Rhenium in Homogeneous Catalysis: [ReBrH(NO)(labile ligand)(large-bite-angle diphosphine)] Complexes as Highly Active Catalysts in Olefin Hydrogenations
Balz Dudle; Kunjanpillai Rajesh; Olivier Blacque; Heinz Berke; Journal of the American Chemical Society 133 (2011) 8168–8178; doi:10.1021/ja107245k

data_4106158
_publ_contact_author             'Dr. Blacque, Olivier'
_publ_contact_author_email       oblacque@aci.uzh.ch
_publ_contact_author_fax         '+41 44 63 54 681'
_publ_contact_author_phone       '+41 44 63 54 651'
_publ_section_title
;
 Rhenium in Homogeneous Catalysis: [ReBrH(NO)(labile
 ligand)(large-bite-angle diphosphine)] Complexes as Highly Active
 Catalysts in Olefin Hydrogenations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8168
_journal_page_last               8178
_journal_paper_doi               10.1021/ja107245k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
' 4 (C76 H64 Br2 D2 N2 O4 P4 Re2 Si2), C6 H6, 8(C H2 Cl2)'
_chemical_formula_sum            'C318 H278 Br8 Cl16 D8 N8 O16 P16 Re8 Si8'
_chemical_formula_weight         7891.89
_chemical_name_systematic
;
Bis[(\m~2~-deuterido)-bromo-(9,9-dimethyl-4,5-bis(diphenylphosphino)-9-\
silaxanthene-P,P')-nitrosyl-rhenium(I)] benzene dichloromethane solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90.00
_cell_angle_beta                 123.840(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   50.5101(15)
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_cell_measurement_reflns_used    23268
_cell_measurement_temperature    183(2)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 2.01.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- An integrated system of Windows programs for the solution,
 refinment and analysis of single crystal X-ray diffraction data,
 Version 1.80.00.
 Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97. Program for crystal structure refinement.
 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows, Version 1.12.
 Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            69440
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.46
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_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.329
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;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.557
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_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.120
_refine_diff_density_min         -2.113
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         17216
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0887P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                10330
_reflns_number_total             17216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107245k_si_002_1.cif
_cod_data_source_block           9e
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4106158