Startseite The crystal structure of bis(3-oxo-1,3-diphenylprop-1-en-1-olato-κ 2 O:O′)-bis(1,4-dioxane-κ 1 O)nickel(II), C38H38O8Ni
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The crystal structure of bis(3-oxo-1,3-diphenylprop-1-en-1-olato-κ 2 O:O′)-bis(1,4-dioxane-κ 1 O)nickel(II), C38H38O8Ni

  • Fanzhi Wei ORCID logo EMAIL logo
Veröffentlicht/Copyright: 3. September 2024

Abstract

C38H38O8Ni, orthorhombic, Cmc21 (no. 36), a = 19.0266(4) Å, b = 8.2409(2) Å, c = 21.4315(5) Å, V = 3,360.38(13) Å3, Z = 4, Rgt (F) = 0.0406, wRref (F 2) = 0.1058, T = 293 K.

CCDC no.: 2344706

The molecular structure is shown in the figure. 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: Colourless needle
Size: 0.16 × 0.06 × 0.05 mm
Wavelength: Cu Kα radiation (1.54184 Å)
μ: 1.27 mm−1
Diffractometer, scan mode: XtaLAB Synergy, ω
θ max, completeness: 73.8°, >99 %
N(hkl)measured, N(hkl)unique, R int: 15,013, 3,348, 0.071
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 3,133
N(param)refined: 223
Programs: CrysAlisPRO, 1 Olex2, 2 SHELX 3 , 4
Table 2:

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

Atom x y z U iso*/U eq
C1 0.500000 0.6348 (5) 0.3927 (2) 0.0429 (10)
H1 0.500000 0.708002 0.359638 0.051*
C2 0.56557 (16) 0.5844 (4) 0.41536 (15) 0.0387 (7)
C3 0.62979 (16) 0.6661 (3) 0.38993 (16) 0.0395 (6)
C4 0.68599 (18) 0.6977 (4) 0.42930 (19) 0.0487 (7)
H4 0.684163 0.664307 0.470718 0.058*
C5 0.74455 (19) 0.7783 (6) 0.4075 (2) 0.0603 (10)
H5 0.781390 0.801260 0.434585 0.072*
C6 0.7490 (2) 0.8251 (5) 0.3459 (3) 0.0619 (12)
H6 0.788757 0.878914 0.331384 0.074*
C7 0.6942 (2) 0.7914 (5) 0.3061 (2) 0.0582 (9)
H7 0.697130 0.821415 0.264319 0.070*
C8 0.63444 (18) 0.7129 (5) 0.32792 (18) 0.0499 (8)
H8 0.597393 0.691593 0.300824 0.060*
C9 0.500000 0.0504 (6) 0.5974 (2) 0.0422 (9)
H9 0.500001 −0.026990 0.628960 0.051*
C10 0.43437 (16) 0.1036 (4) 0.57561 (15) 0.0372 (6)
C11 0.37038 (15) 0.0180 (3) 0.59904 (15) 0.0378 (6)
C12 0.36529 (17) −0.0382 (5) 0.65994 (17) 0.0468 (7)
H12 0.402406 −0.022596 0.687534 0.056*
C13 0.3050 (2) −0.1174 (6) 0.67972 (19) 0.0578 (9)
H13 0.301527 −0.153223 0.720755 0.069*
C14 0.2504 (2) −0.1432 (6) 0.6390 (2) 0.0598 (11)
H14 0.210574 −0.198902 0.652337 0.072*
C15 0.25422 (18) −0.0871 (5) 0.5785 (2) 0.0574 (9)
H15 0.216916 −0.103690 0.551219 0.069*
C16 0.31385 (16) −0.0059 (4) 0.55856 (18) 0.0478 (7)
H16 0.316241 0.033071 0.517886 0.057*
C17 0.5619 (3) 0.5603 (6) 0.6056 (3) 0.0713 (12)
H17A 0.563937 0.677699 0.602844 0.086*
H17B 0.603186 0.516165 0.585230 0.086*
C18 0.5606 (4) 0.5095 (11) 0.6723 (3) 0.102 (2)
H18A 0.562238 0.391990 0.674648 0.122*
H18B 0.601921 0.551708 0.693248 0.122*
C19 0.4382 (2) 0.1224 (6) 0.3919 (2) 0.0628 (10)
H19A 0.396838 0.176140 0.408461 0.075*
H19B 0.436073 0.008797 0.403577 0.075*
C20 0.4393 (3) 0.1375 (8) 0.3226 (3) 0.0808 (14)
H20A 0.397283 0.088154 0.305269 0.097*
H20B 0.439436 0.251296 0.311029 0.097*
Ni1 0.500000 0.34709 (8) 0.49657 (4) 0.0366 (2)
O1 0.57604 (11) 0.4791 (3) 0.45726 (11) 0.0449 (5)
O2 0.42402 (11) 0.2140 (3) 0.53588 (11) 0.0435 (5)
O3 0.500000 0.5024 (5) 0.5755 (2) 0.0607 (10)
O4 0.500000 0.5655 (12) 0.7030 (3) 0.128 (3)
O5 0.500000 0.1946 (5) 0.41744 (19) 0.0568 (10)
O6 0.500000 0.0599 (8) 0.2973 (3) 0.0931 (17)

1 Source of materials

1,3-diphenylpropane-1,3-dione (0.02 mol, 4.485 g) was dissolved in hot ethanol (48 ml) and nickel(II) acetate tetrahydrate (0.01 mol, 2.488 g) were mixed with ethanol (16 ml). Aqueous solution of 1,3-diphenylpropane-1,3-dione solution was fleetingly added to the ethanol mixture of nickel(II) acetate tetrahydrate, and stirred about 48 h at 78 °C. Followed by cooling in an ice bath, the formation of a light green precipitate results. The precipitate was filtered, washed with distilled hot water and ethanol, dried in an oven (90 °C). Subsequently, single crystals of nickel complexes were crystallized by slow evaporation from a mixture of 1,4-dioxane and ethanol.

2 Experimental details

Absorption corrections were performed by using multi-scan program. 1 The structure was solved with Olex2 and SHELX. 2 , 3 , 4 Hydrogen atoms were placed in their geometrically idealized positions. Hydrogen atoms were constrained to ride on their parent atoms.

3 Comment

Nickel compounds are widely used in batteries due to their safety advantages. 5 , 6 The study of nickel-containing complexes in the field of batteries is challenging but also extremely prospective. 7 , 8 Nickel-containing complex Ni(acac)2 with β-diketone derivatives as ligands are also widely used in battery research. 9 In this paper, a β-diketone derivative nickel complex was successfully synthesized for further study of its application in the field of battery materials.

The title compound is a complex with nickel(II) as the central metal. The coordination sites of the compound was occupied by six oxygen atoms. 10 Four oxygen atoms are derived from the bidentate ligand 1,3-diphenylpropane-1,3-dione, the other oxygen atoms are derived from monodentate ligand 1,4-dioxane. 11

In the title molecule, the distances of Ni1–O1 and Ni1–O11 bonds both are 1.997(2) Å, the distances of Ni1–O2 and Ni1–O21 bonds both are 2.001(2) Å, the distance of Ni1–O3 bond is 2.121(4) Å, the distance of Ni1–O31 bond is 2.111(4) Å. 12

In addition, the O21–Ni1–O3 angle is 89.72(12)°, the O2–Ni1–O3 angle is 89.72(12)°, the O2–Ni1–O21 angle is 92.53(13)°, the O2–Ni1–O5 angle is 90.68(12)°, the O21–Ni1–O5 angle is 90.68(12)°, the O1–Ni1–O3 angle is 90.44(12)°, the O11–Ni1–O3 angle is 90.44(12)°, the O1–Ni1–O2 angle is 179.77(13)°, the O1–Ni1–O21 angle is 87.30(8)°, the O11–Ni1–O2 angle is 87.30(8)°, the O11–Ni1–O21 angle is 179.77(13)°, the O1–Ni1–O1 angle is 92.86(13)°, the O1–Ni1–O5 angle is 89.16(12)°, the O11–Ni1–O5 angle is 89.16(12)°, and the O5–Ni1–O3 angle is 179.4(2)°. 13


Corresponding author: Fanzhi Wei, School of Chemical Science and Technology, Yunnan University, Kunming, Yunnan, 650504, P.R. China, E-mail:

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

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

  3. Research funding: None declared.

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Received: 2024-07-11
Accepted: 2024-08-21
Published Online: 2024-09-03
Published in Print: 2024-12-17

© 2024 the author(s), published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of 3-nitrophenol-2,1,3-benzoselenadiazole (1/1), C12H9N3O3Se
  4. Crystal structure of diaqua-(hydroxido)-{μ-[2-(hydroxy)-5-[(4-nitrophenyl)diazenyl]benzoato]}-{2-hydroxy-5-[(4-nitrophenyl)diazenyl]benzoato}-(1,10-phenanthroline)-diterbium hydrate, C38H27.4N8O12.2Tb
  5. Crystal structure of poly[bis(μ3-3-fluoro-4-(1H-1,2,4-triazol-1-yl)benzoato-κ3 O:O′:N)cadmium(II)] – dimethylformamide (1/1), C21H17CdF2N7O5
  6. The crystal structure of 2-amino-N-(pyridin-2-yl)benzamide, C12H11N3O
  7. The crystal structure of 2,3-di(pyridin-2-yl)-2,3-dihydroquinazolin-4(1H)-one, C18H14N4O
  8. Crystal structure of 2-chloro-4-fluorobenzyl (R)-2-(6-methoxynaphthalen-2-yl)propanoate, C21H18ClFO3
  9. Crystal structure of [1-(4-carboxyphenyl)-4-oxo-1,4-dihydropyridazine-3-carboxylic acid]-(methylsulfinyl)methane, C15H16N2O6S
  10. The crystal structure of 2-ethyl-1,1-dimethyl-1H-benzo[e]indole, C16H17N
  11. The crystal structure of (Z)-5-amino-N -hydroxy-1H-pyrazole-4-carboximidamide, C4H7N5O
  12. The crystal structure of 2,2,5-trimethyl-3-(4-(4-(5-phenyl-4,5-dihydroisoxazol-3-yl)thiazol-2-yl)phenyl)imidazolidin-4-one, C24H24N4O2S
  13. The crystal structure of tetrakis(μ2-acetato-κ2 O:O′)-bis[(4′-phenyl-4,2′:6′,4″-terpyridine-κ1 N)dicopper(II)], C25H21CuN3O4
  14. Crystal structure of poly(3-thiophenecarboxylato-κ 3 O,O′:O′)-(methanol-κO)cadmium(II), C11H10O5S2Cd
  15. The crystal structure of dichloridobis[4′-(p-methoxylphenyl)-4,2′:6′,4″-terpyridine-κN] zinc(II), C44H34Cl2N6O2Zn
  16. The crystal structure of 1-(2-carboxyethyl)-1H-imidazole 3-oxide
  17. Crystal structure of 1,1′,1″-(nitrilotris(ethane-2,1-diyl))tris(3-(4-(((E)-pyridin-2-ylmethylene)amino)phenyl)urea), C45H47N13O4
  18. Crystal structure of a (E)-4-bromo-N-(4-(diethylamino)-2-hydroxybenzylidene) benzenaminium acetate ─ 4-bromoaniline (1/1)
  19. Crystal structure of 2,2′-(iminobis(methylene))bis(benzimidazolium) bis(p-toluenesulfonate), C30H31N5O6S2
  20. The crystal structure of alogliptinium meta-chlorobenzoate
  21. Crystal structure of 4-bromobenzyl 2-(6-methoxy-naphthalen-2-yl)propanoate, C21H19BrO3
  22. The hydrated double salt structure of (E)-4-(2-benzylidenehydrazine-1-carbonyl)pyridin-1-ium cation with 2-hydroxybenzoate and benzoate anions
  23. Crystal structure of (R)(R)-5-chloro-3-((S,1E,3E)-3,5-dimethyl-hepta-1,3-dien-1-yl)-7-methyl-6,8-dioxo-2,6,7,8-tetrahydroisoquinolin-7-yl acetate, C21H24ClNO4
  24. The crystal structure of bis(3-oxo-1,3-diphenylprop-1-en-1-olato-κ 2 O:O′)-bis(1,4-dioxane-κ 1 O)nickel(II), C38H38O8Ni
  25. Crystal structure of poly[aqua-(pyridine-3-carboxylato-κ1 N)(pyridine-3-carboxylato-κ2 O,O′) cadmium(II)] dihydrate, C12H14N2O7Cd
  26. The crystal structure of 4-(4-phenyl-5-(((1-(2,4,6-tribromophenyl)-1H-1,2,3-triazol-4-yl)methyl)thio)-4H-1,2,4-triazol-3-yl)pyridine, C22H14Br3N7S
  27. The crystal structure of N-benzylquinoline-2-carbothioamide, C17H14N2S
  28. Crystal structure of bis(3-isopropylphenyl)-4,4′-bipyridinium dichloride dihydrate, C28H30N2⋅2Cl⋅2H2O
  29. The crystal structure of ethyl 2-amino-4-(cyanophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carboxylate, C19H18N2O4
  30. Crystal structure of (4R,10S)-6-hydroxy-7-isopropyl-4,10-dimethyl-1,2,3,5-hexahydro-6,10-epoxyazulen-9-one, C15H22O3
  31. The crystal structure of (E)-(2-(2-hydroxy-3-methoxybenzylidene)aminophenyl)arsonic acid, C14H14AsNO5
  32. The crystal structure of poly[(μ 2-2-aminoisophthalato-κ4O,O′:O″:O″′)-(N-methylpyrrolidone κ1O)-dioxido-uranium(VI)], C13H14N2O7U
  33. The crystal structure of the co-crystal isonicotinamide · terephthalic acid, C8H6O4·2(C6H6N2O)
  34. The crystal structure of (E)-1-phenyl-3-(p-tolylthio)but-2-en-1-one, C17H16OS
  35. The crystal structure of 4,5-bis((Z)-chloro(hydroxyimino)methyl)-1H-imidazol-3-ium chloride monohydrate
  36. The crystal structure of 1,2-bis(4-(dimethylamino)phenyl)ethane-1,2-dione. C18H20N2O2
  37. Crystal structure of 2-chloro-4-fluorobenzyl 2-acetoxybenzoate, C16H12ClFO4
  38. Crystal structure of methyl 1-phenyl-9H-pyrido[3,4-b]indole-3-carboxylate, C19H14N2O2
  39. Crystal structure of (3-(dimethoxymethyl)-5-methoxy-1H-indol-1-yl)(5-fluoro-2-iodophenyl)methanone, C19H17FINO4
  40. Crystal structure of tetrachlorido-bis(1-[(1H-triazole-1-yl)methyl]-1H-benzotriazole-κ2 N:N′)dicopper, C36H32Cu2N24Cl4
  41. Crystal structure of 2-(2,3-bis(4-methoxyphenyl)-1H-pyrrolo[2,3-b]quinoxalin-1-yl)anilin, C30H24N4O2
  42. Crystal structure of 5,7-dihydroxy-2-phenyl-4H-chromen-4-one–N,N-dimethylformamide(1/1), C18H17NO5
  43. The crystal structure of bis(μ 2-biphenyl-2,2′-dicarboxylato)-diaqua-bis(nitrato)-bis(2,2′:6′,2′′-terpyridine)dineodymium(III), C46H32I2N8Nd2O16
  44. Crystal structure of (Z)-4-amino-N -((4-chlorophenyl)(phenyl)methylene)benzohydrazide, C20H16ClN3O
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  46. Crystal structure of (R)-2-((3-(3-aminopiperidin-1-yl)-6-methyl-5-oxo-1,2,4-triazin-4(5H)-yl) methyl)-4-fluorobenzonitrile benzoate monohydrate, C24H27FN6O4
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  48. Crystal structure of (((4-chlorophenyl)sulfonyl)glycinato-κ 2 N,O)bis(1,10-phenanthroline-κ 2 N,N′)cobalt(II) tetrahydrate, C32H30ClCoN5O8S
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  50. Crystal structure of 3-phenoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C27H24O4
  51. 6-(2′,3′-Dihydroxy-3′-methylbutyl)-7-methoxy-8-(3″-methylbut-2″-en-1″-yl)-2H-chromen-2-one, C20H26O5
  52. Crystal structure of bromido-(2,2′:6′,2″-terpyridine-4′-onato-κ3N)palladium(II) methanol solvate
  53. The crystal structure of ethyl 2-amino-(4-nitrophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carboxylate, C20H22N2O6
  54. Crystal structure of (1E,3E,5E)-1,6-bis(4-(pentyloxy)phenyl)hexa-1,3,5-triene, C28H36O2
  55. The crystal structure of tris(2-bromo-4-methylphenyl)amine, C21H18Br3N
  56. The crystal structure of 3-(2,5-dimethylanilino)-1-(2,5-dimethylphenyl)-4-methyl-1H-pyrrole-2,5-dione, C21H22N2O2
  57. Crystal structure of dicarbonyl (μ2-indole-2-carboxylato κ2 O:O′)tris(triphenylarsine-κAs)dirhodium(I) acetone solvate, C68H56As3NO5Rh2
  58. The crystal structure of 4-chloro-2-formylphenyl 4-methylbenzenesulfonate, C14H11ClO4S
  59. Crystal structure of 4-iodobenzyl 2-(6-methoxynaphthalen-2-yl) propanoate, C21H19IO3
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