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_7709820
_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 H20 B2 N'
_chemical_formula_sum            'C28 H39 B2 N3'
_chemical_formula_weight         439.24
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.630(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.0261(3)
_cell_length_b                   41.6493(15)
_cell_length_c                   16.3643(4)
_cell_measurement_reflns_used    29132
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.7250
_cell_measurement_theta_min      2.9870
_cell_volume                     7767.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_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    -48.00 -16.00   1.00   20.00    --  -38.25 -38.00-150.00   32
  2  \w    -42.00 -12.00   1.00   20.00    --  -38.25 -57.00 -60.00   30
  3  \w    -55.00  -2.00   1.00   20.00    --  -38.25 -77.00  60.00   53
  4  \w    -86.00 -48.00   1.00   20.00    --  -38.25 -77.00 -30.00   38
  5  \w    -67.00  36.00   1.00   20.00    --  -38.25  57.00 -90.00  103
  6  \w    -61.00  -7.00   1.00   20.00    --  -38.25 -38.00 120.00   54
  7  \w   -113.00 -42.00   1.00   20.00    --  -38.25-178.00   0.00   71
  8  \w   -107.00 -59.00   1.00   20.00    --  -38.25 -57.00  90.00   48
  9  \w    -80.00 -11.00   1.00   20.00    --  -38.25 -77.00-150.00   69
 10  \w   -129.00 -42.00   1.00   20.00    --  -38.25 178.00-120.00   87
 11  \w   -113.00 -43.00   1.00   20.00    --  -38.25 -57.00 -60.00   70
 12  \w    -54.00 -12.00   1.00   20.00    --  -38.25 -38.00   0.00   42
 13  \w   -118.00 -72.00   1.00   20.00    --  -38.25 -77.00  60.00   46
 14  \w   -131.00 -35.00   1.00   20.00    --  -38.25-178.00  60.00   96
 15  \w   -106.00 -51.00   1.00   20.00    --  -38.25 178.00 -60.00   55
 16  \w    -42.00  -2.00   1.00   20.00    --  -38.25 -77.00 -30.00   40
 17  \w   -117.00 -59.00   1.00   20.00    --  -38.25 -38.00   0.00   58
 18  \w   -111.00 -63.00   1.00   20.00    --  -38.25 -38.00 120.00   48
 19  \w   -117.00 -50.00   1.00   20.00    --  -38.25 -38.00-150.00   67
 20  \w   -115.00 -87.00   1.00   20.00    --  -38.25 -77.00-150.00   28
 21  \w   -117.00 -69.00   1.00   20.00    --  -38.25 -77.00 -90.00   48
 22  \w    -57.00  -2.00   1.00   20.00    --  -38.25 -77.00 -90.00   55
 23  \w    -56.00  -6.00   1.00   20.00    --  -38.25 -57.00  90.00   50
 24  \w     -1.00  24.00   1.00   20.00    --   38.25  96.00 160.55   25
 25  \w     27.00  70.00   1.00   20.00    --   38.25 -99.00 -60.00   43
 26  \w    119.00 145.00   1.00   60.00    --  115.00  67.00  20.49   26
 27  \w     80.00 106.00   1.00   60.00    --  115.00  70.00   4.66   26
 28  \w    110.00 177.00   1.00   60.00    --  115.00  73.00 -33.59   67
 29  \w     38.00  81.00   1.00   60.00    --  115.00-126.00   4.96   43
 30  \w     96.00 122.00   1.00   60.00    --  115.00-126.00   4.96   26
 31  \w     80.00 106.00   1.00   60.00    --  115.00  67.00  20.49   26
 32  \w     82.00 122.00   1.00   60.00    --  115.00  59.00-111.38   40
 33  \w     80.00 107.00   1.00   60.00    --  115.00  73.00 -33.59   27
 34  \w     80.00 106.00   1.00   60.00    --  115.00  74.00-110.33   26
 35  \w     80.00 106.00   1.00   60.00    --  115.00  67.00 -60.35   26
 36  \w     81.00 117.00   1.00   60.00    --  115.00  68.00-146.37   36
 37  \w     83.00 109.00   1.00   60.00    --  115.00  55.00 -38.55   26
 38  \w     83.00 109.00   1.00   60.00    --  115.00  50.00-111.05   26
 39  \w     82.00 111.00   1.00   60.00    --  115.00  57.00 -18.96   29
 40  \w     82.00 108.00   1.00   60.00    --  115.00  58.00 -30.59   26
 41  \w     80.00 106.00   1.00   60.00    --  115.00  71.00 148.14   26
 42  \w    114.00 178.00   1.00   60.00    --  115.00  77.00-180.00   64
 43  \w     79.00 105.00   1.00   60.00    --  115.00  77.00-180.00   26
 44  \w     80.00 175.00   1.00   60.00    --  115.00  69.00 159.35   95
 45  \w    147.00 174.00   1.00   60.00    --  115.00  66.00 124.14   27
 46  \w     82.00 155.00   1.00   60.00    --  115.00  61.00  60.00   73
 47  \w     35.00 116.00   1.00   60.00    --  115.00-111.00 150.00   81
 48  \w     79.00 175.00   1.00   60.00    --  115.00  77.00 -90.00   96
 49  \w     82.00 110.00   1.00   60.00    --  115.00  61.00-150.00   28
 50  \w     32.00  64.00   1.00   60.00    --  115.00 -77.00-120.00   32
 51  \w     78.00 150.00   1.00   60.00    --  115.00 -77.00-120.00   72
 52  \w     79.00 172.00   1.00   60.00    --  115.00  77.00  30.00   93
 53  \w     82.00 108.00   1.00   60.00    --  115.00  61.00 120.00   26
 54  \w     82.00 108.00   1.00   60.00    --  115.00  61.00-180.00   26
 55  \w     79.00 105.00   1.00   60.00    --  115.00  77.00 -30.00   26
 56  \w     84.00 110.00   1.00   60.00    --  115.00  45.00  90.00   26
 57  \w    140.00 173.00   1.00   60.00    --  115.00  45.00  90.00   33
 58  \w     84.00 110.00   1.00   60.00    --  115.00  45.00-150.00   26
 59  \w     79.00 178.00   1.00   60.00    --  115.00  77.00  60.00   99
 60  \w     82.00 177.00   1.00   60.00    --  115.00  61.00   0.00   95
 61  \w     80.00 108.00   1.00   60.00    --  115.00  67.00 -93.29   28
 62  \w     79.00 105.00   1.00   60.00    --  115.00  77.00 120.00   26
 63  \w     50.00 112.00   1.00   60.00    --  115.00-111.00-120.00   62
 64  \w     83.00 109.00   1.00   60.00    --  115.00  53.00 106.99   26
 65  \w    118.00 144.00   1.00   60.00    --  115.00  66.00 124.14   26
 66  \w     81.00 107.00   1.00   60.00    --  115.00  62.00   6.90   26
 67  \w     43.00 150.00   1.00   60.00    --  115.00 -77.00 150.00  107
 68  \w     33.00 101.00   1.00   60.00    --  115.00 -94.00  30.00   68
 69  \w    127.00 152.00   1.00   60.00    --  115.00  73.00  91.99   25
 70  \w     79.00 105.00   1.00   60.00    --  115.00  77.00-120.00   26
 71  \w     82.00 108.00   1.00   60.00    --  115.00  61.00 150.00   26
 72  \w     80.00 106.00   1.00   60.00    --  115.00  73.00  91.99   26
 73  \w     80.00 106.00   1.00   60.00    --  115.00  66.00 124.14   26
 74  \w     82.00 108.00   1.00   60.00    --  115.00  61.00 -60.00   26
 75  \w     82.00 108.00   1.00   60.00    --  115.00  61.00  90.00   26
 76  \w     77.00 153.00   1.00   60.00    --  115.00  30.00 150.00   76
 77  \w     79.00 177.00   1.00   60.00    --  115.00  77.00 -60.00   98
 78  \w    153.00 178.00   1.00   60.00    --  115.00  70.00-116.95   25
 79  \w     82.00 108.00   1.00   60.00    --  115.00  61.00-120.00   26
 80  \w     77.00 103.00   1.00   60.00    --  115.00  30.00-180.00   26
 81  \w     84.00 116.00   1.00   60.00    --  115.00-111.00  90.00   32
 82  \w     34.00  79.00   1.00   60.00    --  115.00-111.00  90.00   45
 83  \w     80.00 106.00   1.00   60.00    --  115.00  70.00-116.95   26
 84  \w    136.00 162.00   1.00   60.00    --  115.00  59.00-111.38   26
 85  \w     82.00 108.00   1.00   60.00    --  115.00  60.00  21.57   26
 86  \w     82.00 147.00   1.00   60.00    --  115.00  59.00-130.00   65
 87  \w    104.00 177.00   1.00   60.00    --  115.00 111.00-150.00   73
 88  \w     79.00 109.00   1.00   60.00    --  115.00  65.00  32.41   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1317921000
_diffrn_orient_matrix_UB_12      -0.0003443000
_diffrn_orient_matrix_UB_13      -0.0516581000
_diffrn_orient_matrix_UB_21      0.0298493000
_diffrn_orient_matrix_UB_22      -0.0024909000
_diffrn_orient_matrix_UB_23      -0.0846485000
_diffrn_orient_matrix_UB_31      -0.0006590000
_diffrn_orient_matrix_UB_32      -0.0368949000
_diffrn_orient_matrix_UB_33      0.0064442000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            156033
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.540
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.127
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         16176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0800
_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^)+(0.0793P)^2^+9.5508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13161
_reflns_number_total             16176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[1-NH2][3-H]'
_cod_original_cell_volume        7767.1(4)
_cod_database_code               7709820
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C28 H33 B2 N3'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.868
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22),
 C23(H23), C30(H30), C31(H31), C32(H32), C37(H37), C38(H38), C39(H39), C46(H46),
  C47(H47), C48(H48), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C69(H69), C70(H70), C71(H71), C73(H73), C74(H74), C75(H75), C86(H86),
  C87(H87), C88(H88), C97(H97), C98(H98), C99(H99)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44B,H44A,H44C), C45(H45A,
 H45B,H45C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              7012
_shelx_hkl_checksum              56355
_olex2_date_sample_data_collection 2018-04-04
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.714
_oxdiff_exptl_absorpt_empirical_full_min 0.467