Copolymerization of Ethylene and Methyl Acrylate by Cationic Palladium Catalysts That Contain Phosphine-Diethyl Phosphonate Ancillary Ligands
Contrella, Nathan D.; Sampson, Jessica R.; Jordan, Richard F.; Organometallics  (2014) 140623145555006–; doi:10.1021/om5004489

data_4083715
_publ_section_title
;
 Copolymerization of Ethylene and Methyl Acrylate by Cationic Palladium
 Catalysts That Contain Phosphine-Diethyl Phosphonate Ancillary Ligands
;
_journal_name_full               Organometallics
_journal_page_first              140623145555006
_journal_paper_doi               10.1021/om5004489
_journal_year                    2014
_chemical_formula_sum            'C18.5 H34 Cl2 O3 P2 Pd'
_chemical_formula_weight         543.69
_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                104.042(7)
_cell_angle_beta                 112.074(6)
_cell_angle_gamma                100.911(7)
_cell_formula_units_Z            4
_cell_length_a                   12.149(5)
_cell_length_b                   13.962(5)
_cell_length_c                   16.151(6)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      1.74
_cell_volume                     2340.0(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22712
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.7991
_exptl_absorpt_correction_T_min  0.7346
_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    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                6099
_reflns_number_total             8341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5004489_si_001.cif
_cod_data_source_block           compound_2c
_cod_original_cell_volume        2340.1(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083715