Ion Pairing and Allyl Dynamics in a Series of [Pd(η3-allyl)(N,N-chelate)](anion) Salts. On the Influence of the BPh4−Anion
Moreno, Aitor; Pregosin, Paul S.; Fuentes, Beatriz; Veiros, Luis F.; Albinati, Alberto; Rizzato, Silvia; Organometallics 28 (2009) 6489–; doi:10.1021/om900697e

data_4070282
_publ_section_title
;
 Ion Pairing and Allyl Dynamics in a Series of
 [Pd(\h3-allyl)(N,N-chelate)](anion) Salts. On the Influence of the
 BPh4&#x2212;Anion
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6489
_journal_paper_doi               10.1021/om900697e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C22 H29 F6 N2 P Pd'
_chemical_formula_weight         572.84
_chemical_name_common
'[Pd(eta3-2-MeC3H4)(py-2-CH=NC6H4(iPr)2-2,6)][PF6]'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2983(6)
_cell_length_b                   10.1408(7)
_cell_length_c                   28.891(2)
_cell_measurement_reflns_used    2897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.45
_cell_volume                     2431.2(3)
_computing_cell_refinement       'SAINTPLUS  (Bruker AXS, 1999)'
_computing_data_collection       'SMART      (Bruker AXS, 2001)'
_computing_data_reduction        'SAINTPLUS  (Bruker AXS, 1999)'
_computing_molecular_graphics
;     
 ORTEP for Windows v1.074 (L.J. Farrugia 1997)
 Mercury CSD 2.2 (Build RC5), CCDC, Cambridge
;
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia, J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.,2008,A64,112)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0338
_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       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            14203
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.3702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                5597
_reflns_number_total             5869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900697e_si_002.cif
_cod_data_source_block           preg127
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4070282
_compound_number                 3h[PF6]