Home Physical Sciences Crystal structure of cyclo[diaqua-bis(μ2-3′,5-dicarboxy-[1,1′-biphenyl]-3,4′-dicarboxylato-κ4O,O′:O′′,O′′′)-bis(4,4′-bis(pyrid-4-yl)biphenyl-K1N)dicadmium(II)], C76H52Cd2N4O18
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Crystal structure of cyclo[diaqua-bis(μ2-3′,5-dicarboxy-[1,1′-biphenyl]-3,4′-dicarboxylato-κ4O,O′:O′′,O′′′)-bis(4,4′-bis(pyrid-4-yl)biphenyl-K1N)dicadmium(II)], C76H52Cd2N4O18

  • Peng-Jiang Li , Shi-Jun Chen , Zhi-Bin Yu and Shi-Hui Li ORCID logo EMAIL logo
Published/Copyright: July 2, 2020

Abstract

C76H52Cd2N4O18, triclinic, P1̄ (no. 2), a = 8.5834(4) Å, b = 10.7034(5) Å, c = 17.6105(8) Å, α = 99.328(4)°, β = 100.580(4)°, γ = 95.281(4)°, V = 1556.94(13) Å3, Z = 1, Rgt(F) = 0.0477, wRref(F2) = 0.1183, T = 293(2) K.

CCDC no.: 2010900

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:0.43 × 0.35 × 0.21 mm
Wavelength:0.71073 Å
μ:0.77 mm−1
Diffractometer, scan mode:Xcalibur, omega
θmax, completeness:25.5°, 98%
N(hkl)measured, N(hkl)unique, Rint:14246, 0.049, 0.0487
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4625
N(param)refined:454
Programs:CrysAlisPRO [1], SHELX [2], [3]
Table 2:

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

AtomxyzUiso*/Ueq
Cd10.71513(3)0.37584(3)0.916003(16)0.02833(13)
N10.8222(5)0.4814(3)0.8310(2)0.0374(9)
N21.7300(5)1.4723(4)0.4479(2)0.0485(11)
O10.7512(4)0.5485(3)1.00903(19)0.0460(8)
H1A0.84470.58711.01420.069*
H1B0.75010.52571.05300.069*
O20.4412(4)0.3764(3)0.89484(18)0.0440(8)
O30.5368(3)0.2383(3)0.81684(17)0.0389(8)
O40.3557(4)0.4143(3)0.71646(19)0.0468(8)
O50.1430(4)0.3476(4)0.6199(2)0.0554(10)
H50.18440.40230.59970.083*
O6−0.5251(4)−0.0428(3)0.8826(2)0.0557(10)
O7−0.4700(4)−0.1838(4)0.9572(3)0.0748(14)
H7−0.5648−0.18440.95920.112*
O80.0422(3)−0.3095(3)1.03363(16)0.0307(7)
O90.2496(3)−0.2307(3)0.99374(18)0.0361(7)
C10.7414(6)0.5540(5)0.7870(3)0.0550(14)
H10.63220.55230.78530.066*
C20.8113(6)0.6308(5)0.7443(3)0.0552(14)
H20.74920.67920.71450.066*
C30.9734(5)0.6370(4)0.7452(2)0.0344(10)
C41.0542(6)0.5605(5)0.7907(3)0.0467(13)
H41.16330.55970.79340.056*
C50.9775(6)0.4867(5)0.8314(3)0.0463(13)
H5A1.03690.43690.86140.056*
C61.0575(6)0.7240(4)0.7050(3)0.0379(11)
C70.9854(6)0.7572(5)0.6352(3)0.0467(12)
H7A0.88110.72210.61200.056*
C81.0666(6)0.8424(5)0.5991(3)0.0443(12)
H81.01660.86110.55150.053*
C91.2196(6)0.8992(4)0.6331(2)0.0358(10)
C101.2903(6)0.8640(5)0.7020(3)0.0517(13)
H101.39440.89940.72560.062*
C111.2125(6)0.7786(5)0.7372(3)0.0474(13)
H111.26520.75710.78340.057*
C121.3052(6)0.9960(4)0.5993(2)0.0356(11)
C131.2661(6)1.0068(4)0.5199(3)0.0401(11)
H131.18330.95100.48630.048*
C141.3491(6)1.0993(4)0.4910(3)0.0392(11)
H141.32191.10320.43790.047*
C151.4718(5)1.1866(4)0.5390(3)0.0347(10)
C161.5089(6)1.1760(4)0.6179(3)0.0404(11)
H161.58941.23340.65200.048*
C171.4292(6)1.0829(4)0.6465(3)0.0418(11)
H171.45921.07770.69930.050*
C181.5617(6)1.2850(4)0.5079(3)0.0376(11)
C191.5021(7)1.3212(6)0.4379(3)0.0620(16)
H191.40271.28330.40870.074*
C201.5886(7)1.4131(6)0.4109(3)0.0621(16)
H201.54421.43490.36330.074*
C211.7885(7)1.4370(5)0.5153(3)0.0553(14)
H211.88921.47530.54260.066*
C221.7093(6)1.3470(5)0.5473(3)0.0503(13)
H221.75561.32820.59550.060*
C230.4211(5)0.2845(4)0.8371(2)0.0269(9)
C240.2544(5)0.2257(4)0.8007(2)0.0264(9)
C250.1868(5)0.1400(4)0.8399(2)0.0295(10)
H250.24720.12270.88560.035*
C260.0313(5)0.0784(4)0.8132(2)0.0262(9)
C27−0.0556(5)0.1027(4)0.7433(2)0.0346(10)
H27−0.15910.06220.72350.042*
C280.0126(5)0.1870(4)0.7037(3)0.0386(11)
H28−0.04680.20270.65720.046*
C290.1652(5)0.2489(4)0.7306(2)0.0304(10)
C30−0.0378(5)−0.0106(4)0.8585(2)0.0262(9)
C310.0598(5)−0.0843(4)0.9007(2)0.0261(9)
H310.1676−0.07970.89860.031*
C32−0.0017(5)−0.1635(4)0.9454(2)0.0235(9)
C33−0.1617(5)−0.1718(4)0.9478(2)0.0259(9)
H33−0.2037−0.22670.97690.031*
C34−0.2615(5)−0.0985(4)0.9068(2)0.0275(9)
C35−0.1988(5)−0.0184(4)0.8627(2)0.0276(9)
H35−0.26480.03080.83550.033*
C360.2330(6)0.3448(4)0.6888(3)0.0358(10)
C370.1030(5)−0.2395(4)0.9931(2)0.0268(9)
C38−0.4319(5)−0.1036(4)0.9132(2)0.0326(10)

Source of material

A mixture of Cd(NO3)2 ⋅ 2H2O (0.1 mmol, 0.027 g), 4,4′-bis(pyrid-4-yl)biphenyl (0.06 g, 0.2 mmol) and 3,3′,4,5′-biphenyl tetracarboxylic acid (H4btc) (0.1 mmol, 0.033 g), was dissolved in 8 mL H2O. The solution was heated in a 23 mL Teflon-lined autoclave under autogenous pressure at 393 K for five days. Cooling to room temperature gave colorless crystals.

Experimental details

Coordinates of hydrogen atoms were added using riding models [3].

Comment

Mixed ligand-MOFs can be constructed from metal ions, carboxylic acids and nitrogen-containing ligands. Normally N-containing ligands are electrically neutral, while carboxylate ligands are negatively charged. Using organic aromatic multicarboxylates yield networks and have been widely utilized to construct MOFs [4], [5]. On the other hand, 4,4′-bis(pyrid-4-yl)biphenyl often serves as bridging ligand [6].

In the title complex, there are one Cd(II) ion, one coordinated water molecule, one H2btc2− ligand, and one 4,4′-bis(pyrid-4-yl)biphenyl ligand in the asymmetric unit. Cd1 is six-coordinated with a distorted octahedral geometry by four O atoms from two H2btc2− and one coordinated water molecule, and one N atom from the biphenyl derivate (see the figure). The Cd—N bond length is 2.284(3) Å and the Cd—O ones are in the range of 2.309(3) to 2.396(2) Å. The bond angles of O—Cd—O are in the range of 56.12(8)° to 155.66(10)°. The coordination leads to a dinuclear cyclic dimer.

References

1. Agilent Technologies: CrysAlisPRO Software system, version 1.171.35.15. Agilent Technologies UK Ltd, Oxford, UK (2011).Search in Google Scholar

2. Sheldrick, G. M.: SHELXT – Integrated space-group and crystal-structure determination. Acta Crystallogr. A71 (2015) 3–8.10.1107/S2053273314026370Search in Google Scholar PubMed PubMed Central

3. Sheldrick, G. M.: Crystal structure refinement with SHELXL. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Search in Google Scholar PubMed PubMed Central

4. Li, S. H.; Zhao, Y.: Synthesis and crystal structure of a new three-dimensional Co(II) coordination polymer based on 3,3′,4,5′-biphenyl tetracarboxylic acid and 4,4′-bipyridine. Inorg. Nano-Met. Chem. 47 (2017) 256–259.10.1080/15533174.2016.1186044Search in Google Scholar

5. Li, S. H.; Zang, J.; Guo, J. B.: Synthesis and crystal structure of a new three-dimensional Ho(II) coordination polymer based on 5′-(4-carboxyphenyl)-[1,1′:3′,1′′-terphenyl] -4,4′′-dicarboxylic acid. Inorg. Nano-Met. Chem. 12 (2017) 1746–1749.10.1080/24701556.2017.1357627Search in Google Scholar

6. Li, S. H.; Hu, X. Z.; Zhao, Y.: Crystal structure of catena poly[diaqua-μ2-4,4′-biphenyl-4,4′-diyldipyridine-κ2N:N′-bis(5-carboxy-2,6-dimethylpyridine-3-carboxylato-O)nickel(II)] dihydrate. Z. Kristallogr. NCS 231 (2016) 157–159.10.1515/ncrs-2015-0066Search in Google Scholar

Received: 2020-04-20
Accepted: 2020-06-19
Published Online: 2020-07-02
Published in Print: 2020-08-26

©2020 Peng-Jiang Li 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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  68. Crystal structure of catena-poly[diaqua-(μ2-tartrato-κ4O,O′:O′′,O′′′)zinc(II)], C4H8O8Zn
  69. The crystal structure of (6aR,6bS,8aS,8bR,9S,11aS,12aS,12bS)-10-(4-acetoxy-3-methylbutyl)-6a,8a,9-trimethyl-3,4,5,6,6a,6b,7,8,8a,8b,9,10,11a,12,12a,12b-hexadecahydro-1H-naphtho[2′,1′:4,5]indeno[2,1-b]furan-4-yl acetate, C31H48O5
  70. Crystal structure of 4,4′-(oxybis(methylene))bis(bromobenzene), C14H12Br2O
  71. Crystal structure of (N,N-dimethylsulphoxide)-[N-(3-ethoxy-2-(oxide)benzylidene)-3-methoxybenzenecarbohydrazonato-κ3N,O,O′]-dioxo-molybdenum(VI), C19H22MoN2O7S
  72. Crystal structure of dichlorido-bis(dimethyl sulphoxide-κO)-bis(4-methylbenzyl-κC1)tin(IV), C20H30Cl2O2S2Sn
  73. Crystal structure of (E)-2-amino-N′-(2-hydroxy-4-(2-(piperidin-1-yl)ethoxy)benzylidene)benzohydrazide monohydrate, C21H26N4O3 ⋅ H2O
  74. Crystal structure of chloridotris(4-chlorophenyl)(dimethyl sulfoxide-κO)tin(IV), C20H18Cl4OSSn
  75. Crystal structure of catena{di-aqua-sodium-[N-(hydroxyethyl), N-isopropyl-dithiocarbamato]}n, [C6H16NNaO2S2]n
  76. Crystal structure of 2,2,4,4,6,6-hexakis(4-chlorophenyl)-1,3,5,2,4,6-trithiatristanninane, C36H24Cl6S3Sn3
  77. Crystal structure of 6-methoxy-3-(5-(3-methoxyphenyl)-1,3,4-oxadiazol-2-yl)-4H-chromen-4-one-methanol (1/1), C20H18N2O6
  78. Crystal structure of hexanedihydrazide, C6H14N4O2
  79. Crystal structure of tert-butyl 2-(hydroxymethyl)-5-{4-[(methoxycarbonyl)amino]phenyl}-2,5-dihydro-1H-pyrrole-1-carboxylate, C18H24N2O5
  80. Crystal structure of [(Z)-O-isopropyl N-(4-nitrophenyl)thiocarbamato-κS]-(triphenylphosphine-κP)-gold(I), C28H26AuN2O3PS
  81. Crystal structure of [O-ethyl N-(4-nitrophenyl)thiocarbamato-κS](tri-4-tolylphosphine-κP)gold(I) tetrahydrofuran solvate, C30H30AuN2O3PS, C4H8O
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