#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/56/2215672.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_2215672
loop_
_publ_author_name
'Li, Ya-Min'
'Zhao, Xiao-Wei'
'Zhang, Jing-Lai'
_publ_section_title
;
 Bis(di-2-pyridylmethanediol-κ²N,N')palladium(II)
 bis(perchlorate)
;
_journal_coeditor_code           SJ2361
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2585
_journal_page_last               m2585
_journal_paper_doi               10.1107/S1600536807045722
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pd (C11 H10 N2 O2)2] (Cl O4)2'
_chemical_formula_moiety         'C22 H20 N4 O4 Pd 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C22 H20 Cl2 N4 O12 Pd'
_chemical_formula_weight         709.72
_chemical_name_systematic
;
Bis(di-2-pyridylmethanediol-κ²N,N')palladium(II) bis(perchlorate)
;
_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                 99.008(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.677(3)
_cell_length_b                   13.929(5)
_cell_length_c                   12.173(5)
_cell_measurement_reflns_used    2779
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0585
_cell_volume                     1285.6(9)
_computing_cell_refinement       'CrystalClear (Rigaku, 2000)'
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalClear (Rigaku, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9661
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.596
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0431P)²+1.6859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                2518
_reflns_number_total             2925
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj2361.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_cell_volume        1285.7(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2215672
_cod_database_fobs_code          2215672
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_type_symbol
_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
Pd Pd1 0.0000 0.5000 0.0000 0.03376(13) Uani d S 1
Cl Cl1 -0.15333(17) 0.38024(9) -0.41355(9) 0.0642(3) Uani d . 1
C C1 0.3177(5) 0.4007(3) -0.0473(3) 0.0456(9) Uani d . 1
H H1A 0.2952 0.3615 0.0107 0.055 Uiso calc R 1
C C2 0.4601(5) 0.3814(3) -0.0988(4) 0.0582(11) Uani d . 1
H H2A 0.5330 0.3293 -0.0767 0.070 Uiso calc R 1
C C3 0.4931(6) 0.4395(4) -0.1826(4) 0.0671(13) Uani d . 1
H H3A 0.5887 0.4270 -0.2189 0.081 Uiso calc R 1
C C4 0.3849(6) 0.5173(4) -0.2141(4) 0.0594(12) Uani d . 1
H H4A 0.4081 0.5579 -0.2707 0.071 Uiso calc R 1
C C5 0.2432(5) 0.5337(3) -0.1610(3) 0.0433(8) Uani d . 1
C C6 0.1147(6) 0.6181(3) -0.1892(3) 0.0490(9) Uani d . 1
C C7 0.0762(5) 0.6930(3) 0.0970(3) 0.0459(9) Uani d . 1
H H7A 0.0411 0.6648 0.1592 0.055 Uiso calc R 1
C C8 0.1333(6) 0.7865(3) 0.1033(4) 0.0560(11) Uani d . 1
H H8A 0.1390 0.8210 0.1692 0.067 Uiso calc R 1
C C9 0.1817(6) 0.8280(3) 0.0109(4) 0.0633(12) Uani d . 1
H H9A 0.2187 0.8916 0.0132 0.076 Uiso calc R 1
C C10 0.1758(6) 0.7757(3) -0.0853(4) 0.0543(10) Uani d . 1
H H10A 0.2097 0.8034 -0.1482 0.065 Uiso calc R 1
C C11 0.1187(5) 0.6813(3) -0.0876(3) 0.0410(8) Uani d . 1
N N1 0.2095(4) 0.4751(2) -0.0785(2) 0.0378(7) Uani d . 1
N N2 0.0696(4) 0.6408(2) 0.0028(2) 0.0376(6) Uani d . 1
O O1 -0.0599(4) 0.5845(2) -0.2184(2) 0.0600(8) Uani d . 1
H H1B -0.0597 0.5349 -0.2546 0.090 Uiso calc R 1
O O2 0.1675(5) 0.6744(2) -0.2722(3) 0.0781(11) Uani d . 1
H H2B 0.1414 0.6475 -0.3325 0.117 Uiso calc R 1
O O3 -0.2926(7) 0.4402(4) -0.4044(7) 0.164(3) Uani d . 1
O O4 -0.1980(10) 0.2889(3) -0.3818(5) 0.166(3) Uani d . 1
O O5 -0.0060(6) 0.4159(3) -0.3402(3) 0.0981(13) Uani d . 1
O O6 -0.1158(11) 0.3796(8) -0.5176(4) 0.236(5) Uani d . 1
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Pd1 N1 . 3_565 180.0
N1 Pd1 N2 . 3_565 93.03(12)
N1 Pd1 N2 3_565 3_565 86.97(12)
N1 Pd1 N2 . . 86.97(12)
N1 Pd1 N2 3_565 . 93.03(12)
N2 Pd1 N2 3_565 . 180.0
O6 Cl1 O3 . . 111.4(6)
O6 Cl1 O4 . . 110.8(5)
O3 Cl1 O4 . . 107.8(4)
O6 Cl1 O5 . . 109.2(4)
O3 Cl1 O5 . . 106.9(4)
O4 Cl1 O5 . . 110.7(3)
N1 C1 C2 . . 121.6(4)
N1 C1 H1A . . 119.2
C2 C1 H1A . . 119.2
C3 C2 C1 . . 118.9(4)
C3 C2 H2A . . 120.6
C1 C2 H2A . . 120.6
C2 C3 C4 . . 120.1(4)
C2 C3 H3A . . 120.0
C4 C3 H3A . . 120.0
C5 C4 C3 . . 119.2(4)
C5 C4 H4A . . 120.4
C3 C4 H4A . . 120.4
N1 C5 C4 . . 120.6(4)
N1 C5 C6 . . 115.9(3)
C4 C5 C6 . . 123.5(4)
O2 C6 O1 . . 112.2(3)
O2 C6 C11 . . 107.1(3)
O1 C6 C11 . . 107.2(3)
O2 C6 C5 . . 110.1(4)
O1 C6 C5 . . 110.7(3)
C11 C6 C5 . . 109.4(3)
N2 C7 C8 . . 121.8(4)
N2 C7 H7A . . 119.1
C8 C7 H7A . . 119.1
C9 C8 C7 . . 118.7(4)
C9 C8 H8A . . 120.6
C7 C8 H8A . . 120.6
C8 C9 C10 . . 120.0(4)
C8 C9 H9A . . 120.0
C10 C9 H9A . . 120.0
C9 C10 C11 . . 119.3(4)
C9 C10 H10A . . 120.4
C11 C10 H10A . . 120.4
N2 C11 C10 . . 120.7(4)
N2 C11 C6 . . 116.9(3)
C10 C11 C6 . . 122.3(4)
C1 N1 C5 . . 119.6(3)
C1 N1 Pd1 . . 120.0(3)
C5 N1 Pd1 . . 120.4(3)
C11 N2 C7 . . 119.4(3)
C11 N2 Pd1 . . 119.9(2)
C7 N2 Pd1 . . 120.6(3)
C6 O1 H1B . . 109.5
C6 O2 H2B . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 N1 . 2.025(3)
Pd1 N1 3_565 2.025(3)
Pd1 N2 3_565 2.031(3)
Pd1 N2 . 2.031(3)
Cl1 O6 . 1.342(5)
Cl1 O3 . 1.375(5)
Cl1 O4 . 1.389(5)
Cl1 O5 . 1.416(4)
C1 N1 . 1.345(5)
C1 C2 . 1.370(6)
C1 H1A . 0.9300
C2 C3 . 1.357(7)
C2 H2A . 0.9300
C3 C4 . 1.382(7)
C3 H3A . 0.9300
C4 C5 . 1.370(6)
C4 H4A . 0.9300
C5 N1 . 1.351(5)
C5 C6 . 1.538(6)
C6 O2 . 1.389(5)
C6 O1 . 1.411(5)
C6 C11 . 1.515(5)
C7 N2 . 1.352(4)
C7 C8 . 1.373(6)
C7 H7A . 0.9300
C8 C9 . 1.366(7)
C8 H8A . 0.9300
C9 C10 . 1.374(6)
C9 H9A . 0.9300
C10 C11 . 1.385(5)
C10 H10A . 0.9300
C11 N2 . 1.342(5)
O1 H1B . 0.8200
O2 H2B . 0.8200
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1B O5 . 0.82 2.03 2.842(5) 168.5
O2 H2B O6 3_564 0.82 1.84 2.636(6) 162.1
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139073238
