Home Crystal structure of diaqua-(N-(1-(pyrazin-2-yl)ethylidene)nicotinohydrazonato-κ3N,N′,O)-bis(nitrato-κ2O,O′)samarium(III), C12H14N7O9Sm
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Crystal structure of diaqua-(N-(1-(pyrazin-2-yl)ethylidene)nicotinohydrazonato-κ3N,N′,O)-bis(nitrato-κ2O,O′)samarium(III), C12H14N7O9Sm

  • Xianjie Mao , Chuntong Li , Gaoyuan Xu and Huijun Li EMAIL logo
Published/Copyright: July 7, 2018

Abstract

C12H14N7O9Sm, monoclinic, P21/c (no. 14), a = 16.770(3) Å, b = 7.7185(16) Å, c = 15.165(3) Å, β = 108.409(3)°, V = 1862.5(7) Å3, Z = 4, Rgt(F) = 0.0262, wRref(F2) = 0.0672, T = 296(2) K.

CCDC no.: 1848002

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:3.22 mm−1
Diffractometer, scan mode:Bruker SMART APEX CCD, ω
θmax, completeness:25.0°, 97%
N(hkl)measured, N(hkl)unique, Rint:9083, 3264, 0.035
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2972
N(param)refined:264
Programs:SHELX [2], Bruker [3]
Table 2:

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

AtomxyzUiso*/Ueq
Sm10.70738(2)0.55866(2)0.30975(2)0.02184(9)
C10.5651(2)0.3708(5)0.4174(3)0.0385(9)
H10.52940.36770.35640.046*
C20.5370(3)0.3013(5)0.4869(3)0.0421(10)
H20.48350.25270.47120.050*
C30.6616(3)0.3759(5)0.5939(3)0.0401(9)
H30.69670.37980.65520.048*
C40.6906(2)0.4458(4)0.5249(3)0.0305(9)
C50.7751(2)0.5216(5)0.5456(3)0.0331(9)
C60.8325(3)0.5340(7)0.6441(3)0.0560(13)
H6A0.88870.55730.64420.084*
H6B0.83140.42660.67560.084*
H6C0.81380.62610.67540.084*
C70.8932(2)0.6748(5)0.4164(3)0.0342(9)
C80.9779(2)0.7560(5)0.4288(3)0.0366(9)
C90.9969(3)0.8315(6)0.3552(3)0.0548(12)
H90.95740.83100.29610.066*
C101.0748(3)0.9079(6)0.3694(4)0.0592(13)
H101.08780.96210.32090.071*
C111.1327(3)0.9013(6)0.4576(4)0.0496(12)
H111.18520.95120.46750.060*
C121.0400(2)0.7564(5)0.5143(3)0.0388(9)
H121.02810.70530.56430.047*
N10.6411(2)0.4416(3)0.4348(2)0.0309(7)
N20.5850(2)0.3028(4)0.5756(2)0.0432(8)
N30.7962(2)0.5732(4)0.4746(2)0.0321(7)
N40.87633(19)0.6442(4)0.4942(2)0.0374(8)
N51.1159(2)0.8258(4)0.5294(3)0.0451(9)
N60.6314(2)0.8925(4)0.3243(2)0.0361(7)
N70.6878(2)0.6083(5)0.1146(2)0.0434(5)
O10.84449(16)0.6429(4)0.33325(19)0.0415(7)
O20.71000(17)0.8799(3)0.3434(2)0.0423(7)
O30.58929(16)0.7532(3)0.3117(2)0.0398(7)
O40.5960(2)1.0339(3)0.3166(3)0.0557(9)
O50.66502(18)0.7248(3)0.16133(18)0.0434(5)
O60.73047(18)0.4833(4)0.1611(2)0.0399(6)
O70.6689(2)0.6150(5)0.0303(2)0.0714(10)
O80.57986(17)0.4242(3)0.2155(2)0.0375(7)
H8B0.57250.34810.17320.056*
H8A0.53090.45600.21410.056*
O90.74889(17)0.2634(3)0.32872(19)0.0375(6)
H9A0.70800.20130.33170.056*
H9B0.78970.25270.37870.056*

Source of material

All chemicals were commercially purchased except for (E)—N′-(1-(pyrazin-2-yl)ethylidene)nicotinohydrazide (HL) which was synthesized according to the literature [1]. A mixture of HL (0.05 mmol, 12.1 mg) and Sm(NO3)3⋅6 H2O (0.10 mmol, 44.7 mg) disolved in absolute ethanol (3 mL) and H2O (3 mL) was placed in a glassbottle (10 mL) at room temperature. Pale yellow block crystals were obtained after a few days.

Experimental details

The structure was solved by Direct Methods and refined with the SHELX crystallographic software package [2, 3] . The hydrogen atoms were placed at calculated positions and refined as riding atoms with isotropic displacement parameters.

Comment

Some hydrazones are well known for their antimicrobial activity [1, 4] . But as hydrazones are prone to undergo degradation and bacteria can develop resistance to them, complexation of hydrazones with biocompatible metal ions may be useful for long-term effectiveness [5]. In the course of our studies on the chemistry of lanthanide compounds, we have prepared and characterized hydrazones as ligands.

As depicted in the figure, the title complex is a mononuclear coordinational compound in which the six-coordinated Sm3+ is surrounded by one acylhydrazone ligand, two water molecules an two nitrato ligands, thus giving distorted octahedral geometry. The bond lengths of Sm—O and Sm—N (2.307(2)−2.641(3) Å) in the title complex are comparable with those found in our previous work [6]. In the solid state, the three dimensional framework is constructed by the intermolecular O—H⋯O and O—H⋯N hydrogen bonds between all moieties.

References

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Sheldrick, G. M.: Crystal refinement with SHELX. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053273314026370Search in Google Scholar PubMed PubMed Central

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

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Received: 2018-04-01
Accepted: 2018-06-07
Published Online: 2018-07-07
Published in Print: 2018-08-28

©2018 Xianjie Mao et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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  73. Crystal structure of caffeinium triiodide – caffeine (1/1), C16H21I3N8O4
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  77. The crystal structure of dichlorido-(1,3-bis(2,6-dimethylphenyl)-1H-imidazol-2(3H)-ylidene)-(morpholine-κ1N)palladium(II), C23H29Cl2N3OPd(II)
  78. The crystal structure of 1-((5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-yl)methyl)-1,3-diphenylurea, C24H21ClN4O
  79. Crystal structure of 6-(2-bromoacetamido)tetrahydro-2H-pyran-2,3,4,5-Tetrayl tetraacetate, C16H22BrNO10
  80. Crystal structure of 5-methylpyrazine-2-carbohydrazide, C6H8N4O
  81. Crystal structure of catena-poly[(μ2-5-(tert-butyl)isophthalato-κ4O,O′:O′′,O′′′)(-4′-(pyridin-4-yl)-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)manganese(II)], C32H28N4O5Mn
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