof(F16A)=1-FVAR(2)
 Sof(F16)=Sof(F20)=Sof(F17)=Sof(F19)=Sof(F18)=Sof(C74)=Sof(C78)=Sof(C75)=
 Sof(C77)=Sof(C76)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C28(H28), C25(H25), C32(H32)
7.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B)
7.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C9(H9), C40(H40), C4(H4), C42(H42), C38(H38), C23(H23),
 C39(H39), C21(H21), C41(H41), C22(H22), C44(H44), C50(H50), C54(H54), C48(H48),
  C46(H46), C45(H45), C51(H51), C52(H52), C47(H47), C53(H53)
7.d Fitted hexagon refined as free rotating group:
 C73(C78A,C77A,C76A,C75A,C74A), C72A(C67A,C68A,C69A,C70A,C71A)
7.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C),
 C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C30(H30A,H30B,
 H30C), C15(H15A,H15B,H15C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C36(H36A,
 H36B,H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-29
_olex2_submission_special_instructions 'No special instructions were received'