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_4086948
_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         'C23 H43 B2 N'
_chemical_formula_sum            'C23 H43 B2 N'
_chemical_formula_weight         355.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-19
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
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_cell_formula_units_Z            4
_cell_length_a                   15.1625(5)
_cell_length_b                   11.1717(2)
_cell_length_c                   13.8554(4)
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.9380
_cell_measurement_theta_min      3.2200
_cell_volume                     2105.41(12)
_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
;
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~
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_diffrn_detector_type            Atlas
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_diffrn_measurement_details
;
  1 omega  -49.00   32.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 81

  2 omega  -51.00   -5.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000 -180.0000 46

  3 omega  -50.00   29.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
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  4 omega -113.00  -66.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000 -180.0000 47

  5 omega   14.00   39.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000  120.0000 25

  6 omega   14.00  105.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000 -120.0000 91

  7 omega   58.00  105.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238  178.0000  120.0000 47

  8 omega   55.00  126.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238 -178.0000 -150.0000 71

  9 omega   70.00  110.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   57.0000  150.0000 40

 10 omega   15.00  115.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000  -60.0000 100

 11 omega   14.00   49.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000    0.0000 35

 12 omega   15.00  102.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000   60.0000 87

 13 omega   87.00  124.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238  178.0000   30.0000 37

 14 omega   14.00   55.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   77.0000 -180.0000 41

 15 omega   23.00   68.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   38.0000   60.0000 45

 16 omega   18.00   63.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3238   57.0000  150.0000 45

 17 omega   82.00  112.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000  -30.0000 30

 18 omega   79.00  174.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  -90.0000 95

 19 omega  138.00  176.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  120.0000 38

 20 omega   82.00  108.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000  -60.0000 26

 21 omega   78.00  176.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000    0.0000 98

 22 omega   82.00  112.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000 -120.0000 30

 23 omega   39.00  139.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093  -77.0000  -90.0000 100

 24 omega   78.00  173.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000   90.0000 95

 25 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000 -120.0000 26

 26 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  120.0000 26

 27 omega   83.00  110.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   57.0000 -138.0684 27

 28 omega   79.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  150.0000 25

 29 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000   60.0000 26

 30 omega   83.00  110.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000    0.0000 27

 31 omega   82.00  110.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000   60.0000 28

 32 omega   82.00  143.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000  -90.0000 61

 33 omega   80.00  118.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   72.0000  -22.0000 38

 34 omega   82.00  108.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000 -180.0000 26

 35 omega  113.00  178.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  -60.0000 65

 36 omega  117.00  178.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000 -150.0000 61

 37 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000 -150.0000 26

 38 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000  -60.0000 26

 39 omega   82.00  108.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000 -150.0000 26

 40 omega  116.00  174.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000   30.0000 58

 41 omega  122.00  148.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   72.0000  -22.0000 26

 42 omega   39.00  121.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093 -125.0000   90.0000 82

 43 omega   82.00  173.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000  150.0000 91

 44 omega   82.00  109.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000  120.0000 27

 45 omega   78.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   77.0000   30.0000 26

 46 omega  116.00  145.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000   90.0000 29

 47 omega   82.00  108.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000   30.0000 26

 48 omega   35.00  104.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093  -94.0000  120.0000 69

 49 omega   82.00  115.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   61.0000   90.0000 33

 50 omega   30.00  107.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093  -94.0000 -150.0000 77

 51 omega   82.00  107.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   65.0000 -177.3714 25

 52 omega   84.00  146.00   1.0000   58.5000
omega____ theta____ kappa____ phi______ frames
    -      108.4093   53.0000 -153.0299 62
;
_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      0.0032480000
_diffrn_orient_matrix_UB_12      -0.0407974000
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_diffrn_orient_matrix_UB_21      -0.0913066000
_diffrn_orient_matrix_UB_22      0.0769604000
_diffrn_orient_matrix_UB_23      -0.0222104000
_diffrn_orient_matrix_UB_31      -0.0670084000
_diffrn_orient_matrix_UB_32      -0.1068559000
_diffrn_orient_matrix_UB_33      -0.0571729000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_number            32791
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_diffrn_reflns_theta_max         72.108
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_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
_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)
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    1.121
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.1605
_exptl_crystal_size_mid          0.1365
_exptl_crystal_size_min          0.0236
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0528P)^2^+0.6261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3301
_reflns_number_total             4153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00935_si_002.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 4086947--4086949.cif.'
_cod_original_cell_volume        2105.42(11)
_cod_database_code               4086948
_chemical_oxdiff_formula         'C23 H43 B2 N'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_shelx_hkl_checksum              62518
_shelx_res_checksum              12982
_shelxl_version_number           2014-3