#------------------------------------------------------------------------------
#$Date: 2017-10-13 10:42:48 +0200 (vie 13 de oct de 2017) $
#$Revision: 201978 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/20/2222088.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_2222088
loop_
_publ_author_name
'Kim, Nam-Ho'
'Hwang, In-Chul'
'Ha, Kwang'
_publ_section_title
;
 Redetermination of
 (2,2'-bipyridine-κ²N,N')dichloridopalladium(II)
 dichloromethane solvate
;
_journal_coeditor_code           KP2220
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m615
_journal_page_last               m616
_journal_paper_doi               10.1107/S1600536809016262
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pd Cl2 (C10 H8 N2)], C H2 Cl2'
_chemical_formula_moiety         'C10 H8 Cl2 N2 Pd, C H2 Cl2'
_chemical_formula_sum            'C11 H10 Cl4 N2 Pd'
_chemical_formula_weight         418.41
_chemical_name_systematic
;
(2,2'-Bipyridine-κ²N,N')dichloridopalladium(II)
dichloromethane solvate
;
_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
_cell_angle_alpha                72.481(2)
_cell_angle_beta                 66.983(2)
_cell_angle_gamma                81.429(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7913(10)
_cell_length_b                   9.1115(11)
_cell_length_c                   10.1846(12)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.25
_cell_volume                     715.58(15)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4221
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0438
_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)+(0.0352P)²+0.5604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                2298
_reflns_number_total             2862
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2220.cif
_cod_data_source_block           I
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2222088
_cod_database_fobs_code          2222088
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.32112(5) 0.28572(4) 0.21130(4) 0.04479(15) Uani d . 1 . .
Cl Cl1 0.36850(18) 0.02764(15) 0.30403(16) 0.0612(4) Uani d . 1 . .
Cl Cl2 0.1458(2) 0.22805(17) 0.11857(19) 0.0720(5) Uani d . 1 . .
N N1 0.2916(5) 0.5169(5) 0.1348(4) 0.0454(10) Uani d . 1 . .
N N2 0.4786(5) 0.3551(5) 0.2803(4) 0.0446(10) Uani d . 1 . .
C C1 0.1884(7) 0.5895(7) 0.0665(6) 0.0545(14) Uani d . 1 . .
H H1 0.126(6) 0.526(6) 0.052(5) 0.058(16) Uiso d . 1 . .
C C2 0.1803(8) 0.7475(7) 0.0175(7) 0.0610(15) Uani d . 1 . .
H H2 0.101(7) 0.800(6) -0.020(6) 0.063(17) Uiso d . 1 . .
C C3 0.2768(8) 0.8325(7) 0.0413(7) 0.0620(16) Uani d . 1 . .
H H3 0.273(6) 0.930(6) 0.018(5) 0.043(14) Uiso d . 1 . .
C C4 0.3831(7) 0.7585(6) 0.1120(6) 0.0515(13) Uani d . 1 . .
H H4 0.451(6) 0.809(6) 0.128(5) 0.046(14) Uiso d . 1 . .
C C5 0.3887(6) 0.6010(6) 0.1590(5) 0.0417(11) Uani d . 1 . .
C C6 0.4959(6) 0.5099(6) 0.2384(5) 0.0466(12) Uani d . 1 . .
C C7 0.6069(8) 0.5739(7) 0.2675(7) 0.0644(16) Uani d . 1 . .
H H7 0.623(7) 0.683(7) 0.236(6) 0.081(19) Uiso d . 1 . .
C C8 0.7003(9) 0.4784(8) 0.3427(8) 0.077(2) Uani d . 1 . .
H H8 0.775(8) 0.512(8) 0.355(7) 0.09(2) Uiso d . 1 . .
C C9 0.6833(8) 0.3223(8) 0.3858(8) 0.0717(18) Uani d . 1 . .
H H9 0.734(6) 0.255(6) 0.442(5) 0.049(15) Uiso d . 1 . .
C C10 0.5692(7) 0.2645(7) 0.3546(7) 0.0579(15) Uani d . 1 . .
H H10 0.562(6) 0.166(6) 0.376(5) 0.043(14) Uiso d . 1 . .
C C11 0.0507(9) 0.1175(7) 0.6220(8) 0.0614(16) Uani d . 1 . .
H H11A -0.043(7) 0.071(6) 0.685(6) 0.062(17) Uiso d . 1 . .
H H11B 0.115(7) 0.087(7) 0.529(7) 0.09(2) Uiso d . 1 . .
Cl Cl3 -0.0049(2) 0.31218(19) 0.55636(18) 0.0740(5) Uani d . 1 . .
Cl Cl4 0.1895(2) 0.1016(2) 0.7099(2) 0.0887(6) Uani d . 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd1 0.0465(2) 0.0387(2) 0.0512(3) -0.00670(17) -0.01825(18) -0.01196(18)
Cl1 0.0744(9) 0.0386(7) 0.0735(9) -0.0059(7) -0.0309(8) -0.0121(7)
Cl2 0.0836(11) 0.0561(9) 0.0965(12) -0.0203(8) -0.0543(9) -0.0117(8)
N1 0.045(2) 0.044(2) 0.048(2) -0.005(2) -0.017(2) -0.0118(19)
N2 0.049(2) 0.039(2) 0.050(2) -0.0036(19) -0.021(2) -0.0121(19)
C1 0.052(3) 0.054(3) 0.062(3) -0.002(3) -0.028(3) -0.012(3)
C2 0.063(4) 0.050(4) 0.068(4) 0.008(3) -0.029(3) -0.009(3)
C3 0.072(4) 0.039(3) 0.074(4) -0.002(3) -0.025(3) -0.016(3)
C4 0.057(3) 0.039(3) 0.063(3) -0.005(3) -0.025(3) -0.016(3)
C5 0.041(3) 0.039(3) 0.044(3) -0.004(2) -0.010(2) -0.016(2)
C6 0.046(3) 0.044(3) 0.045(3) -0.004(2) -0.012(2) -0.011(2)
C7 0.080(4) 0.052(4) 0.078(4) -0.015(3) -0.045(4) -0.013(3)
C8 0.084(5) 0.070(5) 0.097(5) -0.016(4) -0.058(4) -0.009(4)
C9 0.074(4) 0.063(4) 0.092(5) -0.004(3) -0.054(4) -0.009(4)
C10 0.065(4) 0.045(3) 0.067(4) -0.002(3) -0.032(3) -0.008(3)
C11 0.065(4) 0.052(4) 0.072(4) -0.009(3) -0.026(3) -0.019(3)
Cl3 0.0761(10) 0.0652(10) 0.0759(10) 0.0022(8) -0.0354(9) -0.0044(8)
Cl4 0.0906(12) 0.0701(11) 0.1211(15) 0.0040(9) -0.0663(12) -0.0139(10)
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
_geom_angle_publ_flag
N2 Pd1 N1 . . 81.04(16) ?
N2 Pd1 Cl2 . . 174.97(12) ?
N1 Pd1 Cl2 . . 94.27(12) ?
N2 Pd1 Cl1 . . 94.74(12) ?
N1 Pd1 Cl1 . . 175.78(12) ?
Cl2 Pd1 Cl1 . . 89.94(5) ?
C1 N1 C5 . . 119.3(5) ?
C1 N1 Pd1 . . 126.5(4) ?
C5 N1 Pd1 . . 114.2(3) ?
C10 N2 C6 . . 118.9(4) ?
C10 N2 Pd1 . . 126.6(4) ?
C6 N2 Pd1 . . 114.4(3) ?
N1 C1 C2 . . 121.4(6) ?
N1 C1 H1 . . 116(3) ?
C2 C1 H1 . . 123(3) ?
C3 C2 C1 . . 119.7(6) ?
C3 C2 H2 . . 118(4) ?
C1 C2 H2 . . 122(4) ?
C2 C3 C4 . . 119.2(6) ?
C2 C3 H3 . . 124(3) ?
C4 C3 H3 . . 117(3) ?
C5 C4 C3 . . 119.8(5) ?
C5 C4 H4 . . 118(3) ?
C3 C4 H4 . . 123(3) ?
N1 C5 C4 . . 120.6(5) ?
N1 C5 C6 . . 115.2(4) ?
C4 C5 C6 . . 124.2(5) ?
N2 C6 C7 . . 121.4(5) ?
N2 C6 C5 . . 115.0(4) ?
C7 C6 C5 . . 123.6(5) ?
C6 C7 C8 . . 118.8(6) ?
C6 C7 H7 . . 122(4) ?
C8 C7 H7 . . 119(4) ?
C9 C8 C7 . . 120.2(6) ?
C9 C8 H8 . . 118(5) ?
C7 C8 H8 . . 121(5) ?
C8 C9 C10 . . 118.5(6) ?
C8 C9 H9 . . 124(3) ?
C10 C9 H9 . . 117(3) ?
N2 C10 C9 . . 122.2(6) ?
N2 C10 H10 . . 118(3) ?
C9 C10 H10 . . 119(3) ?
Cl4 C11 Cl3 . . 111.0(3) ?
Cl4 C11 H11A . . 111(4) ?
Cl3 C11 H11A . . 106(4) ?
Cl4 C11 H11B . . 106(3) ?
Cl3 C11 H11B . . 103(4) ?
H11A C11 H11B . . 120(5) ?
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 . 2.025(4) yes
Pd1 N1 . 2.029(4) yes
Pd1 Cl2 . 2.2853(14) yes
Pd1 Cl1 . 2.2964(14) yes
N1 C1 . 1.335(6) ?
N1 C5 . 1.360(6) ?
N2 C10 . 1.338(7) ?
N2 C6 . 1.359(6) ?
C1 C2 . 1.375(8) ?
C1 H1 . 0.93(5) ?
C2 C3 . 1.360(8) ?
C2 H2 . 0.93(5) ?
C3 C4 . 1.376(8) ?
C3 H3 . 0.85(5) ?
C4 C5 . 1.369(7) ?
C4 H4 . 0.90(5) ?
C5 C6 . 1.480(7) ?
C6 C7 . 1.371(7) ?
C7 C8 . 1.377(9) ?
C7 H7 . 0.96(6) ?
C8 C9 . 1.369(9) ?
C8 H8 . 0.83(6) ?
C9 C10 . 1.375(8) ?
C9 H9 . 0.90(5) ?
C10 H10 . 0.86(5) ?
C11 Cl4 . 1.743(6) ?
C11 Cl3 . 1.765(6) ?
C11 H11A . 0.90(5) ?
C11 H11B . 0.99(6) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1 Cl2 . 0.93(5) 2.59(5) 3.230(6) 126(4)
C2 H2 Cl2 2_565 0.93(5) 2.79(5) 3.595(7) 145(4)
C10 H10 Cl1 . 0.86(5) 2.68(5) 3.248(6) 125(4)
C11 H11B Cl1 . 0.99(6) 2.63(6) 3.578(8) 161(5)
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 Pd1 N1 C1 . . . . -177.3(4) ?
Cl2 Pd1 N1 C1 . . . . 4.6(4) ?
N2 Pd1 N1 C5 . . . . 2.4(3) ?
Cl2 Pd1 N1 C5 . . . . -175.7(3) ?
N1 Pd1 N2 C10 . . . . 179.8(5) ?
Cl1 Pd1 N2 C10 . . . . -0.3(5) ?
N1 Pd1 N2 C6 . . . . -3.5(3) ?
Cl1 Pd1 N2 C6 . . . . 176.4(3) ?
C5 N1 C1 C2 . . . . 1.2(8) ?
Pd1 N1 C1 C2 . . . . -179.2(4) ?
N1 C1 C2 C3 . . . . -1.3(9) ?
C1 C2 C3 C4 . . . . 1.1(9) ?
C2 C3 C4 C5 . . . . -0.8(9) ?
C1 N1 C5 C4 . . . . -0.9(7) ?
Pd1 N1 C5 C4 . . . . 179.4(4) ?
C1 N1 C5 C6 . . . . 178.7(4) ?
Pd1 N1 C5 C6 . . . . -1.0(5) ?
C3 C4 C5 N1 . . . . 0.8(8) ?
C3 C4 C5 C6 . . . . -178.8(5) ?
C10 N2 C6 C7 . . . . 1.7(8) ?
Pd1 N2 C6 C7 . . . . -175.3(4) ?
C10 N2 C6 C5 . . . . -179.1(4) ?
Pd1 N2 C6 C5 . . . . 4.0(5) ?
N1 C5 C6 N2 . . . . -2.0(6) ?
C4 C5 C6 N2 . . . . 177.6(5) ?
N1 C5 C6 C7 . . . . 177.3(5) ?
C4 C5 C6 C7 . . . . -3.1(8) ?
N2 C6 C7 C8 . . . . -1.0(9) ?
C5 C6 C7 C8 . . . . 179.8(6) ?
C6 C7 C8 C9 . . . . 0.7(11) ?
C7 C8 C9 C10 . . . . -1.2(11) ?
C6 N2 C10 C9 . . . . -2.2(9) ?
Pd1 N2 C10 C9 . . . . 174.4(5) ?
C8 C9 C10 N2 . . . . 1.9(10) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30655793
