Startseite The crystal structure of catena-poly[bis(6-phenylpyridine-2-carboxylato-κ2 N,O)-(μ2-4,4′-bipyridne-κ2 N:N)cadmium(II)], C34H24N4O4Cd
Artikel Open Access

The crystal structure of catena-poly[bis(6-phenylpyridine-2-carboxylato-κ2 N,O)-(μ2-4,4′-bipyridne-κ2 N:N)cadmium(II)], C34H24N4O4Cd

  • Liu Ping , Wang Li-Hua EMAIL logo und Tai Xi-Shi ORCID logo
Veröffentlicht/Copyright: 1. Juni 2023

Abstract

C 34 H 24 N 4 O 4 Cd, monoclinic, C2/c (no. 15), a = 17.5723(7) Å, b = 11.3574(4) Å, c = 15.8345(7) Å, β =  112.345 ( 5 ) ° , V = 2922.9(2)  Å 3 , Z = 4, R g t (F) = 0.0265, w R r e f ( F 2 ) = 0.0613, T = 200 K.

CCDC no.: 2263812

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: Block, colourless
Size: 0.13 × 0.12 × 0.09 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.79 mm−1
Diffractometer, scan mode: SuperNova, ω-scans
θ max, completeness: 25°, >99 %
N(hkl)measured , N(hkl)uniqueR int: 5879, 2574, 0.030
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 2400
N(param)refined: 195
Programs: Bruker programs [1], OLEX2 [2], SHELX [3], DIAMOND [4]
Table 2:

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

x y z U iso*/U eq
Cd1 0.500000 0.38550 (2) 0.750000 0.01761 (9)
O1 0.63719 (9) 0.37679 (13) 0.80362 (12) 0.0265 (4)
O2 0.75446 (10) 0.47327 (17) 0.87204 (14) 0.0494 (5)
N1 0.55439 (11) 0.55001 (17) 0.85284 (13) 0.0250 (4)
N2 0.50012 (11) 0.23581 (17) 0.64730 (13) 0.0235 (4)
C1 0.42839 (17) 0.6118 (2) 0.86948 (18) 0.0355 (7)
C2 0.36646 (19) 0.6972 (3) 0.8459 (2) 0.0505 (8)
H2 0.376030 0.771516 0.827237 0.061*
C3 0.29100 (19) 0.6718 (4) 0.8502 (2) 0.0649 (11)
H3 0.250363 0.729341 0.835096 0.078*
C4 0.2759 (2) 0.5632 (4) 0.8764 (3) 0.0679 (11)
H4 0.224876 0.546648 0.878814 0.082*
C5 0.33590 (17) 0.4778 (3) 0.8995 (2) 0.0522 (8)
H5 0.325390 0.403552 0.917382 0.063*
C6 0.41170 (15) 0.5021 (3) 0.89615 (17) 0.0357 (6)
H6 0.451983 0.443941 0.912013 0.043*
C7 0.51125 (18) 0.6386 (2) 0.87077 (18) 0.0351 (6)
C8 0.5463 (2) 0.7499 (3) 0.8934 (2) 0.0597 (9)
H8 0.515809 0.811629 0.903101 0.072*
C9 0.6262 (2) 0.7682 (3) 0.9015 (3) 0.0680 (11)
H9 0.649663 0.842629 0.915957 0.082*
C10 0.67110 (19) 0.6762 (3) 0.8880 (2) 0.0493 (8)
H10 0.725905 0.686262 0.895817 0.059*
C11 0.63264 (15) 0.5681 (2) 0.86241 (16) 0.0292 (6)
C12 0.67916 (13) 0.4642 (2) 0.84467 (16) 0.0283 (6)
C13 0.56921 (14) 0.1799 (2) 0.65550 (17) 0.0309 (6)
H13 0.618207 0.204551 0.700805 0.037*
C14 0.57194 (14) 0.0871 (2) 0.60026 (18) 0.0306 (6)
H14 0.621811 0.050942 0.608733 0.037*
C15 0.49986 (13) 0.04803 (19) 0.53208 (15) 0.0201 (5)
C16 0.42758 (14) 0.1049 (2) 0.52454 (17) 0.0259 (6)
H16 0.377557 0.081032 0.480643 0.031*
C17 0.43034 (13) 0.1968 (2) 0.58235 (16) 0.0266 (5)
H17 0.381234 0.233736 0.576031 0.032*

1 Source of materials

The title Cd(II) complex was synthesized in the step described below: at room temperature, 0.233 g cadmium nitrate tetrahydrate (0.50 mmol), 0.020 g NaOH (0.5 mmol), and 0.0996 g 6-phenylpyridine-2-carboxylic acid (0.50 mmol) were added to a 100 mL flask containing 15 mL of ethanol solvent and 5 mL water with stirring, and after 0.5 h of reaction, 0.0781 g 4,4 -bipyridine (0.5 mmol) was added to the above solution. The mixture was then reacted for a further 6 h at 75 °C. After cooled, the solution was filtered and the filtrate was allowed to evaporate slowly. The title complex was obtained in 4 weeks.

2 Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93 Å). Their U i s o values were set to 1.2 U e q of the parent atoms.

3 Comment

6–Phenylpyridine-2-carboxylate is an excellent pentadentate ligand, and it can form mononuclear cobalt(II) and copper(II) complexes with bidentate N,O-chelate modes [5, 6], binuclear and tetranuclear lead(II) complexes with tridentate N,O:O-chelate modes [7, 8]. To further investigate the coordination diversity of the 6-phenylpyridine-2-carboxylate a new Cd(III) coordination polymer has been synthesized and structurally characterized. X-ray single crystal diffraction analysis indicates that the title Cd(II) complex forms coordination polymer through the bridging effect of 4,4 -bipyridine with the Cd(II)–Cd(II) distance of 11.805 Å. The molecular structure of the Cd(II) complex is given in the figure (symmetry code: a:1‒x, y, 1.5‒z).

The asymmetric unit consists of one Cd(II)ion, two L anions, and one 4,4 -bipyridine co-ligand. Each Cd(II) atom is coordinated with two oxygen atoms from two L ligands, two nitrogen atoms from two L ligands, and two nitrogen atoms from two 4,4 -bipyridine co-ligands forming a distorted octahedral Cd N 4 O 2 coordination geometry. And N1, N1a, N2, and N2a form the plane of the octahedron, while O1, O1a are in the axial position of the octahedron. The bond angle of O1–Cd–O1a is 174.92 ( 8 ) ° , indicating the octahedral structure is slightly deformed. The Cd–O and Cd–N lengths are 2.2329(15) Å and 2.3531(19)–2.4233(19) Å, respectively. The O–Cd–O, O–Cd–N and N–Cd–N bond angles lie in the range of 174.92 ( 8 ) ° , 71.68(6)– 112.50 ( 6 ) ° , and 79.11(9)– 156.58 ( 6 ) ° , respectively. The bond lengths and bond angles are consistent as reported in the literature [9]. A similar structure has been found in the crystal structure of Zn(II) complex with 6-phenylpyridine-2-carboxylic acid as ligand and 4,4 -bipyridine as co-ligand [10]. The complex molecules form a one-dimensional zigzag chain structure by the bridging of 4,4 -bipyridine.


Corresponding author: Wang Li-Hua, College of Biology and Oceanography, Weifang University, Weifang, Shandong 261061, P.R. China, E-mail:

Funding source: The Science Foundation of Weifang

Award Identifier / Grant number: 2020ZJ1054

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

  2. Research funding: This project was supported by the Science Foundation of Weifang (2020ZJ1054).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

References

1. Bruker. SAINT and SADABS; Bruker AXS Inc.: Madison, Wisconsin, USA, 2000.Suche in Google Scholar

2. Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K., Puschmann, H. OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Crystallogr. 2009, 42, 339–341; https://doi.org/10.1107/s0021889808042726.Suche in Google Scholar

3. Sheldrick, G. M. Crystal structure refinement with SHELXL. Acta Crystallogr. 2015, C71, 3–8; https://doi.org/10.1107/s2053229614024218.Suche in Google Scholar

4. Brandenburg, K. DIAMOND. Visual Crystal Structure Information System. Ver. 3.2; Crystal Impact: Bonn, Germany, 2012.Suche in Google Scholar

5. Wang, L. H., Liang, L., Li, X. T., Cao, S. H., Tai, X. S. The crystal structure of bis(6-phenylpyridine-2-carboxylato-κ2N,O)copper(II), C24H16N2O4Cu. Z. Kristallogr. N. Cryst. Struct. 2021, 236, 1251–1253.10.1515/ncrs-2021-0293Suche in Google Scholar

6. Gao, X., Tai, X. S. The crystal structure of diaqua-bis(6-phenylpyridine-2-carboxylato-κ2N,O)cobalt(II)-water-N,N-dimethylformamide(1/2/1),C27H31N3O9Co. Z. Kristallogr. N. Cryst. Struct. 2022, 237, 393–395; https://doi.org/10.1515/ncrs-2022-0067.Suche in Google Scholar

7. Tai, X. S., Liang, L., Li, X. T., Cao, S. H., Wang, L. H. Crystal structure of diaqua-bis(u2-6-phenylpyridine-2-carboxylato-κ3N,O:O)-bis(6-phenylpyridine-2-carboxylato-κ2N,O)lead(II)-N,N-dimethylformamide-water(1/2/4), C54H58N6O16Pb2. Z. Kristallogr. N. Cryst. Struct. 2021, 236, 1199–1201; https://doi.org/10.1515/ncrs-2021-0277.Suche in Google Scholar

8. Wang, L. H., Tai, H. W., Li, Q. S., Xia, Y. P., Tai, X. S. The crystal structure of tetrakis(6-phenylpyridine-2-carboxylato-κ2N,O)-bis(u2-6-phenylpyridine-2-carboxylato-k2O:O′)-bis(u2-6-phenylpyridine-2-carboxylato-k3N,O:O)tetralead(II), C48H32N4O8Pb2. Z. Kristallogr. N. Cryst. Struct. 2022, 237, 1113–1116.10.1515/ncrs-2022-0119Suche in Google Scholar

9. Tai, X. S., Kong, F. Y., Zhou, X. J., Xia, Y. P. Synthesis, structural characterization and fluorescent property of Cd(II) coordination polymer based on N-nicotinoylglycine ligand. Crystallogr. Rep. 2022, 67, 209–213; https://doi.org/10.1134/s1063774522020225.Suche in Google Scholar

10. Wang, L. H., Tai, X. S., Xia, Y. P. The crystal structure of catena-poly [(m2-4,4′-bipyridine-κ2N:N)-bis(6-phenylpyridine-2-carboxylato-κ2N,O)zinc(II)], C34H24N4O4Zn. Z. Kristallogr. N. Cryst. Struct. 2022, 237, 305–307; https://doi.org/10.1515/ncrs-2022-0003.Suche in Google Scholar

Received: 2023-04-24
Accepted: 2023-05-18
Published Online: 2023-06-01
Published in Print: 2023-08-28

© 2023 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. Crystal structure of a polymorph of potassium picrate, C6H2KN3O7
  4. The crystal structure of (1E,2E)-1,2-bis(quinolin-2-ylmethylene)hydrazine, C20H14N4
  5. 5-Amino-2-chloro-4-fluoro-N-(N-isopropyl-N-methylsulfamoyl) benzamide, C11H15O3ClFN3S
  6. Crystal structure of trans-N 1,N 8-bis(2-cyanoethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane, C22H42N6
  7. The crystal structure of [N-{[2-(oxy)-4-methoxyphenyl](phenyl)methylidene}alaninato]-diphenyl-silicon(IV) – chloroform (1/1), C29H25NO4Si·CHCl3
  8. Crystal structure of tetracarbonyl-{μ-[N-(diphenylphosphanyl)-N,P,P-triphenylphosphinous amide]}-bis[μ-(phenylmethanethiolato)]diiron (Fe–Fe), C48H39Fe2NO4P2S2
  9. Crystal structure of baryte from Mine du Pradet (France)
  10. The crystal structure of [(2,2′-bipyridine-6-carboxylato-κ3 N,N,O)-(6-phenylpyridine-2-carboxylate-κ2 N,O)copper(II)] monohydrate, C23H17N3O5Cu
  11. Crystal structure of bis(μ-benzeneselenolato)-(μ-[N-benzyl-N-(diphenylphosphanyl)-P,P-diphenylphosphinous amide])-tetracarbonyl diiron (Fe–Fe), C47H37Fe2NO4P2Se2
  12. The crystal structure of diaqua-methanol-κ1 O- (3-thiophenecarboxylato-κO)-(2,2′-dipyridyl-κ2 N,N′)manganese(II) 3-thiophenecarboxylate, C21H22N2O7S2Mn
  13. Crystal structure of catena-poly[tetrakis(butyl)-μ2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-κ4 O:O,O′,N-μ2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-κ4 O,N,O′:N′-ditin(IV)], C34H50N6O6Sn2
  14. Crystal structure of 4-chloro-N′-[(1E)-(2-nitrophenyl)methylidene]benzohydrazide, C14H10ClN3O3
  15. The crystal structure of 3-(1′-deoxy-3′,5′-O-dibenzy-β-d-ribosyl)adenine dichloromethane solvate, C49H52Cl2N10O6
  16. The crystal structure of (Z)-4-amino-N′-(1-(o-tolyl)ethylidene)benzohydrazide, C16H17N3O
  17. The co-crystal structure of etoricoxib–phthalic acid (1/1), C18H15ClN2O2S·C8H6O4
  18. Crystal structure of (glycinto-κ 2 O,N )-[5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ 4 N,N ,N ,N ]nickel(II) perchlorate monohydrate C18H42ClN5NiO7
  19. The crystal structure of catena-poly[bis(1-ethylimidazole-k1 N)-(μ 2-benzene-1-carboxyl-3,5-dicarboxylato-κ 2 O, O′)zinc(II)], C19H20N4O6Zn
  20. Crystal structure of 3-(thiazol-2-ylcarbamoyl)-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid, C11H12N2O4S
  21. Rietveld structure analysis of keatite, a rare, metastable SiO2 polymorph
  22. Crystal structure of catena-poly[(μ2-isophthalato-k3 O,O′:O″)(4-(4-pyridyl)-2,5-dipyrazylpyridine-k3 N,N′,N″)cobalt(II)] trihydrate C26H22N6O7Co1
  23. Crystal structure of 3,5–di-O-benzoyl-1,2-O-isopropylidene-α–D-ribose, C22H22O7
  24. The crystal structure of fac-tricarbonyl(6-bromo-2,2-bipyridine-κ2 N,N)-(nitrato-κO)rhenium(I), C13H7BrN3O6Re
  25. The crystal structure of (E)-N′-(4-hydroxy-3-methoxybenzylidene)-2-naphthohydrazide monohydrate, C19H18N2O4
  26. The crystal structure of 5,5′-diselanediyl-bis(2-hydroxybenzaldehyde), C14H10O4Se2
  27. The crystal structure of catena-poly[diaqua-m2-dicyanido-κ2 C:N-dicyanido-κ1 C-bis(4-(pyridin-4-yl)benzaldehyde-κ1N)iron(II)-platinum(II), C28H22N6O4PtFe
  28. Redetermination of the crystal structure of 5,14-dihydro-6,17-dimethyl-8,15-diphenyldibenzo(b,i)(1,4,8,11)tetra-azacyclotetradecine, C32H28N4
  29. Crystal structure of poly[(μ3-2-(3,5-dicarboxyphenyl) benzimidazole-6-carboxylato-κ4O:O:O′:O″)lead(II)] monohydrate, C16H10N2O7Pb
  30. The crystal structure of fac-tricarbonyl(2-pyridin-2-yl-quinoline-κ2 N,N′)-(pyrazole-κN)rhenium(I)nitrate, C20H14N4O3ReNO3
  31. Crystal structure of dibromo-dicarbonyl-bis(tricyclohexylphosphine)-osmium(II) dichloromethane solvate, C38H66Br2O2OsP2
  32. Crystal structure of poly[bis(μ 2-2,6-bis(1-imidazoly)pyridine-κ 2 N:N′)copper(II)] diperchlorate dihydrate, C22H22Cl2CuN10O10
  33. The crystal structure of fac-tricarbonyl(N-benzoyl-N,N-cyclohexylmethylcarbamimidothioato-κ2 S,O)-(pyridine-κN)rhenium(I), C23H24N3O4ReS
  34. Crystal structure of (E)-7-fluoro-2-(4-fluorobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C17H12F2O
  35. Synthesis and crystal structure of 1-((3R,10S,13S, 17S)-3-((2-methoxyphenyl)amino)-10,13-dimethylhexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO2
  36. The crystal structure of fac-tricarbonyl((pyridin-2-yl)methanamino-κ2 N,N′)-((pyridin-2-yl)methanamino-κN)rhenium(I) nitrate, C15H16O3N4Re
  37. The crystal structure of (1-(pyridin-2-yl)-N-(pyridin-2-ylmethyl)-N-((1-(4-vinylbenzyl)-1H-benzo[d]imidazol-2-yl)methyl)methanamine-κ 4 N,N′,N″,N‴)tris(nitrato-kO,O′)-erbium(III), C29H27ErN8O9
  38. Crystal structure of tetracene-5,12-dione, C18H10O2
  39. Crystal structure of (3R,3aS,6R,6aR)-6-hexyl-3-methyltetrahydrofuro[3,4-b]furan-2,4-dione, C13H20O4
  40. The crystal structure of N1,N3-bis((E)-thiophen-2-ylmethylene)isophthalohydrazide monohydrate, C18H16N4O3S2
  41. Crystal structure of methyl ((4-aminobenzyl)sulfonyl)-L-prolinate, C13H18N2O4S
  42. Crystal structure of (E)-3-(3-methoxybenzylidene)benzofuran-2(3H)-one, C16H12O3
  43. Synthesis and crystal structure (E)-1-(4-bromo-2-hydroxyphenyl)-3-(dimethylamino)prop-2-en-1-one, C11H12BrNO2
  44. Synthesis and crystal structure of (S,E)-4-hydroxy-3-(2-((4aR,6aS,7R,10aS,10bR)-3,3,6a,10b-tetramethyl-8-methylenedecahydro-1H-naphtho[2,1-d][1,3]dioxin-7-yl)ethylidene)dihydrofuran-2(3H)-one, C23H34O5
  45. The crystal structure of N,N′-(1,2-phenylene)bis (2-((2-oxopropyl)selanyl)benzamide), C26H24N2O4Se2
  46. The crystal structure of 1-ethyl-2-nitro-imidazole oxide, C5H7N3O3
  47. The crystal structure of 2-(2-fluorophenyl)naphtho[2,1-d]thiazole, C17H10FNS
  48. Crystal structure of (E)-2,4-di-tert-butyl-6-(((2-fluorophenyl)imino) methyl)phenol, C21H26FNO
  49. Synthesis and crystal structure of 3-methyl-2-(methylthio)-4H-chromen-4-one, C12H12O2S
  50. Crystal structure of dithieno[2,3-d:2′,3′-d′]benzo[1,2-b:4,5-b′]dithiophene-5,10-dione, C14H4O2S4
  51. The crystal structure of dimethyl 2,2ʹ-((adamantane-1,3-diylbis(4,1-phenylene)) bis(oxy))diacetate, C28H32O6
  52. The crystal structure of N-(6-chloro-2-methyl-2H-indazol-5-yl)acetamide, C10H10ClN3O
  53. Crystal structure of triaqua-(5-bromoisophthalato-κ1 O)-(2,2′-bipyridine-κ2 N:N′)nickel(II) hydrate, C18H19BrN2NiO8
  54. The crystal structure of 2-amino-4-carboxypyridin-1-ium perchlorate, C6H7ClN2O6
  55. The crystal structure of catena-poly[5-aminonicotinic acid-k1 N-m2-bromido-copper(I)], Cu(C6N2H6O2)Br
  56. The crystal structure of 2,2-bis(3-methoxyphenyl)-1-tosyl-1,2-dihydro- 4,3λ4  -[1,3,2]diazaborolo[4,5,1-ij]quinoline - dichloromethane (1/1)
  57. The crystal structure of catena-poly[bis(6-phenylpyridine-2-carboxylato-κ2 N,O)-(μ2-4,4′-bipyridne-κ2 N:N)cadmium(II)], C34H24N4O4Cd
  58. The crystal structure of 5,7-dinitropyrazolo[5,1-b]quinazolin-9(4H)-one, C10H5N5O5
  59. Crystal structure of rac-1,8-bis(2-carbamoylethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane, C22H46N6O2
  60. The crystal structure of (E)-N -(2-bromobenzylidene)-2-naphthohydrazide, C36H26Br2N4O2
  61. The crystal structure of 5-nitronaphthoquinone, C10H5NO4
  62. The crystal structure of (S, R p )-4–benzhydrylideneamino-12-(4-tert-butyl oxazolin-2-yl)[2.2]paracyclophane, C36H36N2O
  63. Synthesis and crystal structure of 2-(2-oxo-2-(o-tolyl)ethyl)-4H-chromen-4-one, C18H14O3
  64. Crystal structure of 2-(thiazol-2-yl)hexahydro-1H-4,7-epoxyisoindole-1,3(2H)-dione, C11H10N2O3S
  65. Crystal structure of N-(diaminomethylene)-1-(dimethylamino)-1-iminiomethanaminium dichloride, C4H13Cl2N5
  66. Crystal structure of poly[(μ3-3, 5-dichloro-2-hydroxy-benzoato-κ4 Cl,O:O′:O″) silver(I)], C7H3AgCl2O3
  67. The crystal structure of tetrakis(1-isopropylimidazole-κ1 N)-[μ2- imidazole-4,5-dicarboxylato-κ4 O,N,O′,N′)]- trioxido-divanadium, C29H41N10O7V2
  68. Crystal structure of catena-[(μ3-bromido)-(1H-1,2,4-triazol-1-yl)benzoato-κ1 N)copper(I)], C9H7BrCuN3O2
  69. The crystal structure of (E)-4-fluoro-N′-(1-(2-hydroxyphenyl)propylidene)benzohydrazide, C16H15FN2O2
Heruntergeladen am 7.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2023-0201/html
Button zum nach oben scrollen