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_7709814
_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 H20 B2 P, C14 H19 N2'
_chemical_formula_sum            'C28 H39 B2 N2 P'
_chemical_formula_weight         456.20
_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     dual
_audit_creation_date             2018-06-08
_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                90.861(3)
_cell_angle_beta                 107.767(4)
_cell_angle_gamma                91.957(4)
_cell_formula_units_Z            4
_cell_length_a                   12.1822(5)
_cell_length_b                   13.9482(7)
_cell_length_c                   16.4722(6)
_cell_measurement_reflns_used    6908
_cell_measurement_temperature    99.97(15)
_cell_measurement_theta_max      72.2470
_cell_measurement_theta_min      5.3890
_cell_volume                     2663.0(2)
_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      99.97(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.9315
_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   -115.00  -5.00   1.00    5.50    --  -38.50 -19.00 150.00  110
  2  \w    -58.00  33.00   1.00    5.50    --  -38.50  38.00 -30.00   91
  3  \w    -62.00  30.00   1.00    5.50    --  -38.50  57.00-180.00   92
  4  \w     19.00  46.00   1.00    5.50    --   43.45  57.00   0.00   27
  5  \w     58.00  85.00   1.00    5.50    --   43.45  57.00-120.00   27
  6  \w     13.00 115.00   1.00    5.50    --   43.45  77.00  30.00  102
  7  \w      1.00  80.00   1.00    5.50    --   43.45 -99.00 -90.00   79
  8  \w     13.00  62.00   1.00    5.50    --   43.45  77.00   0.00   49
  9  \w     13.00  66.00   1.00    5.50    --   43.45  77.00 120.00   53
 10  \w      2.00  65.00   1.00    5.50    --   43.45 -99.00  60.00   63
 11  \w     64.00  92.00   1.00    5.50    --   43.45  57.00   0.00   28
 12  \w     20.00  79.00   1.00    5.50    --   43.45  77.00  60.00   59
 13  \w     23.00  62.00   1.00    5.50    --   43.45  38.00   0.00   39
 14  \w     15.00  68.00   1.00    5.50    --   43.45  77.00-180.00   53
 15  \w     21.00  48.00   1.00    5.50    --   43.45  57.00-120.00   27
 16  \w     13.00 115.00   1.00    5.50    --   43.45  77.00 -90.00  102
 17  \w     81.00 107.00   1.00   33.00    --  111.00  77.00-150.00   26
 18  \w     85.00 120.00   1.00   33.00    --  111.00  61.00-180.00   35
 19  \w     82.00 108.00   1.00   33.00    --  111.00  71.00 157.77   26
 20  \w     41.00 118.00   1.00   33.00    --  111.00-125.00 -90.00   77
 21  \w     85.00 111.00   1.00   33.00    --  111.00  61.00 -60.00   26
 22  \w    115.00 141.00   1.00   33.00    --  111.00 -77.00 150.00   26
 23  \w     83.00 118.00   1.00   33.00    --  111.00  68.00-132.98   35
 24  \w     85.00 112.00   1.00   33.00    --  111.00  61.00  90.00   27
 25  \w     81.00 107.00   1.00   33.00    --  111.00  76.00-100.93   26
 26  \w     85.00 173.00   1.00   33.00    --  111.00  61.00-150.00   88
 27  \w     31.00 109.00   1.00   33.00    --  111.00 -94.00   0.00   78
 28  \w     85.00 163.00   1.00   33.00    --  111.00  61.00  60.00   78
 29  \w     40.00  98.00   1.00   33.00    --  111.00 -77.00 150.00   58
 30  \w     81.00 108.00   1.00   33.00    --  111.00  77.00   0.00   27
 31  \w     81.00 123.00   1.00   33.00    --  111.00  77.00 -30.00   42
;
_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      -0.0485590000
_diffrn_orient_matrix_UB_12      0.0866513000
_diffrn_orient_matrix_UB_13      0.0347582000
_diffrn_orient_matrix_UB_21      -0.0888415000
_diffrn_orient_matrix_UB_22      0.0114671000
_diffrn_orient_matrix_UB_23      -0.0883767000
_diffrn_orient_matrix_UB_31      -0.0860974000
_diffrn_orient_matrix_UB_32      -0.0676660000
_diffrn_orient_matrix_UB_33      0.0252303000
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36514
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.776
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_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    1.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             984.0
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         14775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0774P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11658
_reflns_number_total             14775
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9671\% 
 around [-0.00 1.00 0.00] (reciprocal) or [0.05 1.00 0.02] (direct)
;
_cod_data_source_file            d2dt00585a2.cif
_cod_data_source_block           '[1-PH2][3-H]'
_cod_original_cell_volume        2662.9(2)
_cod_database_code               7709814
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C28 H39 B2 N2 P'
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.852
_diffrn_oxdiff_ac3_digest_frames
;
01d46385dc5dd0899cea02fd2abdfdb0a700027dcb0
;
_diffrn_oxdiff_ac3_digest_hkl
;
0161c08c684b81f06de33346ca40b28f3f9216
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5177(7)
 0.4823(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C22(H22), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
  C36(H36), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              50129
_shelx_hkl_checksum              14613
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.776
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2