#------------------------------------------------------------------------------
#$Date: 2017-10-13 12:31:46 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/57/2235721.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_2235721
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 (2,2'-Bipyrimidine-κ²N¹,N^1'^)diiodidopalladium(II)
;
_journal_coeditor_code           ZQ2173
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m974
_journal_paper_doi               10.1107/S1600536812028292
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd I2 (C8 H6 N4)]'
_chemical_formula_moiety         'C8 H6 I2 N4 Pd'
_chemical_formula_sum            'C8 H6 I2 N4 Pd'
_chemical_formula_weight         518.37
_chemical_name_systematic
;
(2,2'-Bipyrimidine-κ²N¹,N^1'^)diiodidopalladium(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                 113.1990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1967(10)
_cell_length_b                   15.2274(10)
_cell_length_c                   10.4686(6)
_cell_measurement_reflns_used    4768
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.42
_cell_volume                     2373.1(3)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7042
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.526
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0213P)²+1.3937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                1937
_reflns_number_total             2268
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zq2173.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235721
_cod_database_fobs_code          2235721
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
Pd Pd1 0.15635(2) 0.29183(2) 0.33518(3) 0.02688(10) Uani d . 1 1
I I1 0.254992(19) 0.26771(2) 0.19695(3) 0.03728(10) Uani d . 1 1
I I2 0.16606(2) 0.45868(2) 0.30377(3) 0.04108(11) Uani d . 1 1
N N1 0.0758(2) 0.2998(2) 0.4483(3) 0.0281(8) Uani d . 1 1
N N2 -0.0087(2) 0.2101(2) 0.5372(3) 0.0319(8) Uani d . 1 1
N N3 0.0566(3) 0.0658(3) 0.4549(4) 0.0406(9) Uani d . 1 1
N N4 0.1337(2) 0.1591(2) 0.3566(3) 0.0290(8) Uani d . 1 1
C C1 0.0498(3) 0.3714(3) 0.4974(4) 0.0365(11) Uani d . 1 1
H H1 0.0702 0.4264 0.4846 0.044 Uiso calc R 1 1
C C2 -0.0068(3) 0.3644(3) 0.5664(4) 0.0372(11) Uani d . 1 1
H H2 -0.0241 0.4137 0.6020 0.045 Uiso calc R 1 1
C C3 -0.0364(3) 0.2830(3) 0.5807(4) 0.0359(11) Uani d . 1 1
H H3 -0.0775 0.2777 0.6222 0.043 Uiso calc R 1 1
C C4 0.0465(3) 0.2224(3) 0.4733(4) 0.0279(9) Uani d . 1 1
C C5 0.0804(3) 0.1433(3) 0.4274(4) 0.0308(10) Uani d . 1 1
C C6 0.0876(3) -0.0035(3) 0.4089(5) 0.0458(12) Uani d . 1 1
H H6 0.0726 -0.0596 0.4276 0.055 Uiso calc R 1 1
C C7 0.1411(3) 0.0054(3) 0.3348(5) 0.0474(13) Uani d . 1 1
H H7 0.1613 -0.0434 0.3021 0.057 Uiso calc R 1 1
C C8 0.1636(3) 0.0892(3) 0.3112(4) 0.0360(11) Uani d . 1 1
H H8 0.2003 0.0972 0.2626 0.043 Uiso calc R 1 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'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
N1 Pd1 N4 79.57(13) y
N1 Pd1 I1 175.12(10) ?
N4 Pd1 I1 95.56(9) ?
N1 Pd1 I2 95.66(10) ?
N4 Pd1 I2 173.70(9) ?
I1 Pd1 I2 89.215(14) y
C4 N1 C1 116.9(3) ?
C4 N1 Pd1 114.3(3) ?
C1 N1 Pd1 128.8(3) ?
C4 N2 C3 115.9(4) ?
C5 N3 C6 116.6(4) ?
C8 N4 C5 116.8(4) ?
C8 N4 Pd1 129.3(3) ?
C5 N4 Pd1 113.9(3) ?
N1 C1 C2 120.9(4) ?
N1 C1 H1 119.6 ?
C2 C1 H1 119.6 ?
C3 C2 C1 117.8(4) ?
C3 C2 H2 121.1 ?
C1 C2 H2 121.1 ?
N2 C3 C2 122.5(4) ?
N2 C3 H3 118.7 ?
C2 C3 H3 118.7 ?
N2 C4 N1 126.0(4) ?
N2 C4 C5 117.3(4) ?
N1 C4 C5 116.7(3) ?
N3 C5 N4 125.7(4) ?
N3 C5 C4 118.9(4) ?
N4 C5 C4 115.4(4) ?
N3 C6 C7 122.3(5) ?
N3 C6 H6 118.9 ?
C7 C6 H6 118.9 ?
C8 C7 C6 117.5(5) ?
C8 C7 H7 121.3 ?
C6 C7 H7 121.3 ?
N4 C8 C7 121.2(4) ?
N4 C8 H8 119.4 ?
C7 C8 H8 119.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 2.082(3) y
Pd1 N4 2.082(4) y
Pd1 I1 2.5696(4) y
Pd1 I2 2.5746(5) y
N1 C4 1.335(5) ?
N1 C1 1.342(5) ?
N2 C4 1.325(5) ?
N2 C3 1.343(6) ?
N3 C5 1.309(6) ?
N3 C6 1.338(6) ?
N4 C8 1.332(6) ?
N4 C5 1.363(5) ?
C1 C2 1.376(6) ?
C1 H1 0.9300 ?
C2 C3 1.358(6) ?
C2 H2 0.9300 ?
C3 H3 0.9300 ?
C4 C5 1.479(6) ?
C6 C7 1.379(6) ?
C6 H6 0.9300 ?
C7 C8 1.376(7) ?
C7 H7 0.9300 ?
C8 H8 0.9300 ?
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 I2 . 0.93 2.92 3.525(4) 123.7
C8 H8 I1 . 0.93 2.91 3.522(5) 124.4
C6 H6 N2 5_556 0.93 2.60 3.523(6) 172.5
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
N4 Pd1 N1 C4 -2.9(3)
I2 Pd1 N1 C4 173.0(3)
N4 Pd1 N1 C1 177.6(4)
I2 Pd1 N1 C1 -6.5(4)
N1 Pd1 N4 C8 -179.4(4)
I1 Pd1 N4 C8 0.4(4)
N1 Pd1 N4 C5 0.7(3)
I1 Pd1 N4 C5 -179.5(3)
C4 N1 C1 C2 -1.9(6)
Pd1 N1 C1 C2 177.6(3)
N1 C1 C2 C3 -1.2(7)
C4 N2 C3 C2 -3.0(6)
C1 C2 C3 N2 3.8(7)
C3 N2 C4 N1 -0.4(6)
C3 N2 C4 C5 178.4(4)
C1 N1 C4 N2 2.8(6)
Pd1 N1 C4 N2 -176.7(3)
C1 N1 C4 C5 -176.0(3)
Pd1 N1 C4 C5 4.5(5)
C6 N3 C5 N4 0.0(7)
C6 N3 C5 C4 178.8(4)
C8 N4 C5 N3 0.3(6)
Pd1 N4 C5 N3 -179.8(4)
C8 N4 C5 C4 -178.5(4)
Pd1 N4 C5 C4 1.4(4)
N2 C4 C5 N3 -1.8(6)
N1 C4 C5 N3 177.1(4)
N2 C4 C5 N4 177.2(4)
N1 C4 C5 N4 -3.9(6)
C5 N3 C6 C7 -0.7(7)
N3 C6 C7 C8 1.2(8)
C5 N4 C8 C7 0.2(6)
Pd1 N4 C8 C7 -179.7(3)
C6 C7 C8 N4 -0.9(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30657933
