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_7709818
_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         '2(C14 H19 N2), 2(C15 H18 B2 N), C2 H3 N'
_chemical_formula_sum            'C60 H77 B4 N7'
_chemical_formula_weight         939.52
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                81.602(4)
_cell_angle_beta                 85.872(4)
_cell_angle_gamma                85.229(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8110(5)
_cell_length_b                   16.5987(7)
_cell_length_c                   17.3054(7)
_cell_measurement_reflns_used    9145
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9980
_cell_measurement_theta_min      2.6690
_cell_volume                     2773.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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      100.00(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 0.977
_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    -35.00  -6.00   1.00    1.00    --  -38.50 125.00 -30.00   29
  2  \w   -109.00 -22.00   1.00    1.00    --  -38.50 -38.00 120.00   87
  3  \w    -71.00  39.00   1.00    1.00    --  -38.50  19.00 -60.00  110
  4  \w    -74.00  -9.00   1.00    1.00    --  -38.50 125.00 -90.00   65
  5  \w     55.00  95.00   1.00    1.00    --   42.70-125.00-150.00   40
  6  \w     27.00  72.00   1.00    1.00    --   42.70-125.00  90.00   45
  7  \w     96.00 177.00   1.00    2.50    --  111.00  30.00-180.00   81
  8  \w     66.00 133.00   1.00    2.50    --  111.00 -45.00   0.00   67
  9  \w     43.00  73.00   1.00    2.50    --  111.00-143.00  37.58   30
 10  \w    110.00 176.00   1.00    2.50    --  111.00  77.00  90.00   66
 11  \w     75.00 113.00   1.00    2.50    --  111.00-125.00-180.00   38
 12  \w    103.00 140.00   1.00    2.50    --  111.00  45.00 150.00   37
 13  \w    116.00 173.00   1.00    2.50    --  111.00  77.00  30.00   57
 14  \w     45.00 110.00   1.00    2.50    --  111.00 -45.00  90.00   65
 15  \w     54.00  92.00   1.00    2.50    --  111.00-125.00 -90.00   38
 16  \w     61.00  88.00   1.00    2.50    --  111.00 -94.00  90.00   27
 17  \w     46.00 131.00   1.00    2.50    --  111.00 -61.00-120.00   85
 18  \w    106.00 172.00   1.00    2.50    --  111.00  77.00  60.00   66
 19  \w     99.00 126.00   1.00    2.50    --  111.00-143.00  37.58   27
 20  \w     75.00 109.00   1.00    2.50    --  111.00-114.00 -77.85   34
 21  \w     43.00 113.00   1.00    2.50    --  111.00-125.00  60.00   70
 22  \w     31.00 107.00   1.00    2.50    --  111.00 -94.00  60.00   76
 23  \w     86.00 161.00   1.00    2.50    --  111.00  61.00-150.00   75
 24  \w     71.00 109.00   1.00    2.50    --  111.00-110.00-152.53   38
;
_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      -0.1417015000
_diffrn_orient_matrix_UB_12      0.0127969000
_diffrn_orient_matrix_UB_13      0.0427267000
_diffrn_orient_matrix_UB_21      0.0473683000
_diffrn_orient_matrix_UB_22      0.0748851000
_diffrn_orient_matrix_UB_23      0.0309137000
_diffrn_orient_matrix_UB_31      -0.0509625000
_diffrn_orient_matrix_UB_32      0.0554826000
_diffrn_orient_matrix_UB_33      -0.0731188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.455
_diffrn_reflns_theta_min         2.586
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.125
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         11398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+0.3942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8956
_reflns_number_total             11398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           2[1-CN][3-H]-MeCN
_cod_database_code               7709818
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H37 B2 N3'
_diffrn_oxdiff_digest_frames
;
013b036e75225cbddb9c1ca94ce7185dc40135754c9
;
_diffrn_oxdiff_digest_hkl
;
01f86a0e14ddc494ae0a76ee4376793d23144c
;
_reflns_odcompleteness_completeness 99.90
_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 C(H,H,H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N4(H4A)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C19(H19), C20(H20),
 C21(H21), C23(H23), C24(H24), C25(H25), C33(H33), C34(H34), C35(H35), C37(H37),
  C38(H38), C39(H39), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54)
3.c Disordered Me refined as rotating group:
 C60(H60A,H60B,H60C,H60D,H60E,H60F)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              9957
_shelx_hkl_checksum              95803
_olex2_date_sample_data_collection 2020-10-01
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.806