#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/32/2013288.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_2013288
loop_
_publ_author_name
'Wen-Rui Yao'
'Ze-Hua Liu'
'Qian-Feng Zhang'
_publ_section_title
Dibromo(N,N'-di-2-pyridylamine-κ²N,N')palladium(II)
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m139
_journal_page_last               m140
_journal_paper_doi               10.1107/S0108270103004578
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd Br2 (C10 H9 N3)]'
_chemical_formula_moiety         'C10 H9 Br2 N3 Pd'
_chemical_formula_sum            'C10 H9 Br2 N3 Pd'
_chemical_formula_weight         437.42
_chemical_name_systematic
;
 Dibromo-[N,N-di(pyrid-2-yl)amine]-palladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 95.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3274(8)
_cell_length_b                   9.6764(7)
_cell_length_c                   12.3385(10)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.45
_cell_volume                     1226.52(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
'SHELXTL (Bruker, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9229
_diffrn_reflns_theta_full        28.3
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    8.003
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0496P)²+1.2599P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                2561
_reflns_number_total             3047
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg1159.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013288
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_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
_atom_site_type_symbol
Pd1 0.41999(3) 0.25568(3) 0.74512(2) 0.03152(10) Uani d . 1 . . Pd
Br1 0.44054(5) 0.29502(6) 0.55421(4) 0.05536(16) Uani d . 1 . . Br
Br2 0.28505(5) 0.05654(5) 0.69534(4) 0.05413(15) Uani d . 1 . . Br
N1 0.5465(3) 0.4133(3) 0.7881(3) 0.0325(7) Uani d . 1 . . N
N2 0.4150(3) 0.2174(3) 0.9069(3) 0.0332(7) Uani d . 1 . . N
N3 0.6348(3) 0.2825(4) 0.9389(3) 0.0387(8) Uani d . 1 . . N
H3 0.7084 0.2464 0.9626 0.046 Uiso calc R 1 . . H
C1 0.5495(4) 0.5274(4) 0.7263(3) 0.0383(9) Uani d . 1 . . C
H1 0.4821 0.5426 0.6717 0.046 Uiso calc R 1 . . H
C2 0.6484(5) 0.6225(5) 0.7408(4) 0.0456(10) Uani d . 1 . . C
H2 0.6477 0.7013 0.6976 0.055 Uiso calc R 1 . . H
C3 0.7487(5) 0.5983(5) 0.8208(4) 0.0477(11) Uani d . 1 . . C
H3A 0.8192 0.6585 0.8297 0.057 Uiso calc R 1 . . H
C4 0.7446(4) 0.4853(5) 0.8877(3) 0.0421(9) Uani d . 1 . . C
H4 0.8106 0.4694 0.9434 0.050 Uiso calc R 1 . . H
C5 0.6392(3) 0.3947(4) 0.8704(3) 0.0321(7) Uani d . 1 . . C
C6 0.5247(4) 0.2213(4) 0.9738(3) 0.0336(8) Uani d . 1 . . C
C7 0.5339(5) 0.1616(4) 1.0772(3) 0.0403(9) Uani d . 1 . . C
H7 0.6124 0.1616 1.1216 0.048 Uiso calc R 1 . . H
C8 0.4249(5) 0.1029(5) 1.1119(3) 0.0451(10) Uani d . 1 . . C
H8 0.4292 0.0598 1.1795 0.054 Uiso calc R 1 . . H
C9 0.3097(5) 0.1078(5) 1.0470(4) 0.0465(10) Uani d . 1 . . C
H9 0.2343 0.0721 1.0716 0.056 Uiso calc R 1 . . H
C10 0.3059(4) 0.1655(5) 0.9452(4) 0.0434(10) Uani d . 1 . . C
H10 0.2271 0.1693 0.9014 0.052 Uiso calc R 1 . . H
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 0.02235(16) 0.04018(18) 0.03017(16) -0.00304(11) -0.00630(11) 0.00477(11)
Br1 0.0473(3) 0.0789(4) 0.0370(2) -0.0159(2) -0.00988(19) 0.0078(2)
Br2 0.0544(3) 0.0596(3) 0.0451(3) -0.0220(2) -0.0109(2) 0.0040(2)
N1 0.0262(15) 0.0342(16) 0.0362(16) -0.0005(12) -0.0018(13) 0.0031(13)
N2 0.0278(16) 0.0361(16) 0.0350(17) -0.0024(12) -0.0003(13) 0.0023(13)
N3 0.0247(16) 0.0496(19) 0.0394(18) -0.0011(14) -0.0084(14) 0.0087(15)
C1 0.036(2) 0.042(2) 0.037(2) 0.0019(17) 0.0015(16) 0.0025(16)
C2 0.056(3) 0.039(2) 0.044(2) -0.0072(19) 0.012(2) 0.0021(18)
C3 0.043(2) 0.053(3) 0.047(2) -0.016(2) 0.007(2) -0.009(2)
C4 0.035(2) 0.051(2) 0.040(2) -0.0110(18) -0.0027(17) -0.0039(18)
C5 0.0245(17) 0.0406(19) 0.0303(17) -0.0006(15) -0.0009(14) -0.0034(15)
C6 0.032(2) 0.0351(19) 0.0327(19) 0.0020(15) -0.0004(15) 0.0019(14)
C7 0.051(3) 0.041(2) 0.0282(18) 0.0022(18) -0.0026(17) 0.0006(16)
C8 0.060(3) 0.046(2) 0.0299(19) 0.000(2) 0.0084(19) 0.0025(17)
C9 0.047(3) 0.047(2) 0.049(2) -0.009(2) 0.019(2) 0.0002(19)
C10 0.033(2) 0.052(2) 0.046(2) -0.0020(18) 0.0075(18) -0.0011(19)
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'
Br Br -0.2901 2.4595 '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
Br1 Pd1 Br2 89.07(2) yes
N1 Pd1 N2 87.79(13) yes
N1 Pd1 Br1 91.01(9) yes
N2 Pd1 Br1 176.17(9) yes
N1 Pd1 Br2 175.38(9) yes
N2 Pd1 Br2 91.83(9) yes
C1 N1 Pd1 121.2(3) yes
C5 N1 Pd1 119.2(3) yes
C1 N1 C5 119.0(3) yes
C6 N2 Pd1 119.8(3) yes
C10 N2 Pd1 120.8(3) yes
C6 N2 C10 118.4(4) yes
C5 N3 C6 127.2(3) yes
N1 C1 C2 122.5(4) ?
C1 C2 C3 118.3(4) ?
C2 C3 C4 120.0(4) ?
C3 C4 C5 118.7(4) ?
N1 C5 N3 120.4(3) ?
N1 C5 C4 121.3(4) ?
N3 C5 C4 118.4(4) ?
N2 C6 N3 119.4(3) ?
N2 C6 C7 122.0(4) ?
N3 C6 C7 118.6(4) ?
C6 C7 C8 118.4(4) ?
C7 C8 C9 119.9(4) ?
C8 C9 C10 119.5(4) ?
N2 C10 C9 121.4(4) ?
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 Br1 . 2.4168(6) yes
Pd1 Br2 . 2.4201(5) yes
Pd1 N1 . 2.042(3) yes
Pd1 N2 . 2.036(3) yes
N1 C1 . 1.345(5) yes
N1 C5 . 1.335(5) yes
N2 C6 . 1.332(5) yes
N2 C10 . 1.362(5) yes
N3 C5 . 1.380(5) yes
N3 C6 . 1.389(5) yes
C1 C2 . 1.373(6) ?
C2 C3 . 1.376(7) ?
C3 C4 . 1.373(7) ?
C4 C5 . 1.396(5) ?
C6 C7 . 1.395(5) ?
C7 C8 . 1.368(6) ?
C8 C9 . 1.365(7) ?
C9 C10 . 1.371(6) ?
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
_geom_torsion_publ_flag
N2 Pd1 N1 C5 40.5(3) ?
Br1 Pd1 N1 C5 -135.8(3) ?
N2 Pd1 N1 C1 -148.6(3) ?
Br1 Pd1 N1 C1 35.0(3) yes
N1 Pd1 N2 C6 -42.1(3) ?
Br2 Pd1 N2 C6 133.3(3) ?
N1 Pd1 N2 C10 148.9(3) ?
Br2 Pd1 N2 C10 -35.7(3) yes
C5 N1 C1 C2 3.6(6) ?
Pd1 N1 C1 C2 -167.2(3) ?
N1 C1 C2 C3 0.9(7) ?
C1 C2 C3 C4 -3.6(7) ?
C2 C3 C4 C5 1.8(7) ?
C1 N1 C5 N3 176.5(4) ?
Pd1 N1 C5 N3 -12.5(5) yes
C1 N1 C5 C4 -5.4(6) ?
Pd1 N1 C5 C4 165.6(3) ?
C6 N3 C5 N1 -35.6(6) ?
C6 N3 C5 C4 146.2(4) ?
C3 C4 C5 N1 2.7(6) ?
C3 C4 C5 N3 -179.1(4) ?
C10 N2 C6 N3 -175.6(4) ?
Pd1 N2 C6 N3 15.2(5) yes
C10 N2 C6 C7 6.6(6) ?
Pd1 N2 C6 C7 -162.7(3) ?
C5 N3 C6 N2 34.0(6) ?
C5 N3 C6 C7 -148.0(4) ?
N2 C6 C7 C8 -3.0(6) ?
N3 C6 C7 C8 179.2(4) ?
C6 C7 C8 C9 -2.1(6) ?
C7 C8 C9 C10 3.2(7) ?
C6 N2 C10 C9 -5.4(6) ?
Pd1 N2 C10 C9 163.8(3) ?
C8 C9 C10 N2 0.5(7) ?
