Intramolecular pyridine-based frustrated Lewis-pairs.
Körte, Leif A; Warner, Robin; Vishnevskiy, Yury V.; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9992–10002; doi:10.1039/c5dt01068c

data_7035094
_publ_section_title
;
 Intramolecular pyridine-based frustrated Lewis-pairs.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9992
_journal_page_last               10002
_journal_paper_doi               10.1039/c5dt01068c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C22 H14 B F10 N'
_chemical_formula_sum            'C22 H14 B F10 N'
_chemical_formula_weight         493.15
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-04
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-01-08 deposited with the CCDC.
2015-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5752(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2973(2)
_cell_length_b                   13.7505(2)
_cell_length_c                   12.6885(2)
_cell_measurement_reflns_used    21296
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      30.0370
_cell_measurement_theta_min      3.3790
_cell_volume                     1958.11(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      99.99(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_details
;
  1 omega  -82.00  -35.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -      -18.8719 -178.0000   30.0000 47

  2 omega  -89.00    1.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -      -18.8719  -38.0000  -30.0000 90

  3 omega  -86.00  -13.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -      -18.8719  144.0000  122.9826 73

  4 omega   -9.00   88.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719   77.0000  -60.0000 97

  5 omega  -50.00   37.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719  -57.0000   60.0000 87

  6 omega  -53.00   54.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719  -19.0000 -120.0000 107

  7 omega    6.00   87.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719   57.0000 -150.0000 81

  8 omega   -4.00   70.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719 -118.0000   10.4767 74

  9 omega  -10.00   75.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -       18.8719   77.0000   90.0000 85

 10 omega  -86.00  -12.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -      -18.8719  144.0000  -33.1467 74

 11 omega  -87.00    0.00   1.0000   37.5200
omega____ theta____ kappa____ phi______ frames
    -      -18.8719  -57.0000  -90.0000 87

 12 omega   35.00   79.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8579    0.0000  -90.0000 44

 13 omega   62.00  100.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8579 -178.0000  -60.0000 38

 14 omega  -46.00   23.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8579    0.0000  -90.0000 69

 15 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8579   57.0000 -150.0000 87

 16 omega  -46.00   76.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8579    0.0000  150.0000 122
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0227450000
_diffrn_orient_matrix_UB_12      -0.0480786000
_diffrn_orient_matrix_UB_13      -0.0047070000
_diffrn_orient_matrix_UB_21      0.0372939000
_diffrn_orient_matrix_UB_22      -0.0098700000
_diffrn_orient_matrix_UB_23      -0.0400309000
_diffrn_orient_matrix_UB_31      0.0457119000
_diffrn_orient_matrix_UB_32      -0.0158319000
_diffrn_orient_matrix_UB_33      0.0392534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55604
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         2.564
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.2696
_exptl_crystal_size_mid          0.2259
_exptl_crystal_size_min          0.0311
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0292P)^2^+1.5049P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4928
_reflns_number_total             5687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01068c2.cif
_cod_data_source_block           compound19
_cod_depositor_comments
'Adding full bibliography for 7035093--7035094.cif.'
_cod_original_cell_volume        1958.11(6)
_cod_database_code               7035094
_chemical_oxdiff_formula         'C22 H14 B F10 N'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              60396
_shelxl_version_number           2013-2