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_7709822
_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 Se, C14 H19 N2'
_chemical_formula_sum            'C28 H38 B2 N2 Se'
_chemical_formula_weight         503.18
_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             2018-11-06
_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                 107.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.84533(19)
_cell_length_b                   24.1693(4)
_cell_length_c                   11.8937(2)
_cell_measurement_reflns_used    6503
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2170
_cell_measurement_theta_min      1.9870
_cell_volume                     2692.74(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_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    -93.00   5.00   1.00   17.50    --  -23.50 -77.00 -60.00   98
  2  \w      6.00  93.00   1.00   17.50    --   24.87  57.00  60.00   87
  3  \w      6.00  93.00   1.00   17.50    --   24.87  57.00 -30.00   87
  4  \w      6.00  93.00   1.00   17.50    --   24.87  57.00 150.00   87
  5  \w     35.00  99.00   1.00   17.50    --   24.87 178.00-150.00   64
  6  \w    -44.00  43.00   1.00   17.50    --   24.87 -57.00-180.00   87
  7  \w    -47.00  63.00   1.00   17.50    --   24.87 -19.00 -30.00  110
  8  \w    -44.00  43.00   1.00   17.50    --   24.87 -57.00 -90.00   87
  9  \w     -4.00  94.00   1.00   17.50    --   24.87  77.00-150.00   98
 10  \w     12.00  91.00   1.00   17.50    --   24.87-143.00  80.66   79
 11  \w     -1.00  78.00   1.00   17.50    --   24.87-122.00-145.18   79
 12  \w    -95.00  48.00   1.00   17.50    --  -23.50   0.00-180.00  143
 13  \w    -92.00  -5.00   1.00   17.50    --  -23.50 -57.00  60.00   87
 14  \w    -85.00  -8.00   1.00   17.50    --  -23.50 135.00 171.51   77
 15  \w    -95.00  48.00   1.00   17.50    --  -23.50   0.00-150.00  143
 16  \w    -93.00   5.00   1.00   17.50    --  -23.50 -77.00  60.00   98
 17  \w    -84.00  -8.00   1.00   17.50    --  -23.50 134.00 -85.77   76
 18  \w      6.00  83.00   1.00   17.50    --   24.87-130.00 152.13   77
 19  \w    -46.00  47.00   1.00   17.50    --   24.87 -38.00-150.00   93
 20  \w      6.00  93.00   1.00   17.50    --   24.87  57.00   0.00   87
 21  \w      3.00  95.00   1.00   17.50    --   24.87  38.00 -60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0103555000
_diffrn_orient_matrix_UB_12      -0.0087894000
_diffrn_orient_matrix_UB_13      -0.0589394000
_diffrn_orient_matrix_UB_21      0.0240008000
_diffrn_orient_matrix_UB_22      -0.0268938000
_diffrn_orient_matrix_UB_23      0.0207024000
_diffrn_orient_matrix_UB_31      -0.0710748000
_diffrn_orient_matrix_UB_32      -0.0078057000
_diffrn_orient_matrix_UB_33      -0.0049819000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            131345
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.314
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.466
_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    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0416P)^2^+1.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7541
_reflns_number_total             9163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[1-SeH][3-H]'
_cod_original_cell_volume        2692.74(10)
_cod_database_code               7709822
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H38 B2 N2 Se'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.623
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Se(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Se1B-H1B
 1.39 with sigma of 0.02
 C12-B1 \\sim C12B-B1 \\sim C11-B1 \\sim C11B-B1 \\sim C13B-B2 \\sim C13-B2
\\sim C14B-B2 \\sim C14-B2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C12B)
Uanis(C12) = Uanis(C11B)
Uanis(C13B) = Uanis(C14)
Uanis(C11) = Uanis(C14B)
4. Others
 Sof(Se1B)=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(Se1)=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:
 Se1B(H1B)
5.b Me refined with riding coordinates:
 C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              22962
_shelx_hkl_checksum              20670
_olex2_date_sample_data_collection 2018-10-10
_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 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.798