Home Crystal structure of catena-poly[(5H-pyrrolo[3,2-b:4,5-b′]dipyridine-κ2N,N′)-(μ4-hexaoxidodivanadato)dizinc(II)],C10H9N3O6V2Zn
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Crystal structure of catena-poly[(5H-pyrrolo[3,2-b:4,5-b′]dipyridine-κ2N,N′)-(μ4-hexaoxidodivanadato)dizinc(II)],C10H9N3O6V2Zn

  • Bingchuan Yang ORCID logo , Xueyan Lv , Gang Liu and Rutao Liu EMAIL logo
Published/Copyright: January 11, 2021

Abstract

C10H9N3O6V2Zn, monoclinic, C2/c (no. 15), a = 8.0106(17) Å, b = 29.957(6) Å, c = 12.050(3) Å, β = 95.025(4) Å, V = 2880.6(10) Å3, Z = 8, Rgt(F) = 0.0512, wRref(F2) = 0.1975, T = 296(2) K.

CCDC no.: 2050067

A part of the coordination polymer is shown in the Figure. 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:White block
Size:0.23 × 0.21 × 0.19 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:2.95 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
θmax, completeness:28.5°, 99%
N(hkl)measured, N(hkl)unique, Rint:8830, 3424, 0.052
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2282
N(param)refined:200
Programs:Bruker [1], SHELX [2]
Table 2:

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

AtomxyzUiso*/Ueq
C10.1988 (9)0.4502 (2)0.3684 (6)0.0461 (16)
H10.1666750.4525830.4404730.055*
C20.2184 (10)0.4881 (2)0.3096 (7)0.0539 (19)
H20.1996010.5159540.3403440.065*
C30.2672 (10)0.4844 (2)0.2026 (7)0.0514 (18)
H30.2832730.5098990.1607690.062*
C40.2919 (10)0.4428 (2)0.1584 (6)0.0484 (17)
H40.3228590.4398590.0861160.058*
C50.2700 (8)0.40536 (19)0.2227 (5)0.0325 (13)
C60.2759 (9)0.3203 (2)0.2089 (5)0.0380 (15)
C70.3209 (9)0.2870 (2)0.1342 (5)0.0414 (15)
H70.3611400.2946590.0667100.050*
C80.3040 (10)0.2428 (2)0.1632 (6)0.0505 (18)
H80.3353520.2201930.1164220.061*
C90.2387 (10)0.2325 (2)0.2644 (6)0.0474 (17)
H90.2201030.2031350.2850550.057*
C100.2044 (9)0.2669 (2)0.3300 (5)0.0409 (15)
H100.1653890.2601780.3985220.049*
N10.2245 (6)0.40826 (16)0.3260 (4)0.0327 (11)
N20.2216 (6)0.31022 (17)0.3049 (4)0.0316 (11)
N30.2993 (8)0.36405 (17)0.1734 (4)0.0462 (15)
H3A0.3390450.3660130.1095440.055*
O10.4147 (7)0.34645 (18)0.5235 (4)0.0611 (16)
O20.7334 (7)0.3766 (3)0.5800 (5)0.085 (2)
O30.4566 (8)0.43049 (18)0.5876 (5)0.0686 (16)
O40.5000000.3646 (3)0.7500000.0564 (19)
O50.0329 (6)0.34579 (15)0.5204 (4)0.0446 (11)
O60.0230 (8)0.42726 (18)0.6023 (4)0.0651 (16)
O70.0000000.3567 (2)0.7500000.0457 (17)
V10.52194 (12)0.38141 (4)0.61144 (7)0.0310 (3)
V2−0.04763 (12)0.37835 (3)0.61285 (8)0.0291 (3)
Zn10.21188 (9)0.35568 (2)0.42672 (5)0.0328 (2)

Source of material

To a solution of vanadiumoxy acetylacetonate (1.5 mmol) in H2O (10 mL) was successivley added 2,2′-dipyridine amine (1 mmol) and zinc chloride (0.5 mmol), and then maintained for 4 h at room temperature with consistent stirring, and then heated for four days at 160 °C. After the reaction was completed, the filtrate was left to slowly evaporate at room temperature. The orange-green crystals were obtained. Yield: 23.2%. Anal. Calcd. for C10H9N3O6V2Zn: C, 27.65; H, 2.09; N, 9.67; found: C, 27.56; H 2.14; N 9.78.

Experimental details

All hydrogen atomic positions were taken from a difference Fourier map. Hydrogen atoms were assigned with isotropic displacement factors Uiso(H) = 1.2 times Ueq(C and N). All the H atoms were refined as riding on their parent atom.

Comment

Polyoxovanadates (POVs) belong to the large class of vanadium-oxide clusters with reversible multi-electron redox transformations properties under mild conditions, which allow them to act as multi-functional catalysts in homogeneous or heterogeneous catalytic systems [3], [4], [5], [6]. The organic-inorganic hybrid POVs cluster can endow them more properties and thus exploration of new functionalized organic-inorganic hybrid POVs is an interesting aspect in chemistry [7], [8]. Therefore, lots of studies on transition-metal functionalized POVs structures have been widely reported [9]. In addition, as a class of versatile tridentate N-ligands 2,2′-dipyridine amine (dpa) can be used not only as a base but also as an interesting ligand, and numerous of dpa-based complexes have been reported [10]. However, the examples of dpa-based zinc-polyoxovanadates are still rare.

Single crystal diffraction analysis of the title complex showed that the asymmetric structural unit consists of one neutral bidentate dpa, a zinc cation and a formal [V2O6] unit. The zinc center is coordinated by two nitrogen atoms of dpa and two oxygen atoms from the POV and formed the distorted Td coordination, which was similar with those of reported zinc compounds [11]. The V–O bond distances of VO4 unit are in the range of 1.579(5) and 1.785(3) Å, which is similar with those of reported vanadates complexes [12], [13], [14].

Additionly, Zn–O and V–O bonds between the basic units form the infinite chain organic-inorganic hybrid polymer illustrated in the Figure.


Corresponding author: Rutao Liu, School of Environmental Science and Engineering, Shandong University, Qingdao266237, Shandong, China, E-mail:

Funding source: National Innovation and Entrepreneurship Training Program for College Students

Award Identifier / Grant number: CXCY2020Y021

Award Identifier / Grant number: S202010447012X

Award Identifier / Grant number: X202010447012X

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: National Innovation and Entrepreneurship Training Program for College Students (CXCY2020Y021, S202010447012X, X202010447012X).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2020-11-18
Accepted: 2020-12-14
Published Online: 2021-01-11
Published in Print: 2021-03-26

© 2020 Bingchuan Yang et al., published by De Gruyter, Berlin/Boston

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

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