Biferrocene-Based Diphosphine Ligands: Synthesis and Application of Walphos Analogues in Asymmetric Hydrogenations
Zirakzadeh, Afrooz; Groß, Manuela A.; Wang, Yaping; Mereiter, Kurt; Spindler, Felix; Weissensteiner, Walter; Organometallics 32 (2013) 1075–; doi:10.1021/om3012147

data_4080089
_publ_section_title
;
 Biferrocene-Based Diphosphine Ligands: Synthesis and Application of
 Walphos Analogues in Asymmetric Hydrogenations
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1075
_journal_paper_doi               10.1021/om3012147
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H40 Cl2 Fe2 P2 Pd, C7 H8, 0.5(H2 O)'
_chemical_formula_sum            'C53 H49 Cl2 Fe2 O0.5 P2 Pd'
_chemical_formula_weight         1044.86
_chemical_name_common            '1595 ww magr114 [PdCl2(12)].C7H8.1/2(H2O)'
_chemical_name_systematic
; 
Dichloro-{(S~Fc~)-2-[(R)-1-diphenylphosphinoethyl-\kP]-
(R~Fc~)-2''-diphenylphosphino-?P-1,1''-biferrocene} palladium(II)
toluene monosolvate hemihydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.367(2)
_cell_angle_beta                 90.523(2)
_cell_angle_gamma                104.076(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2688(4)
_cell_length_b                   14.6804(5)
_cell_length_c                   15.1107(4)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.47
_cell_volume                     2276.47(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80353
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         24452
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.8399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                23710
_reflns_number_total             24452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3012147_si_001.cif
_cod_data_source_block           Pd15=1595
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C53 H49 Cl2 Fe2 O0.50 P2 Pd'
_cod_database_code               4080089