Home Physical Sciences Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3
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Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3

  • Kang-Woo Kim EMAIL logo and Man-Young Heo
Published/Copyright: January 29, 2018
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 233 Issue 2

Abstract

C14H36N2Se7Sn3, monoclinic, C2/c (no. 15), a = 23.950(4) Å, b = 13.760(2) Å, c = 20.011(3) Å, β = 114.565(7)°, V = 5997.9(17) Å3, Z = 8, Rgt(F) = 0.0546, wRref(F2) = 0.1393, T = 223 K.

CCDC no.:: 1815879

Parts of the title crystal structure are shown in the figure. Hydrogen atoms are omitted for clarity. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Orange platelet
Size:0.18 × 0.13 × 0.07 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:109.8 cm−1
Diffractometer, scan mode:PHOTON 100 CMOS, φ and ω
2θmax, completeness:57°, >99%
N(hkl)measured, N(hkl)unique, Rint:94011, 7553, 0.096
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 6259
N(param)refined:236
Programs:Bruker programs [1], SHELX [2], ORTEP [3], DIAMOND [4]
Table 2:

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

AtomxyzUiso*/Ueq
Sn10.07732(3)0.44017(5)0.25203(4)0.02088(16)
Sn20.22342(3)0.34304(5)0.25175(4)0.02169(16)
Sn30.20014(3)0.61360(5)0.25293(4)0.02124(16)
Se10.13440(4)0.46558(7)0.15885(5)0.0206(2)
Se20.14803(5)0.29472(8)0.30691(7)0.0286(2)
Se30.12061(5)0.60685(8)0.30734(6)0.0260(2)
Se40.28886(5)0.49279(8)0.30943(6)0.0275(2)
Se50.02808(5)0.42388(9)0.35090(6)0.0277(2)
Se60.31088(5)0.22705(8)0.35065(6)0.0274(2)
Se70.23250(5)0.24958(8)0.14841(6)0.0277(2)
N10.2429(5)0.0233(9)0.4744(6)0.043(3)
N2−0.0209(5)0.7069(8)0.0458(6)0.038(2)
C10.2309(9)−0.0632(17)0.5111(10)0.076(6)
H1A0.2413−0.12120.49200.115*
H1B0.1883−0.06500.50190.115*
H1C0.2555−0.05940.56300.115*
C20.3091(7)0.0229(18)0.4888(11)0.083(7)
H2A0.3187−0.03630.47050.124*
H2B0.33370.02740.54080.124*
H2C0.31770.07730.46460.124*
C30.2271(11)0.1131(17)0.5032(13)0.092(7)
H3A0.18420.11260.49270.138*
H3B0.23610.16850.48020.138*
H3C0.25080.11650.55530.138*
C40.2051(7)0.0157(12)0.3913(8)0.051(4)
H4A0.21800.06690.36750.061*
H4B0.2142−0.04600.37460.061*
C50.1383(10)0.023(2)0.3677(13)0.100(8)
H5A0.1269−0.02110.39770.120*
H5B0.12910.08830.37820.120*
C60.0999(10)0.002(2)0.2921(12)0.093(7)
H6A0.11790.03070.26130.112*
H6B0.05990.03200.27900.112*
C70.0919(14)−0.107(3)0.278(2)0.163(16)
H7A0.0684−0.11890.22650.244*
H7B0.0710−0.13460.30530.244*
H7C0.1316−0.13730.29320.244*
C80.0091(9)0.6204(13)0.0300(10)0.067(5)
H8A0.05150.63460.04240.100*
H8B−0.01120.6046−0.02120.100*
H8C0.00620.56630.05870.100*
C90.0129(8)0.7269(16)0.1266(10)0.072(6)
H9A0.05560.73740.13820.109*
H9B0.00870.67230.15400.109*
H9C−0.00390.78380.13910.109*
C10−0.0856(8)0.6894(17)0.0285(10)0.073(6)
H10A−0.10320.74670.03930.110*
H10B−0.08910.63610.05740.110*
H10C−0.10700.6740−0.02280.110*
C11−0.0089(11)0.7934(15)0.0072(14)0.093(8)
H11A−0.01790.85230.02760.112*
H11B0.03440.79460.01730.112*
C12−0.0446(12)0.7937(16)−0.0716(13)0.090(7)
H12A−0.08420.8231−0.08240.108*
H12B−0.05170.7271−0.08900.108*
C13−0.008(3)0.858(3)−0.121(2)0.21(2)
H13A0.03300.8355−0.10890.252*
H13B−0.03250.8565−0.17360.252*
C14−0.010(3)0.940(3)−0.093(2)0.24(3)
H14A0.00650.9881−0.11500.354*
H14B0.01470.9377−0.04120.354*
H14C−0.05130.9559−0.10260.354*

Source of materials

[CH3COCHC(O)CH3]2SnCl2 (0.020 g, 0.052 mmol), K2Se (0.016 g, 0.10 mmol) and BuMe3NI (0.024 g, 0.10 mmol) were charged to a Pyrex tube with diameter of 9 mm under an argon atmosphere and about 0.5 mL 1:2 (v/v) H2O/MeOH mixture was added as a solvent. While the solvent was 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 110 °C for a day, then cooled to room temperature. Orange red hexagonal plate crystals were isolated by filtration and washed with MeOH and diethyl ether several times. Crystals of (BuMe3N)2[Sn3Se7] were obtained in 61% yield, based on the Sn metal used.

Experimental details

H atoms were positioned geometrically, with C—H = 0.97 (CH2) and 0.96 (CH3) Å with Uiso(H) = 1.2 (1.5 for methyl) Ueq(C). The disorder of the cationic substructure, associated with large ellipsoids even for the carbon atoms, didn’t allow a refinement of the hydrogen atoms nor the refinement of conformation in the case of the methyl groups.

Comment

The title compound, (BuMe3N)2[Sn3Se7], is composed of a 2D layered [Sn3Se7]2− anion and charge-balancing BuMe3N+ cations. (BuMe3N)2[Sn3Se7] is a new member in the family of compounds containing the [Sn3Se7]2− anion and features to be stabilized with a mixed alkyl ammonium cation, BuMe3N+. The cations used to stabilize the [Sn3Se7]2− anion are diverse and can be classified into four different groups: Firstly, alkali metal ions such as Cs+ [5], secondly, organic ammonium cations such as Et4N+, Et3NH+, Pr3NH+, (enH2)2+, NH3(CH2)8NH32+, NH3(CH2)10NH32+ [6], [7], [8], [9], [10], thirdly, metal-amine complex cations such as [Mn(dien)2]2+, [Mn(tatda)]2+, [Fe(tatda)]2+, [Fe(phen)]2+ [11], [12], [13], and fourthly, cations of ionic liquids such as Bzmim+ (Bzmim = 1-benzyl-3-methylimidazolium), prmmim+ (prmmim = 1-propyl-2,3-dimethylimidazolium), bmmim+ (bmmim = 1-butyl-2,3-dimethylimidazolium) [13], [14], [15], [16] have been used as counter cations for the [Sn3Se7]2− anion. Another feature of (BuMe3N)2[Sn3Se7] is that it has been prepared by the use of a Sn(IV) compound and K2Se as reactants instead of elemental Sn and Se. So far, most [Sn3Se7]2− compounds have been prepared by the use of elemental Sn and Se, except a few cases where K2Sn2Se5 or SnSe2 was used as a source of Sn and Se [5, 9, 16].

(BuMe3N)2[Sn3Se7] crystallizes in the space group C2/c. The [Sn3Se7]2− anion in (BuMe3N)2[Sn3Se7] can be depicted as [Sn3Se7]n2n−, considering its 2D polymeric structure. In the layer of [Sn3Se7]n2n−, Sn3Se7 units are interconnected to one another by two edge-sharing μ2-Se atoms to form hexagonal six-membered rings and finally to result in the 2D layer (cf. the figure). The stacking sequences of [Sn3Se7]n2n− layers in [Sn3Se7]2− compounds are either AB or AA. (BuMe3N)2[Sn3Se7] turned out to possess AA stacking of the [Sn3Se7]n2n− layers. The other reported [Sn3Se7]2− compounds with AA stacking of the [Sn3Se7]n2n− layers are Cs2Sn3Se7 and [Emim]5[Sn3Se7]2Cl (Emim = 1-ethyl-3-methylimidazolium) [5, 14] . In the title structure, the Sn—Se distances and the bridging Sn—Se—Sn angles for μ2-Se atoms are in the range of 2.5184(13)–2.7762(12) Å and 88.81(4)−89.31(4)°, respectively. This contribution forms part of our continuing interest in selenidometallates [17].

Acknowledgements

This work was supported by the Incheon National University Research Grant in 2017.

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Received: 2017-8-27
Accepted: 2018-1-9
Published Online: 2018-1-29
Published in Print: 2018-3-28

©2018 Kang-Woo Kim et al., published by De Gruyter, Berlin/Boston

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

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  55. Crystal structure of {5,5′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′}zinc(II), C23H30N4O4Cu
  56. Crystal structure of bis(4-dimethylamino-pyridin-1-ium)tetrafluorosuccinate, C18H22F4N4O4
  57. Crystal structure of dimethyl 3,9-dibenzyl-6,12-dicyclohexyl-3,9-diazahexacyclo [6.4.0.02,7.04,11.05,10]-dodecane-1,11-dicarboxylate, C40H50N2O4
  58. Crystal structure of diethyl 3,9-diphenyl-6,12-bis(3-methoxyphenyl)-3,9-diazahexacyclo[6.4.0.02,7.04,11.05,10]dodecane-1,11-dicarboxylate, C42H42N2O6
  59. Crystal structure of bis(acetato-κO)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)nickel(II), C18H22N4NiO6
  60. Crystal structure of (N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3N,O,O′)-diphenyltin(IV), C28H23FN2O3Sn
  61. Crystal structure of {N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3O,N,O′}dimethyltin(IV), C18H19FN2O3Sn
https://doi.org/10.1515/ncrs-2017-0255
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Articles in the same Issue

  1. Cover and Frontmatter
  2. Crystal structure and optical properties of diaqua-tris(nitrato-κ2O,O′)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl 3-oxide-κN)praseodymium(III), C24H36N9O15Pr
  3. Crystal structure of dimethanol-bis(μ2-methanol-κ2O:O)-bis{3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}dimanganese(II), C38H38Mn2N2O14
  4. Crystal structure of catena-poly[diaqua-bis(μ2-2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κ3O,O′:O′)calcium(II)], C56H48N4Ca2Cl8O12
  5. Crystal structure of catena-poly[triaqua-(isophthalato-κO)-(μ2-1,6-di(1H-imidazol-1-yl)hexane-κ2N:N′)]nickel(II), C20H28N4NiO7
  6. Crystal structure of cyclo[hexaqua-bis[1-[(2-ethyl-1H-imidazol-1-yl) methyl]-1H-benzotriazole-κ2N:N′]-bis(sulfato-κ1O)dicadmium(II)] monohydrate, C24H42Cd2N10O16S2
  7. Crystal Structure of bis(2-fluorbenzoato-κO)-bis(1,10-phenanthroline-κ2N,N′)manganese(II) dihydrate, C38H28F2MnN4O6
  8. Crystal structure of tetrapropylammonium 5-hydroxyisophthalate tetrahydrate, C20H41NO9
  9. Crystal structural of 2-amino-4-(3-bromophenyl)-3-cyano-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydrobenzo[b]pyran, C18H17BrN2O2
  10. Crystal structural of 2-amino-4-(4-methoxyphenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C17H16N2O3
  11. Crystal structure of catena-poly[aqua(μ2-1,3-bis(1H-benzo[d]imidazol-1-yl)propane-κ2N:N′)-(μ2-5-(tert-butyl)isophthalate-κ3O,O′:O′′)nickel(II)], C29H30N4NiO5
  12. Crystal structure of catena-poly[(μ2-dicyanamido-κ2N:N′)-(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O′)copper(II)], C9H8CuN4O
  13. Crystal structure of bis(5,5′-((butane-1,4-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido-k4N,N′,N′′,N′′′)copper(II), C24H32CuN4O4
  14. The crystal structure of the formamide solvate of (17b)-estra-1,3,5(10)-triene-3,17diol, C19H27NO3
  15. Crystal structure of catena-poly[diaqua-bis(μ2-1H-benzo[d]imidazole-5-carboxylato-κ2N:O)nickel(II)] dihydrate, C16H18N4NiO8
  16. Crystal structure of dibromido[(1,2-bis(diisopropylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]nickel(II), C14H38B10NiBr2P2
  17. The crystal structure of catena-poly[aquachlorido(3,3′-([4,4′-bipyridine]-1,1′-diium-1,1′-diylbis(methylene))dibenzoato-κ2O:O′)copper(II)] chloride dihydrate, C26H26Cl2CuN2O7
  18. The crystal structure of N′-(2-nitrobenzylidene)-2-phenylacetohydrazide, C15H13N3O3
  19. Crystal structure of dichlorido bis[1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κ1N]cadmium(II), C30H26CdCl2N10
  20. Crystal structure of aqua-bis(3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole-κ2N,N′)copper(II) sulfate tetrahydrate, C24H28CuN10O9S
  21. Crystal structure of dibromido-carbonyl-(η6-p-cymene)osmium(II), C11H14Br2OOs
  22. Crystal structure of catena-poly[chlorido-(μ2-chlorido)-bis(imidazole-κN)copper(II)] C6H8Cl2CuN4
  23. Crystal structure of [(1,2-bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane-κ2P,P′]dibromidonickel(II)), C26H54B10NiBr2P2
  24. Crystal structure of dichlorido[1,1′-bis(diphenylphosphanyl)ferrocene-κ2P,P′]zinc(II), C34H28FeCl2P2Zn
  25. Crystal structure of tris(μ2-2-(pyridin-2-yl)ethan-1-olato-κ3N,O:O)-trithiocyanato-κN-dicobalt(III), C24H24Co2N6O3S3
  26. The crystal structure of diaqua-2,2′-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))diphenolato-κ4N,N′,O,O′)manganese(III) perchlorate, C20H24MnClN2O4
  27. Crystal structure of bis(μ3-chlorido)-bis(μ2-chlorido)-tetrakis(μ2-2,6-bis (diphenylmethyl)-4-t-butylphenolato)tetralithium(I)dicobalt(II) toluene solvate, C75.5H70Cl2CoLi2O2
  28. The crystal structure of hexaaqua-bis(μ2-3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κ2O:O′)-tetrakis(3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl)propanoato-κO)dierbium(III) octahydrate, C60H76N18O32Er2
  29. Crystal structure of dimethylammonium bis(naphthalene-2,3-diolato)borate, C22H20BNO4
  30. Crystal structure of 2-amino-4-(4-nitro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H17N3O4
  31. The crystal structure of (E)-4-chloro-2-(((5-methylpyridin-2-yl)imino)methyl)phenol, C13H11ClN2O
  32. Crystal structure of bis(N,N,N-trimethylbutanaminium) poly[heptaselenidotristannate(IV)], C14H36N2Se7Sn3
  33. The crystal structure of N-((3,5-di-tert-butyl-4-hydroxyphenyl)(phenyl)methyl)-4-methylbenzenesulfonamide, C28H35N3S
  34. Crystal structure of 2-(4-chlorophenyl)-2,3-dihydro-1H-perimidine, C17H13Cl1N2
  35. The Crystal structure of 2-iodo-1-(p-tolyl)propan-1-one, C10H11IO
  36. Crystal structure of ethyl 1-(4-bromobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17BrN2O2
  37. Crystal structure of ethyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C19H17FN2O2
  38. Crystal structure of catena-poly[diaqua-(μ2-2,5-dihydroxyterephthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C8H8O8Cd
  39. Crystal structure of tetraaqua-bis[6-(1H-imidazol-1-yl-κN)nicotinato]zinc(II), C18H20N6O8Zn
  40. Crystal structure of dichlorido-bis(N-phenyl-2-(quinolin-8-yloxy)acetamide-κ2N,O) – acetone (2/1), C35.5H31N4O4.5Cl2Cu
  41. Crystal Structure of ethyl (E)-3,4-dimethyl-5-((2-(4-methylbenzoyl)hydrazono)methyl)-1H-pyrrole-2-carboxylate — water — ethanol (1/1/1), C20H29N3O5
  42. Crystal structure of 5-((4-(1H-benzo[d]imidazol-2-yl)-2-methoxyphenoxy)methyl)-2-chlorothiazole - trichloromethane - methanol (1/1/1), C20H19Cl4N3O3S
  43. The crystal structure of a matrine derivative: 41S,7aS,12S,13aR,13bR)-12-(4-methylpiperazin-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one, C20H34N4O
  44. Crystal structure of cesium beryllophosphate, Be3Cs2P4O14
  45. Crystal Structure of 3-((3-hydroxybenzyl)ammonio)-3-phenylpropanoate, C16H17NO3
  46. Crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino[3,2-a]isoquinolin-7-ium chloride — 4-hydroxy-3-methoxybenzoic acid — water (2/1/5), C48H54N2Cl2O17
  47. The crystal structure of (1R, 2R)-N1,N2-diferrocenyl-1,2-cyclohexanedicarboxamide, C28H30Fe2N2O2
  48. Crystal structure of N-(2-methylphenyl)ethoxycarbothioamide, C10H13NOS
  49. Crystal Structure of ethyl (E)-2,4-dimethyl-5-((2-tosylhydrazono)methyl)-1H-pyrrole-3-carboxylate monohydrate, C17H23N3O5
  50. Crystal structure of Diiodo-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3N,N′,O)cadium(II) – dimethylformamide (1/1), C19H19N5O2CdI2
  51. Crystal structure of dinitrato-(N′-((quinolin-8-yl)methylene)isonicotinohydrazide κ3-N,N′,O)copper(II), C16H12N6O7Cu
  52. Crystal structure of benzoato-κO-bis(1,3,5-triaza-7-phosphaadamantane-κP)silver(I) monohydrate C19H31AgN6O3P2
  53. Crystal structure of (E)-2-(anthracen-9-ylmethylene)hydrazine-1-carbothioamide, C16H13N3S
  54. The crystal structure of 8-chloro-7-ethyl-1,3-dimethyl-1H-purine-2,6(3H,7H)-dione, C9H11ClN4O2
  55. Crystal structure of {5,5′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′}zinc(II), C23H30N4O4Cu
  56. Crystal structure of bis(4-dimethylamino-pyridin-1-ium)tetrafluorosuccinate, C18H22F4N4O4
  57. Crystal structure of dimethyl 3,9-dibenzyl-6,12-dicyclohexyl-3,9-diazahexacyclo [6.4.0.02,7.04,11.05,10]-dodecane-1,11-dicarboxylate, C40H50N2O4
  58. Crystal structure of diethyl 3,9-diphenyl-6,12-bis(3-methoxyphenyl)-3,9-diazahexacyclo[6.4.0.02,7.04,11.05,10]dodecane-1,11-dicarboxylate, C42H42N2O6
  59. Crystal structure of bis(acetato-κO)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)nickel(II), C18H22N4NiO6
  60. Crystal structure of (N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3N,O,O′)-diphenyltin(IV), C28H23FN2O3Sn
  61. Crystal structure of {N-(3-ethoxy-2-oxidobenzylidene)-4-fluorobenzohydrazonato-κ3O,N,O′}dimethyltin(IV), C18H19FN2O3Sn
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