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_7709819
_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         'C10 H18 B2 P, C14 H19 N2'
_chemical_formula_sum            'C24 H37 B2 N2 P'
_chemical_formula_weight         406.14
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-21
_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                63.869(6)
_cell_angle_beta                 83.717(6)
_cell_angle_gamma                81.570(5)
_cell_formula_units_Z            2
_cell_length_a                   9.2999(6)
_cell_length_b                   11.8087(6)
_cell_length_c                   12.2905(8)
_cell_measurement_reflns_used    5310
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2300
_cell_measurement_theta_min      3.9870
_cell_volume                     1197.16(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.978
_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   -110.00 -18.00   1.00    7.50    --  -38.50 -38.00-180.00   92
  2  \w    -70.00  -8.00   1.00    7.50    --  -38.50 125.00 -30.00   62
  3  \w   -100.00 -18.00   1.00    7.50    --  -38.50 -38.00 -90.00   82
  4  \w     37.00  73.00   1.00    7.50    --   42.89 -99.00 -30.00   36
  5  \w     25.00 110.00   1.00    7.50    --   42.89  57.00 120.00   85
  6  \w     45.00  83.00   1.00    7.50    --   42.89-125.00-180.00   38
  7  \w    121.00 178.00   1.00   38.50    --  111.00  77.00  90.00   57
  8  \w     46.00 124.00   1.00   38.50    --  111.00 -61.00 -30.00   78
  9  \w     56.00 140.00   1.00   38.50    --  111.00 -77.00  90.00   84
 10  \w     32.00  57.00   1.00   38.50    --  111.00 -94.00   0.00   25
 11  \w     77.00 104.00   1.00   38.50    --  111.00 -94.00   0.00   27
 12  \w     42.00  77.00   1.00   38.50    --  111.00-125.00 -90.00   35
 13  \w     96.00 173.00   1.00   38.50    --  111.00  45.00  60.00   77
 14  \w     44.00 119.00   1.00   38.50    --  111.00 -30.00  30.00   75
 15  \w     45.00  76.00   1.00   38.50    --  111.00-125.00-150.00   31
 16  \w     41.00  97.00   1.00   38.50    --  111.00-125.00 -60.00   56
 17  \w     75.00 105.00   1.00   38.50    --  111.00 -94.00  60.00   30
 18  \w     88.00 113.00   1.00   38.50    --  111.00-125.00-150.00   25
 19  \w     32.00 107.00   1.00   38.50    --  111.00 -94.00 -60.00   75
 20  \w     46.00  73.00   1.00   38.50    --  111.00-125.00  60.00   27
 21  \w     32.00  57.00   1.00   38.50    --  111.00 -94.00-150.00   25
 22  \w     82.00 107.00   1.00   38.50    --  111.00 -94.00-150.00   25
 23  \w     82.00 107.00   1.00   38.50    --  111.00 -94.00 -30.00   25
 24  \w     54.00 150.00   1.00   38.50    --  111.00   0.00  60.00   96
;
_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      -0.1388106000
_diffrn_orient_matrix_UB_12      0.0592903000
_diffrn_orient_matrix_UB_13      0.0445077000
_diffrn_orient_matrix_UB_21      -0.0915678000
_diffrn_orient_matrix_UB_22      -0.0297344000
_diffrn_orient_matrix_UB_23      -0.0794236000
_diffrn_orient_matrix_UB_31      -0.0215528000
_diffrn_orient_matrix_UB_32      -0.1302801000
_diffrn_orient_matrix_UB_33      0.1060897000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9697
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.439
_diffrn_reflns_theta_min         4.011
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
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    1.127
_exptl_crystal_description       irregular
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         4917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0454P)^2^+0.2454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4266
_reflns_number_total             4917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[2-PH2][3-H]'
_cod_original_cell_volume        1197.15(14)
_cod_database_code               7709819
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H37 B2 N2 P'
_diffrn_oxdiff_digest_frames
;
014eb6d06750a7643c0367b707ad9f9e83013223745
;
_diffrn_oxdiff_digest_hkl
;
01a0dc651f7f42ea836713f4115c0ba03c1194
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uiso(H1) = Uiso(H2)
2. Others
 Sof(H2)=1-FVAR(1)
 Sof(H1)=FVAR(1)
;
_shelx_res_checksum              13838
_shelx_hkl_checksum              67417
_olex2_date_sample_data_collection 2019-11-20
_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 2.189
_oxdiff_exptl_absorpt_empirical_full_min 0.392