Home Physical Sciences Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraquamanganese(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34MnN2O14
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Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraquamanganese(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34MnN2O14

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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 230 Issue 4

Abstract

C28H34MnN2O14, monoclinic, P21/c (no. 14), a = 11.578(1) Å, b = 11.946(1) Å, c = 11.100(1) Å, β = 95.803(1)°, V = 1527.3 Å3, Z = 2, Rgt(F) = 0.0284, wRref(F2) = 0.1146, T = 296 K.

CCDC no.:: 1267/4349

Source of material

MnCl2·4H2O (0.5 mmol, 0.101 g), H2cmb (3-(carboxy-methyl)benzoic acid, 1.0 mmol, 0.182 g) and 4,4′-bipy (1.0 mmol, 0.157 g) were dissolved in 20 mL ethanol-H2O (ν:ν = 1:1) and then the pH of the mixture was adjusted with KOH (0.1 mol·L−1) to pH = 7.5. After that, the solution was sealed in a 25 mL Teflon reactor and kept under autogeneous pressure at 403 K for 5 days. After cooling to room temperature at a rate of 279 K·h−1, pink block shaped crystals were obtained. Yield: 88 mg (26%, based on Mn). Elemental Analysis calcd. for C28H34MnN2O14(%): C, 49.64; H, 5.06. Found: C, 49.70; H, 5.11.

Table 1

Data collection and handling.

Crystal:Pink blocks, size 0.22×0.23×0.34 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:5.05 cm−1
Diffractometer, scan mode:Bruker APEX II CCD, φ and ω
2θmax:50.98°
N(hkl)measured, N(hkl)unique:7873, 2838
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2575
N(param)refined:206
Programs:SHELX [3]
Table 2

Atomic coordinates and displacement parameters (in Å2).

AtomSitexyzUiso
H(3)4e0.70520.49520.13780.088
H(1W)4e0.98921.14460.18540.058
H(2W)4e1.05941.06610.24380.058
H(4W)4e1.01940.82100.14810.064
H(3W)4e0.97300.77640.04270.064
H(6W)4e0.95880.33290.14300.062
H(5W)4e0.85750.31380.19750.062
H(1)4e0.79171.14860.07570.062
H(2)4e0.59611.14680.08570.060
H(4)4e0.58120.8581−0.09240.054
H(5A)4e0.77800.8653−0.09370.055
H(7)4e0.42640.49710.10150.046
H(9)4e0.18600.32420.25740.055
H(10)4e0.32880.21120.35210.058
H(11)4e0.52090.23850.31900.052
H(13A)4e0.23110.56320.07660.050
H(13B)4e0.14200.51640.16150.050
Table 3

Atomic coordinates and displacement parameters (in Å2).

AtomSitexyzU11U22U33U12U13U23
Mn(1)2a1100.0167(2)0.0293(2)0.0287(2)−0.00082(9)0.0026(1)0.00066(9)
N(1)4e0.8053(1)1.00672(9)−0.0087(1)0.0225(7)0.0369(8)0.0414(8)−0.0025(4)0.0032(6)−0.0026(5)
O(1)4e0.15974(9)0.4565(1)−0.1075(1)0.0315(6)0.0637(8)0.0416(7)−0.0097(5)0.0053(5)−0.0028(6)
O(2)4e0.0546(1)0.3679(1)0.0169(1)0.0430(7)0.0471(7)0.0516(7)−0.0171(5)0.0105(5)−0.0068(5)
O(3)4e0.6351(1)0.4841(1)0.1352(2)0.0292(7)0.0698(9)0.077(1)−0.0061(6)0.0077(7)0.0199(7)
O(4)4e0.6917(1)0.3222(1)0.2193(2)0.0363(7)0.0584(8)0.100(1)0.0064(6)0.0117(7)0.0083(7)
O(5)4e1.01502(9)1.07966(9)0.18078(9)0.0389(6)0.0433(6)0.0323(5)0.0101(4)−0.0010(4)−0.0036(4)
O(6)4e0.9970(1)0.83620(8)0.0764(1)0.0564(7)0.0339(6)0.0369(6)−0.0057(5)−0.0030(5)0.0036(4)
O(7)4e0.92514(9)0.29593(9)0.1921(1)0.0384(6)0.0431(6)0.0424(6)0.0046(5)0.0030(5)−0.0015(4)
C(1)4e0.7490(1)1.0883(1)0.0421(2)0.0223(7)0.0430(9)0.088(1)−0.0037(6)0.0003(8)−0.0240(9)
C(2)4e0.6308(1)1.0881(1)0.0477(2)0.0229(7)0.0411(9)0.085(1)0.0000(6)0.0025(8)−0.0231(8)
C(3)4e0.5637(1)1.0018(1)−0.0024(2)0.0228(9)0.0354(9)0.0297(8)−0.0031(5)0.0010(6)0.0010(5)
C(4)4e0.6222(1)0.9184(1)−0.0563(2)0.0265(7)0.0524(9)0.058(1)−0.0116(7)0.0090(7)−0.0238(8)
C(5)4e0.7410(1)0.9234(1)−0.0572(2)0.0281(8)0.052(1)0.058(1)−0.0080(7)0.0133(7)−0.0213(8)
C(6)4e0.4924(1)0.3707(1)0.2074(1)0.0321(7)0.0426(8)0.0351(7)−0.0049(6)0.0054(6)−0.0090(6)
C(7)4e0.4061(1)0.4391(1)0.1511(1)0.0328(8)0.0451(9)0.0361(8)−0.0065(6)0.0035(6)−0.0052(6)
C(8)4e0.2902(1)0.4223(1)0.1678(1)0.0309(8)0.0444(8)0.0354(8)−0.0049(6)0.0048(6)−0.0130(6)
C(9)4e0.2630(1)0.3363(2)0.2442(2)0.0379(8)0.057(1)0.0443(9)−0.0129(7)0.0116(7)−0.0083(7)
C(10)4e0.3486(2)0.2682(2)0.3010(2)0.051(1)0.050(1)0.0461(9)−0.0112(8)0.0110(8)0.0015(7)
C(11)4e0.4634(1)0.2849(1)0.2818(2)0.0421(9)0.0440(9)0.0435(9)−0.0030(7)0.0032(7)−0.0034(7)
C(12)4e0.6165(1)0.3895(1)0.1883(2)0.0324(8)0.0463(8)0.0411(8)−0.0031(7)0.0041(6)−0.0083(7)
C(13)4e0.1965(2)0.4953(1)0.1045(2)0.033(1)0.043(1)0.050(1)−0.0017(6)0.0037(8)−0.0139(6)
C(14)4e0.1313(1)0.4353(1)−0.0031(1)0.0235(7)0.0351(7)0.0442(8)0.0003(6)0.0038(6)−0.0050(6)

Discussion

In the coordination chemistry, the investigation of transition metal complexes containing coordinated carboxylate ligands is a continuously interesting subject. Polycarboxylate ligands are used as linkers in solid aggregates. The presence of two or more carboxylate groups in different orientations permits the construction of one-, two- or three dimensional frameworks, which can be further reinforced by the presence of intermolecular hydrogen bonds [1]. For example, a flexible aromatic acid that contains two carboxylic groups is 3-(carboxymethyl)benzoic acid (H2cmb). However, the only metal complex which has been published is a binuclear zinc(II) compound [2]. The proper synthetic methods might be difficult to find. In this paper, we describe a complex compound containing H2cmb {[Mn(4,4′-bipy)(H2O)4]·2(Hcmb)·2H2O}n (4,4′-bipy = 4,4′-bipyridine). The asymmetric unit of the title compound contains one half MnII ion, one half 4,4′-bipy ligand, two water ligands, one 3-(carboxylatomethyl)benzoic acid anion (Hcmb–) and one lattice water molecules. In the coordination sphere the doubly charged manganese complex cation, each MnII is located in a distorted octahedron formed by two nitrogen atoms of two 4,4′-bipy molecules and four water ligands. 4,4′-bipy acts as a μ2 ligand and they connect the adjacent MnII to form a one dimensional linear chain structure parallel to the crystallographic a axis (Fig.). The partly deprotonated 3-(carboxylatomethyl)benzoic acid mono anion (Hcmb–) does not participate in coordination and serves as a counterion. They are arranged regularly among the chain structures and are involved in intermolecular O–H⋯O hydrogen bonds with coordinated and uncoordinated water molecules. The chain structure is stabilized and further connected into a three dimensional network via these hydrogen bonds.

Corresponding author: Zhong-Xiang Du, The Institute of the Research on the Design and Application of New Materials, Luoyang Normal University, Luoyang 471022, Henan Province, P. R. China, e-mail: ; and College of Chemistry and Chemical Engineering, Luoyang Normal University

Acknowledgments:

This work was supported by the Cultivation Foundation of Luoyang Normal University (No. 10000857).

References

1. Mehrotra, R. C.; Bohra, R.: Metal Carboxylates, Academic Press, London, 1983.Search in Google Scholar

2. Burrows, A. D.; Harrington, R. W.; Mahon, M. F.; Price, C. E.: The influence of hydrogen bonding on the structure of zinc co-ordination polymers. J. Chem. Soc., Dalton Trans. (2000) 3845–3854..Search in Google Scholar

3. Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Search in Google Scholar PubMed

Received: 2015-5-27
Accepted: 2015-6-26
Published Online: 2015-10-15
Published in Print: 2015-12-1

©2015 Jun-Xia Li et al., published by De Gruyter.

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

Articles in the same Issue

  1. Frontmatter
  2. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidozincate(II), C40H40Br4P2Zn
  3. Crystal structure of chlorido-(2-ethoxy-6-(((quinolin-8-yl)methyl)-phenolato-κ3N,N′,O)-copper(II), C18H15ClCuN2O2
  4. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidocobaltate(II), C40H40Br4CoP2
  5. Crystal structure of di(pyrrolidin-1-yl)methane-thione, C9H16N2S
  6. Crystal structure of ammonium phenylglyoxylate, C8H9NO3
  7. Crystal structure of 2-hydroxy-2-methyl-2-phenyl acetic acid hemihydrate, C9H11O3.50
  8. Crystal structure of 2-((E)-2-(1H-benzo[d]imidazol-2-yl)vinyl)-1H-benzo[d]imidazolium dichloride dihydrate, C16H18Cl2N4O2
  9. Crystal structure of 1,2-dimethylimidazolium iodide, C5H9IN2
  10. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraqua-cobalt(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34CoN2O14
  11. Crystal structure of bis(2,2′-bipyridine-κ2N,N′)-bis(thiophene-3,4-dicarboxylato-κ2O,O′)-cadmium(II), C32H22CdN4O8S2
  12. Crystal structure of tetraaqua-(4,4′-diamino-1,1′-biphenyl-2,2′-disulfonato-κN)(4,4′-bipyridyl-κN)zinc(II) trihydrate, C22H32N4O13S2Zn
  13. Crystal structure of poly[[[(1,3-dimethyl-2-imidazolidinone-κ1O11) zinc(II)]-μ-1,4-benzenedi-carboxylato-κ4O1,O2:O3,O4]—1,3-dimethyl-2-imidazolidinone (1:1)], [Zn(C5H10N2O)(C8H4O4)]· C5H10N2O, C18H24N4O6Zn
  14. Crystal structure of poly[[(1,3-dimethyl-2-imidazolidinone-κ1O) zinc(II)]-μ-furan-2,5-dicarboxylato-κ4O,O′:O′′,O′′′], [Zn(C5H10N2O)(C6H2O5)], C22H24N4O12Zn2
  15. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraquamanganese(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34MnN2O14
  16. Crystal structure of chlorido-tricarbonyl-bis(2-pyridylmethanone-N,N′)-rhenium(I), C14H8ClN2O4Re
  17. Crystal structure of (2-(benzoyl)phenolato-κ2O,O′)-trans-dichlorido -cis- bis(methoxido) niobium(V), C15H15Cl2NbO4
  18. Crystal structure of potassium diaqua dihydroxy(methylenediphosphonato-κ2-O,O′)cobaltate(III), CH10CoKO10P2
  19. Crystal structure of hexakis(4-(dimethylamino)pyridin-1-ium) decavanadate-water (1:16), C42H98N12O44V10
  20. Crystal structure of 4-diethylaminobenzaldehyde isonicotinoylhydrazone monohydrate, C17H20N4O·H2O, C17H22N4O2
  21. Crystal structure of bis[μ-1-[(2-ethyl-1H-imidazol-1-yl)methyl]-1H-benzotriazole-κ2N:N′]bis[dibromido]dimercury(II), C24H26Br4Hg2N10
  22. Crystal structure of poly{bis-[(4,4′-biphenyl-dicarboxylate-κ2O:O′)-μ-1,1′-oxy-bis-(ethane-2,1-diyl)-bis-(1H-imidazole)-κ2N:N′] zinc(II)}dihydrate, C48H48N8O12Zn2
  23. Crystal structure of sodium poly[(μ4-2,2′,2′′-nitrilotriacetato-κ4O,O′,O′′,N)magnesium(II)] monohydrate
  24. The crystal structure of 1-(2-(2-chloroethoxy)phenyl)ethanone
  25. The crystal structure of tris(μ2-1,3-bis(4,4,4-Trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-/κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-O,O′)-diterbium(III)
  26. Crystal structure of (S)-2-(2,2′-diethoxy-[1,1′-binaphthalen]-6-yl)-4,4,5,5-tetra-methyl-2-imidazoline-1-oxyle, C31H33N2O3
  27. Crystal structure of cis-tetrachloridobis-(pyridine-κN)platinum(IV), C10H10Cl4N2Pt
  28. Crystal structure of catena-poly[aqua-(μ2-5-norbornene-2,3-dicarboxylato-κ3O,O′:O′′)-(1,10-phenanthroline-κ2N,N′)zinc(II)], [Zn(C9H8O4)(C12H8N2)(H2O)]n
https://doi.org/10.1515/ncrs-2014-9130
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Articles in the same Issue

  1. Frontmatter
  2. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidozincate(II), C40H40Br4P2Zn
  3. Crystal structure of chlorido-(2-ethoxy-6-(((quinolin-8-yl)methyl)-phenolato-κ3N,N′,O)-copper(II), C18H15ClCuN2O2
  4. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidocobaltate(II), C40H40Br4CoP2
  5. Crystal structure of di(pyrrolidin-1-yl)methane-thione, C9H16N2S
  6. Crystal structure of ammonium phenylglyoxylate, C8H9NO3
  7. Crystal structure of 2-hydroxy-2-methyl-2-phenyl acetic acid hemihydrate, C9H11O3.50
  8. Crystal structure of 2-((E)-2-(1H-benzo[d]imidazol-2-yl)vinyl)-1H-benzo[d]imidazolium dichloride dihydrate, C16H18Cl2N4O2
  9. Crystal structure of 1,2-dimethylimidazolium iodide, C5H9IN2
  10. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraqua-cobalt(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34CoN2O14
  11. Crystal structure of bis(2,2′-bipyridine-κ2N,N′)-bis(thiophene-3,4-dicarboxylato-κ2O,O′)-cadmium(II), C32H22CdN4O8S2
  12. Crystal structure of tetraaqua-(4,4′-diamino-1,1′-biphenyl-2,2′-disulfonato-κN)(4,4′-bipyridyl-κN)zinc(II) trihydrate, C22H32N4O13S2Zn
  13. Crystal structure of poly[[[(1,3-dimethyl-2-imidazolidinone-κ1O11) zinc(II)]-μ-1,4-benzenedi-carboxylato-κ4O1,O2:O3,O4]—1,3-dimethyl-2-imidazolidinone (1:1)], [Zn(C5H10N2O)(C8H4O4)]· C5H10N2O, C18H24N4O6Zn
  14. Crystal structure of poly[[(1,3-dimethyl-2-imidazolidinone-κ1O) zinc(II)]-μ-furan-2,5-dicarboxylato-κ4O,O′:O′′,O′′′], [Zn(C5H10N2O)(C6H2O5)], C22H24N4O12Zn2
  15. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraquamanganese(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34MnN2O14
  16. Crystal structure of chlorido-tricarbonyl-bis(2-pyridylmethanone-N,N′)-rhenium(I), C14H8ClN2O4Re
  17. Crystal structure of (2-(benzoyl)phenolato-κ2O,O′)-trans-dichlorido -cis- bis(methoxido) niobium(V), C15H15Cl2NbO4
  18. Crystal structure of potassium diaqua dihydroxy(methylenediphosphonato-κ2-O,O′)cobaltate(III), CH10CoKO10P2
  19. Crystal structure of hexakis(4-(dimethylamino)pyridin-1-ium) decavanadate-water (1:16), C42H98N12O44V10
  20. Crystal structure of 4-diethylaminobenzaldehyde isonicotinoylhydrazone monohydrate, C17H20N4O·H2O, C17H22N4O2
  21. Crystal structure of bis[μ-1-[(2-ethyl-1H-imidazol-1-yl)methyl]-1H-benzotriazole-κ2N:N′]bis[dibromido]dimercury(II), C24H26Br4Hg2N10
  22. Crystal structure of poly{bis-[(4,4′-biphenyl-dicarboxylate-κ2O:O′)-μ-1,1′-oxy-bis-(ethane-2,1-diyl)-bis-(1H-imidazole)-κ2N:N′] zinc(II)}dihydrate, C48H48N8O12Zn2
  23. Crystal structure of sodium poly[(μ4-2,2′,2′′-nitrilotriacetato-κ4O,O′,O′′,N)magnesium(II)] monohydrate
  24. The crystal structure of 1-(2-(2-chloroethoxy)phenyl)ethanone
  25. The crystal structure of tris(μ2-1,3-bis(4,4,4-Trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-/κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-O,O′)-diterbium(III)
  26. Crystal structure of (S)-2-(2,2′-diethoxy-[1,1′-binaphthalen]-6-yl)-4,4,5,5-tetra-methyl-2-imidazoline-1-oxyle, C31H33N2O3
  27. Crystal structure of cis-tetrachloridobis-(pyridine-κN)platinum(IV), C10H10Cl4N2Pt
  28. Crystal structure of catena-poly[aqua-(μ2-5-norbornene-2,3-dicarboxylato-κ3O,O′:O′′)-(1,10-phenanthroline-κ2N,N′)zinc(II)], [Zn(C9H8O4)(C12H8N2)(H2O)]n
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