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_4081881
_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         'C38 H72 N2 O2 P2 Re, C24 B F20'
_chemical_formula_sum            'C62 H72 B F20 N2 O2 P2 Re'
_chemical_formula_weight         1516.17
_chemical_name_systematic
'Hydrido(nitrosyl)(nitrosoethane-\k<i>N</i>)[bis(triscyclohexyl)phosphane]rhenium(+) tetra(pentafluorophenyl)borate (-)'
_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                105.373(14)
_cell_angle_beta                 102.731(14)
_cell_angle_gamma                99.150(14)
_cell_formula_units_Z            2
_cell_length_a                   13.4696(17)
_cell_length_b                   14.0584(16)
_cell_length_c                   18.237(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.5
_cell_volume                     3160.0(8)
_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 0.941
_diffrn_measured_fraction_theta_max 0.908
_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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.1142
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50381
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.649
_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    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.261
_refine_diff_density_min         -2.699
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         17314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0335P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                11665
_reflns_number_total             17314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400733u_si_005.cif
_cod_data_source_block           3b
_cod_database_code               4081881