Ferrocenyl Diphosphines Containing Stereogenic Phosphorus Atoms. Synthesis and Application in the Rhodium-Catalyzed Asymmetric Hydrogenation
Maienza, Francesca; Wörle, Michael; Steffanut, Pascal; Mezzetti, Antonio; Spindler, Felix; Organometallics 18 (1999) 1041–; doi:10.1021/om980754a

data_4077738
_publ_section_title
;
 Ferrocenyl Diphosphines Containing Stereogenic Phosphorus Atoms.
 Synthesis and Application in the Rhodium-Catalyzed Asymmetric
 Hydrogenation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1041
_journal_paper_doi               10.1021/om980754a
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C36 H38 B2 Fe O2 P2'
_chemical_name_common
'(S,S)-1,1'-Bis(2-methoxyphenyl(phenyl)- phosphino)ferrocene borane''
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                93.309(13)
_cell_angle_beta                 105.005(12)
_cell_angle_gamma                108.641(12)
_cell_formula_units_Z            1
_cell_length_a                   7.8770(10)
_cell_length_b                   8.7930(10)
_cell_length_c                   13.087(2)
_cell_measurement_temperature    298(2)
_cell_volume                     819.8(2)
_computing_cell_refinement       'STOE program package'
_computing_data_collection       'STOE program package'
_computing_data_reduction        'STOE program package'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'STOE IPDS (image plate detector system) '
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9431
_diffrn_reflns_theta_max         24.22
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.8806
_exptl_absorpt_correction_T_min  0.8682
_exptl_absorpt_correction_type   'empirical (DECAY)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(17)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         4872
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0372
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+0.5119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0920
_refine_ls_wR_factor_obs         0.0863
_reflns_number_observed          4463
_reflns_number_total             4872
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980754a.cif
_cod_data_source_block
(S,S)-1,1'-Bis(2-methoxyphenyl(phenyl)phosphino)ferrocene_borane_(S,S-2a)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+0.5119P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+0.5119P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        819.77(19)
_cod_database_code               4077738
_chemical_formula_weightical     642.07