16- and 17-Electron Intermediates in the MeCN/RNC Exchange in Chiral-at-Metal [CpFe(Prophos)NCMe]X (X = I, PF6)
Brunner, Henri; Kurosawa, Takaki; Muschiol, Manfred; Tsuno, Takashi; Ike, Hayato; Organometallics 31 (2012) 3395–; doi:10.1021/om3001789

data_4078171
_publ_section_title
;
 16- and 17-Electron Intermediates in the MeCN/RNC Exchange in
 Chiral-at-Metal [CpFe(Prophos)NCMe]X (X = I, PF6)
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3395
_journal_paper_doi               10.1021/om3001789
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C39 H42 Fe N P2, F6 P'
_chemical_formula_sum            'C39 H42 F6 Fe N P3'
_chemical_formula_weight         787.5
_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                 110.235(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.010(4)
_cell_length_b                   17.660(6)
_cell_length_c                   10.919(4)
_cell_measurement_reflns_used    17103
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_measurement_wavelength     0.71073
_cell_volume                     1811.1(12)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.046
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17530
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.61
_exptl_absorpt_correction_T_max  0.7667
_exptl_absorpt_correction_T_min  0.7303
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7840
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1.4410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.091
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                7381
_reflns_number_total             7840
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3001789_si_003.cif
_cod_data_source_block           (SFe,RC)[CpFe(ProphosCNCy]PF6
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4078171