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_4083389
_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, B 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                 93.63(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.138(6)
_cell_length_b                   12.326(4)
_cell_length_c                   15.347(9)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    200
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1347.6(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.056
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27853
_diffrn_reflns_theta_full        29.407
_diffrn_reflns_theta_max         30.007
_diffrn_reflns_theta_min         2.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.002
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.64
_refine_diff_density_min         -1.54
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0741
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7539
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.0043899
_refine_ls_shift/su_mean         1.0649201
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 13.5 12.3 3.20 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0968
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0968
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5373
_reflns_number_total             7545
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0784
_oxford_refine_ls_scale          0.3819(3)
_oxford_reflns_number_all        7539
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om100564v_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C10 H7 B1 Br1 F4 Mn1 O4'
_cod_database_code               4083389