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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/7/01/10/7011018.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_7011018
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            'C24 H36 N6 O2 Pd'
_chemical_formula_weight         546.99
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7850(10)
_cell_length_b                   16.359(2)
_cell_length_c                   9.3340(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1326.5(3)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2480
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.730
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.071
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1407P)²+0.3458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1939
_refine_ls_wR_factor_obs         0.1689
_reflns_number_observed          1705
_reflns_number_total             2336
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106652h.txt
_cod_data_source_block           cmpd_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+0.3458P] 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^)+(0.1407P)^2^+0.3458P] 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               7011018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.5000 0.5000 0.5000 0.0322(3) Uani 1 d S .
O1 O 0.3494(4) 0.5865(2) 0.4260(5) 0.0449(10) Uani 1 d . .
N1 N 0.2333(5) 0.5878(3) 0.5071(5) 0.0378(11) Uani 1 d . .
N2 N 0.2314(5) 0.5418(3) 0.6171(5) 0.0383(11) Uani 1 d . .
N3 N 0.3515(6) 0.4927(2) 0.6421(7) 0.0375(12) Uani 1 d . .
C1 C 0.3510(6) 0.4398(3) 0.7655(6) 0.0348(12) Uani 1 d . .
C2 C 0.3086(6) 0.4654(4) 0.8987(7) 0.0376(13) Uani 1 d . .
C3 C 0.2980(6) 0.4067(4) 1.0037(7) 0.0451(15) Uani 1 d . .
C4 C 0.3413(7) 0.3257(4) 0.9821(7) 0.051(2) Uani 1 d . .
H4 H 0.3352 0.2871 1.0539 0.060 Uiso 1 d . .
C5 C 0.3926(7) 0.3028(4) 0.8566(7) 0.0486(15) Uani 1 d . .
H5 H 0.4237 0.2492 0.8440 0.080 Uiso 1 d . .
C6 C 0.3974(6) 0.3591(4) 0.7475(6) 0.0404(13) Uani 1 d . .
H6 H 0.4304 0.3433 0.6617 0.040 Uiso 1 d . .
C21 C 0.2756(8) 0.5548(4) 0.9261(8) 0.051(2) Uani 1 d . .
H211 H 0.3026 0.5664 1.0276 0.080 Uiso 1 d . .
H212 H 0.1669 0.5651 0.8979 0.080 Uiso 1 d . .
H213 H 0.3332 0.5888 0.8710 0.080 Uiso 1 d . .
C31 C 0.2440(10) 0.4292(5) 1.1463(9) 0.073(2) Uani 1 d . .
H311 H 0.1448 0.4544 1.1274 0.080 Uiso 1 d . .
H312 H 0.3163 0.4670 1.1988 0.080 Uiso 1 d . .
H313 H 0.2387 0.3809 1.2037 0.080 Uiso 1 d . .
C7 C 0.1090(6) 0.6487(4) 0.4591(7) 0.0408(13) Uani 1 d . .
C8 C -0.0150(8) 0.6409(5) 0.5578(9) 0.058(2) Uani 1 d . .
H81 H -0.0925 0.6826 0.5319 0.080 Uiso 1 d . .
H82 H 0.0302 0.6484 0.6566 0.080 Uiso 1 d . .
H83 H -0.0630 0.5882 0.5458 0.080 Uiso 1 d . .
C9 C 0.1833(8) 0.7325(4) 0.4704(9) 0.067(2) Uani 1 d . .
H91 H 0.1075 0.7730 0.4354 0.070 Uiso 1 d . .
H92 H 0.2653 0.7339 0.4132 0.070 Uiso 1 d . .
H93 H 0.2232 0.7437 0.5698 0.070 Uiso 1 d . .
C10 C 0.0428(8) 0.6282(5) 0.3022(8) 0.058(2) Uani 1 d . .
H101 H -0.0369 0.6669 0.2681 0.080 Uiso 1 d . .
H102 H -0.0009 0.5741 0.2981 0.080 Uiso 1 d . .
H103 H 0.1223 0.6308 0.2431 0.080 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
O1 Pd1 O1 180.0 . 3_666 ?
O1 Pd1 N3 101.1(2) . 3_666 ?
O1 Pd1 N3 78.9(2) 3_666 3_666 ?
O1 Pd1 N3 78.9(2) . . ?
O1 Pd1 N3 101.1(2) 3_666 . ?
N3 Pd1 N3 179.999(1) 3_666 . ?
N1 O1 Pd1 109.4(3) . . ?
N2 N1 O1 122.8(4) . . ?
N2 N1 C7 122.5(4) . . ?
O1 N1 C7 114.7(4) . . ?
N1 N2 N3 113.3(5) . . ?
N2 N3 C1 114.1(5) . . ?
N2 N3 Pd1 115.6(4) . . ?
C1 N3 Pd1 130.3(4) . . ?
C6 C1 C2 120.3(5) . . ?
C6 C1 N3 115.8(5) . . ?
C2 C1 N3 123.9(5) . . ?
C3 C2 C1 118.2(6) . . ?
C3 C2 C21 120.8(6) . . ?
C1 C2 C21 121.0(6) . . ?
C2 C3 C4 120.3(6) . . ?
C2 C3 C31 120.9(6) . . ?
C4 C3 C31 118.7(6) . . ?
C5 C4 C3 120.9(6) . . ?
C4 C5 C6 120.0(6) . . ?
C5 C6 C1 120.0(5) . . ?
N1 C7 C9 107.1(5) . . ?
N1 C7 C10 107.3(5) . . ?
C9 C7 C10 111.3(6) . . ?
N1 C7 C8 108.4(5) . . ?
C9 C7 C8 111.8(6) . . ?
C10 C7 C8 110.7(5) . . ?
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 O1 1.990(4) . ?
Pd1 O1 1.990(4) 3_666 ?
Pd1 N3 1.997(6) 3_666 ?
Pd1 N3 1.997(6) . ?
O1 N1 1.358(6) . ?
N1 N2 1.275(7) . ?
N1 C7 1.497(7) . ?
N2 N3 1.319(7) . ?
N3 C1 1.442(8) . ?
C1 C6 1.399(8) . ?
C1 C2 1.413(8) . ?
C2 C3 1.385(9) . ?
C2 C21 1.521(10) . ?
C3 C4 1.402(9) . ?
C3 C31 1.523(10) . ?
C4 C5 1.368(9) . ?
C5 C6 1.378(8) . ?
C7 C9 1.515(9) . ?
C7 C10 1.531(9) . ?
C7 C8 1.533(8) . ?
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
O1 Pd1 O1 N1 156.5(294) 3_666 . . . ?
N3 Pd1 O1 N1 177.0(3) 3_666 . . . ?
N3 Pd1 O1 N1 -3.0(3) . . . . ?
Pd1 O1 N1 N2 3.2(6) . . . . ?
Pd1 O1 N1 C7 -178.1(4) . . . . ?
O1 N1 N2 N3 -0.9(8) . . . . ?
C7 N1 N2 N3 -179.6(5) . . . . ?
N1 N2 N3 C1 -179.6(5) . . . . ?
N1 N2 N3 Pd1 -1.9(6) . . . . ?
O1 Pd1 N3 N2 2.8(4) . . . . ?
O1 Pd1 N3 N2 -177.2(4) 3_666 . . . ?
N3 Pd1 N3 N2 -147.3(50) 3_666 . . . ?
O1 Pd1 N3 C1 180.0(5) . . . . ?
O1 Pd1 N3 C1 0.0(5) 3_666 . . . ?
N3 Pd1 N3 C1 29.9(50) 3_666 . . . ?
N2 N3 C1 C6 138.4(5) . . . . ?
Pd1 N3 C1 C6 -38.8(7) . . . . ?
N2 N3 C1 C2 -42.1(8) . . . . ?
Pd1 N3 C1 C2 140.6(5) . . . . ?
C6 C1 C2 C3 -7.0(8) . . . . ?
N3 C1 C2 C3 173.6(5) . . . . ?
C6 C1 C2 C21 172.9(5) . . . . ?
N3 C1 C2 C21 -6.5(8) . . . . ?
C1 C2 C3 C4 5.4(8) . . . . ?
C21 C2 C3 C4 -174.6(5) . . . . ?
C1 C2 C3 C31 -176.5(6) . . . . ?
C21 C2 C3 C31 3.6(9) . . . . ?
C2 C3 C4 C5 -0.9(9) . . . . ?
C31 C3 C4 C5 -179.1(6) . . . . ?
C3 C4 C5 C6 -2.1(10) . . . . ?
C4 C5 C6 C1 0.5(9) . . . . ?
C2 C1 C6 C5 4.1(8) . . . . ?
N3 C1 C6 C5 -176.4(5) . . . . ?
N2 N1 C7 C9 117.8(6) . . . . ?
O1 N1 C7 C9 -60.9(7) . . . . ?
N2 N1 C7 C10 -122.6(6) . . . . ?
O1 N1 C7 C10 58.7(6) . . . . ?
N2 N1 C7 C8 -2.9(7) . . . . ?
O1 N1 C7 C8 178.3(5) . . . . ?
