Intramolecular Lewis pairs with two acid sites - reactivity differences between P- and N-based systems.
Körte, Leif A; Blomeyer, Sebastian; Heidemeyer, Shari; Nissen, Jan Hendrick; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17319–17328; doi:10.1039/c6dt03490j

data_7040818
_publ_section_title
;
 Intramolecular Lewis pairs with two acid sites - reactivity differences
 between P- and N-based systems.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17319
_journal_page_last               17328
_journal_paper_doi               10.1039/c6dt03490j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H20 B F10 N'
_chemical_formula_sum            'C22 H20 B F10 N'
_chemical_formula_weight         499.20
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-30
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-09-01 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.1881(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.07264(12)
_cell_length_b                   13.22848(14)
_cell_length_c                   15.00959(18)
_cell_measurement_reflns_used    22692
_cell_measurement_temperature    99.97(14)
_cell_measurement_theta_max      72.1040
_cell_measurement_theta_min      3.0230
_cell_volume                     2131.45(4)
_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~
_diffrn_ambient_temperature      99.97(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_details
;
  1 omega  -50.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 71

  2 omega -107.00  -20.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  150.0000 87

  3 omega  -69.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000 -120.0000 101

  4 omega   82.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 32

  5 omega   19.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000   60.0000 36

  6 omega   25.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 31

  7 omega   14.00   48.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 34

  8 omega   57.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000   90.0000 65

  9 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -120.0000 102

 10 omega   17.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 93

 11 omega   28.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 27

 12 omega   50.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 27

 13 omega   57.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -180.0000 67

 14 omega   13.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 66

 15 omega   13.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 70

 16 omega   66.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 49

 17 omega   85.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

 18 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 26

 19 omega   85.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 28

 20 omega   81.00  169.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 88

 21 omega  118.00  174.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 56

 22 omega   81.00  167.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 86

 23 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -39.6627 26

 24 omega   85.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 27

 25 omega   41.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 37

 26 omega   97.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 25

 27 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 28 omega  133.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 44

 29 omega   81.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 29

 30 omega   81.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 26

 31 omega   85.00  164.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 79

 32 omega   85.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 31

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

 34 omega   81.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 96

 35 omega   40.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  150.0000 99

 36 omega   81.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 29

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

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

 39 omega   50.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -60.0000 91

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

 41 omega   81.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 27

 42 omega  116.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 61

 43 omega   50.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 27

 44 omega   80.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 29

 45 omega   83.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  -93.0000 26

 46 omega   85.00  148.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 63

 47 omega   85.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 9
;
_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      0.0060403000
_diffrn_orient_matrix_UB_12      -0.0737041000
_diffrn_orient_matrix_UB_13      -0.0782702000
_diffrn_orient_matrix_UB_21      -0.1433358000
_diffrn_orient_matrix_UB_22      -0.0038069000
_diffrn_orient_matrix_UB_23      -0.0287805000
_diffrn_orient_matrix_UB_31      -0.0011549000
_diffrn_orient_matrix_UB_32      0.0901060000
_diffrn_orient_matrix_UB_33      -0.0652598000
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30339
_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         71.998
_diffrn_reflns_theta_min         4.118
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.616
_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    1.556
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.5711
_exptl_crystal_size_mid          0.2862
_exptl_crystal_size_min          0.1213
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4017
_reflns_number_total             4197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03490j2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7040818--7040820.cif.'
_cod_database_code               7040818
_chemical_oxdiff_formula         'C22 H20 B F10 N'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              65049
_shelxl_version_number           2014-3