Effect of 2-Substituents on Allyl-Supported Precatalysts for the Suzuki‒Miyaura Reaction: Relating Catalytic Efficiency to the Stability of Palladium(I) Bridging Allyl Dimers
Hruszkewycz, Damian P.; Guard, Louise M.; Balcells, David; Feldman, Nicola; Hazari, Nilay; Tilset, Mats; Organometallics 34 (2015) 381–; doi:10.1021/om501250y

data_4085320
_publ_section_title
;
 Effect of 2-Substituents on Allyl-Supported Precatalysts for the
 Suzuki--Miyaura Reaction: Relating Catalytic Efficiency to the Stability
 of Palladium(I) Bridging Allyl Dimers
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              381
_journal_paper_doi               10.1021/om501250y
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C66 H97 Cl N4 Pd2'
_chemical_formula_weight         1194.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.506(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.273(8)
_cell_length_b                   12.2611(3)
_cell_length_c                   40.243(3)
_cell_measurement_reflns_used    74150
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      3.0
_cell_volume                     6477(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            251076
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.8572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         19743
_refine_ls_number_restraints     788
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+4.4411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                18287
_reflns_number_total             19743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501250y_si_002.cif
_cod_data_source_block           '_II-tBu'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4085320