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_4085317
_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            'C34 H49 Cl N2 Pd'
_chemical_formula_weight         627.60
_chemical_name_systematic
; 
 ? 
;
_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                 97.590(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6038(2)
_cell_length_b                   19.1648(4)
_cell_length_c                   17.7314(13)
_cell_measurement_reflns_used    81013
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      3.0
_cell_volume                     3235.0(3)
_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 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96160
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7968
_exptl_absorpt_correction_T_min  0.7726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9803
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+2.1267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                9317
_reflns_number_total             9803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501250y_si_002.cif
_cod_data_source_block           '_I-tBu'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4085317