Startseite Naturwissenschaften Crystal structure of bis(N,N,N-trimethylethanaminium) poly[bis(μ2-heptaselenido-κ2Se1,Se7)palladate(II)], C10H28N2PdSe14
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Crystal structure of bis(N,N,N-trimethylethanaminium) poly[bis(μ2-heptaselenido-κ2Se1,Se7)palladate(II)], C10H28N2PdSe14

  • Di Wang , Hoseop Yun und Kang-Woo Kim EMAIL logo
Veröffentlicht/Copyright: 29. September 2017

Abstract

C10H28N2PdSe14, monoclinic, P21/c (no. 14), a = 9.4146(7) Å, b = 14.3446(11) Å, c = 12.4731(9) Å, β = 113.403(2)°, V = 1545.9(2) Å3, Z = 2, Rgt(F) = 0.0510, wRref(F2) = 0.1446, T = 293 K.

CCDC no.:: 1574233

The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Polyhedron, black
Size:0.20 × 0.14 × 0.12 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:17.1 mm−1
Diffractometer, scan mode:Rigaku R-axis Rapid S, ω-scans
2θmax, completeness:27.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:14982, 3526, 0.099
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1710
N(param)refined:136
Programs:Rigaku/MSC [1], SHELX [2], WinGX, ORTEP [3], Diamond [4]
Table 2

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

AtomxyzUiso*/Ueq
Pd11.00000.00001.00000.0560(4)
Se10.25052(13)0.43317(9)0.62469(10)0.0680(4)
Se20.24434(16)0.27134(9)0.61734(12)0.0780(4)
Se30.26159(16)0.21996(9)0.44441(12)0.0829(5)
Se40.52638(16)0.19721(9)0.49111(11)0.0731(4)
Se50.59337(15)0.07442(9)0.62466(10)0.0721(4)
Se60.64013(14)0.14936(9)0.80493(10)0.0681(4)
Se70.90510(14)0.15372(8)0.91797(11)0.0672(4)
N10.7835(13)0.0536(8)0.2355(9)0.082(3)
C10.729(2)0.0734(12)0.3312(14)0.130(6)
H1A0.66320.02350.33550.195*
H1B0.67140.13080.31480.195*
H1C0.81620.07860.40440.195*
C20.885(4)0.124(2)0.232(3)0.115(11)*
H2A0.97310.12650.30550.172*
H2B0.83270.18320.21760.172*
H2C0.91950.11130.17060.172*
C30.650(3)0.056(2)0.1200(18)0.099(9)
H3A0.57790.00750.11730.149*
H3B0.68640.04560.05910.149*
H3C0.59980.11520.10920.149*
C40.850(4)−0.044(2)0.246(2)0.118(12)
H4A0.7696−0.08950.23480.142*
H4B0.8885−0.05340.18480.142*
C50.968(5)−0.056(3)0.353(4)0.19(2)
H5A1.0090−0.11800.35830.291*
H5B0.9300−0.04690.41280.291*
H5C1.0488−0.01160.36260.291*
C2X0.839(7)0.153(4)0.197(5)0.104(17)*
H2X10.87430.14160.13560.156*
H2X20.92110.17980.26280.156*
H2X30.75280.19540.16900.156*
C3X0.684(6)−0.021(4)0.163(5)0.13(2)*
H3X10.7161−0.03630.10060.198*
H3X20.5784−0.00100.13050.198*
H3X30.6936−0.07580.21000.198*
C4X0.958(5)0.014(3)0.292(3)0.069(12)*
H4X11.00050.01990.23310.083*
H4X21.01690.05560.35530.083*
C5X0.995(5)−0.086(3)0.341(4)0.068(13)*
H5X11.1049−0.09590.37330.103*
H5X20.9466−0.13040.27900.103*
H5X30.9562−0.09520.40070.103*
  1. Atoms C2-H5C and the atoms C2X-H5X3 are included with an occupancy of 0.63(3) and 0.36(3), respectively.

Source of material

Na2PdCl4 (0.035 g, 0.12 mmol), Na2Se4 (0.129 g, 0.36 mmol) and EtMe3NI (0.102 g, 0.48 mmol) were charged to a Pyrex tube with diameter of 9 mm under an argon atmosphere and about 0.5 mL MeOH was added. While the solvent was being frozen, the Pyrex tube was evacuated and sealed with the use of a flame. The sealed tube heated at 80 °C for 3 days, then cooled to room temperature. Reddish black polyhedral crystals were isolated by filtration and washed with MeOH and diethyl ether. Crystals of [EtMe3N]2[Pd(Se7)2] were obtained in 27% yield, based on the Pd metal used.

Experimental details

One ethyl group and two methyl groups in the EtMe3N+ cation were refined to be disordered 0.64(3)/0.36(3). H atoms were positioned geometrically and treated as riding, with C—H = 0.97 (CH2) and 0.96 (CH3) Å with Uiso(H) = 1.2 (1.5 for methyl) Ueq(C).

Discussion

Recently (Et2Me2N)2[Pd(Se7)2] has been reported as a new metal polyselenide compound possessing the longest bridging polyselenide anion, Se72− ligand [5]. The title compound (EtMe3N)2[Pd(Se7)2] is another metal polyselenide compound with the bridging Se72− ligand. Actually both (EtMe3N)2[Pd(Se7)2] and (Et2Me2N)2[Pd(Se7)2] are structural analogs containing the [Pd(Se7)2]2− coordination polymer. EtMe3N+ is another unsymmetric alkyl ammonium cation, but smaller than Et2Me2N+. The size difference between EtMe3N+ and Et2Me2N+ does not seem to be large enough to show the counterion effects well manifested in Pd polyselenide compounds [6], [7], [8], [9]. Other ammonium cations of similar size, including Et3MeN+ have been also adopted to stabilize the [Pd(Se7)2]2− anion without success. In the title structure (EtMe3N)2[Pd(Se7)2], the Pd atom is sitting on the special position with the site symmetry 1̄ and the square planar geometry around Pd, coordinated by four bridging heptaselenide ligands, is quite ideal as Se—Pd—Se angles are in the range of 89.29(4)–90.71(4)°. The Pd—Se and Se—Se distances are also typical, ranging from 2.4456(11) to 2.4468(11) Å, and from 2.3230(18) to 2.3704(18) Å, respectively, similar to those found in the other [Pd(Sex)2]2− complexes [5], [6], [9], [10], [11], [12], [13]. In the layers of polymeric [Pd(Se7)2]2−, heptaselenide Se72− ligand chains are connecting Pd metal centers, resulting in 32-membered rings composed of four Pd and 28 Se atoms. The distances between two couples of Pd centers faced diagonally in the 32-membered ring are 14.3446(11) and 17.9874(12) Å, respectively. These distances are 15.1503(14) and 17.6160(13) Å for (Et2Me2N)2[Pd(Se7)2]. A little smaller cation, EtMe3N+ is considered to be responsible for the shrinkage of the 32-membered ring into a little narrower shape and smaller size, compared to the ring with the cation, Et2Me2N+.

Acknowledgement

This work was supported by the Incheon National University Research Grant in 2016.

References

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Received: 2017-5-13
Accepted: 2017-9-13
Published Online: 2017-9-29
Published in Print: 2017-11-27

©2017 Di Wang et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of potassium 1-methyl-1H-1,2,3,4-tetrazole-5-thiolate, C2H3N4SK
  3. Crystal structure of bis(3-(3-ethylureido)-N,N-dimethylpropan-1-aminium) bis (μ3-2-(hydroxymethyl)-2-(oxidomethyl)propane-1,3-bis(olato))-(μ6-oxo)-hexakis(μ2-oxo)-hexaoxo-hexavanadium(V) – dichloromethane (1/1), C27H60Cl2N6O23V6
  4. Crystal structure of bis(μ3-methanolato-κ3O:O:O)-bis(μ2-methanolato-κ2O:O)-dimethanol-bis{6,6′-(1,3-dihydroxyl-2-acetylpropane-1,3-diyl)bis(2-chloro-4-bromophenolato)}tetramanganese(III) C40H40Br4Cl4Mn4O16
  5. Synthesis and crystal structure of tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dibromo-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5)tetramanganese(III), C40H40Br8Mn4O16
  6. Synthesis and crystal structure tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dichloro-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5), tetramanganese(III), C40H40Cl8Mn4O16
  7. Crystal structure of bis{5-methoxy-2-((E)-((4-((E)-1-(methoxyimino)ethyl)phenyl)imino)methyl)phenolato-κ2N,O)}copper(II), C34H34CuN4O6
  8. Crystal structure of (E)-1-(2-hydroxy-3-{[2-hydroxybenzylidene]amino}phenyl)ethan-1-one, C15H13NO3
  9. Crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′′:O′′}tricobalt(II), C44H49Cl2Co3N6O12
  10. Crystal structure of bis{μ2-2,4-dichloro-6-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ5O:O,N,N′,O′}dicobalt(II) acetone solvate, C43H48Br4Co2N6O9
  11. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′:O′}trizinc(II), C44H49Cl2N6O12Zn3
  12. Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2O:O′)trizinc(II), C46H56Zn3N6O14
  13. Crystal structure of tris(cyano-(hydrogen tris(3,5-dimethylpyrazolyl)borate))-iron(III) 4-methoxypyridinium monohydrate, C24H32BN10O2Fe
  14. Synthesis and crystal structure of bis{1-(((4-(1-(hydroxyimino)ethyl)phenyl)imino)methyl)naphthalen-2-olato-κ2O,N}copper(II), C38H30CuN4O4
  15. Crystal structure of (E)-1-(4-{[(E)-2-Hydroxy-1-naphthalenylmethylene] amino}phenyl)ethanone oxime, C19H16N2O2
  16. The pseudosymmetric crystal structure of 2-(2-naphthalenyl)-3-nitro-2H-1-benzopyran, C38H26N2O6
  17. Crystal structure of 2-benzoyl-3-(4-methoxyphenyl)cyclopropane-1,1-dicarbonitrile, C19H14N2O2
  18. N′-(5-ethoxycarbonyl-3,4-dimethyl-pyrrol-2-yl-methylidene)-4-hydroxybenzohydrazide monohydrate, C17H21N3O5
  19. The crystal structure of carbonyl-[4-(2,4-dichlorophenylamino)pent-3-en-2-onato-κ2N,O]-(triphenylphosphine-κP)rhodium(I), RhC30H25Cl2NO2P
  20. Crystal structure of (E)-5-(diethylamino)-2-(((1,1,2-trihydroxyethyl)iminio)methyl)phenolate, C15H24N2O4
  21. Crystal structure of poly[(μ2-1,4-bis((2-ethyl-1H-benzo[d]imidazol-1-yl)methyl)benzene-κ2N:N′)(μ2-isophthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C34H30N4O4Cd
  22. Crystal structure of 5,6-Dihydro-9,10-dimethoxybenzo[g]-1,3-benzodioxolo[5,6-a]chinolizinium 3-(4-hydroxyphenyl)-4-oxo-4H-chromen-7-olate - methanol - water (1/1/1), C36H33NO10
  23. A single crystal study on 2-(methylcarbamoyl)benzoic acid, C9H9NO3
  24. Crystal structure of the salt 1,1′-(ethane-1,2-diyl)bis(1,4-diazabicyclo[2.2.2]octan-1-ium) diperchlorate, C14H28N4(ClO4)2
  25. Crystal structure of 2,5-bis((E)-2-(trifluoromethyl)benzylidene)cyclopentan-1-one, C21H14F6O
  26. Crystal structure of catena-poly[(μ2-benzene-1,4-dicarboxylato-κ2O:O′)-(1-ethyl-6-fluoro-7-(4-methylpiperazin-1-ium-1-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylato-κ2O,O′)zinc(II)] 1.25 hydrate, C25H26.5N3O8.25FZn
  27. Crystal structure of 1-methyl-1,4-diazabicyclo[2.2.2]octan-1-ium poly[aqua-bis(μ2-perchlorato-κ3O,O′:O′′)sodium], C7H17Cl2N2NaO9
  28. Crystal structure of trimethyammonium 2,6-dicarboxyisonicotinate monohydrate, C11H16N2O7
  29. Crystal structure of dodecaguanidinium bis(tetrapropylammonium) heptacarbonate, C43H128N38O21
  30. Crystal structure of poly[tetraaqua-bis(μ6-benzene-1,2,4,5-tetracarboxylato)nickel(II)diyttrium(III)]dihydrate, C20H16NiO22Y2
  31. Halogen bonds and π–π interactions in the crystal structure of 1,3,5-trifluoro-2,4,6-triiodobenzene–N,N-dimethylformamide (1/1), C9H7F3I3NO
  32. Crystal structure of guanidinium tetraethylammonium carbonate dihydrate, C10H30N4O5
  33. The crystal structure of oxonium chlorido-ethylenediaminetetraactetotin(IV) hydrate, C10H17ClN2O10Sn
  34. Crystal structure of 8-((E)-((4-((E)-1-((benzyloxy)imino)ethyl)phenyl)imino)methyl)-7-hydroxy-4-methyl-2H-chromen-2-one, C26H22N2O4
  35. Crystal structure of bis{5-(diethylamino)-2-(((2-oxo-2H-chromen-6-yl)imino)methyl)phenolato-κ2O,N}copper(II), C40H38CuN4O6
  36. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri(p-tolyl)phosphine-κP)rhenium(I), C29H28O5PRe
  37. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(benzyldiphenylphosphine-κP)rhenium(I), C27H24O5PRe
  38. Crystal structure of triethylammonium bis{3-(((3-oxidonaphthalen-1-yl)methylene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}manganese(III), C46H38MnN3O8
  39. Crystal structure of bis(N,N,N-ethyldimethylethanaminium) bis(heptaselenido-κ2Se1,Se7)palladate(II), C12H32N2PdSe14
  40. Crystal structure of bis(4-(1H-pyrazol-5-yl)pyridine-κ2N:N′)-bis(2-(2-((2,6-difluorophenyl)amino)phenyl)acetate-κO)cadmium(II), C44H34N8CdCl4O4
  41. Crystal structure of 4,4′-(1,4-phenylene)bis(pyridin-1-ium) catena-poly[diaqua-bis(μ2-3′,5′-dicarboxy-[1,1′-biphenyl]-2,5-dicarboxylato-κ2O:O′] dihydrate, C48H42O22N2Ca
  42. The crystal structure of (S)-2-benzylsuccinic acid, C11H12O4
  43. Crystal structure of poly[aqua-(μ3-4-(pyridin-4-yl)isophthalato-κ4O,O′:O′′:O′′′)-(μ2-5-carboxy-2-(pyridin-4-yl)benzoato-κ2O:O′)yttrium(III)], C26H17N2O9Y
  44. Crystal structure of ethyl 1-(3,4-dimethylphenyl)-5-methyl-1H-1,2,3-triazole-4-carboxylate, C14H17N3O2
  45. Crystal structure of tetrakis(methanol-κO)-bis{μ2-3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olate-κ4O,N;O′:O′}dizinc(II), C38H38Zn2N2O14
  46. Crystal structure of bromido(4,4′-dimethoxy-2,2′-bipyridine-κ2N,N′)(isopropyl(diphenyl)phosphane-κP)copper(I), C27H29BrCuN2O2P
  47. Crystal structure of bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-9,9-dioctylfluorene, C41H64B2O4
  48. Crystal structure of 11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3-f]pyrido[3,2,1-ij]quinoline-10-carbaldehyde - a julolidine derivative, C16H15NO3
  49. Crystal structure of 1,3-dimethyl-5,5-dibenzylbarbituric acid, C20H20N2O3
  50. Crystal structure of bis(N,N,N-trimethylethanaminium) poly[bis(μ2-heptaselenido-κ2Se1,Se7)palladate(II)], C10H28N2PdSe14
  51. Crystal structure of 1-{4-[(5-Chloro-2-hydroxy-benzylidene)amino]phenyl} ethanone O-ethyl-oxime, C17H17ClN2O2
  52. The crystal structure of methyl N-(4-bromophenyl)carbamate, C8H8BrNO2
  53. Synthesis and crystal structure of 1-{4-[(2-hydroxy-benzylidene)amino]phenyl}ethanone oxime, C15H14N2O2
  54. Crystal structure of 1,1′-butanebis(3-methyl-1H-imidazol-3-ium)bis(hexafluorophosphate), C12H20F12N4P2
  55. (E)-N-benzylidene-3-(benzylthio)-5-p-tolyl-4H-1,2,4-triazol-4-amine, C23H20N4S
  56. Crystal structure of ethyl 5-methyl-1-(pyridin-3-yl)-1H-1,2,3-triazole-4-carboxylate, C11H12N4O2
  57. Crystal structure of 5,5-difluoro-10-(4-fluorophenyl)-1,3,7,9-tetramethyl-5H-4l4,5l4-dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinine - a Z′ = 3 structure, C19H18B2F3N2
  58. The crystal structure of the Matrine derivative: 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one hydrate, C23H29N3O
  59. The crystal structure of tris(μ2-1,3-bis(4,4,4-trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-κ2O,O′)dilutetium(III), C50H38F18Lu2O16
  60. The crystal structure of (Z)-2-(3-(2-(4-chlorobenzoyl)hydrazono)-2-oxoindolin-1-yl) acetic acid, C17H12ClN3O4
  61. Synthesis and crystal structure of trans-tetraqua-bis(2-(((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)ammonio)acetato-κO)cobalt(II) hexahydrate, C36H48CoN2O28S2
  62. The crystal structure of N,N-dimethyl-2,6-di-p-tolylpyrimidin-4-amine, C20H21N3
  63. The crystal structure (E)-4-methyl-N′-(2-nitrobenzylidene)benzenesulfonohydrazide, C14H13N3O4S
  64. Crystal structure of catena-poly[(μ2-1,3-bis(benzimidazol-1-yl)propane κ2N:N′)-(μ2-5-methoxyisophthalato-κ2O:O′)zinc(II)] hydrate, C26H24ZnN4O6
  65. The crystal structure of (E)-N′-(quinolin-2-ylmethylene)furan-2-carbohydrazide monohydrate, C15H13N3O3
  66. Crystal structure of 2,8-diphenyl-3,7,9-trioxa-1-azaspiro[4.5]dec-1-ene, C18H17N1O3
  67. Crystal structure of diethyl 2-(4-chlorophenyl)-1,3-dioxane-5,5-dicarboxylate, C16H19ClO6
  68. Crystal structure of 1-(carboxymethyl)-1H-benzo[d][1,2,3]triazole 3-oxide, C8H7N3O3
  69. Crystal structure of (acetylacetonato-κ2O,O′)-(2-amino-6-chlorobenzoato-κO)-oxido(1,10-phenanthroline-κ2N,N′)vanadium(IV) – trichloromethane (1/1)
  70. Crystal structure of (1E,4E)-1,5-bis(4-chlorophenyl)penta-1,4-dien-3-one, C17H12Cl2O
  71. The crystal structure of trans-dibromido-bis(pyridine-κN)platinum(II), C10H10Br2N2Pt
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