Bis[S-hexyl (E)-3-(4-meth­oxy­benzyl­idene)di­thio­carbazato-κ2N3,S]palladium(II)

Zangrando, E.; Begum, M.S.; Howlader, M.B.H.; Sheikh, M.C.; Miyatake, R.

doi:10.1107/S2414314616005216

metal-organic compounds

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ISSN: 2414-3146

Volume 1| Part 4| April 2016| x160521

doi:10.1107/S2414314616005216

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Bis[S-hexyl (E)-3-(4-methoxybenzylidene)dithiocarbazato-κ²N³,S]palladium(II)

E. Zangrando,^a M. S. Begum,^b M. B. H. Howlader,^c M. C. Sheikh ^d and R. Miyatake ^e ^*

^aDepartment of Chemical and Pharmaceutical Sciences, via Giorgieri 1, 34127, Trieste, Italy, ^bDepartment of Chemistry, Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh, ^cDepartment of Chemistry, Rajshahi University, Rajshahi-6205, Bangladesh, ^dDepartment of Applied Chemistry, Faculty of Engineering, University of Toyama, 3190 Gofuku, Toyama, 930-8555, Japan, and ^eCenter for Environmental Conservation and Research Safety, University of Toyama, 3190 Gofuku, Toyama, 930-8555, Japan
^*Correspondence e-mail: miyatake@ctg.u-toyama.ac.jp

Edited by H. Ishida, Okayama University, Japan (Received 1 March 2016; accepted 28 March 2016; online 5 April 2016)

In the title complex, [Pd(C₁₅H₂₁N₂OS₂)₂], the Pd^II ion is located on a crystallographic inversion center. The two Schiff base ligands in a deprotonated imino thiolate form chelate the metal atom via the azomithine N and thiolate S atoms in a trans-square-planar configuration as imposed by the crystal symmetry. The complex has an approximately planar geometry with the exception of the hexyl chains; the mean plane of the five-membered chelate ring makes a dihedral angle of 15.43 (5)° with the benzene ring. In the crystal, the complex molecules are stacked along the a axis.

Keywords: crystal structure; palladium(II) complex; trans-ligand configuration.

CCDC reference: 1403856

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Chemical scheme

Structure description

The molecular structure of the title compound is illustrated in Fig. 1. In the complex, the Pd—S and Pd—N bond lengths are 2.2949 (5) and 2.0358 (14) Å, respectively, with the S1—Pd1—N1 chelating angle of 83.13 (5)°. These values are in agreement with those observed in similar bis(dithiocarbazato)Pd^II complexes, either with a trans configuration of ligands (Khaledi & Mohd Ali, 2011 ; Tampouris et al., 2007 ; Tarafder et al., 2010 ) or with a cis configuration (Begum, Howlader, Sheikh et al., 2015 ; Ali et al., 2002 ; Liu et al., 2011 ; Duan et al., 1998 ; Tampouris et al., 2007). The ligand recently reported (Begum, Howlader, Miyatake et al., 2015 ) rotates about the C9—N2 bond by 180° in order to allow the N,S chelating behavior towards the metal. Upon coordination some salient features are observed, compared to the free ligand The most significant one is an elongation of the C9—S1 bond length; the C9—S1 distance of 1.7311 (17) Å in the present PdL₂ complex is longer than that of 1.6713 (19) Å in the ligand HL, validating the coordination with the deprotonated thiolate S atom. Correspondingly, the present N2—C9 and N1—N2 bond lengths of 1.284 (3) and 1.411 (3) Å, respectively, are shorter and slightly longer than the values of 1.343 (3) and 1.377 (2) Å in the free ligand. In the crystal, the molecules are stacked along the a axis (Fig. 2).

Figure 1
The molecular structure of the title compound, showing displacement ellipsoids at the 50% probability level [symmetry code: (i) −x, −y, −z].

Figure 2
A packing view of the title compound along the a axis.

Synthesis and crystallization

A solution of PdCl₂ (0.044 g, 0.25 mmol) in 25 ml methanol was added to a solution of S-hexyl (E)-3-(4-methoxybenzylidene)dithiocarbazate (0.155 g, 0.5 mmol) in 10 ml methanol. The resulting mixture was refluxed with constant stirring for 4 h. The orange–red precipitate formed was filtered off, washed with methanol and dried in vacuo over anhydrous CaCl₂. Orange–red single crystals of the title compound suitable for X-ray diffraction were obtained by slow evaporation from a solution in a mixture of dichloromethane and acetonitrile (2:1) (m.p. 457 K).

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1.

Table 1
Experimental details

Crystal data
Chemical formula	[Pd(C₁₅H₂₁N₂OS₂)₂]
M_r	725.33
Crystal system, space group	Triclinic, P $[\overline{1}]$
Temperature (K)	173
a, b, c (Å)	4.54371 (18), 11.6697 (6), 15.5677 (8)
α, β, γ (°)	90.8429 (14), 98.1733 (18), 100.3441 (11)
V (Å³)	803.10 (7)
Z	1
Radiation type	Mo Kα
μ (mm⁻¹)	0.87
Crystal size (mm)	0.20 × 0.09 × 0.02

Data collection
Diffractometer	Rigaku R-AXIS RAPID
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995 )
T_min, T_max	0.891, 0.983
No. of measured, independent and observed [F² > 2σ(F²)] reflections	6642, 2935, 2802
R_int	0.017
(sin θ/λ)_max (Å⁻¹)	0.602

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.057, 1.15
No. of reflections	2935
No. of parameters	189
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −0.23
Computer programs: RAPID-AUTO (Rigaku, 2001 ), SIR92 (Altomare et al., 1993 ), SHELXL97 (Sheldrick, 2008 ), ORTEP-3 for Windows (Farrugia, 2012 ) and publCIF (Westrip, 2010 ).

Structural data

CCDC reference: 1403856

Crystal structure: contains datablocks General, I. DOI: 10.1107/S2414314616005216/is4004sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2414314616005216/is4004Isup2.hkl

checkCIF report

Comment top

ENTER TEXT

Experimental top

Structure description top

The molecular structure of the title compound is illustrated in Fig. 1. In the complex, the Pd—S and Pd—N bond lengths are 2.2949 (5) and 2.0358 (14) Å, respectively, with the S1—Pd1—N1 chelating angle of 83.13 (5)°. These values are in agreement with those observed in similar bis(dithiocarbazato)Pd^II complexes, either with a trans configuration of ligands (Khaledi et al., 2011; Tampouris et al., 2007; Tarafder et al., 2010) or with a cis configuration (Begum, Howlader, Sheikh et al., 2015; Ali et al., 2002; Liu et al., 2011; Duan et al., 1998; Tampouris et al., 2007). The ligand recently reported (Begum, Howlader, Miyatake et al., 2015) rotates about the C9—N2 bond by 180° in order to allow the N,S chelating behavior towards the metal. Upon coordination some salient features are observed, compared to the free ligand The most significant one is an elongation of the C9—S1 bond length; the C9—S1 distance of 1.7311 (17) Å in the present PdL₂ complex is longer than that of 1.6713 (19) Å in the ligand HL, validating the coordination with the deprotonated thiolate S atom. Correspondingly, the present N2—C9 and N1—N2 bond lengths of 1.284 (3) and 1.411 (3) Å, respectively, are shorter and slightly longer than the values of 1.343 (3) and 1.377 (2) Å in the free ligand. In the crystal, the molecules are stacked along the a axis (Fig. 2).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2001); cell refinement: RAPID-AUTO (Rigaku, 2001); data reduction: RAPID-AUTO (Rigaku, 2001); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. The molecular structure of the title compound, showing displacement ellipsoids at the 50% probability level [symmetry code: (i) -x, -y, -z].
	Fig. 2. A packing view of the title compound along the a axis.

Bis[S-hexyl (E)-3-(4-methoxybenzylidene)dithiocarbazato-κ²N³,S]palladium(II) top

Crystal data top

[Pd(C₁₅H₂₁N₂OS₂)₂]	Z = 1
M_r = 725.33	F(000) = 376.00
Triclinic, P1	D_x = 1.500 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71075 Å
a = 4.54371 (18) Å	Cell parameters from 7004 reflections
b = 11.6697 (6) Å	θ = 3.1–27.5°
c = 15.5677 (8) Å	µ = 0.87 mm⁻¹
α = 90.8429 (14)°	T = 173 K
β = 98.1733 (18)°	Platelet, orange
γ = 100.3441 (11)°	0.20 × 0.09 × 0.02 mm
V = 803.10 (7) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	2802 reflections with F² > 2σ(F²)
Detector resolution: 10.000 pixels mm^-1	R_int = 0.017
ω scans	θ_max = 25.3°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −5→5
T_min = 0.891, T_max = 0.983	k = −14→14
6642 measured reflections	l = −18→18
2935 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.057	H-atom parameters constrained
S = 1.15	w = 1/[σ²(F_o²) + (0.0251P)² + 0.3967P] where P = (F_o² + 2F_c²)/3
2935 reflections	(Δ/σ)_max < 0.001
189 parameters	Δρ_max = 0.43 e Å⁻³
0 restraints	Δρ_min = −0.23 e Å⁻³
Primary atom site location: structure-invariant direct methods

Crystal data top

[Pd(C₁₅H₂₁N₂OS₂)₂]	γ = 100.3441 (11)°
M_r = 725.33	V = 803.10 (7) Å³
Triclinic, P1	Z = 1
a = 4.54371 (18) Å	Mo Kα radiation
b = 11.6697 (6) Å	µ = 0.87 mm⁻¹
c = 15.5677 (8) Å	T = 173 K
α = 90.8429 (14)°	0.20 × 0.09 × 0.02 mm
β = 98.1733 (18)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	2935 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2802 reflections with F² > 2σ(F²)
T_min = 0.891, T_max = 0.983	R_int = 0.017
6642 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	0 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.15	Δρ_max = 0.43 e Å⁻³
2935 reflections	Δρ_min = −0.23 e Å⁻³
189 parameters

Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pd1	0.0000	0.0000	0.0000	0.02080 (8)
S1	−0.00459 (11)	−0.13653 (4)	0.10464 (3)	0.02995 (12)
S2	0.36335 (11)	−0.12720 (4)	0.27412 (3)	0.02920 (12)
O1	1.5353 (4)	0.49771 (13)	0.23168 (10)	0.0379 (4)
N1	0.3597 (4)	0.08710 (13)	0.08319 (10)	0.0223 (4)
N2	0.4365 (4)	0.04560 (14)	0.16655 (10)	0.0239 (4)
C1	0.7997 (4)	0.25574 (16)	0.11173 (12)	0.0235 (4)
C2	0.9437 (5)	0.34306 (17)	0.06407 (12)	0.0270 (4)
C3	1.1907 (5)	0.42501 (17)	0.10040 (13)	0.0282 (4)
C4	1.2993 (5)	0.42088 (17)	0.18824 (13)	0.0280 (4)
C5	1.1622 (5)	0.33362 (18)	0.23675 (13)	0.0330 (5)
C6	0.9169 (5)	0.25205 (18)	0.19998 (13)	0.0297 (5)
C7	1.6597 (5)	0.59746 (18)	0.18742 (15)	0.0383 (5)
C8	0.5364 (4)	0.17987 (16)	0.06361 (12)	0.0241 (4)
C9	0.2833 (4)	−0.05543 (16)	0.17755 (11)	0.0229 (4)
C10	0.6641 (5)	−0.02298 (18)	0.33661 (12)	0.0281 (4)
C11	0.5519 (5)	0.07304 (18)	0.38258 (12)	0.0283 (5)
C12	0.8067 (5)	0.15415 (18)	0.44003 (12)	0.0297 (5)
C13	0.6976 (5)	0.24810 (19)	0.48976 (13)	0.0320 (5)
C14	0.9466 (5)	0.32555 (19)	0.55097 (14)	0.0349 (5)
C15	0.8324 (6)	0.4187 (2)	0.59973 (16)	0.0448 (6)
H1	0.8693	0.3465	0.0041	0.0325*
H2	1.2847	0.4832	0.0659	0.0339*
H3	1.2389	0.3300	0.2965	0.0396*
H4	0.8266	0.1930	0.2344	0.0356*
H5	1.5003	0.6415	0.1674	0.0460*
H6	1.7440	0.5720	0.1374	0.0460*
H7	1.8201	0.6472	0.2272	0.0460*
H8	0.4834	0.2032	0.0061	0.0289*
H9	0.7793	−0.0649	0.3805	0.0337*
H10	0.8044	0.0130	0.2973	0.0337*
H11	0.4001	0.0372	0.4187	0.0340*
H12	0.4508	0.1192	0.3386	0.0340*
H13	0.9539	0.1922	0.4033	0.0357*
H14	0.9133	0.1072	0.4821	0.0357*
H15	0.6007	0.2975	0.4475	0.0384*
H16	0.5417	0.2100	0.5238	0.0384*
H17	1.1027	0.3639	0.5171	0.0418*
H18	1.0433	0.2764	0.5936	0.0418*
H19	0.6890	0.3813	0.6368	0.0537*
H20	0.7311	0.4663	0.5580	0.0537*
H21	1.0035	0.4684	0.6358	0.0537*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pd1	0.02019 (11)	0.02079 (12)	0.01926 (11)	−0.00035 (8)	0.00101 (7)	−0.00108 (7)
S1	0.0326 (3)	0.0252 (3)	0.0254 (3)	−0.0065 (2)	−0.00314 (19)	0.00252 (19)
S2	0.0342 (3)	0.0249 (3)	0.0250 (3)	0.0003 (2)	−0.00123 (19)	0.00403 (19)
O1	0.0355 (8)	0.0308 (8)	0.0380 (9)	−0.0094 (7)	−0.0067 (7)	0.0002 (7)
N1	0.0230 (8)	0.0230 (8)	0.0203 (8)	0.0034 (7)	0.0022 (6)	0.0000 (6)
N2	0.0255 (8)	0.0242 (9)	0.0202 (8)	0.0023 (7)	0.0000 (6)	0.0011 (6)
C1	0.0220 (9)	0.0219 (10)	0.0256 (10)	0.0031 (8)	0.0019 (7)	−0.0016 (8)
C2	0.0291 (10)	0.0265 (10)	0.0240 (10)	0.0044 (8)	−0.0005 (8)	0.0005 (8)
C3	0.0278 (10)	0.0241 (10)	0.0316 (11)	0.0012 (8)	0.0046 (8)	0.0026 (8)
C4	0.0242 (9)	0.0227 (10)	0.0343 (11)	0.0013 (8)	−0.0005 (8)	−0.0034 (8)
C5	0.0362 (11)	0.0311 (11)	0.0259 (10)	−0.0019 (9)	−0.0049 (9)	0.0012 (9)
C6	0.0312 (10)	0.0277 (11)	0.0266 (10)	−0.0023 (9)	0.0014 (8)	0.0032 (8)
C7	0.0358 (11)	0.0259 (11)	0.0464 (13)	−0.0089 (9)	0.0019 (10)	−0.0016 (10)
C8	0.0237 (9)	0.0253 (10)	0.0225 (9)	0.0041 (8)	0.0010 (7)	0.0008 (8)
C9	0.0239 (9)	0.0240 (10)	0.0207 (9)	0.0050 (8)	0.0030 (7)	−0.0015 (7)
C10	0.0248 (9)	0.0315 (11)	0.0251 (10)	0.0029 (9)	−0.0029 (8)	0.0030 (8)
C11	0.0241 (9)	0.0353 (11)	0.0236 (10)	0.0024 (9)	0.0008 (8)	0.0008 (8)
C12	0.0246 (9)	0.0371 (12)	0.0250 (10)	0.0019 (9)	0.0002 (8)	0.0011 (9)
C13	0.0273 (10)	0.0373 (12)	0.0285 (11)	0.0024 (9)	−0.0008 (8)	−0.0007 (9)
C14	0.0330 (11)	0.0353 (12)	0.0319 (11)	−0.0007 (9)	−0.0009 (9)	−0.0013 (9)
C15	0.0492 (14)	0.0371 (13)	0.0427 (13)	0.0045 (11)	−0.0062 (11)	−0.0071 (10)

Geometric parameters (Å, º) top

Pd1—S1	2.2949 (5)	C14—C15	1.522 (4)
Pd1—S1ⁱ	2.2949 (5)	C2—H1	0.950
Pd1—N1	2.0358 (14)	C3—H2	0.950
Pd1—N1ⁱ	2.0358 (14)	C5—H3	0.950
S1—C9	1.7311 (17)	C6—H4	0.950
S2—C9	1.7564 (19)	C7—H5	0.980
S2—C10	1.8119 (18)	C7—H6	0.980
O1—C4	1.357 (3)	C7—H7	0.980
O1—C7	1.431 (3)	C8—H8	0.950
N1—N2	1.411 (3)	C10—H9	0.990
N1—C8	1.295 (3)	C10—H10	0.990
N2—C9	1.284 (3)	C11—H11	0.990
C1—C2	1.392 (3)	C11—H12	0.990
C1—C6	1.405 (3)	C12—H13	0.990
C1—C8	1.457 (3)	C12—H14	0.990
C2—C3	1.383 (3)	C13—H15	0.990
C3—C4	1.391 (3)	C13—H16	0.990
C4—C5	1.387 (3)	C14—H17	0.990
C5—C6	1.377 (3)	C14—H18	0.990
C10—C11	1.521 (3)	C15—H19	0.980
C11—C12	1.524 (3)	C15—H20	0.980
C12—C13	1.525 (4)	C15—H21	0.980
C13—C14	1.519 (3)

S1—Pd1—S1ⁱ	180.00 (3)	O1—C7—H5	109.469
S1—Pd1—N1	83.13 (5)	O1—C7—H6	109.467
S1—Pd1—N1ⁱ	96.87 (5)	O1—C7—H7	109.464
S1ⁱ—Pd1—N1	96.87 (5)	H5—C7—H6	109.479
S1ⁱ—Pd1—N1ⁱ	83.13 (5)	H5—C7—H7	109.470
N1—Pd1—N1ⁱ	180.00 (9)	H6—C7—H7	109.477
Pd1—S1—C9	95.72 (7)	N1—C8—H8	113.450
C9—S2—C10	102.89 (9)	C1—C8—H8	113.448
C4—O1—C7	118.18 (16)	S2—C10—H9	108.858
Pd1—N1—N2	120.58 (11)	S2—C10—H10	108.853
Pd1—N1—C8	123.64 (13)	C11—C10—H9	108.859
N2—N1—C8	115.75 (14)	C11—C10—H10	108.849
N1—N2—C9	112.98 (14)	H9—C10—H10	107.706
C2—C1—C6	117.37 (16)	C10—C11—H11	109.100
C2—C1—C8	115.14 (16)	C10—C11—H12	109.105
C6—C1—C8	127.46 (17)	C12—C11—H11	109.106
C1—C2—C3	122.68 (17)	C12—C11—H12	109.103
C2—C3—C4	118.89 (18)	H11—C11—H12	107.845
O1—C4—C3	124.42 (18)	C11—C12—H13	108.895
O1—C4—C5	116.13 (18)	C11—C12—H14	108.898
C3—C4—C5	119.45 (17)	C13—C12—H13	108.898
C4—C5—C6	121.28 (19)	C13—C12—H14	108.893
C1—C6—C5	120.31 (19)	H13—C12—H14	107.732
N1—C8—C1	133.10 (18)	C12—C13—H15	108.748
S1—C9—S2	112.82 (10)	C12—C13—H16	108.753
S1—C9—N2	127.04 (14)	C14—C13—H15	108.757
S2—C9—N2	120.13 (13)	C14—C13—H16	108.759
S2—C10—C11	113.56 (14)	H15—C13—H16	107.646
C10—C11—C12	112.47 (17)	C13—C14—H17	108.973
C11—C12—C13	113.37 (17)	C13—C14—H18	108.975
C12—C13—C14	114.00 (18)	C15—C14—H17	108.977
C13—C14—C15	113.04 (19)	C15—C14—H18	108.973
C1—C2—H1	118.658	H17—C14—H18	107.774
C3—C2—H1	118.661	C14—C15—H19	109.470
C2—C3—H2	120.558	C14—C15—H20	109.468
C4—C3—H2	120.548	C14—C15—H21	109.470
C4—C5—H3	119.366	H19—C15—H20	109.477
C6—C5—H3	119.354	H19—C15—H21	109.472
C1—C6—H4	119.844	H20—C15—H21	109.470
C5—C6—H4	119.851

S1—Pd1—N1—N2	−7.46 (11)	N2—N1—C8—C1	−2.8 (3)
S1—Pd1—N1—C8	170.36 (13)	C8—N1—N2—C9	−170.01 (16)
N1—Pd1—S1—C9	4.28 (5)	N1—N2—C9—S1	−3.2 (3)
S1—Pd1—N1ⁱ—N2ⁱ	−172.54 (11)	N1—N2—C9—S2	175.43 (14)
S1—Pd1—N1ⁱ—C8ⁱ	9.64 (13)	C2—C1—C6—C5	0.9 (3)
N1ⁱ—Pd1—S1—C9	−175.72 (5)	C6—C1—C2—C3	−0.7 (3)
S1ⁱ—Pd1—N1—N2	172.54 (11)	C2—C1—C8—N1	174.9 (2)
S1ⁱ—Pd1—N1—C8	−9.64 (13)	C8—C1—C2—C3	177.76 (17)
N1—Pd1—S1ⁱ—C9ⁱ	175.72 (5)	C6—C1—C8—N1	−6.8 (4)
S1ⁱ—Pd1—N1ⁱ—N2ⁱ	7.46 (11)	C8—C1—C6—C5	−177.33 (18)
S1ⁱ—Pd1—N1ⁱ—C8ⁱ	−170.36 (13)	C1—C2—C3—C4	−0.4 (4)
N1ⁱ—Pd1—S1ⁱ—C9ⁱ	−4.28 (5)	C2—C3—C4—O1	−178.54 (19)
Pd1—S1—C9—S2	179.30 (10)	C2—C3—C4—C5	1.4 (3)
Pd1—S1—C9—N2	−2.01 (17)	O1—C4—C5—C6	178.75 (18)
C9—S2—C10—C11	80.84 (13)	C3—C4—C5—C6	−1.2 (4)
C10—S2—C9—S1	−179.47 (11)	C4—C5—C6—C1	0.0 (4)
C10—S2—C9—N2	1.74 (18)	S2—C10—C11—C12	175.70 (11)
C7—O1—C4—C3	7.6 (3)	C10—C11—C12—C13	−177.57 (14)
C7—O1—C4—C5	−172.30 (17)	C11—C12—C13—C14	176.88 (15)
Pd1—N1—N2—C9	8.0 (2)	C12—C13—C14—C15	179.92 (15)
Pd1—N1—C8—C1	179.34 (14)

Symmetry code: (i) −x, −y, −z.

Experimental details

Crystal data
Chemical formula	[Pd(C₁₅H₂₁N₂OS₂)₂]
M_r	725.33
Crystal system, space group	Triclinic, P1
Temperature (K)	173
a, b, c (Å)	4.54371 (18), 11.6697 (6), 15.5677 (8)
α, β, γ (°)	90.8429 (14), 98.1733 (18), 100.3441 (11)
V (Å³)	803.10 (7)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.87
Crystal size (mm)	0.20 × 0.09 × 0.02

Data collection
Diffractometer	Rigaku R-AXIS RAPID
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.891, 0.983
No. of measured, independent and observed [F² > 2σ(F²)] reflections	6642, 2935, 2802
R_int	0.017
(sin θ/λ)_max (Å⁻¹)	0.602

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.057, 1.15
No. of reflections	2935
No. of parameters	189
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −0.23

Computer programs: RAPID-AUTO (Rigaku, 2001), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 2012), publCIF (Westrip, 2010).

Acknowledgements

MBHH and MSB are grateful to the Department of Chemistry, Rajshahi University, for the provision of laboratory facilities. MCS and RM acknowledge the Department of Applied Chemistry, Faculty of Engineering, University of Toyama, Japan, and Center for Environmental Conservation and Research Safety, University of Toyama, Japan, respectively, for providing funds for single-crystal X-ray analysis.

References

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