Startseite Crystal structure of diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4O:O,O′,N)dimanganese(III), C22H28Mn2N8O6
Artikel Open Access

Crystal structure of diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4O:O,O′,N)dimanganese(III), C22H28Mn2N8O6

  • Qiong Wu , Qing Pu , Dian Liu , Hong-Ping Ju EMAIL logo , Yong-Feng Qiao , Xiao-Yan Wang , Yong-Mei Wu , Tao-Yu Zou und Hai Wang
Veröffentlicht/Copyright: 21. Juli 2017

Abstract

C22H28Mn2N8O6, triclinic, P1̅ (no. 2), a = 7.2827(15) Å, b = 8.6433(17) Å, c = 11.410(2) Å, α = 98.58(3)°, β = 96.15(3)°, γ = 107.67(3)°, V = 667.8(2) Å3, Z = 1, Rgt(F) = 0.0414, wRref(F2) = 0.0972, T = 293(2) K.

CCDC no.:: 1534484

The title 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:Dark-green pillar
Size:0.35 × 0.18 × 0.15 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:9.9 cm−1
Diffractometer, scan mode:Rigaku RAXIS RAPID IP, φ and ω
2θmax, completeness:55°, >99%
N(hkl)measured, N(hkl)unique, Rint:6593, 3041, 0.047
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2482
N(param)refined:172
Programs:SHELX [1], Rigaku programs [2]
Table 2

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

AtomxyzUiso*/Ueq
Mn1−0.00166(5)0.91026(4)0.87763(3)0.03005(16)
O3−0.1103(3)1.0652(2)0.95540(15)0.0329(4)
O2−0.2781(3)0.7163(2)0.91414(17)0.0460(5)
O10.0933(3)0.7421(2)0.82476(15)0.0435(4)
N1−0.1351(3)0.8998(3)0.71247(18)0.0339(4)
N20.2557(3)1.1140(3)0.85423(19)0.0446(6)
N30.2749(3)1.1586(3)0.7617(2)0.0406(5)
C10−0.0749(4)0.8426(3)0.6183(2)0.0392(6)
H10A−0.13070.85510.54460.047*
C9−0.2508(4)1.1358(4)0.7785(2)0.0443(6)
H9A−0.12121.20650.77310.053*
H9B−0.34381.18820.75160.053*
C10.1434(4)0.7099(3)0.7168(2)0.0372(5)
C11−0.2614(4)1.1202(4)0.9075(2)0.0479(7)
H11A−0.25051.22670.95460.057*
H11B−0.38701.04240.91260.057*
C8−0.2938(4)0.9702(4)0.6967(2)0.0442(6)
H8A−0.41260.89350.71250.053*
H8B−0.31620.98310.61400.053*
C50.1300(5)0.7225(4)0.5069(2)0.0518(7)
H5A0.08150.75530.43950.062*
C20.2687(4)0.6169(3)0.7056(3)0.0464(6)
H2B0.31420.57930.77150.056*
N40.2960(5)1.2001(4)0.6714(3)0.0702(9)
C60.0692(4)0.7620(3)0.6168(2)0.0387(6)
C12−0.2869(7)0.5494(4)0.9100(4)0.0817(13)
H12A−0.41150.48700.92670.123*
H12B−0.18520.54490.96900.123*
H12C−0.26990.50340.83160.123*
C40.2579(6)0.6376(4)0.4969(3)0.0602(9)
H4A0.30100.61730.42410.072*
C30.3252(5)0.5805(4)0.5953(3)0.0564(8)
H3A0.40830.51780.58700.068*

Source of materials

Salicylaldehyde (0.122 g, 1.0 mmol), tris(hydroxymethyl)aminomethane (0.121 g, 1.0 mmol) and triethylamine (0.101 g, 1.0 mmol) were dissolved in methanol (25 mL), forming a yellow solution. Mn(NO3)2⋅6H2O (0.144 g, 0.5 mmol) and sodium azide (0.076 g, 1 mmol) were successively added to the solution with stirring. The resulting dark brown suspension was heated at 65 °C for 3 h and the color slowly changed to browne. After filtration, the brown filtrate was sealed in a beaker and kept undisturbed at room temperature. The dark-green needle-shaped crystals were isolated after one week (Yield: 75% based on Mn).

Experimental details

H atoms were generated geometrically and refined as riding atoms with C—H = 0.93 Å and Uiso(H) = 1.2 times Ueq(C) for H atoms, with C—H = 0.97 Å and Uiso(H) = 1.2 times Ueq(C) for methylene H atoms.

Comment

Design and synthesis of polynuclear transition metal aggregates have attracted great interest not only because of their potential application in biology, catalysis and material science but also owing to their intriguing variety of architectures and topologies [3, 4] . In this field, the manganese Schiff base complex is a fruitful subclass of transition metal compounds, which have been paid much attention on their bioinorganic and physical aspects such as to imitate the oxygen evolution center (OEC) in photosystem (PSII) and single-molecule magnets (SMMs) [5, 6] . A number of manganese clusters with extraordinary topologies have been reported [7, 8] . However, related research involving azide is rather rare [9]. Hence, we selected azide and single-arm Schiff base ligand salicylideneamino-3-hydroxypropane as starting material, and isolated a new complex [Mn2(C20H20N2O4)(N3)2(CH3OH)2].

The crystal structure of title compound consists of a discrete binuclear cluster. The Mn(III) ions are six-coordinated: equatorial sites are defined by three oxygen atoms and one nitrogen atom from the Schiff base ligand, the axial sites are occupied by one oxygen atom of methanolato ligand and one nitrogen atom from azide. The bond lengths of Mn—O(N) are in the range of 1.8417(19)–2.319(2) Å. The bond angles around Mn(III) ions range from 78.76 to 174.53°. All the bond lengths are within normal ranges. In addition, the benzoimidazol rings in adjacent molecules are almost parallel. The average interplanar distance is 3.771(2) Å, which suggests π–π interactions.

Award Identifier / Grant number: 611660071

Award Identifier / Grant number: 1564023

Funding statement: This work was supported by Science and Technology Bureau of Kunming projects (No. 2015-05-A-H-02-3105; 2015-05-B-H-02-3003), Fund for Less Developed Regions of the National Natural Science Foundation of China (No. 611660071, 1564023), Agricultural plastic film and products research and development of Plateau area (No. DH1606).

References

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Received: 2017-2-20
Accepted: 2017-7-4
Published Online: 2017-7-21
Published in Print: 2017-9-26

©2017 Qiong Wu et al., published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of 2-(2-ethoxyphenyl)-7-propyl-5-methylimidazo[5,1-f][1,2,4]triazin-4(3H)-one, C17H20N4O2
  3. Crystal structure of catena-poly[aqua-(μ3-1,3,5-benzenetricarboxylato-κ3O:O′:O′′)-[μ3hydroxy-(1,3-di-(μ2-1,2,4-triazole-4-yl)benzoato-κ2N:N′)copper(II)], C19H16Cu2N6O9
  4. Crystal structure of poly[aqua-(μ3-3,5-di(4H-1,2,4-triazolyl-4-κ3N,N′:N′′)benzenecarboxylato)silver(I)], C11H9AgN6O3
  5. Crystal structure of tetrapropylammonium hydrogen carbonate, C13H29NO3
  6. Crystal structure of poly[μ2-acetato-κ3-O,O′:O′)diaqua(μ3-isophthalato-κ4O,O′:O′′:O′′′)yttrium(III)] monohydrate, C20H24O17Y2
  7. Crystal structure of catena-poly[dichlorido-(μ2-4-(1H-pyrazol-3-yl)-pyridine-κ2N,N′)]cadmium(II), C48H42Cd3Cl16N18
  8. Crystal structure of bis(tetraethylammonium) [1,1′-biphenyl]-2,2′-dicarboxylate trihydrate, C30H54N2O7
  9. Crystal structure of poly[(thiophene-3,4-dicarboxylato-κ1O)bis[1,2-bis(4-pyridyl)ethane-κ2N:N′]silver(I)] octahydrate, C30H42Ag2N4O12S
  10. The crystal structure of amine-(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)silver(I) dihydrate, C9H13AgN4O4
  11. Crystal structure of poly[tetrakis(μ2-cyanido-κ2N:O)-cyanido-tris(pyridine)dicobalt(II/III)], C20H15Co2N8
  12. Crystal structure of bis(pyridine)-bis(2-formyl-4,6-dichlorophenolato)cobalt(II), C24H16Cl4CoN2O4
  13. Crystal structure of (E)-1-(4-(((E)-5-bromo-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C16H15BrN2O2
  14. Crystal structure of catena-poly[(μ2-3-(1H-pyrazol-4-yl)-5-(pyridin-4-yl)-1,2,4-triazole-κ N:N′)-bis(benzoato-κO)zinc(II)], C24H18N6O4Zn
  15. Hydrothermal synthesis and crystal structure of a poly[aqua-(μ4-4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(μ2-1-(4-(1H-imidazol-1-yl)benzyl)-1H-1,2,4-triazole-κ2N:N′) dimanganese(II)], [Mn2(C9H6O4)2(C12H11N5)(H2O)]
  16. Crystal structure of diaqua-catena-poly[diaqua-bis(μ2-5-(4-(1H-1,2,4-triazol-1-yl)phenyl)tetrazol-2-ido-κ2N:N′)cobalt(II)] dihydrate, C20H24CoN14O4
  17. Crystal structure of bis(μ3-2,2′-azanediylbis(ethan-1-olato)-κ5O:O,N,O′:O′)-tetrachlorido-bis(μ2-2-((2-hydroxyethyl)amino)ethan-1-olato-κ3N,O:O)dicobalt(II)dicobalt(III), C16H38Cl4Co4N4O8
  18. Crystal structure of poly[μ4-(4-(carboxylatomethyl)benzoato-κ4O:O′:O′′:O′′′)-(2-(4-(1H-imidazol-1-yl)phenyl)-1H-benzo[d]imidazole-κN)manganese(II)] [Mn(C9H6O4)(C16H12N4)]
  19. Crystal structure of 4-chloro-6-phenylpyrimidine, C10H7ClN2
  20. The crystal structure of [6-methoxy-2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1(2H)-one]difluoroborane, C13H10BF5O3
  21. Crystal structure of 3,3′-(butane-1,4-diylbis(azanylylidene))bis(1-phenylbut-1-en-1-olato)-κ4N,N′,O,O′]copper(II), C24H26N2O2Cu
  22. Crystal structure of tetraaqua-bis((E)-N′-(2-bromobenzylidene)isonicotinohydrazide-κN)zinc(II) dinitrate, C26H28N8O12Br2Zn
  23. Crystal structure of 2-amino-4-(4-bromophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13BrN2O2
  24. A single crystal study on tert-butyl-4-((4-(4-bromo-2-fluorophenylamino)-6-methoxyquinazolin-7-yloxy)methyl)piperidine-1-carboxylate, C26H30BrFN4O4
  25. 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-κ3O,O′,N)zinc(II), C36H26N2O4Zn
  26. Crystal structure of diaqua-bis(5′-(pyridin-1-ium-4-yl)-1H-[3,3′-bi(1,2,4-triazol)]-2′-ide-κ2N,N′)cobalt(II) — bis(5-(pyridin-4-yl-κN)-1H,1′H-3,3′-bi(1,2,4-triazole))octamolybdate – water (2/1/8), C27H33CoMo4N21O19
  27. Crystal structure of 3-cyclohexyl-2-(cyclohexylimino)-2,3-dihydro-6,8-diiodo-4H-1,3-benzoxazin-4-one, C20H24I2N2O2
  28. Crystal structure of dinitrato-κO-bis(tris((1H-benzo[d]imidazol-2-yl)methyl)amine-κ4N,N′,N′′,N′′′)-(μ2-cyclohexane-1,4-dicarboxylato-κ4O,O′:O′′,O′′′)dimanganese(II) – methanol – water (1/6/2), C62H80Mn2N16O18
  29. Crystal structure of bis(2-hydroxyethyl(phenyl)carbamodithioate)nickel(II), C18H20N2NiO2S4
  30. Crystal structure of methyl 1-(4-fluorobenzyl)-4-methoxy-5-oxopyrrolidine-3-carboxylate, C14H16FNO4
  31. Crystal structure of di-μ-iodido-bis(6-(p-tolyl)-2,2′-bipyridine-κ2N,N′)dicopper(I) — 2-(diphenylphosphoryl)benzoic acid (1/2), C36H29CuIN2O3P
  32. Crystal structure of 2-amino-4-(3-bromo-4-fluoro-phenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C18H16BrFN2O2
  33. Crystal structure of bis(μ2-2-chlorobenzoato-κ3O,O′:O′)-(2-chlorobenzoato-κO)-(2-chlorobenzoato-κO,O′)-bis(1,10-phenanthroline-κ2N,N′)-dicadmium(II) monohydrate, C52H36Cd2Cl4N4O10
  34. Crystal structure of 2-(8a-methyl-5-oxo-hexahydroimidazo [1,2-a]pyridin-1(5H)-yl)-2-oxoethyl acetate, C12H18N2O4
  35. Crystal structure of (E)-N,N-diethyl-2-(5-nitrothiazol-2-yl)-1-phenylethen-1-amine, C15H17N3O2S
  36. Crystal structure of diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4O:O,O′,N)dimanganese(III), C22H28Mn2N8O6
  37. The crystal structure of bis(2-(2,2,2-trifluoroacetyl)-3,4-dihydronaphthalen-1-olato-κ2O,O′)copper(II), C24H16CuF6O4
  38. Crystal structure of hexaaquanickel(II) bis((E)-4-((4-(dimethylamino)phenyl)diazenyl)benzenesulfonate), C28H40N6NiO12S2
  39. Crystal structure of catena-poly[aqua-(μ2-hexamethylenetetramine-κ2N:N′)-bis(2,6-difluorobenzoato-κ2O:O′)cadmium(II)]monohydrate, C20H22CdF4N4O6
  40. Crystal structure of 3-benzyl-2,3-dihydro-2-thioxoquinazolin-4(1H)-one, C15H12N2OS
  41. Crystal structure of bis(μ2-ferrocenecarboxylato-κ2O:O′)-bis(1,10-phenanthroline-κ2N,N′)-(μ2-methanolato2O,O)dicopper(II) tetrafluoroborate – acetonitrile (1/1), C49H40BCu2F4Fe2N5O5
  42. The crystal structure of tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)silver(I) chloride dihydrate, C24H60AgClN12O6P4
  43. Crystal structure of 5-ethyl-2-(p-tolyl)-1,3-dioxane-5-carboxylic acid, C14H18O4
  44. Crystal structure of 2-(4-fluorophenyl)-1,3-dimethyl-1H-perimidin-3-ium iodide, C19H16ClIN2
  45. Crystal structure of catena-poly[(μ2-hexamethylenetetramine-κ2N:N′)-tetrakis(μ2-2,6-difluorobenzoato-κ2O:O′)dicopper(II)], C34H24Cu2F8N4O8
  46. Crystal structure of ethyl 3-hydroxy-5-methyl-2-(4-(m-tolyl)-1H-1,2,3-triazol-1-yl)-[1,1′-biphenyl]-4- carboxylate, C25H24N3O3
  47. The crystal structure of carbonyl(2-oxopyridin-1(2H)-olato-κ2O,O′)-(diphenylcyclohexylphosphine-κP)rhodium(I), C24H25NO3PRh
  48. Crystal structure of bis((pyrazin-2-ylmethyl)(pyrazine-2-carbonyl)amido-κ3N,N′,N′′)copper(II), C20H16CuN10O2
  49. Crystal structure of catena-poly[tetraaqua-(μ2-succinonitrile-κ2N:N′)cobalt(II)] dinitrate, C4H12CoN4O10
  50. The crystal structure of 1,1′-bisisoquinoline, C18H12N2
  51. Crystal structure of bis(hydroxydi(pyridin-2-yl)methanolato-κ3N,N′,O)cobalt(III) perchlorate dihydrate, C22H22ClCoN4O10
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