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_4110350
_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_absolute_configuration rmad
_chemical_formula_moiety         'C21 H26 N2 O P Re'
_chemical_formula_sum            'C21 H26 N2 O P Re'
_chemical_formula_weight         539.61
_chemical_name_common
Cp-methyl-nitrosyl-(methyl-phenyl-(o-dimethylaminophenyl)phosphine)rhenium
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.582(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.060(2)
_cell_length_b                   15.729(5)
_cell_length_c                   8.241(3)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.048
_cell_measurement_theta_min      2.5785
_cell_volume                     1001.3(5)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.0'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16220
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    6.160
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.417234
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.257
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0394P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                3742
_reflns_number_total             3909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057089zsi20051121_112211.cif
_cod_data_source_block           09fabol
_cod_database_code               4110350