Startseite Crystal structure of diaqua-dinitrato-κO-bis(4-(1H-pyrazol-3-yl)pyridine-κN)manganese(II), C16H18MnN8O8
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Crystal structure of diaqua-dinitrato-κO-bis(4-(1H-pyrazol-3-yl)pyridine-κN)manganese(II), C16H18MnN8O8

  • Guang-Zhou Zhu , Chun-Ling Li , Yu-Yu Feng , Xiao-Wan Feng und Feng-Lei Yang EMAIL logo
Veröffentlicht/Copyright: 8. Oktober 2016

Abstract

C16H18MnN8O8, monoclinic, P21/c (no. 14), a = 7.3533(3) Å, b = 11.8078(5) Å, c = 12.6376(5) Å, β = 110.028(2)°, V = 1030.92(7) Å3, Z = 2, Rgt(F) = 0.0312, wRref(F2) = 0.1166, S = 1.043, T = 296(2) K.

CCDC no.:: 1503288

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:Colourless blocks Size 0.27 × 0.23 × 0.14 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:7.1 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:54°, >99%
N(hkl)measured, N(hkl)unique, Rint:8857, 2236, 0.017
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2055
N(param)refined:151
Programs:SHELX [7], Diamond [8], Bruker programs [9]
Table 2

Fractional atomic coordinates and displacement parameters (in Å2).

AtomxyzUiso*/Ueq
Mn10.50000.50000.50000.02988(16)
O10.8650(2)0.56665(13)0.3902(2)0.0901(6)
O20.89154(16)0.40273(11)0.32733(10)0.0498(3)
O30.66127(14)0.43670(10)0.39142(10)0.0442(3)
O40.74584(15)0.48553(10)0.65517(11)0.0442(3)
H10.70710.47440.70790.053*
H20.84990.50460.65790.053*
N10.57536(16)0.68401(10)0.48636(10)0.0346(3)
N20.74416(16)1.07534(10)0.37029(10)0.0354(3)
N30.81112(18)1.18097(10)0.40000(12)0.0405(3)
H3A0.82241.23310.35070.049*
N40.80747(17)0.47020(12)0.37065(11)0.0358(3)
C10.6512(2)0.74828(13)0.57831(13)0.0408(4)
H1A0.66530.71650.64800.049*
C20.7093(2)0.85873(13)0.57546(12)0.0390(3)
H2B0.76150.89940.64200.047*
C30.68967(16)0.90944(11)0.47217(11)0.0301(3)
C40.60762(19)0.84342(12)0.37653(12)0.0346(3)
H4A0.58810.87350.30550.042*
C50.5554(2)0.73315(12)0.38756(12)0.0363(3)
H5A0.50300.69030.32240.044*
C60.75293(18)1.02668(13)0.46760(12)0.0312(3)
C70.82469(19)1.10240(13)0.55718(13)0.0389(3)
H7A0.84401.08900.63280.047*
C80.8602(2)1.19959(13)0.51055(14)0.0433(4)
H8A0.90951.26650.54830.052*

Source of material

Firstly, 3-(4-pyridyl)pyrazole was prepared by using 4-acetyl pyridine, N,N-dimethylacetamide, diethyl methylal and hydrazine under conditions previously discribed [1]. Then, the 1 mL aqueous solution of Mn(NO3)2 (0.1 mol/L) was slowly droped into the 10 mL acetonitrile solution of 4-(1H-pyrazol-3-yl)pyridine (14.5 mg, 0.1 mmol) and triethylamine (16 mL, 0.1 mmol). The mixture was stirred at room temperature for 30 min. After filtration, colorless block-shaped crystals were obtained by evaporation within one week.

Experimental details

The H atoms were calculated geometrically and refined as riding, with C—H = 0.93–0.98 Å except for H1 and H2, and with Uiso(H) = 1.2Ueq (parent atom).

Discussion

4-(1H-Pyrazol-3-yl)pyridines have been widely studied as important ligands [2] and as precursors of the preparation for pharmaceutical active compounds [3, 4]. In the title compound, all the bond lengths are within normal ranges, similar to its two analogues [5, 6]. The Mn(II) is coordinated by two 4-(1H-Pyrazol-3-yl)pyridines, two nitrate and two water ligands. The complexes of the title compound are interlinked to form 3D supramolecular networks by classical hydrogen bonds: O4—H1⋯N2′ (′ = x, 1,5 − y, 0.5 + z): 2.8157(2) Å, O4—H2⋯O2 ′′ (′′ = 2 − x, 2 − y, 1 − z): 2.915(2) Å, N3—H3A⋯O2′′′ (′′′ = x, 1 + y, z): 2.9015(2) Å.

Acknowledgements:

We are grateful to a Project funded by the Main Research Project of the Natural Science Foundation of the Jiangsu Higher Education Institutions (14KJB150008) and the Major Basic Research Project (11KJA430009), the Major Research Project of the Natural Science Foundation of the Jiangsu Normal University (13XLA04), National Natural Science Foundation of China (NSFC) 21271091, Top-notch Academic program Project (TAPP) and PAPD of Jiangsu Higher Education Institutions for financial support.

References

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Received: 2016-5-22
Accepted: 2016-9-8
Published Online: 2016-10-8
Published in Print: 2017-1-1

©2016 Guang-Zhou Zhu 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. Editorial
  3. Twenty years of crystal structure publication and the road ahead
  4. Crystal Structures
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  6. Crystal structure of (R)-1-(2,3-dihydro-1H-pyrrolizin-5-yl)-2,3-dihydroxypropan-1-one, C10H13NO3
  7. Crystal structure of (E)-4-nitro-2-((2-phenoxyphenylimino)methyl)phenol, C19H14N2O4
  8. Crystal structure of 3,3′-di(furan-2-yl)-5,5′-bi-1,2,4-triazine
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  12. Crystal structure of 2-(5-(4-fluorophenyl)-3-p-tolyl-4,5-dihydro-1H-pyrazol-1-yl)-4-(5-methyl-1-p-tolyl-1H-1,2,3-triazol-4-yl)thiazole, C29H25FN6S
  13. Crystal structure of poly-[aqua-(μ7-benzene-1,3,5-tricarboxylato)-(μ3-1,2,4-triazol-1-ido)dicobalt(II)], C11H7Co2N3O7
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  17. Crystal structure of 1-(adamantan-1-yl)-3-(3-chlorophenyl)thiourea, C17H21ClN2S
  18. Crystal structure of 3-(adamantan-1-yl)-1-(4-bromophenyl)urea, C17H21BrN2O
  19. Crystal structure of (Z)-Ethyl 2-cyano-2-(3-phenylthiazolidin-2-ylidene) acetate, C14H14N2O2S
  20. Crystal structure of methyl 2b-ethyl-1a,2a,2b,2b1,3,5,10,11-octahydro-1H-oxireno[2′,3′:6,7]indolizino[8,1-cd]carbazole-4-carboxylate, C21H24N2O3
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  22. Crystal structure of 1,2,3-trimethyl-2,3-dihydro-1H-perimidine, C14H16N2
  23. Crystal structure of bis(2,6-dihydroxymethyl)pyridine-κ3N,O,O′)-bis(μ2-6-chloropyridin-2-olato-κ3N,O:O)-bis(6-chloropyridin-2-olato-κO)-bis(nitrato-κ2O,O′)digadolinium(III), C34H30Cl4Gd2N8O14
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  28. Crystal structure of 2-[(2-oxo-thiazolidine-3-carbonyl)sulfamoyl]-methy-benzoic acid methyl ester, C13H14N2O6S2
  29. Crystal structure of N′-(2-phenylacetyl)thiophene-2-carbohydrazide monohydrate, C13H14N2O3S
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  32. Crystal structure of dibromido-bis[μ-1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κN]mercury(II), C30H26Br2HgN10
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