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.
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.
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] |
Atom | x | y | z | Uiso*/Ueq |
---|---|---|---|---|
Ni1 | 0.5 | 0.5 | 0.0 | 0.04087(17) |
O1 | 0.6752(2) | 0.4855(2) | 0.2841(2) | 0.0661(5) |
O2 | 0.45084(19) | 0.33073(18) | 0.16609(18) | 0.0483(4) |
N1 | 0.3319(2) | 0.6523(2) | 0.0870(2) | 0.0453(4) |
N2 | −0.0213(3) | 0.9730(3) | 0.2604(3) | 0.0610(5) |
C1 | 0.5444(4) | 0.2716(4) | 0.4412(3) | 0.0675(7) |
H1a | 0.4494(4) | 0.1876(4) | 0.4219(3) | 0.1013(10)* |
H1b | 0.6498(4) | 0.2162(4) | 0.4722(3) | 0.1013(10)* |
H1c | 0.5224(4) | 0.3478(4) | 0.5269(3) | 0.1013(10)* |
C2 | 0.5622(3) | 0.3709(3) | 0.2885(3) | 0.0473(5) |
C3 | 0.1833(3) | 0.5919(3) | 0.1409(3) | 0.0502(5) |
H3 | 0.1607(3) | 0.4745(3) | 0.1399(3) | 0.0602(6)* |
C4 | 0.0632(3) | 0.6911(3) | 0.1972(3) | 0.0519(5) |
H4 | −0.0381(3) | 0.6407(3) | 0.2307(3) | 0.0623(6)* |
C5 | 0.0920(3) | 0.8688(3) | 0.2046(3) | 0.0466(5) |
C6 | 0.2488(3) | 0.9326(3) | 0.1500(3) | 0.0478(5) |
H6 | 0.2771(3) | 1.0491(3) | 0.1525(3) | 0.0574(6)* |
C7 | 0.3594(3) | 0.8220(3) | 0.0932(3) | 0.0474(5) |
H7 | 0.4608(3) | 0.8682(3) | 0.0564(3) | 0.0568(6)* |
C8 | 0.0066(4) | 1.1563(3) | 0.2604(4) | 0.0678(7) |
H8a | −0.0879(4) | 1.2074(3) | 0.3045(4) | 0.1017(10)* |
H8b | 0.1136(4) | 1.1891(3) | 0.3255(4) | 0.1017(10)* |
H8c | 0.0128(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].
Funding source: Henan University of Science and Technology
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).
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©2019 Zhuang-Yu Li et al., published by De Gruyter, Berlin/Boston
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