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_4084941
_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            'C37 H47 Cl6 N O6 P2 Pd S'
_chemical_formula_weight         1014.86
_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                76.281(7)
_cell_angle_beta                 83.507(7)
_cell_angle_gamma                84.045(8)
_cell_formula_units_Z            2
_cell_length_a                   9.123(4)
_cell_length_b                   12.185(6)
_cell_length_c                   20.514(10)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.61
_cell_measurement_theta_min      1.73
_cell_volume                     2194.1(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1235
_diffrn_reflns_av_sigmaI/netI    0.2418
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18361
_diffrn_reflns_theta_full        23.61
_diffrn_reflns_theta_max         23.61
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.778
_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    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.759
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.759
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                2785
_reflns_number_total             6491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009988_si_002.cif
_cod_data_source_block           Compound_2c
_cod_depositor_comments
'Adding full bibliography for 4084939--4084944.cif.'
_cod_original_cell_volume        2194.1(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084941