Dual Role of Doubly Reduced Arylboranes as Dihydrogen- and Hydride-Transfer Catalysts.
von Grotthuss, Esther; Prey, Sven E.; Bolte, Michael; Lerner, Hans-Wolfram; Wagner, Matthias; Journal of the American Chemical Society 141 (2019) 6082–6091; doi:10.1021/jacs.9b01998

data_4128424
_publ_section_title
;
 Dual Role of Doubly Reduced Arylboranes as Dihydrogen- and
 Hydride-Transfer Catalysts.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6082
_journal_page_last               6091
_journal_paper_doi               10.1021/jacs.9b01998
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C36 H58 B2 Li2 O9'
_chemical_formula_sum            'C36 H58 B2 Li2 O9'
_chemical_formula_weight         670.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 102.873(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3173(13)
_cell_length_b                   12.8231(8)
_cell_length_c                   20.9241(18)
_cell_measurement_reflns_used    15847
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      3.29
_cell_volume                     3744.9(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29657
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.719
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 2440 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         12967
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                8412
_reflns_number_total             12967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01998_si_002.cif
_cod_data_source_block           wa2589
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4128424
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              97722
_shelx_hkl_checksum              65002