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_4081880
_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         'C24 B F20, C20 H48 N2 O2 P2 Re'
_chemical_formula_sum            'C44 H48 B F20 N2 O2 P2 Re'
_chemical_formula_weight         1275.79
_chemical_name_systematic
'Hydrido(nitrosyl)(nitrosoethane-\k<i>N</i>){bis[tris(1-methyletyl)phosphane]}rhenium(+) tetra(pentafluorophenyl)borate (-)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.623(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.897(2)
_cell_length_b                   12.7097(15)
_cell_length_c                   21.218(2)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.70
_cell_volume                     4993.1(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.951
_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  0.1126
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            65591
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.611
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.444
_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            yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.756
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         14934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.756
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                8159
_reflns_number_total             14934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400733u_si_004.cif
_cod_data_source_block           3a
_cod_original_cell_volume        4993.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081880