Air-Stable Pd(R-allyl)LCl (L= Q-Phos, P(t-Bu)3, etc.) Systems for C-C/N Couplings: Insight into the Structure-Activity Relationship and Catalyst Activation Pathway
Carin C. C. Johansson Seechurn; Sébastien L. Parisel; Thomas J. Colacot; Journal of Organic Chemistry 76 (2011) 7918–7932; doi:10.1021/jo2013324

data_4026623
_publ_section_title
;
 Air-Stable Pd(R-allyl)LCl (L= Q-Phos, P(t-Bu)3, etc.) Systems for C-C/N
 Couplings: Insight into the Structure-Activity Relationship and Catalyst
 Activation Pathway
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7918
_journal_page_last               7932
_journal_paper_doi               10.1021/jo2013324
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C35 H61 Br N2 P2 Pd2, 0.5(C6 H14), C H2 Cl2'
_chemical_formula_sum            'C39 H70 Br Cl2 N2 P2 Pd2'
_chemical_formula_weight         992.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.785(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0675(2)
_cell_length_b                   21.9913(5)
_cell_length_c                   18.8256(4)
_cell_measurement_reflns_used    53461
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     4386.73(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24554
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.954
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.064
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         10054
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.610
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                6184
_reflns_number_total             10054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2013324_si_007.cif
_cod_data_source_block           jm1011
_cod_original_cell_volume        4386.72(16)
_cod_database_code               4026623