Kinetic Resolution of Planar-Chiral (η5-Bromocyclopentadienyl)manganese(I) Complexes by Molybdenum-Catalyzed Asymmetric Ring-Closing Metathesis
Ogasawara, Masamichi; Tseng, Ya-Yi; Liu, Qiang; Chang, Ninghui; Yang, Xicheng; Takahashi, Tamotsu; Kamikawa, Ken; Organometallics 36 (2017) 1430–; doi:10.1021/acs.organomet.7b00125

data_4087327
_publ_section_title
;
 Kinetic Resolution of Planar-Chiral
 (\h5-Bromocyclopentadienyl)manganese(I) Complexes by Molybdenum-Catalyzed
 Asymmetric Ring-Closing Metathesis
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1430
_journal_paper_doi               10.1021/acs.organomet.7b00125
_journal_volume                  36
_journal_year                    2017
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C23 H19 Br Mn O2 P'
_chemical_formula_sum            'C23 H19 Br Mn O2 P'
_chemical_formula_weight         493.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.417(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            6
_cell_length_a                   14.2787(7)
_cell_length_b                   10.5264(5)
_cell_length_c                   21.8552(10)
_cell_measurement_reflns_used    26336
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.08
_cell_volume                     3166.7(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1.1'
_computing_publication_material  'CrystalStructure 4.1.1 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29478
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_min         3.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_T_max  0.456
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6382 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     757
_refine_ls_number_reflns         13982
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0211P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                11709
_reflns_number_total             13982
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om7b00125_si_002.cif
_cod_data_source_block           Br-Cp-Mn
_cod_database_code               4087327
_shelx_res_checksum              11041
_shelx_hkl_checksum              98801