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_7709813
_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_absolute_configuration ad
_chemical_formula_moiety         'C14 H18 B2'
_chemical_formula_sum            'C14 H18 B2'
_chemical_formula_weight         207.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.68940(11)
_cell_length_b                   10.29021(14)
_cell_length_c                   12.63823(14)
_cell_measurement_reflns_used    17389
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.2030
_cell_measurement_theta_min      4.5030
_cell_volume                     1260.11(3)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -58.00  23.00   1.00   12.00    --  -38.50  38.00 -30.00   81
  2  \w    -92.00  -4.00   1.00   12.00    --  -38.50 125.00 150.00   88
  3  \w    -85.00  -2.00   1.00   12.00    --  -38.50 125.00 -30.00   83
  4  \w     74.00 105.00   1.00   12.00    --   43.45  77.00 150.00   31
  5  \w     14.00  74.00   1.00   12.00    --   43.45  77.00 -90.00   60
  6  \w     35.00  62.00   1.00   12.00    --   43.45  38.00-180.00   27
  7  \w     23.00 113.00   1.00   12.00    --   43.45  38.00 -90.00   90
  8  \w     19.00  53.00   1.00   12.00    --   43.45  77.00 150.00   34
  9  \w     13.00  98.00   1.00   12.00    --   43.45  77.00   0.00   85
 10  \w     19.00  49.00   1.00   12.00    --   43.45  57.00 -30.00   30
 11  \w     13.00  82.00   1.00   12.00    --   43.45  77.00  90.00   69
 12  \w    -28.00  39.00   1.00   12.00    --   43.45 -38.00  90.00   67
 13  \w     25.00  84.00   1.00   12.00    --   43.45  38.00  90.00   59
 14  \w     19.00  85.00   1.00   12.00    --   43.45  57.00-150.00   66
 15  \w     65.00 109.00   1.00   12.00    --   43.45  57.00 -30.00   44
 16  \w     15.00  40.00   1.00   12.00    --   43.45  77.00-150.00   25
 17  \w     86.00 114.00   1.00   48.00    --  111.00  61.00  90.00   28
 18  \w     85.00 115.00   1.00   48.00    --  111.00  61.00 150.00   30
 19  \w     63.00 105.00   1.00   48.00    --  111.00 -94.00-180.00   42
 20  \w     85.00 112.00   1.00   48.00    --  111.00  61.00  60.00   27
 21  \w     86.00 116.00   1.00   48.00    --  111.00  61.00 -90.00   30
 22  \w     42.00 133.00   1.00   48.00    --  111.00 -45.00 -90.00   91
 23  \w     41.00 115.00   1.00   48.00    --  111.00-125.00 150.00   74
 24  \w     85.00 149.00   1.00   48.00    --  111.00  61.00-180.00   64
 25  \w     85.00 111.00   1.00   48.00    --  111.00  61.00 120.00   26
 26  \w    123.00 159.00   1.00   48.00    --  111.00  69.00 -24.55   36
 27  \w     81.00 166.00   1.00   48.00    --  111.00  77.00 -60.00   85
 28  \w     81.00 160.00   1.00   48.00    --  111.00  77.00 -90.00   79
 29  \w     81.00 155.00   1.00   48.00    --  111.00  77.00   0.00   74
 30  \w     81.00 108.00   1.00   48.00    --  111.00  77.00-120.00   27
 31  \w     85.00 133.00   1.00   48.00    --  111.00  61.00-150.00   48
 32  \w     43.00 133.00   1.00   48.00    --  111.00 -45.00  90.00   90
 33  \w     32.00 102.00   1.00   48.00    --  111.00 -94.00 -60.00   70
 34  \w     81.00 163.00   1.00   48.00    --  111.00  77.00 150.00   82
 35  \w     85.00 112.00   1.00   48.00    --  111.00  61.00 -30.00   27
 36  \w     76.00 118.00   1.00   48.00    --  111.00-125.00  60.00   42
 37  \w    115.00 173.00   1.00   48.00    --  111.00 125.00-180.00   58
 38  \w    134.00 161.00   1.00   48.00    --  111.00  61.00  30.00   27
 39  \w     36.00 110.00   1.00   48.00    --  111.00 -94.00-120.00   74
 40  \w     82.00 107.00   1.00   48.00    --  111.00  77.00-180.00   25
 41  \w     86.00 113.00   1.00   48.00    --  111.00  61.00  30.00   27
 42  \w     85.00 118.00   1.00   48.00    --  111.00  61.00   0.00   33
 43  \w     85.00 112.00   1.00   48.00    --  111.00  61.00 -60.00   27
 44  \w     81.00 108.00   1.00   48.00    --  111.00  77.00 120.00   27
 45  \w     89.00 115.00   1.00   48.00    --  111.00  45.00-120.00   26
 46  \w    118.00 176.00   1.00   48.00    --  111.00  77.00-150.00   58
 47  \w     86.00 111.00   1.00   48.00    --  111.00  61.00-120.00   25
 48  \w     81.00 108.00   1.00   48.00    --  111.00  77.00-150.00   27
 49  \w     89.00 174.00   1.00   48.00    --  111.00  45.00 120.00   85
 50  \w     89.00 152.00   1.00   48.00    --  111.00  45.00 -90.00   63
 51  \w     81.00 115.00   1.00   48.00    --  111.00  77.00  60.00   34
 52  \w    128.00 164.00   1.00   48.00    --  111.00  61.00  90.00   36
 53  \w     83.00 109.00   1.00   48.00    --  111.00  69.00 -24.55   26
 54  \w     86.00 176.00   1.00   48.00    --  111.00  58.00  46.62   90
;
_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      -0.0345893000
_diffrn_orient_matrix_UB_12      -0.0534435000
_diffrn_orient_matrix_UB_13      -0.1107188000
_diffrn_orient_matrix_UB_21      -0.1392971000
_diffrn_orient_matrix_UB_22      0.0721018000
_diffrn_orient_matrix_UB_23      0.0025789000
_diffrn_orient_matrix_UB_31      0.0683725000
_diffrn_orient_matrix_UB_32      0.1198555000
_diffrn_orient_matrix_UB_33      -0.0508349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17567
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.137
_diffrn_reflns_theta_min         5.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.522
_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    1.096
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.488
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1087 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0684P)^2^+0.1084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5050
_reflns_number_total             5111
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9925\% 
 around [-0.00 0.55 0.83] (reciprocal) or [-0.00 0.71 0.71] (direct)
Component 3 rotated by 3.2778\% 
 around [0.20 0.10 0.97] (reciprocal) or [0.32 0.15 0.93] (direct)
;
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           1
_cod_database_code               7709813
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C14 H18 B2'
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.818
_diffrn_oxdiff_ac3_digest_frames
;
01915c363ed02423d1b16c58d7d52cde3502783af0f
;
_diffrn_oxdiff_ac3_digest_hkl
;
01d00261c589d4282ad2ef2158a96b2cf37728
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.606(5)
 0.234(3) 0.160(4)
;
_shelx_res_checksum              12016
_shelx_hkl_checksum              97090
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.655
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3