Startseite The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4
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The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4

  • Zhen-Zhen Shi ORCID logo EMAIL logo , Shu-Yang Chen ORCID logo , Jun-Ling Chen ORCID logo , Shu-Zhou Yun und Xing-Fang Fu
Veröffentlicht/Copyright: 7. November 2024
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Zeitschrift für Kristallographie - New Crystal Structures
Aus der Zeitschrift Zeitschrift für Kristallographie - New Crystal Structures Band 240 Heft 1

Abstract

C33H25N7O8Zn4, triclinic, P1̄ (no. 2), a = 12.1524(7) Å, b = 12.2035(7) Å, c = 14.2730(7) Å, α = 78.669(4)°, β = 66.615(5)°, γ = 62.482(6)°, V = 1722.83(19) Å3, Z = 2, R gt(F) = 0.0405, wRref (F 2) = 0.1128, T = 293(2) K.

CCDC no.: 2372259

The title crystal structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Yellow block
Size: 0.18 × 0.10 × 0.07 mm
Wavelength:

μ:		 Mo Kα radiation (0.71073 Å)

2.81 mm−1
Diffractometer, scan mode:

θ max, completeness:		 SuperNova, ω

26.4°, >99 %
N(hkl)measured, N(hkl)unique, R int: 14,593, 7023, 0.023
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 5148
N(param)refined: 473
Programs: Bruker, 1 SHELX, 2 , 3 , 4 Diamond 5
Table 2:

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

Atom x y z U iso*/U eq
Zn1 0.21165(4) 0.01652(4) −0.12247(3) 0.04315(14)
Zn2 −0.03881(4) 0.07655(4) −0.17134(3) 0.04346(14)
Zn3 0.12496(4) −0.19123(4) −0.11148(3) 0.04318(14)
Zn4 0.24211(5) −0.08058(5) −0.32739(3) 0.05190(15)
C1 0.4320(4) 0.0788(3) −0.1836(3) 0.0394(9)
C2 0.5420(4) 0.0997(4) −0.2407(4) 0.0550(11)
H2 0.576496 0.131591 −0.210946 0.066*
C3 0.6007(5) 0.0722(5) −0.3437(4) 0.0669(14)
H3 0.674768 0.086468 −0.383785 0.080*
C4 0.5502(5) 0.0244(5) −0.3861(4) 0.0668(14)
H4 0.589573 0.005908 −0.455150 0.080*
C5 0.4375(4) 0.0031(5) −0.3249(3) 0.0586(12)
C6 0.3624(4) 0.1051(3) −0.0728(3) 0.0392(9)
C7 0.4044(4) 0.1457(3) −0.0165(3) 0.0474(10)
H7 0.480371 0.159375 −0.047344 0.057*
C8 0.3331(4) 0.1664(4) 0.0866(3) 0.0504(10)
H8 0.360838 0.194131 0.125564 0.061*
C9 0.2215(4) 0.1459(3) 0.1311(3) 0.0464(10)
H9 0.173331 0.159276 0.200438 0.056*
C10 0.1802(4) 0.1047(3) 0.0716(3) 0.0365(8)
C11 0.1905(4) −0.2250(4) 0.2986(3) 0.0502(10)
C12 0.2307(6) −0.2718(5) 0.3805(4) 0.0724(15)
H12 0.316882 −0.330572 0.371730 0.087*
C13 0.1399(6) −0.2297(5) 0.4773(4) 0.0823(17)
H13 0.165535 −0.260447 0.534010 0.099*
C14 0.0152(6) −0.1447(5) 0.4893(4) 0.0723(15)
H14 −0.045307 −0.117030 0.554160 0.087*
C15 −0.0237(5) −0.0972(5) 0.4024(3) 0.0571(12)
C16 0.2809(4) −0.2635(4) 0.1920(3) 0.0476(10)
C17 0.4069(5) −0.3558(4) 0.1660(4) 0.0601(12)
H17 0.441872 −0.400717 0.216080 0.072*
C18 0.4816(5) −0.3813(4) 0.0634(4) 0.0621(13)
H18 0.567881 −0.443105 0.044718 0.074*
C19 0.4300(4) −0.3168(4) −0.0105(4) 0.0520(11)
H19 0.480423 −0.333895 −0.079161 0.062*
C20 0.3004(4) −0.2249(3) 0.0188(3) 0.0409(9)
C21 −0.1492(4) 0.4339(4) 0.0403(3) 0.0508(11)
C22 −0.1403(5) 0.5302(4) −0.0268(4) 0.0700(14)
H22 −0.179716 0.610085 −0.003121 0.084*
C23 −0.0723(6) 0.5063(5) −0.1294(4) 0.0830(17)
H23 −0.067100 0.570936 −0.175308 0.100*
C24 −0.0127(5) 0.3891(4) −0.1644(4) 0.0686(14)
H24 0.033377 0.373053 −0.233670 0.082*
C25 −0.0222(4) 0.2924(4) −0.0934(3) 0.0426(9)
C26 −0.2227(4) 0.4481(4) 0.1515(4) 0.0518(11)
C27 −0.2806(5) 0.5588(4) 0.1994(4) 0.0672(13)
H27 −0.274346 0.628782 0.162463 0.081*
C28 −0.3484(5) 0.5639(5) 0.3034(5) 0.0783(16)
H28 −0.389225 0.638283 0.336921 0.094*
C29 −0.3557(5) 0.4617(5) 0.3567(4) 0.0716(14)
H29 −0.399857 0.465443 0.426951 0.086*
C30 −0.2961(4) 0.3485(4) 0.3058(4) 0.0586(12)
N1 0.3806(3) 0.0315(3) −0.2251(2) 0.0466(8)
N2 0.2517(3) 0.0848(3) −0.0282(2) 0.0359(7)
N3 0.0655(3) −0.1380(3) 0.3092(2) 0.0463(8)
N4 0.2294(3) −0.2000(3) 0.1190(2) 0.0415(8)
N5 −0.0906(3) 0.3176(3) 0.0056(2) 0.0410(8)
N6 −0.2297(3) 0.3442(3) 0.2038(3) 0.0477(8)
O1 0.3929(3) −0.0443(4) −0.3655(2) 0.0805(11)
O2 0.0747(2) 0.0845(2) 0.10920(19) 0.0418(6)
O3 0.2434(3) −0.1608(2) −0.0464(2) 0.0451(6)
O4 −0.1431(3) −0.0171(3) 0.4156(2) 0.0700(9)
O5 0.0327(3) 0.1786(2) −0.1216(2) 0.0451(6)
O6 −0.3047(3) 0.2524(3) 0.3571(2) 0.0694(9)
O7 0.1391(2) −0.0464(2) −0.18649(18) 0.0390(6)
N7 0.7194(14) 0.6645(12) 0.5877(11) 0.215(4)
C33 0.796(2) 0.6898(19) 0.5925(16) 0.283(6)
H33 0.851670 0.708564 0.531457 0.339*
O8 0.8148(16) 0.6954(13) 0.6824(11) 0.352(6)
C31 0.7105(17) 0.6912(14) 0.4946(10) 0.294(7)
H31A 0.697628 0.775195 0.476448 0.441*
H31B 0.636722 0.680830 0.494824 0.441*
H31C 0.790659 0.636744 0.445733 0.441*
C32 0.6373(16) 0.6502(14) 0.7081(14) 0.342(10)
H32A 0.608758 0.723324 0.743427 0.513*
H32B 0.693547 0.579815 0.737296 0.513*
H32C 0.561423 0.639207 0.714427 0.513*

1 Source of material

All reagents used were purchased and used without further purification. A mixture of 6,6′-dihydroxy-2,2′-bipyridine(H2 dhbp, 24.4 mg, 0.1 mmol) and Zn(OAc)2 ⋅ 2H2O (22.0 mg, 0.1 mmol) was dissolved in 2 mL H2O and 2 mL dimethylformamide (DMF). The resulting solution was placed in a 25 mL Teflon-lined stainless steel reactor, which was sealed and heated to 413 K for 72 h. After the mixture was cooled to room temperature over 24 h, yellow crystals of the title complex were obtained.

2 Experimental details

Absorption corrections were applied by using multi-scan program. 1 The structure was refined with the SHELXL software package. 2 , 3 , 4 The figure of the title crystal structure was drawn by the Diamond software. 5 Hydrogen atoms attached to C were treated as riding atoms. The U iso values of the hydrogen atoms of water molecules were set to 1.5 U eq (O) and the U iso values of all other hydrogen atoms were set to 1.2 U eq (C).

3 Comment

The modification of commonly used diimine ligands, such as bipyridine, is a convenient method to design and synthesize various metal complexes suitable for different applications. 6 , 7 , 8 , 9 According to literature, the incorporation of different substituents (such as –OH, –CN, –OCH3, –COOH and so on) on the different positions of the 2,2′-bipyridine ligands into various metal complexes could efficiently modify their properties and applications. 10 , 11 , 12 , 13 , 14 , 15

The molecular structure of the title complex contains two connected asymmetrical units-[ZnII 4], each of which composes of four Zn(II) ions, one μ 4–O, three deprotonated dhbp2− ligands, and one free DMF solvent molecule (see the Figure). All Zn(1), Zn(2), and Zn(3) ions are five-coordinate to display distorted triangular bipyramidal geometries. The equatorial plane is occupied by two hydroxyl O and one N atom from three different dhbp2−, whereas the axial places are one μ 4–O and one N atoms from one dhbp2−. Among them, μ 4–O is located at the vertex position of these triangular bipyramidal axes, and the bond angles of O(7)–Zn(1)–N(2), O(7)–Zn(2)–N(4)#1, O(7)–Zn(3)–N(5)#1 (symmetry codes: #1 −x, −y, −z) are 167.28, 165.86, and 166.92°, respectively, all close to linear. Each Zn(4) shows a tetrahedral geometry and coordinates with a μ 4–O and three hydroxyl O atoms from three different dhbp2− ligands. The Zn–O bond lengths range from 1.921 to 2.182 Å, while the Zn–N bond lengths range from 2.004 to 2.069 Å.

The whole molecular structure of the title complex consists of two of the aforementioned asymmetrical [ZnII 4] pyramids bridged by a μ 4–O bridge, resulting an octanuclear {ZnII 8} cluster. The {ZnII 8}-core can be viewed in a bicapped anti-trigonal-prism, in which six Zn(II) construct the anti-trigonal-prism and other two Zn(II) are located at the cap sites. All Zn⋯Zn distances range from 3.100 to 4.106 Å. The periphery of {ZnII 8 } is surrounded by six dhpb2− ligands, forming a zero dimensional molecular structure, which is very similar to that of the reported two novel 3d-4f clusters with {CoII 6 LnIII 2} (Ln = Dy, Ho) cores. 7 These {ZnII 8} clusters are further linked together by intermolecular interactions (C–H⋯O hydrogen bonds) to form a three-dimensional supramolecular structure, and the solvents (DMF) are placed at the void of the structure.

Corresponding author: Zhen-Zhen Shi, College of Chemistry and Pharmaceutical Engineering, Nanyang Normal University, Nanyang, Henan 473061, P.R. China, E-mail:

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Competing interests: The authors declare no conflicts of interest regarding this article.

  3. Research funding: We gratefully acknowledge the financial support by Science and Technology Research Key Program of Henan Province (212102210461) and Nanyang Normal University Scientific Research Foundation Project (2023ZX002 and 2018ZX007).

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Received: 2024-07-21
Accepted: 2024-10-18
Published Online: 2024-11-07
Published in Print: 2025-02-25

© 2024 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  47. The crystal structure of methyl 4-(4-(methylsulfonyl)phenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C19H21NO5S
  48. Crystal structure of 1′,3′-dihydro-2,2′-spirobi[indene]-1,3-dione, C17H12O2
  49. Crystal structure of (E)-2,2′,3,3′-tetrahydro-[1,1′-biindenylidene]-4,4′-diol, C18H16O2
  50. Crystal structure of di-glycylglycinium squarate dihydrate, C12H22N4O12, at 105 K
  51. Crystal structure of {[(4-fluorophenyl)methyl]triphenylphosphonium}dibromocopper(I), [C25H21FP]+[CuBr2]−
  52. Crystal structure of poly[diaqua-bis(μ2-5-((pyridin-4-yl-methyl)amino)benzene-1,3-dicarboxylato-κ 2 N:O)cadmium(II)], C28H26CdN4O10
https://doi.org/10.1515/ncrs-2024-0311
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Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of the co-crystal 2,4,6-triamino-1,3,5-triazine-1,3-dioxide — acetic acid (1/2) C7H14N6O6
  4. Crystal structure of the dinuclear mercury(II) complex bis(μ2-bromido)-dibromido-bis{1-[(benzotriazol-1-yl)methyl]-1-H-1,3-(2-ethyl-5-methyl-imidazol)-κ1 N} dimercury(II), C26H30N10Hg2Br4
  5. Crystal structure of poly[hexaqua-pentakis(μ4-2,2′-bipyridine-4,4′-dicarboxylato-κ4 O:O′:O″:O‴)-(μ2-2,2′-bipyridine-4,4′-dicarboxylato-κ2 O:O)tetraytterbium(III)] hydrate, C36H26N6O16Yb2
  6. Hydrothermal synthesis and crystal structure of catena-poly[(1,10-phenanthroline-κ 2 N,N′)-bis(μ 2-nitroisophthalato-κ 3 O,O′:O″)nickel(II)], C20H13NiN3O7
  7. Crystal structure of 72,73,75,76-tetrafluoro-25,44-dimethyl-31,33,36,38-tetraoxo-31,32,33,36,37,38-hexahydro-3(2,7)-benzo[lmn][3,8]phenanthrolina-1,5(4,1)-dipyridin-1-iuma-2,4(1,2),7(1,4)-tribenzenacyclooctaphane-11,51-diium hexafluoridophosphate, [C46H28F4N4O4][PF6]2, a dicationic cyclophane
  8. Crystal structure of (E)-2-(4-(1H-imidazol-1-yl)benzylidene)-7-fluoro-3,4-dihydronaphthalen-1(2H)-one, C20H15FN2O
  9. The salt crystal structure of etoricoxib hydrochloride, C18H16Cl2N2O2S
  10. The structure of t-butyl 7-[2-(4-fluorophenyl)-3-phenyl-4-(phenylcarbamoyl)-5-(propan-2-yl)-1H-pyrrol-1-yl]-3,5-dihydroxyheptanoate, C37H43FN2O5
  11. The crystal structure of (μ4-oxo)-tri(μ4-2,2′-bipyridine-6,6′-bis(olato)-κ5 O,O′:N:N′:O″)tetrazinc(II) – methylformamide (1/1), C33H25N7O8Zn4
  12. The co-crystal structure of 4-chlorobenzophenone–salicylhydrazide(1/1), C20H17ClN2O3
  13. Crystal structure of 9-fluoro-4-(6-methoxypyridin-2-yl)-5,6-dihydrobenzo[h]quinazolin-2-amine, C18H15FN4O
  14. The crystal structure of the co-crystal composed of benzhydrazide and 5-aminoisophthalic acid, C8H7NO4⋅C7H8N2O
  15. The cocrystal structure of praziquantel-hesperetin (1/1), C35H38N2O8
  16. Crystal structure of new barium manganese fluorides dihydrates, Ba10Mn2F25·2H2O
  17. The crystal structure of bis[μ2-(3-(3-(pyridin-2-yl)-1H-pyrazol-1-yl)propanoate-κ2O:N)-bis(2,2′-bipyridine-κ2 N, N′)dicopper(II)]dinitrate, C42H36Cu2N12O10
  18. Crystal structure of (3,6-di(2-pyridyl)-4-phenylaminopyridazine-κ2N,N′)-bis(2-(p-toluene)pyridinyl-κ2C,N)-iridium(III) hexafluorophosphate –dichloromethane (1/1), C45H37Cl2F6IrN7P
  19. The crystal structure of 2-(2′-carboxybenzyl)benzoic acid, C15H12O5
  20. The crystal structure of dichlorido-[(E)-N′,N″-bis((2E,3E)-3-(hydroxyimino)butan-2-ylidene)-2-((E)-3-(hydroxyimino)butan-2-ylidene)hydrazine-1-carbohydrazonhydrazide-κ 4 N 4]cobalt(II), C13H22N9O3Cl2Co
  21. Crystal structure of (−)-flavesine H, C15H22N2O2
  22. Crystal structure of 3-methoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H22O4
  23. Crystal structure of dicarbonyl(2-oxopyridin-1(2H)-olato-κ 2 O,O)iridium(I), C7H4IrNO4
  24. The crystal structure of 4-(3-(triphenylphosphonio)propyl)piperazin-1-ium dibromide trihydrate, C25H37Br2N2O3P
  25. The crystal structure of ethyl 5,6-dihydroxybenzofuran-3-carboxylate, C11H10O5
  26. Crystal structure of 14-(R)-(2′-cyano-phenoxy)-3,19-diacetyl andrographolide, C31H37NO7
  27. The twinned crystal structure of 10-(4-methyl benzoate)-2,8-diethyl-5,5-difluoro-1,3,7,9-tetramethyl-5H-di-pyrrolo[1,2-c:2′,1′-f] [1,3,2]diazaborinin-4-ium-5-uide, C25H29BF2N2O2
  28. The crystal structure of (9H-thioxanthen-9- ylidene)hydrazine monohydrate, C13H11N2SO0.5
  29. The crystal structure of pyridinium diaqua-{1,2-phenylenebis((carboxylatocarbonyl)amido-κ4 N,N′,O,O′)manganese(III), C15H14MnN3O8
  30. Crystal structure of the hydrogen storage active high entropy phase Tb0.82Sm0.18Ni0.83Co0.17Mg
  31. Crystal structure of diaqua-bis[5-methyl-1-(1H-pyrazol-3-yl)-1H-1,2,3-triazole-4-carboxylato-κ 2 N,O)]manganese(II), C14H16MnN10O6
  32. Crystal structures of diiodido-3-((pyridin-2-ylmethylene)amino)-2-(pyridin-3-yl)-2,3-dihydroquinazolin-4(1H)-one-cadmium(II)
  33. Synthesis and crystal structure of methyl 4-(2-ethoxy-2-oxoethoxy)-3,5-dimethoxybenzoate, C14H18O7
  34. Crystal structure of isoxazolo[4,5-b]pyridin-3-amine, C6H5N3O
  35. Crystal structure of 4-chloro-1-isobutyl-1H-imidazo, C14H14ClN3
  36. The crystal structure of 1,1,1,2,2,2-hexakis(2-methyl-2-phenylpropyl)distannane,C60H78Sn2
  37. The crystal structure of (2,7-dimethoxynaphthalene-1,8-diyl)bis((3-nitrophenyl)methanone), C26H18N2O8
  38. Crystal structure of diaqua-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II) dinitrate dihydrate, C60H76Cl8N14O14Zn
  39. The crystal structure of diphenyl bis(2-((diphenoxyphosphoryl)amino)ethyl)phosphoramidate monohydrate C40H42N3O10P3
  40. Crystal structure of 4,4′-bis(dibromomethyl)-1,1′-biphenyl, C14H10Br4
  41. Crystal structure of CaPtZn
  42. Crystal structure of 3-chloro-5-(trifluoromethyl)pyridine-2-carboxylic acid, C7H3ClF3NO2
  43. The crystal structure of (3′-(2-bromophenyl)-2-phenyl-[2,2′-bioxiran]-3-yl)(phenyl)methanone, C92H68O12Br4
  44. Crystal structure of ethyl 4-(4-benzylpiperazin-1-yl)benzoate, C20H24N2O2
  45. The crystal structure of bis(selenocyanato-κ1 N)-bis(methanol)-bis((1E,2E)-1,2-bis (1-(pyridin-4-yl)ethylidene)-hydrazine)iron(II) methanol solvate, C34H44FeN10O4Se2
  46. Crystal structure of (E)-1-(5-bromo-2-hydroxyphenyl)-3-(5-(4-methoxyphenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)prop-2-en-1-one, C26H21BrN2O4
  47. The crystal structure of methyl 4-(4-(methylsulfonyl)phenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C19H21NO5S
  48. Crystal structure of 1′,3′-dihydro-2,2′-spirobi[indene]-1,3-dione, C17H12O2
  49. Crystal structure of (E)-2,2′,3,3′-tetrahydro-[1,1′-biindenylidene]-4,4′-diol, C18H16O2
  50. Crystal structure of di-glycylglycinium squarate dihydrate, C12H22N4O12, at 105 K
  51. Crystal structure of {[(4-fluorophenyl)methyl]triphenylphosphonium}dibromocopper(I), [C25H21FP]+[CuBr2]−
  52. Crystal structure of poly[diaqua-bis(μ2-5-((pyridin-4-yl-methyl)amino)benzene-1,3-dicarboxylato-κ 2 N:O)cadmium(II)], C28H26CdN4O10
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Heruntergeladen am 8.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2024-0311/html
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