Cationic Planar Chiral (η6-Arene)Mn(CO)3+Complexes: Resolution, NMR Study in Chiral-Oriented Solvents, and Applications to the Enantioselective Synthesis of 4-Substituted Cyclohexenones and (η6-Phosphinoarene)Mn(CO)3+Complexes
Eloi, Antoine; Rose-Munch, Françoise; Rose, Eric; Pille, Ariane; Lesot, Philippe; Herson, Patrick; Organometallics 29 (2010) 3876–; doi:10.1021/om100564v

data_4066670
_publ_section_title
;
 Cationic Planar Chiral (\h6-Arene)Mn(CO)3+Complexes: Resolution, NMR
 Study in Chiral-Oriented Solvents, and Applications to the
 Enantioselective Synthesis of 4-Substituted Cyclohexenones and
 (\h6-Phosphinoarene)Mn(CO)3+Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3876
_journal_paper_doi               10.1021/om100564v
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H7 Br1 Mn1 O4, B1 F4'
_chemical_formula_sum            'C10 H7 B Br F4 Mn O4'
_chemical_formula_weight         412.80
_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
_cell_angle_alpha                90
_cell_angle_beta                 93.477(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1425(8)
_cell_length_b                   12.3410(11)
_cell_length_c                   15.3631(11)
_cell_measurement_reflns_used    154
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      5
_cell_volume                     1351.7(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12596
_diffrn_reflns_theta_full        27.308
_diffrn_reflns_theta_max         30.008
_diffrn_reflns_theta_min         2.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.990
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.98
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.207(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9246
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6738
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.0089078
_refine_ls_shift/su_mean         0.0445233
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.32P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0961
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0961
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5420
_reflns_number_total             6743
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0582
_oxford_reflns_number_all        6738
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om100564v_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C10 H7 B1 Br1 F4 Mn1 O4'
_cod_database_code               4066670