Synthesis, Structures, and Ethylene Dimerization Reactivity of Palladium Alkyl Complexes That Contain a Chelating Phosphine–Trifluoroborate Ligand
Kim, Youngmin; Jordan, Richard F.; Organometallics 30 (2011) 4250–; doi:10.1021/om200472x

data_4063560
_publ_section_title
;
 Synthesis, Structures, and Ethylene Dimerization Reactivity of Palladium
 Alkyl Complexes That Contain a Chelating Phosphine--Trifluoroborate
 Ligand
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4250
_journal_paper_doi               10.1021/om200472x
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C35 H49 B Cl F3 K O7 P Pd'
_chemical_formula_weight         861.47
_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                88.880(4)
_cell_angle_beta                 88.417(4)
_cell_angle_gamma                80.507(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6347(18)
_cell_length_b                   10.183(2)
_cell_length_c                   21.685(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.88
_cell_volume                     1879.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22706
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.7668
_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    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.456
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.648
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.6723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                7602
_reflns_number_total             8997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200472x_si_002.cif
_cod_data_source_block           cpd3
_cod_depositor_comments
;

2021-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C70 H98 B2 Cl2 F6 K2 O14 P2 Pd2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1722.94
_cod_database_code               4063560