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_4067312
_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         'C23 H35 N4 O2 Pd2 +, F6 P -, 0.75(C4 H10 O)'
_chemical_formula_sum            'C26 H42.5 F6 N4 O2.75 P Pd2'
_chemical_formula_weight         812.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.382(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.2448(10)
_cell_length_b                   8.7037(4)
_cell_length_c                   13.8195(5)
_cell_measurement_reflns_used    13640
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      1.45
_cell_volume                     3369.1(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13640
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.9201
_exptl_absorpt_correction_T_min  0.6937
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.399
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6334
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+11.4809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                5630
_reflns_number_total             6334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900835f_si_002.cif
_cod_data_source_block           af3a
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C26 H42.50 F6 N4 O2.75 P Pd2'
_cod_database_code               4067312