Palladium(II) Complexes of the First Pincer (Se,N,Se) Ligand, 2,6-Bis((phenylseleno)methyl)pyridine (L): Solvent-Dependent Formation of [PdCl(L)]Cl and Na[PdCl(L)][PdCl4] and High Catalytic Activity for the Heck Reaction
Das, Dipanwita; Rao, G. K.; Singh, Ajai K.; Organometallics 28 (2009) 6054–; doi:10.1021/om900570g

data_4070017
_publ_section_title
;
 Palladium(II) Complexes of the First Pincer (Se,N,Se) Ligand,
 2,6-Bis((phenylseleno)methyl)pyridine (L): Solvent-Dependent Formation of
 [PdCl(L)]Cl and Na[PdCl(L)][PdCl4] and High Catalytic Activity for the
 Heck Reaction
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6054
_journal_paper_doi               10.1021/om900570g
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C19 H17 Cl5 N Na Pd2 Se2'
_chemical_formula_sum            'C19 H17 Cl5 N Na Pd2 Se2'
_chemical_formula_weight         830.30
_chemical_name_systematic
; 
 ? 
;
_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                76.084(6)
_cell_angle_beta                 84.604(6)
_cell_angle_gamma                82.053(6)
_cell_formula_units_Z            2
_cell_length_a                   8.792(3)
_cell_length_b                   12.411(4)
_cell_length_c                   12.624(4)
_cell_measurement_reflns_used    6003
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.34
_cell_volume                     1321.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_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            12503
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    4.645
_exptl_absorpt_correction_T_max  0.459
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_meas      2.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rods
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.167
_refine_diff_density_max         3.448
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+11.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                4106
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900570g_si_002.cif
_cod_data_source_block           2
_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_cell_volume        1321.6(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070017