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_4083717
_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            'C30 H34 F6 N O3 P2 Pd Sb'
_chemical_formula_weight         860.67
_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                90.576(8)
_cell_angle_beta                 98.520(8)
_cell_angle_gamma                94.955(8)
_cell_formula_units_Z            2
_cell_length_a                   9.912(4)
_cell_length_b                   11.513(5)
_cell_length_c                   14.292(6)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      1.78
_cell_volume                     1606.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14870
_diffrn_reflns_theta_full        28.55
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.7875
_exptl_absorpt_correction_T_min  0.5454
_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    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                5323
_reflns_number_total             7648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5004489_si_001.cif
_cod_data_source_block           compound_3a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083717