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BY 4.0 license Open Access Published by De Gruyter (O) September 27, 2019

Crystal structure of Bis(acetato-κ2O,O′)-bis[4-(dimethylamino)pyridine-κN]nickel(II), C18H26N4NiO4

  • Zhuang-Yu Li , E. Liu , Fang-fang Jian EMAIL logo and Tong-ling Liang

Abstract

C18H26N4NiO4, triclinic, P1̄ (no. 2), a = 7.7547(16) Å, b = 7.8666(16) Å, c = 8.2798(17) Å, α = 90.46(3)°, β = 96.24(3)°, γ = 93.25(3)°, V = 501.24(18) Å3, Z = 1, Rgt(F) = 0.0294, wRref(F2) = 0.0873, T = 310 K.

CCDC no.: 1943409

The molecular structure is shown in the figure. In the figure only the asymmetric unit is labelled. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Green block
Size:0.43 × 0.32 × 0.16 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.00 mm−1
Diffractometer, scan mode:Enraf-Nonius CAD-4, ω
θmax, completeness:25.0°, 98%
N(hkl)measured, N(hkl)unique, Rint:2365, 1738, 0.011
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1688
N(param)refined:124
Programs:CAD-4 [1], XCAD4 [2], Olex2 [3]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.50.50.00.04087(17)
O10.6752(2)0.4855(2)0.2841(2)0.0661(5)
O20.45084(19)0.33073(18)0.16609(18)0.0483(4)
N10.3319(2)0.6523(2)0.0870(2)0.0453(4)
N2−0.0213(3)0.9730(3)0.2604(3)0.0610(5)
C10.5444(4)0.2716(4)0.4412(3)0.0675(7)
H1a0.4494(4)0.1876(4)0.4219(3)0.1013(10)*
H1b0.6498(4)0.2162(4)0.4722(3)0.1013(10)*
H1c0.5224(4)0.3478(4)0.5269(3)0.1013(10)*
C20.5622(3)0.3709(3)0.2885(3)0.0473(5)
C30.1833(3)0.5919(3)0.1409(3)0.0502(5)
H30.1607(3)0.4745(3)0.1399(3)0.0602(6)*
C40.0632(3)0.6911(3)0.1972(3)0.0519(5)
H4−0.0381(3)0.6407(3)0.2307(3)0.0623(6)*
C50.0920(3)0.8688(3)0.2046(3)0.0466(5)
C60.2488(3)0.9326(3)0.1500(3)0.0478(5)
H60.2771(3)1.0491(3)0.1525(3)0.0574(6)*
C70.3594(3)0.8220(3)0.0932(3)0.0474(5)
H70.4608(3)0.8682(3)0.0564(3)0.0568(6)*
C80.0066(4)1.1563(3)0.2604(4)0.0678(7)
H8a−0.0879(4)1.2074(3)0.3045(4)0.1017(10)*
H8b0.1136(4)1.1891(3)0.3255(4)0.1017(10)*
H8c0.0128(4)1.1940(3)0.1510(4)0.1017(10)*
C9−0.1892(4)0.9084(4)0.3024(4)0.0798(8)
H9a−0.2512(4)1.0008(4)0.3395(4)0.1197(13)*
H9b−0.2546(4)0.8553(4)0.2085(4)0.1197(13)*
H9c−0.1731(4)0.8263(4)0.3871(4)0.1197(13)*

Source of material

A mixture of Ni(CH3CO2)2⋅H2O (0.2 g, 0.01 mol) and 4-(dimethylamino)pyridine (DMAP) (0.15 g, 1 mmol) were mixed in methanol (40 mL) and stirred in refluxing for 8 h. The reacted mixture was filtered, and the filtrate was allowed to stand for 16 days to finally obtain small green block-like crystals of the title complex.

Experimental details

Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

Comment

Metal-organic coordination polymers (CPs) have received extensive attention due to their structural diversity and their potential applications in molecular adsorption, separation, gas storage, ion exchange, catalysis and sensing [4], [5].

The molecular structure of the title compound is shown in the figure. In the title complex, Ni(II) ions located at the center of inversion are coordinated by two N atoms of the two 4-(dimethylamino)pyridine (DMAP) ligands at the top and four O atoms of two crystallographically related acetate anions. In the coordination geometry, the Ni1-N1, Ni1-O1 and Ni1-O2 bond lengths are 2.005, 2.592 and 1.974 Å respectively, in a regular distance range [6], [7], [8]. The N1-Ni1-O1, N1-Ni-O2 and O1-Ni1-O2 bond angles are 88.798(59), 90.563(63) and 55.610(56)°, respectively. Generally all bond lengths in all moieties are in the expected ranges [9].

Award Identifier / Grant number: 135100001

Funding statement: The authors would like to thank the financial supports from the Henan University of Science and Technology Distinguished Professor Open Fund (Grant No. 135100001).

References

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Received: 2019-06-28
Accepted: 2019-07-29
Published Online: 2019-09-27
Published in Print: 2019-12-18

©2019 Zhuang-Yu Li et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 Public License.

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