t-Bu-QuinoxP* Ligand: Applications in Asymmetric Pd-Catalyzed Allylic Substitution and Ru-Catalyzed Hydrogenation
Tsuneo Imamoto; Miwako Nishimura; Aya Koide; Kazuhiro Yoshida; Journal of Organic Chemistry 72 (2007) 7413–7416; doi:10.1021/jo071192k

data_4024178
_publ_contact_author_address
;Department of Chemistry
Faculty of Science
Chiba University
Yayoi-cho, Inage-ku, Chiba 263-8522
Japan
;
_publ_contact_author_email       imamoto@faculty.chiba-u.jp
_publ_contact_author_fax         +81-43-290-2791
_publ_contact_author_name        'Tsuneo Imamoto'
_publ_contact_author_phone       +81-43-290-2791
_publ_section_title
;
 t-Bu-QuinoxP* Ligand: Applications in Asymmetric Pd-Catalyzed
 Allylic Substitution and Ru-Catalyzed Hydrogenation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7413
_journal_page_last               7416
_journal_paper_doi               10.1021/jo071192k
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety
'C18 H28 Cl2 N2 P2 Pd, C18 H28 Cl2 N2 P2 Pd, C H2 Cl2, C H2 Cl2'
_chemical_formula_sum            'C38 H60 Cl8 N4 P4 Pd2'
_chemical_formula_weight         1193.27
_chemical_name_common            PdCl2(t-Bu-QuinoxP*)
_chemical_name_systematic
;
 [(R,R)-2,3-bis((tert-butyl)methylphosphino)quinoxaline]dichloropalladium
;
_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                90.01
_cell_angle_beta                 99.03
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9747(3)
_cell_length_b                   15.2901(6)
_cell_length_c                   10.4868(4)
_cell_measurement_reflns_used    6630
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.38
_cell_volume                     1262.86(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_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  0.0089
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7078
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.6976
_exptl_absorpt_correction_T_min  0.6324
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         6106
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                6009
_reflns_number_total             6106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo071192k-File001.cif
_cod_data_source_block           yoshida9_p1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4024178