Home Crystal structure of catena-poly[μ2-2,2′-(1,3-phenylene)diacetato-κ4O,O′:O′′,O′′′)-(μ2-1,6-bis(2-methyl-1H-benzo[d]imidazol-1-yl)hexane-κ2N:N′)cadmium(II)], C32H34CdN4O4
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Crystal structure of catena-poly[μ2-2,2′-(1,3-phenylene)diacetato-κ4O,O′:O′′,O′′′)-(μ2-1,6-bis(2-methyl-1H-benzo[d]imidazol-1-yl)hexane-κ2N:N′)cadmium(II)], C32H34CdN4O4

  • Lu Liu EMAIL logo , Chunying Xu , Huiling Gao and Yuping Zhang
Published/Copyright: April 7, 2017

Abstract

C32H34CdN4O4, triclinic, P1̅ (no. 2), a = 10.120(2) Å, b = 12.223(2) Å, c = 13.403(3) Å, α = 105.70(3)°, β = 98.41(3)°, γ = 108.04(3)°, V = 1468.9(7) Å3, Z = 2, Rgt(F) = 0.0625, wRref(F2) = 0.1721, T = 293(2) K.

CCDC no.:: 1538605

Table 1

Data collection and handling.

Crystal:Colourless irregular-shaped
Size:0.20 × 0.17 × 0.15 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:7.9 cm−1
Diffractometer, scan mode:Rigaku Saturn, φ and ω
2θmax, completeness:55.8°, >98%
N(hkl)measured, N(hkl)unique, Rint:13952, 6900, 0.056
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3943
N(param)refined:372
Programs:Crystal Clear [10], SHELX [11]

The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 2

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

AtomxyzUiso*/Ueq
Cd10.24037(4)0.47326(4)0.73938(3)0.04303(17)
N10.0826(5)0.3139(5)0.5948(4)0.0482(12)
N2−0.0446(6)0.1907(5)0.4308(4)0.0572(14)
N30.3854(5)0.3668(4)0.7662(4)0.0390(11)
N40.5153(5)0.2752(5)0.8350(4)0.0444(12)
C10.3033(7)−0.1046(6)0.8413(5)0.0610(18)
H1A0.2261−0.13060.87490.073*
H1B0.3752−0.13680.86230.073*
C20.3701(7)0.0342(6)0.8838(5)0.0563(17)
H2A0.30900.06600.84690.068*
H2B0.37230.06230.95920.068*
C30.5190(7)0.0863(6)0.8712(5)0.0567(17)
H3A0.51810.05480.79640.068*
H3B0.58160.05870.91170.068*
C40.5814(7)0.2269(6)0.9088(5)0.0522(16)
H4A0.56660.25900.97910.063*
H4B0.68400.25440.91530.063*
C50.5437(6)0.2719(6)0.7370(5)0.0435(14)
C60.6354(7)0.2276(7)0.6840(6)0.0625(19)
H60.68760.18710.71160.075*
C70.6437(8)0.2473(8)0.5894(6)0.077(2)
H70.70400.21950.55200.092*
C80.5669(7)0.3068(7)0.5461(5)0.0616(19)
H80.57700.31800.48140.074*
C90.4758(7)0.3494(6)0.5976(5)0.0531(16)
H90.42430.38950.56880.064*
C100.4631(6)0.3306(5)0.6943(5)0.0433(14)
C110.4210(6)0.3319(5)0.8484(5)0.0423(13)
C120.3612(7)0.3515(6)0.9434(5)0.0528(16)
H12A0.31280.40770.94310.079*
H12B0.43780.38441.00730.079*
H12C0.29440.27500.94140.079*
C13−0.2440(7)0.1600(6)0.2799(5)0.0570(17)
H13A−0.31210.11920.31420.068*
H13B−0.23120.24580.30300.068*
C14−0.1010(7)0.1471(7)0.3137(5)0.067(2)
H14A−0.11270.06190.28510.080*
H14B−0.03150.19300.28310.080*
C15−0.0846(7)0.1250(6)0.4979(6)0.0541(16)
C16−0.1798(7)0.0090(7)0.4810(7)0.072(2)
H16−0.2333−0.04220.41230.087*
C17−0.1938(8)−0.0286(8)0.5660(8)0.081(3)
H17−0.2568−0.10690.55560.097*
C18−0.1148(8)0.0483(8)0.6695(7)0.076(2)
H18−0.12770.02120.72710.092*
C19−0.0181(7)0.1638(7)0.6876(6)0.0578(18)
H190.03590.21430.75640.069*
C20−0.0035(6)0.2029(6)0.5998(5)0.0496(15)
C210.0548(7)0.3030(7)0.4924(5)0.0536(16)
C220.1200(8)0.3987(7)0.4475(6)0.071(2)
H22A0.04560.41000.40290.106*
H22B0.18180.37430.40570.106*
H22C0.17490.47400.50490.106*
C230.0368(6)0.5186(6)0.8294(5)0.0474(15)
C24−0.0941(7)0.5238(7)0.8715(7)0.067(2)
H24A−0.17840.45680.82270.081*
H24B−0.08280.51130.94020.081*
C25−0.1199(6)0.6396(6)0.8847(5)0.0475(15)
C26−0.0428(7)0.7435(7)0.9730(6)0.064(2)
H260.03030.74251.02320.076*
C27−0.0733(8)0.8475(7)0.9869(6)0.072(2)
H27−0.02120.91621.04670.087*
C28−0.1795(7)0.8512(6)0.9138(6)0.0620(19)
H28−0.19770.92290.92410.074*
C29−0.2596(6)0.7509(6)0.8256(5)0.0483(15)
C30−0.2279(6)0.6465(6)0.8122(5)0.0473(15)
H30−0.28090.57810.75230.057*
C31−0.3828(6)0.7502(7)0.7478(6)0.067(2)
H31A−0.36800.72830.67630.080*
H31B−0.38580.83170.76610.080*
C32−0.5256(6)0.6608(6)0.7484(5)0.0445(14)
O10.1010(5)0.4558(5)0.8589(4)0.0611(13)
O20.0716(5)0.5715(4)0.7654(4)0.0607(13)
O3−0.5518(4)0.6603(4)0.8368(3)0.0530(11)
O4−0.6115(4)0.5900(4)0.6611(3)0.0552(12)

Source of material

The title complex was prepared under the hydrothermal conditions. A mixture of 1,6-bis(2-methyl-1H-benzo[d]imidazol-1-yl)hexane (34.6 mg, 0.1 mmol), phenylenediacetic acid (19.2 mg, 0.1 mmol), Cd(Ac)2⋅2H2O (53.3 mg, 0.2 mmol), sodium hydroxide solution (0.2 mol/L, 1 mL) and H2O (10 mL) were placed in a Teflon-lined stainless steel vessel, heated to 160 °C for 3 day and then cooled to room temperature. Colorless block crystals of the title compound were acquired.

Experimental details

The structure was solved by direct methods and refined with a full-matrix least-squares technique SHELXL software package [10]. The hydrogen atoms were placed at calculated positions and refined as riding atoms.

Discussion

Great attention in the design and construction of coordination networks has been attracted owing to their intriguing structural motifs and potential applications [1], [2], [3], [4]. The design of effective ligands are crucial to the structural tuning of the resulting complexes [5], [6], [7], [8]. The bis(methyl-benzimidazole) ligand with a −(CH2)6 spacer (hbmb) are a good choice. The characteristics are as follows: (a) the longer alkyl spacers −(CH2)6 often causes structural diversities. (b) the 2-position substituent methyl may be conducive to enrich coordination ability of hbmb with metal ions.

The asymmetric unit of the title complex contains one Cd(II) atom, one hbmb ligand and one 2,2′-(1,3-phenylene)diacetato ligand (phda). The figure illustrates the coordination environment of the Cd(II) ions. The Cd center is six-coordinated by four oxygen atoms (O1, O2, O3A and O4A) belonging to two symmetry related phda ligands as well as two nitrogen atoms two symmetry related hbmb ligands (cf. the figure). The Cd—O and Cd—N bond distances lie in the ranges of 2.293(4)–2.441(4) Å and 2.286(5)–2.293(4) Å, respectively, which is well comparable with reported ones [9]. The hbmb adopts symmetrical trans-conformation with the Ndonor⋯N—Csp3⋯Csp3 torsion angle of 61.297°. phda adopts an asymmetric conformation. In the title complex, each m-phda2− anion links two Cd(II) atoms resulting in a 1D chain structure with the Cd⋯Cd distance of 10.12 Å. Two Cd(II) atoms and two hbmb ligands form a 26-membered ring. The 26-membered rings and m-phda2− anion are further interlinked via metal knots yielding a double-chain structure.

Acknowledgement

This work was financially supported by the research start-up fund of Henan Institute of Science and Technology, the key scientific research project funding scheme of colleges and universities of henan province (16A150007) and the Iconic Innovation Project of Henan Institute of Science and Technology (2015BZ02).

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Received: 2016-10-21
Accepted: 2017-3-23
Published Online: 2017-4-7
Published in Print: 2017-5-24

©2017 Lu Liu et al., published by De Gruyter, Berlin/Boston

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

Articles in the same Issue

  1. Cover and Frontmatter
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  57. Crystal structure of 4-(2-ammonioethyl)morpholin-4-ium dichloride monohydrate, C6H18Cl2N2O2
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  60. Crystal structure of 4-bromo-2-(1H-pyrazol-3-yl)phenol, C9H7BrN2O
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