Startseite Crystal structure of poly-[(μ6-benzene-1,2,4,5-tetracarboxylato)-(μ2-1,2-bis(imidazol-1-ylmethyl)benzene)dicobalt(II)], Co2C24H16N4O8
Artikel Open Access

Crystal structure of poly-[(μ6-benzene-1,2,4,5-tetracarboxylato)-(μ2-1,2-bis(imidazol-1-ylmethyl)benzene)dicobalt(II)], Co2C24H16N4O8

  • Ping Liu , Qiuxia Liu , Ning Zhao , Caixia An und Zhaoxun Lian EMAIL logo
Veröffentlicht/Copyright: 25. Februar 2017

Abstract

Co2C24H16N4O8, triclinic, P1̅ (no. 2), a = 7.3859(13) Å, b = 9.5719(17) Å, c = 16.442(3) Å, α = 77.450(3)°, β = 85.065(3)°, γ = 84.844(3)°, V = 1127.4(3) Å3, Z = 2, Rgt(F) = 0.0457, wRref(F2) = 0.1058, T = 296(2) K.

CCDC no.:: 1527486

A part of the title 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 1:

Data collection and handling.

Crystal:Red block
Size:0.28 × 0.26 × 0.22 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:15.3 cm−1
Diffractometer, scan mode:Bruker SMART, ω-scans
2θmax, completeness:57°, >98%
N(hkl)measured, N(hkl)unique, Rint:7302, 5323, 0.028
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3694
N(param)refined:343
Programs:Bruker SADABS, SMART, SAINT [9, 10] , SHELX [11], OLEX2 [12]
Table 2:

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

AtomxyzUiso*/Ueq
Co10.97356(6)0.20552(5)0.69818(3)0.01958(12)
Co20.52786(6)0.24612(4)0.77168(3)0.01901(12)
O10.3776(3)0.1168(3)0.85465(14)0.0284(6)
O20.1343(3)0.2298(2)0.79471(13)0.0243(5)
O3−0.2199(3)0.1467(3)0.80040(13)0.0273(5)
O4−0.3165(4)0.2724(3)0.89311(16)0.0414(7)
O50.5147(3)0.1919(3)0.66590(15)0.0357(6)
O60.8000(3)0.1405(3)0.62196(15)0.0338(6)
O70.8361(3)−0.2341(2)0.40639(14)0.0277(5)
O80.8304(3)−0.0250(2)0.32035(14)0.0292(6)
N10.9002(4)0.4218(3)0.67857(17)0.0293(7)
N20.8709(5)0.6465(3)0.6898(2)0.0380(8)
N30.4485(5)0.6773(3)0.7657(2)0.0452(9)
N40.4497(4)0.4555(3)0.75251(18)0.0293(7)
C10.8631(7)0.5072(4)0.6030(2)0.0514(12)
H10.85180.47430.55460.062*
C20.8454(7)0.6452(4)0.6087(3)0.0588(14)
H20.82060.72430.56610.071*
C30.9062(5)0.5108(4)0.7282(2)0.0337(9)
H30.93220.48230.78390.040*
C40.8694(7)0.7777(4)0.7230(3)0.0585(14)
H4A0.77960.84870.69560.070*
H4B0.98780.81670.71000.070*
C50.8261(6)0.7508(4)0.8154(3)0.0440(11)
C60.9678(7)0.7111(5)0.8661(4)0.0608(14)
H61.08620.70640.84190.073*
C70.9410(10)0.6787(6)0.9502(4)0.083(2)
H71.04020.65210.98280.100*
C80.7716(13)0.6848(6)0.9868(4)0.089(2)
H80.75350.66011.04460.107*
C90.6258(9)0.7271(5)0.9390(4)0.0740(17)
H90.50920.73300.96490.089*
C100.6494(6)0.7616(4)0.8520(3)0.0468(11)
C110.4874(7)0.7995(4)0.8015(4)0.0697(17)
H11A0.38260.82500.83650.084*
H11B0.50980.88190.75680.084*
C120.3714(6)0.6798(4)0.6941(3)0.0538(13)
H120.32670.76110.65720.065*
C130.3710(6)0.5434(4)0.6858(3)0.0449(11)
H130.32490.51360.64200.054*
C140.4939(5)0.5405(4)0.7987(3)0.0382(10)
H140.55030.50910.84860.046*
C150.2079(4)0.1408(3)0.85219(19)0.0200(7)
C160.0955(4)0.0644(3)0.92556(18)0.0174(6)
C17−0.0938(4)0.0868(3)0.93520(18)0.0189(7)
C18−0.1850(4)0.0228(3)1.00859(19)0.0198(7)
H18−0.31110.03841.01430.024*
C19−0.2126(4)0.1787(4)0.87221(19)0.0225(7)
C200.6331(4)0.1410(3)0.61963(19)0.0208(7)
C210.5612(4)0.0703(3)0.55715(18)0.0179(6)
C220.6821(4)0.0173(3)0.49966(19)0.0197(7)
H220.80560.02960.49960.024*
C230.6248(4)−0.0526(3)0.44278(18)0.0180(7)
C240.7692(4)−0.1082(4)0.38491(19)0.0209(7)

Source of material

A mixture of CoCl2⋅4H2O (0.048 g, 0.2 mmol), 1,2-bis(imidazole-1-ylmethyl)benzene (1,2-BIB) (0.046 g 0.2 mmol), benzene-1,2,4,5-tetracarboxylic acid (BTA)(0.025 g, 0.1 mmol), NaOH (0.008 g, 0.2 mmol) and H2O (10 mL) were stirred for about 30 min. The resulting solution was sealed in a Teflon-lined stainless autoclave and heated to 423 K for 3 days. The autoclave was cooled to ambient temperature spontaneously. Red single crystals (about 86%, based on Co input) were recovered by vacuum filtration and drying in air.

Experimental details

C-bound H atoms were geometrically placed (C—H = 0.95 Å) and refined as riding with Uiso(H) = 1.2Ueq(C).

Discussion

The design and synthesis of coordination polymers (CPs) and especially metal organic frameworks (MOFs) have developed rapidly owing to applications of these materials in a variety of fields [1, 2] . The 1, 2-bis(imidazole-1-ylmethyl)benzene (1,2-BIB) is an important semi-flexible N-donor ligand, and some fascinating archetypal structures based on the 1,2-BIB ligand are reported [3, 4] . 1, 2, 4, 5-benzenetertracarboxylate (BTA) have also been extensively employed in the preparation of CPs [5]. Furthermore, it has been shown that the combination of carboxylate linkers along with semi-flexible N-donor ligands is a good choice for the construction of new CPs [6], [7], [8].

As shown in Figure, the asymmetric unit of the title compound contains two unique Co(II) atoms, one 1,2-BIB ligand, and two halves of BTA ligands. The Co1 center is six-coordinated with a distorted-octahedral geometry, defined by five oxygen atoms from three different BTA ligands, and one nitrogen atom from one 1,2-BIB ligand. The Co—N is 2.054(3) Å, and Co—O lengths are in the range of 1.969(2)–2.209(2) Å, which is comparable to values reported for related Co(II) complexes [4]. The Co2 atom is surrounded by one nitrogen donor from one 1,2-BIB ligand, as well as three oxygen atoms from different BTA anions, which exhibits a slightly distorted tetrahedron coordination sphere. The Co—O bond lengths range between 1.933(2) and 2.058(2) Å, while the Co—N bond length is 1.999(3) Å, which are in the normal ranges [4]. Both cyrstallographically independent BTA ligands are coordinated in an octa-dentate, coordination mode. They are located around different inversion centres of the triclinic space group (cf. the figure). Two symmetry-related carboxylate groups containing (O7, O8) of a BTA ligand are coordinated to two Co(II) atoms in chelating mode, while the other carboxylat groups are coordinated to four metal atoms in bridge-monodentate mode. The symmetry-related carboxylate groups (O1, O2) of the crystallographically independent BTA ligand act as a μ2-bridging function to connect two metal atoms in monodentated mode. Each of the two symmetry-related carboxylate groups of this second BTA ligand connect two metal atoms by its O3 and O3′ atom (cf. the figure). All these coordinations result in a two dimensional grid structure.

Acknowledgement

This work was supported financially by Natural Science Foundation of Henan Provincial Education Department (Nos. 14 A150023 and 15 A110048).

References

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Received: 2016-8-18
Accepted: 2017-1-15
Published Online: 2017-2-25
Published in Print: 2017-3-1

©2017 Ping Liu 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
  2. The crystal structure of triphenylphosphineoxide – 2,5-dichloro-3,6-dihydroxycyclohexa-2,5-diene-1,4-dione (2/1), C42H32Cl2O6P2
  3. Crystal structure of poly-[diaqua-[bis(μ2-hydroxy)-bis(μ4-3,4,5,6-tetrachlorophthalato-κ3O,O′:O′; κ2O′′:O′′′)dilanthanum(III)], C8H3Cl4LaO6
  4. Crystal structure of 1,1′-(3,4-diphenylthieno[2,3-b]thiophene-2,5-diyl)bis[1-phenyl-methanone], C32H20O2S2
  5. Crystal structure of 4a-hydroxy-9-(3,5-dibromo-phenyl)-3,4,4a,5,6,7,9,9a-octahydro-2H-xanthene-1,8-dione, C19H18Br2O4
  6. Crystal structure of 5-hydroxy-4,6,9,10-tetramethyl-1-oxo-6-vinyldecahydro-3a,9-propanocyclopenta[8]annulen-8-yl 2-((2-methyl-1-(3-methylbenzamido)propan-2-yl)thio)acetate, C34H49NO5S
  7. Crystal structure of pyridinium bis(naphthalane-2,3-diolato-κ2O,O′)borate monohydrate, C25H20BNO5
  8. Crystal structure of 1,1′-((1E,1′E)-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))bis(naphthalen-2-olato)nickel(II), C72H52N4O8Ni2
  9. The crystal structure of 3-(2-acetyl-4-butyramido-phenoxy)-2-hydroxy-N-isopropylpropan-1-aminium tetraphenylborate, C42H49BN2O4
  10. Crystal structure of 4-bromobenzyl (Z)-N′-(adamantan-1-yl)-4-phenylpiperazine-1-carbothioimidate, C28H34BrN3S
  11. Crystal structure of poly-[(μ6-benzene-1,2,4,5-tetracarboxylato)-(μ2-1,2-bis(imidazol-1-ylmethyl)benzene)dicobalt(II)], Co2C24H16N4O8
  12. Crystal structure of catena-(bis(μ2-1, 2-bis(imidazole-1-ylmethyl)benzene-κN:N′)-dichlororido-nickel(II)), C28H28Cl2N8Ni
  13. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-(4-methoxyphenyl)prop-2-en-1-one, C15H16N2O3
  14. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-phenylprop-2-en-1-one, C14H14N2O2
  15. Crystal structure of (E)-2-(4-hydroxy-3-methoxybenzylidene)-6-methoxy-3,4-dihydronaphthalen-1(2H)-one, C19H18O4
  16. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-(4-ethoxyphenyl)-3-hydroxyprop-2-en-1-one, C16H18N2O3
  17. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-(p-toly)prop-2-en-1-one, C15H16N2O2
  18. Crystal structure of 1-acetyl-3-(3-chlorophenyl)-5-(4-isopropylphenyl)-4,5-dihydro-(1H)-pyrazole, C20H21ClN2O
  19. The crystal structure of 1-methyl-2,4-dinitro-5-iodoimidazole, C4H3IN4O4
  20. The crystal structure of 4-chloro-3,5-dinitroaniline, C6H4ClN3O4
  21. Crystal structure of N,N-dimethyl-N′-(2-methyl-4-oxo-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-3(4H)-yl)formimidamide, C14H18N4OS
  22. Crystal structure of tetrakis(μ2-acetato-κ2O:O′)-bis[μ3-4-chloro-2,6-bis((methylimino)methyl)phenolato-κ2N,O:O,N′]-(μ4-oxido)tetracopper(II), C28H32Cl2Cu4N4O11
  23. Crystal structure of catena-poly[diaqua-bis(μ2-ethane-1,2-diyl-bis(pyridine-3-carboxylate-κ2N:N′))copper(II)] dinitrate, C28H28CuN6O16
  24. Synthesis and crystal structure of catena-poly[(μ2-nicotinato-κ2O,O′: κ1N)-(nitrato-κ1O)-(bis(2-benzimidazol-ylmethyl)amine-κ3N,N′,N′′)lead(II)], C22H18N7O5Pb
  25. The twinned crystal structure of (4SR)-7-benzyl-2,4,8,8-tetramethyl-7,8-dihydroimidazo[5,1-c][1,2,4]triazine-3,6(2H,4H)-dione, C16H20N4O2
  26. Crystal structure of (Z)-3-hydroxy-3-(4-methoxyphenyl)-1-(pyridin-2-yl)prop-2-en-1-one, C15H13NO3
  27. Crystal structure of 2-amino-4-(2,3-dichlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H12Cl2N2O2
  28. Crystal structure of catena-poly[(μ2-butane-1,4-diyl-bis(pyridine-3-carboxylato-κN))silver(I)] tetrafluoroborate, C16H16AgN2O4BF4
  29. Crystal structure of poly[diaqua-(1,10-phenanthroline-κ2N,N′)-(μ2-2,5-dihydroxytere-phthalato)-bis(μ4-2,5-dihydroxyterephthalato)dicerium(III)], C24H16CeN2O10
  30. Crystal structure of 5,7,4′-trihydroxy-3,8,3′-trymethoxyflavone, C18H16O8
  31. Crystal structure of N-(3,4-dichlorobenzylidene)-4-methylaniline, C14H11Cl2N
  32. Crystal structure of 4-(3-Methoxy-phenyl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydro-quinoline-3-carboxylic acid ethyl ester, C22H27NO4
  33. Crystal structure of 2-amino-4-(3-fluorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13FN2O2
  34. Crystal structure of 1,1,(3,4-dihydroxythieno[2,3-b] thiophene-2,5-diyl)bis(2-bromoethanone), C10H6Br2O4S2
  35. The crystal structure of N,N′-(4,4′-oxydibenzyl)-bisisonicotinamide 3.5 hydrate, C24H24N4O6
  36. Crystal structure of catena-poly[hexakis(μ2-chlorido)-hexakis(4-(1H-pyrazol-5-yl)pyridine-κN)tricadmium(II)], Cd3C48H42Cl6N18
  37. Crystal structure of 2-(4-(dimethylamino)phenyl)-1,3-dimethyl-1H-perimidin-3-ium iodide, C21H22I1N3
  38. Crystal structure of 4-(1,3-dimethyl-2,3-dihydro-1H-perimidin-2-yl)benzonitrile, C20H17N3
  39. Crystal structure of tetrakis(μ2-acetato-κ2O:O′)-bis(2,2′-sulfonyldipyrazine-κ1N)dicopper(II), C24H24Cu2N8O12S2
  40. Crystal structure of 1-(4-chlorophenyl)-6,8-diphenyl-1H-pyrazolo[4,3-c]quinoline, C28H18ClN3
  41. Crystal structure of methyl 3-((1-(2-(methoxycarbonyl)benzyl)-1H-1,2,3-triazol-4-yl)methoxy)-2-naphthoate, C24H21N3O5
  42. Crystal structure of (tris(2-pyridylmethyl)amine-κ4N,N′,N′′,N′′′′)-chloranilato-κO,O′-zinc(II) – methanol (1/1), C25H22Cl2N4O5Zn
  43. Crystal structure of 1,1-dimethyl-3-(4-methoxyphenyl)urea, C10H14N2O2
  44. Crystal structure of 4a-Hydroxy-9-(2-nitro-phenyl)-3,4,4a,5,6,7,9,9a-octahydro-2H-xanthene-1,8-dione, C19H19NO6
  45. Crystal structure of chlorido-(η6–1-isopropyl-4-methyl benzene)-(1-(pyridin-2-yl)-N-(p-tolyl)methanimine-κ2N,N′)ruthenium(II) hexafluorophosphate(V), C23H26ClF6N2PRu
  46. Crystal structure of phenyl(2-phenyl-2,3-dihydro-1H-perimidin-2-yl)methanone, C24H18N2O
  47. Crystal structure of (E)-3-methyl-4-((3-(5-methyl-1-phenyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazol-4-yl)methylene)-1-phenyl-1H-pyrazol-5(4H)-one, C29H23N7O
  48. Crystal structure of 2-(4-(2-butyl-1,3-dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-6-yl)piperazin-1-yl)-2-oxoethyldiethylcarbamodithioate, C27H34N4O3S2
  49. Crystal structure of poly-[diaqua-bis(μ-4,4′-bipyridine-κ2N:N′)cobalt(II)] bis(4-chlorobenzenesulfonate) – 4,4′-bipyridine – water (1/1/2), C42H40Cl2CoN6O10S2
  50. Crystal structure of (η6-benzene)-(N-(2,6-dimethylphenyl)-1-(pyridin-2-yl)methanimine-κ2N,N′)ruthenium(II) perchlorate monohydrate, C20H20Cl2N2O5Ru
  51. Crystal structure of 4,10,16,22-tetrahydroxy-6,12,18,24-tetramethoxy-2,8,14,20-tetraethylphenylresorcin[4]arene – ethyl acetate (1/1), C68H72O10
  52. Crystal structure of chlorido-(N-(2,5-dichlorophenyl)-1-(pyridin-2-yl)methanimine-κ2N,N′)(η6-1-isopropyl-4-methyl benzene) ruthenium (II) tetrafluoroborate, C22H22Cl3N2BF4Ru
  53. Crystal structure of 3-(5-methyl-1-p-tolyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazole-4-carbaldehyde, a rare Z′ = 3 structure, C20H17N5O
  54. Crystal structure of 5-(5-(4-chlorophenyl)-1-phenyl-1H-pyrazol-3-yl)-N-phenyl-1,3,4-thiadiazol-2-amine, C23H16ClN5S
  55. Crystal structure of 7-hydroxy-3-(4-hydroxyphenyl)-4H-1-benzopyran-4-one-N,N-dimethylformamide (1/1), C18H17NO5
  56. Crystal structure of halogen-bonded 2-chloro-1,10-phenanthroline—1,4-diiodotetrafluorobenzene (2/1), C30H14Cl2F4I2N4
  57. Crystal structure of 1-(4,4-dimethyl-2,6-dithioxo-1,3,5-triazinan-1-yl)-3-(diethylaminocarbonyl)thiourea, C11H20N6OS3
  58. Crystal structure of methyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C18H15FN2O2
  59. Crystal structure of 1,1-dimethyl-3-(4-methylphenyl)urea, C10H14N2O
  60. Crystal structure of yttrium gallium antimonide, Y5Ga1.24Sb2.77
  61. Crystal structure of 2-(bis(4-methoxyphenyl)amino)-2-oxoacetic acid, C16H15NO5
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