Startseite Crystal structure of (dimethylformamide-κO)(perchlorato-κ2O,O′){μ2-6,6′-((1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-methoxyphenolate)-κ8N,N′,O:O,O′:O′,O′′,O′′′}sodium(I)nickel(II), C25H23Br2ClN3NaNiO9
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Crystal structure of (dimethylformamide-κO)(perchlorato-κ2O,O′){μ2-6,6′-((1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-methoxyphenolate)-κ8N,N′,O:O,O′:O′,O′′,O′′′}sodium(I)nickel(II), C25H23Br2ClN3NaNiO9

  • Qingguo Meng , Chen Yue , Jiangkun Yu , Qingyun Liu und Jitao Lu EMAIL logo
Veröffentlicht/Copyright: 10. März 2018

Abstract

C25H23Br2ClN3NaNiO9, monoclinic, P21/n (no. 14), a = 15.595(4) Å, b = 10.993(3) Å, c = 18.660(5) Å, β = 114.536(4), V = 2910.2(14) Å3, Z = 4, Rgt(F) = 0.0390, wRref(F2) = 0.0998, T = 293 K.

CCDC no.: 1825595

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:Colorless block
Size:0.21 × 0.15 × 0.11 mm
Wavelength:Mo radiation (0.71073 Å)
μ:3.58 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
θmax, completeness:27.7°, >99%
N(hkl)measured, N(hkl)unique, Rint:16821, 6678, 0.035
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3992
N(param)refined:393
Programs:Bruker programs [1], SHELX [2], OLEX2 [3]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.02437(3)0.22736(4)0.99954(2)0.03812(12)
Na10.10600(10)0.26663(12)0.85809(8)0.0530(4)
Br1−0.26624(3)0.74480(4)0.78779(2)0.06748(15)
Br20.35619(3)−0.28026(4)1.09436(3)0.07031(15)
Cl10.26998(7)0.43203(9)0.85196(6)0.0574(3)
O10.00350(16)0.3294(2)0.91574(12)0.0438(5)
O2−0.00289(17)0.4422(2)0.79237(13)0.0530(6)
O30.11197(16)0.1584(2)0.96945(12)0.0458(6)
O40.23071(18)0.1020(2)0.91047(14)0.0569(7)
O50.0323(2)0.1807(3)0.73615(16)0.0753(8)
O60.2134(2)0.3506(3)0.79185(18)0.0982(11)
O70.2606(3)0.5497(3)0.8201(2)0.0994(11)
O80.3643(2)0.3931(4)0.88111(19)0.1063(12)
O90.2350(2)0.4291(3)0.91208(15)0.0778(9)
N1−0.06207(19)0.3021(2)1.02925(15)0.0389(6)
N20.04339(19)0.1175(2)1.08009(14)0.0399(6)
N30.0000(2)0.1853(3)0.60707(19)0.0711(10)
C1−0.0691(2)0.2457(3)1.09520(19)0.0403(8)
C2−0.0118(2)0.1446(3)1.12281(18)0.0439(8)
C3−0.0127(3)0.0792(3)1.1860(2)0.0558(10)
H30.0250650.0106441.2043270.067*
C4−0.0696(3)0.1164(4)1.2211(2)0.0616(11)
H4−0.0702550.0730491.2636710.074*
C5−0.1255(3)0.2170(4)1.1941(2)0.0588(10)
H5−0.1631910.2415381.2192150.071*
C6−0.1274(3)0.2826(3)1.1306(2)0.0513(9)
H6−0.1665770.3498851.1119530.062*
C7−0.1143(2)0.4569(3)0.92802(18)0.0405(8)
C8−0.0560(2)0.4193(3)0.89152(18)0.0387(8)
C9−0.0624(2)0.4836(3)0.82363(18)0.0401(8)
C10−0.1235(2)0.5788(3)0.79397(19)0.0465(9)
H10−0.1269270.6200740.7493310.056*
C11−0.1806(2)0.6133(3)0.8317(2)0.0482(9)
C12−0.1767(2)0.5562(3)0.8973(2)0.0476(9)
H12−0.2146220.5818710.9219180.057*
C13−0.1128(2)0.3965(3)0.99617(19)0.0446(8)
H13−0.1514550.4274351.0187060.053*
C14−0.0123(3)0.4925(4)0.7190(2)0.0643(11)
H14A−0.0748270.4773030.6797570.096*
H14B0.0328260.4553330.7032600.096*
H14C−0.0013630.5785730.7247240.096*
C150.1602(2)−0.0068(3)1.06129(18)0.0394(8)
C160.1648(2)0.0645(3)1.00023(18)0.0384(7)
C170.2304(2)0.0283(3)0.96927(19)0.0446(8)
C180.2862(2)−0.0717(3)0.9976(2)0.0483(9)
H180.329241−0.0937230.9772460.058*
C190.2781(2)−0.1406(3)1.05700(19)0.0454(8)
C200.2178(2)−0.1105(3)1.08900(19)0.0455(8)
H200.214185−0.1576601.1290210.055*
C210.0999(2)0.0252(3)1.09780(18)0.0442(8)
H210.100945−0.0249691.1383070.053*
C220.2917(3)0.0701(4)0.8731(2)0.0736(13)
H22A0.3561650.0736140.9110920.110*
H22B0.2824840.1263020.8311470.110*
H22C0.277343−0.0107740.8521890.110*
C230.0547(3)0.1919(4)0.6815(3)0.0648(11)
H230.1180890.2068220.6944590.078*
C24a−0.0876(10)0.123(2)0.5919(11)0.148(11)
H24Aa−0.0884890.0462180.5667430.222*
H24Ba−0.1396290.1716950.5580370.222*
H24Ca−0.0926930.1087350.6407240.222*
C250.0348(4)0.2003(5)0.5464(3)0.1039(18)
H25A0.0093780.2736960.5174600.156*
H25B0.0156780.1320480.5112170.156*
H25C0.1023660.2052340.5705490.156*
C24Aa−0.1020(8)0.195(3)0.5768(12)0.142(11)
H24Da−0.1302860.1216210.5486960.212*
H24Ea−0.1233180.2630700.5418640.212*
H24Fa−0.1198080.2053670.6198620.212*
  1. aOccupancy: 0.5.

Source of materials

The Schiff-base ligand was synthesized by condensation of 1,2-diaminobenzene and 5-bromo-3-methoxyl-2-hydroxybenzaldehyde with the molar ratio 1:2 in ethanol. The synthesis of the title complex was carried out by reacting Ni(ClO4)2⋅6H2O, CH3COONa and the schiff-base ligand (1:2:1, molar ratio) in DMF. Stirring was continued for half an hour at room temperature. The mixture was filtered and the filtrate was evaporated in air without disturbed. After 1 month, block red-brown crystals suitable were obtained with a yield about 55%.

Experimental details

A terminal methyl group was refined with disorder model and SADI and RIGU restrains to get better models. Uiso values of hydrogen atoms were set to 1.2Ueq or 1.5Ueq of the parent atoms.

Comment

Because not only of their interesting structures, but also more important of the great potential applications in many fields, the Schiff-base ligand based complexes have all along attracted much attention [4], [5], [6]. Among which, the complexes containing paramagnetic transition ion(s) based-on the salen types of quasi-planar chelate ligands have been widely studied in the molecular magnetism field owing to their interesting magnetic properties [7], [8], [9]. For example new sandwich-type heterometallic ZnII—LnIII clusters based on a methoxy substituted salicylamide salen-like ligand [Zn2Er3(HL)2(H2L)2(OH)2(NO3)3] (NO3)2.2CH3OH(Zn2Er3), [Zn2Yb3(HL)2(H2L)2(OH)2(NO3)3] (NO3)2.2CH3OH (Zn2Yb3), H3L = 1-(2-hydroxy-4-methoxy-benzamido)-2-(2-hydroxy-3-methoxybenzylideneamino)-ethane were reported. The magnetic susceptibility measurements shows that Zn2Er3 displays antiferromagnetic interactions with zero field slow magnetization relaxation diagnostic of single-molecule-magnet [10]. The Ghosh group reported three trinuclear hetero-metallic complexes with a reduced salen type Schiff base ligand and further investigated their maganetic properties [11].

Herein, we report the synthesis and crystal structure of a heterometallic NiNa complex, which can maybe act as a suitable assemble segment to prepare multimetallic molecule-based magnetic material.

The Ni ion is four-coordinated by a N2O2 unit from the Schiff-base ligand, forming a square planar geometry. The Ni—O and Ni—N bond lengths are almost equal to each other with the average value of 1.841 Å and 1.852 Å, respectively. The mean deviation of the plane formed by NiN2O2 is only 0.01(2) Å, indicating that these five atoms are in a perfect plane. The coordination sphere of the Na ion is a distorted pentagonal bipyramid, in which the five equatorial positions are from a O4 unit of the Schiff-base ligand and one O atom of ClO4 ion and the axial ones occupied by one O atom of the coordinated DMF molecule and one O atom of ClO4 ion. The distances between the Na atom and the seven O atoms are with slight difference within a narrow range from 2.287(4) to 2.627(4) Å. Additionally, this complex forms a supramolecular three-dimensional structure based on weak intermolecular C—H⋯O and C—H⋯Cl interactions.

Acknowledgements

We gratefully thank the financial support of the Shandong Provincial Natural Science Foundation (ZR2015BM005), Science and Technology Program of Weifang (2017GX014).

References

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Received: 2017-12-2
Accepted: 2018-2-24
Published Online: 2018-3-10
Published in Print: 2018-5-24

©2018 Qingguo Meng 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. Bis(tetraethylammonium) carbonate – boric acid – water (1/2/5), C17H56B2N2O14
  3. Crystal structure of 4-methoxy-6-phenyl-2H-pyran-2-one, C12H10O3
  4. Crystal structure of tris{(3-((E)-(((E)-2-oxidobenzylidene)hydrazono)methyl)-2-oxo-2H-chromen-4-olato-κ3O,N:N′)}dicobalt(III)tris(dimethylformamide), C60H50Co2N9O15
  5. Crystal structure of poly[bis(1-methyl-[4,4′-bipyridin]-1-ium-κN)-tetrakis(μ3-sulfato-κ3O:O′:O′′)trizinc(II)], C22H22Zn3N4O16S4
  6. Crystal structure of (5Z,10Z)-3,13-dichloro-17,18-dioxo-5,11-diphenyl-8,9,17,18-tetrahydro-7H-dibenzo[e,n][1,4,8,12]tetraazacyclopentadecine-16,19-diido-κ4N,N′,N′′,N′′′)copper(II), C31H22N4O2Cl2Cu
  7. Crystal structure of bis{5-methoxy-2-(((2-oxo-2H-chromen-6-yl)imino)methyl)phenolato-κ2N,O}zinc(II), C34H24N2O8Zn
  8. Crystal structure of 2,2′-((((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))diphenolato-κ2N4O)nickel(II), C28H22N2O4Ni
  9. Crystal structure of 1,1′-((1E,1′E)-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))bis(naphthalen-2-olato)cobalt(II), C36H26N2O4Co
  10. Crystal structure of camptothecin, C20H16N2O4
  11. Crystal structure of (2-(chlorophenyl)-5-methyl-1,3-dioxane-5-carboxylato–κ2O,O′)(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4N,N′,N′′,N′′′)nickel(II) perchlorate monohydrate, Ni(C16H36N4)(C12H12O4Cl)ClO4⋅H2O
  12. Crystal structure of 3-(2-chloro-6-methoxyquinolin-3-yl)-5-phenylisoxazole (C19H13ClN2O2)
  13. Crystal structure of tetrakis(μ2-acetato-κ2O:O′)-bis{[(E)-2,6-diisopropyl-N-(pyridin-3-ylmethylene)aniline]copper (II)}, C44H56Cu2N4O8
  14. Crystal structure of diethyl 2-(2-chlorophenyl)-1,3-dioxane-5,5-dicarboxylate, C16H19Cl1O6
  15. Crystal structure of (μ2-2,2′-bipyridine-3,3′-dicarboxylato)-bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)-di-nickel(II) perchlorate N,N′-dimethylformamide solvate, C50H92Cl2N12Ni2O14
  16. Crystal structure of catena-poly[triaqua(μ2-1,2-bis(4-pyridyl)ethane-κ2N:N′)-(1,2-bis(4-pyridyl)ethane-κN)nickel(II)] 2-aminonicotinate nitrate – 1,2-bis(4-pyridyl)ethane – water (2/1/8), C36H44N8NiO12
  17. Hydrothermal synthesis and crystal structure of poly[bis(μ2-3-(3,5-dicarboxyphenoxy)phthalato-κ3O,O′:O′′)-(μ2-1,2-di(pyridin-4-yl)ethane-κ2N:N′)copper(II)], C22H14CuNO9
  18. Crystal structure of catena-poly[aqua-(methanol-κO)-bis(μ2-4-(pyridin-4-yl)benzoato-κ2N:O)-bis(triphenylphospine-κP)disilver(I)], C61H52Ag2N2O6P2
  19. The crystal structure of 6-(4-bromobenzyl)-1,3,5-trimethyl-7-phenyl-1,5-dihydro-2H-pyrrolo[3,2-d]pyrimidine-2,4(3H)-dione, C22H20BrN3O2
  20. Synthesis and crystal structure of catena-poly[bis(2-(2-((2,6-dichlorophenyl)amino)phenyl)acetato-κO2O′,O′′)-(μ2-1,4-di(pyridin-4-yl)benzene-κ2N:N′)zinc(II)], C44H32N4ZnCl4O4
  21. Crystal structure of diaqua-bis[N-phenyl-2-(quinolin-8-yloxy)acetamide-κ3-N,O,O′]-nitrato(κ2O,O′)-cerium(III) dinitrate - acetone (1/2), C40H44N7O17Ce
  22. Crystal structure of the 2D coordination polymer poly[aqua(μ2-2,2′-(1,2-phenylene)diacetato-κ3O,O′:O′)-(μ2-4,4′-bis((1H-1,2,4-triazol-1-yl)methyl)-1,1′-biphenyl-κ2N:N′)cobalt(II)], C28H26CoN6O5
  23. Crystal structure of (dimethylformamide-κO)(perchlorato-κ2O,O′){μ2-6,6′-((1,2-phenylenebis(azanylylidene))bis(methanylylidene))bis(4-bromo-2-methoxyphenolate)-κ8N,N′,O:O,O′:O′,O′′,O′′′}sodium(I)nickel(II), C25H23Br2ClN3NaNiO9
  24. The crystal structure of catena-poly[bis((4-aminophenyl)sulfonyl)(pyrimidin-2-yl)amido-κ2N,N′)-bis(μ2-4,4′-bipyridine-N,N′2N:N′)zinc(II) – methanol (1/2), C32H34N10O6S2Zn
  25. Synthesis and crystal structure poly[aqua(μ3-2-(((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)ammonio)acetate-κ4O,O′:O′′:O′′′) sodium] monohydrate, C18H18NNaO11S
  26. Crystal structure of methyl 4′-amino-3′,5′-diisopropyl-[1,1′-biphenyl]-4-carboxylate, C20H25NO2
  27. Crystal structure of (η6-1-isopropyl-4-methyl benzene)-(N-(2,5-dichlorophenyl)-1-(pyridin-2-yl)methanimine-κ2N,N′)ruthenium(II) perchlorate, C22H22Cl4N2O4Ru
  28. Crystal structure of 2-(2-(1-Chlorocyclopropyl)-3-(2-chlorophenyl)-2-hydroxypropyl)-1H-1,2,4-triazole-3(2H)-thione, C14H15Cl2N3OS
  29. Crystal structure of methyl 4′-amino-3′,5′-dimethyl-[1,1′-biphenyl]-4-carboxylate, C16H17NO2
  30. The crystal structure of 1-(5-ferrocenyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)pentan-1-on, C19H19F3FeN2O
  31. The crystal structure of (3S,12R,20R,24S)-3,12-diacetyl-20,24-epoxy-dammarane-3,12,25-triol acetone solvate, C34H56O6
  32. Crystal structure of methyl 10-(pyridin-4-yl)-anthracene-9-carboxylate, C21H15NO2
  33. Crystal structure of catena-poly[diaqua-bis(di(N2,N6-dihydroxypyridine-2,6-dicarboxamide))potassium(I)]tetrahydrate, C14H25N6O14K
  34. Crystal structure of poly{[μ2-(E)-1,4-bis(1H-benzo[d]imidazol-1-yl)but-2-ene-κ2N:N′][μ3–cyclohexane-1,4-dicarboxylato-κ4O,O′:O′′:O′′′]cadmium(II)}, C26H26CdN4O4
  35. Crystal structure of poly[aqua(μ3-[2,2′-bipyridine]-3,3′-dicarboxylato-κ4N,N′:O:O′)zinc(II)] – dimethylformamide (1/1), C15H15N3O6Zn
  36. The crystal structure of poly[tetraaqua-tris(μ2-2,6-di(1H-imidazol-1-yl)naphthalene-κ2N:N′)-bis(thiophene-2,5-dicarboxylato-κ1O)]dicobalt(II), C30H24CoN6O6S
  37. Crystal structure of (S)-1-(5-(anthracen-9-yl)-3-phenyl-4,5-dihydro-1H-pyrazol-1-yl)propan-1-one, C26H22N2O
  38. Crystal structure of 5-methyl-3,3-diphenyl-1-tosyl-1,2,3,4-tetrahydropyridine, C25H25NO2S
  39. Synthesis and crystal structure of μ-[1,1′-di(mesitylphosphanido)ferrocene]bis[η5-cyclopentadienylnickel(II)] tetrahydrofurane solvate, C42H48FeNi2OP2
  40. Synthesis and crystal structure of (E)-1-(4-(((E)-5-chloro-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H15ClN2O2
  41. Crystal structure of bis(1-(phenylsulfonyl)-2-(1-(pyrazin-2-yl)ethylidene)hydrazin-1-ido-κ3N,N′,O)nickel(II), C24H22N8O4S2Ni
  42. Crystal Structure of bis(1-(phenylsulfonyl)-2-(1-(pyrazin-2-yl)ethylidene)hydrazin-1-ido-κ3N,N′,O)copper(II), C24H22N8O4S2Cu
  43. Synthesis and crystal structure of poly[aqua{μ3-(1S,2S)-1-((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)pyrrolidin-1-ium-2-carboxylato-κ4O,O′:O′′:O′′′}sodium(I)] monohydrate, C21H22NNaO11S
  44. Halogen bonds in the crystal structure of 1,4-diiodotetrafluorobenzene–1,2-bis(4-pyridyl)propane (1/1), C19H14F4I2N2
  45. Crystal structure of bis(μ-N-i-propyl-N-n-propyldithiocarbamato-κ2S:S′) bis(N-i-propyl-N-n-propyldithiocarbamato-κ2S,S′)dizinc(II), C28H56N4S8Zn2
  46. Crystal structure of bis(μ-N-i-propyl-N-n-propyldithiocarbamato-κ3S,S′:S)bis(N-i-propyl-N-n-propyldithiocarbamato-κ2S,S′)dicadmium(II), C28H56Cd2N4S8
  47. Crystal structure of bis(μ2-di-n-butyldithiocarbamato-κ3S,S′:S3S:S:S′)-hexacarbonyl-di-rhenium(I), C24H36N2O6Re2
  48. Crystal structure of 7-(4-methylphenyl)imidazo[1,2-a][1,3,5]triazin-4-amine, C12H11N5
  49. Crystal structure of the co-crystal O-isopropyl phenylcarbamothioate – 4,4′-bipyridine (2/1), C15H17N2OS
  50. Crystal structure of the coordination polymer catena-poly[chlorido-{μ2-2-(((3,5-dimethyl-1H-pyrazol-1-yl)methyl)amino)-3-hydroxybutanoato-κ4N,N,O:O′}copper(II)], C11H16ClCuN2O3
  51. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-di(ethanol)-bis{μ2-5-(N,N′-diethylamine)-5′-methoxyl-2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato-κ6O:O,N,N,O′:O′}trinickel(II) – ethanol – acetonitrile (1/2/2), C58H86Ni3N8O18
  52. Crystal structure of the bis((E)-O-ethyl-N-phenylthiocarbamate) – 4,4′-bipyridine co-crystal (2/1), C28H30N4O2S2
  53. Crystal structure of the (E)-O-methyl-N-phenyl-thiocarbamate – 4,4′-bipyridine (1/1), C18H17N3OS
  54. Crystal structure of bis(μ2-diethyldithiocarbamato-κ3S,S′:S′)-bis(tricyclohexylphosphane-κP)dicopper(I), C46H86Cu2N2P2S4
  55. Crystal structure of N-(3-chlorophenyl)ethoxycarbothioamide, C9H10ClNOS
  56. Crystal structure of bis(μ2-pyrrolidine-1-carbodithioato-κ3S,S′:S;κ3S:S:S′)-bis(tricyclohexylphosphane-P)-di-copper(I), C46H82Cu2N2P2S4
  57. Crystal structure of N-(2-chlorophenyl)methoxycarbothioamide, C8H8ClNOS
  58. Crystal structure of chlorido-methanol-(N-(2-(oxy)-3-methoxybenzylidene)pyridine-4-carbohydrazonato-κ3O,N,O′)-(4-methylphenyl)methyl-tin(IV), C23H24ClN3O4Sn
  59. Crystal structure of N-(3-chlorophenyl)(propan-2-yloxy)carbothioamide, C10H12ClNOS
  60. Crystal structure of 1-[(Z)-[4-(4-methoxyphenyl)butan-2-ylidene]amino]-3-phenylurea, C18H21N3O2
  61. A triclinic polymorph of bis(μ-N,N-bis(2-hydroxyethyl)dithiocarbamato-κ3S,S′:S′) bis(N,N-bis(2-hydroxyethyl)dithiocarbamato-κ2S:S′)zinc(II), C20H40N4O8S8Zn2
Heruntergeladen am 17.11.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2017-0309/html
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