Catalytic Dehydrogenation of (Di)Amine-Boranes with a Geometrically Constrained Phosphine-Borane Lewis Pair
Boudjelel, Maxime; Sosa Carrizo, E. Daiann; Mallet−Ladeira, Sonia; Massou, Stéphane; Miqueu, Karinne; Bouhadir, Ghenwa; Bourissou, Didier; ACS Catalysis 8 (2018) 4459–; doi:10.1021/acscatal.8b00152

data_4515588
_publ_section_title
;
 Catalytic Dehydrogenation of (Di)Amine-Boranes with a Geometrically
 Constrained Phosphine-Borane Lewis Pair
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4459
_journal_paper_doi               10.1021/acscatal.8b00152
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C28 H24 B F12 P'
_chemical_formula_sum            'C28 H24 B F12 P'
_chemical_formula_weight         630.25
_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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                101.690(3)
_cell_angle_beta                 106.173(2)
_cell_angle_gamma                109.985(2)
_cell_formula_units_Z            4
_cell_length_a                   13.4140(8)
_cell_length_b                   13.7860(8)
_cell_length_c                   18.1493(10)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      3.17
_cell_volume                     2859.7(3)
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47076
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         4.095
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+1.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10160
_reflns_number_total             13643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00152_si_002.cif
_cod_data_source_block           2
_cod_database_code               4515588
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2014-3
_shelx_res_checksum              11447
_shelx_hkl_checksum              95733