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Crystal structure of potassium bis(pentaselenido-κ 2 Se 1,Se 5)palladate(II), K2[Pd(Se5)2]

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Published/Copyright: March 27, 2023
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 238 Issue 3

Abstract

K2PdSe10, orthorhombic, Pcma (no. 55), a = 8.293(3) Å, b = 10.987(3) Å, c = 16.432(5) Å, V = 1497.1(8) Å3, Z = 4, R gt(F) = 0.0349, wR ref (F 2) = 0.0688, T = 173(2) K.

CCDC no.: 2247451

Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Black block
Size: 0.17 × 0.10 × 0.10 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 6.0 mm−1
Diffractometer, scan mode: Bruker APEXII, φ and ω
θ max, completeness: 56.6°, >99%
N(hkl) measured , N(hkl) unique, R int: 13239, 9148, 0.025
Criterion for I obs, N(hkl) gt: I obs > 2σ(I obs), 7183
N(param) refined: 686
Programs: Bruker [1], SHELX [2], WinGX [3], Diamond [4]
Table 2:

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

Atom X y z U iso*/U eq
Pd1 0.000000 0.24848 (7) 0.000000 0.01540 (18)
Se1 −0.29166 (9) 0.23077 (7) 0.01754 (4) 0.01795 (18)
Se2 −0.34455 (9) 0.16713 (7) 0.15235 (4) 0.01867 (18)
Se3 −0.17289 (13) 0.000000 0.17631 (6) 0.0205 (3)
Se4 0.03532 (9) 0.26779 (7) 0.14648 (4) 0.01865 (18)
Se5 0.30080 (9) 0.33339 (7) 0.17514 (4) 0.01978 (18)
Se6 0.35360 (13) 0.500000 0.08944 (6) 0.0212 (3)
K1 −0.2224 (3) 0.500000 0.12557 (15) 0.0303 (6)
K2 0.2671 (3) 0.000000 0.11187 (15) 0.0318 (7)

1 Source of material

K2PdCl4 (0.040 g, 0.12 mmol), K2Se4 (0.190 g, 0.48 mmol) and Et3NHCl (0.033 g, 0.24 mmol) were charged to a Pyrex tube with a diameter of 9 mm under an argon atmosphere and about 0.5 mL MeOH was added as a solvent. While the solvent being frozen, the Pyrex tube was evacuated under vacuum and sealed with the use of a flame. The sealed tube was placed in an oven and heated at 80 °C for 3 days, then cooled to room temperature. Black platelet crystals were isolated by filtration and washed with MeOH and diethyl ether several times. Crystals of K2[Pd(Se5)2] were obtained in 26% yield, based on the Pd metal used.

2 Experimental details

2.1 Comment

The title compound, K2[Pd(Se5)2], which has been prepared by the solvothermal reaction of K2PdCl4, K2Se4 and Et3NHCl with methanol as a solvent, is composed of a 1D polymeric [Pd(Se5)2]2− anion and charge-balancing K+ cations. The 1D structure of [Pd(Se5)2]2− is the first example among the members of Pd polyselenide family [Pd(Se x )2]2− (x = 2 − 7) [5], [6], [7], [8], [9], [10], [11], [12], [13], [14]. Actually the chain structure of [Pd(Se5)2]2− is quite unprecedented in the metal polyselenide chemistry [15, 16]. Two independent pairs of symmetrically equivalent Se5 2− bridging ligands connect adjacent Pd(II) atoms alternatively in a helical screw mode to form a chain. So far, the bridging pentaselenide, Se5 2− has been rarely found in compounds such as (H3NCH2CH2NH2)2[Pd(Se5)2], (Ph4P)4[Cu2(Se4)(Se5)2], and (R4E)4[{In(Se4)2}2(μ–Se5)] (R = Ph, E = P; R = Et, Pr, E = N) [7, 17, 18].

The other two compounds containing [Pd(Se5)2]2− anions are (H3NCH2CH2NH2)2[Pd(Se5)2], which has a layered structure of [Pd(Se5)2]2−, and (Et4N)5[2Pd(Se4)2·0.5Pd(Se5)2], which has a 0D molecular [Pd(Se5)2]2− [6, 7]. Compared to the synthetic condition of K2[Pd(Se5)2], use of PdCl2 and water instead of K2 PdCl4 and methanol, respectively, had been reported to yield another K2PdSe10, which is better described as K4[Pd(Se4)2][Pd(Se6)2] [5]. The K4[Pd(Se4)2][Pd(Se6)2] is composed of interpenetrating 3D [Pd(Se4)2]2− and [Pd(Se6)2]2− frameworks. In addition, the methanothermal reaction of K2PdCl4 and K2Se5 in a 1:6 M ratio at 80 °C had been reported to produce K6[Pd(Se5)4] containing a molecular [Pd(Se5)4]4− anion, composed of a Pd(II) metal center and four dangling Se5 2− ligands [7]. When K2Se4 was used in less amount instead of K2Se5, the title compound, K2[Pd(Se5)2] instead of K6[Pd(Se5)4] was produced. Dangling Se5 2− ligands of molecular [Pd(Se5)4]6− anions are supposed to be connected additionally by Pd(II) atoms in excess to form a [Pd(Se5)2]2− chain. For the synthesis of K2[Pd(Se5)2], Et3NH+ organic cations seemed to be necessary at least to yield good enough crystals for single crystal X-ray diffraction study.

For the structure of [Pd(Se5)2]2− in K2[Pd(Se5)2], the square planar geometry around Pd(II), coordinated by four bridging pentaselenide ligands, is quite ideal as Se–Pd–Se angles are in the range of 90.26(2)–90.54(2)°. The Pd–Se and Se–Se distances are also typical, ranging from 2.4339(10) to 2.4435(10) Å, and from 2.3507(11) to 2.3640(12) Å, respectively, similar to those found in the other [Pd(Se x )2]2− complexes [5], [6], [7], [8], [9], [10], [11], [12], [13], [14]. The distances between the adjacent Pd atom centers in the 1D chain structure of [Pd(Se5)2]2− are 5.4601(18) Å and 5.5269(19) Å, respectively. Considering the distances, 8.507 Å, between the Pd atom centers in the 2D layered structure of  [ P d ( S e 5 ) 2 ] 2 − , the bridging Se5 2− ligands need to be much more folded and twisted to fit in the shorter distances for the 1D chain structure of [Pd(Se5)2]2−. Around each of the two K cations in K2[Pd(Se5)2], six Se atoms are present inside the range of 3.9 Å, and the closest Se atoms are Se4(3.346(2) Å) for K1 and Se1(3.315(2) Å) for K2, respectively.

Corresponding author: Kang-Woo Kim, Department of Chemistry, Research Institute for Natural Sciences, Incheon National University, Incheon 22012, Korea, E-mail:

Acknowledgements

This work was supported by the Incheon National University Research Grant in 2018.

  1. Author contribution: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: Incheon National University Research Grant in 2018.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2023-02-21
Accepted: 2023-03-09
Published Online: 2023-03-27
Published in Print: 2023-06-27

© 2023 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ncrs-2023-0081
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of phenyl(3,3-dichloro-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one)methanone, C7H4Cl2N2O
  4. Crystal structure of poly[diaqua-bis(μ 2-1,4-diaminobutane-N:N′)cobalt(II)] dichloride, C8H28Cl2CoN4O2
  5. Synthesis and crystal structure of (4aR,7S)-7-hydroxy-7-isopropyl-1,1-dimethyldecahydro-2H,6H-8a,4a-(epoxymethano)phenanthren-12-one, C20H32O3
  6. The crystal structure of 1-(2-chlorobenzyl)-3-(3,5-dichlorophenyl)urea, C14H11Cl3N2O
  7. Crystal structure of tetrapropylammonium-1,3,5-thiadiazole-5-amido-2-carbamate – 1,2,4-thiadiazole-3,5-diamine – water (1/1/1), C17H37N9O3S2
  8. Tetrabutylammonium 1,3,5-thiadiazole-5-amido-2-carbamate—1,2,4-thiadiazole-3,5-diamine— water (1/1/1), C21H45N9O3S2
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  18. The crystal structure of catena-[nitrato-κ 2 O,O′-(μ 3-3-iodobenzene-1,2-dicarboxylato-κ 4 O:O′:O″,O‴)-(2,2′:6′,2″-terpyridine-κ 3 N,N′,N″)lanthanum(III)], C23H14IN4O7La
  19. Redetermination of crystal structure of [bis(pyridin-2-ylmethyl)amine-κ 3 N,Nʹ,Nʺ]chloridopalladium(II) chloride monohydrate
  20. Crystal structure of catena-poly[triaqua-[bis(m2-4-(1H-1,2,4-triazol-1-yl)benzoato-k2O:O')-(4-(1H-1,2,4-triazol-1-yl)benzoato-k1O)-praseodymium (III) monohydrate], C27H26N9O10Pr
  21. Crystal structure of trans-diaqua-bis(methyl methylcarbamohydrazonothioato-κ2 N,N′) nickel(II) iodide semihydrate, C6H22N6O2NiS2I2·0.5H2O
  22. The crystal structure of 2-(2-fluoro-4-methyl-5-((2,2,2-trifluoroethyl)thio)phenyl)isoindolin-1-one, C17H13F4NOS
  23. The crystal structure of di-μ-1-naphthylacetato-κ 3 O,O′:O;κ 3 O:O,O′-bis[(1-naphthylacetato-κ 2 O,O′)(2,2′-bipyridine-κ 2 N,N′)lead(II)] monohydrate, C68H54N4O9Pb2
  24. Crystal structure of tetrapropylammonium guanidinium 4,4′-sulfonyldibenzoate monohydrate, C27H44N4O7S
  25. Crystal structure of bis(tetrapropylammonium) terephthalate – 1-(diaminomethylene)thiourea – water (1/2/4) C18H40N5O4S
  26. Crystal structure of (E)-7-fluoro-2-(4-morpholinobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C21H20FNO2
  27. The crystal structure of poly[diaqua-bis(μ 3-5-bromobenzene-1,3-dicarboxylato-κ 3 O,O,O′)-(μ 2-1,3-bis-(4-pyridyl)-propane-κ 2 N,N′)-dizinc(II))] – 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
  28. The crystal structure of 2-bromo-1,3-phenylene bis(4-methylbenzenesulfonate), C20H17BrO6S2
  29. Crystal structure of europium dichromium icosaaluminum, EuCr2Al20
  30. The crystal structure of N′1,N′3-di((E)-benzylidene) isophthalohydrazide dihydrate, C 22 H 22 N 4 O 4
  31. Crystal structure of 7α,11α-dihydroxy-15-oxo-ent-kauran-16-en-19,6β-olide, C20H26O5
  32. Crystal structure of 4-chloro-N′-[(1E)-pyridin-3-ylmethylidene]benzohydrazide, C13H10ClN3O
  33. The crystal structure of (Z)-3-(1-(2-((E)-4-isopropylbenzylidene)hydrazinyl)ethylidene) chroman-2,4-dione, C21H20N2O3
  34. Crystal structure of E-7-fluoro-2-(2-(trifluoromethyl)benzylidene)-3,4-dihydronaphthalen-1(2H)-one, C18H12F4O
  35. Crystal structure of bis(6-aminopyridine-2-carboxylato–k2O,N)-bis(N,N-dimethylformamide-k1 O)zinc(II), C18H24N6O6Zn
  36. Crystal structure of 5-(adamantan-1-yl)-3-[(4-{[2-(trifluoromethyl)phenyl]-methyl}piperazin-1-yl)methyl]-1,3,4-oxadiazole-2(3H)-thione, C25H31F3N4OS
  37. Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea – water (2/2/1), C30H72N10O7S2
  38. Crystal structure of tris(2,2′-bipyridine-κ2 N,N′)iron(II) triiodide – dichloromethane (2/1), C61H50Cl2Fe2I12N12
  39. Crystal structure of 2-amino-3-[2-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-ethylideneamino]-but-2-enedinitrile, C17H17N5
  40. The crystal structure of 1-(2-chlorophenyl)-3-cycloheptylurea, C14H19ClN2O
  41. Crystal structure of potassium bis(pentaselenido-κ 2 Se 1,Se 5)palladate(II), K2[Pd(Se5)2]
  42. The crystal structure of 5,10-bis(2-methoxyethyl)-5,10-dihydro-[1,2,3,4]tetrathiocino[5,6-b:8, 7-b′]diindole, C22H22N2O2S4
  43. The crystal structure of 4-(4-iodophenyl)-5H-1,2,3-dithiazole-5-thione, C8H4INS3
  44. Crystal structure of bis{μ2-(4-acetyl-phenoxy)acetato-κ2 O:O′}-bis{μ2-(4-acetyl-phenoxy)acetato-κ3 O,O′:O)- bis{(4-acetyl-phenoxy)acetato-κ2 O,O′}-bis(phenanthrolin-κ2 N,N′)didysprosium(III) tetrahydrate, C84H78N4O28Dy2
  45. Crystal structure of Eu2Pd3.37(1)Zn13.63(1)
  46. Crystal structure of 2-methoxy-4-(methoxy-carbonyl)phenyl 2-chloro-4-fluorobenzoate, C16H12ClFO5
  47. Crystal structure of catena-poly[bis(μ2-dicyanamide-κ2 N:N′)-bis(4-vinylpyridine-κN)-copper(II)], C18H14CuN8
  48. The crystal structure of iguratimod-dimethylformamide (1/1), C17H14N2O6S·C3H7NO
  49. Synthesis and crystal structure of 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO
  50. The crystal structure of diaqua-bis(4-bromo-2-formylphenoxy)zinc(II), C14H12Br2O6Zn
  51. The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
  52. The crystal structure of (E)-N′-(1-(4-fluorophenyl)propylidene)-2-hydroxybenzohydrazide, C16H15FN2O2
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