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#$Date: 2016-03-25 12:46:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179814 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/10/7011021.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_7011021
loop_
_publ_author_name
'Zbigniew Ciunik'
'Juliusz A. Wolny'
'Mikołaj F. Rudolf'
'Stanisław Wołowiec'
_publ_section_title
;
 cis--trans isomerism and rotational isomerism in triazene-1-oxide
 bis-chelates of palladium(II)
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              885
_journal_page_last               895
_journal_paper_doi               10.1039/b106652h
_journal_year                    2002
_chemical_formula_sum            'C16 H20 N6 O2 Pd'
_chemical_formula_weight         434.78
_space_group_IT_number           2
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                103.96(3)
_cell_angle_beta                 95.80(3)
_cell_angle_gamma                107.42(3)
_cell_formula_units_Z            2
_cell_length_a                   8.223(2)
_cell_length_b                   8.536(2)
_cell_length_c                   14.290(3)
_cell_measurement_temperature    293(2)
_cell_volume                     912.4(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3458
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.039
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_obs          0.0211
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+0.2015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0586
_refine_ls_wR_factor_obs         0.0573
_reflns_number_observed          2929
_reflns_number_total             3215
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106652h.txt
_cod_data_source_block           cmpd_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.2015P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.2015P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7011021
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.05285(2) 0.34580(2) 0.406007(11) 0.03240(7) Uani 1 d . .
O1 O 0.3022(2) 0.4948(2) 0.43937(13) 0.0467(4) Uani 1 d . .
O1' O 0.0573(2) 0.2660(2) 0.52718(12) 0.0432(4) Uani 1 d . .
N1 N 0.3403(3) 0.5692(3) 0.3675(2) 0.0448(5) Uani 1 d . .
N1' N -0.1045(3) 0.1708(3) 0.52923(15) 0.0428(4) Uani 1 d . .
N2 N 0.2279(3) 0.5476(3) 0.29319(15) 0.0434(5) Uani 1 d . .
N2' N -0.2327(3) 0.1281(2) 0.45837(14) 0.0409(4) Uani 1 d . .
N3 N 0.0721(2) 0.4416(3) 0.29153(14) 0.0386(4) Uani 1 d . .
N3' N -0.1910(2) 0.1873(2) 0.38370(14) 0.0377(4) Uani 1 d . .
C1 C -0.0560(3) 0.4284(3) 0.2110(2) 0.0378(5) Uani 1 d . .
C1' C -0.3382(3) 0.1413(3) 0.3074(2) 0.0374(5) Uani 1 d . .
C2 C -0.0425(3) 0.3667(3) 0.1127(2) 0.0463(5) Uani 1 d . .
C2' C -0.3398(3) 0.0415(3) 0.2140(2) 0.0428(5) Uani 1 d . .
C3 C -0.1741(4) 0.3604(4) 0.0409(2) 0.0566(7) Uani 1 d . .
C3' C -0.4854(4) 0.0011(4) 0.1415(2) 0.0559(7) Uani 1 d . .
C4 C -0.3141(4) 0.4084(4) 0.0637(2) 0.0585(7) Uani 1 d . .
C4' C -0.6239(4) 0.0554(4) 0.1617(2) 0.0610(7) Uani 1 d . .
C5 C -0.3270(4) 0.4653(4) 0.1607(2) 0.0527(6) Uani 1 d . .
C5' C -0.6204(4) 0.1544(4) 0.2549(2) 0.0526(6) Uani 1 d . .
C6 C -0.1986(3) 0.4755(3) 0.2339(2) 0.0439(5) Uani 1 d . .
C6' C -0.4766(3) 0.1987(3) 0.3281(2) 0.0445(5) Uani 1 d . .
C7 C 0.1042(5) 0.3051(6) 0.0841(2) 0.0651(8) Uani 1 d . .
C7' C -0.1945(4) -0.0257(4) 0.1910(2) 0.0575(7) Uani 1 d . .
C8 C 0.5145(4) 0.6937(5) 0.3852(3) 0.0650(8) Uani 1 d . .
C8' C -0.1265(5) 0.0987(4) 0.6120(2) 0.0528(6) Uani 1 d . .
H3 H -0.1754(45) 0.3235(45) -0.0172(26) 0.073(10) Uiso 1 d . .
H4 H -0.3961(44) 0.4063(41) 0.0146(24) 0.068(9) Uiso 1 d . .
H5 H -0.4167(43) 0.4904(40) 0.1718(23) 0.064(9) Uiso 1 d . .
H6 H -0.2028(34) 0.5114(34) 0.2996(20) 0.045(7) Uiso 1 d . .
H71 H 0.0950(64) 0.2470(63) 0.0107(39) 0.130(17) Uiso 1 d . .
H72 H 0.1329(59) 0.2412(61) 0.1275(34) 0.118(15) Uiso 1 d . .
H73 H 0.2015(49) 0.3974(49) 0.0987(26) 0.073(11) Uiso 1 d . .
H81 H 0.5126(46) 0.7971(48) 0.4373(28) 0.081(11) Uiso 1 d . .
H82 H 0.5218(47) 0.7353(47) 0.3284(28) 0.077(11) Uiso 1 d . .
H83 H 0.5881(56) 0.6505(52) 0.4100(30) 0.093(14) Uiso 1 d . .
H2' H -0.4711(35) 0.2637(37) 0.3891(21) 0.046(7) Uiso 1 d . .
H3' H -0.4880(42) -0.0708(42) 0.0782(25) 0.068(9) Uiso 1 d . .
H4' H -0.7167(47) 0.0211(43) 0.1098(25) 0.078(10) Uiso 1 d . .
H5' H -0.7105(45) 0.1943(42) 0.2647(23) 0.069(9) Uiso 1 d . .
H71' H -0.2191(62) -0.0846(60) 0.1286(36) 0.118(16) Uiso 1 d . .
H72' H -0.1914(50) -0.0939(52) 0.2233(28) 0.084(13) Uiso 1 d . .
H73' H -0.0810(47) 0.0622(45) 0.2139(24) 0.068(9) Uiso 1 d . .
H81' H -0.0810(45) 0.0144(47) 0.6118(25) 0.075(10) Uiso 1 d . .
H82' H -0.2513(57) 0.0510(52) 0.6078(28) 0.095(13) Uiso 1 d . .
H83' H -0.0742(48) 0.1870(50) 0.6708(28) 0.084(11) Uiso 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
N3 Pd1 N3' 106.67(8) . . ?
N3 Pd1 O1 79.00(8) . . ?
N3' Pd1 O1 174.22(7) . . ?
N3 Pd1 O1' 174.29(7) . . ?
N3' Pd1 O1' 78.99(8) . . ?
O1 Pd1 O1' 95.34(8) . . ?
N1 O1 Pd1 109.32(13) . . ?
N1' O1' Pd1 108.81(13) . . ?
N2 N1 O1 122.9(2) . . ?
N2 N1 C8 120.9(2) . . ?
O1 N1 C8 115.8(2) . . ?
N2' N1' O1' 123.0(2) . . ?
N2' N1' C8' 119.9(2) . . ?
O1' N1' C8' 116.7(2) . . ?
N1 N2 N3 113.9(2) . . ?
N1' N2' N3' 113.8(2) . . ?
N2 N3 C1 113.1(2) . . ?
N2 N3 Pd1 114.9(2) . . ?
C1 N3 Pd1 131.77(15) . . ?
N2' N3' C1' 112.1(2) . . ?
N2' N3' Pd1 114.75(15) . . ?
C1' N3' Pd1 132.54(15) . . ?
C6 C1 C2 120.4(2) . . ?
C6 C1 N3 117.3(2) . . ?
C2 C1 N3 122.2(2) . . ?
C2' C1' C6' 121.5(2) . . ?
C2' C1' N3' 119.4(2) . . ?
C6' C1' N3' 119.1(2) . . ?
C3 C2 C1 117.1(2) . . ?
C3 C2 C7 120.4(3) . . ?
C1 C2 C7 122.5(2) . . ?
C1' C2' C3' 117.4(2) . . ?
C1' C2' C7' 122.3(2) . . ?
C3' C2' C7' 120.3(2) . . ?
C4 C3 C2 122.3(3) . . ?
C4' C3' C2' 121.5(3) . . ?
C3 C4 C5 119.8(3) . . ?
C3' C4' C5' 120.4(3) . . ?
C6 C5 C4 119.7(3) . . ?
C4' C5' C6' 119.5(3) . . ?
C5 C6 C1 120.6(3) . . ?
C5' C6' C1' 119.7(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
Pd1 N3 1.998(2) . ?
Pd1 N3' 1.998(2) . ?
Pd1 O1 1.999(2) . ?
Pd1 O1' 2.009(2) . ?
O1 N1 1.348(3) . ?
O1' N1' 1.344(3) . ?
N1 N2 1.273(3) . ?
N1 C8 1.459(3) . ?
N1' N2' 1.283(3) . ?
N1' C8' 1.463(3) . ?
N2 N3 1.323(3) . ?
N2' N3' 1.320(3) . ?
N3 C1 1.438(3) . ?
N3' C1' 1.432(3) . ?
C1 C6 1.394(3) . ?
C1 C2 1.404(3) . ?
C1' C2' 1.395(3) . ?
C1' C6' 1.399(3) . ?
C2 C3 1.394(4) . ?
C2 C7 1.508(4) . ?
C2' C3' 1.399(4) . ?
C2' C7' 1.504(4) . ?
C3 C4 1.375(4) . ?
C3' C4' 1.383(4) . ?
C4 C5 1.380(4) . ?
C4' C5' 1.387(4) . ?
C5 C6 1.376(4) . ?
C5' C6' 1.388(4) . ?
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
N3 Pd1 O1 N1 -1.16(14) . . . . ?
N3' Pd1 O1 N1 168.3(6) . . . . ?
O1' Pd1 O1 N1 179.69(14) . . . . ?
N3 Pd1 O1' N1' 166.1(6) . . . . ?
N3' Pd1 O1' N1' -6.63(14) . . . . ?
O1 Pd1 O1' N1' 174.53(14) . . . . ?
Pd1 O1 N1 N2 2.1(3) . . . . ?
Pd1 O1 N1 C8 175.0(2) . . . . ?
Pd1 O1' N1' N2' 6.2(3) . . . . ?
Pd1 O1' N1' C8' 179.1(2) . . . . ?
O1 N1 N2 N3 -2.0(3) . . . . ?
C8 N1 N2 N3 -174.5(3) . . . . ?
O1' N1' N2' N3' -0.4(3) . . . . ?
C8' N1' N2' N3' -173.1(2) . . . . ?
N1 N2 N3 C1 175.8(2) . . . . ?
N1 N2 N3 Pd1 0.7(3) . . . . ?
N3' Pd1 N3 N2 -178.6(2) . . . . ?
O1 Pd1 N3 N2 0.3(2) . . . . ?
O1' Pd1 N3 N2 8.8(8) . . . . ?
N3' Pd1 N3 C1 7.5(2) . . . . ?
O1 Pd1 N3 C1 -173.6(2) . . . . ?
O1' Pd1 N3 C1 -165.1(6) . . . . ?
N1' N2' N3' C1' -178.3(2) . . . . ?
N1' N2' N3' Pd1 -5.9(2) . . . . ?
N3 Pd1 N3' N2' -172.2(2) . . . . ?
O1 Pd1 N3' N2' 18.6(8) . . . . ?
O1' Pd1 N3' N2' 7.1(2) . . . . ?
N3 Pd1 N3' C1' -1.7(2) . . . . ?
O1 Pd1 N3' C1' -171.0(6) . . . . ?
O1' Pd1 N3' C1' 177.5(2) . . . . ?
N2 N3 C1 C6 -119.8(2) . . . . ?
Pd1 N3 C1 C6 54.2(3) . . . . ?
N2 N3 C1 C2 61.8(3) . . . . ?
Pd1 N3 C1 C2 -124.3(2) . . . . ?
N2' N3' C1' C2' -119.2(2) . . . . ?
Pd1 N3' C1' C2' 70.1(3) . . . . ?
N2' N3' C1' C6' 61.2(3) . . . . ?
Pd1 N3' C1' C6' -109.4(2) . . . . ?
C6 C1 C2 C3 1.9(3) . . . . ?
N3 C1 C2 C3 -179.7(2) . . . . ?
C6 C1 C2 C7 -176.6(3) . . . . ?
N3 C1 C2 C7 1.8(4) . . . . ?
C6' C1' C2' C3' 0.2(4) . . . . ?
N3' C1' C2' C3' -179.4(2) . . . . ?
C6' C1' C2' C7' -178.2(3) . . . . ?
N3' C1' C2' C7' 2.3(4) . . . . ?
C1 C2 C3 C4 -1.4(4) . . . . ?
C7 C2 C3 C4 177.2(3) . . . . ?
C1' C2' C3' C4' -1.0(4) . . . . ?
C7' C2' C3' C4' 177.4(3) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C2' C3' C4' C5' 1.0(5) . . . . ?
C3 C4 C5 C6 0.8(4) . . . . ?
C3' C4' C5' C6' -0.1(5) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C2 C1 C6 C5 -1.1(4) . . . . ?
N3 C1 C6 C5 -179.6(2) . . . . ?
C4' C5' C6' C1' -0.8(4) . . . . ?
C2' C1' C6' C5' 0.7(4) . . . . ?
N3' C1' C6' C5' -179.7(2) . . . . ?
