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_7709815
_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 B2 S, C14 H19 N2'
_chemical_formula_sum            'C28 H38 B2 N2 S'
_chemical_formula_weight         456.28
_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             2018-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.83180(10)
_cell_length_b                   24.3010(2)
_cell_length_c                   11.73750(10)
_cell_measurement_reflns_used    24806
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2170
_cell_measurement_theta_min      3.6350
_cell_volume                     2666.14(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.01(10)
_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 1.000
_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     10.00  37.00   1.00    1.00    --   -1.89 -99.00 120.00   27
  2  \w    -47.00 -20.00   1.00    1.00    --   -1.89  57.00  60.00   27
  3  \w    -92.00 -64.00   1.00    1.00    --   -1.89 178.00-150.00   28
  4  \w    -62.00 -35.00   1.00    1.00    --   -1.89 178.00-150.00   27
  5  \w    -99.00  44.00   1.00    1.00    --   -1.89 -57.00  90.00  143
  6  \w     -9.00  95.00   1.00    1.00    --   -1.89  57.00  60.00  104
  7  \w    -99.00 -53.00   1.00    1.00    --    1.89 178.00 150.00   46
  8  \w    -49.00 -16.00   1.00    1.00    --  -62.45 -77.00-150.00   33
  9  \w   -109.00 -51.00   1.00    1.00    --  -62.45  77.00  90.00   58
 10  \w   -165.00 -60.00   1.00    1.00    --  -62.45 -77.00 120.00  105
 11  \w    -10.00  41.00   1.00    1.00    --  -62.45  77.00  90.00   51
 12  \w   -153.00 -48.00   1.00    1.00    --  -62.45 -45.00 -90.00  105
 13  \w    -56.00 -17.00   1.00    1.00    --  -62.45 -68.00  65.66   39
 14  \w   -166.00-120.00   1.00    1.00    --  -62.45 -77.00 -60.00   46
 15  \w    -92.00 -39.00   1.00    1.00    --  -62.45 125.00  60.00   53
 16  \w   -151.00 -16.00   1.00    1.00    --  -62.45 -77.00-120.00  135
 17  \w    -43.00 -17.00   1.00    1.00    --  -62.45 -64.00 142.10   26
 18  \w    -42.00 -16.00   1.00    1.00    --  -62.45 -77.00  30.00   26
 19  \w    -45.00 -19.00   1.00    1.00    --  -62.45 -45.00 -90.00   26
 20  \w   -123.00 -74.00   1.00    1.00    --  -62.45 -77.00-150.00   49
 21  \w   -156.00 -47.00   1.00    1.00    --  -62.45 -64.00 142.10  109
 22  \w   -165.00 -89.00   1.00    1.00    --  -62.45 -77.00   0.00   76
 23  \w    -58.00 -16.00   1.00    1.00    --  -62.45 -77.00 -60.00   42
 24  \w    -44.00 -16.00   1.00    1.00    --  -62.45 -77.00 120.00   28
 25  \w   -164.00 -60.00   1.00    1.00    --  -62.45 -68.00  65.66  104
 26  \w    -50.00 -17.00   1.00    1.00    --  -62.45 -77.00   0.00   33
 27  \w   -135.00 -62.00   1.00    1.00    --  -62.45 -77.00  30.00   73
 28  \w   -109.00 -23.00   1.00    1.00    --  -62.45  77.00 -30.00   86
 29  \w     16.00  41.00   1.00    1.00    --   62.45  82.00-146.82   25
 30  \w     16.00  41.00   1.00    1.00    --   62.45  82.00  35.92   25
 31  \w     16.00  41.00   1.00    1.00    --   62.45  81.00 143.42   25
 32  \w     26.00 114.00   1.00    1.00    --   62.45-125.00-150.00   88
 33  \w    103.00 145.00   1.00    1.00    --   62.45  77.00 120.00   42
 34  \w     16.00  43.00   1.00    1.00    --   62.45  77.00 120.00   27
 35  \w     77.00 150.00   1.00    1.00    --  123.00  77.00-120.00   73
 36  \w     77.00 138.00   1.00    1.00    --  123.00  77.00  60.00   61
 37  \w     78.00 168.00   1.00    1.00    --  123.00  63.00  90.00   90
 38  \w    100.00 175.00   1.00    1.00    --  123.00 111.00-180.00   75
 39  \w     77.00 103.00   1.00    1.00    --  123.00  77.00-150.00   26
 40  \w     78.00 104.00   1.00    1.00    --  123.00  77.00 150.00   26
 41  \w     78.00 156.00   1.00    1.00    --  123.00  63.00 150.00   78
 42  \w     77.00 139.00   1.00    1.00    --  123.00  77.00-180.00   62
 43  \w    109.00 137.00   1.00    1.00    --  123.00  63.00-120.00   28
 44  \w     78.00 178.00   1.00    1.00    --  123.00  66.00 -20.61  100
 45  \w     77.00 103.00   1.00    1.00    --  123.00  77.00  30.00   26
 46  \w     73.00 148.00   1.00    1.00    --  123.00 178.00  90.00   75
 47  \w     87.00 113.00   1.00    1.00    --  123.00-111.00-150.00   26
 48  \w     79.00 105.00   1.00    1.00    --  123.00  57.00 119.42   26
 49  \w    113.00 139.00   1.00    1.00    --  123.00  63.00 -30.00   26
 50  \w     78.00 105.00   1.00    1.00    --  123.00  63.00-120.00   27
 51  \w     78.00 103.00   1.00    1.00    --  123.00  63.00 -30.00   25
 52  \w     78.00 109.00   1.00    1.00    --  123.00  63.00  30.00   31
 53  \w     27.00  72.00   1.00    1.00    --  123.00-111.00-150.00   45
 54  \w    126.00 174.00   1.00    1.00    --  123.00  63.00 -90.00   48
 55  \w     78.00 104.00   1.00    1.00    --  123.00  63.00 -90.00   26
 56  \w     78.00 107.00   1.00    1.00    --  123.00  63.00  11.72   29
 57  \w     78.00 104.00   1.00    1.00    --  123.00  63.00-180.00   26
 58  \w     42.00 113.00   1.00    1.00    --  123.00-111.00 -60.00   71
 59  \w     28.00 113.00   1.00    1.00    --  123.00-111.00 120.00   85
 60  \w     28.00  64.00   1.00    1.00    --  123.00-111.00   0.00   36
 61  \w     78.00 117.00   1.00    1.00    --  123.00  50.00 -60.00   39
 62  \w     78.00 104.00   1.00    1.00    --  123.00  77.00   0.00   26
 63  \w     78.00 104.00   1.00    1.00    --  123.00  70.00 -74.84   26
 64  \w     78.00 104.00   1.00    1.00    --  123.00  63.00   0.00   26
 65  \w     29.00  86.00   1.00    1.00    --  123.00-111.00 -30.00   57
 66  \w    135.00 164.00   1.00    1.00    --  123.00  63.00-150.00   29
 67  \w     78.00 104.00   1.00    1.00    --  123.00  63.00-150.00   26
 68  \w     77.00 103.00   1.00    1.00    --  123.00  50.00-150.00   26
 69  \w     19.00 168.00   1.00    1.00    --  123.00 -77.00 120.00  149
 70  \w     77.00 102.00   1.00    1.00    --  123.00  50.00-180.00   25
 71  \w     78.00 175.00   1.00    1.00    --  123.00  57.00  45.35   97
 72  \w     77.00 151.00   1.00    1.00    --  123.00  66.00 128.99   74
 73  \w     78.00 104.00   1.00    1.00    --  123.00  61.00 -41.00   26
 74  \w     78.00 117.00   1.00    1.00    --  123.00  63.00 120.00   39
 75  \w     78.00 103.00   1.00    1.00    --  123.00  63.00  60.00   25
 76  \w     77.00 109.00   1.00    1.00    --  123.00  50.00-120.00   32
 77  \w     78.00 104.00   1.00    1.00    --  123.00  63.00 -60.00   26
 78  \w     77.00 103.00   1.00    1.00    --  123.00  50.00 120.00   26
 79  \w    108.00 171.00   1.00    1.00    --  123.00  77.00   0.00   63
 80  \w     28.00 112.00   1.00    1.00    --  123.00-111.00  60.00   84
 81  \w     77.00 177.00   1.00    1.00    --  123.00  75.00 -68.56  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0194894000
_diffrn_orient_matrix_UB_12      0.0165488000
_diffrn_orient_matrix_UB_13      -0.1308318000
_diffrn_orient_matrix_UB_21      -0.1150805000
_diffrn_orient_matrix_UB_22      0.0421150000
_diffrn_orient_matrix_UB_23      0.0051813000
_diffrn_orient_matrix_UB_31      0.1163150000
_diffrn_orient_matrix_UB_32      0.0444008000
_diffrn_orient_matrix_UB_33      0.0438446000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.346
_diffrn_reflns_theta_min         3.638
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.137
_exptl_crystal_description       irregular
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0485P)^2^+0.9261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5029
_reflns_number_total             5265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[1-SH][3-H]'
_cod_database_code               7709815
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C28 H38 B2 N2 S'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1B-H1B
 1.306 with sigma of 0.02
 C14-B2 \\sim C14B-B2 \\sim C13-B2 \\sim C13B-B2 \\sim C11B-B1 \\sim C11-B1
\\sim C12B-B1 \\sim C12-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12B) = Uanis(C12)
Uanis(C11) = Uanis(C11B)
Uanis(C14) = Uanis(C14B)
Uanis(C13) = Uanis(C13B)
Uanis(S1B) = Uanis(S1)
Uiso(H1) = Uiso(H1B)
4. Others
 Sof(S1B)=Sof(H1B)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12B)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(S1)=Sof(H1)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=FVAR(1)
5.a Riding coordinates:
 S1B(H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12B(H12D,
 H12E,H12F), C13(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C14(H14A,H14B,H14C),
 C14B(H14D,H14E,H14F), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              34407
_shelx_hkl_checksum              21417
_olex2_date_sample_data_collection 2018-05-17
_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.836