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_4084943
_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            'C29 H38 Cl Mg0.5 O6 P2 Pd S'
_chemical_formula_weight         730.60
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.106(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.213(9)
_cell_length_b                   16.984(6)
_cell_length_c                   20.882(7)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.60
_cell_measurement_theta_min      1.57
_cell_volume                     9173(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.1219
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36949
_diffrn_reflns_theta_full        23.60
_diffrn_reflns_theta_max         23.60
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.8669
_exptl_absorpt_correction_T_min  0.7917
_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    1.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                4062
_reflns_number_total             6768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009988_si_002.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 4084939--4084944.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C29 H38 Cl Mg0.50 O6 P2 Pd S'
_cod_database_code               4084943