Diastereoselective Proton Transfer: A Route to Enantiomerically Pure Half-Sandwich Rhenium Complexes
Frank Bock; Frank Fischer; Wolfdieter A. Schenk; Journal of the American Chemical Society 128 (2006) 68–69; doi:10.1021/ja057089z

data_4110351
_publ_contact_author
; 
             Prof. Dr. Wolfdieter A. Schenk
             Institut f\"ur Anorganische Chemie
             Universit\"at W\"urzburg
             Am Hubland
             D-97074 W\"urzburg
             Germany
;
_publ_contact_author_email       wolfdieter.schenk@mail.uni-wuerzburg.de
_publ_contact_author_fax         '+49 931 8884605'
_publ_contact_author_phone       '+49 931 8885259'
_publ_section_title
;
 Diastereoselective Proton Transfer: A Route to Enantiomerically Pure
 Half-Sandwich Rhenium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              68
_journal_page_last               69
_journal_paper_doi               10.1021/ja057089z
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C21 H26 N2 O4 P Re S'
_chemical_formula_weight         619.67
_chemical_name_common            unlike-[CpRe(NO){P(Me)(Ph)(C6H4o-NMe2)}]O3SMe
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.908(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1512(7)
_cell_length_b                   13.6587(11)
_cell_length_c                   14.6425(7)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      6.6
_cell_volume                     2209.0(3)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Stoe-IPDS
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.1048
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14054
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    5.698
_exptl_absorpt_correction_T_max  0.32145
_exptl_absorpt_correction_T_min  0.31395
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.1000
_refine_diff_density_max         1.189
_refine_diff_density_min         -2.600
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.0733
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2793
_reflns_number_total             4507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057089zsi20051121_112233.cif
_cod_data_source_block           bocrhe2l1
_cod_original_cell_volume        2209.0(2)
_cod_database_code               4110351