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_7709821
_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         'C12 H21 As B2 N, C14 H19 N2'
_chemical_formula_sum            'C26 H40 As B2 N3'
_chemical_formula_weight         491.15
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-16
_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                64.302(3)
_cell_angle_beta                 88.211(3)
_cell_angle_gamma                78.193(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1038(4)
_cell_length_b                   11.6718(4)
_cell_length_c                   12.9599(4)
_cell_measurement_reflns_used    9206
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4540
_cell_measurement_theta_min      3.7600
_cell_volume                     1345.18(9)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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 -11.00   1.00    4.50    --  -42.08 -77.00-150.00   47
  2  \w    -89.00 -36.00   1.00    4.50    --  -42.08 178.00-150.00   53
  3  \w   -116.00 -89.00   1.00    4.50    --  -42.08 -77.00-150.00   27
  4  \w    -52.00 -24.00   1.00    4.50    --  -42.08 -38.00 -90.00   28
  5  \w   -115.00 -67.00   1.00    4.50    --  -42.08 -38.00 120.00   48
  6  \w   -112.00 -22.00   1.00    4.50    --  -42.08 -38.00-150.00   90
  7  \w   -106.00 -15.00   1.00    4.50    --  -42.08 -57.00  60.00   91
  8  \w    -48.00 -11.00   1.00    4.50    --  -42.08 -77.00 120.00   37
  9  \w    -86.00 -11.00   1.00    4.50    --  -42.08 -77.00 -60.00   75
 10  \w   -115.00 -11.00   1.00    4.50    --  -42.08 -77.00  30.00  104
 11  \w   -127.00 -40.00   1.00    4.50    --  -42.08 178.00 120.00   87
 12  \w    -60.00 -23.00   1.00    4.50    --  -42.08 -38.00 120.00   37
 13  \w    -25.00  65.00   1.00    4.50    --   42.08 -57.00  90.00   90
 14  \w     57.00 126.00   1.00    4.50    --   42.08 178.00 120.00   69
 15  \w     40.00 118.00   1.00   18.00    --  111.00-125.00 -60.00   78
 16  \w     83.00 110.00   1.00   18.00    --  111.00  61.00   0.00   27
 17  \w     85.00 178.00   1.00   18.00    --  111.00  56.00 107.44   93
 18  \w     84.00 174.00   1.00   18.00    --  111.00  61.00 -30.00   90
 19  \w     30.00 108.00   1.00   18.00    --  111.00 -94.00  60.00   78
 20  \w    134.00 161.00   1.00   18.00    --  111.00  61.00-122.81   27
 21  \w    127.00 178.00   1.00   18.00    --  111.00  60.00 133.99   51
 22  \w     37.00 138.00   1.00   18.00    --  111.00 -77.00  90.00  101
 23  \w     83.00 120.00   1.00   18.00    --  111.00  61.00-180.00   37
 24  \w     83.00 113.00   1.00   18.00    --  111.00  61.00  30.00   30
 25  \w     80.00 111.00   1.00   18.00    --  111.00  77.00 -60.00   31
 26  \w     83.00 110.00   1.00   18.00    --  111.00  61.00 150.00   27
 27  \w     80.00 177.00   1.00   18.00    --  111.00  77.00  60.00   97
 28  \w     83.00 145.00   1.00   18.00    --  111.00  61.00  60.00   62
 29  \w     87.00 114.00   1.00   18.00    --  111.00  45.00 -90.00   27
 30  \w     83.00 110.00   1.00   18.00    --  111.00  61.00  90.00   27
 31  \w     80.00 107.00   1.00   18.00    --  111.00  77.00 -90.00   27
 32  \w     80.00 107.00   1.00   18.00    --  111.00  77.00-120.00   27
 33  \w     83.00 110.00   1.00   18.00    --  111.00  61.00-122.81   27
 34  \w     80.00 108.00   1.00   18.00    --  111.00  77.00  30.00   28
 35  \w     80.00 178.00   1.00   18.00    --  111.00  77.00   0.00   98
 36  \w     84.00 178.00   1.00   18.00    --  111.00  61.00-150.00   94
 37  \w     60.00 140.00   1.00   18.00    --  111.00 -77.00 -90.00   80
 38  \w     83.00 111.00   1.00   18.00    --  111.00  61.00 120.00   28
 39  \w     81.00 152.00   1.00   18.00    --  111.00  77.00-180.00   71
 40  \w     80.00 107.00   1.00   18.00    --  111.00  77.00 -30.00   27
 41  \w     80.00 114.00   1.00   18.00    --  111.00  77.00 150.00   34
 42  \w     87.00 116.00   1.00   18.00    --  111.00  45.00-120.00   29
 43  \w     83.00 178.00   1.00   18.00    --  111.00  61.00 -90.00   95
 44  \w     85.00 177.00   1.00   18.00    --  111.00  61.00 -60.00   92
 45  \w     87.00 115.00   1.00   18.00    --  111.00  53.00 120.55   28
 46  \w     85.00 111.00   1.00   18.00    --  111.00  60.00 133.99   26
 47  \w     82.00 108.00   1.00   18.00    --  111.00  68.00   4.26   26
;
_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      0.0150447000
_diffrn_orient_matrix_UB_12      0.0586055000
_diffrn_orient_matrix_UB_13      -0.1304653000
_diffrn_orient_matrix_UB_21      -0.0682584000
_diffrn_orient_matrix_UB_22      0.1357646000
_diffrn_orient_matrix_UB_23      -0.0107506000
_diffrn_orient_matrix_UB_31      0.1395792000
_diffrn_orient_matrix_UB_32      0.0245095000
_diffrn_orient_matrix_UB_33      0.0184467000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.126
_diffrn_reflns_theta_min         3.793
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_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    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.8401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4548
_reflns_number_total             5261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[2N--C(CD3)AsH2][3-H]'
_cod_original_cell_volume        1345.17(9)
_cod_database_code               7709821
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 H20.62 As B2 N, C14 H19 N2'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.712
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
 C12-C11 \\sim C12B-C11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(As1) = Uanis(C12B)
Uanis(C12) = Uanis(As1B)
4. Others
 Sof(As1B)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(As1)=Sof(H1A)=Sof(H1B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
5.a Me refined with riding coordinates:
 C12B(H12D,H12E,H12F)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C18(H18),
 C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              14047
_shelx_hkl_checksum              41899
_olex2_date_sample_data_collection 2018-07-11
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.687