#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004638.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7004638
loop_
_publ_author_name
'Griffith, Darren'
'Chopra, Atish'
'Müller-Bunz, Helge'
'Marmion, Celine J.'
_publ_section_title
;
 The reduction of platinum(IV) and palladium(IV) ions by
 2,6-pyridinedihydroxamic acid
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              6933
_journal_page_last               6939
_journal_paper_doi               10.1039/b809584a
_journal_year                    2008
_chemical_formula_moiety         'C14 H8 N2 O8 Pd, 2 (H2 O)'
_chemical_formula_sum            'C14 H12 N2 O10 Pd'
_chemical_formula_weight         474.66
_chemical_name_systematic
;
?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.176(2)
_cell_angle_beta                 88.064(2)
_cell_angle_gamma                73.046(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7526(8)
_cell_length_b                   10.2338(11)
_cell_length_c                   10.4818(11)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.17
_cell_measurement_theta_min      2.74
_cell_volume                     792.61(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16408
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0379P)²+0.5329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                4322
_reflns_number_total             4567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809584a.txt
_cod_data_source_block           nol21
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3136(2) 0.42390(17) 0.44904(15) 0.0182(3) Uani 1 1 d . . .
H1O1 H 0.374(5) 0.340(4) 0.438(3) 0.043(10) Uiso 1 1 d . . .
H2O1 H 0.363(5) 0.470(4) 0.419(3) 0.034(9) Uiso 1 1 d . . .
O2 O 0.6196(2) 0.02670(17) 0.12535(16) 0.0165(3) Uani 1 1 d . . .
H1O2 H 0.685(5) -0.044(4) 0.134(3) 0.038(10) Uiso 1 1 d . . .
H2O2 H 0.618(5) 0.052(4) 0.056(4) 0.037(10) Uiso 1 1 d . . .
Pd Pd 0.898269(17) 0.213109(13) 0.193560(13) 0.00993(5) Uani 1 1 d . . .
N1 N 0.8263(2) 0.39084(16) 0.08433(16) 0.0114(3) Uani 1 1 d . . .
C1 C 0.8960(2) 0.37620(19) -0.03514(18) 0.0120(3) Uani 1 1 d . . .
C6 C 1.0450(3) 0.24495(19) -0.04871(18) 0.0127(3) Uani 1 1 d . . .
O3 O 1.07975(19) 0.16204(15) 0.05335(13) 0.0145(3) Uani 1 1 d . . .
O4 O 1.1303(2) 0.22497(15) -0.14893(14) 0.0160(3) Uani 1 1 d . . .
C2 C 0.8412(3) 0.4764(2) -0.13415(19) 0.0138(3) Uani 1 1 d . . .
H2 H 0.893(4) 0.460(3) -0.210(3) 0.025(7) Uiso 1 1 d . . .
C3 C 0.7063(3) 0.5959(2) -0.1094(2) 0.0157(4) Uani 1 1 d . . .
H3 H 0.663(4) 0.662(3) -0.175(3) 0.019(7) Uiso 1 1 d . . .
C4 C 0.6384(3) 0.6126(2) 0.0142(2) 0.0145(4) Uani 1 1 d . . .
H4 H 0.548(4) 0.693(3) 0.040(3) 0.030(8) Uiso 1 1 d . . .
C5 C 0.7045(3) 0.5093(2) 0.11041(19) 0.0121(3) Uani 1 1 d . . .
C7 C 0.6471(3) 0.53354(19) 0.24733(19) 0.0131(3) Uani 1 1 d . . .
O5 O 0.7843(2) 0.50953(15) 0.32375(14) 0.0149(3) Uani 1 1 d . . .
H1O5 H 0.750(5) 0.522(4) 0.389(3) 0.038(10) Uiso 1 1 d . . .
O6 O 0.4892(2) 0.57685(16) 0.27638(15) 0.0179(3) Uani 1 1 d . . .
N2 N 0.9561(2) 0.03223(17) 0.29924(15) 0.0113(3) Uani 1 1 d . . .
C8 C 0.8202(3) 0.02466(19) 0.38047(18) 0.0123(3) Uani 1 1 d . . .
C13 C 0.6718(2) 0.15673(19) 0.38812(19) 0.0126(3) Uani 1 1 d . . .
O7 O 0.69490(19) 0.26044(14) 0.31819(14) 0.0146(3) Uani 1 1 d . . .
O8 O 0.5423(2) 0.16375(15) 0.46046(15) 0.0180(3) Uani 1 1 d . . .
C9 C 0.8204(3) -0.0931(2) 0.45527(19) 0.0136(3) Uani 1 1 d . . .
H9 H 0.722(3) -0.089(2) 0.508(2) 0.008(6) Uiso 1 1 d . . .
C10 C 0.9679(3) -0.2089(2) 0.44596(19) 0.0144(3) Uani 1 1 d . . .
H10 H 0.969(4) -0.286(3) 0.493(3) 0.017(7) Uiso 1 1 d . . .
C11 C 1.1086(3) -0.2011(2) 0.36403(19) 0.0138(3) Uani 1 1 d . . .
H11 H 1.215(4) -0.271(3) 0.355(3) 0.023(7) Uiso 1 1 d . . .
C12 C 1.0992(3) -0.07876(19) 0.29204(18) 0.0122(3) Uani 1 1 d . . .
C14 C 1.2553(2) -0.06820(19) 0.20628(18) 0.0130(3) Uani 1 1 d . . .
O9 O 1.3318(2) 0.01950(16) 0.24323(15) 0.0164(3) Uani 1 1 d . . .
H1O9 H 1.412(5) 0.020(3) 0.200(3) 0.033(9) Uiso 1 1 d . . .
O10 O 1.3006(2) -0.13996(15) 0.11686(15) 0.0174(3) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1O1 O1 H2O1 109(4) . . ?
H1O2 O2 H2O2 109(4) . . ?
O7 Pd O3 172.73(6) . . ?
O7 Pd N1 96.62(6) . . ?
O3 Pd N1 81.71(6) . . ?
O7 Pd N2 81.95(6) . . ?
O3 Pd N2 99.28(6) . . ?
N1 Pd N2 176.28(6) . . ?
C5 N1 C1 119.31(16) . . ?
C5 N1 Pd 128.44(13) . . ?
C1 N1 Pd 111.57(12) . . ?
N1 C1 C2 122.47(17) . . ?
N1 C1 C6 114.17(16) . . ?
C2 C1 C6 123.28(17) . . ?
O4 C6 O3 123.91(18) . . ?
O4 C6 C1 120.55(17) . . ?
O3 C6 C1 115.44(16) . . ?
C6 O3 Pd 113.89(12) . . ?
C1 C2 C3 118.32(18) . . ?
C1 C2 H2 117.8(19) . . ?
C3 C2 H2 123.9(19) . . ?
C4 C3 C2 119.16(18) . . ?
C4 C3 H3 121.0(18) . . ?
C2 C3 H3 119.8(18) . . ?
C3 C4 C5 119.42(18) . . ?
C3 C4 H4 124.3(19) . . ?
C5 C4 H4 116.3(19) . . ?
N1 C5 C4 121.09(18) . . ?
N1 C5 C7 119.24(17) . . ?
C4 C5 C7 119.57(17) . . ?
O6 C7 O5 126.45(19) . . ?
O6 C7 C5 121.04(18) . . ?
O5 C7 C5 112.42(16) . . ?
C7 O5 H1O5 109(3) . . ?
C12 N2 C8 118.66(17) . . ?
C12 N2 Pd 129.37(13) . . ?
C8 N2 Pd 111.77(12) . . ?
N2 C8 C9 122.88(17) . . ?
N2 C8 C13 114.70(16) . . ?
C9 C8 C13 122.36(17) . . ?
O8 C13 O7 123.50(18) . . ?
O8 C13 C8 120.93(18) . . ?
O7 C13 C8 115.51(16) . . ?
C13 O7 Pd 114.28(12) . . ?
C8 C9 C10 118.33(18) . . ?
C8 C9 H9 117.2(15) . . ?
C10 C9 H9 124.4(15) . . ?
C11 C10 C9 119.00(18) . . ?
C11 C10 H10 121.8(18) . . ?
C9 C10 H10 119.2(18) . . ?
C10 C11 C12 119.40(18) . . ?
C10 C11 H11 125.1(18) . . ?
C12 C11 H11 115.5(18) . . ?
N2 C12 C11 121.70(18) . . ?
N2 C12 C14 118.68(17) . . ?
C11 C12 C14 119.59(17) . . ?
O10 C14 O9 127.18(19) . . ?
O10 C14 C12 120.75(18) . . ?
O9 C14 C12 112.03(16) . . ?
C14 O9 H1O9 110(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1O1 0.86(4) . ?
O1 H2O1 0.74(4) . ?
O2 H1O2 0.75(4) . ?
O2 H2O2 0.75(4) . ?
Pd O7 1.9872(14) . ?
Pd O3 1.9933(14) . ?
Pd N1 2.0078(16) . ?
Pd N2 2.0147(16) . ?
N1 C5 1.344(2) . ?
N1 C1 1.350(2) . ?
C1 C2 1.381(3) . ?
C1 C6 1.508(3) . ?
C6 O4 1.222(2) . ?
C6 O3 1.292(2) . ?
C2 C3 1.395(3) . ?
C2 H2 0.88(3) . ?
C3 C4 1.386(3) . ?
C3 H3 0.92(3) . ?
C4 C5 1.392(3) . ?
C4 H4 0.96(3) . ?
C5 C7 1.507(3) . ?
C7 O6 1.212(2) . ?
C7 O5 1.306(2) . ?
O5 H1O5 0.73(4) . ?
N2 C12 1.342(2) . ?
N2 C8 1.348(2) . ?
C8 C9 1.381(3) . ?
C8 C13 1.504(3) . ?
C13 O8 1.226(2) . ?
C13 O7 1.291(2) . ?
C9 C10 1.394(3) . ?
C9 H9 0.92(2) . ?
C10 C11 1.382(3) . ?
C10 H10 0.89(3) . ?
C11 C12 1.391(3) . ?
C11 H11 0.93(3) . ?
C12 C14 1.507(3) . ?
C14 O10 1.218(2) . ?
C14 O9 1.300(2) . ?
O9 H1O9 0.76(3) . ?
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
_geom_hbond_site_symmetry_A
O1 H1O1 O8 0.86(4) 1.89(4) 2.730(2) 162(3) .
O1 H2O1 O6 0.74(4) 2.15(4) 2.860(2) 162(4) .
O2 H1O2 O4 0.75(4) 1.98(4) 2.733(2) 176(4) 2_755
O2 H2O2 O10 0.75(4) 2.11(4) 2.826(2) 159(4) 2_755
O5 H1O5 O1 0.73(4) 1.84(4) 2.561(2) 170(4) 2_666
O9 H1O9 O2 0.76(3) 1.78(4) 2.531(2) 170(4) 1_655
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Pd N1 C5 13.43(17) . . . . ?
O3 Pd N1 C5 -173.71(17) . . . . ?
N2 Pd N1 C5 80.6(10) . . . . ?
O7 Pd N1 C1 -156.91(13) . . . . ?
O3 Pd N1 C1 15.96(13) . . . . ?
N2 Pd N1 C1 -89.7(9) . . . . ?
C5 N1 C1 C2 -3.0(3) . . . . ?
Pd N1 C1 C2 168.33(15) . . . . ?
C5 N1 C1 C6 173.87(17) . . . . ?
Pd N1 C1 C6 -14.81(19) . . . . ?
N1 C1 C6 O4 -173.38(18) . . . . ?
C2 C1 C6 O4 3.5(3) . . . . ?
N1 C1 C6 O3 3.1(2) . . . . ?
C2 C1 C6 O3 179.92(18) . . . . ?
O4 C6 O3 Pd -173.10(16) . . . . ?
C1 C6 O3 Pd 10.6(2) . . . . ?
O7 Pd O3 C6 62.5(5) . . . . ?
N1 Pd O3 C6 -14.68(13) . . . . ?
N2 Pd O3 C6 161.69(13) . . . . ?
N1 C1 C2 C3 -1.2(3) . . . . ?
C6 C1 C2 C3 -177.77(18) . . . . ?
C1 C2 C3 C4 3.0(3) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C1 N1 C5 C4 5.3(3) . . . . ?
Pd N1 C5 C4 -164.36(15) . . . . ?
C1 N1 C5 C7 -171.13(17) . . . . ?
Pd N1 C5 C7 19.2(3) . . . . ?
C3 C4 C5 N1 -3.4(3) . . . . ?
C3 C4 C5 C7 172.99(18) . . . . ?
N1 C5 C7 O6 -133.0(2) . . . . ?
C4 C5 C7 O6 50.5(3) . . . . ?
N1 C5 C7 O5 50.2(2) . . . . ?
C4 C5 C7 O5 -126.28(19) . . . . ?
O7 Pd N2 C12 -174.32(18) . . . . ?
O3 Pd N2 C12 12.92(18) . . . . ?
N1 Pd N2 C12 118.0(9) . . . . ?
O7 Pd N2 C8 10.99(13) . . . . ?
O3 Pd N2 C8 -161.77(13) . . . . ?
N1 Pd N2 C8 -56.6(10) . . . . ?
C12 N2 C8 C9 -1.1(3) . . . . ?
Pd N2 C8 C9 174.25(15) . . . . ?
C12 N2 C8 C13 176.15(16) . . . . ?
Pd N2 C8 C13 -8.5(2) . . . . ?
N2 C8 C13 O8 -178.59(18) . . . . ?
C9 C8 C13 O8 -1.4(3) . . . . ?
N2 C8 C13 O7 -1.3(3) . . . . ?
C9 C8 C13 O7 175.98(18) . . . . ?
O8 C13 O7 Pd -172.05(16) . . . . ?
C8 C13 O7 Pd 10.7(2) . . . . ?
O3 Pd O7 C13 88.2(4) . . . . ?
N1 Pd O7 C13 164.46(14) . . . . ?
N2 Pd O7 C13 -12.08(14) . . . . ?
N2 C8 C9 C10 0.0(3) . . . . ?
C13 C8 C9 C10 -177.04(18) . . . . ?
C8 C9 C10 C11 0.9(3) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C8 N2 C12 C11 1.3(3) . . . . ?
Pd N2 C12 C11 -173.05(14) . . . . ?
C8 N2 C12 C14 -176.92(17) . . . . ?
Pd N2 C12 C14 8.7(3) . . . . ?
C10 C11 C12 N2 -0.5(3) . . . . ?
C10 C11 C12 C14 177.74(18) . . . . ?
N2 C12 C14 O10 -119.0(2) . . . . ?
C11 C12 C14 O10 62.7(3) . . . . ?
N2 C12 C14 O9 63.2(2) . . . . ?
C11 C12 C14 O9 -115.1(2) . . . . ?
