#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/29/2232971.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2232971
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 trans-Dichloridobis(4-phenylpyridine-κN)palladium(II)
;
_journal_coeditor_code           TK5025
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1895
_journal_paper_doi               10.1107/S160053681105063X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pd Cl2 (C11 H9 N)2]'
_chemical_formula_moiety         'C22 H18 Cl2 N2 Pd'
_chemical_formula_sum            'C22 H18 Cl2 N2 Pd'
_chemical_formula_weight         487.68
_chemical_name_systematic
;
trans-Dichloridobis(4-phenylpyridine-κN)palladium(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.572(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4270(15)
_cell_length_b                   23.680(4)
_cell_length_c                   8.8554(14)
_cell_measurement_reflns_used    4007
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.37
_cell_volume                     1936.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6848
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.243
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.875028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0291
_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/[σ²(Fo²)+(0.0380P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                1866
_reflns_number_total             2358
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            tk5025.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232971
_cod_database_fobs_code          2232971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.0000 0.125997(10) 0.7500 0.02513(11) Uani d S 1 2 . .
Cl Cl1 -0.23973(8) 0.12738(3) 0.76980(10) 0.04242(19) Uani d . 1 1 . .
N N1 0.0000 0.04062(12) 0.7500 0.0249(6) Uani d S 1 2 . .
N N2 0.0000 0.21085(11) 0.7500 0.0251(6) Uani d S 1 2 . .
C C1A 0.1164(12) 0.0107(3) 0.8189(15) 0.034(2) Uani d P 0.53(2) 1 A 1
H H1A 0.2009 0.0306 0.8673 0.040 Uiso calc PR 0.53(2) 1 A 1
C C2A 0.1188(12) -0.0469(3) 0.8225(15) 0.033(2) Uani d P 0.53(2) 1 A 1
H H2A 0.2030 -0.0659 0.8754 0.040 Uiso calc PR 0.53(2) 1 A 1
C C1B 0.0744(13) 0.0112(3) 0.8716(14) 0.028(2) Uani d P 0.47(2) 1 A 2
H H1B 0.1266 0.0316 0.9575 0.034 Uiso calc PR 0.47(2) 1 A 2
C C2B 0.0776(12) -0.0470(4) 0.8759(14) 0.030(2) Uani d P 0.47(2) 1 A 2
H H2B 0.1318 -0.0661 0.9631 0.036 Uiso calc PR 0.47(2) 1 A 2
C C3 0.0000 -0.07819(14) 0.7500 0.0258(8) Uani d S 1 2 . .
C C4 0.0000 -0.14083(14) 0.7500 0.0274(8) Uani d S 1 2 . .
C C5 0.1253(3) -0.17118(10) 0.8113(3) 0.0323(6) Uani d . 1 1 . .
H H5 0.2114 -0.1514 0.8553 0.039 Uiso calc R 1 1 A .
C C6 0.1257(3) -0.22957(11) 0.8090(3) 0.0337(6) Uani d . 1 1 A .
H H6 0.2127 -0.2496 0.8481 0.040 Uiso calc R 1 1 . .
C C7 0.0000 -0.25900(15) 0.7500 0.0315(9) Uani d S 1 2 . .
H H7 0.0000 -0.2991 0.7500 0.038 Uiso calc SR 1 2 A .
C C8 0.0559(3) 0.23996(10) 0.8782(3) 0.0312(6) Uani d . 1 1 A .
H H8 0.0957 0.2198 0.9695 0.037 Uiso calc R 1 1 . .
C C9 0.0575(3) 0.29803(11) 0.8819(3) 0.0316(6) Uani d . 1 1 . .
H H9 0.0981 0.3171 0.9749 0.038 Uiso calc R 1 1 A .
C C10 0.0000 0.32924(14) 0.7500 0.0242(7) Uani d S 1 2 . .
C C11 0.0000 0.39200(14) 0.7500 0.0260(8) Uani d S 1 2 . .
C C12A 0.0602(10) 0.4220(2) 0.8820(9) 0.038(2) Uani d P 0.512(12) 1 A 1
H H12A 0.1017 0.4022 0.9735 0.046 Uiso calc PR 0.512(12) 1 A 1
C C13A 0.0605(9) 0.4803(3) 0.8817(10) 0.044(2) Uani d P 0.512(12) 1 A 1
H H13A 0.1025 0.5004 0.9727 0.053 Uiso calc PR 0.512(12) 1 A 1
C C12B 0.1230(8) 0.4222(2) 0.8248(8) 0.0280(17) Uani d P 0.488(12) 1 A 2
H H12B 0.2060 0.4025 0.8778 0.034 Uiso calc PR 0.488(12) 1 A 2
C C13B 0.1226(9) 0.4806(2) 0.8206(8) 0.0347(19) Uani d P 0.488(12) 1 A 2
H H13B 0.2072 0.5009 0.8666 0.042 Uiso calc PR 0.488(12) 1 A 2
C C14 0.0000 0.50968(15) 0.7500 0.0344(9) Uani d S 1 2 . .
H H14 0.0000 0.5498 0.7500 0.041 Uiso calc SR 1 2 A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Pd1 N1 . . 180.0
N2 Pd1 Cl1 . 2_556 89.182(17)
N1 Pd1 Cl1 . 2_556 90.818(17)
N2 Pd1 Cl1 . . 89.182(17)
N1 Pd1 Cl1 . . 90.818(17)
Cl1 Pd1 Cl1 2_556 . 178.36(3)
C1A N1 C1A 2_556 . 116.5(7)
C1A N1 C1B . 2_556 109.6(3)
C1A N1 C1B 2_556 . 109.6(3)
C1B N1 C1B 2_556 . 118.1(7)
C1A N1 Pd1 2_556 . 121.8(3)
C1A N1 Pd1 . . 121.8(3)
C1B N1 Pd1 2_556 . 120.9(4)
C1B N1 Pd1 . . 120.9(4)
C8 N2 C8 . 2_556 118.2(3)
C8 N2 Pd1 . . 120.91(15)
C8 N2 Pd1 2_556 . 120.91(15)
N1 C1A C2A . . 123.0(7)
N1 C1A H1A . . 118.5
C2A C1A H1A . . 118.5
C1A C2A C3 . . 121.0(6)
C1A C2A H2A . . 119.5
C3 C2A H2A . . 119.5
N1 C1B C2B . . 122.7(7)
N1 C1B H1B . . 118.6
C2B C1B H1B . . 118.6
C1B C2B C3 . . 119.7(7)
C1B C2B H2B . . 120.2
C3 C2B H2B . . 120.2
C2A C3 C2A . 2_556 115.4(7)
C2A C3 C2B 2_556 . 109.2(4)
C2A C3 C2B . 2_556 109.2(4)
C2B C3 C2B . 2_556 117.1(8)
C2A C3 C4 . . 122.3(3)
C2A C3 C4 2_556 . 122.3(3)
C2B C3 C4 . . 121.5(4)
C2B C3 C4 2_556 . 121.5(4)
C5 C4 C5 2_556 . 118.0(3)
C5 C4 C3 2_556 . 120.99(16)
C5 C4 C3 . . 120.99(16)
C6 C5 C4 . . 120.9(3)
C6 C5 H5 . . 119.5
C4 C5 H5 . . 119.5
C5 C6 C7 . . 120.3(3)
C5 C6 H6 . . 119.9
C7 C6 H6 . . 119.9
C6 C7 C6 . 2_556 119.5(3)
C6 C7 H7 . . 120.2
C6 C7 H7 2_556 . 120.2
N2 C8 C9 . . 122.3(2)
N2 C8 H8 . . 118.9
C9 C8 H8 . . 118.9
C8 C9 C10 . . 120.6(2)
C8 C9 H9 . . 119.7
C10 C9 H9 . . 119.7
C9 C10 C9 2_556 . 116.1(3)
C9 C10 C11 2_556 . 121.95(16)
C9 C10 C11 . . 121.95(16)
C12A C11 C12A . 2_556 118.4(6)
C12A C11 C12B 2_556 . 107.2(4)
C12A C11 C12B . 2_556 107.2(4)
C12B C11 C12B . 2_556 119.1(5)
C12A C11 C10 . . 120.8(3)
C12A C11 C10 2_556 . 120.8(3)
C12B C11 C10 . . 120.5(3)
C12B C11 C10 2_556 . 120.5(3)
C13A C12A C11 . . 120.7(6)
C13A C12A H12A . . 119.6
C11 C12A H12A . . 119.6
C14 C13A C12A . . 120.3(6)
C14 C13A H13A . . 119.8
C12A C13A H13A . . 119.8
C13B C12B C11 . . 119.8(5)
C13B C12B H12B . . 120.1
C11 C12B H12B . . 120.1
C14 C13B C12B . . 120.5(6)
C14 C13B H13B . . 119.7
C12B C13B H13B . . 119.7
C13A C14 C13A 2_556 . 119.5(6)
C13A C14 C13B . 2_556 107.3(4)
C13A C14 C13B 2_556 . 107.3(4)
C13B C14 C13B 2_556 . 120.2(6)
C13A C14 H14 2_556 . 120.2
C13A C14 H14 . . 120.2
C13B C14 H14 2_556 . 119.9
C13B C14 H14 . . 119.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N2 . 2.009(3) y
Pd1 N1 . 2.022(3) y
Pd1 Cl1 2_556 2.3018(8) ?
Pd1 Cl1 . 2.3018(8) y
N1 C1A 2_556 1.345(8) ?
N1 C1A . 1.345(8) ?
N1 C1B 2_556 1.354(9) ?
N1 C1B . 1.354(9) ?
N2 C8 . 1.342(3) ?
N2 C8 2_556 1.342(3) ?
C1A C2A . 1.364(10) ?
C1A H1A . 0.9500 ?
C2A C3 . 1.388(8) ?
C2A H2A . 0.9500 ?
C1B C2B . 1.381(11) ?
C1B H1B . 0.9500 ?
C2B C3 . 1.413(9) ?
C2B H2B . 0.9500 ?
C3 C2A 2_556 1.388(8) ?
C3 C2B 2_556 1.413(9) ?
C3 C4 . 1.483(5) ?
C4 C5 2_556 1.396(3) ?
C4 C5 . 1.396(3) ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.384(3) ?
C6 H6 . 0.9500 ?
C7 C6 2_556 1.384(3) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.376(3) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.396(3) ?
C9 H9 . 0.9500 ?
C10 C9 2_556 1.396(3) ?
C10 C11 . 1.486(5) ?
C11 C12A . 1.389(6) ?
C11 C12A 2_556 1.389(6) ?
C11 C12B . 1.409(6) ?
C11 C12B 2_556 1.409(6) ?
C12A C13A . 1.381(8) ?
C12A H12A . 0.9500 ?
C13A C14 . 1.379(8) ?
C13A H13A . 0.9500 ?
C12B C13B . 1.384(8) ?
C12B H12B . 0.9500 ?
C13B C14 . 1.383(7) ?
C13B H13B . 0.9500 ?
C14 C13A 2_556 1.379(8) ?
C14 C13B 2_556 1.383(7) ?
C14 H14 . 0.9500 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
Cl1 Pd1 N1 C1A 2_556 2_556 -144.2(8)
Cl1 Pd1 N1 C1A . 2_556 35.8(8)
Cl1 Pd1 N1 C1A 2_556 . 35.8(8)
Cl1 Pd1 N1 C1A . . -144.2(8)
Cl1 Pd1 N1 C1B 2_556 2_556 -110.4(7)
Cl1 Pd1 N1 C1B . 2_556 69.6(7)
Cl1 Pd1 N1 C1B 2_556 . 69.6(7)
Cl1 Pd1 N1 C1B . . -110.4(7)
Cl1 Pd1 N2 C8 2_556 . -79.23(14)
Cl1 Pd1 N2 C8 . . 100.77(14)
Cl1 Pd1 N2 C8 2_556 2_556 100.77(14)
Cl1 Pd1 N2 C8 . 2_556 -79.23(14)
C1A N1 C1A C2A 2_556 . -0.9(5)
C1B N1 C1A C2A 2_556 . -31.3(6)
C1B N1 C1A C2A . . 81.7(13)
Pd1 N1 C1A C2A . . 179.1(5)
N1 C1A C2A C3 . . 1.8(9)
C1A N1 C1B C2B 2_556 . 30.4(6)
C1A N1 C1B C2B . . -79.2(13)
C1B N1 C1B C2B 2_556 . 0.2(5)
Pd1 N1 C1B C2B . . -179.8(5)
N1 C1B C2B C3 . . -0.5(9)
C1A C2A C3 C2A . 2_556 -0.9(4)
C1A C2A C3 C2B . . -83.7(14)
C1A C2A C3 C2B . 2_556 28.3(6)
C1A C2A C3 C4 . . 179.1(4)
C1B C2B C3 C2A . . 79.8(13)
C1B C2B C3 C2A . 2_556 -28.6(6)
C1B C2B C3 C2B . 2_556 0.2(4)
C1B C2B C3 C4 . . -179.8(4)
C2A C3 C4 C5 . 2_556 174.0(8)
C2A C3 C4 C5 2_556 2_556 -6.0(8)
C2B C3 C4 C5 . 2_556 141.4(7)
C2B C3 C4 C5 2_556 2_556 -38.6(7)
C2A C3 C4 C5 . . -6.0(8)
C2A C3 C4 C5 2_556 . 174.0(8)
C2B C3 C4 C5 . . -38.6(7)
C2B C3 C4 C5 2_556 . 141.4(7)
C5 C4 C5 C6 2_556 . 1.06(18)
C3 C4 C5 C6 . . -178.94(18)
C4 C5 C6 C7 . . -2.1(4)
C5 C6 C7 C6 . 2_556 1.05(18)
C8 N2 C8 C9 2_556 . -0.01(19)
Pd1 N2 C8 C9 . . 179.99(19)
N2 C8 C9 C10 . . 0.0(4)
C8 C9 C10 C9 . 2_556 -0.01(18)
C8 C9 C10 C11 . . 179.99(18)
C9 C10 C11 C12A 2_556 . -178.8(5)
C9 C10 C11 C12A . . 1.2(5)
C9 C10 C11 C12A 2_556 2_556 1.2(5)
C9 C10 C11 C12A . 2_556 -178.8(5)
C9 C10 C11 C12B 2_556 . -137.3(4)
C9 C10 C11 C12B . . 42.7(4)
C9 C10 C11 C12B 2_556 2_556 42.7(4)
C9 C10 C11 C12B . 2_556 -137.3(4)
C12A C11 C12A C13A 2_556 . -0.2(5)
C12B C11 C12A C13A . . 79.4(8)
C12B C11 C12A C13A 2_556 . -36.9(6)
C10 C11 C12A C13A . . 179.8(5)
C11 C12A C13A C14 . . 0.4(10)
C12A C11 C12B C13B . . -80.1(8)
C12A C11 C12B C13B 2_556 . 35.0(5)
C12B C11 C12B C13B 2_556 . -1.5(4)
C10 C11 C12B C13B . . 178.5(4)
C11 C12B C13B C14 . . 3.1(8)
C12A C13A C14 C13A . 2_556 -0.2(5)
C12A C13A C14 C13B . 2_556 38.0(6)
C12A C13A C14 C13B . . -79.6(8)
C12B C13B C14 C13A . 2_556 -39.6(6)
C12B C13B C14 C13A . . 76.8(8)
C12B C13B C14 C13B . 2_556 -1.6(4)
