Startseite Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
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Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10

  • Lu Wei-Hong ORCID logo EMAIL logo , Hong Zu-Chen , Li Jia-Hui und Huang Miao
Veröffentlicht/Copyright: 21. Juni 2024

Abstract

C14H10BiKN2O10, triclinic, P1̄ (no. 2), a = 7.029(8) Å, b = 10.460(9) Å, c = 11.891(9) Å, α = 71.19(2)°, β = 80.57(3)°, γ = 85.18(4)°, V = 815.9(13) Å3, Rgt (F) = 0.0512, wRref (F 2) = 0.1410, Z = 2, T = 296(2) K.

The molecular 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: Colorless block
Size: 0.22mm×0.18mm×0.12mm
Wavelength:

μ:
Mo Kα radiation (0.71073 Å)

11.1 mm−1
Diffractometer, scan mode:

θ max, completeness:
Bruker APEX-II, φ and ω

27.5°, 99 %
N(hkl)measured, N(hkl)unique, R int: 7260, 3674, 0.052
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 3584
N(param)refined: 253
Programs: CrysAlisPRO, 1 SHELX 2 , 3
Table 2:

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

Atom x y z U iso*/U eq
Bi1 0.36264 (3) −0.17566 (2) 0.64687 (2) 0.02032 (14)
C1 0.7146 (11) 0.4210 (7) 0.4577 (7) 0.0237 (14)
C2 0.6432 (10) 0.2332 (7) 0.6244 (7) 0.0229 (13)
C3 0.7694 (11) 0.4923 (8) 0.5286 (7) 0.0292 (15)
H3 0.808511 0.581061 0.494595 0.035*
C4 0.6957 (12) 0.2974 (8) 0.7001 (7) 0.0288 (15)
H4 0.685060 0.253744 0.782406 0.035*
C5 0.7634 (12) 0.4260 (8) 0.6517 (8) 0.0302 (15)
H5 0.804966 0.468659 0.700441 0.036*
C6 0.5683 (11) 0.0916 (8) 0.6725 (7) 0.0247 (15)
C7 0.7246 (10) 0.4796 (7) 0.3256 (7) 0.0245 (14)
C8 0.2487 (11) −0.2422 (7) 0.9399 (7) 0.0238 (15)
C9 0.7341 (10) −0.2882 (7) 0.7839 (6) 0.0210 (13)
C10 0.4589 (10) −0.2863 (7) 0.9231 (7) 0.0231 (13)
C11 0.7548 (12) −0.3886 (8) 0.9902 (7) 0.0286 (15)
H11 0.823575 −0.435432 1.052480 0.034*
C12 0.8466 (11) −0.3558 (8) 0.8721 (7) 0.0257 (14)
H12 0.976214 −0.377916 0.853322 0.031*
C13 0.5633 (11) −0.3528 (8) 1.0163 (7) 0.0267 (14)
H13 0.504448 −0.372981 1.095677 0.032*
C14 0.8104 (11) −0.2427 (7) 0.6513 (7) 0.0231 (13)
K2 0.8606 (3) 0.8559 (2) 0.15305 (16) 0.0309 (4)
N1 0.6543 (8) 0.2933 (6) 0.5067 (5) 0.0208 (11)
N2 0.5457 (9) −0.2566 (6) 0.8087 (6) 0.0217 (11)
O1 0.7693 (9) 0.5995 (6) 0.2759 (6) 0.0360 (13)
O2 0.6784 (8) 0.4052 (5) 0.2687 (5) 0.0267 (11)
O3 0.5142 (9) 0.0434 (6) 0.7829 (5) 0.0300 (12)
O4 0.5633 (8) 0.0330 (5) 0.5946 (5) 0.0259 (11)
O5 0.1808 (7) −0.1805 (6) 0.8430 (5) 0.0265 (11)
O6 0.1636 (9) −0.2670 (6) 1.0425 (5) 0.0325 (12)
O7 0.6831 (8) −0.2257 (5) 0.5801 (5) 0.0252 (10)
O8 0.9832 (8) −0.2271 (7) 0.6173 (5) 0.0338 (13)
O10 0.8404 (9) 0.9603 (6) −0.0864 (6) 0.0351 (13)
H10A 0.716679 1.005512 −0.101799 0.042*
H10B 0.865964 0.891879 −0.126431 0.042*
O11 0.8837 (10) 0.9285 (7) 0.3626 (6) 0.0412 (14)
H11A 0.807780 0.868572 0.430763 0.062*
H11B 0.835222 1.019709 0.351257 0.062*

1 Source of materials

The title compound was synthesized by mixing [Bi(HPydc)3(Bi(pydcH)(pydcH2)(pydc))(Bi(pydcH)(pydcH2)(pydc))] (1 mmol), K2CO3(2 mmol), and 30 mL distilled water into a 50 mL glass beaker. The compound of [Bi(HPydc)3(Bi(pydcH)(pydcH2)(pydc)) (Bi(pydcH)(pydcH2)(pydc))] was prepared according to ref. [4]. The glass beaker was heated to 343 K in an oven and kept there for 5 h. When the glass beaker was cooled down to room temperature, the colorless block crystals were obtained by slow solvent evaporation for 10 days.

2 Experimental details

The single crystals were carefully selected for data collection which was performed for compound by Bruker APEX–II CCD X-ray diffractometer. The structure of the compound was solved by Direct Methods, and then refined on F 2. 1 3 Moreover, the hydrogen atoms were fixed geometrically at calculated distances, and allowed to ride on the parent atoms. Alerts level A and B are attributed to the high residual electron density peaks of central Bi1 atom. These peaks that are too near the Bi that they do not be interpreted as true atoms.

3 Comment

As we know, organic ligands in coordination chemistry, especially nitrogen-containing heterocyclic acids, 5 , 6 have various coordination modes. Some bismuth-based compounds have many potential applications. 7 , 8 Bismuth(III) is known to form stable chelate complexes with pydcH2 (pydcH2 = 2,6-pyridine dicarboxylate) and various crystal structures have been reported. 9 , 10 The Bi III center is six-coordinated by four O atoms and two N from μ 2-pyridine 2,6-dicarboxylato-ligands, to form a octahedral coordination geometry, and the K I center also is six-coordinated by six O from μ 2-pyridine 2,6-dicarboxylato and μ 2-aqua ligands. The coordination bond lengths and angles around the Bi III are in the range of 2.307(6)–2.712(6) Å and 65.8(2)–151.6(2)°, respectively. And the coordination bond lengths and angles around the K I are in the range of 2.683(6)–2.861(8) Å and 74.6(2)–161.5(2)°. Bi and K atoms are linked by H2O molecules and pyridine 2,6-dicarboxylato- to form the three-dimensional network.


Corresponding author: Lu Wei-Hong, School of Chemistry and Materials Science, Key Laboratory of Functional Metal-organic Compounds of Hunan Province, Key Laboratory of Functional Organometallic Materials of Hunan Province College, Hengyang 421008, P.R. China; and College of Chemistry and Materials Science, Hengyang Normal University, Hengyang 421008, 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: This work was supported by Scientific Research Projects of Education Department of Hunan Province (22B0723).

References

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Received: 2024-05-06
Accepted: 2024-05-23
Published Online: 2024-06-21
Published in Print: 2024-08-27

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

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

Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
  3. The crystal structure of hexaquazinc(II) poly[hexakis(μ2-4-methylbenzenesulfinato-κ2O:O′) dizinc(II)]
  4. The crystal structure of poly[((2-(4,5-dihydro-1H-pyrazol-4-yl)-1,3-dioxoisoindoline-5-carbonyl)oxy)(1-(dimethylamino)ethoxy)zinc[II]], C16H14ZnN4O5
  5. Crystal structure of bis[(triaqua-4-iodopyridine-2,6-dicarboxylato-κ 3 N,O,O )cobalt(II)] trihydrate, C14H22N2O17I2Co2
  6. Crystal structure of bis(methanol-κO)-bis(nitrato-kO)-bis(1-((2-(2-chloro-4-(4-chlorophenoxy)phenyl)-4-methyl-1,3-dioxolan-2-yl)methyl)-1H-1,2,4-triazole-κN)cadmium(II), C40H42O14N8Cl4Cd
  7. Crystal structure of poly[μ2-dichlorido-(μ2-1-[(2,4-dimethyl-1H-triazole-1-yl)methyl]-1H-benzotriazole-κ2N:N′)cadmium(II)], C11H12CdN6Cl2
  8. The crystal structure of (3aS, 4R, 7S, 7aR)-hexahydro-4, 7-methano-1H-isoindole-1, 3-(2H)-dione, C9H11NO2
  9. The crystal structure of N-(acridin-9-yl)-4-chloro-N-(4-chloro-butanoyl) butanamide, C21H20Cl2N2O2
  10. Crystal structure of 3,3′-dimethoxy-4,4′-oxy-di-benzaldehyde, C16H14O5
  11. The crystal structure of tetrakis(μ 2-2-amino-3,5-dibromobenzoate-κ 2 O:O′)-octakis(n-butyl-κ 1 C)-bis(μ 3-oxo)tetratin(II), C60H92Br8N4O10Sn4
  12. Crystal structure of methyl-1-(naphthalen-1-yl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b] indole-3-carboxylate, C23H20N2O2
  13. Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea(1/1)
  14. Crystal structure of 6,6′-((1E,1′E)-((2-phenylpyrimidine-4,6-diyl)bis(hydrazin-2-yl-1-ylidene))bis(methaneylylidene))bis(2-methoxyphenol)monohydrate, C26H26N6O5
  15. Crystal structure of bis(N,N,N-trimethylbutanaminium) tetrathiotungstate(VI), (BuMe3N)2[WS4]
  16. The crystal structure of 2,3,9-triphenyl-9-(2-phenylbenzofuran-3-yl)-9H-9λ 5-benzo[4,5][1,2]oxaphospholo[2,3-b][1,2,5]oxadiphosphole 2-oxide, C40H28O4P2
  17. Crystal structure of 1–methyl-3-propyl-4-nitro-1H-pyrazole-5-carboxylic acid, C8H11N3O4
  18. Crystal structure of N-(benzo[d]thiazol-2-yl)-2-chloroacetamide, C9H7ClN2OS
  19. The crystal structure of N-benzyl-2-chloro-N-(p-tolyl) acetamide, C16H16ClNO
  20. Crystal structure of 3,4-dimethoxybenzyl 2-(6-methoxynaphthalen-2-yl)propanoate, C23H24O5
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  22. Crystal structure of poly[(μ3-5-bromoisophthalato-κ4 O,O′ :O″,O‴)-(μ2-1,2-bis(1,2,4-triazole-1-ylmethyl)benzene-κ2 N:N′)cobalt(II)], C20H15BrCoN6O4
  23. The crystal structure of bis(2-(piperidin-1-ium-4-yl)-1Hbenzo[d]imidazol-3-ium) dihydrogen decavanadate, C24H36N6O28V10
  24. Crystal structure of diaqua-bis(1-(3-carboxyphenyl)-5-methyl-4-oxo-1,4-dihydropyridazine3-carboxylato-O,O′)-cobalt(ii)dihydrate, C26H36N4O14Co
  25. Crystal structure of poly[(μ2-5-bromoisophthalato-κ4 O,O :O ,O )-(μ2-1,4-bis(2-methylimidazol-1-ylmethyl)benzene-N:N)cadmium(II)], C24H21BrCdN4O4
  26. The crystal structure of dimethyl 8-(3-methoxy-2-(methoxycarbonyl)-3-oxoprop-1-en-1-yl)-4-methyl-1-(p-tolyl)-1,3a,4,8b-tetrahydro-3H-furo[3,4-b]indole-3,3-dicarboxylate. C28H29NO9
  27. Crystal structure of (3R)-1-(3,5-dimethoxyphenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate chloride, C21H23ClN2O4
  28. Synthesis and crystal structure of 3-(4,5-dihydroisoxazol-3-yl)-2-methyl-4-(methylsulfonyl)benzoic acid, C12H13NO5S
  29. The crystal structure of hexaaquamagnesium(II) bis-3-(1,2,3,4-tetrahydrobenzo[4,5]imidazo[1,2-α]pyridin-1-yl)benzoate, C36H42N4O10Mg
  30. Crystal structure of 4-formyl-2-methoxyphenyl 2-acetoxybenzoate, C17H14O6
  31. Crystal structure of poly[octakis(μ-oxido)-tris(μ-1,1′-[[1,1′-biphenyl]-4,4′-diylbis(methylene)]bis(1H-imidazole))-tetrakis(oxido)-tetra-vanadium-dimanganese(II)dihydrate], C30H29MnN6O7V2
  32. Crystal structure of 4,8a-bis(4-chlorophenyl)-1,5,6-tris(4-fluorobenzyl)-1,4,4a,4b,5,6,8a,8b-octahydrocyclobuta[1,2-b:3,4-c′]dipyridine-3,8-dicarbonitrile, C45H33Cl2F3N4
  33. Crystal structure of benzo[d][1,3]dioxol-5-ylmethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C22H20O5
  34. Crystal structure of N-benzoyl-N-phenylhydroxylaminato-dicarbonylrhodium(I), [Rh(BNA)CO2]
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  36. The crystal structure of methyl ((4-aminobenzyl)sulfonyl)-d-prolinate, C13H18N2O4S
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  38. Crystal structure of poly[(μ 2-5-hydroxyisophthalato-κ4 O,O′:O″,O‴)-(μ 2-1,4-bis(2-methylimidazolyl)-1-butene-N:N′)nickel(II)], C20H20NiN4O5
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  54. Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
  55. The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
  56. The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 )
  57. Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
  58. Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
  59. Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
  60. Crystal structure of (R)-N, N -dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
  61. Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
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