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_4088198
_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
'C36 H59 Al N2 O P, B C24 F20, C6 H5.95 Br0.05'
_chemical_formula_sum            'C66 H64.95 Al B Br0.05 F20 N2 O P'
_chemical_formula_weight         1354.90
_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             2015-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3265(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.88268(18)
_cell_length_b                   15.0778(3)
_cell_length_c                   33.4651(5)
_cell_measurement_reflns_used    11092
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5540
_cell_measurement_theta_min      3.9080
_cell_volume                     6414.41(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
;
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      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000  -60.0000 81

  2 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000   60.0000 81

  3 omega   82.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000    0.0000 92

  4 omega  123.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000 -120.0000 26

  5 omega   82.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000 -120.0000 26

  6 omega   41.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -30.0000 41

  7 omega   38.00  129.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000 -150.0000 91

  8 omega   38.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 36

  9 omega   83.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   90.0000 91
;
_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      0.0292124000
_diffrn_orient_matrix_UB_12      -0.0042438000
_diffrn_orient_matrix_UB_13      0.0464733000
_diffrn_orient_matrix_UB_21      -0.0650649000
_diffrn_orient_matrix_UB_22      -0.0856367000
_diffrn_orient_matrix_UB_23      0.0004161000
_diffrn_orient_matrix_UB_31      0.0979260000
_diffrn_orient_matrix_UB_32      -0.0555960000
_diffrn_orient_matrix_UB_33      -0.0042001000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            21703
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.114
_diffrn_reflns_theta_min         3.923
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.972
_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    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             2791
_exptl_crystal_size_max          0.2208
_exptl_crystal_size_mid          0.1353
_exptl_crystal_size_min          0.0722
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         11649
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0480P)^2^+2.1270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10266
_reflns_number_total             11649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00927_si_002.cif
_cod_data_source_block           hasj151027b
_cod_original_cell_volume        6414.41(17)
_cod_database_code               4088198
_chemical_oxdiff_formula         'C H N Al B F O P Cl'
_reflns_odcompleteness_completeness 99.17
_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. Rigid body (RIGU) restrains
 C66, C65, C64, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H62(0.95) Br1(0.05)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C16(H16), C13(H13), C28(H28)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C21(H21), C23(H23), C11(H11), C22(H22), C9(H9), C10(H10), C65(H65),
 C66(H66), C64(H64), C63(H63), C61(H61), C62(H62)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C34(H34A,H34B,H34C),
 C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C36(H36A,H36B,
 H36C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              97961
_shelx_hkl_checksum              71667
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-27
_olex2_submission_special_instructions 'No special instructions were received'