Dinuclear Allylpalladium Complexes ofC2-Symmetric Pyrazolate-Bridged Bis(oxazoline) Ligands (pyrbox's): Structures, Dynamic Behavior, and Application in Asymmetric Allylic Alkylation
Ficks, Arne; Sibbald, Connor; John, Michael; Dechert, Sebastian; Meyer, Franc; Organometallics 29 (2010) 1117–; doi:10.1021/om900835f

data_4067311
_publ_section_title
;
 Dinuclear Allylpalladium Complexes ofC2-Symmetric Pyrazolate-Bridged
 Bis(oxazoline) Ligands (pyrbox's): Structures, Dynamic Behavior, and
 Application in Asymmetric Allylic Alkylation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1117
_journal_paper_doi               10.1021/om900835f
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H31 N4 O2 Pd2 +, B F4 -'
_chemical_formula_sum            'C29 H31 B F4 N4 O2 Pd2'
_chemical_formula_weight         767.19
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.5487(4)
_cell_length_b                   13.5487(4)
_cell_length_c                   27.8944(10)
_cell_measurement_reflns_used    38453
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.74
_cell_volume                     4434.5(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38453
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.7586
_exptl_absorpt_correction_T_min  0.5979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.487
_refine_diff_density_min         -2.309
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+38.5766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                5283
_reflns_number_total             5482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900835f_si_002.cif
_cod_data_source_block           af2
_cod_original_sg_symbol_H-M      'P 6(1)'
_cod_database_code               4067311