Diastereomer Ratio of Products as a Mechanistic Probe in Epimerization and Ligand Exchange of Chiral-at-Metal [CpFe(Prophos)NCMe]X (X = I, PF6)
Brunner, Henri; Ike, Hayato; Muschiol, Manfred; Tsuno, Takashi; Koyama, Kazuhiro; Kurosawa, Takaki; Zabel, Manfred; Organometallics 30 (2011) 3666–; doi:10.1021/om2003893

data_4064881
_publ_section_title
;
 Diastereomer Ratio of Products as a Mechanistic Probe in Epimerization
 and Ligand Exchange of Chiral-at-Metal [CpFe(Prophos)NCMe]X (X = I, PF6)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3666
_journal_paper_doi               10.1021/om2003893
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H40 Fe O3 P3, P F6'
_chemical_formula_sum            'C35 H40 F6 Fe O3 P4'
_chemical_formula_weight         802.4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_beta                 116.418(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.169(4)
_cell_length_b                   16.952(5)
_cell_length_c                   11.648(4)
_cell_measurement_reflns_used    12858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.95
_cell_measurement_theta_min      6.19
_cell_measurement_wavelength     0.71073
_cell_volume                     1798.3(11)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF08 (Beurskens et al, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAPID-RAXIS'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17651
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.8733
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7877
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.7254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.126
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                5362
_reflns_number_total             7877
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2003893_si_002.cif
_cod_data_source_block           (SFe,RC)[CpFe(Prophos)P(OMe)3]PF6
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4064881