Startseite Crystal structure of tetraaqua-bis((E)-N′-(2-bromobenzylidene)isonicotinohydrazide-κN)zinc(II) dinitrate, C26H28N8O12Br2Zn
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Crystal structure of tetraaqua-bis((E)-N′-(2-bromobenzylidene)isonicotinohydrazide-κN)zinc(II) dinitrate, C26H28N8O12Br2Zn

  • Yuan Hou-Qun , Xie Hui-Ming , Xiao Wei , Hu Chun-Yan und Bao Guang-Ming EMAIL logo
Veröffentlicht/Copyright: 14. Juli 2017

Abstract

C26H28N8Br2O12Zn, monoclinic, P21/n (no. 14), a =7.8948(10) Å, b = 17.404(2) Å, c = 11.9437(15) Å, β = 98.719(2)°, V = 1622.1(4) Å3, Z = 2, Rgt(F) = 0.0269, wRref(F2) = 0.0680, T = 296(2) K.

CCDC no.:: 1556629

The title crystal structure is shown in the figure (i: −x + 1, y, −z). 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:Yellow blocks
Size:0.20 × 0.10 × 0.10 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:33.0 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
2θmax, completeness:58°, >98%
N(hkl)measured, N(hkl)unique, Rint:15443, 4217, 0.020
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3426
N(param)refined:279
Programs:Bruker [1], SHELX [2]
Table 2

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

AtomxyzUiso*/Ueq
Zn10.50000.00000.00000.02494(7)
N10.56438(18)0.12028(7)0.03575(12)0.0274(3)
C10.5217(3)0.17652(10)−0.03931(17)0.0401(5)
H10.458(3)0.1646(14)−0.104(2)0.053(7)*
C20.5754(3)0.25183(10)−0.02167(16)0.0415(5)
H20.541(3)0.2897(15)−0.077(2)0.067(8)*
C30.6780(2)0.27141(9)0.07893(14)0.0265(3)
C40.7190(2)0.21377(10)0.15747(15)0.0329(4)
H30.784(3)0.2267(13)0.230(2)0.051(6)*
C50.6611(2)0.13993(10)0.13319(15)0.0324(4)
H40.689(3)0.1001(12)0.1864(18)0.035(5)*
C60.7496(2)0.35057(9)0.10863(14)0.0285(3)
O10.8397(2)0.36233(7)0.19919(11)0.0428(3)
N20.7073(2)0.40520(8)0.02997(13)0.0329(3)
H50.650(3)0.3965(13)−0.032(2)0.038(6)*
N30.7763(2)0.47784(8)0.04752(13)0.0333(3)
C70.7270(3)0.52519(10)−0.03125(16)0.0348(4)
H60.645(3)0.5144(14)−0.092(2)0.052(7)*
C80.7897(2)0.60414(9)−0.02715(16)0.0324(4)
C90.8941(3)0.63147(11)0.06931(19)0.0442(5)
H70.923(3)0.5966(14)0.129(2)0.052(7)*
C100.9507(3)0.70659(12)0.0746(2)0.0537(6)
H81.019(4)0.7226(18)0.140(3)0.080(9)*
C110.9059(3)0.75562(12)−0.0139(2)0.0561(6)
H90.944(3)0.8080(16)−0.012(2)0.059(7)*
C120.8047(3)0.73040(12)−0.1113(2)0.0497(5)
H100.778(3)0.7593(16)−0.173(2)0.064(8)*
C130.7487(3)0.65491(10)−0.11729(17)0.0366(4)
Br10.61335(4)0.621635(13)−0.25411(2)0.05686(9)
O20.5055(2)0.01571(8)−0.17631(12)0.0356(3)
H110.462(3)0.0447(15)−0.217(2)0.042(7)*
H120.577(3)−0.0046(14)−0.203(2)0.042(7)*
O30.24140(17)0.03158(8)−0.03380(13)0.0367(3)
H130.174(3)0.0025(14)−0.072(2)0.047(7)*
H140.186(3)0.0443(16)0.018(2)0.059(8)*
N40.0957(2)0.08346(9)0.22401(13)0.0347(3)
O40.25312(19)0.08954(9)0.24922(15)0.0531(4)
O50.0003(2)0.09650(10)0.29478(12)0.0504(4)
O60.03326(18)0.06302(9)0.12546(12)0.0460(3)

Source of material

A mixture of Zn(NO3)2⋅6H2O (120 mg, 0.4 mmol), 2-bromobenzaldehyde (80 mg, 0.4 mmol), and isonicotinyl hydrazine (55 mg, 0.4 mmol) was dissolved in 20 mL MeOH, which was stirred at 333 K for 2 h. The solution was filtered, and the filtrate was allowed to stand at room temperature. Light yellow block crystals were obtained after 1 week (yield: 120 mg, 34.5%).

Experimental details

All hydrogen atoms are refined freely.

Discussion

The design and construction of metallosupramolecular architectures have received much attention in recent years in view of their unique structures and potential applications in fluorescence, magnetism, catalyst, and molecular recognition [3], [4], [5]. Schiff bases bearing the −N = CH− functional groups are widely used to synthesize metallosupramolecular complexes because of their excellent coordination capabilities and biological activities [6, 7] . Aroylhydrazones are a kind of special Schiff bases, having the —C(O)—NH—N = CH— functional groups. It was reported that the aroylhydrazones have various coordination modes which affected by their own structures and the reaction conditions such as solvent, pH, anions and so on [8]. However, we here report the crystal structure of a mononuclear zinc complex containing (E)-N′-(2-bromobenzylidene)isonicotinohydrazide as a neutral ligand.

The asymmetric unit of the title structure consists of one half of a Zn2+, one organic ligand, two water molecules, and one NO3 ion. Each Zn2+ is six coordinated in an octahedron geometry, with two nitrogen atoms from two organic ligands (Zn1—N1 = 2.1809(13) Å), four water molecules (Zn1—O2 = 2.1304(14) Å, Zn1—O3 = 2.0936(13) Å). The nitrogen atoms are located at the axial positions, and the four water molecules are located in the equatorial plane. The organic ligands coordinate to Zn2+ by their terminal nitrogen atoms (cf. the figure). The distance of C7—N3 is 1.267(2) Å, indicating the formation of C = N. The torsion angels of C3—C6—N2—N3, C6—N2—N3—C7, N2—N3—C7—C8 are −175.92(15)°, −179.38(18)°, −178.94(17)°, respectively, which suggest planarity of this moiety. There are many hydrogen bonding interactions in the crystal packing. Each [ZnL2(H2O)4]2+ unit is hydrogen bonded with adjacent ones through O2—H11⋯O1 hydrogen bonds (O2—H11⋯O1 = 2.800(2) Å). In addition, the water molecules are hydrogen bonded to NO3 counter anions (O2—H12⋯O4 = 2.872(2) Å, O3—H13⋯O6 = 2.809(2) Å, O3—H14⋯O6 = 2.751(2) Å). Furthermore, each NO3 ion is hydrogen bonded to one neighboring imino nitrogen atom (N2—H5⋯O5 = 3.028(2) Å). Thus, a 3 D supramolecular network is formed.

Acknowledgement

This work was supported by the National Nature Foundation of China [No. 21461011 and 31560712], the Natural Science Foundation of Jiangxi Province [No. 20112BBF60024, 20151BAB204014].

References

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Received: 2017-1-18
Accepted: 2017-6-21
Published Online: 2017-7-14
Published in Print: 2017-9-26

©2017 Yuan Hou-Qun et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of 2-(2-ethoxyphenyl)-7-propyl-5-methylimidazo[5,1-f][1,2,4]triazin-4(3H)-one, C17H20N4O2
  3. Crystal structure of catena-poly[aqua-(μ3-1,3,5-benzenetricarboxylato-κ3O:O′:O′′)-[μ3hydroxy-(1,3-di-(μ2-1,2,4-triazole-4-yl)benzoato-κ2N:N′)copper(II)], C19H16Cu2N6O9
  4. Crystal structure of poly[aqua-(μ3-3,5-di(4H-1,2,4-triazolyl-4-κ3N,N′:N′′)benzenecarboxylato)silver(I)], C11H9AgN6O3
  5. Crystal structure of tetrapropylammonium hydrogen carbonate, C13H29NO3
  6. Crystal structure of poly[μ2-acetato-κ3-O,O′:O′)diaqua(μ3-isophthalato-κ4O,O′:O′′:O′′′)yttrium(III)] monohydrate, C20H24O17Y2
  7. Crystal structure of catena-poly[dichlorido-(μ2-4-(1H-pyrazol-3-yl)-pyridine-κ2N,N′)]cadmium(II), C48H42Cd3Cl16N18
  8. Crystal structure of bis(tetraethylammonium) [1,1′-biphenyl]-2,2′-dicarboxylate trihydrate, C30H54N2O7
  9. Crystal structure of poly[(thiophene-3,4-dicarboxylato-κ1O)bis[1,2-bis(4-pyridyl)ethane-κ2N:N′]silver(I)] octahydrate, C30H42Ag2N4O12S
  10. The crystal structure of amine-(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)silver(I) dihydrate, C9H13AgN4O4
  11. Crystal structure of poly[tetrakis(μ2-cyanido-κ2N:O)-cyanido-tris(pyridine)dicobalt(II/III)], C20H15Co2N8
  12. Crystal structure of bis(pyridine)-bis(2-formyl-4,6-dichlorophenolato)cobalt(II), C24H16Cl4CoN2O4
  13. Crystal structure of (E)-1-(4-(((E)-5-bromo-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H15BrN2O2
  14. Crystal structure of catena-poly[(μ2-3-(1H-pyrazol-4-yl)-5-(pyridin-4-yl)-1,2,4-triazole-κ N:N′)-bis(benzoato-κO)zinc(II)], C24H18N6O4Zn
  15. Hydrothermal synthesis and crystal structure of a poly[aqua-(μ4-4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(μ2-1-(4-(1H-imidazol-1-yl)benzyl)-1H-1,2,4-triazole-κ2N:N′) dimanganese(II)], [Mn2(C9H6O4)2(C12H11N5)(H2O)]
  16. Crystal structure of diaqua-catena-poly[diaqua-bis(μ2-5-(4-(1H-1,2,4-triazol-1-yl)phenyl)tetrazol-2-ido-κ2N:N′)cobalt(II)] dihydrate, C20H24CoN14O4
  17. Crystal structure of bis(μ3-2,2′-azanediylbis(ethan-1-olato)-κ5O:O,N,O′:O′)-tetrachlorido-bis(μ2-2-((2-hydroxyethyl)amino)ethan-1-olato-κ3N,O:O)dicobalt(II)dicobalt(III), C16H38Cl4Co4N4O8
  18. Crystal structure of poly[μ4-(4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(2-(4-(1H-imidazol-1-yl)phenyl)-1H-benzo[d]imidazole-κN)manganese(II)] [Mn(C9H6O4)(C16H12N4)]
  19. Crystal structure of 4-chloro-6-phenylpyrimidine, C10H7ClN2
  20. The crystal structure of [6-methoxy-2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1(2H)-one]difluoroborane, C13H10BF5O3
  21. Crystal structure of 3,3′-(butane-1,4-diylbis(azanylylidene))bis(1-phenylbut-1-en-1-olato)-κ4N,N′,O,O′]copper(II), C24H26N2O2Cu
  22. Crystal structure of tetraaqua-bis((E)-N′-(2-bromobenzylidene)isonicotinohydrazide-κN)zinc(II) dinitrate, C26H28N8O12Br2Zn
  23. Crystal structure of 2-amino-4-(4-bromophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13BrN2O2
  24. A single crystal study on tert-butyl-4-((4-(4-bromo-2-fluorophenylamino)-6-methoxyquinazolin-7-yloxy)methyl)piperidine-1-carboxylate, C26H30BrFN4O4
  25. 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-κ3O,O′,N)zinc(II), C36H26N2O4Zn
  26. Crystal structure of diaqua-bis(5′-(pyridin-1-ium-4-yl)-1H-[3,3′-bi(1,2,4-triazol)]-2′-ide-κ2N,N′)cobalt(II) — bis(5-(pyridin-4-yl-κN)-1H,1′H-3,3′-bi(1,2,4-triazole))octamolybdate – water (2/1/8), C27H33CoMo4N21O19
  27. Crystal structure of 3-cyclohexyl-2-(cyclohexylimino)-2,3-dihydro-6,8-diiodo-4H-1,3-benzoxazin-4-one, C20H24I2N2O2
  28. Crystal structure of dinitrato-κO-bis(tris((1H-benzo[d]imidazol-2-yl)methyl)amine-κ4N,N′,N′′,N′′′)-(μ2-cyclohexane-1,4-dicarboxylato-κ4O,O′:O′′,O′′′)dimanganese(II) – methanol – water (1/6/2), C62H80Mn2N16O18
  29. Crystal structure of bis(2-hydroxyethyl(phenyl)carbamodithioate)nickel(II), C18H20N2NiO2S4
  30. Crystal structure of methyl 1-(4-fluorobenzyl)-4-methoxy-5-oxopyrrolidine-3-carboxylate, C14H16FNO4
  31. Crystal structure of di-μ-iodido-bis(6-(p-tolyl)-2,2′-bipyridine-κ2N,N′)dicopper(I) — 2-(diphenylphosphoryl)benzoic acid (1/2), C36H29CuIN2O3P
  32. Crystal structure of 2-amino-4-(3-bromo-4-fluoro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H16BrFN2O2
  33. Crystal structure of bis(μ2-2-chlorobenzoato-κ3O,O′:O′)-(2-chlorobenzoato-κO)-(2-chlorobenzoato-κO,O′)-bis(1,10-phenanthroline-κ2N,N′)-dicadmium(II) monohydrate, C52H36Cd2Cl4N4O10
  34. Crystal structure of 2-(8a-methyl-5-oxo-hexahydroimidazo [1,2-a]pyridin-1(5H)-yl)-2-oxoethyl acetate, C12H18N2O4
  35. Crystal structure of (E)-N,N-diethyl-2-(5-nitrothiazol-2-yl)-1-phenylethen-1-amine, C15H17N3O2S
  36. Crystal structure of diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4O:O,O′,N)dimanganese(III), C22H28Mn2N8O6
  37. The crystal structure of bis(2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1-olato-κ2O,O′)copper(II), C24H16CuF6O4
  38. Crystal structure of hexaaquanickel(II) bis((E)-4-((4-(dimethylamino)phenyl)diazenyl)benzenesulfonate), C28H40N6NiO12S2
  39. Crystal structure of catena-poly[aqua-(μ2-hexamethylenetetramine-κ2N:N′)-bis(2,6-difluorobenzoato-κ2O:O′)cadmium(II)]monohydrate, C20H22CdF4N4O6
  40. Crystal structure of 3-benzyl-2,3-dihydro-2-thioxoquinazolin-4(1H)-one, C15H12N2OS
  41. Crystal structure of bis(μ2-ferrocenecarboxylato-κ2O:O′)-bis(1,10-phenanthroline-κ2N,N′)-(μ2-methanolato2O,O)dicopper(II) tetrafluoroborate – acetonitrile (1/1), C49H40BCu2F4Fe2N5O5
  42. The crystal structure of tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)silver(I) chloride dihydrate, C24H60AgClN12O6P4
  43. Crystal structure of 5-ethyl-2-(p-tolyl)-1,3-dioxane-5-carboxylic acid, C14H18O4
  44. Crystal structure of 2-(4-fluorophenyl)-1,3-dimethyl-1H-perimidin-3-ium iodide, C19H16ClIN2
  45. Crystal structure of catena-poly[(μ2-hexamethylenetetramine-κ2N:N′)-tetrakis(μ2-2,6-difluorobenzoato-κ2O:O′)dicopper(II)], C34H24Cu2F8N4O8
  46. Crystal structure of ethyl 3-hydroxy-5-methyl-2-(4-(m-tolyl)-1H-1,2,3-triazol-1-yl)-[1,1′-biphenyl]-4- carboxylate, C25H24N3O3
  47. The crystal structure of carbonyl(2-oxopyridin-1(2H)-olato-κ2O,O′)-(diphenylcyclohexylphosphine-κP)rhodium(I), C24H25NO3PRh
  48. Crystal structure of bis((pyrazin-2-ylmethyl)(pyrazine-2-carbonyl)amido-κ3N,N′,N′′)copper(II), C20H16CuN10O2
  49. Crystal structure of catena-poly[tetraaqua-(μ2-succinonitrile-κ2N:N′)cobalt(II)] dinitrate, C4H12CoN4O10
  50. The crystal structure of 1,1′-bisisoquinoline, C18H12N2
  51. Crystal structure of bis(hydroxydi(pyridin-2-yl)methanolato-κ3N,N′,O)cobalt(III) perchlorate dihydrate, C22H22ClCoN4O10
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