Startseite 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
Artikel Open Access

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

  • WeiCan Zhao , Jing Shi und YanJun Hou EMAIL logo
Veröffentlicht/Copyright: 16. Oktober 2017

Abstract

C50H38F18Lu2O16, monoclinic, C2/c (no. 15), a = 15.7024(12) Å, b = 12.6169(10) Å, c = 29.715(2) Å, β = 91.919(10)°, V = 5883.7(8) Å3, Z = 4, Rgt(F) = 0.0273, wRref(F2) = 0.066, T = 273 K.

CCDC no.:: 886433

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:Block, colorless
Size:0.32 × 0.32 × 0.30 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:3.46 mm−1
Diffractometer, scan mode:Bruker APEX2, φ and ω-scans
2θmax, completeness:28.3°, 97.1%
N(hkl)measured, N(hkl)unique, Rint:23077, 7247, 0.016
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 6388
N(param)refined:445
Programs:Bruker programs [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Lu10.08988(2)0.22420(2)0.37582(2)0.03603(5)
O10.23313(15)0.20960(19)0.38860(8)0.0475(6)
O20.14349(14)0.16603(18)0.31086(7)0.0422(5)
O30.13601(17)0.37220(19)0.41200(8)0.0513(6)
O40.06174(15)0.35881(16)0.32652(7)0.0411(5)
O50.11593(15)0.05166(19)0.39545(9)0.0497(6)
O6−0.01857(14)0.12852(17)0.34312(8)0.0429(5)
O70.0638(2)0.2006(2)0.45440(9)0.0645(7)
O8−0.04543(16)0.3006(2)0.39911(10)0.0627(7)
F10.42648(19)0.0788(4)0.38025(12)0.1242(14)
F20.40274(19)0.2310(3)0.40830(13)0.1016(11)
F30.3543(2)0.0952(3)0.43786(11)0.1065(11)
F4Aa0.2372(7)0.6149(6)0.4150(4)0.126(4)
F5Aa0.1420(5)0.5741(8)0.4619(3)0.166(4)
F6Aa0.2512(6)0.4819(6)0.4586(3)0.125(3)
F5Bb0.1850(8)0.5127(9)0.4741(3)0.106(3)
F4Bb0.2094(8)0.6302(7)0.4255(4)0.083(3)
F6Bb0.2869(5)0.4924(8)0.4308(3)0.097(3)
F7Ac0.0901(7)−0.2211(6)0.3951(4)0.134(5)
F8Ac0.2026(4)−0.1277(7)0.4064(4)0.122(3)
F9Ac0.1109(7)−0.1266(8)0.4526(3)0.156(3)
F7Bd0.1719(5)−0.1777(6)0.3695(2)0.096(2)
F8Bd0.1862(6)−0.1127(6)0.4338(3)0.089(3)
F9Bd0.0786(5)−0.2047(7)0.4190(3)0.078(3)
C10.3688(2)0.1382(4)0.39841(14)0.0607(10)
C20.2862(2)0.1503(3)0.37035(12)0.0447(7)
C30.2786(2)0.0970(3)0.33010(12)0.0476(8)
H30.32330.05450.32110.057*
C40.2044(2)0.1056(2)0.30213(11)0.0394(6)
C50.19455(19)0.0414(3)0.26000(11)0.0397(7)
C60.2453(2)−0.0468(3)0.25176(13)0.0513(8)
H60.2898−0.06430.27190.062*
C70.2299(2)−0.1083(3)0.21387(14)0.0583(10)
H70.2641−0.16680.20850.070*
C80.1640(2)−0.0831(3)0.18399(13)0.0511(8)
H80.1538−0.12500.15860.061*
C90.11228(19)0.0048(3)0.19141(11)0.0405(7)
C100.12899(19)0.0671(3)0.22923(11)0.0401(7)
H100.09590.12690.23410.048*
C110.2006(3)0.5310(3)0.43326(17)0.0874(18)
C120.1489(2)0.4647(3)0.39897(12)0.0471(8)
C130.1231(2)0.5116(3)0.35913(13)0.0527(9)
H130.13790.58200.35420.063*
C140.0751(2)0.4577(2)0.32538(10)0.0391(6)
C150.0372(2)0.5177(3)0.28643(11)0.0449(7)
C160.00000.4641(3)0.25000.0394(9)
H160.00000.39040.25000.047*
C170.0371(4)0.6280(3)0.28584(14)0.0843(17)
H170.06220.66510.30980.101*
C180.00000.6831(6)0.25000.0842(19)
H180.00000.75680.25000.101*
C190.1251(3)−0.1312(4)0.40545(19)0.0801(16)
C200.0797(2)−0.0335(3)0.38638(12)0.0466(8)
C210.0070(2)−0.0508(3)0.36027(15)0.0570(10)
H21−0.0128−0.11980.35640.068*
C22−0.03807(19)0.0325(3)0.33928(11)0.0396(7)
C230.1333(4)0.1736(6)0.48481(16)0.1012(19)
H23A0.16600.23600.49190.152*
H23B0.16900.12220.47090.152*
H23C0.11140.14450.51190.152*
C240.0054(4)0.2744(5)0.47369(17)0.0876(16)
H24A0.03100.34430.47590.105*
H24B−0.00920.25160.50360.105*
C25−0.0715(3)0.2772(5)0.4437(2)0.0909(17)
H25A−0.10040.20930.44420.109*
H25B−0.11050.33120.45380.109*
C26−0.1165(3)0.3157(5)0.3684(2)0.0860(15)
H26A−0.15030.25230.36710.129*
H26B−0.09620.33120.33900.129*
H26C−0.15060.37360.37850.129*
  1. Occupancies: a = 0.59; b = 0.41; c = 0.55, d = 0.45

Source of material

The title compound is easily synthesized by means of reported procedures [3]. To a methanol solution of 1,3-bis(4,4,4-trifluoro-1,3-dioxobutyl)phenyl (1 g, 2.8 mmol), NaOH (0.2 g, 5.6 mmol) was added, and the mixture was allowed to stir for 5 min. To this methanol solution, LuCl3⋅6H2O (1.86 mmol) was added, and the mixture was allowed to stir for 24 h at ambient temperature. Water was then added to this mixture, and the precipitate thus formed was filtered, washed with water, and dried in air to give the title compound in a yield of 62.1%. Crystals were obtained in about two weeks by recrystallization from DME/hexane.

Experimental details

All H atoms on C atoms were placed in idealized positions [C—H = 0.96 (methyl), 0.97 (methylene) and 0.93 Å (aromatic)] and included in the refinement in the riding-model approximation, with Uiso(H) = 1.5Ueq(methyl C) and 1.2Ueq(methylene and aromatic C). The F4, F5 and F6 atoms are disordered (cf. table 2). The non-hydrogen atoms in the structure of the title complex were refined with anisotropic displacement parameters.

Discussion

Lutetium(III) complexes have wide range applications in catalysis in the past few years [4], [5], [6]. Some directly related structures of the title structure have been reported [3, 7–8]. In the title crystal structure, the bond distances and bond angles are all in normal range [9]. The crystal structure features weak intermolecular C—H⋯F and C—H⋯O hydrogen bonds.

Acknowledgement

We are grateful for financial support by the Education Department of Hei longjiang Province of China (no. 12521413).

References

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Received: 2017-6-19
Accepted: 2017-10-3
Published Online: 2017-10-16
Published in Print: 2017-11-27

©2017 WeiCan Zhao 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
Heruntergeladen am 16.10.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2017-0145/html?lang=de
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