Frustrated Lewis pair chemistry of hydride sponges
Becker, Christian; Schwabedissen, Jan; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00585A

data_7709823
_publ_section_title
;
 Frustrated Lewis pair chemistry of hydride sponges
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00585A
_journal_year                    2022
_chemical_formula_moiety         'C14 H19 N2, C14 H19 B2'
_chemical_formula_sum            'C28 H38 B2 N2'
_chemical_formula_weight         424.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.0174(12)
_cell_angle_beta                 90.4587(13)
_cell_angle_gamma                110.2753(14)
_cell_formula_units_Z            4
_cell_length_a                   12.06495(18)
_cell_length_b                   14.3416(2)
_cell_length_c                   15.7603(2)
_cell_measurement_reflns_used    57556
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      35.9150
_cell_measurement_theta_min      1.7990
_cell_volume                     2557.95(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00  63.00   1.00   32.00    --   24.96 -19.00  60.00  110
  2  \w     -4.00  94.00   1.00   32.00    --   24.96  77.00  90.00   98
  3  \w      3.00  96.00   1.00   32.00    --   24.96  38.00-120.00   93
  4  \w     -4.00  94.00   1.00   32.00    --   24.96  77.00 -90.00   98
  5  \w    -46.00  96.00   1.00   32.00    --   24.96   0.00-180.00  142
  6  \w     35.00  99.00   1.00   32.00    --   24.96 178.00  90.00   64
  7  \w      6.00  93.00   1.00   32.00    --   24.96  57.00  30.00   87
  8  \w    -20.00  65.00   1.00   32.00    --   24.96 -99.00  60.00   85
  9  \w    -20.00  65.00   1.00   32.00    --   24.96 -99.00-150.00   85
 10  \w     -4.00  94.00   1.00   32.00    --   24.96  77.00-180.00   98
 11  \w    -10.00  72.00   1.00   32.00    --   24.96-111.00 -38.38   82
 12  \w    -98.00 -34.00   1.00   32.00    --  -23.50 178.00  60.00   64
 13  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00-150.00  143
 14  \w    -73.00   6.00   1.00   32.00    --  -23.50 115.00  40.00   79
 15  \w    -95.00 -42.00   1.00   32.00    --  -23.50-170.00 168.00   53
 16  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00-120.00  143
 17  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00-180.00  143
 18  \w    -20.00  65.00   1.00   32.00    --   24.96 -99.00-180.00   85
 19  \w      3.00  96.00   1.00   32.00    --   24.96  38.00 -30.00   93
 20  \w     -4.00  94.00   1.00   32.00    --   24.96  77.00 -30.00   98
 21  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00 -60.00  143
 22  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00 -30.00  143
 23  \w    -95.00  48.00   1.00   32.00    --  -23.50   0.00 -90.00  143
 24  \w     77.00 136.00   1.00   32.00    --   67.05  77.00  88.01   59
 25  \w     -1.00  84.00   1.00   32.00    --   67.05 -45.00 150.00   85
 26  \w      5.00  73.00   1.00   32.00    --   67.05 -77.00  60.00   68
 27  \w      6.00  84.00   1.00   32.00    --   67.05 -77.00 -90.00   78
 28  \w     38.00  63.00   1.00   32.00    --   67.05  77.00 -60.00   25
 29  \w     81.00 130.00   1.00   32.00    --   67.05  77.00 -60.00   49
 30  \w     38.00  68.00   1.00   32.00    --   67.05  77.00  30.00   30
 31  \w     74.00 127.00   1.00   32.00    --   67.05  77.00  30.00   53
 32  \w     25.00 105.00   1.00   32.00    --   67.05-125.00  60.00   80
 33  \w     38.00  65.00   1.00   32.00    --   67.05  77.00-150.00   27
 34  \w     77.00 131.00   1.00   32.00    --   67.05  77.00-150.00   54
 35  \w     -3.00 105.00   1.00   32.00    --   67.05 -94.00 150.00  108
 36  \w     38.00  68.00   1.00   32.00    --   67.05  77.00 -30.00   30
 37  \w     75.00 124.00   1.00   32.00    --   67.05  77.00 -30.00   49
 38  \w     38.00  63.00   1.00   32.00    --   67.05  77.00  60.00   25
 39  \w     78.00 131.00   1.00   32.00    --   67.05  77.00  60.00   53
 40  \w     86.00 131.00   1.00   32.00    --   67.05 125.00  90.00   45
 41  \w     38.00  63.00   1.00   32.00    --   67.05  77.00   0.00   25
 42  \w     82.00 130.00   1.00   32.00    --   67.05  77.00   0.00   48
 43  \w     38.00  66.00   1.00   32.00    --   67.05  77.00 -90.00   28
 44  \w     76.00 116.00   1.00   32.00    --   67.05  77.00 -90.00   40
 45  \w     38.00  64.00   1.00   32.00    --   67.05  77.00-180.00   26
 46  \w     78.00 129.00   1.00   32.00    --   67.05  77.00-180.00   51
 47  \w     38.00  64.00   1.00   32.00    --   67.05  77.00 150.00   26
 48  \w     78.00 132.00   1.00   32.00    --   67.05  77.00 150.00   54
 49  \w     38.00  64.00   1.00   32.00    --   67.05  77.00-120.00   26
 50  \w     79.00 136.00   1.00   32.00    --   67.05  77.00-120.00   57
 51  \w     38.00  63.00   1.00   32.00    --   67.05  77.00 120.00   25
 52  \w     75.00 101.00   1.00   32.00    --   67.05  77.00 120.00   26
 53  \w     38.00  65.00   1.00   32.00    --   67.05  77.00  88.01   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116334000
_diffrn_orient_matrix_UB_12      -0.0040172000
_diffrn_orient_matrix_UB_13      -0.0442922000
_diffrn_orient_matrix_UB_21      -0.0189000000
_diffrn_orient_matrix_UB_22      -0.0525407000
_diffrn_orient_matrix_UB_23      0.0029845000
_diffrn_orient_matrix_UB_31      -0.0586149000
_diffrn_orient_matrix_UB_32      -0.0017987000
_diffrn_orient_matrix_UB_33      0.0074123000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            249239
_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         36.318
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
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    1.102
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         24769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0680P)^2^+0.8049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17081
_reflns_number_total             24769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[1-H][3-H]'
_cod_database_code               7709823
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C28H38B2N2
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
;
_shelx_res_checksum              17076
_shelx_hkl_checksum              82274
_olex2_date_sample_data_collection 2017-10-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.887