Startseite Crystal structure of (1,2-dicarba-closo-dodecaborane-1,2-dithiolato κ2S,S′)-bis(1,10-phenanthroline κ2N,N′)zinc(II), C26H26B10Zn4S2
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Crystal structure of (1,2-dicarba-closo-dodecaborane-1,2-dithiolato κ2S,S′)-bis(1,10-phenanthroline κ2N,N′)zinc(II), C26H26B10Zn4S2

  • Yang Liguo EMAIL logo , Wang Xin , Niu Yongsheng , Song Haixiang , Tian Dayong und Gao Linna
Veröffentlicht/Copyright: 10. Dezember 2018

Abstract

C26H26B10Zn4S2, monoclinic, P21/n, a = 14.3766(13) Å, b = 11.6360(11) Å, c = 18.9460(15) Å, β = 104.9630(10)°, V = 3061.9(5) Å3, Z = 4, Rgt(F) = 0.0451, wRref(F2) = 0.0999, T = 298(2) K [1–3].

CCDC no.: 1877320

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:White block
Size:0.27 × 0.21 × 0.13 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.97 mm−1
Diffractometer, scan mode:SMART detector, φ and ω
θmax, completeness:25.0°, >99%
N(hkl)measured, N(hkl)unique, Rint:15258, 5384, 0.062
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2805
N(param)refined:388
Programs:Bruker [1], SHELX [2, 3]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.78564(3)0.29522(4)0.04003(3)0.05495(17)
N10.8058(2)0.1992(3)−0.05845(19)0.0543(8)
N20.8066(2)0.1107(3)0.0727(2)0.0562(9)
N30.7309(3)0.4452(3)−0.03250(16)0.0526(9)
N40.6271(2)0.2699(3)0.00060(17)0.0551(9)
S10.76439(8)0.36279(9)0.15525(6)0.0615(3)
S20.95305(8)0.34981(9)0.06878(6)0.0595(3)
C10.8764(3)0.4242(3)0.1974(2)0.0566(11)
C20.9713(3)0.4174(3)0.1541(2)0.0550(11)
C30.8055(3)0.0681(4)0.1380(3)0.0701(13)
H30.78650.11590.17110.084*
C40.8316(3)−0.0449(4)0.1587(3)0.0791(14)
H40.8267−0.07310.20360.095*
C50.8643(3)−0.1129(4)0.1120(3)0.0843(15)
H50.8842−0.18760.12550.101*
C60.8683(3)−0.0712(4)0.0436(3)0.0667(12)
C70.8376(3)0.0420(3)0.0262(2)0.0547(11)
C80.8372(3)0.0880(4)−0.0440(2)0.0550(11)
C90.8696(3)0.0202(4)−0.0940(3)0.0649(12)
C100.9022(3)−0.0929(4)−0.0741(3)0.0849(16)
H100.9234−0.1381−0.10730.102*
C110.9030(4)−0.1361(4)−0.0086(3)0.0862(16)
H110.9266−0.20990.00340.103*
C120.8650(3)0.0690(5)−0.1625(3)0.0782(14)
H120.88460.0266−0.19770.094*
C130.8320(3)0.1782(4)−0.1775(3)0.0762(14)
H130.82870.2110−0.22290.091*
C140.8031(3)0.2401(4)−0.1240(3)0.0669(12)
H140.78060.3147−0.13500.080*
C150.7833(3)0.5309(4)−0.0483(2)0.0615(12)
H150.85000.5276−0.03110.074*
C160.7419(4)0.6256(4)−0.0899(2)0.0723(14)
H160.78040.6846−0.09960.087*
C170.6451(4)0.6306(4)−0.1159(2)0.0771(15)
H170.61700.6935−0.14350.092*
C180.5870(4)0.5418(4)−0.1016(2)0.0614(12)
C190.6343(3)0.4497(4)−0.0588(2)0.0551(11)
C200.5783(3)0.3562(3)−0.0417(2)0.0498(10)
C210.4783(3)0.3582(4)−0.0681(2)0.0605(12)
C220.4331(4)0.4530(5)−0.1114(3)0.0796(14)
H220.36650.4544−0.12910.095*
C230.4859(4)0.5404(5)−0.1270(2)0.0801(14)
H230.45480.6012−0.15530.096*
C240.4265(3)0.2663(5)−0.0499(2)0.0726(13)
H240.35980.2646−0.06630.087*
C250.4750(4)0.1789(4)−0.0077(2)0.0762(14)
H250.44170.11660.00460.091*
C260.5747(3)0.1846(4)0.0164(2)0.0652(12)
H260.60670.12500.04550.078*
B10.9233(4)0.4192(5)0.2894(3)0.0784(18)
H10.88590.37990.32720.094*
B20.8852(4)0.5497(5)0.2449(3)0.0708(16)
H20.82230.59620.25330.085*
B30.9124(4)0.5450(4)0.1590(3)0.0547(13)
H3A0.86600.58680.11040.066*
B40.9734(4)0.3336(5)0.2300(3)0.0675(15)
H4A0.96700.23940.22750.081*
B50.9946(4)0.5448(6)0.3119(3)0.0891(19)
H5A1.00360.58890.36460.107*
B60.9882(4)0.6230(5)0.2316(3)0.0784(16)
H60.99270.71740.23130.094*
B71.0391(4)0.5380(4)0.1739(3)0.0660(15)
H71.07610.57720.13590.079*
B81.0767(4)0.4073(5)0.2185(3)0.0712(15)
H81.13920.36000.21000.085*
B91.0497(4)0.4094(6)0.3047(3)0.0891(19)
H91.09410.36410.35260.107*
B101.0907(4)0.5355(5)0.2694(3)0.0845(18)
H10A1.16210.57220.29430.101*

Source of material

Solvents, which were employed, were dried with appropriate drying agents and distilled under dinitrogen prior to use. Dichloromethane was used without purification. The 1,2-dithiolato-1,2-dicarba-closo-dodecaborane was prepared according to the literature method [4].

Zn(OAc)2⋅4H2O (54.9 mg, 0.25 mmol) was added to a suspension of 1,2-(Hs)2-1,2-C2B10H10 (55.1 mg, 0.25 mmol) and 1,10-phenanthroline (49.6 mg, 0.25 mmol) in dichloromethane (10 mL). The mixture was stirred for 6 h at room temperature under the protection of dry nitrogen. Then a colourless solution formed. Crystals were obtained by slow evaporation of a dichloromethane-n-hexane solution. (30.4 mg, 22.9%). m.p. 288–289 K. FTIR (KBr) v (cm−l): 2981, 2961, 2921, 2864; 2611, 2601, 2583, 2553.

Experimental details

All H atoms were placed geometrically and treated as riding on their parent atoms, with B—H 1.10, C—H 0.96, with Uiso(H) = 1.2Ueq(B), Uiso(H) = 1.5Ueq(C).

Comment

Transition metal complexes containing chelating 1,2-dicarba-closo-dodecaborane-1,2-dithiolato ligands have attracted interest to take advantage of the unique molecular structure of carborane in recent years [5], [6], [7]. Although there are some mononuclear complexes with carboranyl ligands [8], [9], [10] the zinc complex with the dithiolato ligands has not been reported.

The figure depicts a perspective of the complex showing the atom numbering. The environment of the Zn atom is six coordinated, in which two positions are occupied by the two sulphur atoms, four positions are occupied by the nitrogen atoms of two 1,10-phenanthroline ligand. The bond lengths of Zn1—S1 and Zn1—S2 are 2.413 Å and 2.411 Å, respectively. The bond lengths of Zn1—N1, Zn1—N2, Zn1—N3 and Zn1—N4 are 2.253 Å, 2.233 Å, 2.235 Å and 2.223 Å, respectively.

Acknowledgements

This work was supported by Henan science and technology project (Nos. 172102210161, 172102310166), the Key Scientific Research Projects of Colleges and Universities, Henan Province (Nos. 18A150020) and the Research Fund of Anyang Institute of Technology (Nos. YJJ2016014).

References

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Received: 2018-09-05
Accepted: 2018-11-06
Published Online: 2018-12-10
Published in Print: 2019-03-26

©2019 Yang Liguo et al., published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

  1. Cover and Frontmatter
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  3. Crystal structure of ethyl 2-amino-4-(4-ethoxyphenyl)-5-oxo-4H,5H-pyrano[3,2-c] chromene-3-carboxylate, C23H21NO6
  4. Crystal structure of ethyl 2-amino-4-(4-bromothiophen-2-yl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carboxylate, C16H16BrNO4S
  5. The crystal structure of 6-amino-2-methyl-8-(4-(methylthio)phenyl)-2,3,8,8a-tetrahydroisoquinoline-5,7,7(1H)-tricarbonitrile – ethanol (1/1), C20H19N5S
  6. Crystal structure of 6-amino-8-(4-isopropylphenyl)-2-methyl-2,3,8,8a-tetrahydroisoquinoline-5,7,7(1H)-tricarbonitrile-ethanol (1/1), C24H29N5O
  7. Crystal structure of 1,1′-(ethane-1,2-diyl)bis(3-ethyl-1H-imidazol-3-ium)bis(hexafluorido phosphate), C12H20F12N4P2
  8. Crystal structure of dimethyl (3aS,6R,6aS,7S)-2-pivaloyl-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a1,6a-dicarboxylate, C21H25NO8
  9. Crystal structure of methyl 4-(4-bromothiophen-2-yl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C18H20BrNO3S
  10. Hydrothermal synthesis and crystal structure of catena-poly[bis(4-((pyridin-4-ylmethyl)amino)benzoato-κ3N:O,O′)zinc(II) – 1,2-di(pyridin-4-yl)ethene – water (1/1/1), C38H34N6O5Zn
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  15. Crystal structure of 2-((tert-butyldimethylsilyl)oxy)-5-methylisophthalaldehyde, C15H22O3Si
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  17. Crystal structure of tetrakis(n-butyl)-(μ2-1,2-bis(2-oxidobenzoyl)hydrazine-1,2-diido-κ6N,O,O′:N′,O′′,O′′′)ditin(IV), C30H44N2O4Sn2
  18. Crystal structure of ethyl 2-amino-4-(4-hydroxy-3-methoxyphenyl)-7-methyl-5-oxo-4H,5H-pyrano-[4,3-b]pyran-3-carboxylate, C19H19NO7
  19. Crystal structure of 3-aminopyrazine-2-carbohydrazide, C5H7N5O
  20. Crystal structure of ethanol-bis(N-((5-(ethoxycarbonyl)-3,4-dimethyl-1H-pyrrol-2-yl)methylene)benzohydrazonato-κ2N,O)copper(II), C36H42N6O7Cu
  21. Crystal structure of 3-methyl-2-oxo-2H-chromen-7-yl propionate, C13H12O4
  22. Crystal structure of 2-(dimethylamino)ethyl 4-aminobenzoate, C11H16N2O2
  23. Crystal structure of 3-(benzo[d]thiazol-2-ylamino)isobenzofuran-1(3H)-one, C15H10N2O2S
  24. Crystal structure of 3-((1H-benzo[d]imidazol-2-yl)amino)-2-(1H-benzo[d]imidazol-2-yl)isoindolin-1-one, C22H16N6O
  25. Crystal structure of (2,2′-bipyridine-κ2N,N′)bis(4-(dimethylamino)phenyldiphenylphosphane-κP)copper(I) tetrafluoroborate, C50H48BCuF4N4P2
  26. Crystal structure of citric acid–acetonitrile (1/1), C8H11NO7
  27. Crystal structure of diethyl 2-(4-methoxyphenyl)-1-phenyl-1,2-dihydropyridine-3,5-dicarboxylate, C24H25NO5
  28. The crystal structure of poly[triaqua-bis(μ3-2,5-dihydroxyterephthalato-κ4O,O′:O′′:O′′′)-(μ4-oxalato-κ4O,O′:O′′,O′′′)cerium(III)], C9H10CeO11
  29. Crystal structure of 1-(5-(anthracen-9-yl)-3-(4-hydroxyphenyl)-4,5-dihydro-1H-pyrazol-1-yl)propan-1-one, C26H22N2O2
  30. Synthesis and crystal structure of 5-(8-(((2-carboxyethyl)ammonio)methyl)-7-hydroxy-4-oxo-4H-chromen-3-yl)-2-hydroxybenzenesulfonate trihydrate, C19H23NO12S
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  32. Crystal structure of 1-((R)-(2′-(dimethylamino)-[1,1′-binaphthalen]-2-yl))-3-((S)-2-hydroxy-1-phenylethyl)thiourea, C31H29N3OS
  33. Crystal structure and photochemical property of 1,8-bis(p-tolylthio)pyrene, C30H22S2
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  37. Bis(ethanol-κO)-bis(6-aminopicolinato-κ2N,O)magnesium(II), C16H22O6N4Mg
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  55. Crystal structure of (4S,4aS,6aR,6bR,12aS,12bR,14aS,14bR)-3,3,6a,6b,9,9,12a-heptamethyloctadecahydro-1H,3H-4,14b-ethanophenanthro[1,2-h]isochromene, C30H50O
  56. Crystal structure of (E)-4-((2-fluoro-3-(trifluoromethyl)benzylidene)amino)-3-methyl-1H-1,2,4-triazole-5(4H)-thione, C11H8F4N4S
  57. Crystal structure of 5-(4-fluorophenyl)-4-methyl-2,4-dihydro-3H-1,2,4-triazole-3-thione, C9H8FN3S
  58. Crystal structure of catena-poly[(1-(4-fluorophenyl)-N–(5-((trimethylstannyl)thio)-1,3,4-thiadiazol-2-yl)methanimine], (C12H14FN3S2Sn)n
  59. The crystal structure of 4-(methoxycarbonyl)benzoic acid, C9H8O4
  60. The crystal structure of N,N′-(6-(thiophen-2-yl)-1,3,5-triazine-2,4-diyl)bis(2-methylpropane-2-sulfonamide) – ethyl acetate(2/1), C34H54N10O6S6
  61. Crystal structure of N′-(1-(2-hydroxyphenyl)ethylidene)-5-methyl-1-phenyl-1H-1,2,3-triazole-4-carbohydrazide, C18H17N5O2
  62. Crystal structure of 3-(4-methoxyphenyl)-1-phenylprop-2-yn-1-one, C16H12O2
  63. Crystal structure of N′-(1-(benzofuran-2-yl)ethylidene)-2-cyanoacetohydrazide, C13H11N3O2
  64. Crystal structure of hexa-μ2-chlorido-μ4-oxido-tetrakis(1-vinyl-1H-imidazole-κN)tetracopper(II), C20H24Cu4Cl6N8O
  65. Crystal structure of N′-((1E,2E)-4-(7-methoxy-2-oxo-2H-chromen-8-yl)-2-methylbut-2-en-1-ylidene)-4-methylbenzenesulfonohydrazide, C22H22O5N2S
  66. Crystal structure of 2-acetyl pyrene, C18H12O
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