Startseite Crystal structure of poly[diaqua-di-μ2-hydroxido-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ4O:O′:O′′:O′′′)-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ5O,O:O′:O′′:O′′′)disamarium(III)] – bipyridine (2/1), C21H11NF16O12Sm2
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Crystal structure of poly[diaqua-di-μ2-hydroxido-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ4O:O′:O′′:O′′′)-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ5O,O:O′:O′′:O′′′)disamarium(III)] – bipyridine (2/1), C21H11NF16O12Sm2

  • Xun Feng EMAIL logo , Rui Wang , Xin Yi Wang , Ying Ying Zhang und Xi Xi Jia
Veröffentlicht/Copyright: 18. Oktober 2018

Abstract

C21H11NF16O12Sm2, triclinic, P1̄ (no. 2), a = 7.7872(5) Å, b = 9.9149(6) Å, c = 16.9804(10) Å, α = 79.4970(10)°, β = 76.8620(10)°, γ = 78.1480(10)°, V = 1236.80(13) Å3, Z = 2, Rgt(F) = 0.0411, wRref(F2) = 0.1158, T = 293(2) K.

CCDC no.: 1858555

A part of the polymeric title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Colorless block
Size:0.23 × 0.18 × 0.14 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:4.83 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
θmax, completeness:25°, >99%
N(hkl)measured, N(hkl)unique, Rint:6329, 4361, 0.033
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3872
N(param)refined:367
Programs:Bruker programs [1], SHELX [2]
Table 2:

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

AtomxyzUiso*/Ueq
Sm10.10291(4)0.66089(3)0.42809(2)0.01455(13)
Sm20.58450(4)0.68458(3)0.50455(2)0.01407(13)
F0AA0.9623(7)0.6434(6)0.0192(3)0.0560(14)*
F10.4518(7)0.4711(7)0.1642(3)0.0603(16)
F1AA0.2178(7)1.0924(5)0.7822(3)0.0424(12)*
F20.6675(8)0.5382(7)0.0216(4)0.0639(16)*
F41.0449(6)0.6741(6)0.1546(3)0.0477(13)
F5−0.0309(6)0.6761(5)0.7021(3)0.0391(11)
F6−0.0720(9)0.7061(6)0.8571(3)0.0575(16)
F70.0562(10)0.9144(7)0.8989(3)0.0674(18)
N10.3550(11)0.9429(12)0.2129(5)0.060(3)
O10.3557(6)0.5915(5)0.3233(3)0.0281(11)
O1W0.2236(7)0.8714(5)0.3722(3)0.0300(12)
H1WA0.31430.87750.40080.045*
H1WB0.27490.87010.31530.045*
O20.5393(6)0.3988(5)0.3592(3)0.0211(10)
O2W0.6545(6)0.8396(5)0.5886(3)0.0254(11)
H2WA0.77490.80890.59720.038*
H2WB0.64280.93330.56060.038*
O30.6991(7)0.6237(5)0.3732(3)0.0293(12)
O40.9823(7)0.6242(6)0.3169(3)0.0382(14)
O50.0445(6)0.8044(5)0.5441(3)0.0262(11)
O60.3122(6)0.8569(5)0.5317(3)0.0203(10)
O7−0.1661(6)0.8305(5)0.4234(3)0.0197(10)
O80.5717(6)0.9137(5)0.3942(3)0.0249(11)
O90.3373(5)0.5785(4)0.4962(3)0.0159(9)
H90.28010.57950.54450.024*
O100.8701(5)0.5891(4)0.5411(3)0.0160(9)
H100.87630.62090.58270.024*
C0AA0.8571(10)0.6079(8)0.0896(5)0.0312(17)*
C10.4973(9)0.5092(7)0.3142(4)0.0211(15)
C20.6323(9)0.5422(8)0.2366(4)0.0222(15)
C30.5968(10)0.5218(9)0.1645(5)0.0316(17)
C40.7071(11)0.5551(9)0.0915(5)0.0354(18)*
C54696(14)0.9891(11)0.0444(7)0.054(3)*
C60.8965(10)0.6242(8)0.1610(4)0.0275(16)
C70.7880(8)0.5921(7)0.2359(4)0.0196(14)
C80.8280(9)0.6149(7)0.3132(4)0.0226(15)
C90.1588(8)0.8424(6)0.5712(4)0.0177(14)
C100.1188(8)0.8701(7)0.6576(4)0.0178(13)
C110.0309(10)0.7812(7)0.7189(5)0.0249(16)
C120.0105(11)0.7958(8)0.7987(5)0.0335(18)
C130.0759(12)0.8999(9)0.8198(4)0.0360(19)
C140.1591(10)0.9880(8)0.7607(4)0.0272(16)
C150.1835(8)0.9749(7)0.6795(4)0.0173(13)
C16−0.2677(8)0.9173(6)0.3836(4)0.0172(13)
C170.3396(16)0.8533(14)0.1670(8)0.069(3)
C180.3967(16)0.8693(13)0.0824(7)0.070(3)
C190.4805(16)1.0797(15)0.0927(8)0.079(4)
C210.4214(16)1.0572(15)0.1779(7)0.074(4)

Source of material

An organic compound (3,4,5,6-tetrafluoro-1,2 phthalate acid, abbreviated as Tfpa) (0.047 g, 0.2 mmol) in a solution of water/alcohol (v/v = 1.2, 10 mL) was mixed with an aqueous solution of 0.2 mmol Sm(NO3)3 ⋅ 6H2O, 0.042 g and a solution (10 mL) of 4,4′-bipyridine (abbreviated as bipy) (0.2 mmol, 0.032 g). After stirring for 30 min, the pH value was adjusted to 4.5 using nitric acid. The mixture was placed into 25 mL Teflon-lined autoclave and under autogenous pressure this mixture was heated at 155 °C for 72 h, and then the autoclave was cooled over a period of 24 h at a rate 5 °C/h. After filtration, the product was washed with distilled water and then dried. Colorless crystals of title compound were obtained suitable for X-ray diffraction analysis. Yield: 0.0156 g (43%) based on lanthanide element. Elemental analysis (%): calcd. for C21H11NF16O12Sm2: C 27.36, H 1.20, N 1.52, found: C 27.52, H 1.17, N 1.60. IR (KBr pellet, cm−1): 3339s, 2198s, 1704vs, 1617s, 1546s, 1467s, 12639s, 1132s, 866m, 793s, 660s.

Experimental details

The coordinates of the H-atoms at the water molecules were refined with the O-H distance restrained to 0.85 Å. The Uiso values of the hydrogen atoms of methyl groups were set to 1.5Ueq(C) and the Uiso values of all other hydrogen atoms were set to 1.2Ueq (C, N).

Discussion

It is well known that aromatic multi-carboxylic acid, and the corresponding deprotonated anions such as isophthalic acid are very important building blocks of many important compounds widely used in many fields [3], [4] . Lanthanide 3+ ions are usually selected as luminescent centers owing to their high luminescent quantum yield, long lifetime and large Stokes shifts [5]. In order to further study the coordination behavior and role of samarium(III) cation in the selfassembly processes in the presence of fluorine substituted dicarboxylate and nitrogen-heterocyclic compound, the title complex has been synthesized and systematically characterized.

The structure contains two discrete parts: a 4,4′-bipyridine molecule and a Sm(III) coordination polymer. The asymmetric unit of the coordination unit polymer consists of two kinds of Sm(III) ion, two Tfpa ligands, two hydroxido ligands and two coordination water molecules, as illustrated in the figure. In this unit, the first Sm(III) ion is eight folded coordinated with an O8 donor set, among which five oxygen atoms are derivated from Tfpa ligand, one oxygen atom is from water molecule, another oxygen atom is derivated from hydroxyl group, completing the dodecahedron geometry around the central ion. As for the second Sm(III) cation, it is coordinated with an O9 donor set, the polyhedron around this Sm(III) ion is best described as a distorted monocapped anti-prism, as shown in the figure. The oxygen atoms are derivated from Tfpa ligand, water molecule, and hydroxyl group, respectively. The bipy does not coordinate with the Sm(III) ion. This is obvious different from the transition metal compound [6]. The first kind of Tfpa ligand using two carboxylate bridging two adjacent Sm(III) cations, and the second kind of Tfpa ligand one carboxylate connects two adjacent Sm(III) cations in both chelate and mono coordination fashions. Both oxygen atoms from hydroxyl group adopt μ3-fashion connecting three neighboring Sm(III) ions. This coordination mode is also found in other lanthanide compound [7]. The Sm(III)—O bond distances are in range from 2.310(3) to 2.668(4) Å, with average of 2.48 Å. Bond angles of O-Sm(III)-O are in range of 41.34(8) to 159.19(8)°. All the bond lengths and bond angles are in accordance to the reported relevant literatures [8]. As for another carboxylate, it employs mono coordination mode linking two adjacent Sm(III) ions in the same time. Two carboxylate from the Tfpa ligand doubly bridges two adjacent Sm(III) cations, resulting in the dinuclear units with Sm⋯Sm separation of just 3.922 Å. The dinuclear units are further connected into one dimensional double chain through the carboxylate from the Tfpa ligand [9], [10] . This coordination architecture is different from similar lanthanide compound based on fluorine substituted ligand [11].

Acknowledgements

This work was supported by the Foundation for Science & Technology Innovation Talents in Henan province (Nos. 14HASTIT014 and 164100510012), Natural Science Foundation of China (Nos. 21671114 and U1604143), and the Tackle Key Problem of Science and Technology Project of Henan Province, China (no. 182102310897).

References

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Received: 2018-05-13
Accepted: 2018-07-26
Published Online: 2018-10-18
Published in Print: 2018-12-19

©2018 Xun Feng et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of bis(6,6′-((ethane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(2,4-diiodophenolato)-κ4N,N′,O,O′)cer(IV), C32H20CeI8N4O4
  3. Crystal structure of (6,6′-((ethane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(2-chlorophenolato-κ2N,O))copper(II), C16H12Cl2CuN2O2
  4. Crystal structure of poly[aqua-(μ3-4-(pyridin-4-yl)isophthalato-κ4O,O′:O′′:O′′′)-(μ2-5-carboxy-2-(pyridin-4-yl)benzoato-κ2O:O′)samarium(III)], C26H18N2O9Sm
  5. Crystal structure of 1-{4-[(2-hydroxy-5-nitrobenzylidene)amino]phenyl}ethanone O-methyl oxime, C16H15N3O4
  6. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-bis(μ2-1-(8-(2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)naphthalen-2-olato-κ6O:O,N,N′,O′:O′)trizinc(II), C44H38Zn3N4O12
  7. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)–bis(μ2–(8-(2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)naphthalen-2-olato-κ6O:O,N,N′,O′:O′)tricobalt(II), C44H38Co3N4O12
  8. Crystal structure of poly[aqua(μ4-2,2′,2′′-nitrilotriacetato-κ6O1,O3,O5:O2:O4:O6)-yttrium(III)], C6H8NO7Y
  9. Crystal structure of catena-poly[bromido-(μ2-pyrazine-2-carboxylato-κ3N:N′,O)copper(II)], C10H6N4Cu2O4Br
  10. Crystal structure of poly[dodekais(μ2-2,6-difluorobenzoato-κ2O:O′)-bis((μ3-hexamethylenetetramine-κ3N:N′:N′′)hexacopper(II)], C48H30N4O12F12Cu3
  11. Crystal structure of methyl 4-(4-hydroxy-3-nitrophenyl)-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C18H18N2O6
  12. Crystal structure of N-phenyl-2-(propan-2-ylidene)hydrazine-1-carbothioamide, C10H13N3S
  13. Crystal structure of sodium caesium zinc phosphate, NaCsZnP2O7
  14. Crystal structure of methyl 4-(4-isopropylphenyl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydro-quinoline-3-carboxylate, C23H29NO3
  15. Crystal structure of catena-poly[bis(μ2-1,3-di(4H-1,2,4-triazol-4-yl)benzene-κ2N:N′)-bis(thiocyanato-κ1N)cobalt(II), C22H16CoN14S2
  16. Crystal structure of catena-poly[(μ2-2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-κ2N:N′)-bis(2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-κ1N)-bis(thiocyanato-κ1N)cobalt(II)], C38H24CoN14S5
  17. Crystal structure of bis(2,5-di(pyridin-2-yl)-1,3,4-thiadiazole-κ2N,N′)-bis(thiocyanato-κ1N)cobalt(II), C26H16CoN10S4
  18. Crystal structure of (bis((1H-benzo[d]imidazol2-yl)methyl)amine-κ3N,N′,N′′)-(pyridine-2,6-dicarboxylato-κ3N,O,O′)zinc(II) — methanol — water (1/2/1), C25H28N6O7Zn
  19. Crystal structure of catena-poly[triaqua-(μ2-5-methoxy-isophthalato-κ2O:O′)copper(II)], C9H12CuO8
  20. Structure and photochromism of 1-[2-methyl-5-phenyl-3-thienyl]-2-[2-methyl-5-(4-chlorophenyl)-3-thienyl]3,3,4,4,5,5-hexafluorocyclopent-1-ene, C27H16ClF6S2
  21. Crystal structure of methyl 4-(3-phenoxyphenyl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C26H27NO4
  22. Crystal structure of poly[diaqua-di-μ2-hydroxido-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ4O:O′:O′′:O′′′)-(μ4-3,4,5,6-tetrafluoro-1,2-phthalato-κ5O,O:O′:O′′:O′′′)disamarium(III)] – bipyridine (2/1), C21H11NF16O12Sm2
  23. Crystal structural of diethyl 4-(3,5-dibromo-4-hydroxyphenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate, C19H21Br2NO5
  24. Crystal structure of catena-poly[tetraaqua(μ2-4-(1H-imidazol-1-yl)pyridine-κ2N:N′))zinc(II)] thiophene-2,5-dicarboxylate, C14H17N3O8ZnS
  25. Crystal structure of (20S)-20-(dimethylamino)-3-(tigloylamino)-5α-pregn-2,16-dien-4-one, C28H42N2O2
  26. Crystal structure of rac-trans-N,N′-bis(3,5-diiodosalicylidene)-1,2-cyclohexanediamine, C20H18I4N2O2
  27. Crystal structure of 2-bromo-7-(4-(dimethylamino)phenyl)-10-methylacridin-9 (10H)-one, C22H19BrN2O
  28. Crystal structure of catena-poly[(μ2-pentane-1,5-dicarboxylato-κ2O:O′)-(μ2-2-[(1H-imidazol-1-yl)methyl]-6-methyl-1H-benzimidazole-κ2N:N′)zinc(II)] sesquihydrate, C17H21N4O5.5Zn
  29. Crystal structure of ethyl 2-amino-4-(3,4-difluorophenyl)-5-oxo-4H,5H-pyrano[3,2-c] chromene-3-carboxylate, C21H15F2NO5
  30. Crystal structure of 9-(5-methylthiophen-2-yl)-3,4,5,6,7,9-hexahydro-1H-xanthene-1,8(2H)-dione, C18H18O3S
  31. Crystal structure of [5,5′-((propane-1,3-diylbis(azanylylidene))bis(ethan-1-yl-2-ylidene))bis(3-(ethoxycarbonyl)-2,4-dimethylpyrrol-1-ido)-κ4N,N′,N′′,N′′′]nickel(II), C23H30N4O4Ni
  32. Crystal structure of (Z)-2-(2-(1,3-dioxo-1-(phenylamino)butan-2-ylidene)hydrazineyl) terephthalic acid-dimethylsulfoxide (1/1), C18H15N3O6 ⋅ C2H6OS
  33. Crystal structure of (2E,4Z)-dimethyl 4-((phenylamino)methylene)pent-2-enedioate, C14H15N1O4
  34. Crystal structure of (2Z,2′Z)-1,1′-(pyridine-2,6-diyl) bis(3-hydroxy-3-phenylprop-2-en-1-one), C23H17NO4
  35. Crystal structure of ethyl 2-amino-4-(3-bromophenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carboxylate, C21H16BrNO5
  36. Crystal structure of bis(μ2-3,5-dichloro-2-oxidobenzoato-κ4O,O′:O′,O′′)-hexakis(μ2-pivalato-κ2O:O′)-bis(pivalato-κ2O,O′)-tetrakis(1,10-phenanthroline-κ2N,N′)tetragadolinium(III), C102H108Cl4Gd4N8O22
  37. Crystal structure of catena-poly[aqua-bis(formato-κ1O)-(μ2-1,1′-(oxybis(1,4-phenylene))-bis(1H-1,2,4-triazole)-κ2N:N′)copper(II)]hydrate, C18H16CuN6O6
  38. Crystal structure of 5-bromo-2-(naphthalen-6-yl)pyridine, C15H10BrN
  39. Crystal structure of N-(4-methoxybenzyl)pyridazin-3-amine- a rare Z′ = 4 structure, C12H13N3O
  40. Crystal structure of bis(perchlorato-κ1O)-bis(3,4,5-trimethoxy-N-(pyridin-2-yl)benzamide-κ2N,O)copper(II), C32H30Cl2CuN4O16
  41. Crystal structure of methyl 4-methyl-2,5-di(pyridin-4-yl)-1H-pyrrole-3-carboxylate monohydrate C17H15N3O2⋅H2O
  42. Crystal structure of dimethyl 5-(10-(methoxycarbonyl)anthracen-9-yl) isophthalate,C26H20O6
  43. Crystal structure of tert-butyl (R)-(1-(benzylamino)-3-methoxy-1-oxopropan-2-yl)carbamate, C16H24N2O4
  44. Crystal structure of aqua-bis(1,5-dimethyl-2-phenyl-4-(((E)-4-pyridylmethylene)amino)pyrazolidin-3-one-κN)-(nitrato-κO)-(nitrato-κ2O,O′)zinc(II), C34H34N10O9Zn
  45. Crystal structure of catena-poly[dichlorido-(μ2-1,5-dimethyl-2-phenyl-4-((pyridin-4-ylmethylene)amino)-1,2-dihydro-3H-pyrazol-3-one-κ2N:O)cobalt(II)] – methanol (1/1), C18H20Cl2CoN4O2
  46. Crystal structure of poly[diaqua-bis(μ2-1-(4-(1H-imidazol-1-yl)benzyl)-1H-1,2,4-triazole-κ2N:N′)manganese(II)]bis(2-carboxybenzoate) dihydrate, MnC40H40N10O12
  47. The crystal structure of 4-((3,4-dichlorobenzylidene)amino)-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one, C18H15Cl2N3O
  48. Crystal structure of bis(2-methoxy-6-((2-(pyrimidin-2-yl)hydrazono)methyl)phenolato-κ3N,N′,O)iron(III) perchlorate, C24H22N8O8ClFe
  49. The crystal structure of 2-[4-hydroxy-3-methoxyphenyl]-4,4,5,5-tetramethylimidazoline-3-oxide-1-oxyl, C14H19N2O4
  50. Crystal structure of diaqua-bis(3,3-dimethylacrylato-κ2O,O′)zinc(II), C10H18ZnO6
  51. Crystal structure of dichloro-tetrakis[(E)-1-(4-chlorophenyl)-4,4-dimethyl-2-(1H-1,2,4-triazol-1-yl)pent-1-en-3-ol-κN]cadmium (II), C60H74CdCl6N12O4
  52. Crystal structure of (20R)-20,25-epoxy-dammaran-3,12-dione, C30H48O3
  53. Crystal structure of (E)-3′,6′-bis(ethylamino)-2′,7′-dimethyl-2-((pyridin-2-ylmethylene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C32H31N5O2
  54. The crystal structure of 2-(4-fluorophenyl)-1,3,4-oxadiazole, C8H5FN2O
  55. Crystal structure of (2,2′-bipyridine-κ2N,N′)bis(tri(p-tolyl)phosphine-κP)copper(I) tetrafluoroborate – 4,4′-bipyridine (2/1), C57H54BCuF4N3P2
  56. The crystal structure of 2,6-dimethyl-3,5-dinitrocyclohexa-2,5-diene-1,4-dione, C8H6N2O6
  57. The crystal structure of 2,3-dimethyl-1,4-dinitrobenzene – a Z′ = 4 structure, C8H8N2O4
  58. Crystal structure of [(1,2-η)-1,2,3,4,5-pentamethyl-cyclopenta-2,4-dien-1-yl] (1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-κ6N2,O4) rubidium (I), [Rb(diaza-18-crown-6)]Cp*, C22H41N2O4Rb
  59. Crystal structure of 2-(4-fluorophenyl)-N-phenyl-2-(phenylamino)ethanesulfonamide – toluene (1/0.5), C23.5H23FN2O2S
  60. Crystal structure of pyrene-4-aldehyde, C17H10O
  61. Crystal structure of 2-(furan-2-yl)-5-methyl-1,3-dioxane-5-carboxylic acid, C10H12O5
  62. Crystal structure of 2-(4-chlorophenyl)-3-phenyl-1,8-naphthyridine, C20H13N2Cl
  63. Crystal structure and photochromism of 1-(2-ethyl-5-formylthiophen-3yl)-2-(2-cyano-1,5-dimethyl-4-pyrrl)-3,3,4,4,5,5-hexafluorocyclopent-1-ene, C19H14F6N2OS
  64. Crystal structure of 2-(4-bromophenyl)-1,3-dimethyl-1H-perimidin-3-ium iodide, C19H16BrIN2
  65. Crystal structure of 2-(4-(dimethylamino)phenyl)-10-methylacridin-9(10H)-one, C22H20N2O
  66. Crystal structure of 4-(acetoxymethyl)-6-(3-acetyl-3-(4-fluorophenyl)thioureido)cyclohex-4-ene-1,2,3-triyl triacetate, C24H26FN2O9S
Heruntergeladen am 21.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2018-0138/html
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