#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/25/2212533.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_2212533
loop_
_publ_author_name
'Valdés-Martínez, Jesús'
'Toscano, Rubén A.'
'Germán-Acacio, Juan Manuel'
_publ_section_title
;
 4,4'-Bipyridinium tetrachloridopalladate(II)
;
_journal_coeditor_code           DN2131
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m870
_journal_page_last               m871
_journal_paper_doi               10.1107/S1600536807008483
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C10 H10 N2) [Pd Cl4]'
_chemical_formula_moiety         'C10 H10 N2 2+, Cl4 Pd 2-'
_chemical_formula_sum            'C10 H10 Cl4 N2 Pd'
_chemical_formula_weight         406.40
_chemical_name_systematic
;
4,4'-Bipyridinium tetrachloridopalladate(II)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_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                 90.649(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.7180(10)
_cell_length_b                   11.754(2)
_cell_length_c                   8.015(2)
_cell_measurement_reflns_used    2186
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.08
_cell_volume                     632.9(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material
'publCIF Westrip, 2007) and enCifer (Allen et al.,  2004)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2552
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  0.8554
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0232
_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)+(0.0295P)²+0.5871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                591
_reflns_number_total             613
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2131.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               2212533
_cod_database_fobs_code          2212533
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
Pd Pd1 1.0000 0.0000 0.0000 0.03097(18) Uani d S 1
Cl Cl1 0.79728(13) 0.13796(7) 0.10751(11) 0.0519(3) Uani d . 1
N N1 0.4434(6) 0.0000 0.2829(5) 0.0489(10) Uani d SD 1
H H1 0.558(4) 0.0000 0.234(6) 0.059 Uiso d SD 1
C C2 0.3630(5) 0.0972(3) 0.3246(5) 0.0560(9) Uani d . 1
H H2 0.4243 0.1651 0.2950 0.067 Uiso calc R 1
C C3 0.1888(5) 0.0993(3) 0.4116(5) 0.0502(8) Uani d . 1
H H3 0.1330 0.1686 0.4417 0.060 Uiso calc R 1
C C4 0.0965(6) 0.0000 0.4544(5) 0.0333(9) Uani d S 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 0.0321(3) 0.0306(3) 0.0304(3) 0.000 0.00733(17) 0.000
Cl1 0.0506(6) 0.0374(5) 0.0684(6) 0.0049(3) 0.0275(4) -0.0009(4)
N1 0.035(2) 0.074(3) 0.038(2) 0.000 0.0092(16) 0.000
C2 0.048(2) 0.056(2) 0.065(2) -0.0062(18) 0.0137(17) 0.0120(18)
C3 0.0444(19) 0.0395(19) 0.067(2) -0.0008(14) 0.0182(16) 0.0016(16)
C4 0.034(2) 0.036(2) 0.0301(19) 0.000 0.0019(16) 0.000
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'
N N 0.0061 0.0033 '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'
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
Cl1 Pd1 Cl1 2_755 . 89.94(4)
Cl1 Pd1 Cl1 6 . 90.06(4)
Cl1 Pd1 Cl1 5_755 . 180.00(5)
C2 N1 C2 6 . 121.6(4)
C2 N1 H1 6 . 119.1(3)
C2 N1 H1 . . 119.1(3)
N1 C2 C3 . . 120.2(4)
N1 C2 H2 . . 119.9
C3 C2 H2 . . 119.9
C4 C3 C2 . . 120.3(3)
C4 C3 H3 . . 119.8
C2 C3 H3 . . 119.8
C3 C4 C3 6 . 117.2(4)
C3 C4 C4 6 5_556 121.4(2)
C3 C4 C4 . 5_556 121.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 Cl1 . 2.2920(8)
N1 C2 6 1.309(4)
N1 C2 . 1.309(4)
N1 H1 . 0.87(3)
C2 C3 . 1.369(5)
C2 H2 . 0.9300
C3 C4 . 1.367(4)
C3 H3 . 0.9300
C4 C3 6 1.367(4)
C4 C4 5_556 1.496(8)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 Cl1 0.87(3) 2.51(3) 3.214(3) 139.4(5)
