Startseite Crystal structure of the coordination polymer catena-poly[(1,2-di(pyridin-4-yl)ethane-κN)-(μ2-2-nitroisophthalato-κ2O:O′)zinc(II)], C20H17N3O7Zn
Artikel Open Access

Crystal structure of the coordination polymer catena-poly[(1,2-di(pyridin-4-yl)ethane-κN)-(μ2-2-nitroisophthalato-κ2O:O′)zinc(II)], C20H17N3O7Zn

  • Guang-Zhen Liu EMAIL logo , Lu-Ping Ma und Ru Jia
Veröffentlicht/Copyright: 9. Oktober 2019

Abstract

C20H17N3O7Zn, monoclinic, P21/n (no. 14), a = 10.4368(3) Å, b = 15.1527(5) Å, c = 12.9007(3) Å, β = 101.900(3)°, V = 1996.36(10) Å3, Z = 4, Rgt(F) = 0.0410, wRref(F2) = 0.0898, T = 293(2) K.

CCDC no.: 1953494

A part of the molecular structure 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:Colourless block
Size:0.36 × 0.33 × 0.27 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.28 mm−1
Diffractometer, scan mode:SuperNova, ω
θmax, completeness:28.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:20317, 4466, 0.038
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3729
N(param)refined:281
Programs:Olex2 [1], SHELX [2], [3], CrysAlisPRO [4]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.89979(3)0.38717(2)0.56375(2)0.02860(10)
O10.68499(19)0.35737(14)0.69036(15)0.0485(5)
O1W0.94251(19)0.49672(12)0.64465(13)0.0412(5)
H1WA0.96670.53730.60530.062*
H1WB1.01140.48910.69440.062*
O20.8708(2)0.29882(13)0.66243(15)0.0465(5)
O30.53519(17)0.14114(12)0.98166(13)0.0347(4)
O40.6547(2)0.19044(16)1.13325(14)0.0574(6)
O50.5052(2)0.30051(15)0.85146(19)0.0579(6)
O60.5387(2)0.19727(15)0.74532(15)0.0556(6)
N10.7530(2)0.41113(14)0.43740(16)0.0322(5)
N20.1051(3)0.48538(18)−0.16684(18)0.0522(7)
N30.5746(2)0.24749(15)0.81933(17)0.0342(5)
C10.7818(3)0.31110(16)0.71605(19)0.0312(6)
C20.8100(2)0.26564(16)0.82256(18)0.0268(5)
C30.9390(2)0.25657(18)0.8762(2)0.0382(6)
H31.00650.26990.84160.046*
C40.9687(3)0.2281(2)0.9800(2)0.0458(7)
H41.05560.22331.01520.055*
C50.8700(3)0.20672(18)1.0313(2)0.0384(6)
H50.89090.18961.10200.046*
C60.7393(2)0.21026(16)0.97938(18)0.0281(5)
C70.7129(2)0.24070(15)0.87552(17)0.0249(5)
C80.6368(3)0.18000(17)1.03781(19)0.0323(6)
C90.6605(3)0.4719(2)0.4366(2)0.0462(7)
H90.65870.50230.49890.055*
C100.5673(3)0.4917(2)0.3470(3)0.0573(9)
H100.50410.53450.34970.069*
C110.5683(3)0.4478(2)0.2538(2)0.0526(8)
C120.6595(3)0.3822(2)0.2559(2)0.0519(8)
H120.66010.34880.19560.062*
C130.7498(3)0.36622(19)0.3474(2)0.0413(7)
H130.81160.32210.34700.050*
C140.4741(4)0.4708(3)0.1501(3)0.0744(12)
H14A0.46990.53450.14240.089*
H14B0.50840.44710.09140.089*
C150.3409(3)0.4364(2)0.1443(2)0.0573(9)
H15A0.30180.46490.19750.069*
H15B0.34480.37350.15840.069*
C160.2575(3)0.4536(2)0.0346(2)0.0467(7)
C170.2602(3)0.3977(2)−0.0491(2)0.0525(8)
H170.31360.3480−0.03940.063*
C180.1835(3)0.4155(2)−0.1475(2)0.0533(8)
H180.18680.3768−0.20290.064*
C190.1050(4)0.5395(2)−0.0874(3)0.0664(10)
H190.05160.5892−0.09950.080*
C200.1792(4)0.5269(2)0.0126(3)0.0679(11)
H200.17650.56820.06550.081*

Source of material

All reagents used in the synthesis were of analytical grade and used as purchased without further purification. The mixtures of 2-nitroisophthalic acid (nipc) (0.1 mmol, 21.1 mg), Zn(OAC)2 ⋅ 2H2O (0.1 mmol, 22.0 mg), 1,2-bi(4-pyridyl)ethane (bpa) (0.1 mmol, 18.4 mg) and H2O (6.0 mL) was placed in a 23 mL Teflon liner stainless steel reactor. The vessel was heated to 393 K for 4 days, and then slowly cooled to room temperature. Colorless crystals were obtained, and further crystals were filtered off, washed with mother liquid, and dried under ambient conditions. Yield 46%.

Experimental details

A suitable crystal was selected and mounted on a SuperNova, Single source at offset/far, EosS2 diffractometer. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program and refined with the ShelXL [3] refinement package. All hydrogen atoms were placed in calculated positions with a riding model.

Comment

A coordination polymer is generally formed by self-assembly through coordination bonds between ligands and central metal ions or clusters to produce one-, two-, or three-dimensional metal-organic coordination network [5], [6], [7]. Porous coordination polymers (PCPs) are of great interest due to their potential applications in guest exchange and separation, gas storage, and selective catalysis, etc [8], [9], [10]. For many years, it has been demonstrated that intermolecular weak interactions including H-bonds, π–π interactions, and even van der Waals forces are able to create stable molecular networks in crystalline solids that are reproducible, thermally stable, and resilient upon undergoing dynamic processes [11], [12]. Our work focuses on the design and synthesis of functional PCPs based on multitopic organic ligands. We select 2-nitroisophthalate (nipc) as the assembly ligand, considering its following characteristics: (a) it is a bent ligand with the two carboxylate groups located at appropriate angles (approximately 120°), which may allow it to connect metal ions to generate 1D helical chains; (b) the nitro and carboxylate groups of the ligand can act as hydrogen-bond donors. In addition, the dipyridyl-type pillar ligands, such as 4,4′-bipyridine (bpy), 1,2-bi(4-pyridyl)ethane (bpa), 1,2-di(4-pyridyl)-ethylene(dpe), 1,3-di(4-pyridyl)propane (bpp), and trans-1-(2-pyridyl)-2-(4-pyridyl)ethylene (ppe), are known to be ideal connectors for the propagation of coordination networks and can provide a synergistic coordination together with carboxylate ligands [13], [14], [15]. To the best of our knowledge, coordination polymers constructed from the nipc ligand are rather rare.

The asymmetric unit contains one Zn(II) atom, one bpa molecule, one nipc dianion and one coordinated H2O. Each Zn(II) ion is four coordinated by three oxygen atoms from two carboxylate groups of nipc and one coordinated water (Zn—O: 1.9138(18) Å – 1.9797(17) Å), and one nitrogen atom of the bpa ligand (Zn—N: 2.026(2) Å), displaying a highly distorted tetrahedral coordination environment. Each nipc anion through a bis(monodentate) coordinated mode bridges adjacent Zn(II) atoms to yield an undulating helical chain along the [111] direction, with bpa ligands as free lateral arms; in contrast to a similar 2D network containing analogous ligands [16]. The paralleled chains are connected by H-bonds between H2O molecule and carboxylate oxygen atom of nipc ligand [O(1W)-H(1WA)⋯O(3); d(O1⋯O3) = 2.767(2) Å; degree (H—O⋯O3) = 161.6°] forming a open layered motif. Two adjacent layer blocks are connected by H-bonds between H2O molecule and pyridine N atoms of bpa molecules [O(1W)-H(1WB)⋯N(2); d(O1⋯N2) = 2.668(3) Å; degree (H—O⋯N2) = 155.5°] producing its 3D supramolecular network.

Award Identifier / Grant number: 21571093

Funding statement: This work was supported by the National Natural Science Foundation of China (no. 21571093).

References

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Received: 2019-07-18
Accepted: 2019-09-13
Published Online: 2019-10-09
Published in Print: 2019-12-18

©2019 Guang-Zhen Liu et al., published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

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  37. Crystal structure of 2-[(1E)-{[1,3-dihydroxy-2-(hydroxymethyl)propan-2-yl]iminiumyl}methyl]-5-(dodecyloxy)benzen-1-olate, C23H39NO5
  38. Crystal structure of 12-(2-hydroxybenzoyl)benzo[f]pyrido[1,2-a]indole-6,11-dione, C23H13NO4
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  45. Crystal structure of 3-(3-(4-carboxyphenyl)ureido)pyridin-1-ium perchlorate, C26H24Cl2N6O14
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  50. Crystal structure of (4-chloro-N-[(2-oxido-5-chlorophenyl)methylidene] benzene-carbohydrazonato-κ3N,O,O′)bis(2-fluorobenzyl)tin(IV), C28H20Cl2F2N2O2Sn
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  53. Crystal structure of bromido-dimethyl-4-tolyl-(triphenylphosphine oxide)tin(IV), C27H28BrOPSn
  54. Crystal structure of 2-(bis(2-hydroxyethyl)ammonio)ethane-1-sulfonate, C6H15NO5S
  55. Crystal structure of bis[triaqua-(μ2-1,2-di(4-pyridyl)ethylene-κ2N:N′)-(4-sulfonatobenzoato-κ2O,O′)zinc(II)], C13H15NO8SZn
  56. Crystal structure of 2-((2-(3-hydroxy-7-methylene-2,3-dihydro-7H-furo[3,2-g]chromen-2-yl)propan-2-yl)oxy)-6-(hydroxymethyl)tetrahydro-2H-pyran-3,4,5-triol – a marmesin derivative, C20H24O10
  57. Crystal structure of octa(4-chlorobenzyl)-dichlorido-bis(μ2-methanolato)-bis(μ3-oxo)-tetratin(IV), C58H54Cl10O4Sn4
  58. Crystal structure of iodido-triphenyl-(triphenylphosphine oxide)tin(IV), C36H30IOPSn
  59. Crystal structure of dichlorido-bis(4-methylphenyl-κC)-bis(triphenylarsine oxide-κO)tin(IV), C50H44As2Cl2O2Sn
  60. Crystal structure of 4-benzyl-1-oxo-N-phenethyl-1H-[1,4]oxazino [4,3-b]indazole-3-carboxamide, C26H21N3O3
  61. Crystal structure of bis{(N-[(5-chloro-2-oxidophenyl)methylidene]-2-hydroxybenzenecarbohydrazonato)-dioxo-molybdenum(VI)}(μ2-4,4′-bipyridine), C38H26Cl2Mo2N6O10
  62. Crystal structure of dichlorido-octamethyl-bis(μ3-oxido)-bis(μ2-2-(phenylamino)ethanolato-κ2O:O)tetratin(IV), C24H44Cl2N2O4Sn4
  63. The crystal structure of 1-(2-(2-(imidazo[1,5-a]pyridine-4-ium)ethoxy)ethyl)-imidazo[1,5-a]pyridine-4-ium bis(hexafluorophosphate) — acetonitrile (1/1), C18H20ON4F12P2
  64. Crystal structure of cyclo[tetra(μ2-cyanido)-tetracyanido-bis(1,4,7,10-tetraazacyclododecane-κ4N,N′,N′′,N′′′)dinickel(II)dipalladium(II)] hexahydrate, C24H52N16Ni2O6Pd2
  65. Crystal structure of (dimethyl sulfoxide)-dioxido-[2-hydroxy-N′-(4-oxo-4-phenylbutan-2-ylidene)benzohydrazidato κ3N,O,O′]molybdenum(VI), C19H20MoN2O6S
  66. Crystal structure of bis(acetylacetonato-κ2O,O′)-(ethanolamine-κ2N,O)copper(II), C14H25CuNO5
  67. Crystal structure of chlorido-diphenyl-(isopropyl(propyl)carbamodithioato-κ2S,S′)tin(IV), C19H24ClNS2Sn
  68. The crystal structure of bis(imidazole-1-yl)methane monohydrate, C7H10N4O
  69. The crystal structure of bis(4-nitroimidazole-1-1yl)methane, C7H6N6O4
  70. Crystal structure of di(naphthalen-2-yl)sulfane, C20H14S
  71. Crystal structure of 3-acetyl-6-bromo-4-hydroxy-2H-chromen-2-one, C11H7BrO4
  72. Crystal structure of N′2,N′6-bis((E)-1-(pyrazin-2-yl)ethylidene)pyridine-2,6-dicarbohydrazide — methanol (1/2), C21H25N9O4
  73. The crystal structure of 3-nitro-4-(p-tolylamino)-2H-chromen-2-one, C16H12N2O4
  74. The crystal structure of 1,2-bis((4-methoxyphenyl)ethynyl)benzene, C24H18O2
  75. Crystal structure of a low-temperature (100 K) polymorph of catena-poly[(μ2-4,4′-bipyridine-κ2N,N′)-bis(O,O′-diethyldithiophosphato-κ1S)zinc(II)], C18H28N2O4P2S4Zn
  76. The pseudosymmetric low temperature polymorph of catena-poly[(μ2-4,4′-bipyridyl-κN,N′)-bis(O,O′-diethyldithiophosphato-κS)-cadmium(II)], {C18H28CdN2O4P2S4}n
  77. Crystal structure of 3-iodophthalic acid, C8H5IO4
  78. The crystal structure of tert-butyl (tert-butoxy(oxo)methyl)(5-bromo-2-fluorophenyl)carbamate, C16H21BrFNO4
  79. The crystal structure of bis(μ2-5,7-dichloroquinolin-8-olato-κ3N,O:O)-tetrakis(5,7-dichloroquinolin-8-olato-κ2N,O)bis(methanol-κ1O)dieuropium(III) — toluene (1/1), C63H39Cl12Eu2N6O8
  80. Crystal structure of dichlorido-(N′-(1-(3-ethylpyrazin-2-yl)ethylidene)-4-methoxybenzohydrazide-κ3N,N′,O)cadmium(II), C16H18N4O2Cl2Cd
  81. A redetermination of the crystal structure of catena-poly[(bis(O,O′-isopropyl dithiophosphato-κ2S,S′)-(μ2-1,2-bis(3-pyridylmethylene)hydrazine-κ2N,N′)cadmium(II)], {C24H38CdN4O4P2S4}n
Heruntergeladen am 18.11.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2019-0510/html?lang=de
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