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_7040819
_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         'C36 H17 B2 F20 P'
_chemical_formula_sum            'C36 H17 B2 F20 P'
_chemical_formula_weight         882.08
_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             2014-11-28
_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                100.459(5)
_cell_angle_beta                 101.468(5)
_cell_angle_gamma                103.921(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4739(4)
_cell_length_b                   11.1509(5)
_cell_length_c                   17.5370(11)
_cell_measurement_reflns_used    14323
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      30.0510
_cell_measurement_theta_min      2.0230
_cell_volume                     1710.34(17)
_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      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9996
_diffrn_measurement_details
;
  1 omega  -10.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   19.0000   60.0000 44

  2 omega   55.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   19.0000   60.0000 39

  3 omega    6.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   57.0000  120.0000 86

  4 omega    6.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   57.0000  -60.0000 76

  5 omega   -4.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   77.0000 -180.0000 92

  6 omega   -4.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708   77.0000    0.0000 86

  7 omega  -41.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708  -57.0000 -120.0000 84

  8 omega   -9.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708  -99.0000 -180.0000 74

  9 omega  -47.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708  -19.0000  -60.0000 110

 10 omega   44.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708 -137.0000   61.0000 43

 11 omega  -46.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8708  -38.0000   60.0000 81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0684000000
_diffrn_orient_matrix_UB_12      0.0414044000
_diffrn_orient_matrix_UB_13      -0.0018182000
_diffrn_orient_matrix_UB_21      0.0225904000
_diffrn_orient_matrix_UB_22      0.0190455000
_diffrn_orient_matrix_UB_23      0.0424614000
_diffrn_orient_matrix_UB_31      0.0343519000
_diffrn_orient_matrix_UB_32      -0.0498604000
_diffrn_orient_matrix_UB_33      0.0007753000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0271
_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       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         1.939
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87824
_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    1.713
_exptl_crystal_description       irregular
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.2574
_exptl_crystal_size_mid          0.2111
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0375P)^2^+0.8404P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8267
_reflns_number_total             9970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03490j2.cif
_cod_data_source_block           compound13
_cod_depositor_comments
'Adding full bibliography for 7040818--7040820.cif.'
_cod_original_cell_volume        1710.34(16)
_cod_database_code               7040819
_chemical_oxdiff_formula         'C36 H17 B2 F20 P'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_res_checksum              10472
_shelxl_version_number           2013-2