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#$Date: 2025-08-21 00:21:57 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301837 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/95/4319527.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_4319527
loop_
_publ_author_name
'Nilkamal Maiti'
'Satyanarayan Pal'
'Surajit Chattopadhyay'
_publ_section_title
;
 Reaction of 2-(Phenylazo)aniline with Na2PdCl4: Formation of a
 2-(Phenylazo)imino Complex of Bivalent Palladium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2204
_journal_page_last               2205
_journal_paper_doi               10.1021/ic000369p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H20 N6 Pd'
_chemical_formula_weight         498.86
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.877(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.2220(11)
_cell_length_b                   14.8034(19)
_cell_length_c                   11.1229(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1019.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2624
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.935
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          1.585
_refine_ls_shift/su_mean         0.353
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²+0.0734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                1672
_reflns_number_total             2322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000369p.cif
_cod_data_source_block           IC000369P
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0734P] 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^)+(0.0451P)^2^+0.0734P] 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               4319527
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_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.0000 0.0000 0.5000 0.03054(10) Uani 1 d S . .
N3 N -0.0062(3) 0.11930(15) 0.41841(19) 0.0382(5) Uani 1 d . . .
H3 H -0.1293 0.1364 0.3837 0.046 Uiso 1 calc R . .
N1 N 0.2585(3) 0.04767(14) 0.60701(17) 0.0331(4) Uani 1 d . . .
N2 N 0.3919(3) 0.11046(14) 0.58494(18) 0.0344(4) Uani 1 d . . .
C1 C 0.3289(4) 0.00022(16) 0.7170(2) 0.0331(5) Uani 1 d . . .
C2 C 0.1813(5) -0.01693(18) 0.7999(3) 0.0408(6) Uani 1 d . . .
H2 H 0.0406 0.0048 0.7860 0.049 Uiso 1 calc R . .
C3 C 0.2439(5) -0.0662(2) 0.9027(2) 0.0495(7) Uani 1 d . . .
H3A H 0.1458 -0.0772 0.9588 0.059 Uiso 1 calc R . .
C4 C 0.4527(5) -0.0993(2) 0.9227(3) 0.0516(7) Uani 1 d . . .
H4 H 0.4938 -0.1339 0.9910 0.062 Uiso 1 calc R . .
C5 C 0.5998(5) -0.0810(2) 0.8412(3) 0.0477(7) Uani 1 d . . .
H5 H 0.7405 -0.1026 0.8555 0.057 Uiso 1 calc R . .
C6 C 0.5397(4) -0.03079(19) 0.7384(2) 0.0373(5) Uani 1 d . . .
H6 H 0.6397 -0.0179 0.6842 0.045 Uiso 1 calc R . .
C7 C 0.3555(4) 0.16720(16) 0.4893(2) 0.0330(5) Uani 1 d . . .
C8 C 0.5304(4) 0.2263(2) 0.4725(2) 0.0409(6) Uani 1 d . . .
H8 H 0.6576 0.2217 0.5238 0.049 Uiso 1 calc R . .
C9 C 0.5159(5) 0.2894(2) 0.3831(3) 0.0471(6) Uani 1 d . . .
H9 H 0.6345 0.3251 0.3704 0.057 Uiso 1 calc R . .
C10 C 0.3187(5) 0.30009(19) 0.3100(3) 0.0466(6) Uani 1 d . . .
H10 H 0.3072 0.3444 0.2504 0.056 Uiso 1 calc R . .
C11 C 0.1461(4) 0.24745(17) 0.3245(2) 0.0404(6) Uani 1 d . . .
H11 H 0.0168 0.2581 0.2770 0.048 Uiso 1 calc R . .
C12 C 0.1572(4) 0.17539(16) 0.4114(2) 0.0337(5) Uani 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'
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 Pd N3 180.0 3_556 . ?
N3 Pd N1 86.32(8) 3_556 3_556 ?
N3 Pd N1 93.68(8) . 3_556 ?
N3 Pd N1 93.68(8) 3_556 . ?
N3 Pd N1 86.32(8) . . ?
N1 Pd N1 180.0 3_556 . ?
C12 N3 Pd 127.40(17) . . ?
N2 N1 C1 111.64(19) . . ?
N2 N1 Pd 128.91(16) . . ?
C1 N1 Pd 118.89(15) . . ?
N1 N2 C7 122.5(2) . . ?
C6 C1 C2 120.2(2) . . ?
C6 C1 N1 120.5(2) . . ?
C2 C1 N1 119.2(2) . . ?
C3 C2 C1 119.8(3) . . ?
C2 C3 C4 120.1(3) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 120.5(3) . . ?
C5 C6 C1 119.4(3) . . ?
N2 C7 C8 114.5(2) . . ?
N2 C7 C12 126.1(2) . . ?
C8 C7 C12 119.3(2) . . ?
C9 C8 C7 121.6(2) . . ?
C8 C9 C10 119.2(3) . . ?
C11 C10 C9 121.5(3) . . ?
C10 C11 C12 121.7(3) . . ?
N3 C12 C7 122.0(2) . . ?
N3 C12 C11 121.5(2) . . ?
C7 C12 C11 116.6(2) . . ?
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
Pd N3 1.984(2) 3_556 ?
Pd N3 1.984(2) . ?
Pd N1 2.0275(19) 3_556 ?
Pd N1 2.0275(19) . ?
N3 C12 1.321(3) . ?
N1 N2 1.286(3) . ?
N1 C1 1.439(3) . ?
N2 C7 1.357(3) . ?
C1 C6 1.387(4) . ?
C1 C2 1.390(4) . ?
C2 C3 1.379(4) . ?
C3 C4 1.385(4) . ?
C4 C5 1.380(4) . ?
C5 C6 1.382(4) . ?
C7 C8 1.424(4) . ?
C7 C12 1.438(3) . ?
C8 C9 1.360(4) . ?
C9 C10 1.410(4) . ?
C10 C11 1.349(4) . ?
C11 C12 1.437(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139133583
