#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/03/2240338.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_2240338
loop_
_publ_author_name
'Dyakonenko, Viktorita V.'
'Zholob, Olga O.'
'Orysyk, Svitlana I.'
'Pekhnyo, Vasily I.'
_publ_section_title
;
 Crystal structure of
 dichlorido{4-[(E)-(methoxyimino-κN)methyl]-1,3-thiazol-2-amine-κN³}palladium(II)
;
_journal_coeditor_code           WM5096
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m10
_journal_page_last               m11
_journal_paper_doi               10.1107/S2056989014026619
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Pd Cl2 (C5 H7 N3 O S)]'
_chemical_formula_moiety         'C5 H7 Cl2 N3 O Pd S'
_chemical_formula_sum            'C5 H7 Cl2 N3 O Pd S'
_chemical_formula_weight         334.50
_chemical_name_systematic
Dichlorido{4-[(E)-(methoxyimino-κN)methyl]-1,3-thiazol-2-amine-κN³}palladium(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.347(3)
_cell_length_b                   13.583(2)
_cell_length_c                   16.411(3)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    294
_cell_measurement_theta_max      31.6830
_cell_measurement_theta_min      3.7590
_cell_volume                     969.0(7)
_computing_cell_refinement
;
CrysAlis CCD (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis CCD (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis RED (Agilent, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      294
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4284
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Agilent, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' '
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.355
_refine_ls_abs_structure_details
;
Flack (1983), 969 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.39(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0225P)²+0.1807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                2028
_reflns_number_total             2106
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm5096sup1.cf
_cod_data_source_block           I
_cod_database_code               2240338
_cod_database_fobs_code          2240338
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
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_occupancy
Pd Pd1 0.15497(6) 0.986930(16) 0.742144(12) 0.02751(7) Uani d 1
Cl Cl1 -0.1238(2) 1.04846(7) 0.84901(5) 0.0396(2) Uani d 1
Cl Cl2 -0.0192(2) 1.11559(6) 0.66418(5) 0.0411(2) Uani d 1
S S1 0.6968(2) 0.84020(7) 0.53414(5) 0.0394(2) Uani d 1
O O1 0.2794(6) 0.86291(19) 0.88793(12) 0.0379(6) Uani d 1
N N1 0.3271(7) 0.87185(19) 0.80514(14) 0.0306(6) Uani d 1
N N2 0.3996(6) 0.91712(19) 0.65287(15) 0.0291(6) Uani d 1
N N3 0.3636(8) 1.0058(2) 0.53113(15) 0.0489(8) Uani d 1
H H3A 0.2466 1.0498 0.5526 0.059 Uiso calc 1
H H3B 0.4153 1.0104 0.4807 0.059 Uiso calc 1
C C1 0.5024(9) 0.8046(3) 0.92925(18) 0.0389(8) Uani d 1
H H1A 0.4798 0.8132 0.9870 0.058 Uiso calc 1
H H1B 0.7050 0.8249 0.9130 0.058 Uiso calc 1
H H1C 0.4729 0.7366 0.9156 0.058 Uiso calc 1
C C2 0.4954(8) 0.8100(2) 0.76650(18) 0.0328(7) Uani d 1
H H2 0.5819 0.7552 0.7916 0.039 Uiso calc 1
C C3 0.5408(8) 0.8314(2) 0.68133(18) 0.0315(7) Uani d 1
C C4 0.7074(9) 0.7815(3) 0.62715(19) 0.0375(8) Uani d 1
H H4 0.8138 0.7236 0.6379 0.045 Uiso calc 1
C C5 0.4632(8) 0.9318(2) 0.57529(18) 0.0317(7) 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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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
Cl1 Pd1 Cl2 88.54(4)
N1 Pd1 Cl1 94.96(8)
N1 Pd1 Cl2 176.43(8)
N1 Pd1 N2 79.34(10)
N2 Pd1 Cl1 173.65(8)
N2 Pd1 Cl2 97.20(8)
C4 S1 C5 90.16(16)
N1 O1 C1 114.6(2)
O1 N1 Pd1 121.1(2)
C2 N1 Pd1 117.8(2)
C2 N1 O1 121.0(3)
C3 N2 Pd1 112.1(2)
C5 N2 Pd1 137.0(2)
C5 N2 C3 110.9(3)
H3A N3 H3B 120.0
C5 N3 H3A 120.0
C5 N3 H3B 120.0
O1 C1 H1A 109.5
O1 C1 H1B 109.5
O1 C1 H1C 109.5
H1A C1 H1B 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
N1 C2 H2 122.4
N1 C2 C3 115.2(3)
C3 C2 H2 122.4
N2 C3 C2 115.6(3)
C4 C3 N2 116.1(3)
C4 C3 C2 128.3(3)
S1 C4 H4 125.0
C3 C4 S1 110.0(3)
C3 C4 H4 125.0
N2 C5 S1 112.9(2)
N3 C5 S1 121.7(2)
N3 C5 N2 125.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 Cl1 2.2897(10)
Pd1 Cl2 2.2943(9)
Pd1 N1 2.018(3)
Pd1 N2 2.044(3)
S1 C4 1.723(3)
S1 C5 1.742(3)
O1 N1 1.380(3)
O1 C1 1.423(4)
N1 C2 1.282(4)
N2 C3 1.397(4)
N2 C5 1.318(4)
N3 H3A 0.8600
N3 H3B 0.8600
N3 C5 1.313(4)
C1 H1A 0.9600
C1 H1B 0.9600
C1 H1C 0.9600
C2 H2 0.9300
C2 C3 1.441(4)
C3 C4 1.332(5)
C4 H4 0.9300
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
N3 H3A Cl2 . 0.86 2.34 3.124(3) 151.4
N3 H3B Cl1 2_574 0.86 2.48 3.280(3) 155.9
N3 H3B O1 2_574 0.86 2.45 3.015(3) 124.0
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
Pd1 N1 C2 C3 0.1(4)
Pd1 N2 C3 C2 -1.4(4)
Pd1 N2 C3 C4 -179.5(3)
Pd1 N2 C5 S1 179.58(19)
Pd1 N2 C5 N3 -1.1(6)
Cl1 Pd1 N1 O1 -7.0(2)
Cl1 Pd1 N1 C2 176.4(3)
Cl1 Pd1 N2 C3 -25.3(9)
Cl1 Pd1 N2 C5 155.6(5)
Cl2 Pd1 N1 O1 161.6(12)
Cl2 Pd1 N1 C2 -14.9(15)
Cl2 Pd1 N2 C3 -179.7(2)
Cl2 Pd1 N2 C5 1.2(3)
O1 N1 C2 C3 -176.4(3)
N1 Pd1 N2 C3 1.1(2)
N1 Pd1 N2 C5 -178.0(4)
N1 C2 C3 N2 0.9(5)
N1 C2 C3 C4 178.7(4)
N2 Pd1 N1 O1 175.8(3)
N2 Pd1 N1 C2 -0.7(3)
N2 C3 C4 S1 -0.2(4)
C1 O1 N1 Pd1 -156.2(2)
C1 O1 N1 C2 20.2(4)
C2 C3 C4 S1 -178.0(3)
C3 N2 C5 S1 0.5(4)
C3 N2 C5 N3 179.8(3)
C4 S1 C5 N2 -0.5(3)
C4 S1 C5 N3 -179.8(3)
C5 S1 C4 C3 0.4(3)
C5 N2 C3 C2 177.9(3)
C5 N2 C3 C4 -0.2(4)
