Startseite Crystal structure of diaqua-(N-(1-(pyrazin-2-yl)ethylidene)pyridin-1-ium-4-carbohydrazonate-κ3N,N′,O)-tris[nitrato-κ2O,O′)lanthanum(III), C12H15N8O12La
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Crystal structure of diaqua-(N-(1-(pyrazin-2-yl)ethylidene)pyridin-1-ium-4-carbohydrazonate-κ3N,N′,O)-tris[nitrato-κ2O,O′)lanthanum(III), C12H15N8O12La

  • Liu Jinli und Zhang Peiling EMAIL logo
Veröffentlicht/Copyright: 15. August 2018

Abstract

C12H15N8O12La, monoclinic, P21/c (no. 14), a = 8.3267(7) Å, b = 28.348(2) Å, c = 9.1097(8) Å, β = 107.5410(10)°, V = 2050.3(3) Å3, Z = 4, Rgt(F) = 0.0236, wRref(F2) = 0.0559, T = 296(2) K.

CCDC no.: 1858151

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:Yellow block
Size:0.30 × 0.20 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:2.16 mm−1
Diffractometer, scan mode:Bruker SMART APEX, ω
θmax, completeness:25.0°, 97%
N(hkl)measured, N(hkl)unique, Rint:10367, 3601, 0.031
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3194
N(param)refined:305
Programs:SHELX [1], Bruker [2]
Table 2:

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

AtomxyzUiso*/Ueq
La10.86828(2)0.15301(2)0.79298(2)0.02360(7)
C11.2067(4)0.21208(12)1.0869(4)0.0373(8)
H11.19200.23321.00580.045*
C21.3175(4)0.22363(13)1.2289(4)0.0438(9)
H21.37310.25251.24100.053*
C31.2594(5)0.15434(13)1.3231(4)0.0449(9)
H31.27610.13331.40460.054*
C41.1461(4)0.14220(12)1.1830(3)0.0314(7)
C51.0495(4)0.09800(11)1.1610(3)0.0302(7)
C61.0770(5)0.06339(13)1.2909(4)0.0449(9)
H6A1.19550.05811.33600.067*
H6B1.02240.03411.25230.067*
H6C1.03070.07581.36740.067*
C70.7456(4)0.04803(10)0.8674(4)0.0298(7)
C80.6317(4)0.00601(11)0.8394(4)0.0322(7)
C90.6575(4)−0.03089(11)0.9439(4)0.0392(8)
H90.7484−0.03031.03330.047*
C100.5485(5)−0.06815(12)0.9147(5)0.0466(9)
H100.5642−0.09280.98500.056*
C110.3920(5)−0.03459(13)0.6817(5)0.0560(10)
H110.3013−0.03660.59240.067*
C120.4968(5)0.00377(12)0.7069(4)0.0456(9)
H120.47720.02810.63520.055*
N11.1206(3)0.17200(9)1.0620(3)0.0313(6)
N21.3462(4)0.19471(11)1.3475(3)0.0494(8)
N30.9415(3)0.09231(8)1.0270(3)0.0296(6)
N40.8467(3)0.05117(9)1.0083(3)0.0327(6)
N50.4214(4)−0.06923(12)0.7871(4)0.0510(9)
N61.1969(3)0.12365(11)0.7267(3)0.0392(7)
N70.8166(4)0.15276(9)0.4318(3)0.0352(6)
N80.6465(4)0.18546(11)0.9964(3)0.0389(7)
O10.7315(3)0.07597(7)0.7553(2)0.0357(5)
O21.1533(3)0.16562(10)0.7161(3)0.0565(7)
O31.1149(3)0.09569(9)0.7833(3)0.0540(7)
O41.3147(3)0.10959(10)0.6829(3)0.0547(7)
O50.8429(4)0.19200(8)0.4934(3)0.0562(7)
O60.8133(4)0.11807(9)0.5121(3)0.0545(7)
O70.7957(4)0.14813(8)0.2917(3)0.0517(7)
O80.7794(3)0.20594(8)0.9930(3)0.0445(6)
O90.6243(3)0.14498(8)0.9423(3)0.0479(6)
O100.5469(4)0.20499(13)1.0501(4)0.0851(11)
O110.9116(3)0.24303(7)0.7732(2)0.0389(5)
H11A0.87170.25170.67950.058*
H11B0.88520.26010.85830.058*
O120.5670(3)0.17786(10)0.6498(3)0.0494(6)
H12A0.51370.15520.59110.074*
H12B0.56850.20220.59270.074*
H50.353(6)−0.0913(17)0.763(5)0.079(16)*

Source of material

All chemicals were commercially purchased except for (E)-N′-(1-(pyrazin-2-yl)ethylidene)isonicotinohydrazide (HL) which was synthesized according to the literature [3]. A mixture of HL (0.05 mmol, 12.1 mg) and La(NO3)3 ⋅ 6 H2O (0.10 mmol, 43.3 mg) disolved in a absolute methanol (3 mL) and H2O (3 mL) was placed in a glass bottle (10 mL) at room temperature. Green block crystal were obtained after 3 days.

Experimental details

The structure was solved by Direct Methods and refined with the SHELX crystallographic software package [1, 2] . The hydrogen atoms were placed at calculated positions and refined as riding atoms with fixed isotropic displacement parameters.

Comment

Hydrazones are a class of compounds which are well known for their antimicrobial activity [4]. But as hydrazones are prone to undergo degradation and bacteria can develop resistance to them, complexation of hydrazones with biocompatible metal ions is useful in this regard for long-term effectiveness [5]. In the course of our studies on the chemistry of lanthanide compounds, we have prepared and characterized a number of chelates containing hydrazones as ligands. Herein we report a new La(III) complex derived from (E)-N′-(1-(pyrazin-2-yl)ethylidene)isonicotinohydrazide, producing the title complex.

The title complex is a mononuclear coordination compound in which the eleven-coordinated La3+ is surrounded by three nitrates, two water molecules and one independent κ3N,N′;O coordinated organic ligand thus giving distorted monocapped pentagonal prism geometry. The bond lengths of La—O and La—N (2.439(8)−2.893(6) Å) in the title complex are comparable with those found in our previous work [6]. In the solid state, the three dimensional connection is constructed by the O—H⋯O and O—H⋯N hydrogen bonds.

References

Sheldrick, G. M.: Crystal refinement with SHELX. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053273314026370Suche in Google Scholar PubMed PubMed Central

Bruker. SMART and SAINT. Bruker AXS Inc., Madison, WI, USA (2007).Suche in Google Scholar

Das, L. K.; Diaz, C.; Ghosh. A.: Antiferromagnetic mixed-valence Cu two-dimensional coordination polymers constructed by double oximato bridged Cu dimers and CuISCN based one-dimensional anionic chains. Cryst. Growth Des. 15 (2017) 3939–3949.10.1021/acs.cgd.5b00560Suche in Google Scholar

Yan, L.-L.; Cai, H.-X.: Crystal structure of 3-benzyl-2,3-dihydro-2-thioxoquinazolin-4(1H)-one. Z. Kristallogr. NCS 232 (2017) 811–812.10.1515/ncrs-2017-0054Suche in Google Scholar

Bakale, R. P.; Pathan, A. H.; Naik, G. N.; Machakanur, S. S.; Mangannavar, C. V.; Muchchandi, I. S.; Gudasi, K. B.: Synthesis and characterization of transition metal complexes of hydrochloride salt of 3-chlorobenzaldehyde hydralazine hydrazone: a new class of possible anti-cariogenic agents. Appl. Organomet. Chem. 28 (2014) 720–724.10.1002/aoc.3190Suche in Google Scholar

Xu, Z.-Q.; Mao, X.-J.; Zhang, X.; Cai, H.-X.; Bie, Xu, J.; Jia, L.: Synthesis, crystal structures and antitumou activities of three Ln(III) complexes with 2-acetylpyridine picolinohydrazone. Chin. J. Inorg. Chem. 31 (2015) 2249–2256.Suche in Google Scholar

Received: 2018-04-02
Accepted: 2018-07-25
Published Online: 2018-08-15
Published in Print: 2018-11-27

©2018 Liu Jinli 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 di-μ2-aqua-tetraaqua-bis(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)disodium(I) C18H24N6Na2O10
  3. Crystal structure of diaqua-bis(2-bromo-4-chloro-6-formylphenolato-κ2O,O′)cobalt(II), C16H16Cl2CrN3O7
  4. Crystal structure of catena-poly[(μ2-1-(4-(1H-pyrazol-1-yl)phenyl)ethan-1-one-κ2N:O)-bis(1,1,1-trifluoro-4-oxo-4-(thiophen-2-yl)but-2-en-2-olato-κ2O,O′)copper(II)], C27H18CuF6N2O5S2
  5. Crystal structure of ethyl 2-amino-4-(3,5-difluorophenyl)-7-methyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-3-carboxylate, C18H15F2NO5
  6. Crystal structure of 5,5′-dimethoxy-2,2′-[1,1′-(ethylenedioxydinitrilo)diethylidyne]diphenol, C20H24N2O6
  7. Crystal structure of (E)-1-(4-(((E)-3,5-dichloro-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H14Cl2N2O2
  8. Crystal structure of 2,3,9,10,16,17,23,24-octakis(2,6-dimethylphenoxy)phthalocyanine - trichloromethane (1/2), C98H84Cl6N8O8
  9. Crystal structure of methyl 2-((1-(2-(methoxycarbonyl)benzyl)-1H-1,2,3-triazol-4-yl)methoxy)-1-naphthoate, C24H21N3O5
  10. Crystal structure of catena-poly[(μ2-3,3′-thiodipropionato-κ2O:O′)-(bipyridine-κ2N,N′)copper(II)] C16H16CuN2O4S
  11. Crystal structure of [4-chloro-2-(((2-((3-ethoxy-2-oxidobenzylidene)amino)phenyl)imino)(phenyl)methyl)phenolato-κ4N,N′,O,O′}nickel(II) - ethyl acetate (1/1), C32H29ClN2NiO5
  12. Crystal structure of (4-(4-chlorophenyl)-5-ethyl-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, C29H52Cl2N4NiO9
  13. Crystal structure of ethyl 2-amino-4-(3,4-dimethylphenyl)-7-methyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-3-carboxylate, C20H21NO5
  14. Structure and photochromism of 1,2-bis[2-methyl-5-(3-quinolyl)-3-thienyl]-3,3,4,4,5,5-hexafluorocyclopent-1-ene, C33H20F6N2S2
  15. Crystal structure of catena-poly[diaqua-bis(μ2-3,5-di(1H-1,2,4-triazol-1-yl)benzoate-κ2N:N′)cobalt(II))] 2.5 hydrate, C22H23CoN12O8.50
  16. The crystal structure of dichlorido(1,3-dimesityl-1H-3λ4-imidazol-2-yl)(morpholine-κN)palladium(IV), C25H33Cl2N3OPd
  17. Crystal structure of catena-poly[bis(4,4′-dipyridylaminium-kN)-(μ2-germanowolframato-κ2O:O′)-(2,2′-bipyridine-κ2N,N′)copper(II)] with a Keggin-type heteropolyoxoanion, [Cu(C10H8N2)(C10H10N3)2][GeW12O40] ⋅ H2O
  18. Crystal structure of diaqua-(N-(1-(pyrazin-2-yl)ethylidene)pyridin-1-ium-4-carbohydrazonate-κ3N,N′,O)-tris[nitrato-κ2O,O′)lanthanum(III), C12H15N8O12La
  19. The crystal structure of 2-hydroxy-4-((2-hydroxy-4-methoxy-3,6-dimethylbenzoyl)oxy)-3,6-dimethylbenzoic acid–methanol (1/1), C20H24O8
  20. Crystal structure of guanidinium tetrapropylammonium bis(hydrogencarbonate) dihydrate, C15H40N4O8
  21. Crystal structure of (Z)-2-bromo-3-(3,5-di-tert-butyl-4-hydroxyphenyl)-1-phenylprop-2-en-1-one, C23H27BrO2
  22. Crystal structure of 2-(4-(4H-1,2,4-triazol-4-yl)phenyl)acetic acid, C10H9N3O4
  23. Crystal structure of 4,4′-(1,4-phenylene)bis(1H-imidazol-3-ium)bis(2-carboxybenzoate), C30H26N4O8
  24. Crystal structure of 4,4′-(4,10-diphenyl-4,10-dihydropyreno[4,5-d:9,10-d′]diimidazole-5,11-diyl)bis(N,N-diphenylaniline), C66H44N6
  25. Crystal structure of catena-poly[diaqua-bis(μ2-5-(3-(1H-imidazol-5-yl)phenyl)tetrazol-2-ido-κ2N:N′)cobalt(II)], C20H18CoN12O2
  26. Crystal structure of 1,3-dimethyl-2-(p-tolyl)-1H-perimidin-3-ium iodide 1.5 hydrate, C20H22IN2O1.5
  27. Crystal structure of 2-(4-methoxyphenyl)chromane, C16H16O2
  28. Crystal structure of poly[(μ2-2-carboxy-5-nitroisophthalato-κ2O:O′)-(μ2-4-((1H-imidazol-1-yl)methyl)pyridine-κ2N:N′)zinc(II)], C18H12N4O8Zn
  29. Crystal structure of bis(1-((2-ethyl-4-methyl-1H-imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κ2N:N′)tetraiodidodicadmium(II), [Cd2(C13H15N5)2I4]
  30. Crystal structure of tetramethylammonium bis(acetato-κ1O)-tetrakis(μ3-3-((hydroxyimino)methyl)-5-methoxy-2-oxidobenzoate-κ5O,O′:O′,N:O′′)tetrazinc(II) — N,N′-dimethylformamide — water (1/2/2), C62H96Zn4N10O28
  31. Crystal structure of poly[(μ4-5-tert-butylisophthalato-κ4O:O′:O′′:O′′′)-(1,3-dimethyl-2-imidazolidinone-κO)zinc(II)] C17H22N2O5Zn
  32. Crystal structure of [tris(2-benzimidazolylmethyl)amine-κ4N,N′,N′′,N′′′]-[(pyridine-2,6-dicarboxylato-κ2O,N)]cadmium(II)–methanol (1:3) C34H36CdN8O7
  33. The crystal structure of bis(1H-benzo[d]imidazol-2-amine-κN)-diiodidocadmium(II), C14H14CdI2N6
  34. Crystal structure of tetrakis(1H-benzimidazol-2-amine)-κN)-bis(μ2-sulfonato-κ2O:O′)dizinc(II) - methanol (1/1), C30H36N12O10S2Zn2
  35. Crystal structure of 3β-methoxy-20α-dimethylamino-pregn-5-ene, C24H41NO
  36. Crystal structure of dimethyl 4,4′-oxydibenzoate, C16H14O5
  37. Crystal structure of catena-poly[diiodido-(μ2-1,5-dimethyl-2-phenyl-4-((pyridin-3-ylmethylene)amino)-1,2-dihydro-3H-pyrazol-3-one-κ2N:O)zinc(II)], C17H16I2N4OZn
  38. Crystal structure of 4-((E)-((E)-5-(2-fluorobenzylidene)-1-((4-fluorophenyl)sulfonyl)-4-oxopiperidin-3-ylidene)methyl)benzonitrile, C26H18F2N2O3S
  39. Crystal structure of bis(acetato-κ1O)-bis(1-(pyridin-2-yl)ethan-1-one oxime-κ2N,N′)zinc(II), C18H22N4O6Zn
  40. The crystal structure of 9-butoxy-2-(hydroxymethyl)-2H-imidazo[1,5-a]quinolin-10-ium bromide, C17H21O2N2Br
  41. Crystal stucture of 2-(tert-butyl)-6-(hydroxymethyl)-4-methylphenol, C12H18O2
  42. Crystal structure of catena-poly[(2-(5-chloroquinolin-8-yloxy)-1-(pyrrolidin-1-yl)ethan-1-one-κ3N,O,O′)-(dinitrato-κ2O,O′)mercury(II)], C15H15N4O8ClHg
  43. Crystal structure of dimethyl (3aS,6R,6aS,7S)-1H,3H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-3a1,6a-dicarboxylate, C16H16O7
  44. The crystal structure of 2-(dimethoxymethyl)-4-(4-methylphenyl)-1H-imidazole—petroleum ether-chloroform (3/1), C27H33Cl3N4O4
  45. Crystal structure of 8-(trifluoromethyl)imidazo[1,2-a]pyridine-3-carbaldehyde, C9H5F3N2O
  46. The crystal structure of N,N-diethyl-4,6-bis(naphthalen-2-yloxy)-1,3,5-triazin-2-amine, C27H24N4O2
  47. Crystal structure of 5-bromo-7-chloro-3,3a-dihydrocyclopenta[b]chromen-1(2H)-one, C12H8BrClO2
  48. Crystal structure of 2-(bis(4-fluorophenyl)methylene)hydrazine-1-carbothioamide, C14H11F2N3S
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