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_4083385
_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         'C21 H25 Mn1 O5'
_chemical_formula_sum            'C21 H25 Mn O5'
_chemical_formula_weight         412.35
_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                 103.796(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.152(2)
_cell_length_b                   27.425(3)
_cell_length_c                   12.8037(19)
_cell_measurement_reflns_used    115
_cell_measurement_temperature    200
_cell_measurement_theta_max      23
_cell_measurement_theta_min      4
_cell_volume                     4144.0(11)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 0.995
_diffrn_measured_fraction_theta_max 0.980
_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  0.040
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            77635
_diffrn_reflns_theta_full        28.205
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_min         1.638
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details 'Flack (1983), 10304 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1117
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         16294
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.046751
_refine_ls_structure_factor_coef F
_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: 
 0.862 0.674E-01 0.542 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0568
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0381
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              38
_reflns_limit_k_min              -38
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                17837
_reflns_number_total             22392
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0349
_oxford_reflns_number_all        22387
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_duplicate_entry             4066671
_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.

'_refine_ls_hydrogen_treatment' value 'refu' changed to
'refU' 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_cell_volume        4144.0(12)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C21 H25 Mn1 O5'
_cod_database_code               4083385