Lewis Acid Modification and Ethylene Oligomerization Behavior of Palladium Catalysts That Contain a Phosphine-Sulfonate-Diethyl Phosphonate Ancillary Ligand
Contrella, Nathan D.; Jordan, Richard F.; Organometallics 33 (2014) 7199–; doi:10.1021/om5009988

data_4084944
_publ_section_title
;
 Lewis Acid Modification and Ethylene Oligomerization Behavior of
 Palladium Catalysts That Contain a Phosphine-Sulfonate-Diethyl
 Phosphonate Ancillary Ligand
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7199
_journal_paper_doi               10.1021/om5009988
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C50 H60 Cl2 Mg O12 P4 Pd2 S2'
_chemical_formula_weight         1348.99
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.644(8)
_cell_angle_beta                 75.041(8)
_cell_angle_gamma                71.388(7)
_cell_formula_units_Z            2
_cell_length_a                   11.858(5)
_cell_length_b                   13.105(6)
_cell_length_c                   21.732(10)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      1.64
_cell_volume                     3086(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30789
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.8993
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.830
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                7661
_reflns_number_total             11267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009988_si_002.cif
_cod_data_source_block           SI_((1a)PdMe)2(u-Cl)MgCl
_cod_depositor_comments
'Adding full bibliography for 4084939--4084944.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084944