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_4085319
_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_moiety         'C63 H81 Pd2 N4 Cl'
_chemical_formula_sum            'C63 H81 Cl N4 Pd2'
_chemical_formula_weight         1142.61
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-27
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.562(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   14.2768(4)
_cell_length_b                   12.3949(3)
_cell_length_c                   17.6537(12)
_cell_measurement_reflns_used    14630
_cell_measurement_temperature    93
_cell_measurement_theta_max      63.66
_cell_measurement_theta_min      2.60
_cell_volume                     3009.5(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type  SATURN
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53850
_diffrn_reflns_theta_full        63.65
_diffrn_reflns_theta_max         63.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.514
_exptl_absorpt_correction_T_max  0.332
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2009)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1192.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.810
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3855 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9052
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.0098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                8593
_reflns_number_total             9052
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om501250y_si_002.cif
_cod_data_source_block           '_II-Ph'
_cod_original_formula_sum        'C63 H81 Pd2 N4 Cl'
_cod_database_code               4085319