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_4070280
_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            'C40 H35 B N2 Pd'
_chemical_formula_weight         660.91
_chemical_name_common            '[Pd(eta3-2-MeC3H4)(phen)][BPh4]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                115.1870(10)
_cell_angle_beta                 112.8440(10)
_cell_angle_gamma                90.0920(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3407(12)
_cell_length_b                   12.2866(13)
_cell_length_c                   13.5838(15)
_cell_measurement_reflns_used    1930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.94
_cell_measurement_theta_min      2.44
_cell_volume                     1546.5(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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18083
_diffrn_reflns_theta_full        27.23
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                4428
_reflns_number_total             6845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900697e_si_002.cif
_cod_data_source_block           preg126
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               4070280
_compound_number                 3b[BPh4]