Startseite Crystal structure of catena-(bis(μ2-1, 2-bis(imidazole-1-ylmethyl)benzene-κN:N′)-dichlororido-nickel(II)), C28H28Cl2N8Ni
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Crystal structure of catena-(bis(μ2-1, 2-bis(imidazole-1-ylmethyl)benzene-κN:N′)-dichlororido-nickel(II)), C28H28Cl2N8Ni

  • Ping Liu , Qiuxia Liu , Ning Zhao , Caixia An und Zhaoxun Lian EMAIL logo
Veröffentlicht/Copyright: 15. Februar 2017

Abstract

C28H28Cl2N8Ni, monoclinic, P21/c, a = 8.521(5) Å, b = 10.255(6)) Å, c = 15.414(9) Å, β = 91.209(9)°, V = 1346.6(13) Å3, Z = 2, Rgt(F) = 0.0360, wRref(F2) = 0.0916, T = 296(2) K.

CCDC no.:: 1526290

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

Table 1:

Data collection and handling.

Crystal:Green block
Size:0.32 × 0.28 × 0.27 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:9.5 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:57.6°, >99%
N(hkl)measured, N(hkl)unique, Rint:8533, 3401, 0.027
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2786
N(param)refined:178
Programs:Bruker programs [10, 11] , SHELX [12], OLEX2 [13]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.00001.00000.50000.02810(11)
Cl1−0.17547(6)1.06435(5)0.37806(3)0.04321(14)
N10.06376(19)0.83528(15)0.43302(10)0.0365(4)
N30.32413(19)0.22418(15)0.35580(10)0.0366(3)
N40.18288(17)0.09890(15)0.43864(10)0.0340(3)
N20.1612(2)0.64656(16)0.39900(12)0.0498(5)
C140.1810(2)0.19045(18)0.38008(12)0.0355(4)
H140.08950.22810.35770.043*
C110.3681(3)0.3210(2)0.29157(13)0.0456(5)
H11A0.27350.35790.26550.055*
H11B0.42550.27810.24600.055*
C30.1260(3)0.7279(2)0.46327(14)0.0468(5)
H30.14350.71040.52190.056*
C10.0603(3)0.8203(2)0.34543(13)0.0451(5)
H10.02120.88160.30610.054*
C100.4668(2)0.42926(19)0.32850(13)0.0403(4)
C120.4247(3)0.1475(2)0.40064(17)0.0549(6)
H120.53350.14720.39740.066*
C50.4057(3)0.5247(2)0.38130(15)0.0465(5)
C20.1209(3)0.7050(2)0.32390(14)0.0514(5)
H20.13270.67200.26820.062*
C130.3370(2)0.0717(2)0.45089(17)0.0539(6)
H130.37650.00890.48900.065*
C60.5012(4)0.6232(2)0.41095(18)0.0673(7)
H60.46000.68800.44600.081*
C90.6220(3)0.4353(3)0.30756(18)0.0609(7)
H90.66410.37130.27220.073*
C40.2369(4)0.5212(2)0.4072(2)0.0683(8)
H4A0.18080.45840.37120.082*
H4B0.23130.49200.46700.082*
C70.6556(4)0.6278(3)0.3898(2)0.0790(9)
H70.71930.69490.41080.095*
C80.7162(3)0.5342(3)0.3380(2)0.0791(9)
H80.82130.53720.32320.095*

Source of material

A mixture of NiCl2⋅6H2O (0.024 g, 0.1 mmol), 1,2-bis(imidazole-1-ylmethyl)benzene (1, 2-BIB) (0.046 g, 0.2 mmol), and H2O (10 mL) was stirred for about 30 min. The resulting solution was sealed in a Teflon-lined stainless autoclave and heated to 393 K for 3 days. The bottle was then rapidly cooled to ambient temperature. Green single crystals (about 76%, based on Ni input) were recovered by vacuum filtration and were dried in air.

Experimental details

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

Discussion

The design and construction of metal-organic coordination polymers is of current interest, owing to their variety of potential applications [1, 2] . 1,2-Bis(imidazole-1-ylmethyl)benzene (1,2-BIB) is a very important nitrogen-containing heterocyclic ligand, and has been widely used in the synthesis of coordination polymers [3, 4] . Its two imidazolyl groups can rotate on the -(CH2)- group to accommodate the coordination geometries of the central metal atoms in various connection mode. In the compounds reported previously, the ligand exhibits different conformations to coordinate metal centers. The results indicate that this ligand exhibits special ability to form compounds and plays an important role in determining the final molecular conformation. Our research group has reported a few coordination polymers constructed from bis(imidazolyl) ligands. The third order nonlinear optical properties of these compounds in films or in solutions were also discussed [5], [6], [7]. As a continuation of our work, we report the synthesis and structure of the title compound.

The asymmetric unit of the title structure is comprised of one Ni(II)ion, one 1,2-BIB molecule, and one chloride ion, as shown in the figure. The Ni(II) atom is located on an inversion centre (symmetry code: 0, 1, 0.5) and is placed in an octahedral coordination environment, defined by four nitrogen atoms from four different 1,2-BIB molecules and two chloride ions. N1, N1(−x, 2−y, 1−z), N4(x, 1+y, z) and N4(−x, 1−y, 1−z) atoms are located on the basal plane. Two chloride ions occupy the apical positions. The bond distances Ni-N are in the range of 2.0586(17) and 2.1008(17) Å, which are all consistent with corresponding bond lengths found in the literature [5], [6], [7]. The Ni—Cl bond distance is 2.4669(11)Å, similar to the values observed in the comparable compound [8], but longer than those found in this compound [9]. The 1,2-BIB ligand coordinates to the two metal centers in a trans configuration, similar to that found in comparable structures [5]. In the title compound, each metal center is surrounded by four 1, 2-BIB ligands, resulting in a joint-like chain structure. In another comparable structure, 1,2-BIB is connected to the Ni(II) center to form a two-dimensional layered structure [6].

Acknowledgements

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

References

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Received: 2016-6-11
Accepted: 2017-1-10
Published Online: 2017-2-15
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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