Novel C~2~-Symmetric Planar Chiral Diphosphine Ligands and Their Application in Pd-Catalyzed Asymmetric Allylic Substitutions
Delong Liu; Fang Xie; Wanbin Zhang; Journal of Organic Chemistry 72 (2007) 6992–6997; doi:10.1021/jo0711440

data_4024145
_publ_section_title
;
 Novel C~2~-Symmetric Planar Chiral Diphosphine Ligands and
 Their Application in Pd-Catalyzed Asymmetric Allylic Substitutions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6992
_journal_page_last               6997
_journal_paper_doi               10.1021/jo0711440
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C39 H34 Cl4 Fe O4 P2 Pd'
_chemical_formula_weight         932.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_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                   10.5308(5)
_cell_length_b                   10.5308(5)
_cell_length_c                   35.165(2)
_cell_measurement_reflns_used    5619
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.029
_cell_measurement_theta_min      4.509
_cell_volume                     3899.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1162
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            23692
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79488
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.339
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8266
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                6276
_reflns_number_total             8266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0711440-File005.cif
_cod_data_source_block           cd26426
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4024145