Re(I) Catalysed Isomerisation of Propargylic Alcohols into α,β-Unsaturated Carbonyl Compounds: An Unprecedented Recyclable Catalytic System in Ionic Liquids.
García-Álvarez, Joaquún; Díez, Josefina; Gimeno, José; Seifried, Christine M.; Chem.Commun. 47 (2011) 6470–6472; doi:10.1039/c1cc10768b

data_7106465
_publ_section_title
;
 Re(I) Catalysed Isomerisation of Propargylic Alcohols into
 \a,\b-Unsaturated Carbonyl Compounds: An Unprecedented Recyclable
 Catalytic System in Ionic Liquids.
;
_journal_name_full               Chem.Commun.
_journal_page_first              6470
_journal_page_last               6472
_journal_paper_doi               10.1039/c1cc10768b
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C32 H32 N O5 P3 Re S, F6 Sb'
_chemical_formula_sum            'C32 H32 F6 N O5 P3 Re S Sb'
_chemical_formula_weight         1057.51
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 98.605(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.2549(2)
_cell_length_b                   18.9630(3)
_cell_length_c                   36.8567(8)
_cell_measurement_reflns_used    15261
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7125
_cell_measurement_theta_min      2.1182
_cell_volume                     7777.7(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0827
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device       CCD
_diffrn_measurement_device_type
'Goniometer Xcalibur,detector:Ruby(Gemini Mo)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_sigmaI/netI    0.1924
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            82656
_diffrn_reflns_theta_full        30.75
_diffrn_reflns_theta_max         30.75
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.684
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         21798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.684
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                8859
_reflns_number_total             21798
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cc10768b.txt
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7106465