Home Crystal structure of (bis(2,2′-bipyridine-κ2N,N′))-(3,5-dinitrosalicylato-κ2O,O′)nickel(II), C27H18N6NiO7
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Crystal structure of (bis(2,2′-bipyridine-κ2N,N′))-(3,5-dinitrosalicylato-κ2O,O′)nickel(II), C27H18N6NiO7

  • Guixiang Xie EMAIL logo , Zhiwei Tang , Yan Dong and Decai Wen
Published/Copyright: March 7, 2017

Abstract

C27H18N6NiO7, monoclinic, P21/n (no. 14), a = 8.0981(15) Å, b = 21.660(3) Å, c = 14.170(2) Å, β = 95.215(4)°, V = 2475.1(7) Å3, Z = 4, Rgt(F) = 0.0418, wRref(F2) = 0.0965, T = 293 K.

CCDC no.:: 1502340

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:Green block
Size:0.30 × 0.20 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:8.5 cm−1
Diffractometer, scan mode:Weissenberg IP, ω-scans
2θmax, completeness:55°, >99%
N(hkl)measured, N(hkl)unique:5669, 5669
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3438
N(param)refined:370
Programs:SHELX [8], TeXan [9]
Table 2

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

AtomxyzUiso*/Ueq
Ni10.63824(5)0.369630(15)0.82529(2)0.03136(10)
N10.4773(3)0.32126(12)0.51319(17)0.0447(6)
N20.7725(4)0.49713(13)0.40091(18)0.0518(7)
N30.4443(3)0.40647(10)0.89026(15)0.0345(5)
N40.7371(3)0.37073(10)0.96577(15)0.0360(5)
N50.5721(3)0.27725(10)0.84337(15)0.0351(5)
N60.8285(3)0.32325(10)0.76747(15)0.0358(5)
O10.6898(4)0.54809(10)0.73997(15)0.0802(9)
O20.7257(3)0.45594(9)0.80703(12)0.0416(5)
O30.5161(2)0.37271(9)0.69458(12)0.0383(5)
O40.3583(3)0.30630(12)0.55192(17)0.0703(8)
O50.5333(3)0.28864(11)0.45306(18)0.0724(8)
O60.7607(4)0.47301(12)0.32309(15)0.0781(9)
O70.8426(4)0.54636(12)0.41698(17)0.0773(8)
C10.6580(4)0.46127(12)0.64086(18)0.0357(7)
C20.5725(3)0.40326(12)0.62811(17)0.0317(6)
C30.5564(4)0.38101(12)0.53290(18)0.0338(6)
C40.6198(4)0.41060(13)0.45965(19)0.0374(7)
H4A0.60860.39380.39900.045*
C50.7002(4)0.46530(13)0.47659(18)0.0377(7)
C60.7174(4)0.49082(13)0.56618(19)0.0399(7)
H6A0.77020.52870.57570.048*
C70.6922(4)0.49141(13)0.7361(2)0.0436(8)
C80.3002(4)0.42438(13)0.8469(2)0.0444(8)
H8A0.28190.41910.78170.053*
C90.1765(4)0.45034(15)0.8943(2)0.0557(9)
H9A0.07640.46230.86210.067*
C100.2057(5)0.45804(15)0.9905(3)0.0585(9)
H10A0.12460.47551.02470.070*
C110.3529(4)0.44020(14)1.0359(2)0.0494(8)
H11A0.37320.44521.10110.059*
C120.4724(4)0.41454(12)0.98418(19)0.0356(7)
C130.6366(4)0.39508(12)1.02631(19)0.0369(7)
C140.6877(5)0.40219(15)1.1212(2)0.0551(9)
H14A0.61780.41991.16220.066*
C150.8427(6)0.38273(18)1.1540(2)0.0682(11)
H15A0.87950.38751.21770.082*
C160.9438(5)0.35632(17)1.0935(2)0.0629(10)
H16A1.04890.34211.11490.075*
C170.8849(4)0.35148(14)0.9996(2)0.0484(8)
H17A0.95310.33370.95780.058*
C180.4495(4)0.25710(14)0.8913(2)0.0472(8)
H18A0.37210.28550.90930.057*
C190.4315(5)0.19650(15)0.9156(2)0.0564(9)
H19A0.34570.18450.95090.068*
C200.5403(5)0.15414(15)0.8874(2)0.0558(9)
H20A0.52930.11270.90290.067*
C210.6657(4)0.17290(13)0.8362(2)0.0463(8)
H21A0.73980.14440.81500.056*
C220.6808(4)0.23533(12)0.81622(18)0.0339(6)
C230.8154(4)0.26097(13)0.7653(2)0.0379(7)
C240.9238(5)0.22531(16)0.7204(2)0.0604(10)
H24A0.91470.18250.72020.072*
C251.0465(5)0.25398(18)0.6756(3)0.0723(12)
H25A1.11990.23060.64360.087*
C261.0603(5)0.31717(16)0.6781(3)0.0618(10)
H26A1.14400.33710.64910.074*
C270.9486(4)0.34994(15)0.7241(2)0.0462(8)
H27A0.95670.39280.72520.055*

Source of material

A mixture of Ni(OAc)2⋅2H2O (0.1 mmol), 2,2′-bipyridine (0.1 mmol), 3,5-dinitrosalicylic acid (0.2 mmol) in distilled water (10 mL) was filled in a 20 mL Teflon-lined stainless steel reactor. The solution was heated to 453 K for 3 days, then slowly cooled to room temperature to get green block-like crystals.

Experimental details

H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C—H = 0.93 Å and Uiso(H) = 1.2 Ueq(C)].

Discussion

A lot of attention has been paid to salicylate complexes because of their structural features and biological applications. Complexs with salicylato and N-donor ligands, were found to display diverse structure types [1], [2], [3]. A large number of hydrogen-bonded supramolecular architectures based on bipyridine and carboxylato ligands have been reported [4]. Though the functional groups such as NO2 are able to form robust and strong hydrogen bond, the syntheses of metal-organic supramolecular assemblies employing organic ligands with NO2 groups are limited [5]. Up to now, only 3,5-dinitrosalicylato complexes have been reported [6, 7] .

In the title crystal structure the Ni(II) atom exhibits an octahedral coordination geometry, defined by four N atoms of two 2,2′-bipy ligands and two O atoms from one 3,5-(NO2)2sal ligand. The Ni-N(4) and Ni-N(6) distances are equivalent, while the Ni—N(3) bond (2.053 Å) is significantly shorter than Ni—N(3) (2.093 Å). The bipyridine rings of 2,2′-bipy containing N3 and N4 are approximately coplanar, exhibiting a dihedral angle of 2.0(1)°, while the bipyridine rings of the other 2,2′-bipy containing N5 and N6 are non-coplanar with a dihedral angle of 11.4(2)°. The 3,5-(NO2)2sal ligand is coordinated to Ni(II) atom via one oxygen atom of the carboxylate group (O2) and one oxygen atom from the phenolate group (O3). The carboxylate group of the 3,5-(NO2)2sal ligand is rotated relatively to the aromatic ring with a dihedral angle of 36.8(2)°. The adjacent mononuclear units are further connected to each other by C—H⋯O hydrogen bonds formed between the NO2 groups of 3,5-(NO2)2sal ligands and phenyl hydrogens of 2,2′-bipy.

Acknowledgement

We thank the Foundation of Education Department of Fujian Province, PR China (No. JB12220, JB12214, JK2012048).

References

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Received: 2016-9-5
Accepted: 2017-2-17
Published Online: 2017-3-7
Published in Print: 2017-5-24

©2017 Guixiang Xie et al., published by De Gruyter, Berlin/Boston

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

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