Home Crystal structure of bis(2-(2-hydroxymethyl)pyridine-κ2N,O)-bis(pivalato-κO)nickel(II), C22H32N2NiO6
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Crystal structure of bis(2-(2-hydroxymethyl)pyridine-κ2N,O)-bis(pivalato-κO)nickel(II), C22H32N2NiO6

  • Guo Yuhua , Yu Youzhu EMAIL logo , Shi Weiyun , Wei Aimin and Wang Fengli
Published/Copyright: April 7, 2017

Abstract

C22H32N2NiO6, monoclinic, C2/c (no. 15), a = 12.7943(7) Å, b = 11.7513(6) Å, c = 16.7322(9) Å, β = 96.337(2)°, V = 2500.3(2) Å3, Z = 4, Rgt(F) = 0.0278, wRref(F2) = 0.0816, T = 293(2) K.

CCDC no.:: 1540206

The asymmetric unit of the title crystal structure is shown in the figure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Blue block
Size:0.20 × 0.19 × 0.17 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:8.1 cm−1
Diffractometer, scan mode:Bruker CCD, φ and ω
2θmax, completeness:57°, >99%
N(hkl)measured, N(hkl)unique, Rint:21674, 3105, 0.019
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2875
N(param)refined:146
Programs:Bruker programs [1], SHELX [2], DIAMOND [3]
Table 2

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

AtomxyzUiso*/Ueq
Ni10.25000.75000.00000.03263(9)
O20.18858(10)0.50895(9)0.08027(6)0.0547(3)
N10.09804(9)0.78900(10)0.01640(7)0.0397(2)
C50.23339(10)0.57867(11)0.12941(8)0.0365(3)
C70.02563(11)0.72494(13)−0.02591(9)0.0425(3)
C10−0.03726(16)0.89293(19)0.06937(15)0.0801(6)
H10−0.05710.95110.10230.096*
C9−0.11168(15)0.8279(2)0.02570(17)0.0868(7)
H9−0.18280.84170.02850.104*
C30.33939(18)0.5984(2)0.26378(11)0.0769(6)
H3A0.33830.58740.32050.115*
H3B0.34390.67830.25250.115*
H3C0.39920.56000.24650.115*
C20.2318(3)0.42371(18)0.23187(12)0.0988(9)
H2A0.28930.38630.21050.148*
H2B0.16660.39650.20470.148*
H2C0.23420.40770.28830.148*
C10.1458(2)0.6103(3)0.24986(15)0.1049(9)
H1A0.08190.58210.22120.157*
H1B0.15090.69080.24120.157*
H1C0.14550.59560.30630.157*
C60.06647(11)0.63562(13)−0.07891(9)0.0463(3)
H6A0.02400.5675−0.07750.056*
H6B0.06000.6630−0.13390.056*
O10.27094(8)0.67205(9)0.11049(6)0.0457(2)
C8−0.08069(14)0.74203(16)−0.02235(15)0.0674(5)
H8−0.13030.6964−0.05180.081*
C110.06703(13)0.87107(15)0.06389(11)0.0575(4)
H110.11770.91460.09410.069*
O30.17319(7)0.60821(8)−0.05421(5)0.0389(2)
H30.17690.5703−0.01280.058*
C40.23990(13)0.55062(13)0.21941(8)0.0480(3)

Source of materials

All reagents and solvents employed were commercially available and used as received without further purification. [Ni2(μ-OH2)(O2CCMe3)4(HO2CCMe3)4] was synthesized according to the reference method [4]. Then a mixture of [Ni2(μ-OH2)(O2CCMe3)4(HO2CCMe3)4] (0.1 mmol, 0.095 g) and 2-pyridinemethanol (0.5 mmol, 0.055 g) was heated in acetonitrile (10 mL) at 413 K for 2 d in a sealed 15 mL Teflon-lined stainless steel vessel under autogenous pressure. After cooling to room temperature at a rate of 10 K ⋅ h−1, blue block crystals were isolated, washed with acetonitrile and then dried in air, obtaining crystals in 30% yield.

Experimental details

H atoms were treated as riding atoms with distances C—H = 0.96 (CH3), 0.97 (CH2), 0.93 Å (ArH), and Uiso(H) = 1.2Ueq(C) for CH or CH2 groups, Uiso(H) = 1.5Ueq(C) for CH3 or OH groups.

Discussion

Since the discovery of the [Mn12O12(O2CR)16(H2O)4] family of single-molecule magnets (SMMs) in 1993, a great number of such complexes have been discovered, almost all of them being Mn clusters containing at least some Mn(II) centers [5]. However, there are few Ni(II) complexes showing SMMs effect [6], [7], [8], [9]. Regarding the construction of complex materials, the 2-pyridinemethanol ligand has proven to be extremely versatile for the synthesis of structures due to its ability to engage simultaneously in several different coordination modes. [Ni2(μ-OH2)(O2CCMe3)4(HO2CCMe3)4] was an excellent precursor to construct some new nickel based coplexes. To enlarge nickel(II) based materials we report here the synthesis and crystal structure of a new mononuclear nickel complex using 2-pyridinemethanol and [Ni2(μ-OH2)(O2CCMe3)4(HO2CCMe3)4] as the reagents.

The asymmetric unit contains one half of the title complex (cf. the figure). The hexacoordinate Ni(II) coordination environment is composed of two crystallographically related nitrogen atoms of two 2-pyridinemethanol groups with a Ni1—N1 bond length of 2.045 Å, two oxygen atoms of two 2-pyridinemethanol groups with the N1–N3 bond length of 2.090 Å, and two oxygen atoms of two pivalato ligands with a Ni1–O1 bond length to be 2.054 Å. The average Ni—O bond length (2.072 Å) is typical and comparable with those observed in the related complexes (2.067 Å) [10]. The crystal packing does not exhibit hydrogen bonds or classical interactions.

Acknowledgement

This work was supported by the Foundation of Anyang Institute of Technology.

References

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Received: 2016-10-17
Accepted: 2017-3-25
Published Online: 2017-4-7
Published in Print: 2017-5-24

©2017 Guo Yuhua 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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