Startseite Crystal structure of biaqua(2,2′-bipyridine-4,4′-dicarboxylato-κ2N,N′)(pyridine-2,6-dicarboxylato-κ3O,N,O′)nickel(II) hydrate, C19H15N3NiO10
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Crystal structure of biaqua(2,2′-bipyridine-4,4′-dicarboxylato-κ2N,N′)(pyridine-2,6-dicarboxylato-κ3O,N,O′)nickel(II) hydrate, C19H15N3NiO10

  • Jin-Ke Jiang , Ying-Wen Yang und Hui Jiang ORCID logo EMAIL logo
Veröffentlicht/Copyright: 4. Oktober 2019

Abstract

C19H15N3NiO10, monoclinic, P21/c (no. 14), a = 12.7175(10) Å, b = 10.6780(10) Å, c = 15.0802(16) Å, β = 96.786(9)°, V = 2033.5(3) Å3, Z = 4, Rgt(F) = 0.0358, wRref(F2) = 0.0960, T = 293(2) K.

CCDC no.: 1938460

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:Green block
Size:0.24 × 0.22 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.02 mm−1
Diffractometer, scan mode:XtaLAB Pro, ω
θmax, completeness:29.9°, 99%
N(hkl)measured, N(hkl)unique, Rint:22810, 5266, 0.029
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4244
N(param)refined:302
Programs:CrysAlisPRO [1], SHELX [2], [3], WinGX/ORTEP [4]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.84135(2)0.36710(2)0.69566(2)0.02922(8)
C10.70667(17)0.4616(2)0.83749(16)0.0438(5)
H10.7691950.4610940.8763000.053*
C20.61472(18)0.5023(3)0.86990(17)0.0467(5)
H20.6154420.5286500.9287500.056*
C30.52209(17)0.5024(2)0.81175(16)0.0422(5)
C40.52411(16)0.4613(2)0.72554(16)0.0419(5)
H40.4622150.4598500.6859740.050*
C50.61879(15)0.4222(2)0.69800(15)0.0353(4)
C60.62660(15)0.3810(2)0.60602(15)0.0353(4)
C70.53850(17)0.3548(2)0.54547(16)0.0424(5)
H50.4709430.3594420.5630600.051*
C80.55168(19)0.3218(2)0.45917(16)0.0441(5)
C90.6533(2)0.3186(2)0.43498(16)0.0466(5)
H70.6644330.3013150.3763530.056*
C100.73795(18)0.3413(2)0.49905(15)0.0413(5)
H60.8061000.3356170.4828230.050*
C110.41925(18)0.5453(2)0.84244(17)0.0465(5)
C120.4585(2)0.2899(2)0.39212(18)0.0520(6)
C131.03089(14)0.39946(18)0.61165(13)0.0305(4)
C141.11847(17)0.3659(2)0.57033(17)0.0422(5)
H91.1668080.4259890.5563780.051*
C151.13241(19)0.2408(2)0.55026(18)0.0493(6)
H101.1897100.2164890.5212830.059*
C161.06112(17)0.1522(2)0.57333(17)0.0409(5)
H111.0694210.0680360.5598490.049*
C170.97737(14)0.19152(18)0.61682(14)0.0309(4)
C181.00001(15)0.53119(18)0.63515(13)0.0310(4)
C190.89373(14)0.10798(18)0.64980(15)0.0324(4)
N10.72618(13)0.37106(16)0.58367(12)0.0330(3)
N20.71014(12)0.42301(17)0.75361(12)0.0347(4)
N30.96324(12)0.31244(15)0.63390(11)0.0284(3)
O10.41016(17)0.5689(3)0.91797(14)0.0781(7)
O20.34376(14)0.5535(2)0.77592(13)0.0650(6)
H30.2911020.5848120.7934660.097*
O30.36887(16)0.2950(3)0.42567(15)0.0709(6)
H80.3201670.2800560.3864560.106*
O40.46925(18)0.2639(2)0.31612(14)0.0711(6)
O51.05591(13)0.61827(14)0.61420(11)0.0425(4)
O60.91722(11)0.54046(13)0.67501(10)0.0362(3)
O70.82414(10)0.16576(13)0.68847(10)0.0357(3)
O80.89770(12)−0.00642(14)0.63829(13)0.0482(4)
O1W0.92419(11)0.35060(13)0.82186(10)0.0365(3)
H1A0.9408760.2727030.8334190.055*
H1B0.9855210.3875940.8244090.055*
O2W0.79751(14)0.75986(18)0.68385(14)0.0595(5)
H2A0.8422300.7004380.6862870.089*
H2B0.8288000.8289880.6771100.089*

Source of material

The Ni(CH3COO)2 (0.08840 g, 0.5 mmol) and pyridine-2,6-dicarboxylic acid (0.04187 g, 0.25 mmol) in 10 mL H2O/methanol (1:4, v/v) reacted for one and a half hours. And 2,2′-bipyridine-4,4′-dicarboxylic acid (0.2442 g, 1 mmol) was put into the solution. The filtrate was kept at 293 K to obtain green block crystals.

Experimental details

Data of crystal were collected via CrysAlisPRO at 293 K [1], the structure was solved by SHELXT [2] program and refined by SHELXL [3] within WinGX [4].

Comment

As is shown in the left part of picture, the Ni1 is six-coordinated by one oxygen atom from water, two nitrogen atoms from one 2,2′-bipyridine-4,4′-dicarboxylic acid ligand, one nitrogen atom and two oxygen atoms from the pyridine-2,6-dicarboxylato ligand (cf. the figure). Thus, there is one free water molecule. Most importantly, the weak interactions such as CH⋯O, OH⋯O could be found and make the crystal structure become 3D supermolecule structure. All geometric parameters are in the expected ranges and agree with an analogous Cu complex [5].

Acknowledgements

This work was supported by the Youth Foundation of Jilin Agricultural Science and Technology University (No. 20190392).

References

1. Rigaku Corporation: CrysAlisPRO. Rigaku Corporation, Yarnton, Oxfordshire, England (2015).Suche in Google Scholar

2. Sheldrick, G. M.: SHELXT – integrated space-group and crystal-structure determination. Acta Crystallogr. A71 (2015) 3–8.10.1107/S2053273314026370Suche in Google Scholar PubMed PubMed Central

3. Sheldrick, G. M.: Crystal structure refinement with SHELXL. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Suche in Google Scholar PubMed PubMed Central

4. Farrugia, L. J.: WinGX and ORTEP for Windows: an update. J. Appl. Crystallogr. 45 (2012) 849–854.10.1107/S0021889812029111Suche in Google Scholar

5. Fainerman-Melnikova, M.; Clegg, J. K.; Pakchung, A. A. H.; Jensen, P.; Codd, R.: Structural diversity of complexes between Cu(II) or Ni(II) and endocyclic oxygen- or nitrogen-containing ligands: synthesis, X-ray structure determinations and circular dichroism spectra. CrystEngComm 12 (2010) 4217–4225.10.1039/c0ce00323aSuche in Google Scholar

Received: 2019-07-12
Accepted: 2019-09-02
Published Online: 2019-10-04
Published in Print: 2019-12-18

©2019 Jin-Ke Jiang et al., published by De Gruyter, Berlin/Boston

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

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  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
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