Synthesis and Use in Asymmetric Hydrogenations of Solely Planar Chiral 1,2-Disubstituted and 1,2,3-Trisubstituted Ferrocenyl Diphosphines: A Comparative Study
Wang, Yaping; Weissensteiner, Walter; Spindler, Felix; Arion, Vladimir B.; Mereiter, Kurt; Organometallics 26 (2007) 3530–; doi:10.1021/om700405a

data_4073501
_publ_section_title
;
 Synthesis and Use in Asymmetric Hydrogenations of Solely Planar Chiral
 1,2-Disubstituted and 1,2,3-Trisubstituted Ferrocenyl
 Diphosphines:&#x00A0; A Comparative Study
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3530
_journal_paper_doi               10.1021/om700405a
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety
'C39 H38 Cl2 Fe P2 Pd, 0.5(C H2 Cl2), 0.5(C2 H6 O)'
_chemical_formula_sum            'C40.5 H42 Cl3 Fe O0.5 P2 Pd'
_chemical_formula_weight         867.28
_chemical_name_common
'1152 YW238-1 [PdCl2(9c)].(1/2CH2Cl2+1/2EtOH)'
_chemical_name_systematic
; 
((R~p~)-1-Diphenylphosphino-2-bis-(3,5-dimethylphenyl)phosphinomethyl-
ferrocene)-dichloropalladium(II), solvate with dichloromethane and ethanol 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5451(5)
_cell_length_b                   17.7582(8)
_cell_length_c                   18.3153(8)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.09
_cell_volume                     3755.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52642
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.194
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS, V2.10'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         10927
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+1.8363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                10802
_reflns_number_total             10927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700405a-file002.cif
_cod_data_source_block           PdCl2+9c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C40.50 H42 Cl3 Fe O0.50 P2 Pd'
_cod_database_code               4073501