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_4086947
_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         'C13 H26 B N'
_chemical_formula_sum            'C13 H26 B N'
_chemical_formula_weight         207.16
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-13
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6406(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.30266(15)
_cell_length_b                   12.21955(19)
_cell_length_c                   11.0832(2)
_cell_measurement_reflns_used    11881
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.1010
_cell_measurement_theta_min      5.6300
_cell_volume                     1229.34(4)
_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 1.0000
_diffrn_measured_fraction_theta_max 0.9952
_diffrn_measurement_details
;
  1 omega  -74.00   15.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  102.0000 -160.0000 89

  2 omega   44.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -102.0000   96.0000 26

  3 omega   49.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -102.0000   96.0000 25

  4 omega  115.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  102.0000 -160.0000 25

  5 omega  -64.00   30.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  120.0000 94

  6 omega  -94.00  -64.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000   60.0000 30

  7 omega  -61.00   29.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000    0.0000 90

  8 omega  -40.00  -14.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000   60.0000 26

  9 omega  -93.00  -21.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -60.0000 72

 10 omega   13.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 96

 11 omega   18.00   61.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000   60.0000 43

 12 omega   13.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 97

 13 omega   18.00   54.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 36

 14 omega   15.00   75.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 60

 15 omega   14.00   68.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 54

 16 omega   74.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 38

 17 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

 18 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 26

 19 omega   85.00  112.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 27

 20 omega   85.00  158.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 73

 21 omega   81.00  106.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 25

 22 omega   86.00  118.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 32

 23 omega   81.00  151.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 70

 24 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 26

 25 omega  129.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 49

 26 omega   86.00  160.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 74

 27 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 26

 28 omega   31.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 77

 29 omega   81.00  175.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 94

 30 omega   81.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 93

 31 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   62.0000  172.0213 26

 32 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 26

 33 omega   85.00  135.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 50

 34 omega   82.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 32

 35 omega   85.00  161.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 76

 36 omega  135.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 43

 37 omega   96.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 26

 38 omega   42.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 55

 39 omega   85.00  127.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 42

 40 omega   31.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 56

 41 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 26

 42 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 26

 43 omega   43.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 26

 44 omega   41.00  121.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 80

 45 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000 -126.8862 26

 46 omega   89.00  131.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 42

 47 omega   85.00  161.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 76

 48 omega   87.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   60.0000   98.6881 26

 49 omega  124.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 52

 50 omega   86.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 86

 51 omega   85.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 28

 52 omega   85.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 31

 53 omega   41.00  141.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -90.0000 100

 54 omega   49.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 37
;
_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      -0.0998234000
_diffrn_orient_matrix_UB_12      0.1018122000
_diffrn_orient_matrix_UB_13      -0.0130487000
_diffrn_orient_matrix_UB_21      -0.1141452000
_diffrn_orient_matrix_UB_22      -0.0649396000
_diffrn_orient_matrix_UB_23      0.0529567000
_diffrn_orient_matrix_UB_31      0.0762859000
_diffrn_orient_matrix_UB_32      0.0361344000
_diffrn_orient_matrix_UB_33      0.1316112000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20960
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.376
_diffrn_reflns_theta_min         5.462
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.119
_exptl_crystal_description       irregular
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.1386
_exptl_crystal_size_mid          0.0706
_exptl_crystal_size_min          0.0603
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0456P)^2^+0.3095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2336
_reflns_number_total             2565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00935_si_002.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 4086947--4086949.cif.'
_cod_database_code               4086947
_chemical_oxdiff_formula         'C12 H12 B N'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_shelx_hkl_checksum              97084
_shelx_res_checksum              26706
_shelxl_version_number           2014-3