Startseite Crystal structure of catenapoly[diaqua-(μ24,4′-bipyridine)-κ2N:N′)-bis(2,6-difluorobenzoate)-κO)nickel(II)] ethanol monosolvate, C28H30F4N2O8Ni
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Crystal structure of catenapoly[diaqua-(μ24,4′-bipyridine)-κ2N:N′)-bis(2,6-difluorobenzoate)-κO)nickel(II)] ethanol monosolvate, C28H30F4N2O8Ni

  • Yuan Hou-Qun , Xiao Wei , Hu Chun-Yan und Bao Guang-Ming EMAIL logo
Veröffentlicht/Copyright: 6. Januar 2016

Abstract

C28H30F4N2O8Ni, Monoclinic, P21/n, a = 10.164(7) Å, b = 13.927(9) Å, c = 11.409(8) Å, β = 111.863(10) V = 1498.9(18) Å3, Z = 2, Rgt(F) = 0.0389, wRref(F2) = 0.0957, T = 296(2) K.

CCDC no.:: 1009374

Source of material

An aqueous solution (5 ml) of 2,6-difluorobenzoate (65 mg, 0.41 mmol), NaHCO3 (35 mg, 0.42 mmol) was added into an aqueous solution of Ni(NO3)2·6H2O (150 mg, 0.52 mmol). To the mixture an ethanolic solution of 4,4′-bipyridine (35 mg, 0.22 mmol) was added, resulting a light green solution. Green crystals were obtained after two weeks (yield 73 mg, 54%). Anal. Calcd. for C28H30F4N2O8Ni (%): C, 51.17; H, 4.60; N, 4.26. Found (%): C, 51.30; H, 4.45; N, 4.38.

Table 1

Data collection and handling.

Crystal:Green, Block, size 0.13×0.15×0.19 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:7.23 cm−1
Diffractometer, scan mode:CCD area detector, φ and ω scans
2θmax:56.76°
N(hkl)measured, N(hkl)unique:9246, 3649
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2771
N(param)refined:206
Programs:SHELX [17]
Table 2

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

AtomSitexyzUiso
H(4)4e0.69820.18140.36080.086
H(5)4e0.79990.16570.21160.104
H(6)4e0.6620.13910.00310.116
H(1)4e−0.014(4)0.172(3)−0.002(3)0.11(1)
H(2)4e−0.150(3)0.150(2)−0.093(3)0.059(7)
H(8)4e0.08430.1242−0.17910.059
H(9)4e0.09190.128−0.37630.062
H(11)4e−0.1043−0.1261−0.44470.05
H(12)4e−0.1059−0.1225−0.24510.049
H(13)4e0.42950.14270.69140.156
H(13A)4e0.40630.05090.60670.156
H(13B)4e0.44320.14910.55930.156
H(14A)4e0.6190.03590.75010.132
H(14B)4e0.63910.06330.62490.132
H(4A)4e0.70090.20350.70010.126
Table 3

Atomic displacement parameters (Å2).

AtomSitexyzU11U22U33U12U13U23
Ni(1)2a0.00.00.00.0323(2)0.0362(2)0.0185(2)−0.0001(1)0.0123(1)−0.0005(1)
O(1)4e0.2047(1)0.05001(9)0.0582(1)0.0343(6)0.0432(8)0.0345(7)−0.0022(6)0.0160(5)−0.0009(6)
C(1)4e0.2516(2)0.1341(1)0.0747(2)0.0344(9)0.047(1)0.0241(9)−0.0016(8)0.0127(7)−0.0030(8)
O(2)4e0.1808(1)0.2095(1)0.0604(2)0.0383(7)0.0436(8)0.057(1)0.0011(6)0.0106(7)−0.0097(7)
C(2)4e0.4101(2)0.1439(1)0.1148(2)0.037(1)0.040(1)0.046(1)−0.0013(8)0.0186(9)−0.0013(9)
C(3)4e0.4982(2)0.1613(2)0.2376(2)0.041(1)0.047(1)0.055(1)−0.0025(9)0.013(1)−0.005(1)
F(1)4e0.4354(2)0.1700(1)0.3240(1)0.0646(9)0.114(1)0.0439(8)−0.0129(8)0.0125(7)−0.0171(8)
C(4)4e0.6425(3)0.1698(2)0.2766(3)0.040(1)0.060(2)0.093(2)−0.002(1)−0.001(1)−0.004(1)
C(5)4e0.7021(3)0.1607(2)0.1872(4)0.037(1)0.075(2)0.147(3)0.002(1)0.032(2)−0.001(2)
C(6)4e0.6209(3)0.1445(3)0.0632(4)0.063(2)0.121(3)0.133(3)0.001(2)0.068(2)−0.008(2)
C(7)4e0.4764(3)0.1364(2)0.0295(3)0.052(1)0.097(2)0.070(2)−0.006(1)0.037(1)−0.010(2)
F(2)4e0.3924(2)0.1206(2)−0.0928(2)0.090(1)0.227(3)0.065(1)−0.016(1)0.053(1)−0.031(1)
O(3)4e−0.0867(2)0.1367(1)−0.0221(1)0.0381(7)0.0418(7)0.0325(8)0.0012(6)0.0131(6)−0.0001(6)
N(1)4e−0.0104(2)0.0005(1)−0.1902(1)0.0401(8)0.0416(8)0.0204(7)−0.0012(7)0.0149(6)0.0002(6)
C(8)4e0.0462(3)0.0727(2)−0.2330(2)0.076(2)0.048(1)0.027(1)−0.016(1)0.025(1)−0.0073(9)
C(9)4e0.0514(3)0.0755(2)−0.3521(2)0.087(2)0.046(1)0.031(1)−0.025(1)0.031(1)−0.0061(9)
C(10)4e−0.0035(2)0.0003(1)−0.4357(2)0.0387(9)0.044(1)0.0187(8)0.0000(8)0.0129(7)−0.0002(7)
C(11)4e−0.0641(2)−0.0741(2)−0.3924(2)0.053(1)0.049(1)0.027(1)−0.0162(9)0.0199(9)−0.0083(8)
C(12)4e−0.0649(2)−0.0713(2)−0.2714(2)0.050(1)0.050(1)0.028(1)−0.0115(9)0.0207(9)−0.0038(8)
C(13)4e0.4594(3)0.1093(3)0.6320(3)0.080(2)0.132(3)0.084(2)−0.025(2)0.013(2)0.023(2)
C(14)4e0.6072(3)0.0873(2)0.6897(4)0.083(2)0.072(2)0.123(3)−0.017(2)−0.024(2)0.028(2)
O(4)4e0.6964(2)0.1646(1)0.7524(2)0.077(1)0.081(1)0.062(1)−0.026(1)−0.011(1)0.028(1)

Experimental details

H atoms bound to C atoms and O4 were places in calculated positions and refined as riding on their parent atoms, with C–H = 0.93 Å (aromatic), C–H = 0.96 Å (methylene), C–H = 0.97 Å (ethylene), and O–H = 0.82 Å, and with Uiso(H) = 1.5 Ueq(C) for methyl H atoms and 1.2 Ueq(C) for all other H atoms. The hydrogen atoms bound to O3 were refined without restraints.

Discussion

The rational design and construction of coordination polymers with multidimensional structures are of much current interest due to their intriguing topological structures as well as their potential applications such as catalysis, separation, gas storage, luminescence, and magnetism [1–5]. The self-assembly of organic molecules and metal ions is a well known strategy for the construction of coordination polymers. The fluorine substituted organic molecules are good candidates for construction of functional coordination polymers because they are more stable against oxidation and show enhanced thermal stability [6]. The pentafluorobenzoate as ligand has been reported in some studies, while only few complexes with 2,6-difluorobenzoate (dfba) have been reported [7–12]. Meanwhile, 4,4′-bipyridine (bpy) is a common N-donor ligand, which has been widely used as bridging ligand to construct diverse structural networks [13–16]. In this paper, we report the synthesis, crystal structure of {[Ni(dfba)2(bpy)(H2O)2]·EtOH}n.

The asymmetric unit of the title complex consists of half of a Ni2+ ion, one dfba ligand, half of a bpy ligand, one coordination water molecule and an ethanol molecule. Each Ni2+ ion is roughly octahedrally coordinated by two oxygen atoms from two different dfba ligands (Ni1-O1 = 2.0553(18) Å), two nitrogen atoms from two bpy ligands (Ni1-N1 = 2.133(2) Å), and two water molecules (Ni1-O3 = 2.0735(18) Å). The carboxyl group of each dfba ligand adopts monodentate coordination mode. All identucal ligands around each Ni2+ ion are in trans-position to each other. Each bpy ligand bridges to two Ni2+ ions and the distance between Ni2+ ions is 11.41 Å. Thus, a one-dimensional chain structure is formed along the c axis. Ethanol molecules exist among the one-dimensional chains. The coordinated water molecule is hydrogen-bonded to the uncoordinated oxygen atom of the carboxylate group and ethanol molecule (O3–H1⋯O2 = 2.719(3), O3–H2⋯O4 = 2.722(3) Å). The ethanol molecule is also hydrogen-bonded with another uncoordinated oxygen atom of carboxylate group (O4–H4A⋯O2 = 2.765(3) Å). Thus, a 16-membered ring is formed, and the 1-D chains are extended to a three-dimensional network through the hydrogen bonding interactions.


Corresponding author: Bao Guang-Ming, School of Animal Science and Technology, Jiangxi Agricultural University, Nanchang 330045, People's Republic of China, e-mail:

Acknowledgements

This work was supported by the National Nature Foundation of China [No. 21461011], the Natural Science Foundation of Jiangxi Province [No. 20132BAB204004] and the Research Foundation of Educational Department of Jiangxi Province [No. 20132BAB213002 and 20142BAB214017]. The authors thank the responsible editor for supplying the figure.

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Received: 2015-4-9
Accepted: 2015-11-2
Published Online: 2016-1-6
Published in Print: 2016-3-1

©2016 Yuan Hou-Qun et al., published by De Gruyter.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
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  3. Crystal structure of 5-methyl-2-phenyl-1,3-dioxane-5-carboxylic acid, C12H14O4
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  48. Crystal structure of hexaaquamanganese(II) bis(3-carboxythiophene-2-carboxylate) C12H18MnO14S2
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  53. Crystal structure of catena-poly[tetraaqua-(μ2-4,4′-bipyridine-k2N:N′)-zinc(II)] fumarate tetrahydrate, C14H26N2O12Zn
  54. Crystal structure of triaqua-(1,10-phenanthroline)-(dihydrogen-3,3′,3′′-(2,4,6-trioxo-1,3,5-triazinane-1,3,5-triyl)tripropanoato) cobalt(II)dihydrogen-3,3′,3′′-(2,4,6-trioxo-1,3,5-triazinane-1,3,5-triyl)tripropanoate, C72H82Co2N16O42
  55. Crystal structure of poly[dibromido-(μ2–4,4′-bis-(pyrid-4-yl)biphenyl-κ2N:N′)lead(II)], C22H16N2PbBr2
  56. Crystal structure of catena-poly[diaqua-bis(μ2-5-carboxy-2-(pyridin-4-yl)benzoato-κ2O:N)-cobalt(II)]dihydrate, C26H24N2O12Co
  57. Crystal structure of 5-(4-pyridyl)pyrimidine–4,4′-bipyridine–1,3,5-benzenetriol–water (1:1:1:1), C25H23N5O4
  58. Crystal structure of 5-hydroxy-4-((4-hydroxyphenyl)imino)naphthalen-1(4H)-one monohydrate, C16H11NO3 · 0.5H2O
  59. Crystal structure of 2-amino-N-(4-methoxyphenyl)benzamide, C14H14N2O2
  60. Crystal structure of (2,5-dihydroxyphenyl)-(4-hydroxy-3,5-dimethoxyphenyl)methanone, C15H14O6
  61. Crystal structure of dichlorido[bis(2-hydroxyethyl)5′-([2,2′:6′,2′′-terpyridin]-4′-yl)-[1,1′:3′,1′′-terphenyl]-4,4′′-dicarboxylato]zinc(II), C39H31Cl2N3O6Zn
  62. Crystal structure of bis[4-(3-carboxy-6-fluoro-1-(4-fluorophenyl)-4-oxo-1,4-dihydroquinolin-7-yl)piperazin-1-ium] benzene-1,4-dicarboxylate (C20H18F2N3O3)2(C8H4O4), C48H40F4N6O10
  63. Crystal structure of (2,5-dihydroxyphenyl)-(4-methoxyphenyl)methanone, C14H12O4
  64. Crystal structure of photochromic 1-(2-methyl-5-phenyl-3-thienyl-2-[2-methyl-5-(4-ethoxylphenyl)-3-thienyl] 3,3,4,4,5,5-hexafluoro-cyclopent-1-ene, C29H22F6OS2
  65. Crystal structure of poly[diaquabis(μ2-biphenyl-2,4′-dicarboxylato-κ2O:O′)tris(μ2-1,1′-biphenyl-4,4′-diylbis(1H-imidazole)-κ2N:N′)dicobalt(II)] monohydrat, C82H64N12O11Co2
  66. Crystal structure of 2-amino-4-(3,4-difluorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H12N2O2F2
  67. Crystal structure of poly[(di-μ2-aqua-κ2O:O)bis(μ5-oxalato-1:2κ2O1; 1κ1O2; 3:4:5κ3O3; 3κ1O4)(μ4-oxalato-1:2κ2O1; 2:3κ2O2; 3:4κ2O3; 4:1κ2O4)dizinc(II)disodium(I)]
  68. Crystal structure of tetraethylammonium hexachloridotantalate(V), C8H20Cl6NTa
  69. Crystal structure of (E)-2,4-dibromo-6-(((2-nitrophenyl)imino)methyl)phenol, C13H8Br2N2O3
  70. The crystal structure of 6-chloro-2,4-diphenylquinoline
  71. Crystal structure of (E)-2-(((1,10-phenanthrolin-5-yl)imino)methyl)-5-methylphenol monohydrate, C20H15N3O·H2O
  72. Crystal structure of tris(3-(2-pyridyl)pyrazole)zinc(II)tetrachlorido zincate(II), C24H21Cl4N9Zn2
  73. Crystal structure of 4-chloro-N,N-diethyl-6-(piperidin-1-yl)-1,3,5-triazin-2-amine, C12H20ClN5
  74. The crystal structure of 4-allyl-5-benzyl-2,4-dihydro-3H-1,2,4-triazol-3-one, C12H13N3O
  75. Crystal structure of diethyl 2-(((2-(pyridin-3-ylthio)phenyl)amino)methylene)malonate, C19H20N2O4S
  76. Crystal structure of fac-tricarbonyl(2-(isopropylimino)methyl-5-methylphenolatido-κ2N,O)(pyridine-κN)rhenium(I), C19H19N2O4Re
  77. Crystal structure of 1,3,6,8-tetrakis(p-tolylthio)pyrene, C44H34S4
  78. Crystal structure of catena-poly-(diaqua-(μ2-1,2-bis(4-pyridyl)ethene-κ2N:N′)-(4-methylphthalato-κ2O,O′)-cobalt(II)trihydrate, C21H26CoN2O9
  79. Crystal structure of tetraethylammonium fac-tricarbonyl(hexafluoroacetylacetonato-κ2O,O′)-(nitrato-κO)rhenium(I), C16H21O8N2F6Re
  80. Crystal structure of 3-(thiophen-2-yl)-5-(p-tolyl)-4,5-dihydro-1H-pyrazole-1-carboxamide
  81. Crystal structure of bis(1-ethyl-3-methylimidazolium) tetrabromidocadmate(II), [C6H11N2]2[CdBr4]
  82. Crystal structure of N′-(adamantan-2-ylidene)-isonicotinohydrazide, C16H19N3O
  83. Crystal structure of trans-tetraaquabis(4-(pyridin-4-ylsulfonyl)pyridine-κN)cobalt(II) diperchlorate dihydrate, C20H28Cl2CoN4O18S2
  84. Crystal structure of (Z)-4-(furan-2-yl(p-tolylamino)methylene)-3-methyl-1-p-tolyl-1H-pyrazol-5(4H)-one, C23H21N3O2
  85. Crystal structure of 2-[(4-fluorobenzyl)sulfanyl]-4-(2-methylpropyl)-6-oxo-1,6-dihydropyrimidine-5-carbonitrile, C16H16FN3OS
  86. Crystal structure of poly[octaaqua-tris(benzene-1,2,4,5-tetracarboxylato)tetralanthanum(III)] hexahydrate, C30H34La4O38
  87. Crystal structure of trans-tetraaqua-bis(4,4′-sulfonyldipyridine-κN)zinc(II) diperchlorate dihydrate, C20H28Cl2ZnN4O18S2
  88. Crystal structure of 4-nitro-thiophene-2-carboxylic acid, a structure with a Z′ = 4, C5H3NO4S
  89. Crystal structure of dirubidium trimercury(II) tetraselenide, Rb2Hg3Se4
  90. Crystal structure of 5-(adamantan-1-yl)-3-[(4-chloroanilino)methyl]-2,3-dihydro-1,3,4-oxadiazole-2-thione, C19H22ClN3OS
  91. Crystal structure of hexaaquamagnesium(II) 5,5′-bitetrazole-1,1′-diolate, C2H12N8O8Mg
  92. The crystal structure of catena-poly[(μ2-1,1′-benzene-1,4-diylbis(1H-benzimidazole-κ2N:N′)silver(I)] nitrate, C20H14N5AgO3
  93. The crystal structure of 1-(2-(4-chlorophenoxy)-4-chlorophenyl)ethanone, C14H10Cl2O2
  94. The crystal structure of 3,5-dinitro-1,3,5-oxadiazinane, C3H6N4O5
  95. Crystal structure of methyl 5-methoxy 1H-indole-2-carboxylate, C11H11NO3
  96. Crystal structure of (Z)-1-(((3-acetyl-2-hydroxyphenyl)amino)methylene)naphthalen-2(1H)-one, C19H15NO3
  97. Crystal structure of (Z)-5-(4-chlorobenzylidene)-2-thioxothiazolidin-4-one —dimethylsulfoxide (1:1), C12H12ClNO2S3
  98. Crystal structure of 5,5′-((4-(trifluoromethyl)phenyl)methylene)bis(1,3-dimethylpyrimidine-2,4,6(1H,3H,5H)-trione) – diethylamine – dichloromethane (1/1/1) C25H32Cl2F3N5O6
  99. Crystal structure of 2-(dimethylsulfanylidene)-N-(4-methoxyphenyl)-3-oxo-3-phenylpropanamide
  100. Crystal structure of (1,10-phenanthroline-κ2N,N′)bis(thiocyanato-κN)platinum(II), C14H8N4PtS2
  101. Crystal structure of di(μ2-chlorido)bis[2-(2-pyridyl)phenyl-κ2N,C1]dipalladium(II), C22H16Cl2N2Pd2
  102. Crystal structure of trans-dibromidodi(pyridine-κN)palladium(II), PdBr2(C5H5N)2
Heruntergeladen am 1.10.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2015-0057/html
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