Efficient and Highly Stereoselective Syntheses of New P-Chiral 1,5-Diphosphanylferrocene Ligands and Their Use in Enantioselective Hydrogenation
Weiping Chen.; Stanley Roberts; John Whittall; Chemical Communications  (2006) –; doi:10.1039/b601952h

data_7101257
_publ_section_title
;
Efficient and Highly Stereoselective Syntheses of New
P-Chiral 1,5-Diphosphanylferrocene Ligands and Their Use in
Enantioselective Hydrogenation
;
_journal_issue                   27
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b601952h
_journal_year                    2006
_chemical_formula_sum            'C32 H31 Fe O3 P'
_chemical_formula_weight         550.39
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.636(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.210(4)
_cell_length_b                   7.142(3)
_cell_length_c                   20.061(8)
_cell_measurement_reflns_used    2144
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      3.17
_cell_volume                     1315.4(9)
_computing_cell_refinement       Bruker-SAINT
_computing_data_collection       Bruker-SMART
_computing_data_reduction        Bruker-SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.1118
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6160
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                2484
_reflns_number_total             3385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601952h.txt
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7101257