Stable preformed chiral palladium catalysts for the one-pot asymmetric reductive amination of ketones.
Rubio-Pérez, Laura; Pérez-Flores, F Javier; Sharma, Pankaj; Velasco, Luis; Cabrera, Armando; Organic letters 11 (2009) 265–268; doi:10.1021/ol802336m

data_1503719
_publ_section_title
;
 Stable preformed chiral palladium catalysts for the one-pot asymmetric
 reductive amination of ketones.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              265
_journal_page_last               268
_journal_paper_doi               10.1021/ol802336m
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C44 H32 Br2 P2 Pd'
_chemical_formula_sum            'C44 H32 Br2 P2 Pd'
_chemical_formula_weight         888.86
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                   11.9124(3)
_cell_length_b                   11.9124(3)
_cell_length_c                   26.1910(13)
_cell_measurement_reflns_used    6233
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.72
_cell_measurement_theta_min      2.31
_cell_volume                     3716.6(2)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23A (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX AXS CCD area detector'
_diffrn_measurement_method       '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  0.0947
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30513
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  0.6659
_exptl_absorpt_correction_T_min  0.3895
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXTL V 6.12 (Sheldrick, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 1318 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                2781
_reflns_number_total             3272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol802336m_si_003.cif
_cod_data_source_block           100coa05
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'No' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1503719
_solved_by                       'Simon Hernandez-Ortega'