Efficient Lewis Acid Promoted Alkene Hydrogenations Using Dinitrosyl Rhenium(−I) Hydride Catalysts
Jiang, Yanfeng; Huang, Wenjing; Schmalle, Helmut W.; Blacque, Olivier; Fox, Thomas; Berke, Heinz; Organometallics 32 (2013) 7043–; doi:10.1021/om400733u

data_4081878
_publ_section_title
;
 Efficient Lewis Acid Promoted Alkene Hydrogenations Using Dinitrosyl
 Rhenium(&#x2212;I) Hydride Catalysts
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7043
_journal_paper_doi               10.1021/om400733u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C36 H43 B F15 N2 O2 P2 Re, 2(C7 H8)'
_chemical_formula_sum            'C50 H59 B F15 N2 O2 P2 Re'
_chemical_formula_weight         1263.94
_chemical_name_systematic
'Hydrido{nitroso[tris(perfluorophenyl)borane-\k<i>N</i>]}{bis[tris(1-methylethyl)phopshane]rhenium ditoluene solvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.361(12)
_cell_angle_beta                 90.335(12)
_cell_angle_gamma                113.642(11)
_cell_formula_units_Z            2
_cell_length_a                   12.3134(12)
_cell_length_b                   14.7301(14)
_cell_length_c                   15.8643(16)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      2.80
_cell_volume                     2634.8(5)
_computing_cell_refinement       IPDS
_computing_data_collection
' IPDS [Stoe & Cie (1999). IPDS. Stoe & Cie, Darmstadt, Germany] '
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    ' see manuscript'
_computing_publication_material
; publCIF [Westrip, S. P. (2010). <i>J. Appl. Cryst.</i> <b>43</b>, 920--925],
 WinGX [Farrugia, L. J. (1999). <i>J. Appl. Cryst.</i> <b>32</b>, 837--838]
;
_computing_structure_refinement  'SHELXL-97 [Sheldrick, 2008]'
_computing_structure_solution
' SHELXS-97 [Sheldrick, G. M. (2008). <i>Acta Cryst.</i> A<b>64</b>, 112--122]'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f rotation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47075
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965). <i>Acta Cryst.</i>
<b>18</b>, 1035--1038).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.652
_refine_diff_density_min         -4.166
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.0048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         14370
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.4838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                12103
_reflns_number_total             14370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400733u_si_002.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2634.8(4)
_cod_database_code               4081878