Dynamic Exchange in Intramolecular Lewis Pairs with Multiple Lewis-Acidic Functions
Körte, Leif A.; Blomeyer, Sebastian; Peters, Jan-Hendrik; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Organometallics 36 (2017) 742–; doi:10.1021/acs.organomet.6b00935

data_4086949
_publ_section_title
;
 Dynamic Exchange in Intramolecular Lewis Pairs with Multiple Lewis-Acidic
 Functions
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              742
_journal_paper_doi               10.1021/acs.organomet.6b00935
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C33 H60 B3 N'
_chemical_formula_sum            'C33 H60 B3 N'
_chemical_formula_weight         503.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                75.750(10)
_cell_angle_beta                 80.154(8)
_cell_angle_gamma                82.275(9)
_cell_formula_units_Z            2
_cell_length_a                   8.4657(7)
_cell_length_b                   13.0744(18)
_cell_length_c                   14.2825(15)
_cell_measurement_reflns_used    10926
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.3920
_cell_measurement_theta_min      3.4850
_cell_volume                     1502.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.7736
_diffrn_measurement_details
;
  1 omega -116.00   -5.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000 -120.0000 111

  2 omega   -3.00   25.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 28

  3 omega  -49.00   32.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   60.0000 81

  4 omega   58.00  127.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -150.0000 69

  5 omega   87.00  125.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000   30.0000 38

  6 omega   58.00  108.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -178.0000  -60.0000 50

  7 omega   55.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 34

  8 omega  112.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -90.0000 29

  9 omega   82.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 35

 10 omega   42.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 55

 11 omega   41.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 56

 12 omega   34.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 70

 13 omega   42.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 50

 14 omega   55.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 29

 15 omega   41.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 31

 16 omega   91.00  143.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 52

 17 omega   85.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 37

 18 omega   65.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 33

 19 omega   44.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 27

 20 omega   53.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 69

 21 omega  122.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  150.0000 56

 22 omega  147.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   60.0000 27

 23 omega  130.00  164.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 34

 24 omega   41.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 56

 25 omega   75.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  120.0000 101

 26 omega   61.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 48

 27 omega    2.00   31.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   90.0000  -45.6620 29

 28 omega -110.00  -23.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   60.0000 87

 29 omega  -40.00  -14.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -150.0000 26

 30 omega    6.00   31.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   90.0000   80.5784 25

 31 omega  -21.00   55.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       43.6988  -19.0000 -120.0000 76

 32 omega   20.00   45.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -100.8749 25

 33 omega   18.00   43.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000 -177.8802 25

 34 omega   19.00   44.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -40.9003 25

 35 omega   19.00   44.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  139.6188 25

 36 omega   33.00   99.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -42.7078 66

 37 omega   32.00   57.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   38.3074 25

 38 omega   32.00   58.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000 -105.5856 26

 39 omega   34.00   60.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  111.2689 26

 40 omega   36.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000 -161.9716 28

 41 omega   36.00   75.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   60.9649 39

 42 omega   36.00   79.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -16.2079 43

 43 omega   41.00   67.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  155.7043 26

 44 omega   46.00   72.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   69.0000  127.1461 26

 45 omega   48.00   96.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   59.0000   30.3296 48

 46 omega   53.00   84.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   59.0000 -160.1006 31

 47 omega   55.00  118.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   65.0000   32.5280 63

 48 omega   57.00   92.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000 -102.1248 35

 49 omega   74.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   50.0000    3.8243 31

 50 omega  142.00  167.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   50.0000    3.8243 25

 51 omega   79.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000 -150.0000 26

 52 omega   79.00  140.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  -60.0000 61

 53 omega  121.00  147.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  -90.0000 26

 54 omega   80.00  106.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  -90.0000 26

 55 omega   84.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000   90.0000 25

 56 omega   84.00  157.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000   30.0000 73

 57 omega  151.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000   60.0000 26

 58 omega   83.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  -30.0000 26

 59 omega   84.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000   60.0000 27

 60 omega   79.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  120.0000 25

 61 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000 -150.0000 26

 62 omega   83.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000 -180.0000 26

 63 omega   86.00  112.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   45.0000   30.0000 26

 64 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000   30.0000 26

 65 omega   79.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000   60.0000 26

 66 omega   87.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000  -60.0000 30

 67 omega   84.00  110.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000  120.0000 26

 68 omega   83.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   61.0000  150.0000 26

 69 omega   79.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000   90.0000 26

 70 omega  119.00  164.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.7376   77.0000  -30.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1732053000
_diffrn_orient_matrix_UB_12      -0.0533212000
_diffrn_orient_matrix_UB_13      -0.0143345000
_diffrn_orient_matrix_UB_21      0.0626041000
_diffrn_orient_matrix_UB_22      0.1093825000
_diffrn_orient_matrix_UB_23      -0.0433996000
_diffrn_orient_matrix_UB_31      0.0214202000
_diffrn_orient_matrix_UB_32      0.0080146000
_diffrn_orient_matrix_UB_33      0.1028162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16286
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.126
_diffrn_reflns_theta_min         3.226
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method
'no single crystals, but were non-merohedrically twinned by rotation of 180 deg. around 0 0 1, ratio 97:3. '
_exptl_crystal_size_max          0.2978
_exptl_crystal_size_mid          0.0652
_exptl_crystal_size_min          0.0608
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6431
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0837P)^2^+0.0686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4973
_reflns_number_total             6431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00935_si_002.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 4086947--4086949.cif.'
_cod_database_code               4086949
_chemical_oxdiff_formula         'C33 H60 B3 N1'
_diffrn_oxdiff_twin_integration_method simultaneous
_shelx_hkl_checksum              47157
_shelx_res_checksum              954
_shelxl_version_number           2014-3