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_4063561
_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            'C27 H28 B F3 N P Pd'
_chemical_formula_weight         571.68
_chemical_name_systematic
; 
 ? 
;
_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                94.117(6)
_cell_angle_beta                 100.285(6)
_cell_angle_gamma                90.082(7)
_cell_formula_units_Z            2
_cell_length_a                   10.125(4)
_cell_length_b                   10.831(4)
_cell_length_c                   11.555(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.80
_cell_volume                     1243.5(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15028
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.8761
_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    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.838
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0828P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                4492
_reflns_number_total             5977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200472x_si_002.cif
_cod_data_source_block           cpd4
_cod_original_cell_volume        1243.5(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063561