Tuning the Dissociation of the Fe‒PPh2(OR) Bond in Chiral-at-Metal Complexes [CpFe(Prophos)PPh2(OR)]PF6(R = Me, Et,iPr,tBu). The Preparative Trick of N2Bubbling
Brunner, Henri; Kurosawa, Takaki; Muschiol, Manfred; Tsuno, Takashi; Balázs, Gábor; Bodensteiner, Michael; Organometallics 32 (2013) 4904–; doi:10.1021/om400631m

data_4081360
_publ_section_title
;
 Tuning the Dissociation of the Fe--PPh2(OR) Bond in Chiral-at-Metal
 Complexes [CpFe(Prophos)PPh2(OR)]PF6(R = Me, Et,iPr,tBu). The
 Preparative Trick of N2Bubbling
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4904
_journal_paper_doi               10.1021/om400631m
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H44 Fe O P3, C4 H8 O2, F6 P'
_chemical_formula_sum            'C49 H52 F6 Fe O3 P4'
_chemical_formula_weight         982.64
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.386(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.360(4)
_cell_length_b                   18.091(5)
_cell_length_c                   11.767(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.14
_cell_measurement_wavelength     0.71073
_cell_volume                     2307.8(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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17484
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku software'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0000P)^2^+3.6549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                6331
_reflns_number_total             7241
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400631m_si_001.cif
_cod_data_source_block           (RFe,RC)-[CpFe(Prophos)PPh2(OMe)]PF6
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4081360